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TriStar II 3020 Operator's Manual

TriStar II 3020 Operator's Manual

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Published by: Rosario Isidro Yocupicio Gaxiola on Jun 05, 2013
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TriStar II 3020

Operator’s Manual
V1.03

302-42801-01 July 2009

Adobe Acrobat Reader is a registered trademark of Adobe Systems, Inc. Alconox is a registered trademark of the Alconox Company. Fomblin is a resistered trademark of Solvay S.A. Micromeritics is a registered trademark of Micromeritics Instrument Corporation. Microsoft, Windows, and Windows Vista are registered trademarks of Microsoft Corporation.

© Micromeritics Instrument Corporation 2008-2009. All rights reserved. The software described in this manual is furnished under a license agreement and may be used or copied only in accordance with the terms of the agreement.

WARRANTY
MICROMERITICS INSTRUMENT CORPORATION warrants for one year from the date of shipment each instrument it manufactures to be free from defects in material and workmanship impairing its usefulness under normal use and service conditions except as noted herein. Our liability under this warranty is limited to repair, servicing and adjustment, free of charge at our plant, of any instrument or defective parts when returned prepaid to us and which our examination discloses to have been defective. The purchaser is responsible for all transportation charges involving the shipment of materials for warranty repairs. Failure of any instrument or product due to operator error, improper installation, unauthorized repair or alteration, failure of utilities, or environmental contamination will not constitute a warranty claim. The materials of construction used in MICROMERITICS instruments and other products were chosen after extensive testing and experience for their reliability and durability. However, these materials cannot be totally guaranteed against wear and/ or decomposition by chemical action (corrosion) as a result of normal use. Repair parts are warranted to be free from defects in material and workmanship for 90 days from the date of shipment. No instrument or product shall be returned to MICROMERITICS prior to notification of alleged defect and authorization to return the instrument or product. All repairs or replacements are made subject to factory inspection of returned parts. MICROMERITICS shall be released from all obligations under its warranty in the event repairs or modifications are made by persons other than its own authorized service personnel unless such work is authorized in writing by MICROMERITICS. The obligations of this warranty will be limited under the following conditions: 1. Certain products sold by MICROMERITICS are the products of reputable manufacturers, sold under their respective brand names or trade names. We, therefore, make no express or implied warranty as to such products. We shall use our best efforts to obtain from the manufacturer, in accordance with his customary practice, the repair or replacement of such of his products that may prove defective in workmanship or materials. Service charges made by such manufacturer are the responsibility of the ultimate purchaser. This states our entire liability in respect to such products, except as an authorized person of MICROMERITICS may otherwise agree to in writing. If an instrument or product is found defective during the warranty period, replacement parts may, at the discretion of MICROMERITICS, be sent to be installed by the purchaser, e.g., printed circuit boards, check valves, seals, etc. Expendable items, e.g., sample tubes, detector source lamps, indicator lamps, fuses, valve plugs (rotor) and stems, seals and O-rings, ferrules, etc., are excluded from this warranty except for manufacturing defects. Such items which perform satisfactorily during the first 45 days after the date of shipment are assumed to be free of manufacturing defects.

2.

3.

Purchaser agrees to hold MICROMERITICS harmless from any patent infringement action brought against MICROMERITICS if, at the request of the purchaser, MICROMERITICS modifies a standard product or manufactures a special product to the purchaser’s specifications. MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its products other than the liability stated above. This warranty is in lieu of all other warranties, express or implied, including, but not limited to, the implied warranties of merchantability or fitness for use.

4356 Communications Drive Domestic Sales - (770) 662-3633 International Sales - (770) 662-3660

Norcross, GA 30093-1877

Fax (770) 662-3696

Domestic Repair Service - (770) 662-3666 Customer Service - (770) 662-3636

TriStar II 3020

Table of Contents

TABLE OF CONTENTS

1. GENERAL DESCRIPTION
Organization of the Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Equipment Description. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Krypton Option . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Vacuum Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Degasser . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Internet Access . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1 1-3 1-4 1-4 1-5 1-5 1-6 1-7 1-8

2. USER INTERFACE
Instrument Components and Connectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Front Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Sample Compartment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Side Panel. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Rear Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Turning the Analyzer On and Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Turning the Analyzer On . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Turning the Analyzer Off. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Using the Software. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Shortcut Keys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Dialog Boxes and Subdialog Boxes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Selecting Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Selecting Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . File Name Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . How-To Videos . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Installation Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Online Manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Using Bookmarks. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Using the Table of Contents, Index, and other Links. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Table of Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Cross References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Using the Find Command . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Printing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Menu Structure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Main Menu Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Windows Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Help Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1 2-1 2-2 2-3 2-4 2-5 2-5 2-5 2-6 2-6 2-6 2-8 2-11 2-13 2-14 2-15 2-15 2-17 2-17 2-19 2-19 2-20 2-20 2-21 2-22 2-23 2-23 2-24 2-24

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TriStar II 3020

3. OPERATIONAL PROCEDURES
Specifying Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1 Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1 Basic Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-4 Defining Parameter Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6 Sample Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-6 Degas Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-8 Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-9 Adsorptive Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-10 Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-12 Creating a Sample Information File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14 Advanced Format . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-14 Basic and Restricted Formats . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-16 Preparing for Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-18 Cleaning and Labeling Sample Tubes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-18 Determining the Sample Mass . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-21 Degassing the Sample. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-23 Installing the Sample Tube . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-24 Installing the Analysis Dewar. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-25 Performing an Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-27 Standard Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-27 QuickStart Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-29 Printing File Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-31 Listing File Statistics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-33 Exporting Isotherm Data. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-34 Generating Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-35 Multiple Sample Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-35 Multiple Graph Overlays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-38

4. SOFTWARE AND SETUP MODIFICATIONS
Installing the Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1 Using the Setup Program for Other Functions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6 Installing Subsequent Software Versions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-8 Adding an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9 Ethernet Switch . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-9 Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-10 Moving an Analyzer from One Computer to Another Computer. . . . . . . . . . . . . . . . . . . . . 4-11 Moving a Configured Analyzer to a New Computer . . . . . . . . . . . . . . . . . . . . . . . . . . 4-11 Moving a Configured Analyzer to a Computer with an Existing Analyzer . . . . . . . . . 4-15 Removing an Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-16 Changing the Analyzer Setup Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-17 Reinstalling Calibration Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-19 Uninstalling the Analysis Program . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-20

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Table of Contents

5. FILE MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Open . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Sample Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Restricted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Sample Tube. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Degas Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Analysis Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Adsorptive Properties. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Summary Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Isotherm Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . BET/Langmuir Surface Area Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Freundlich Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Temkin Isotherm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . t-Plot Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Alpha-S Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . f-Ratio Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . BJH Adsorption/Desorption Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Dollimore-Heal Adsorption/Desorption Report Options . . . . . . . . . . . . . . . . . . . . . . . Horvath-Kawazoe Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . DFT Pore Size . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . DFT Surface Energy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Dubinin Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . MP-Method Report Options. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Options Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Sample Log Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Validation Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Entered or Collected Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Save . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Save As. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Sample and Parameter Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . t-Curve and Alpha-S Files . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Save All . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Close. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Close All. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Print . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Export. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Format of Data Output . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Convert. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Exit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1 5-3 5-4 5-5 5-8 5-10 5-11 5-13 5-15 5-28 5-31 5-35 5-37 5-39 5-42 5-44 5-46 5-52 5-55 5-57 5-64 5-65 5-71 5-74 5-75 5-80 5-85 5-85 5-86 5-87 5-91 5-91 5-92 5-92 5-93 5-93 5-93 5-94 5-95 5-96 5-97 5-98 5-99

6. UNIT MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1 Sample Analysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-3

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QuickStart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-8 Krypton Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-11 Blank Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-12 Enable Manual Control. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-14 Show Instrument Schematic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-17 Show Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-19 Show Instrument Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-21 Unit Configuration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-23 Diagnostics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-24 Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-27 Zero Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-27 Match Transducers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-28 Servo Valve. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-28 Store Instrument Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-29 Save to File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-29 Load from File . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-30 Service Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-30

7. REPORTS MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1 Start Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-3 Close Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5 Open Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-5 SPC Report Options . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-6 Regression Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-7 Control Chart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-11 Heat of Adsorption Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-15 Printed Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19 Header. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19 Onscreen Reports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-19 Tool Bar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-20 Shortcut Menus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-24 Zoom Feature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-28 Axis Cross Hair. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-28 Report Examples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-29 Isotherm Plot. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-30 BET Surface Area Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-31 BET Surface Area Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-32 t-Plot Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-33 BJH Adsorption: Cumulative Pore Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-34 BJH Desorption: Pore Volume Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-35 Dollimore-Heal Desorption: Pore Volume/Area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-36 Summary Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-37 Sample Log Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-38

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8. OPTIONS MENU
Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Option Presentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Restricted . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Sample Defaults . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Advanced . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Basic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Units . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Graph Grid Lines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Live Graph . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Parameter Files Directory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Service Test Mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1 8-2 8-3 8-4 8-5 8-6 8-6 8-10 8-12 8-13 8-14 8-15 8-15

9. TROUBLESHOOTING AND MAINTENANCE
Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Preventive Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Lubricating Elevator Drive Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Cleaning the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Cleaning the Analysis Dewar. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Replacing Port Filter and O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Replacing the Sample Tube O-ring . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Inspecting and Changing Vacuum Pump Oil. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Inspecting the Oil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Changing or Adding Oil . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Replacing the Alumina in the Oil Vapor Trap . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Changing the Vacuum Pump Exhaust Filter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Performing a Leak Test . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Connecting Gases. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Guidelines for Connecting Gases to the Analyzer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Disconnecting the Depleted Bottle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Connecting a Replacement Gas Bottle. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Cleaning and Verifying the Gas Line. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Specifying Gas Ports . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Calibrating the System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Zero Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Match Transducers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Servo valve. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1 9-3 9-4 9-4 9-4 9-6 9-7 9-8 9-8 9-8 9-11 9-15 9-16 9-19 9-19 9-19 9-21 9-24 9-28 9-29 9-29 9-30 9-30

10. ORDERING INFORMATION

A. FORMS
Sample Data Worksheet. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-3

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B. ERROR MESSAGES
2400 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2500 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4000 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6000 Series . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1 B-12 B-18 B-34

C. CALCULATIONS
Saturation Pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1 Relative Pressure Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1 Volume Adsorbed Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3 Free Space. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3 Measured. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-3 Calculated . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-4 Equilibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-5 Thermal Transpiration Correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-6 BET Surface Area. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-7 Langmuir Surface Area. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-9 t-Plot . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-10 BJH Pore Volume and Area Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-12 Explanation of Terms . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-12 Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-13 Compendium of Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-21 Horvath-Kawazoe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-22 Slit Pore Geometry (original HK). . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-22 Cylinder Pore Geometry (Saito/Foley) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-23 Sphere Pore Geometry (Cheng/Yang) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-24 Cheng/Yang Correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-25 Interaction Parameter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-26 Additional Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-27 Interaction Parameter Components. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-28 Dubinin-Radushkevich . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-30 Dubinin-Astakhov. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-32 MP-Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-36 Freundlich Isotherm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-38 Temkin Isotherm. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-39 DFT (Density Functional Theory) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-40 The Integral Equation of Adsorption . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-40 Application to Surface Energy Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-41 Application to Pore Size Distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-41 Performing the Deconvolution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-42 Regularization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-42 SPC Report Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-43 Regressions Chart Variables. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-43 Control Chart Variables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-43 Summary Report. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-45 References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-47

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Table of Contents

D. FREE-SPACE CORRECTION
Measure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-2 Calculate. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-2 Enter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-3

E.

ETHERNET CONFIGURATION
E-1 E-1 E-4 E-7 E-7 E-8

Configuring the Ethernet Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Windows XP Professional . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Windows Vista . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Configuring the Firewall Setting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Windows XP Professional . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Windows Vista . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

F. DFT MODELS
Models Based on Statistical Thermodynamics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Theoretical Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Molecular Simulation Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Molecular Dynamics Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Monte Carlo Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Density Functional Formulation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Models Included. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Non-Local Density Functional Theory with Density Independent Weights . . . . . . . . Modified Non-Local Density Functional Theory with Density-Dependent Weights . Models Based on Classical Theories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Surface Energy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Pore Size. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Models Included. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Kelvin Equation with Halsey Thickness Curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Kelvin Equation with Harkins and Jura Thickness Curve . . . . . . . . . . . . . . . . . . . . . . Kelvin Equation with Broekhoff-de Boer Thickness Curve . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1 F-1 F-2 F-2 F-2 F-3 F-7 F-7 F-7 F-11 F-11 F-11 F-12 F-12 F-12 F-13 F-15

G. MAINTAINING HIGH PURITY GASES
Using Metal Gas Lines. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Removing Trapped Air. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Purge Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Evacuation Method. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . G-1 G-1 G-2 G-3

INDEX

Jul 09

vii

TriStar II 3020

Organization of the Manual

1. GENERAL DESCRIPTION
This manual provides a description of the TriStar 3020, its menu options, and operating instructions. Installation instructions are located on the installation disk included with your software. To help you operate the TriStar more efficiently: • read Chapter 2, User Interface, before operating the analyzer and its software • use the step-by-step instructions in Chapter 3 when performing common operations

Organization of the Manual
This operator’s manual is organized as follows: Chapter 1 GENERAL DESCRIPTION Provides a general description of the TriStar 3020 and its features and specifications. Chapter 2 USER INTERFACE Provides instrument and software interface. Chapter 3 OPERATIONAL PROCEDURES Provides step-by-step procedures for the operations performed with the TriStar 3020. Chapter 4 SOFTWARE AND SETUP MODIFICATIONS Provides instructions for installing software updates and for modifying analyzer setup configurations. Chapter 5 FILE MENU Provides a description of the choices available on the File menu. Chapter 6 UNIT MENU Provides a description of the choices available on the Unit menu. Chapter 7 REPORTS MENU Provides a description of the choices available on the Reports menu.

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Organization of the Manual

TriStar II 3020

Chapter 8

OPTIONS MENU Provides a description of the choices available on the Options menu.

Chapter 9

TROUBLESHOOTING AND MAINTENANCE Provides user maintenance and service information.

Chapter 10

ORDERING INFORMATION Provides ordering information for TriStar system components.

Appendix A

FORMS Contains a copy of the Sample Information Worksheet. This form is used to assist you in obtaining your sample mass.

Appendix B

ERROR MESSAGES Lists the error messages that may be displayed by the software and includes a cause and action for each.

Appendix C

CALCULATIONS Provides the calculations used by the TriStar program.

Appendix D

FREE-SPACE CORRECTION Provides a discussion of the free-space measurements available with TriStar.

Appendix E

ETHERNET CONFIGURATION Provides information on configuring an ethernet port and specifying firewall settings.

Appendix F

DFT MODELS Provides information on DFT models.

Appendix G

MAINTAINING HIGH PURITY GASES Provides information on the importance of maintaining high purity gases.

Index

INDEX Provides quick access to a subject matter.

1-2

Apr 08

TriStar II 3020

Organization of the Manual

Conventions
This manual uses the icons shown below to identify notes of importance, cautions, and warnings.
Notes contain important information pertinent to the subject matter.

Warnings contain information that help you prevent actions that may cause personal injury.

Cautions contain information that help you prevent actions that may damage the analyzer or one of its components.

Apr 08

1-3

Equipment Description

TriStar II 3020

Equipment Description

The TriStar 3020 is an automated gas adsorption analyzer which contains three ports, allowing you to analyze up to three samples simultaneously. Also featured is a dedicated port for measuring the saturation pressure (Po) on a continuous basis. Surface areas as low as 0.01 m2/g can be measured using nitrogen and as low as 0.001 m2/g with the Krypton option. Up to 1000 data points can be collected, allowing you to observe minute details of the isotherm. You can operate up to four TriStar analyzers with one computer. The TriStar II 3020 system consists of the TriStar analyzer, a SmartPrep degasser (optional) for preparing samples, a vacuum pump, and a computer for entering analysis and report options.

Krypton Option
The Krypton option enables you to measure surface areas as low as 0.001 m2/g using krypton as the adsorptive. Your TriStar system must be equipped with a 10-mmHg transducer and a high-vacuum pump to provide this capability. Refer to Ordering Information, page 10-1 for ordering information.

1-4

Apr 08

TriStar II 3020

Equipment Description

Software
The TriStar 3020 analysis program operates in a Windows® environment. This makes operation of the TriStar easier and allows you to run other applications while an automatic operation is in progress. The report system provided in the analysis program allows you to manipulate and customize reports in a variety of ways. You can zoom in on portions of the graphs or shift the axes to examine fine details. Scalable graphs can be copied to the clipboard and pasted into other applications. Reports can be customized with your choice of fonts and a company logo added to the report header for an impressive presentation. Refer to Onscreen Reports, page 7-19 for the options available for reports. To make it easier for you to obtain information, an online manual is included on the Help menu. This enables you to access the desired information in just a couple of mouse clicks. Refer to Online Manual, page 2-17 for additional information and navigation methods. Also included on the Help menu are a variety of How-To videos. These videos are designed to visually step you through procedures such as creating sample files, changing the vacuum pump oil and alumina, etc.

Vacuum Pump
A vacuum pump is required for sample analysis with the TriStar analyzer. Vacuum pumps used with the TriStar must meet the following criteria. They must: • be able to achieve vacuums better than 20 µmHg at the instrument inlet • contain an anti-suckback valve to prevent vacuum pump oil from backing up into the analyzer in the event of a vacuum pump failure • contain an NW16 inlet port for connection to the TriStar An oil-based or oil-free vacuum pump can be used with the TriStar (an oil-free pump is required if you have the Krypton option installed). Appropriate vacuum pumps are available from Micromeritics. (Refer to Ordering Information, page 10-1 for ordering information.)

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1-5

Equipment Description

TriStar II 3020

Degasser
Micromeritics has available the following degassing units for preparing samples: • SmartPrep 065 The SmartPrep uses flowing-gas to remove adsorbed contaminants from the surface and pores of your sample. It contains six sample ports, each one independently controlled for greater flexibility. It contains two serial ports, one for connecting to the computer and the other available for connecting an additional SmartPrep. In fact, you can connect up to four SmartPreps, one to the other, allowing the capability of up to 24 preparation ports at one time. The SmartPrep also can be controlled through the TriStar application and is the recommended degassing unit for the TriStar. • VacPrep 061 The VacPrep degasses up to six samples at up to 400 ºC with either flowing gas or evacuation. • FlowPrep 060 The FlowPrep degasses up to six samples at up to 400 ºC with flowing gas. Refer to Chapter 10, page 10-1 for ordering information.

1-6

Apr 08

TriStar II 3020

Internet Access

Internet Access
Visit www.micromeritics.com to learn more about Micromeritics, our products, and applications. Our site is user-friendly, easy to navigate, and informative. Its content is summarized below.
About Micromeritics

A brief history of Micromeritics, office locations, awards/certifications, career opportunities, and a virtual tour of its headquarters Product information and printable brochures Application Notes, Product Bulletins, Tech Tips, Technical Articles/papers, and important application links Catalog of instruments and accessories, allowing you to place your order online Press releases, Events calendar, microReports, and latest Micromeritics news updates Provides laboratory tips and access to the Micromeritics Analytical Services web site Customer support contacts, product registration, instrument training information, Material Safety Data Sheets, and account registration Details of the Grant Program established for non-profit organizations and universities Contact information, office locations, maps and driving directions to the Micromeritics facility, and registration for the microReport newsletter

Products Applications

Online Catalog

News and Press

Lab Service

Customer Support

Grant Program

Contact Us

Be sure to browse our site to see the many ways in which we can assist you.

Apr 08

1-7

Specifications

TriStar II 3020

Specifications
The TriStar 3020 has been designed and tested to meet the specifications provided below.
Characteristic Specification Pressure Measurement

Absolute Range: Resolution: Accuracy: Linearity: Relative P/Po range: Resolution:

0 to 950 mmHg Within 0.05 mmHg Within 0.5% Within 0.25% of full scale (transducer manufacturer’s specification) 0 to 1.0 P/Po < 10-4
Analysis

Specific Surface Area: Total Surface Area: Pore Volume: Dewar duration:

From 0.01 m2/g, nitrogen unit From 0.001 m2/g, krypton unit From 0.1 m2, nitrogen unit From 0.01 m2, krypton unit From 4 x 10-6 cm3/g > 24 hours
Adsorptive Gases

Nitrogen unit:

Nitrogen; argon, carbon dioxide, or other non-corrosive gases; butane, methane, or other light hydrocarbon vapors. Oxygen can also be used only with an appropriate vacuum pump. Same as Nitrogen unit, plus the capability to perform krypton surface area analyses at lower pressures.

Krypton unit:

The TriStar should be operated in a properly vented environment when using flammable or toxic gases.
Manifold Temperature

Accuracy: Resolution:

± 0.25 ºC Within 0.1 ºC

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Apr 08

TriStar II 3020

Specifications

Characteristic

Specification Vacuum System

Nitrogen unit: Krypton unit:

Must accommodate 20 x 10-3 mmHg or better; uses oil-based or oilfree vacuum pump Must accommodate 0.1 x 10-3 mmHg; oil-free vacuum pump required
Environment

Temperature: Humidity:

10 and 35 ºC (50 to 95 ºF), operating; 0 to 50 ºC (0 to 122 ºF), nonoperating 20 to 80% relative, noncondensing
Physical

Height: Width: Depth: Weight:

74 cm (29 in.) 40 cm (16 in.) 51 cm (20 in.) 37 kg (82 lbs)
Electrical

Voltage: Power: Frequency:

100/120, 220/240 VAC 150 VA, maximum 50 to 60 Hz
Computer

Minimum requirements:

Pentium 333 MHz computer (or equivalent) 512 megabytes of main memory 20-gigabytes hard drive Ethernet port (capable of communicating with a 10 base-T ethernet card) CD-ROM drive 1024 x 768 video display capability Windows® XP Professional or Windows Vista® operating system

Apr 08

1-9

TriStar II 3020

Instrument Components and Connectors

2. USER INTERFACE
This chapter contains information to familiarize you with the hardware and software components of the TriStar II 3020. It is recommended that you read this chapter before attempting to operate the TriStar system.

Instrument Components and Connectors
Front Panel

Power indicator

Blinks when power is applied to the analyzer; illuminates when analysis program is initiated and ready for operation. Sliding door which encloses the sample compartment.

Sample Compartment door

Mar 09

2-1

Instrument Components and Connectors

TriStar II 3020

Sample Compartment

Sample ports (three)

Saturation pressure (Po) tube

Diagram of port locations

Elevator

Sample ports

For installing sample tubes; you can install up to three sample tubes. For measuring the saturation pressure. Provides a pictorial representation of port numbers and their locations. Allows placement of the Dewar around the sample and Po tubes.

Po tube Diagram

Elevator

2-2

Mar 09

TriStar II 3020

Instrument Components and Connectors

Side Panel

Ethernet connector

RS232 connector

Ethernet connector

For connecting the ethernet cable, allowing communication between the analyzer and the computer. Used by service personnel to perform calibration procedures.

RS-232 connector

Mar 09

2-3

Instrument Components and Connectors

TriStar II 3020

Rear Panel
Analysis inlet valves

Vacuum Pump connector

Maximum inlet pressure

Helium inlet valve

On/Off switch

Power cord connector

Gas Inlet Valves

Inlets V8, V9, and V14 are for analysis gases; inlet V7 is dedicated to helium. For attaching the vacuum pump hose. For turning the analyzer on and off. For connecting the analyzer to the power supply.

Vacuum Pump connector On/Off switch Power connector

2-4

Mar 09

TriStar II 3020

Turning the Analyzer On and Off

Turning the Analyzer On and Off
Turning the Analyzer On
1. Place the computer, monitor, and printer ON/OFF switches in the ON position. 2. Place the TriStar analyzer ON/OFF switch in the ON ( | ) position. The pump will turn on automatically if it is plugged into the electrical outlet; allow the pump to operate for two hours before performing analyses.

Turning the Analyzer Off
Always exit the analysis program and Windows before turning off the computer. Failure to do so could result in loss of data.

1. Select Close from the System menu or Exit from the File menu. If an analysis is in progress, the following message is displayed:
2459- An Instrument is busy. A delay in restarting this application could result in loss of new data. Continue program exit? Yes No

If you click Yes and the analysis program closes, the analysis continues and data continue to be collected. Reports that are queued under the Print Manager will print. If, however, a power failure occurs and an uninterruptible power supply (UPS) is not attached to the analyzer, the data collected after exiting the analysis program are lost. 2. Place the computer, monitor, and printer ON/OFF switches in the OFF position. 3. Place the TriStar analyzer ON/OFF switch in the OFF position.

Mar 09

2-5

Using the Software

TriStar II 3020

Using the Software
The TriStar 3020 analysis program operates in the Windows environment and requires familiarity with standard Windows operations such as using the mouse, menus, and dialog boxes. While this manual provides brief instructions for such standard operations, you may have to refer to your Windows documentation or to its online help system to clarify functions which are specific to Windows.

Shortcut Menus
Shortcut menus (sometimes referred to as context-sensitive menus or pop-up menus) are available for certain components on the instrument schematic when in manual mode, and for onscreen graphs and tabular reports. These menus are accessed by selecting the item for which you want to display its menu and clicking the right mouse button. For example, right-click in a column of an onscreen report and the following menu is displayed.

Shortcut Keys
Shortcut keys can be used to activate some menu commands. Shortcut keys or key combinations (if assigned) are listed to the right of the menu item. Instead of opening the menu and choosing the command, simply press the key combination. For example, to open a sample information file, press F2; the Open Sample Information dialog is displayed. You can also use shortcut keys to access a menu or any function that contains an underlined letter by pressing Alt plus the underlined letter in the command. For example, to access the File menu, press Alt, then F. Table 2-1 provides a list of the keys available in the TriStar 3020 analysis program.

2-6

Mar 09

TriStar II 3020

Using the Software

Table 2-1. Shortcut Keys
Key(s) F1 F2 Function

Access online operator’s manual Open a sample information file Clear the field of existing date (Select Dates dialog) Open an analysis conditions file Insert the current date (select Dates dialog) Open an adsorptive properties file Display a calendar to choose a date (Select Dates dialog) Open a report options file Tile windows Cascade windows Start a report Close all open reports Generate a Heat of Adsorption report Exit the analysis program List sample information files List analysis conditions files List adsorptive properties files List report options files Access shortcut menu of (1) selected component on instrument schematic, or (2) onscreen reports

F3

F4

F5 F6 F7 F8 F9 F10 Alt + F4 Shift + F2 Shift + F3 Shift + F4 Shift + F5 Shift + F9

Mar 09

2-7

Using the Software

TriStar II 3020

Dialog Boxes and Subdialog Boxes
Dialog boxes are displayed when an item followed by an ellipsis (...) is selected. Subdialog boxes are displayed when a push button on a dialog box is selected. Both types of dialogs may contain one or more of the following:

Dialog box

Subdialog box

Data entry field

These fields may be either numeric (numbers only) or alphanumeric (numbers, letters, or printable characters). If you make an invalid entry in either of these fields, an error message occurs.
Alphanumeric field

Numeric fields

2-8

Mar 09

TriStar II 3020

Using the Software

Information bar

Some dialog boxes contain information pertinent to the selected field in an information bar across the bottom of the dialog. For example, a range is shown for fields in which numeric entries are required.
Selected field

Displays range for selected field.

List

A list contains selections from which you may choose one or more items. To select an item on the list: Highlight the selection, then double-click or press the Spacebar. An item is selected when it is preceded with a check mark.

Indicates item is selected.

Push Button

A push button is used to display subdialog boxes in which to enter additional information about the subject matter. For example, this push button displays a dialog for specifying a range of dates (explained later in this chapter).

Push buttons also may be used to cause an action. For example, Cancel closes the open dialog, discarding any information you may have entered.

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Radio Button

Radio buttons are contained within a group box. These buttons are used to select options; you may choose only one item.

Check Box

Check boxes also are used to select options. You may make as many selections as you wish.

Drop-down List

A drop-down list is indicated by a down arrow to the right of the field. Drop-down lists contain a list of options from which you may choose one
Down Arrow

Some of the more commonly used push buttons are:
Browse

Displays a dialog which allows you to select a file for the subject matter. Allows you to copy file values from an existing file into the one you are creating. After the values have been copied into the file, you can edit them as desired. The file from which the values were copied is not affected and remains intact. Saves the information entered in the open dialog but allows the dialog to remain open.

Replace

Save

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Using the Software

Close

Closes the open dialog. If the dialog contains changes that have not been saved, you are prompted to save them before the dialog closes.

Selecting Files
Sample information is stored in files and saved under file names. Some dialogs contain a Files list window, which displays a list of files available for that particular operation. For example, the Open Sample Information dialog:
Choose a new Status category to limit the files displayed in the Files list box.

Click to specify a range of dates.

Choose the drive/directory. Choose the file you wish to open.

From the list of files in the Files list window, highlight the file you wish to open and doubleclick, or click OK. If you do not see the desired file, it may be in another directory. Go to the Directories list window and choose the correct drive and/or directory. You may limit the list of files displayed in the Files list window by choosing one or more of the following: • Use wildcard characters in the path name you enter in the File name field. Wildcard characters such as * and ? can be used to filter file names. For example, you can limit the list of files displayed to those beginning with 01 by entering 01*.smp.

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• Enter a range of dates. Click Date Range; the Select Dates dialog is displayed.

Select the Show Date Range radio button. This enables the From and To fields allowing you to enter a beginning and ending date. Alternatively, you can double-click in each field to display a calendar to set a date. The range of dates remains the default until you change the dates or select Show All Dates. For convenience, the following function keys are available when the Select Dates dialog is displayed:
F2 F3 F4

Clears the field Inserts the current date Displays a calendar from which to select a date

You can change the date format by using the International Date Format function on the Windows Control Panel.

• Select a file status from the Status drop-down list. Table 2-2 describes each file status. Table 2-2. File Status and Description
Status Description

All Analyzing Complete Entered No analysis Prepared Preparing

All sample information files in the specified directory and within the specified range of dates. Sample information files that are currently being used for analysis or are in the degassing process. Sample information files that were used in an analysis that has been completed. Sample information files that contain manually entered data. Sample information files that have not been used to perform an analysis. Sample information files that have been used in an automatic degas operation, but not for an analysis. Sample information files currently being used in an automatic degas operation.

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Using the Software

• Navigate to a different directory. The current directory is displayed above the Directories list window. You can change directories by double-clicking a directory in the Directories list window, double-clicking [...] to move up one level, or by entering the desired directory in the File Name field. For example, enter C:\3020\files\sample\*.smp to display sample files in the 3020\files\sample directory on your local drive.

Displays the current directory.

Double-click to move up one level.

Double-click to open the listed directory.

Selecting Reports
Reports are selected from the Report Options dialog, or any dialog containing a Selected Reports list. Simply select (highlight) the report and then double-click, or press the Spacebar. A report is selected when it is preceded with a check mark (3). Reports are deselected in the same manner.

Indicates a report is selected.

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File Name Conventions
For sample information files, a default file name (the next available sequence number) and a default extension display. For Sample tube, Degas conditions, Analysis conditions, Adsorptive properties, and Report options, only a default extension displays. The following table shows the file name extensions for the TriStar 3020 analysis program. Table 2-3. Default File Name Extensions
File Type Extension

Sample information Sample tube Degas conditions Analysis conditions Adsorptive properties Report options Export to disk (ASCII) Report to disk List to disk Thickness curve Alpha-s curve

SMP STP DEG ANC ADP RPO EXP RPT LST THK ALS

The following types are available for reports saved from the Report window: Report Spreadsheet ASCII REP XLS TXT

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Using the Software

How-To Videos
For your convenience and to make it easier for you to perform common operations, How-To videos have been included in the software. These videos visually step you through a procedure; for example, one of the How-To videos is designed to assist you in properly preparing your sample.

These videos are accessible from the Help menu; take a few minutes to view the ones available. Included in this group of videos is one entitled Using the How-to Videos. This module provides information and tips on using the videos; you may want to view this one first.

Installation Instructions
Also included, but not accessible from the Help menu, are the System Installation videos used for initial installation of your analyzer. To access these videos: 1. Open Windows Explorer and navigate to the directory in which you installed the application; the default directory is win3020 and is the directory shown in this example. 2. Double-click on the system installation directory to display its contents.

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3. Double-click on the file named Menu.exe; the menu for the Installation Instructions is displayed.

4. Click on the desired procedure to launch the video.

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Online Manual

Online Manual
For your convenience, the Operator’s Manual is available online. You can access the manual by selecting Help, then Operator’s Manual from the analysis program main menu. The manual appears in an Adobe® Acrobat® Reader®. Following are some tips to help you quickly locate the information you need in the manual. Refer to the Adobe Acrobat Help system (click the Help button on the Acrobat menu) for more information on the Acrobat features you can use while viewing the manual.

Using Bookmarks
Click the Bookmarks tab to list and access the topics included in the manual.

Bookmarks

Topics

Navigation Pane

Topic Pane

You can use the + and − buttons next to topics as they are used in Windows Explorer to expand or collapse the topic list.

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To display a topic, click the topic name in the Bookmarks section. The related information appears in the topic pane of the window as shown in the following example.

Click bookmark to display topic.

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Online Manual

Using the Table of Contents, Index, and other Links
Links provide direct access to selected information. All links appear in blue type. Links are contained in: • • • the table of contents index entries cross-references within the manual

Table of Contents To display the table of contents, click Table of Contents in the Bookmarks section. When the table of contents is displayed, you can click an entry to display its associated page. For example, clicking Using the Software in the table of contents, displays the page containing information about the software.

Click topic name in table of contents to display topic.

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Online Manual

TriStar II 3020

Index To use the index in the online manual, click the Bookmarks tab, scroll down to INDEX (the last topic in Bookmarks), then click the + button to expand the index. The letters A through Z are displayed. Click a letter to display its corresponding index entries as shown in the following example.

Click a letter to display its index entries.

After you display the entries, locate the item of interest and click on the page reference to access the information. Cross References Cross-references work in the same manner. In the example below, clicking on the crossreference, FILE MENU (shown on the screen in blue type) will display the first page of the chapter describing the commands found on the File menu.

FILE MENU Provides a description of the commands available on the File menu.

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Online Manual

Using the Find Command
The Adobe Acrobat Find command provides another method of easily accessing specific information. For example, suppose you want to know how the Save as command works. You could select Edit > Find from the Adobe Acrobat menu, then enter Save as in the Find dialog. The following example shows the results.

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Online Manual

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Printing
You can print the entire manual, a selected page, or range of pages. There are several options for printing. You can: • Select the printer icon ( ) on the Adobe Acrobat toolbar.

A standard Print dialog is displayed. Select the page(s) to print, then click OK. When using this option (or the next one), be sure to enter the page number(s) displayed in Adobe Acrobat; do not use the page number(s) listed in the footer(s) of the manual.
Do not use number in footer of the manual.

Enter this number.

Select File > Print. A standard Print dialog is displayed. Select the page(s) to print, then click OK.

Click the Thumbnails tab. Thumbnails of manual pages are displayed. a. Click the pages you want to print. b. Right-click to display a shortcut menu, then select Print Pages. c. A standard Print dialog is displayed; click OK.

Thumbnails tab

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Menu Structure

Menu Structure
SmartPrep drop-down menu displays here if a SmartPrep unit is being used with the TriStar.

Main Menu Bar
All functions for the TriStar 3020 are accessed from the main menu bar. Brief descriptions are provided below; refer to the chapter given in parentheses for a detailed description of the options contained on that menu.

File

Allows you to manage sample and parameter files. (Chapter 5, FILE MENU) Enables you to perform analyses, calibrations, and other instrument operations. (Chapter 6, UNIT MENU) Displays only if you have a SmartPrep degassing unit installed on the TriStar. The options contained on this menu are explained in the SmartPrep operator’s manual. Enables you to generate, close, and customize reports. (Chapter 7, REPORTS MENU) Allows you to edit sample defaults, specify your system configuration, and select data presentation formats. (Chapter 8, OPTIONS MENU) Enables you to arrange the windows and icons on your screen. It also displays the names of all open windows. (this chapter, page 2-24) Displays Help topics. (this chapter, page 2-24)

Unit [n]

SmartPrep

Reports

Options

Windows

Help

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Menu Structure

TriStar II 3020

Windows Menu

The choices on this menu allow you to arrange your open windows and icons. Tile Resizes all open windows and arranges them side by side so that the contents of all open windows are visible. Resizes all open windows and arranges them in a stacked fashion. The active window is positioned on top of the stack. Each window’s title remains visible, making it easy to select other windows. Arranges the symbols for all minimized windows in an orderly manner.

Cascade

Arrange Icons

The Windows menu also displays all open files; the active window is preceded with a check mark.

Help Menu

Help

Provides access to the online operator’s manual and the How-To videos. Displays information about the TriStar 3020 analysis program.

About TriStar 3020

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Specifying Sample Defaults

3. OPERATIONAL PROCEDURES
This chapter contains step-by-step procedures for operating the TriStar. It does not provide detailed descriptions of the fields in the dialogs used to perform these procedures. Chapters 5 though 8 contain details for the dialogs. At the beginning of each procedure, you will find the location of the dialog used in that procedure.

Specifying Sample Defaults
Sample information files include the information required by the TriStar to perform an analysis and collect data. The TriStar automatically generates sample information file names and assigns the default values which you specify. Sample defaults can be specified using the Advanced or Basic format.

Advanced Format
You can move from one set of parameters to another by clicking the parameter tab or by using Next and Prev. The values you specify in the parameter portions of the sample file (Sample Tube, Degas Conditions, Analysis Conditions, Adsorptive Properties, and Report Options) are saved as the defaults for newly created parameter files. For example, after specifying defaults for a sample file in the Advanced format: • Select File > Open > Sample Information, then click Yes to create the file, and the defaults you specify display for all parameters. • Select File > Open > Analysis Conditions, enter a file name; then click OK, and the defaults you specify in the Analysis Conditions portion of the Advanced Sample Defaults dialog display in the fields. Refer to Advanced, page 8-6 for a detailed description of the fields on this dialog.

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Specifying Sample Defaults

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1. Select Options > Sample Defaults; the Sample Defaults dialog is displayed.

2. In the Sequence field, specify a default string. This is the number that is incrementally sequenced and displays in the File name field when you select File > Open > Sample information. 3. In the field on the right of the Sample line, enter a format for the identification. Be sure to include the $ symbol if you wish to have the sample file number included as part of the identification. You can use up to 42 alphanumeric characters. You can also edit the label (Sample); for example, you may wish to use Sample Material. You can enter up to 15 characters in this field. 4. Edit the Operator and Submitter lines as desired. Or you may have either (or both) of these lines omitted entirely by selecting Omit. 5. If bar code information is not applicable, select Omit to omit this field from the sample information dialog. Or, if you prefer to use this line for some other type of information, edit the label. 6. You can enter a sample mass or have it calculated automatically; choose the desired method. • Enter: enter a default value in the Mass field. • Calculate: enter default values in the Empty tube and Sample+tube fields Regardless of which method you choose, the choice can be changed when you create a sample file.

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Specifying Sample Defaults

7.

Enter a default value in the Density field. This value is applicable only when using a calculated free space.

8. In the Type of Data group box, choose whether you wish to collect data automatically or enter it manually. 9. If you plan to report statistical process control (SPC) information, enter appropriate information. These are user-definable parameters that can be entered and tracked along with other statistical process control data; refer to Sample Defaults, page 8-8 for additional information on these parameters. 10. After you complete the Sample Information dialog, click on the parameter tabs to open associated dialogs; specify defaults as desired. The defaults you specify for parameters serve as the defaults for new parameter files. For example, the values you specify in the Analysis conditions portion of the sample file display as the default values for a newly created standalone Analysis conditions file. 11. Click Save, then Close.

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Specifying Sample Defaults

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Basic Format
Perform the following steps to establish defaults for a sample information file in the Basic format. The defaults you establish with this format also serve as defaults for files created

using the Restricted format.
When specifying defaults in the Basic format, you will have to select default parameter files. You may wish to define parameter files before entering sample defaults (refer to Defining Parameter Files, page 3-6). Refer to Basic, page 8-10 for a detailed description of the fields on this dialog. 1. Select Options > Sample Defaults; the Sample Defaults dialog is displayed.

2. In the Sequence field, specify a default string. This is the number that is incrementally sequenced and displays in the File name field when you select File > Open > Sample information. 3. In the field on the right of the Sample line, enter a format for the identification. Be sure to include the $ symbol if you wish to have the sample file number included as part of the identification. You can use up to 42 alphanumeric characters You can also edit the label (Sample); for example, you may wish to use Sample Material. You can enter up to 15 characters in this field.

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Specifying Sample Defaults

4.

You can enter a sample mass or have it calculated automatically; choose the desired method. • Enter: enter a default value in the Mass field. • Calculate: enter default values in the Empty tube and Sample+tube fields Regardless of which method you choose, the choice can be changed when you create a sample file.

5.

Enter a default value in the Density field. This value is applicable only when using a calculated free space.

6. Select the down arrow to the right of the following fields to choose default parameter files: • • • • • Sample Tube Degas Conditions Analysis Conditions Adsorptive Properties Report Options

7. Click Save, then Close.

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Defining Parameter Files

TriStar II 3020

Defining Parameter Files
The following file types can exist as part of the sample information file, as well as individual parameter files: • • • • • Sample tube Degas conditions Analysis conditions Adsorptive properties Report options

Having these files exist independently allows you to use them over and over again. Several predefined parameter files are included with the TriStar program. Although these files may come close to the needs of your laboratory, you may wish to define additional ones. Or you can use a predefined file as a starting point. You can do this by creating a new file and then clicking Replace. A dialog is displayed so that you can select the existing parameter file. Then you can make any changes you need to make and the original file remains unchanged. Make sure you save these files to the directory specified as the Parameter File directory, or they will not be included in the drop-down lists on the Basic and Restricted sample information dialogs. Unless you have changed the parameter file directory, the software defaults to the correct directory (refer to Parameter Files Directory, page 8-15 for detailed information). Parameter files may be created using either the Basic or Advanced format.

Sample Tube
Sample tube files are applicable only when using Calculate as the free-space method. Refer to Sample Tube, page 5-11 for a detailed description of the fields on this dialog. Be sure you have performed a blank analysis using the sample tube for which you are creating a Sample Tube file. You will use the data obtained from the blank analysis in your Sample Tube file. 1. Selct File > Open > Sample Tube; the Open Sample Tube File dialog is displayed. 2. Enter a name in the File name field, then click OK.

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Defining Parameter Files

3. Click Yes to create the file; the Sample Tube dialog is displayed:

4. Enter a description in the Sample Tube field. Be sure to use an intuitive description so that you can recognize it easily. Most users enter the serial number of the sample tube and/or size. 5. Click Load from Sample File; the Open Sample Information File dialog is displayed. 6. Select the file you used in the blank run with this sample tube, then click OK to copy the data for the warm and cold free space and the non-ideality factor into the Sample Tube dialog. 7. Select whether a filler rod and/or an isothermal jacket was used in the blank run. 8. If a vacuum seal was used, select the one you used; if not, leave the default of None selected. 9. Click Save, then Close.

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Defining Parameter Files

TriStar II 3020

Degas Conditions
Degas Conditions files contain degassing information for sample preparation. These files are used only if you are using the SmartPrep Degasser. Refer to Degas Conditions, page 5-13 for a detailed description of the fields on this dialog. 1. Select File > Open >Degas conditions; the Degas Conditions dialog is displayed. 2. Enter a name in the File name field, then click OK. 3. Click Yes to create the file; the Degas Conditions dialog is displayed:

4. Enter a description in the Description field. Be sure to use an intuitive description so that you can recognize it easily. 5. Enter up to five stages of degassing (soak temperature, ramp rate, and soak time). 6. Click Save, then Close.

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Defining Parameter Files

Analysis Conditions
Analysis conditions specify the data used to guide an analysis. Refer to Analysis Conditions, page 5-15 for a detailed description of the fields on this dialog. 1. Select File > Open > Analysis conditions; the Analysis Conditions dialog is displayed. 2. Enter a name in the File name field, then click OK. 3. Click Yes to create the file; the Analysis Conditions dialog is displayed:

4. Enter a description in the Description field. Be sure to use an intuitive description so that you can recognize it easily. 5. Choose whether you wish to have the isotherm collected by target pressures or in dose increments. Use the push button(s) adjacent to your choice to specify details. 6. Click Preparation to specify evacuation rate and time, and leak test values. 7. Click Free Space to specify how the free space is to be measured. 8. Click pº and T to specify how the saturation pressure (Po) is to be measured and the analysis bath temperature. 9. Click Equilibraiton to specify the equilibration times for relative pressure ranges. 10. Click Backfill to choose backfill options. 11. Click Save, then Close.

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Defining Parameter Files

TriStar II 3020

Adsorptive Properties
Adsorptive properties provide the adsorptive (analysis gas) characteristics for the analysis. Refer to Adsorptive Properties, page 5-28 for a detailed description of the fields on this dialog. 1. Select File > Open > Adsorptive properties; the Open Adsorptive Properties dialog is displayed. 2. Enter a name in the File name field, then click OK. 3. Click Yes to create the file; the Adsorptive Properties dialog is displayed:

4. Enter a description in the Adsorptive field; most users enter the gas and the temperature. 5. Enter the mnemonic for the Adsorptive gas; for example, N2. 6. Click Psat vs. T to view or edit the values in the Psat vs. Temperature table.

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Defining Parameter Files

7. Select the Non-condensing Adsorptive option if this file is to be used for a noncondensing gas. 8. Enter information (or accept the defaults) in the following fields: Maximum manifold pressure Non-ideality factor Density conversion factor Therm. tran. hard-sphere diameter Molecular cross-sectional area 9. Select the applicable dosing method; choose From Psat tube for krypton and Normal for all other gases. 10. Click Save, then Close.

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Defining Parameter Files

TriStar II 3020

Report Options
Report options files specify the type of reports which can be generated from an analysis or from manually entered data. They also contain report details such as axis scale, axis range, and column headings. These report options files may be used to generate reports automatically at any time during or after the analysis. Of course, reports generated during analysis can only report on data collected up to the time of the report. Report options files may contain tabular reports only, plots only, or both tabular reports and plots. They may also contain user-defined report tables. Report options files also may be defined to include overlay options. The TriStar program enables you to overlay up to eight plots of different samples onto a ninth plot of the same type. Or you can overlay one plot type onto a different plot type from the same analysis. Refer to Generating Graph Overlays, page 3-35 for instructions on generating overlays. Refer to Report Options, page 5-31 for a detailed description of the fields on this dialog. 1. Select File > Open > Report Options; the Open Report Options File dialog is displayed. 2. Enter a name in the File name field, then click OK. 3. Click Yes to create the file; the Report Options dialog is displayed:

4. Enter a description (up to 42 characters) in the Description field. Enter an identifier that gives a more intuitive description of the file’s contents. For example, BJH Adsorption Report Options.

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Defining Parameter Files

5. Select Show report title and enter the title you wish to appear at the top of the report. Deselect this option if you prefer not to have a report title.
If your company logo exists as a bitmap (bmp) or enhanced metafile (emf), you can have it display in the report header by selecting Show graphic. Click Browse to select the file; use the Height and Width fields to specify the size.

6. If you wish to compare the same type of graph from multiple files, click Overlays and choose the files. Then be sure you edit the graph from the Selected Reports window and choose Samples from the Overlay drop-down list. 7. The reports that may be generated are listed in the Selected Reports list. a. Double-click on the reports you wish to include in this file; this places a check mark before them and indicates they are selected. b. Click Edit to specify report options; be sure the report is highlighted and selected. 8. Click Save, then Close.

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Creating a Sample Information File

TriStar II 3020

Creating a Sample Information File
Whether you choose to create your sample file in advance or at the time of analysis, a sample information file must be created for each analysis. The sample information file consists of information groups which, collectively, identify the sample, guide the analysis, and specify report options. A sample file may be created in any of the sample presentation formats: • Advanced. This format provides complete access to all parts of the sample file, allowing you to edit parameters quickly and conveniently. • Basic. This format presents a single window from which you select predefined parameter files. You can also switch to the Advanced format if you wish to view or edit details. • Restricted. This format presents a single window from which you select predefined parameter files. You cannot, however, switch to the Advanced format for editing.

Advanced Format
The Advanced format presents all parts of the sample file in an index card manner. This format lets you customize your sample file, allowing you quick access to all parameters. Refer to Advanced, page 5-5 for a detailed description of the fields on this dialog. 1. Select File > Open > Sample Information; the Open Sample Information File dialog is displayed. 2. Accept the next sequenced file number or enter a new name in the File name field. 3. Click OK, then Yes to create the file; the Sample Information dialog is displayed.

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Creating a Sample Information File

These fields may not display if omitted in sample defaults.

4. Enter a description in the Sample field, or edit the one established in sample defaults. 5. In the Operator field, enter the name of the person who will be performing the analysis. 6. In the Submitter field, enter the name of the department, company, etc. submitting the sample for analysis. 7. Select Enter to enter a value for the sample’s mass (if different from the default value), or Calculate to have the mass calculated automatically. If you select Calculate, you must enter weights for the Empty tube and the Tube + sample. Enter a value in the Density field (or accept the default). This value is applicable only when using a calculated free space.

8.

9. Choose whether you are going to use manually entered data or have data collected. 10. Unless you are gathering statistical process control information, it is unnecessary to enter parameter values. These are user-definable parameters that can be entered and tracked along with other statistical process control data; refer to Sample Defaults, page 8-8 for information on user parameters. 11. After you complete the Sample Information dialog, click on the parameter tabs to open associated dialogs and edit as desired. Instructions for completing these dialogs are explained in Defining Parameter Files, page 3-6. 12. After you have completed all parameters, click Save, then Close.

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Creating a Sample Information File

TriStar II 3020

Basic and Restricted Formats
The Basic and Restricted formats are the easiest and simplest way to create a sample file. You simply create your sample information file using predefined parameter files (explained in this chapter beginning on page 3-6). If more detailed conditions or custom files are required, you must use the Advanced format (explained on page 3-14). • If you are using the Basic format, you can switch to the Advanced format when editing is required. • If you are using the Restricted format, you cannot edit parameter files. Refer to Basic, page 5-8 for a detailed description of the fields on this dialog. 1. Select File > Open > Sample Information; the Open Sample Information File dialog is displayed. 2. Accept the next sequenced file number or enter a new name in the File name field. 3. Click OK; then Yes to create the file; the Basic Sample Information dialog is displayed.

The Restricted dialog does not contain an Advanced push button.

4. Enter a description in the Sample field, or edit the one established in sample defaults. 5. Select Enter to enter a value for the sample’s mass (if different from the default value), or Calculate to have the mass calculated automatically. If you select Calculate, you must enter weights for the Empty tube and the Tube + sample. Enter a value in the Density field (or accept the default). This value is applicable only when using a calculated free space.

6.

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Creating a Sample Information File

7. Click on the down arrow to the right of each of the following fields to choose parameter files: • • • • • Sample tube Degas conditions (if using the SmartPrep degasser) Analysis conditions Adsorptive properties Report options

If you have an existing sample file containing the values you wish to use for this file, click Replace All to choose the file and copy the values into the current file.

8. Click Save, then Close.

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Preparing for Analysis

TriStar II 3020

Preparing for Analysis
The table shown here outlines the tasks necessary to properly prepare for an analysis, as well as the location of the procedure for performing the task. It is best to perform the tasks in the order given in the table.
Task Name and Location

Clean the sample tube Create the sample file Weigh your sample Degas your sample Load sample on sample port Fill Dewar and check LN2 level

Cleaning and Labeling Sample Tubes, page 3-18 Creating a Sample Information File, page 3-14 Determining the Sample Mass, page 3-21 Degassing the Sample, page 3-23 Installing the Sample Tube, page 3-24 Installing the Analysis Dewar, page 3-25

Cleaning and Labeling Sample Tubes
Sample tubes and filler rods must be clean and dry before samples are added and weighed. The following procedures are recommended. Refer to Table 3-1 for a list of materials needed to clean and weigh samples. Table 3-1. Materials Required to Clean and Weigh Sample Tubes
Supplied by Micromeritics Supplied by User

Sample tube Filler rod (if used) Sample tube brush Stopper for sample tube Sample tube rack Sample weighing support Sample data worksheet (copied from Appendix A of this manual)

Drying oven Ultrasonic cleaning unit Detergent Rubber gloves or lint-free cloth Acetone or isopropyl alcohol Safety glasses Waste container Analytical balance Pipe cleaners

1. Turn on the drying oven used for heating the sample tubes and filler rods and set the temperature to 110 ºC. 2. Check the reservoir of the ultrasonic cleaning unit to make sure it is clean.

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Preparing for Analysis

3. Using 5 grams of Alconox (or other suitable detergent) per 500 mL of warm water, fill the reservoir of the ultrasonic unit with enough water to cover the sample tubes and filler rods. Make sure the detergent is dissolved before placing the sample tubes and filler rods into the water. If too much detergent is used, it may be difficult to rinse from the sample tubes. 4. Fill the sample tubes with warm water and place them in the reservoir of the ultrasonic cleaning unit. Place the filler rods in the bowl also. Turn on the ultrasonic cleaning unit for approximately fifteen minutes.

5. Using rubber gloves, remove the sample tubes and filler rods from the reservoir. 6. Clean the interior of the sample tubes with the brush supplied with the TriStar System. 7. Rinse the sample tubes and filler rods thoroughly with hot water, then with isopropyl alcohol or acetone.
If isopropyl alcohol or acetone is not available, deionized water may be used to rinse the sample tubes.

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Preparing for Analysis

TriStar II 3020

8. Stand the sample tubes on the sample tube rack and place the filler rods in a basket or in the rack. Bake in a vacuum oven for two hours. 9. Remove the sample tubes and filler rods from the oven and allow them to cool.
Do not insert the filler rods at this time. Filler rods are inserted just before the sample tube is installed on the analysis port.

10. Wipe a rubber stopper with a lint-free cloth. 11. Label the sample tube and stopper for identification.

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Preparing for Analysis

Determining the Sample Mass
Analysis results are expressed in units of surface area per gram of sample; therefore, it is important the true sample mass be known. The true mass is best calculated as follows: • Weigh the Sample Tube Set (sample tube and stopper or seal frit) before degas • Weigh the Sample Tube Set with sample before degas and subtract from the weight of the Sample Tube Set • Weigh the Sample Tube Set with sample after degas and subtract from the weight of the Sample Tube Set • Weigh the Sample Tube Set with sample after analysis and subtract from the weight of the Sample Tube Set For your convenience, a Sample Data Worksheet for recording the weights and calculating the mass is included in Appendix A. You may make copies as needed. Make a copy of the Sample Data Worksheet, then proceed with the instructions provided below. 1. Write the Sample Tube Identification on the Sample Data Worksheet. 2. Place the sample weighing support on the balance. Tare the balance and allow it to stabilize at zero (0). 3. Place the sample tube set on the sample weighing support, and place it on the balance.

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4. Record the stabilized weight on the Sample Data Worksheet as Mass for empty sample tube set. Remove the sample weighing support and sample tube set from the balance.
Do not touch the sample with bare hands while performing the following steps. Doing so could affect the accuracy of results.

5. Place a sample container on the balance; slowly add the desired amount of sample to the container. 6. Remove the rubber stopper (or seal frit) from the sample tube. 7. Using the sample tube funnel (provided in the accessories kit), pour the sample from the weighing container into the sample tube.

Funnel

8. Replace the rubber stopper (or seal frit). 9. Weigh the sample tube set containing the sample; record the value on the Sample Data Worksheet as Sample tube set plus sample mass (Before Degas). 10. Subtract the Mass for empty sample tube set from the Mass of sample tube set plus sample; record this value as the Sample mass (Before Degas).

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Preparing for Analysis

Degassing the Sample
After the sample has been weighed, use a degassing unit to remove any contaminants which may have adsorbed to the surface or pores of your sample. Appropriate degassing units are available from Micromeritics. Refer to Ordering Information, page 10-1 for ordering information. If you are using the SmartPrep degasser, a menu will display on the menu bar of the TriStar application. You can degas your sample using commands on this menu and information you enter in the Degas Conditions dialog. Refer to the SmartPrep operator’s manual for operating instructions. After degassing is complete, perform the following steps: 1. Weigh the sample tube set containing the sample; record the weight on the Sample Data Worksheet as Sample tube set plus sample mass (After Degas). 2. Subtract the Mass for empty sample tube set (Before Degas) from the Sample tube set plus sample mass (After Degas) to obtain the sample’s mass; record this value as Sample mass (After Degas).

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Installing the Sample Tube
To attach a sample tube to a port, follow the steps below. 1. Remove the sample tube stopper. 2. If using a filler rod: hold the sample tube horizontally and carefully slide the filler rod into the tube.

Do not hold the rod vertically and drop the rod into the tube; this could break the rod and/or the tube.

3. If using an isothermal jacket, slide the jacket down over the stem of the sample tube until it touches the bulb of the sample tube. 4. Insert the Po tube into the center hole of the Dewar cover and slide the cover up; make sure the tapered side of the cover is facing downward. 5. Insert the sample tube through one of the holes in the cover.

O-ring

Ferrrule

Connector Nut Dewar Cover

6. Place the connector nut, ferrule, and O-ring onto the sample tube stem. 7. Attach the sample tube to the analysis port. Make sure it is fully in the port; secure in place by screwing the connector nut onto the analysis port. Hand-tighten the connector nut. 8. Slide the Dewar cover upward until it stops.

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Preparing for Analysis

Installing the Analysis Dewar
Prepare the analysis Dewar after you have installed the sample tube(s),
Always handle Dewars with care. Any product incorporating a vacuum is a potential safety hazard and should be treated with caution. Always observe the precautions listed below.

We recommend the following be observed when handling Dewars containing liquefied gases: • Protect yourself by wearing 1) goggles (or a face shield), 2) an insulated or rubber apron, and 3) insulated gloves. • When pouring liquefied gases from one container to another: 1) cool the receiving container gradually to minimize thermal shock, 2) pour the liquefied gas slowly to prevent splashing, and 3) vent the receiving container to the atmosphere. • Use a plastic stirring rod when stirring substances in a Dewar containing liquefied gases (or other materials of extremely low temperature). Do not use a glass or metal stirring rod unless it is coated with some type of protective coating. • Do not remove the mesh covering from the Dewar flask. This covering is in place so that you can maintain a secure grip on the Dewar. • Do not handle heavy objects above the Dewar. If unavoidable, place a protective cover over the Dewar’s opening. If an object of sufficient weight is accidentally dropped into the Dewar, shattering may occur.

Install the analysis Dewar as follows: 1. Place the analysis Dewar onto the elevator. 2. Fill the Dewar with the analysis bath liquid (liquid nitrogen) to about 5 cm (2 in.) from the top.
Incorrect fluid levels can lead to measurement errors. You should check the level of the bath liquid before each analysis.

3. Insert the dipstick into the Dewar and check the level of the analysis bath liquid. Condensation should not exceed the Level Indicator mark.

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Level indicator mark Wetness or frozen condensation indicates bath liquid level

4. Allow approximately 30 minutes (for best results) for the temperature of the Dewar to stabilize with that of the bath liquid. Then recheck the level of the bath liquid; add additional liquid if necessary.
It is not necessary to allow time for stabilization unless the Dewar has not been in use for a while.

5. Close the sample compartment door.

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Performing an Analysis

Performing an Analysis
After the sample has been degassed and transferred to the analysis port, you may begin analysis. The TriStar provides two types of analyses from which you may choose: • Standard - allows you to perform up to three analyses using different analysis conditions. • QuickStart - allows you to perform multiple sample analyses using the same analysis conditions.

Standard Analysis
Refer to Sample Analysis, page 6-3 for a detailed description of the fields on this dialog. 1. Select Unit > Sample analysis; the Analysis dialog is displayed.

2. Click Browse to choose a sample information file to be used for each port you plan to use. 3. The sample identification, sample mass, and sample density contained in the sample information file are displayed. Verify the sample mass and density. The density value is applicable only if you are using the Calculate method for the free-space determination. 4. The Po and bath temperature are displayed; these values may be edited if desired.

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5. Select Report after analysis to have reports generated automatically when the analysis completes. Be sure to designate the destination if you choose this option. 6. Click Export after analysis to have isotherm data exported automatically when the anlaysis completes. 7. Click Start to start the analysis; an analyzing view of the window is displayed so that you can view data as it is collected. A short delay is encountered before the port status changes from the Idle state. 8. After the analysis is finished, remove the sample tube and dispose of the sample accordingly.
Use caution when removing the sample tube if a hanging filler rod is being used. The sample tube O-ring or Dewar cover may snag the filler rod retaining ring. Loosen the snag gently; excessive force may break the tip of the filler rod.

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Performing an Analysis

QuickStart Analysis
It is not necessary to prepare sample files in advance when using the QuickStart method. Sample files are assigned automatically and given default conditions. You can replace file contents if desired on the second view of the QuickStart dialog. Refer to QuickStart, page 6-8 for a detailed description of the fields on this dialog. 1. Select Unit > QuickStart analysis; the following dialog is displayed.

2. Enter an identifier for this series of samples. 3. Enter the operator’s name in the Operator field. 4. Select Report After Analysis if you wish to have reports generated automatically after the analyses. Be sure to specify a destination if you choose this option. 5. Click Export after analysis to have isotherm data exported automatically as analyses are completed. 6. Click Next; the following dialog is displayed.

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File names are assigned automatically and given default conditions. Click Replace All adjacent to the Sample field if you wish to replace parameter values with those of another file. 7. Be sure the ports you are using in the analyses are selected. 8. Enter the sample’s mass and density for each port. The density is only applicable if you are using Calculate as the free-space method. 9. Ensure that the Po value and bath temperature are correct; edit if needed. 10. Click Start to start the analysis; the following actions occur: • A view of the data collection as it progresses is displayed. A short delay is encountered before the port status changes from the Downloading state. If desired, you can obtain a report on the data collected so far by selecting the appropriate Report Port [n] push button; the report is printed to the screen. • When the analysis finishes, the first view of the QuickStart dialog is displayed. 11. Repeat steps 5 through 9 to perform additional analyses or click Close to close the QuickStart dialog. 12. After the analysis is finished, remove the sample tube and dispose of the sample accordingly.
Use caution when removing the sample tube if a hanging filler rod is being used. The sample tube O-ring or Dewar cover may snag the filler rod retaining ring. Loosen the snag gently; excessive force may break the tip of the filler rod.

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Printing File Contents

Printing File Contents
Using the Print command on the File menu, you can print the contents of one or more sample or parameter files. Refer to Print, page 5-94 for a detailed description of the fields on this dialog. 1. Select File > Print > (file type); a dialog similar to this one is displayed.

Choose the destination.

Choose the file(s) you wish to print.

Click to complete the printing process.

2. From the Files list, select the file(s) you wish to print. If you plan to print multiple files, hold down Ctrl while selecting the files. 3. At the Destination field, click the down arrow and choose a destination for file output. • Printer; the Copies field is enabled allowing you to print up to four copies. Output goes to the printer specified as the default printer. • File; the File name field is enabled allowing you to enter a name for the file, or you can accept the default.

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4.

Click OK, the contents of the requested file(s) is(are) sent to the selected destination; this example shows a sample information file printed to the Screen.

Header

Close: closes the dialog Print: prints the report to the default printer Header: toggles the header on and off Prev and Next: enabled when the report contains multiple pages allowing you to advance

to other pages

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Listing File Statistics

Listing File Statistics
You can generate a list of the following information on one or more sample or parameter files: • • • • • File name Date the file was created (or last edited) Time the file was created (or last edited) File identification Status

Refer to List, page 5-95 for a detailed description of the fields on this dialog. 1. Select File > List> (file type); a dialog similar to this one is displayed.

Choose the destination.

Choose the file you wish to print.

Click to complete the operation.

2.

From the Files list, choose the desired file(s). If you wish to include all files in the list, leave all files deselected. At the Destination field, click the down arrow and choose a destination for file output. • Printer; the Copies field is enabled allowing you to print up to four copies. Output goes to the printer specified as the default printer. • File; the File name field is enabled allowing you to enter a name for the file, or you can accept the default.

3.

4.

Click OK, a list for the requested file(s) is sent to the specified destination.

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Exporting Isotherm Data

TriStar II 3020

Exporting Isotherm Data
Export allows you to copy the isotherm data in a sample information file and export it as ASCII text. If saved to a File, the data can be imported into applications such as spreadsheets. The output file consists of four columns containing the elapsed time, absolute pressure, relative pressure, and specific volume adsorbed. Refer to Export, page 5-96 for a detailed description of the fields on this dialog. 1. Select File > Export; the Sample Information File Export dialog is displayed.

2. From the Files list box, select the file(s) you wish to export. If you plan to export multiple files, hold down Ctrl while selecting the desired files. 3. In the Settings group box, choose a Destination for your exported file. a. If you choose File as the destination, select the file type. Then enter a name in the File name field or accept the default. If you have selected multiple files, individual files are exported as their file name. You can also change the destination path if desired. b. If you choose Printer, the Copies field is enabled; you can print up to four copies. 4. Click OK; the file is exported to the specified destination.

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Generating Graph Overlays

Generating Graph Overlays
Use the graph overlay function when you wish to compare graphically multiple graph options. Graphical lines are differentiated by the use of varying symbols and reported in a legend on the report. Overlays may be generated in two ways: • Multiple Sample Overlays Overlay up to eight plots of the same type with that of the current plot • Multiple Graph Overlays Overlay two different types of plots from one sample. This type of overlay is available only for BJH Adsorption/Desorption DFT Pore Size/Surface Energy Dollimore-Heal Adsorption/Desorption Horvath-Kawazoe M-P Method You must use the Advanced format for generating overlays. Select Options > Options presentation > Advanced to access the Advanced mode, or click the Advanced push button on the Basic Sample Information dialog.

Multiple Sample Overlays
To overlay the same type of graph on multiple samples: 1. Select File > Open > Sample Information to display the Open Sample Information File dialog. 2. Select a sample on which to overlay graphs of other samples, then click OK; the Sample Information dialog is displayed. 3. Click the Report Options tab to display the Report Options dialog.

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4. Choose the type of report from the Selected Reports window; then click Edit. 5. Choose the type of report for which you wish to generate overlays, click Edit, and perform the steps listed for that report: If you are overlaying this type of report.... Isotherm

Then .... Select the desired plot(s) from the Select Reports group box. Click Options (becomes enabled when the plot is selected) adjacent to the selected plot Select the Overlay samples check box, then click OK. Click OK again to return to the Report Options dialog..

BET Surface Area Langmuir Surface Area Freundlich Temkin t-Plot Alpha-S f-Ratio

Select the Overlay Samples check box. Click OK.

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Generating Graph Overlays

If you are overlaying this type of report.... BJH Adsorption BJH Desorption Dollimore-Heal Adsorption Dollimore-Heal Desorption MP-Method

Then .... Choose the report variable from the Selected Reports window, then click Edit. Click on the down arrow at the Overlay field and choose Samples; then click OK. Click OK again to close the report variable’s dialog and return to the Report Options dialog.

6. From the Report Options dialog, click Overlays; the Graph Overlays Samples dialog is displaed.

7. Click Browse to the right of the Sample [n] field; the Plot Overlay Sample Selection dialog is displayed. 8. Choose the file containing the graph you wish to overlay, then click OK. You may choose up to eight files in this manner. 9. After selecting your files, click OK to return to the Report Options dialog. 10. Click Save if you wish to save your selections; you can still generate the overlays even if you do not wish to save them. 11. Select Reports > Start report; the Start Report dialog with the name of your edited file highlighted is displayed. 12. Click OK; the Select Reports dialog is displayed. 13. Ensure that the desired graph is selected, then click OK .

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Multiple Graph Overlays
Multiple graph overlays can only be generated for: • • • • • • • • BJH Adsorption BJH Desorption DFT Pore Size DFT Surface Energy Dollimore-Heal Adsorption Dollimore-Heal Desorption Horvath-Kawazoe MP-Method

1. Select File > Open > Sample Information to display the Open Sample Information File dialog. 2. Select the desired file, then click OK; the Sample Information dialog is displayed. 3. Click the Report Options tab to access the Report Options dialog.

4. Select the type of report on which you wish to have overlays generated; this example shows BJH Adsorption.

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Generating Graph Overlays

5. Highlight BJH Adsorption and click Edit; the BJH Adsorption dialog is displayed.

Select the report variable.

Click to choose the second report variable.

6. From the Selected Reports window, select the report variable on which you wish to have another variable overlaid, then click Edit. A dialog similar to this one is displayed.

Displays the first report variable.

Choose the second variable from this drop-down list.

7. From the Overlay drop-down list, choose the report variable you wish to overlay, then click OK. 8. Click OK again to return to the Report Options dialog. 9. Click Save if you wish to save your selections; you can still generate the overlays even if you do not wish to save them. 10. Select Reports > Start report; the Start Report dialog with the name of your edited file highlighted is displayed. 11. Click OK; the Select Reports dialog is displayed. 12. Ensure that the desired graph is selected, then click OK.

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TriStar II 3020

Installing the Software

4. SOFTWARE AND SETUP MODIFICATIONS
This chapter provides instructions for: • Installing the software, beginning on this page • Using the Setup Program for Other Functions, page 4-6 You can also install the TriStar program for offline data manipulation on a computer other than the one controlling the analyzer. This allows you to: • create or edit sample and parameter files • generate reports on completed sample files Review the Micromeritics PROGRAM License Agreement for restrictions on the use of another copy of the analysis program.

Installing the Software
Be sure you have completed the following tasks before installing the software for the first time. • Configure the ethernet port the analyzer will use (refer to Configuring the Ethernet Port, page E-1) • Disable the firewall setting for the connection between your computer and analyzer (refer to Configuring the Firewall Setting, page E-7) • Connect the analyzer to the configured port and turn the analyzer on.
If installing multiple analyzers, connect the ethernet switch to the configured port and the analyzers to the ethernet switch (refer to Ethernet Switch, page 4-9); turn the analyzers on.

Install the program as follows: 1. 2. Select Start > Run from the Windows menu bar. Enter the name of the drive designator, followed by analyzersetup. For example: e:analyzersetup.

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Installing the Software

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3.

Click OK; the Ethernet Introduction dialog is displayed. This screen outlines the steps that should be completed before installing the software.

If all of the steps have not been completed, click Cancel and perform the steps; then restart the installation program. Do not proceed with installation until these tasks have been completed. 4. Click OK; the New Installation dialog is displayed.

The Destination Folder group box displays the amount of current disk space required for the analysis program, and the directory into which the application will be installed. If you prefer a different directory for installation, click Browse to select the desired directory.

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Installing the Software

The TriStar application should not be installed on a network drive with shared access. Multiple users cannot operate the application at the same time.

5.

Select the check box just below the Destination Folder group box to add an icon to your desktop; this enables quick access to the analysis program. The TriStar icon is added to the Micromeritics folder by default. If you prefer a different folder, enter or select one from the drop-down list. The Install this application for All Users check box enables you to allow or prohibit users other than the installer to access the application. • Select the check box to allow access for all users logged onto Windows. • Deselect the check box to allow access for only the user installing the application.

6.

7.

8.

Click Next; the Analyzer configuration dialog is displayed.

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Installing the Software

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a. In the Step 1 group box: If .... you are installing the analysis program at initial installation: Then .... select the number of analyzers you are installing.

you plan to use the select 0 analysis program for offline data reduction: you are moving an select 0 (Refer to Moving an Analyzer from One Comanalyzer from another puter to Another Computer, page 4-11.) computer to this one: b. In the Step 2 group box, enter the serial number(s) for the analyzer(s) you are attaching to this computer. 9. Click Next; the Ethernet Ports dialog is displayed.

10. Choose one of the following: If .... the port you configured is listed: Then .... select the port and proceed to the next step.

the port you plan to use Click Specify, the Specify Ethernet Port dialog is displayed. has been configured but Enter the remaining portion of the IP address in the enabled is not listed: fields, then proceed to the next step.

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Installing the Software

11. Click Next; the calibration files are installed. If you are installing more than one analyzer, the Calibration File Installation dialog instructing you how to proceed with installation of other calibration files is displayed. Read the instructions carefully; they are restated here. a. Remove this setup CD. b. Insert the CD containing the files for the analyzer serial number requested. IMPORTANT: To prevent the CD from AutoPlay, hold down the Shift key before you close the CD door. Do not release the Shift key until the CD light stops blinking. c. When the CD lights ceases to blink, click Next. After the calibration files are installed, you will be prompted to reinsert the original setup CD. The application software is installed after installation of all calibration files. 12. The Installation Complete dialog containing the Readme file will display when installation is complete. This dialog may also contain other important notices. After reading the information contained in this dialog, click Finish to close it. 13. Choose one: If .... you are installing the analysis program with regard to the installation video: you are installing the analysis program independent of the installation video and have no other operations to perform: Then .... Return to the Installation Instructions menu and continue with the next procedure. Remove the program CD and store in a secure location. The original program CD contains calibration files specific to your instrument. Upgrade CDs do not contain calibration files. Therefore, it is important that you maintain your original program CD in a secure location in the event calibration files need to be reinstalled.

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Using the Setup Program for Other Functions
After initial installation of the analysis program, the application setup program can be used to: • • • • • • • install software upgrades, page 4-8 add an analyzer, page 4-9 move an analyzer from one computer to another computer, page 4-11 change the analyzer setup (port configuration), page 4-17 remove an analyzer from the computer, page 4-16 reinstall calibration files, page 4-19 uninstall the analysis program, page 4-20

To start the application setup program: 1. 2. Ensure that the analysis program is not operating and the analyzer is idle. Insert the CD into your CD-ROM drive; after a few seconds the menu for the TriStar installation instructions is displayed.

If Autorun is not enabled on your computer, proceed to Step 4.

Click here to close the menu.

3. 4.

Click X in the upper right-hand corner to close the installation menu. Select Start from the Status bar, then Run from the start menu.

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Using the Setup Program for Other Functions

5.

Enter the drive designator of the CD-ROM drive, followed by setup. For example: e:setup Alternatively, you can click Browse, navigate to the CD-ROM drive, and select setup.exe.

6.

Click OK; the setup Welcome screen showing the options available is displayed.

Options available for the TriStar program are enabled.

7.

Select the operation you wish to perform. Procedures for performing each operation are in subsequent sections. After the requested operation is completed, the setup Welcome screen is again displayed. A confirmation message indicating completion of the operation is shown in the lower section of the dialog.

Indicates status of last operation performed.

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Using the Setup Program for Other Functions

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8. 9.

After you have completed all desired operations, click Exit to close the Welcome screen. Remove the CD and store in a secure location.

Installing Subsequent Software Versions
When you install a software upgrade, the system installs all of the application files and any status files that do not already exist on the computer. Existing analyzer status files are not affected and default and data files are not overwritten. There are three types of subsequent installation; the software version controlled by the setup program is: • a later version than the version installed on the computer • the same version as the version installed on the computer • an earlier version than the version installed on the computer The setup program automatically detects which type of installation applies and customizes the selection in the Setup dialog accordingly. 1. Start the Setup program (refer to Using the Setup Program for Other Functions, page 4-6). Choose the software option; remember, only the applicable option will display: • Upgrade software to version (number) from version (number) • Reinstall software version (number) • Downgrade software to version (number) from version (number) 3. Click Start File Installation; the application installs the software and displays the setup Welcome dialog.

2.

4-8

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Using the Setup Program for Other Functions

Adding an Analyzer
An ethernet switch is required when connecting multiple analyzers. After connecting the ethernet switch, continue with the software section. Ethernet Switch An Ethernet switch with a straight-through cable is required when installing multiple analyzers. 1. 2. Connect the power cord of the Ethernet switch to an appropriate power outlet. Disconnect the ethernet cable of the current analyzer from the computer; do not disconnect it from the analyzer. Connect one end of the straight-through cable to the Ethernet switch and the other end to the computer. Connect the ethernet cable of the current analyzer to a numbered port on the Ethernet switch (do not use the uplink port). Connect one end of the Ethernet cable (for the analyzer you are adding) to the connector labeled Ethernet on the rear panel of the analyzer and the other end to a numbered port on the Ethernet switch. Repeat this step for each analyzer you are adding. The finished configuration should look like the following illustration.

3.

4.

5.

Ethernet switch

Be sure cables are not connected to the uplink port.

6.

Turn on the analyzer that was added. Also ensure that the computer and current analyzer are on.

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Software 1. 2. Insert the analysis program CD for the analyzer you are adding into the CD-ROM drive. Start the Setup program (refer to Using the Setup Program for Other Functions, page 4-6). Select Add an analyzer, then click Next; the Set up analyzer being added dialog is displayed.

3.

You may see the Ethernet Introduction screen. This information is not applicable since you are connecting to an ethernet switch which is connected to a port that has been configured. Click OK to close the screen and proceed.

4. 5.

Enter the serial number of the analyzer being added. Click Next; the calibration files are installed and the Welcome screen is displayed.

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Using the Setup Program for Other Functions

Moving an Analyzer from One Computer to Another Computer
Use the instructions in this section to move a configured analyzer (along with its status, calibration, and log file) from one computer (Source PC) to a different computer (Destination PC). This operation does not move sample or parameter files. Use a file management program such as Explorer or a backup/restore utility to move these types of files. Moving a Configured Analyzer to a New Computer This section provides steps for moving a configured analyzer to a computer that does not have an analyzer installed.
If the analysis program is already installed on the destination computer, begin with Step 2.

1.

Install the analysis program on the destination computer (refer to Installing the Software, page 4-1). Be sure to select 0 as the number of instruments on the Analyzer Configuration screen; all related instrument information will be transferred in the Move operation. Start the application setup program on the source computer (refer to Using the Setup Program for Other Functions, page 4-6). Select Move an analyzer from one PC to another PC, then click Next; the Move analyzer operation dialog is displayed.

2.

3.

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Using the Setup Program for Other Functions

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4.

Select Source PC, then click Next; the following dialog is displayed.

5.

From the drop-down list in the Step 1 group box, select the analyzer that is to be moved from this computer. In the Step 2 group box, click Browse to select a location for storing the status, calibration, and log files associated with the source computer. If possible, the location should be a shared network drive. If this is not possible, select a local folder and then use a transfer utility to copy its contents from the Source PC to the Destination PC.

6.

Sample and parameter files are not copied and moved with the analyzer. Use a file management program such as Explorer or a backup/restore utility to move these files.

7.

Click Next; the files are copied to the specified location and the setup Welcome screen is displayed. Start the Setup program on the destination computer. Select Move an analyzer from one PC to another PC; the Move analyzer operation dialog is displayed (shown on previous page).

8. 9.

4-12

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Using the Setup Program for Other Functions

10. Select Destination PC, then click Next; the Ethernet Introduction screen is displayed. This screen outlines the steps that should be completed to configure the ethernet port to which the analyzer is connected to on the computer.

If these tasks have not been completed, click Cancel and complete them; then restart the setup program. Do not proceed until the ethernet port in the computer has been configured. 11. Click OK; the Move analyzer information dialog to this PC dialog is displayed.

12. In the Step 1 group box, enter the serial number of the unit you are moving to this computer. 13. In the Step 2 group box, click Browse to choose the location of the files that were stored previously from the Source computer.

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14. Click Next; the files are transferred and the Ethernet Ports dialog is displayed.

Select the desired ethernet port. 15. Click Next; the setup Welcome screen is displayed. 16. Turn on the analyzer and start the analysis program.

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Using the Setup Program for Other Functions

Moving a Configured Analyzer to a Computer with an Existing Analyzer This section provides steps for moving a configured analyzer to a computer that already has the analysis program and a configured analyzer installed, this being the second analyzer. When installing two analyzers on one computer, additional hardware is required. Refer to Adding an Analyzer, page 4-9. 1. Perform Steps 2 through 7 (steps for Source computer) of the procedure Moving an Analyzer from One Computer to Another Computer, page 4-11. Disconnect the Ethernet cable of the analyzer from the Source computer (or Ethernet switch). Reconnect the cable to the Ethernet switch for the Destination computer. You must use a switch when attaching multiple analyzers. Refer to Ethernet Switch, page 4-9 for configuring ethernet connections using a switch. After ethernet connections have been established, return to page 4-12 and begin with Step 8 (steps for Destination computer). You will not see the Ethernet Ports dialog (Step 13) since an ethernet port has already been assigned. Turn on both analyzers and start the analysis program.

2.

3.

4.

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TriStar II 3020

Removing an Analyzer
You can remove an analyzer from the computer as follows. When you remove an analyzer, the status files are removed as well. 1. Start the Setup program. Refer to Using the Setup Program for Other Functions, page 4-6. Select Remove an analyzer, then click Next; the Remove an analyzer dialog is displayed.

2.

3.

From the drop-down list, choose the serial number of the analyzer you wish to remove.

This operation removes the selected instrument from the list of attached instruments. It does not remove calibration and status files associated with the analyzer, nor does it remove sample and parameter data files.

4.

Click Remove; the analyzer is removed and the Welcome screen is displayed.

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Using the Setup Program for Other Functions

Changing the Analyzer Setup Configuration
This option allows you to change the ethernet port being used by the analyzer(s). For example if the current ethernet port malfunctions, you would use this option to move the analyzer to another ethernet port. Be sure that the ethernet port you are switching to has been configured and the firewall setting between the computer and the analyzer is turned off. Refer to Configuring the Ethernet Port, page E-1 and Configuring the Firewall Setting, page E-7. 1. Start the Setup program. Refer to Using the Setup Program for Other Functions, page 4-6.

2. Select Change analyzer setup, then click Next; the Ethernet Introduction screen is displayed. This screen outlines the steps that should be completed to configure the ethernet port to which the analyzer will be connected.

If these tasks have not been completed, click Cancel and complete them; then restart the setup program. Do not proceed until the ethernet port in the computer has been configured.

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TriStar II 3020

3.

Click OK; the Ethernet Ports dialog is displayed.

4.

Choose one of the following: If .... the port you plan to use is listed: the port you plan to use has been configured but is not listed: Then .... select the port and proceed to the next step. Click Specify, the Specify Ethernet Port dialog is displayed. Enter the remaining portion of the IP address in the enabled fields, then proceed to the next step.

5.

Click Next; the change is completed and the Welcome screen is displayed.

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Using the Setup Program for Other Functions

Reinstalling Calibration Files
Calibration files specific to the analyzer are contained on the original program CD; they are not contained on an update CD. It is important that you store your original program CD in a safe location. CDs containing calibration files will always end with a suffix of 99. Update CDs end with a suffix of 00. Reinstall calibration files as follows: 1. Using the CD containing the appropriate calibration files, start the Setup program. Refer to Using the Setup Program for Other Functions, page 4-6. Select Re-install calibration files for an analyzer, then click Next: If .... you have only one analyzer installed Then .... the calibration files are installed and the Welcome screen is displayed.

2.

you have multiple ana- select the appropriate analyzer, then click Next; the calilyzers installed, a bration files are installed and the Welcome screen is dialog enabling you to displayed. choose the desired analyzer is displayed.

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Uninstalling the Analysis Program
You can remove the analysis program as follows. When you perform this operation, the application removes the analysis program, status files, analyzer setup files, and resulting empty directories. It does not remove data files. 1. Start the Setup program. Refer to Using the Setup Program for Other Functions, page 4-6. Select Uninstall, then click Next; the Uninstall dialog is displayed.

2.

3.

Click Uninstall; the Select Uninstall Method dialog is displayed.

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Using the Setup Program for Other Functions

4.

Choose one of the following: • Automatic: click Next; the system uninstalls the software automatically and the setup Welcome dialog is displayed. • Custom: click Next; a series of dialogs is displayed, allowing you to choose the files you wish to uninstall. After all files are selected and uninstalled, the setup Welcome dialog is displayed.

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Description

5. FILE MENU
The File menu contains options which allow you to manage sample and parameter files.

Description

Listed below are brief descriptions of the File menu options. Detailed descriptions follow this section.\ Open Opens an existing sample or parameter file, or enables you to create a new one. Page 5-3. Saves the file in the active window. Page 5-91. Saves the file in the active window as a different name. You also can use this option to save a subset of the sample file as a parameter file. Page 5-91. Saves all open files. Page 5-93. Closes the file in the active window. Page 5-93. Closes all open files. Page 5-93. Prints the contents of a sample or parameter file. Page 5-94.

Save Save As

Save All Close Close All Print

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5-1

Description

TriStar II 3020

List

Generates a list of certain information for sample or parameter files. Page 5-95. Exports the isotherm data contained in a sample file. Page 5-96. Exits the analysis program. Page 5-99.

Export Exit

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TriStar II 3020

Open

Open
Open enables you to open an existing sample information or parameter file, or to create a new one. Regardless of which file type you select, a dialog similar to the one shown here is displayed.

Does not display for parameter files.

File name

For sample information files, this field contains the next sequenced file name generated by the analysis program. For parameter files, the file name displayed includes an asterisk (*) and a default extension as follows: *.STB for sample tubes *.DEG for degas conditions *.ANC for analysis conditions *.ADP for adsorptive properties *.RPO for report options If you are creating a new file, enter a name in the File name field. If you are editing an existing file, select a file from the list.

Refer to Selecting Files, page 2-11 for a description of the other fields on this dialog.

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Sample Information
Sample information files contain information used to control the analysis. Therefore, every analysis must be linked with a sample information file before the analysis can proceed. A sample information file is comprised of the following: • • • • • • • Sample identification Sample tube parameters Degas conditions (if using automatic degassing) Analysis conditions Adsorptive properties Report options Entered or collected (appears after analysis is complete) data

Parts of the sample information file can also exist as parameter files which are separate from the sample information file itself. Having these files exist independently allows you to use them as many times as you wish. For example, if you typically use the same analysis conditions for many of your analyses, you can create an analysis conditions file containing those conditions. Then when you create your sample file, select that file for your analysis conditions. Once it becomes part of the new sample file, you can edit it in any way you wish without changing the file from which it was copied. Sample information files are presented in three formats: Advanced, Basic and Restricted.
Specify or change your format by selecting Options > Option presentation.

• Advanced Presents all parts of the sample information file in a single, index card tabbed dialog. • Basic Presents the entire sample information file in a single dialog. • Restricted Presents the sample information file in a single dialog similar to the Basic format with certain functions disabled.

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Open

Advanced When you open an existing sample information file or create a new one using the Advanced format, all parts of the sample file are displayed in a tabbed dialog. The Advanced format allows you to customize sample files. Refer to Advanced Format, page 3-14 for step-by-step instructions for creating an Advanced sample information file.

A Collected Data tab displays here when analysis is complete. An Entered Data tab displays if you choose Manually entered allowing you to enter the data.

The prompts for the Sample, Operator, Submitter, and Bar Code fields may be customized by selecting Options > Sample defaults. Refer to Sample Defaults, page 8-6 for instructions on customizing these prompts. Sample Displays the default file description or the description of the file you are opening. You may enter a new description or edit the existing one. You can use up to 50 alphanumeric characters. Operator Submitter Enter the name of the operator who will be performing the analysis and the name of the person (or department) submitting the sample for analysis. You may use up to 40 alphanumeric characters

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Bar Code

This field enables you to enter bar code information. If bar code information is not used, you can use this field to enter additional information about the sample; for example, you may wish to enter the lot number of your sample. This field will also accept data from a bar code reader. You can use up to 40 alphanumeric characters.

Mass

You can enter a sample mass or have the mass calculated automatically. Enables the Sample Mass field allowing you to enter a value. Enables the Empty tube and Sample + tube fields, allowing you to enter appropriate values. These values are used to calculate the mass of the sample,
Mass sample = Mass sample + tube – Mass tube

Enter Calculate

Density

This value is used only for the Calculated free-space method; it is ignored for other methods. Use 0.000 for a blank analysis.

Type of Data

Choose whether data are to be collected automatically by the analysis program or manually entered. If you choose Manually entered, an “Entered” tab is added so that you may enter the desired data. You cannot enter data if you are creating the file on a computer that is not attached to the analyzer.

User Parameters

These fields are used primarily for SPC (Statistical Process Control) reporting. However, they can be used for other data as well. You may wish to enter specific analysis conditions or sample criteria. These parameters print on the Options report. Select Options > Sample Defaults to specify the parameters you wish to report. The parameter(s) you specify replace the User Parameter label(s). If desired, you can have these fields omitted from the sample information file (refer to Sample Defaults, page 8-6).

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Open

Add Log Entry

Displays the Add Log Entry dialog.

Enter information pertinent to the sample file. For example, if you are not using the SmartPrep for automatic degassing, you may wish to enter external degassing information. Any information you enter here is printed as part of the sample log report. You may make multiple entries by selecting this push button as many times as you wish.
Replace All

Allows you to copy an existing sample file’s values into the sample information file you are creating. A dialog is displayed so that you may select the desired file. Click OK; the values are copied into the new file automatically. You may edit the values in the new file; the file from which they were copied remains unchanged. This replaces all parameters of the entire sample information file, excluding any collected data.

Each of the individual tabbed dialogs contains a Replace push button if you wish only to replace specific parameters and not the entire file contents.

Comments

Enter comments about the sample or its analysis conditions. Comments entered here are printed in the header of the reports. Saves the information you have specified for this sample file. Closes the dialog. If changes have been made in the dialog and have not been saved, you will be prompted to save before the dialog closes. Displays the sample information file in the basic format.

Save

Close

Basic

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Basic When you open an existing sample information file or create a new one using the Basic format, all parts of that file are contained on a single dialog. With the Basic format, you can quickly create a sample information file using previously defined parameter files. This format also allows you to switch to the Advanced format to view or edit parameters. Refer to Basic and Restricted Formats, page 3-16 for step-by-step instructions for creating a Basic sample information file.

Sample

Displays the default file description (new files) or the description in the file you are opening. You may enter a new description or edit the existing one. You may use up to 50 alphanumeric characters.

Mass

You can enter a sample mass or have the mass calculated automatically. Enables the Sample Mass field allowing you to enter a value. Enables the Empty tube and Sample + tube fields, allowing you to enter appropriate values. These values are used to calculate the mass of the sample,
Mass sample = Mass sample + tube – Mass tube

Enter Calculate

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Open

Density

Enter the density of the sample to be analyzed. This value is used only for the Calculated free-space method; it is ignored for other methods. Use 0.000 when performing a blank analysis.

Sample Tube Degas Conditions Analysis Conditions Adsorptive Properties Report Options

The drop-down lists for these fields contain previously defined files; those included with the analysis program as well as any you may have created specifically for your laboratory. Degas Conditions files are pertinent only if you are using the SmartPrep for degassing samples.

Add Log Entry

Displays a dialog so that you may enter pertinent information relating to the sample file. For example, if you are not using automatic degassing, you may wish to enter external degassing information. Any information you enter here is printed as part of the sample log report. You may make multiple entries by selecting this push button as many times as you wish. Alllows you to copy the values from all parameters of an existing sample file into the one you are creating. A dialog is displayed so that you may select the desired file. Click OK; the values are copied into the new file automatically. You may edit the values in the new file; the file from which they were copied remains unchanged. Saves the information you have specified for this sample file. Closes the dialog. If a file containing unsaved changes is open, you are prompted to save before the dialog closes. Displays the sample information file in the advanced format, allowing you to view or edit parameters.

Replace All

Save

Close

Advanced

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Restricted A third format is provided to control access to some portions of the sample information file. The Restricted format displays in the same manner as the Basic presentation format.

This format displays in the same manner as the Basic format; however, it does not allow you to switch to the Advanced format.

The fields on this dialog are identical to the ones on the Basic Information dialog except that this dialog does not contain an Advanced push button allowing you to switch to the Advanced format. This format is also password-protected, preventing the operator from making changes to file parameters. Refer to Restricted, page 8-5 for additional information on the Restricted format. Restricted presentation is ideal for laboratories in which standard analysis procedures are established by a lab manager, while one or more lab technicians actually perform the analyses. The lab manager can create independent parameters files containing standard sets of operating conditions, then the operator(s) can use Restricted mode for daily operations, selecting the standard parameter files from the drop-down lists.

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Open

Sample Tube
This dialog allows you to store sample tube information. Before creating a Sample Tube file, you should perform a blank analysis (no sample) using the sample tube. A sample tube file can be created as an independent parameter file or as part of the sample information file.
Be sure to save this file to the directory you specified as the Parameter files directory if it is to be included in the drop-down list on the Basic and Restricted Sample Information dialogs (see Parameter Directory in Chapter 8).

Sample Tube

Contains the description of the current file. If this is a new file, this field contains the description you specified as the default. You can enter a new description or add to the existing one if desired.

Replace

Use this push button to replace the values of the current file with those from an existing file. The Open Sample Tube dialog is displayed, allowing you to choose a file. After the values are copied into the current file, you can edit them as desired. Displays the warm free space for the current file. Displays the cold free space for the current file.

Warm free space Cold free space

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Non-ideality factor

Displays the non-ideality factor determined during the blank analysis. Select this option if an isothermal jacket is to be used in the analysis. An isothermal jacket is used to maintain a constant temperature profile along the sample tube stem during an extended analysis (more than 1 or 2 hours).

Use isothermal jacket

Use filler rod

Select this option if a filler rod is to be used in the sample tube. A filler rod is used to reduce the stem free-space volume, resulting in reduction of free-space error.

Vacuum seal type

If the sample tube is to be transferred under vacuum to the analysis port, select the seal type to be used. If not, leave None selected. Click this push button to choose the sample file that was used in the blank analysis. The data for the Warm and Cold free spaces, the port volume, and the non-ideality factor will be copied into the sample tube file.

Load From Sample File

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Open

Degas Conditions
This dialog is used when using the SmartPrep Degasser for degassing your sample. If you are not using the SmartPrep, you can use the dialog to record information used with a different degassing unit.
Be sure to save this file to the directory you specified as the Parameter files directory if it is to be included in the drop-down list on the Basic and Restricted Sample Information dialogs (see Parameter Directory in Chapter 8).

Description

If you are opening an existing file, this field contains the description. If this is a new file, enter a description; at least one character is required. You can use up to 40 alphanumeric characters.

Replace

Allows you to copy the values of an existing degas conditions file into the file you have open. A dialog is displayed so that you may select the desired file. Click OK; the values are copied into the new file automatically. You may edit the values in the new file; the file from which they were copied remains unchanged. Allows you to enter up to five stages of degas conditions

Conditions Table

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Soak Temperature

Enter the temperature at which the sample is to soak while flowing gas. Enter the rate at which the temperature is to change when advancing to the soak temperature. Enter the amount of time to soak the sample. Inserts a row into the conditions table. A row is inserted above the selected line; the cursor moves to the new line. Deletes the selected row from the conditions table. Clears all the table of all but one entry; one entry is required. The rows do not have to be selected.

Ramp Rate

Soak Time
Insert

Delete

Clear

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Open

Analysis Conditions
This dialog is used to specify the analysis conditions for your sample. An analysis conditions file can be created as an independent parameter file or as part of the sample information file.
Be sure to save this file to the directory you specified as the Parameter files directory if it is to be included in the drop-down list on the Basic and Restricted Sample Information dialogs (see Parameter Files Directory, page 8-15).

Description

If you are opening an existing file, this field contains the description. If you are creating a new file, enter a description; at least one character is required. You can use up to 40 alphanumeric characters.

Replace

Allows you to replace the values in the current analysis conditions file with those from an existing file. A dialog is displayed so that you may select the desired file. Click OK; the values are copied into the new file automatically. The choices in this group box allow you to specify how you wish to have isotherms collected.

Isotherm Collection

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Target Pressures

Select this option to have isotherms collected by specifying target pressures. When you select this option, Pressures and Options (directly to the right of this field) become enabled. Select each push button to verify or edit data. Displays the Entered Pressures dialog.

Pressures

Edit the existing pressure table or clear the table and enter a new pressure table. A pressure table is a table of relative pressure points (and possibly calculation assignments) at which data (isotherms) are to be collected. The relative pressures may span the entire range of 0.00000001 to 0.995 P/Po. There must be one adsorption branch followed optionally by one desorption branch. Several analysis conditions files containing complete pressure tables are included with the TriStar software. These files (and all other parameter files) can be edited. If you want to use any of these files, it is recommended that you use the Save As option on the File menu to save the file as a different name; then make your changes.

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Open

Pressures

(continued)

The pressure table for automatically collected data includes the pressure points for data collection and (when Use calculation assignments is selected) identifies calculations through which the data are processed.
Insert Range

Displays the Insert Pressure Range dialog.

This dialog allows you to specify the starting pressure, the ending pressure, the number of points to insert within the specified range, and whether you wish to have linear or geometric progression. Choose Linear to insert evenly spaced points into your table. Choose Geometric from low pressure to insert geometrically spaced points from the low pressure range. For example, if you wish to insert 5 points with a 0.01 starting pressure and a 0.16 ending pressure, the following points are inserted into the table: 0.01 0.02 0.04 0.08 0.16

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Pressures (continued)

Choose Geometric towards saturation to insert geometrically spaced points from the saturation pressure. For example, if you wish to insert 5 points with a 0.99 starting pressure and a 0.84 ending pressure, the following points are inserted into the table: 0.99 0.98 0.96 0.92 0.84
Insert Predefined

Displays the Insert Predefined Pressures dialog.

Choose predefined pressure points for surface area, t-Plot micropore and/or BJH adsorption/desorption. Click on the down arrow of each field to choose the desired set of points. You can also specify Adsorption/desorption total pore volume and saturation.
Insert

Inserts a row into the pressure table. A row is inserted above the selected line; the cursor moves to the new line.
Delete

Deletes the selected row.
Clear

Clears all entries from the table. The rows do not have to be selected.

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Open

Options

Allows you to specify target pressure options; the Target Pressure Options dialog is displayed.

First Pressure Fixed Dose Select this option to have the sample dosed with a specified amount of gas until the first pressure point is reached. This initial dosing quickly meets the adsorptive demand of the sample. The first point on the pressure table is the threshold value. Once this first pressure point is reached, points are equilibrated and recorded in accordance with the specified pressure table. You may wish to use this mode if you are performing a standard nitrogen analysis of microporous or highly mesoporous materials such as catalysts. If the first pressure table point is low, and you expect the gas uptake of the sample to be high, choosing this mode can shorten the time required to reach the first point on the pressure table. Maximum volume increment Select this option to specify when additional data points are to be collected between target pressures in regions of high adsorption. When the maximum increment has been adsorbed since the last collected data point, another point is equilibrated and collected. When using this option, reaching pressure points exactly is not important; therefore, the tolerances should be set relatively large (10 mmHg and 10% or so) for proper functioning of the algorithm. The pressure table should also have several points scattered over the region of interest. During desorption, this field is treated as a maximum volume “decrement” value.

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Options

(continued)

Absolute pressure tolerance Relative pressure tolerance These values are used to determine how close the actual pressure must be to each target pressure from the pressure table. At lower pressures the relative tolerance value is lower, and at higher pressures the absolute tolerance value is lower. For example: Experiment 1: you have an absolute tolerance of 5 mmHg, a relative tolerance of 5%, and a target pressure of 40 mmHg; 5% of 40 mmHg is 2 mmHg. Since 2 mmHg (relative tolerance) is lower than 5 mmHg (absolute tolerance), 2 mmHg is used. Therefore a minimum pressure of 38 mmHg (40 - 2) must be attained to collect data for a target pressure of 40 mmHg. Experiment 2: you have an absolute tolerance of 5 mmHg, a relative tolerance of 5%, and a target pressure of 200 mmHg; 5% of 200 mmHg is 10 mmHg. Since 5 mmHg (absolute tolerance) is lower than 10 mmHg (relative tolerance), 5 mmHg is used. Therefore a minimum pressure of 195 mmHg (200 5) must be attained to collect data for a target pressure of 200 mmHg. Normally, surface area measurement points are widely spaced, and the resulting measurement is not very sensitive to the precise location of points so wider tolerances may be used. Unnecessarily tight tolerances lengthen the analysis.

Dose Increments

In this form of dosing, there is no predefined pressure table. The sample is dosed repeatedly with a fixed amount of gas and isotherm points are collected after equilibrating each dose. Each entry in the table defines how much to dose for a segment of the isotherm.

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Options

Displays the Dose Increments dialog.

Insert or edit target ranges for up to 10 dose increments. The current specified dose increments are displayed. The ending relative pressure and the dose amount (entered or as the fraction of the previous volume adsorbed) for each target range are shown.
Insert Edit

Displays the Dose Increment Edit dialog.

Ending pressure Enter the desired ending pressure of this segment. Dose increment Select this option to have the sample dosed with a specified amount of gas for each isotherm point taken.

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Insert Edit

(continued)

Percent of previous Select this option to have the sample dosed with a percentage of the volume adsorbed during the previous interval of the table. For example if in the previous segment 5 cm3 STP of gas was adsorbed and you enter 40% in this field, this segment will dose 2 cm3 STP for each isotherm point taken. This feature is disabled for the first entry of the dose increment table.

Delete

Deletes the selected range. Clears the table of all entries except one; one entry is required.

Clear

Absolute pressure dosing

Select this option to specify pressure targets in mmHg, mbar, or kPa instead of relative pressure. This option is typically selected when using adsorptives at analysis conditions above the critical point of the gas; for example, H2 adsorption on carbon at liquid nitrogen temperature. Displays the Analysis Preparation dialog.

Preparation

Fast evacuation

Select this option for samples (such as pellets) that do not fluidize or shed particles during evacuation. These fields are enabled when Fast evacuation is not desired, allowing you to enter an evacuation rate and the pressure at which unrestricted sample evacuation is to begin.

Evacuation rate Unrestricted evac. from

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Open

Evacuation time

Enables you to enter the length of time for preliminary evacuation, which takes place prior to the free-space measurement. Enables the system to check for system leaks or sample outgassing before the analysis. The leak test seals the sample tube and monitors the pressure. If the pressure rises more than 0.15 mmHg, the analysis does not proceed and you are notified with a message. While leak testing slightly increases analysis time, it prevents the continuation of analysis and collection of erroneous data if a leak exists. When you select this option, the Leak test duration field is enabled so that you can specify how long the pressure is to be monitored.

Leak test

Use TranSeal

Select this option if you are using the TranSeal to transfer the sample from the preparation port to the analysis port under vacuum. Displays the Free Space dialog, allowing you to specify the type of free-space measurement you wish to use.

Free Space

Refer to Appendix D, page D-1 for a discussion of free-space methods.

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Measure

Measures the free space automatically over the sample prior to data collection. Lower Dewar for evacuation Lowers the Dewar during evacuation. Evacuation time Enter the time you wish to allow for evacuation after the freespace measurement. Outgas test Checks the system for sample outgassing after the free-space measurement. The outgas test seals the sample tube and monitors the pressure. If the pressure rises more than 0.025 mmHg within the time specified in the Outgas test duration field, outgassing is present. If outgassing is found, the test repeats up to nine times with a 30-minute evacuation time between each test. If the 10th test fails, the analysis does not proceed and you are notified of its cancellation. Outgas testing slightly increases analysis time, but it prevents continuation of analysis and collection of erroneous data if outgassing is present.

Enter

Enables the Warm free space and Cold free space fields so that you may enter the free space manually. The warm free space is the sample tube gas capacity measured at room temperature. The cold free space is the sample tube gas capacity measured with the Dewar raised.

Calculate

Select this option to have the free-space measurement calculated using the sample and tube parameters. If you choose this option for a tube in which there is no sample, be sure to enter 0 in the Density field.

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pº and T

Displays the pº and Temperature Options dialog.

This dialog provides six options for obtaining the saturation pressure (pº) and analysis bath temperature. Clicking on each option prompts you for the entry of related parameters in the lower portion of the dialog.
Option Prompts for...

1

the analysis bath temperature. This method measures the pº on a continuous basis; enabling you to measure every data point without slowing down the analysis.

2

an analysis bath temperature. This method measures the pº on a continuous basis and over the sample, then adjusts the measured pº in the sample tube to agree with the pº over the sample.

3

a pº and analysis bath temperature, or an analysis bath temperature only (when Absolute pressure dosing is selected on the Analysis conditions dialog). This method uses the values you enter in the fields.

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Option

Prompts for...

4

a psat gas. If this is a Krypton analysis, be sure to select the Krypton @ 77.35 K SOLID option from the dropdown list. Click Psat vs T to edit the values of the Psat vs T table if desired. Editing the values in the current table does not affect the ones of the original table.

5

an analysis bath temperature and an estimate for the initial pº. This method measures the pº over the sample. After the pº is measured, the value is reapplied to all data points.

6

an analysis bath temperature. This method calculates the pº at the time of analysis using the temperature you enter.

Options 1, 2, and 5 cannot be used for krypton analyses. If you have selected From Psat tube (for krypton analysis) on the analysis dialog and a pº option other than 3, 4, or 6 was selected , an error message is displayed when you attempt to start the analysis.
Equilibration

Displays the Equilibration dialog.

Does not display when Absolute dosing is selected.

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Relative Pressure (P/Po) Equilibration interval

The relative pressure for which the equilibration interval will be applied. The number of seconds between successive pressure readings during equilibration. At least 11 pressure readings for each equilibration are required to obtain an accurate reading of the pressure changes. • Long equilibration intervals tend to lengthen analyses, but improve data integrity. Short equilibration intervals produce a faster analysis but may reduce the accuracy of data.

Minimum equilibration delay at P/Po> = 0.995

The value entered in this field determines the minimum number of seconds required before equilibration can occur for a relative pressure greater than or equal to 0.995. This field does not display if you select Absolute pressure dosing on the analysis conditions dialog.

Backfill

Displays the Sample Backfill Options dialog, allowing you to select options for backfilling the sample tube at the start and end of an analysis.

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Adsorptive Properties
This dialog allows you to specify the characteristics of the gases used in the TriStar system. An Adsorptive properties file can be created as an independent parameter file or as part of the sample information file.
Be sure to save this file to the directory you specified as the Parameter files directory if it is to be included in the drop-down list on the Basic and Restricted Sample Information dialogs (see Parameter Files Directory, page 8-15).

Adsorptive

If this is a new file, this field contains the name of the default adsorptive gas. Enter a description for the adsorptive gas for which you are creating the file. You can use up to 40 alphanumeric characters.

Mnemonic

The mnemonic name for the adsorptive gas; for example, N2 for nitrogen, CO2 for carbon dioxide, etc. Select this option if this file is for a non-condensing gas (adsorptive). You must also select the Absolute pressure dosing option on the Analysis Conditions dialog when you select Non-condensing Adsorptive. When you select this option, the Density conversion factor field and the Psat vs. T push button become disabled.

Non-condensing Adsorptive

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Maximum manifold pressure Non-ideality factor

The maximum gas pressure allowed in the manifold.

Enter a factor to compensate for the forces of attraction between molecules in a real gas. Enter the density conversion factor. The density conversion factor is determined by obtaining the ratio of the gas volume (STP) to the liquid volume. The thermal transpiration hard-sphere diameter.

Density conversion factor

Therm. tran. hard-sphere diameter Molecular cross-sectional area
Replace

The molecular cross-sectional area.

Allows you to replace the values in the current adsorptive properties file with those from another file. A dialog is displayed so that you may select the desired file. Click OK; the values are copied into the new file automatically. You may edit the values in the new file; the file from which they were copied remains unchanged. Displays the Psat vs. Temperature dialog for the adsorptive gas; this example shows for Nitrogen.

Psat vs. T

This table contains saturation pressures and their corresponding temperatures. The table may include as many as ten entries; at least two are required.

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Psat vs. T

(continued)

Edit the table by moving the cursor to the desired saturation pressure or temperature and entering a different value. Points always have to be in an ascending order. If you try to add a point which is less than the previous one, you will receive an error message. Inserts a new row. A row is inserted above the selected line; the cursor moves to the new line. Deletes the selected row. Select the manner in which the sample tube is dosed. Select From Psat tube for krypton. Select Normal for all other gases.

Insert

Delete

Dosing Method

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Report Options
This dialog allows you to specify report options for a new file or to edit an existing one. A report options file can be created as an independent parameter file or as part of the sample information file.
Be sure to save this file to the directory you specified as the Parameter files directory if it is to be included in the drop-down list on the Basic and Restricted Sample Information dialogs (see Parameter Files Directory, page 8-15).

Description

If you are editing an existing file, this field displays a description of the report options file. You may change the name if you wish. If this is a new file, the default report options description is displayed. Enter a name for this file. You can use up to 40 alphanumeric characters.

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Show report title

Enables you to enter a title for your report. If this is a new file, the title you specified as the default is displayed. You can accept the default title or enter a new one. You can enter up to 50 alphanumeric characters. If you deselect this option, a title will not display on the report.

Show graphic

Select this option to have a graphic display above the report title. The graphic can be in a bitmap (bmp) or an enhanced metafile (emf) format. For example, you may wish to display your company logo. Click Browse to choose the graphic, then use the Height and Width fields to specify a size. This image can be edited from the report window.

Replace

Allows you to replace the values in the current report options file with those from an existing file. A dialog is displayed so that you may select the desired file. Click OK; the values are copied into the new file automatically. You may edit the values in the new file; the file from which they were copied remains unchanged.

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Overlays

Displays the Graph Overlay Samples dialog.

Choose the sample files you wish to overlay onto selected plots. Click Browse to the right of the Sample [n] field to choose a file. You may select up to eight files. Use the Clear push button to clear the field of its entry. After choosing your file(s), be sure to select the Overlay samples option for each report type you plan to overlay. Refer to Generating Graph Overlays, page 3-35 for instructions on generating overlays. Apply thermal transpiration correction Select this option to correct for the temperature-induced pressure difference between the manifold and the chilled sample tube. This option is most significant for pressures less than approximately 1.0 mmHg. Never use filler rods in the sample tube when applying correction for thermal transpiration. Always use thermal transpiration when performing micropore analyses. Inside diameter of sample tube Enabled when you select Apply thermal transpiration correction, so that you may enter the inside diameter of the sample tube.

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Selected Reports

Contains a list of available reports: • • • • • • • • • • • • • • • • • • • • • Summary Isotherm BET Surface Area Langmuir Surface Area Freundlich Temkin t-Plot Alpha-S Method f-Ratio Method BJH Adsorption BJH Desorption Dollimore-Heal Adsorption Dollimore-Heal Desorptioin Horvath-Kawazoe DFT Pore Size DFT Surface Energy Dubinin MP-Method Options Sample Log Validation

Refer to Selecting Reports, page 2-13 for information on selecting reports.
Edit

Displays an associated dialog for the selected report. Editing options for available reports are shown in subsequent sections. You cannot edit the Options and Sample Log reports.

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Summary Report The summary report provides a condensed listing of selected data results. Click Edit for Summary report options; the Summary Report Options dialog is displayed.

The choices on this dialog allow you to choose the types of data to include in the Summary report. If you choose Adsorption or Desorption total for Pore Volume data, the P/Po field is enabled so that you can enter the relative pressure at which to calculate the total pore volume. If Use calculation assignments (Collected Data screen) is not selected, the isotherm is interpolated to this value and that point used for the Total pore volume calculation. Otherwise, the point selected with calculation assignment is used. This dialog also enables you to specify Pass/Fail criteria for up to four parameters.
Select All

Selects all choices on the dialog. Deselects all choices on the dialog.

Deselect All

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Pass/Fail Selection

Displays the parameter you selected on the Pass/Fail Options dialog. Displays the Pass/Fail Optioins dialog so that you can choose a parameter on which to specify pass/fail criteria.

Pass/Fail

Upper/Lower

Select these options to specify upper and lower limits for the selected parameter; a valid range for the selected field is displayed in the information bar. You can leave the range open by deselecting one of the limits. For example; if you wish to leave the upper limit open, deselect the Upper check box and specify a value only for the Lower limit. Each of these fields has a message line in which you can enter advice to the operator if a failure occurs. You may enter up to 120 characters in each field.

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Isotherm Report Options The isotherm report indicates adsorption (up to saturation pressure) and desorption (down from saturation pressure) of a gas by a solid held at constant temperature.

Select Reports

Lists the types of reports offered. Choices: Tabular Report, Linear plot, Logarithmic plot, Linear Absolute plot, Logarithmic Absolute plot Pressure Composition plot

Options

Displays the related Plot Options dialog; this example shows the dialog for the Linear plot.

All plot dialogs contain the same options. You can plot the graphs as a curve, points, or both.

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Options

(continued)

Select Overlay samples to overlay data from the current plot with data from other samples. The other sample files are selected by clicking Overlays on the Report Options dialog. Autoscale options enable you to have the X- and/or Y-axes automatically scaled. Linear X-axes begin at zero, and logarithmic X-axes begin at an appropriate value. Y-axes begin at zero. The system uses the highest values collected during analysis as the ending points for axes ranges. If you choose not to autoscale data, the From and To fields are enabled, allowing you to specify a range. Data collected outside these ranges are not included in the plot. The value entered in the To field must be greater than the value entered in the From field. The X-axis fields show the relative pressure.The Y-axis fields show the quantity of gas adsorbed

Tabular Options

Enables you to have Run Time and/or Time Between Points reported. Run time reports the time elapsed from the beginning of the analysis to the finish. Time between points reports the time relapsed between each point. Also enables you to report Weight % when plotting pressure composition.

Plot Options

Enables you to choose the type of isotherm you wish to plot. You can plot the adsorption and/or the desorption isotherm. Enables you to choose the manner in which the volume adsorbed is reported. These data are reported by default as Per Gram (cm3/g). However, you can choose to report data Per BET Surface Area (cm3/m2) or Per Other Surface Area (m2/g). If the latter field is selected, a field is enabled allowing you to enter a value. The Adsorbate Molecular Weight field is enabled when you choose Pressure Composition plot, allowing you to enter the molecular weight of the adsorbate. This plot is useful for plotting pressure as a function of Weight % adsorbed; for example, H2 adsorbed on carbon.

Volume Adsorbed

Weight

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BET/Langmuir Surface Area Report Options • The BET calculation obtains the sample surface area value by determining the monolayer volume of adsorbed gas from the isotherm data. Refer to BET Surface Area, page C-7 for additional information. • The Langmuir calculation determines the surface area of a sample by relating the surface area to the volume of gas adsorbed as a monolayer. Refer to Langmuir Surface Area, page C-9 for additional information. The Langmuir and BET Surface Area dialogs include the same fields; the operating instructions for both are the same.
Displays as Langmuir Surface Area Report Options if the Langmuir report is being edited.

Tabular report BET (or Langmuir) Transform plot BET (or Langmuir) Isotherm plot Overlay samples

Select this option to have a tabular report of the plotted data. Generates a traditional BET (Langmuir) surface area plot that is used to determine monolayer volume and BET C constant. Uses the BET (Langmuir) monolayer volume and constant to produce an isotherm. Allows you to overlay data of the selected type from the current plot with data from other samples. The other samples are selected by clicking Overlays on the Report Options screen.

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Autoscale x-axis Autoscale y-axis

Select these options to have the X- and/or Y-axes scaled automatically. Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges. The X-Axis Range fields show the relative pressure. The Y-Axis Range fields show the quantity of gas adsorbed.

From/To fields

Enabled when you choose not to autoscale data (deselect the Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot. The values entered in the To field must be greater than the value entered in the From field. Displays the Report Relative Pressure Table dialog so that you may edit or enter relative pressure points.

Pressures

Does not display for Langmuir.

If Use calculation assignments is not selected on the collected/Entered dialog, the isotherm is interpolated to these pressure points, and those interpolated values are used in the BET calculations. If Use calculation assignments is selected, collected data are used.

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Insert Predefined

Displays the Surface Area Report Pressure Selection dialog, allowing you to select predefined points. Choices: None, 1 Point, 3 Point, 5 Point, 5 Point Low Pressure

Does not display for the Langmuir report.
Insert

Inserts a row into the table above the selected line; the cursor moves to the new line. Deletes the selected row. Removes all but the one required entry from the table. The rows do not have to be selected. A warning message requesting confirmation is displayed before the table is cleared.

Delete Clear

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Freundlich Report Options The Freundlich isotherm is an empirical isotherm that is used to model low-pressure adsorption data. It can also be applied to model some micropore isotherms.

Refer to Freundlich Isotherm, page C-38 for information on report calculations. Specify monolayer capacity In this field, enter the monolayer capacity of the sample.

Absolute pressure range

Allows you to enter a pressure range when calculation assignments are not requested.

Tabular report

Select this option to have a tabular report of the pressure points generated.

Transform plot

Plots the log(p) vs log(Q) in a straight line.

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Isotherm plot

Plots the absolute pressure vs quantity adsorbed. Shows best fit line.

Overlay samples

Choose this option to overlay Freundlich isotherm data from the current file with the same type of data from other samples (files). The desired files are chosen by clicking Overlays on the Report Options dialog.

Autoscale x-axis Autoscale y-axis

Select these options to have the X- and/or Y-axis scaled automatically. Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges. The X-axis shows the log of absolute pressure and the Y-axis shows the quantity of gas adsorbed.

From/To fields

Enabled when you choose not to autoscale data (deselect the Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot.

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Temkin Isotherm The Temkin isotherm is used to model adsorption data where the heat of adsorption drops linearly with increasing coverage.

Refer to Temkin Isotherm, page C-39 for information on report calculations. Specify monolayer capacity Specify differential heat of adsorption at zero surface coverage Absolute pressure range Tabular report In this field, enter the monolayer capacity of the sample.

Enter the differential heat of adsorption at zero surface coverage. This allows inclusion of all Temkin constants.

Allows you to enter a pressure range when calculation assignments are not requested. Select this option to have a tabular report of the pressure points generated

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Transform plot Temkin Isotherm plot

Plots a linear form of the Temkin isotherm. Overlays the Temkin isotherm with the analysis data.

Overlay samples

Choose this option to overlay Temkin isotherm data from the current file with the same type of data from other samples (files). The desired files are chosen by selecting Overlays on the Report Options dialog.

Autoscale x-axis Autoscale y-axis

Select these options to have the X- and/or Y-axis scaled automatically. Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. The X-axis shows the natural log of absolute pressure and the Y-axis shows the quantity of gas adsorbed. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges.

From/To fields

Enabled when you choose not to autoscale data (deselect the Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot.

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t-Plot Report Options The t-Plot calculation allows quantitative analysis of the area and total volume ascribed to micropores. Matrix area, the area external to micropores, is directly determined and often proves to be a valuable way of characterizing complex mixed materials.

Refer to t-Plot, page C-10 for information on report calculations. Thickness Curve Presents the type of thickness curves available. • • • • • • Reference Kruk-Jaroniec-Sayari Halsey Harkins and Jura Broekhoff-de Boer Carbon Black STSA

You can also apply the Frenkel-Halsey-Hill thickness curve using the Halsey option, and entering the appropriate values in the equation. Use Edit to edit the values in the equation.
Edit

Displays the equation for the type of thickness curve selected so that you may view or edit the values.

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Reference

Displays the Entered t-Curve dialog allowing you to define a t-curve by entering the relative pressure and thickness values.

This table can also be created in another application if desired and imported into this dialog using Open. When creating the table in another application, the file must be saved as ASCII text with a THK extension. Use a two-column format with the relative pressures in the first column and the thickness values in the second column. Columns must be separated by a space (or a tab).
Open

Allows you to import the values from an existing thickness curve (THK) into this table. One predefined curve is shipped with the analysis program and is found in the Referenc directory. The Referenc directory is defaulted when you select this push button. After the values are copied into the table, you may edit them if desired. Editing these values will not affect the file from which they were copied.
Save As

Enables you to save the current table of values as a thickness curve. After the table is saved you can use Open to import the values (see above)
Clear

Clears the table of all but one entry; one entry is required

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Kruk-Jaroniec-Sayari

Displays the Kruk-Jaroniec-Sayari Thickness Equation dialog.

The values shown in the above dialog are the defaults; you can edit them if desired. Halsey Displays the Halsey Thickness Equation dialog.

The Halsey method is sometimes referred to as FrenkelHalsey-Hill. The values shown in the above dialog are the defaults; you can edit them if desired. Refer to t-Plot, page C-10 for more information.

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Harkins and Jura

Displays the Harkins and Jura Thickness Equation dialog.

You can edit the values for the numerator, first element of the denominator, and exponent. Refer to t-Plot, page C-10 for more information. Broekhoff-de Boer Displays the Broekhoff-de Boer Thickness Equation dialog.

You can edit the values for the multiplier, numerator, and exponent. Carbon Black STSA Displays the Carbon Black STSA Thickness Equation dialog.

All coefficients can be edited. Refer to t-Plot, page C-10 for more information.

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Surface Area group box

Allows you to choose the surface area value used for thickness calculations. You can use BET (most commonly used), Langmuir, or enter one of preference. Displays the Report Relative Pressure Range dialog so that you may specify minimum and maximum relative pressures to use with this report.

Pressure Range

If Use calculation assignments is not selected on the Collected/Entered dialog, all of the nonoutlier points of the collected data within the specified range are used for calculating the data for this report. If Use calculation assignments is selected, collected data points which are assigned to this report type are used.

Fitted Thickness Range

Provides two fields, allowing you to enter the minimum and maximum thicknesses you wish to include in the thickness curve. The values entered for the thicknesses can be expressed in angstroms or nanometers. Select Options > Units to specify desired units.

Surface area correction factor

This value corrects for surface areas that are not smooth and brings the values for BET surface area and micropore surface area into accordance. For most samples, the default value of 1.000 is adequate. Select this option to have a tabular report generated. Select this option to have a graphical representation of data.

Tabular report t-Plot

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Overlay samples

Allows you to overlay data from the current sample file with data from other sample file(s). The other sample file(s) are chosen by clicking Overlays on the Report Options screen. Select these options to have the X- and/or Y-axes scaled automatically. Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges.

Autoscale x-axis Autoscale y-axis

From/To fields

Enabled when you choose not to autoscale data (deselect the Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot. The value entered in the To field must be greater than the value entered in the From field. The X-Axis Range fields show the relative pressure The Y-Axis Range fields show the quantity of gas adsorbed.

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Alpha-S Plot The Alpha-S plot converts the standard adsorption isotherm into a dimensionless isotherm using the quantity adsorbed at a relative pressure of 0.4.

Table

Provides two columns for entering the relative pressure (first column) and the alpha-s values (second column). This table can also be created in another application if desired and imported into this dialog using Open. When creating the table in another application, the file must be saved as ASCII text with an ALS extension. Use a two-column format with the relative pressures in the first column and the alpha-s values in the second column. Columns must be separated by a space (or a tab).

Insert

Inserts a row above the selected row. A row cannot be inserted if the value in the selected row is at its lowest value; values must be strictly increasing. For example, in the table shown above, the default value is 0.000000001. Therefore you must use Ctrl + Down arrow to insert rows. Deletes the selected row.

Delete

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Clear

Clears the table of all but one entry; one entry is required. Allows you to import the values from an existing alpha-s curve (ALS) into the table. One predefined curve is shipped with the analysis program and is located in the Referenc directory. The Referenc directory is defaulted when you click this push button. After the values are copied into the table, you may edit them if desired. Editing these values will not affect the file from which they were copied. Enables you to save the current table of values under a file name. Provides two fields for entering the minimum and maximum relative pressures from which the fit will be determined. Enables you to enter the surface area from the reference curve. This value is used to calculate the sample surface area. Provides two fields for entering a pressure range when calculation assignments are not used. Choose this option to have a tabular report generated Choose this option to have the data plotted as a graph. Allows you to overlay data from the current sample file with data from other sample files. The other sample files are chosen by clicking Overlays on the main Report Options screen. Select these options to have the X- and/or Y-axes scaled automatically. Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges.

Open

Save As

Fitted alpha-S Range

Ref. surface area

Relative pressure range

Tabular report Alpha-S Plot Overlay samples

Autoscale x-axis Autoscale y-axis

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From/To fields

Enabled when you choose not to autoscale data (deselect the Autoscale option), allowing you to specify the beginning and ending ranges of the X- and/or Y-axis. Data collected outside these ranges are not included in the plot. The value entered in the To field must be greater than the value entered in the From field. The X-Axis Range fields show the relative pressure. The Y-Axis Range fields show the quantity of gas adsorbed.

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f-Ratio Plot The f-Ratio report allows you to take the measured isotherm and normalize it using a reference isotherm.

Reference Isotherm

Displays the sample file you choose as a reference. You should always choose a file containing an isotherm measured from a non-porous sample of the same material as the current sample. Click to choose the sample file you wish to use as a reference for the isotherm. Allows you to enter a pressure range when calculations assignments are not used. Choose this option to have a tabular report generated The tabular report contains four columns: relative pressure, quantity adsorbed for the isotherm of interest, quantity adsorbed for the reference isotherm, and the ratio of the quantities adsorbed. Choose this option to have the data plotted as a graph.

Browse

Relative pressure range

Tabular report

f-Plot

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Overlay samples

Allows you to overlay data from the current sample file with data from other sample files. The other sample files are chosen by clicking Overlays on the Report Options screen. Select these options to have the X- and/or Y-axes scaled automatically. Both X- and Y-axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data, the From and To fields are enabled, allowing you to enter the ranges.

Autoscale x-axis Autoscale y-axis

From/To fields

Enabled when you choose not to autoscale the axis, allowing you to enter a range.

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BJH Adsorption/Desorption Report Options The BJH calculation determines the mesopore volume/area distribution which accounts for both the change in adsorbate layer thickness and the liquid condensed in pore cores. You can generate BJH reports from both adsorption and desorption data.
Or BJH Desorption Report Options

Does not display on the Desorption dialog.

The BJH Adsorption and Desorption dialogs include the same fields; the operating instructions for both are the same.

Thickness Curve

Presents the type of thickness curves available. • • • • • • Reference Kruk-Jaroniec-Sayari Halsey Harkins and Jura Broekhoff-de Boer Carbon Black STSA

The choices in this group box allow you to choose the type of thickness curve you wish to use; you can also edit values in the equation, if desired.

An incomplete pore distribution may be generated if you select a thickness curve which is not a good match for the sample being analyzed.

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Edit

Displays the equation for the type of thickness curve selected. Refer to t-Plot Report Options, page 5-46 for an explanation of the dialogs associated with this push button. Enter the minimum diameter (radius or width) of pores you wish to have included in the BJH reports. The value entered in this field must be less than the value entered in the Maximum BJH field. Enter the maximum diameter (radius or width) of pores you wish to have included in the BJH reports. The value entered in this field must be greater than the value entered in the Minimum BJH field. During adsorption calculations, the software assumes that all pores are closed at one end. Sometimes a percentage of pores may be open at both ends, causing disagreement in the adsorption and desorption data or in the values for total volume and total BJH pore volume. In this field, you may enter the fraction of pores open at both ends to compensate for this error. This field is not shown on the BJH Desorption Report Options dialog.

Minimum BJH (diameter, radius, or width)

Maximum BJH (diameter, radius, or width)

Fraction of pores open at both ends

Adsorptive

Displays the BJH Adsorptive Options dialog.

The recommended adsorptives and their values are shown. You may specify up to six additional adsorptive/adsorbate property factor combinations.

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Adsorptive

(continued)

The adsorbate property factor is the combination of constants in the numerator of the BJH equation which is specific to the type of gas used. Adsorbate property factors may be specified in angstroms or nanometers. Select Options > Units to specify units. Smooths all differential calculations, eliminating variations in the differential computation caused by noise in the input data. Select Larger to report the total volume found in pores larger than the current pore size. This is the traditional way in which BJH data are displayed. Select Smaller to report the total volume found in pores smaller than the current pore size.

Smooth differentials

Cumulative Reports

Pressure Range

Displays the Report Relative Pressure Range dialog so that you may enter the range of pressures to use with this report. • If Use calculation assignments is not selected on the Collected/Entered dialog, all of the non-outlier points of the collected data within the specified range are used for calculating the data for this report If Use calculation assignments is selected, collected data points which are assigned to this report type are used.

Selected Reports

Contains a list of available BJH reports: • • • • • • • Tabular Report Cumulative Pore volume dV/d* Pore Volume dV/dlog(*) Pore volume Cumulative Pore Area dA/d* Pore Area dA/dlog(*) Pore Area

* = width, radius, or diameter You can measure pore width (w), pore radius (R), or pore diameter (D) for BJH reports. Select Options > Units to choose the desired measurement.

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Selected Reports (continued)

Choose a report by double-clicking on the report name or highlight the report name and press the Spacebar. A report is selected when it is preceded with a check mark. Reports are deselected in the same manner.

Edit

Allows you to edit the selected report. Editing options for available reports are shown in the following sections.

Tabular Report Click Edit for the BJH Adsorption/Desorption tabular report to specify the method of data reduction; the BJH Adsorption (or Desorption) Tabular Report Options dialog is displayed.

Fixed pore size table

Specify exact pore sizes for which volume or area data are reported. Only the pore sizes within the specified range are reported. When you select this option, the Table push button is enabled so that you may enter or edit a fixed pore size table.

Collected points

Includes all relative pressure points collected by the system

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Columns

Displays the BJH Adsorption (or Desorption) Tabular Report Column Options dialog.

The default column title appears next to the column number. Each column includes a drop-down list of the data types available for inclusion in the report. You can measure pore width, pore radius, or pore diameter.
Table

Enabled when you choose Fixed pore size table. Displays the BJH Adsorption (or Desorption) Fixed Pore Size Table dialog so that you may enter or edit a fixed pore size table.

The fixed pore size table must contain a minimum of two points and may include as many as 1000. The points must be strictly decreasing.

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Insert

Inserts a row into the pressure table. The row is inserted above the selected row and the cursor moves to the new row. Deletes the selected row from the pressure table. Clears all points from the pressure table; none have to be selected.

Delete

Clear

Plot Options Click Edit for BJH Adsorption/Desorption plots to specify plotting methods and to customize plots. A dialog similar to the following is displayed when you select a BJH plot

Plot curve Plot points X-axis Linear/Logarithmic

Plot data as a curve, points, or both.

Lists the scale options for the x-axis. Choose whether you wish to have the X-axis on a logarithmic or linear scale.

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Autoscale

Select this option to have the x-axis scaled automatically. The lowest and highest values collected during analysis are used as the beginning and ending points. When you deselect this option, the adjacent fields are enabled so that you can specify beginning and ending values. Data ranges are displayed in the information bar across the bottom of the dialog when a cursor is in a numerical data field.

Y-axis Variable Overlay

Lists the options for the y-axis. Choose the desired variable for the Y-axis. Displays a list of overlay choices. You may choose to overlay the current plot with data from other samples or with other plots from this sample. Select this option to have the y-axis scaled automatically. The lowest and highest values collected during analysis are used as the beginning and ending points. When you deselect this option, the adjacent fields are enabled so that you can specify beginning and ending values. Data ranges are displayed in the information bar across the bottom of the dialog when a cursor is in a numerical data field.

Autoscale

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Dollimore-Heal Adsorption/Desorption Report Options You can generate DH reports from both adsorption and desorption data.

Or Dollimore-Heal Desorption Report Options

The options for Dollimore-Heal reports are the same as those for the BJH reports with the exception of BJH Correction and Adsorptive properties; this item is not applicable to DH reports. Refer to BJH Adsorption/Desorption Report Options, page 5-57 for a description of the fields on this dialog.

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Horvath-Kawazoe Report Options

Pore Geometry

Select the option in this group box which best represents the physical geometry of the micropores in the sample material. If you choose Sphere, interaction parameters are disabled. Refer to Horvath-Kawazoe, page C-22 for information on report calculations.

Apply Cheng/Yang correction

Allows you to apply the Cheng/Yang correction to the pore size analysis. This correction substitutes the Langmuir equation of state for Henry’s Law in the Horvath-Kawazoe derivation (see Appendix C, page C-25 for calculations).

Smooth differentials

Smooths the differential calculations, eliminating variations in the differential computation caused by noise in the input data.

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Pressure Range

Displays the Report Relative Pressure Range dialog so that you may specify minimum and maximum relative pressures to use with this report. • If Use calculation assignments is not selected on the Collected/Entered dialog, all of the nonoutlier points of the collected data within the specified range are used for calculating the data for this report. If Use calculation assignments is selected, collected data points which are assigned to this report type are used.

Interaction Parameter

Select one of the options in this group box to determine which interaction parameter is used during report generation. These options are disabled when you choose Sphere as the pore geometry.

Computed

The interaction parameter is calculated using the parameters on the Horvath-Kawazoe Physical Properties dialog. You can click Properties to view or edit these parameters. Each time you change one of the parameters, the interaction parameter is recalculated. Refer to Interaction Parameter, page C-26 for the formula for computing the interaction parameter.

Entered

The value you enter in the adjacent field will be used.

Properties

Use this push button to view or edit the constants (used during report generation) describing the physical properties of the adsorbent and adsorptive; the Horvath-Kawazoe Physical Properties dialog is displayed.

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Properties

(continued)

These options are disabled if Entered is selected as the interaction parameter.

Adsorbent Group Box

Contains the parameters for the sample. If you select Computed for the interaction parameter, all fields are enabled and can be edited if desired. If you select Entered, only the values in the Diameter and Diameter at zero energy fields may be edited. Description The name of the adsorbent used in the analysis. Click on the down arrow to make a new selection. Each time you change the selection, the values for that adsorbent are displayed in the appropriate fields. Diameter The diameter of the sample atom. Diameter at zero energy The diameter of an atom at zero interaction energy, (2/5)1/6 x diameter. Polarizability The polarizability of the adsorbent. Magnetic susceptibility The magnetic susceptibility of the adsorbent. Density The density per unit area of the adsorbent

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Adsorptive Group Box

Contains the parameters for the adsorptives (provided with the software and/or user-defined). If you select Computed for the interaction parameter, all fields are enabled and can be edited if desired. If you select Entered, only the values in the Diameter and Diameter at zero energy fields may be edited. Mnemonic The mnemonic name of the adsorptive gas in use. Click on the down arrow to make a new selection. Each time you change the selection, the values for that adsorptive display in the appropriate fields. If no parameters have been defined, the default values are displayed. Diameter The diameter of the adsorptive atom. Diameter at zero energy The diameter of an atom at zero interaction energy, (2/5)1/6 x diameter. Polarizability The polarizability of the adsorptive. Magnetic susceptibility The magnetic susceptibility of the adsorptive. Density The density per unit area of the adsorptive.

Selected Reports

Lists the available Horvath-Kawazoe reports. Choose a report by double-clicking on the report name or highlight the report name and press the Spacebar. A report is selected when it is preceded with a check mark. The following reports are available: • • • Tabular Report Cumulative Pore Volume dV/dw Pore Volume

Edit

Allows you to edit the selected report.

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Tabular Report Options Displays the Horvath-Kawazoe Tabular Report Column Options dialog so that you can select the type of data to display in each column.

The default column title displays next to the column number. Each column includes a dropdown list of the types of data to include in the report.

Plot Options Selecting a Horvath-Kawazoe plot option from the Horvath-Kawazoe Report Options dialog enables you to specify the plotting method used for your report and to customize the plot. Plots for Cumulative Pore Volume and dV/dw Pore Volume are available. When you select either of these plots from the Horvath-Kawazoe Report Options dialog, a dialog like the following is displayed.

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Plot curve Plot points

Plot data as a curve, points, or both.

X-axis options

Choose Autoscale to have the x-axis scaled automatically. The X-axis begins at zero and the system uses the highest value collected during analysis as the ending point. If you deselect Autoscale, the adjacent fields are enabled so that you may enter a beginning and ending value. Data collected outside these ranges are not included in the plot. X-axis range fields show pore radius or diameter in angstroms or nanometers. Data ranges are displayed in the information bar across the bottom of the dialog when the cursor is in a numerical data entry field.

Y-axis options

Click on the down-arrow at the Variable field to choose a variable for the Y-axis. Click on the down-arrow at the Overlay field to overlay the plot with data from other samples. Choose Autoscale to have the y-axis scaled automatically. Y-axes begin at zero. The system uses the highest value collected during analysis as the ending point. If you deselect Autoscale, the corresponding fields are enabled so that you may enter a beginning and ending value. Data collected outside these ranges are not included in the plot. Y-axis range fields show the quantity of gas adsorbed Data ranges are displayed in the information bar across the bottom of the dialog when the cursor is in a numerical data entry field.

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DFT Pore Size

Type

Drop-down list containing the types of models available; DFT or Classical. DFT models are based on the density functional theory. Classical models are based on the Kelvin equation and thickness for determining the pore size distribution. Refer to Appendix F, page F-1 for a discussion on models. Refer to DFT (Density Functional Theory), page C-40 for information on report calculations.

Geometry

Drop-down list containing pore shapes available; Slit or Cylinder. Lists the models that meet the criteria specified and which match the adsorbate and temperature of the sample data. The models display in alphabetical order with the first one automatically selected; you may select any one desired. If the list is empty, there were no models that meet the selected criteria.

Models

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Pressure Range

Displays the Report Relative Pressure Range dialog so that you may specify minimum and maximum relative pressures to use with this report. • If Use calculation assignments is not selected on the Collected/Entered dialog, all of the nonoutlier points of the collected data within the specified range are used for calculating the data for this report. • If Use calculation assignments is selected, collected data points which are assigned to this report type are used.

Regularization

These choices enable you to choose the extent of smoothing you wish to have applied to your data, or your can choose None. If you choose Entered, its field is enabled allowing you to enter a number giving a relative weight for the smoothing during deconvolution. Larger values produce more smoothing.

Reports to Generate

Displays the types of reports available. • • • • • • • • • • Tabular Report Isotherm table Cumulative area graph Incremental area graph Differential area graph Cumulative volume graph Incremental volume graph Differential volume graph Log goodness of fit graph* Goodness of fit graph*

Graph details can be edited by selecting the Edit push button. *These graphs cannot be edited.

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Edit

Use this push button to edit details of a selected graph; a dialog like the following is displayed.
Displays the type of graph you are editing.

This push button is disabled for tables and Goodness of Fit graphs. Plot Type Enables you to choose the manner in which you wish to display plotted data; as a curve or as a histogram. Select these options to have the axes scaled automatically. If you deselect one or both of these options, you must enter a range in the related Axis Range fields which become enabled automatically. Overlay This drop-down list contains the type of overlays available for the current graph. Choose Samples to overlay the same type of graph as the current one from other data reductions. Then select Overlays on the Report Options dialog to choose your files (explained on page 5-33). Axis Range The fields in this group box become enabled when you deselect Autoscale, allowing you to specify beginning and ending values for the X- and/or Y-axis. Data collected outside these ranges are not included in the plot. Valid ranges for a selected field are displayed in the information bar across the lower portion of the dialog. The X-axis displays the energy and the Y-axis displays the area.

Autoscale Options

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DFT Surface Energy

The fields on the DFT Surface Energy dialog are identical to those on the DFT Pore Size dialog with the following exceptions: Geometry drop-down list Is not applicable to the Surface Energy report and, therefore, does not display on its dialog. Displays the types of reports available. • • • • • • • Tabular report Isotherm table Cumulative area graph Incremental area graph Differential area graph Log goodness of fit graph Goodness of fit graph

Reports to Generate

Graph details can be edited by selecting the Edit push button.

Refer to the previous section for the DFT Pore Size report beginning on page 5-71 for information on the fields contained on this dialog.

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Dubinin Report Options

Report Type

Allows you to specify the type of report you wish to generate. At least one type of report must be selected. Select Radushkevich to generate the Radushkevich report. Select Astakhov to generate the Astakhov report. With this choice, you may select Optimize exponent. If you do not select this option, the Exponent field is enabled so that you can enter a value. Refer to Dubinin-Astakhov, page C-32 and DubininRadushkevich, page C-30 for information on report calculations.

Fitted relative pressure range

Allows you to specify minimum and maximum limits on relative pressures included in the line fit. Data collected outside these limits are not included in the line fit.

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Adsorptive

Allows you to specify up to ten adsorptive/affinity coefficient (beta) combinations. The Dubinin Adsorptive Options dialog is displayed.

Pressure Range

Displays the Report Relative Pressure Range dialog so that you may specify minimum and maximum relative pressures to use with this report. • If Use calculation assignments is not selected on the Collected/Entered dialog, all of the non-outlier points of the collected data within the specified range are used for calculating the data for this report If Use calculation assignments is selected, collected data points which are assigned to this report type are used.

Selected Reports

Lists the available Dubinin reports. Choose a report by double-clicking on the report name or highlight the report name and press the spacebar. A report is selected when it is preceded with a check mark. The following reports are available: • • • Dubinin Tabular Report Transformed Isotherm dV/dw Pore Volume (Astakhov only)

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Tabular Report Options Selecting Tabular Report from the Dubinin Report Options dialog enables you to customize your report with up to six columns of data for Astakhov reports and up to five columns of data for Radushkevich reports. The Dubinin Tabular Report Column Options dialog is displayed.

The default column title appears next to the column number. Each column includes a dropdown list of the data types to include in the report. The value for n (shown in column 5) is the optimized exponent if Optimized Astakhov exponent is selected on the Dubinin Report Options dialog. If not, then the value for n is the entered exponent value.

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Transformed Isotherm Plot Options Selecting Transformed Isotherm from the Dubinin Plot Option dialog enables you to restrict the line fit to a portion of the isotherm. The Dubinin Transformed Isotherm Plot Options dialog is displayed.

Overlay Samples

Select this option to overlay the current plot with data from other samples. Then click Overlays on the Report Options dialog to choose the sample files. Select these options to have the X- and/or Y-axes automatically scaled. Both axes begin at zero; the system uses the highest values collected during analysis as the ending points for axis ranges. If you choose not to autoscale data for either (or both) axis, the corresponding fields are enabled so that you may enter a beginning and ending value. The X-axis shows the quantity of gas adsorbed at standard temperature and pressure. The Y-axis shows the log of relative pressure. Data ranges are displayed in the information bar across the bottom of the dialog when the cursor is in a numerical data entry field.

Autoscale x-axis Autoscale y-axis

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Pore Volume Options When you select dV/dw Pore Volume from the Dubinin Report Options dialog, the Dubinin dV/dw Pore Volume Options dialog is displayed.

Plot curve Plot points Overlay samples

Plot data as a curve, points, or both.

Select this option to overlay data from other samples. Then click Overlays on the Report Options dialog to choose the files. Select these options to have the X- and/or Y-axes automatically scaled. Both axes begin at zero; the system uses the highest values collected during analysis as the ending points. If you choose not to autoscale data for either (or both) axis, the corresponding fields are enabled so that you may enter a beginning and ending value. Data collected outside these ranges are not included in the plot. Data ranges are displayed in the information bar across the bottom of the dialog when the cursor is in a numerical data entry field.

Autoscale x-axis Autoscale y-axis

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MP-Method Report Options

Pore size can be expressed in Angstroms or nanometers. Select Options > Units to specify the desired unit.

Thickness Curve

Select the thickness curve type from this group box. You must choose either the Halsey equation or the Harkins-Jura equation. Use Equation to edit the values in the equation. Refer to MP-Method, page C-36 for information on report calculations.

Harkins and Jura

Displays the Harkins and Jura Thickness Equation dialog.

You can edit the values for the numerator, first element of the denominator, and exponent.

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Halsey

Displays the Halsey Thickness Equation dialog.

You can edit the values for the multiplier, numerator, and exponent.
Equation

Displays the equation for the type of thickness curve selected. Lists the available MP-Method reports. Choose a report by double-clicking on the report name or highlight the report name and press the spacebar. A report is selected when it is preceded with a check mark (3). The following reports are available: • • • • • MP Tabular Report Cumulative Pore Volume dV/dw Pore Volume Cumulative Pore Area dA/dw Pore Area

Selected Reports

The data for these reports are measured in pore width only.
Edit

Enables you to edit the selected report. Displays the Report Relative Pressure Range dialog so that you may specify minimum and maximum relative pressures to use with this report. • If Use calculation assignments is not selected on the Collected/Entered dialog, all of the non-outlier points of the collected data within the specified range are used for calculating the data for this report If Use calculation assignments is selected, collected data points which are assigned to this report type are used.

Pressure Range

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Tabular Report Options Selecting Tabular Report from the MP-Method Report Options dialog enables you to customize your report with up to six columns of data. The MP-Method Tabular Report Column Options dialog is displayed.

The default column title appears next to the column number for columns three through six. Each of these columns includes a drop-down list of the data types to include in the report. The following data types are available: • • • • • • Incremental Pore Volume cumulative Pore volume dV/Dw Pore volume Incremental Pore Area Cumulative Pore Area dA/dw Pore Area

Columns 1 and 2 are fixed and cannot be edited.
The MP-Method reports hydraulic radius only. If you select Pore size in diameter from the Unit Selection dialog, pore size in radius will be reported.

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Plot Options Selecting an MP-Method plot option from the MP-Method Report Options dialogs enables you to specify the plotting method used for your report and to customize the plot. The following plots are available: • • • • Cumulative Pore Volume dV/dw Pore Volume Cumulative Pore Area dA/dw Pore Area

When you select any of the plots from the MP-Method Report Options dialog, a dialog similar to the following one is displayed. The fields on all dialogs are the same.

Plot curve Plot points X-Axis

Plot data as a curve, points, or both.

Choose Autoscale to have the x-axis scaled automatically. The X-axis begins at zero and the system uses the highest values collected during analysis as the ending point. If you deselect Autoscale, the corresponding fields are enabled so that you may enter a beginning and ending value. Data collected outside these ranges are not included in the plot. Data ranges are displayed in the information bar across the bottom of the dialog when the cursor is in a numerical data entry field.

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Y-Axis Variable Overlay

Click on the down-arrow to choose a variable for the Y-axis. You can use the choices in this drop-down list to overlay plots. You can choose a different type of plot for the current sample to overlay with the listed Variable, or you can choose Samples to overlay the variable plot with the same type of plot from other samples. Click Overlays on the Reports Options dialog to choose the samples. Choose this option to have the y-axis scaled automatically. Y-axes begin at zero. The system uses the highest values collected during analysis as the ending points for axes ranges. If you deselect this option, the corresponding fields are enabled so that you may enter a beginning and ending value. Data collected outside these ranges are not included in the plot. Y-axis range fields show the volume of gas adsorbed. Data ranges are displayed in the information bar across the bottom of the dialog when the cursor is in a numerical data entry field.

Autoscale

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Options Report The Options report is a subset of the contents report; it provides pertinent information for the following: • • • • • • • • Sample tube Degas conditions Adsorptive properties Analysis conditions Free space Po and temperature Equilibration Isotherm collection

Sample Log Report The Sample Log report displays the following: • Manual control operations performed during analysis • Information entered using Add Log Entry on the sample file editor • Warnings and/or errors which occurred during analysis

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Validation Report Use this report to have your data examined by the software to determine if the results are within typical ranges.

If the data for any report(s) you selected for validation are determined to be out of range, a warning is displayed and suggestions are given for corrective action. This information is also detailed in the report and plotted on the graph as a unique plot symbol.

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Entered or Collected Data
If you select Manually Entered on the Advanced view of the Sample information dialog, an Entered tab is added enabling you to enter the data.

If you select Automatically collected, a Collected tab is added after the analysis is completed.

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Pressure table

For collected data, columns for the following are displayed: • • • • • absolute pressure relative pressure quantity adsorbed outliers (if Use calculation assignments is not selected) calculation assignments for each requested report option (if Use calculation assignments is selected)

For entered data, columns for the following are displayed: • absolute or relative pressure, depending on the selection in the Pressures group box quantity adsorbed


Insert

Enabled for entered data. Inserts a row into the pressure table. Enabled for entered data. Deletes the selected row. Enabled for entered data. Clears the table of all but one entry; one is required. If selected, allows you to assign the points for each report type. If deselected, each report (with the exception of Langmuir and BET) uses a range of pressures as selected in the report options. The Langmuir and BET reports interpolate to entered relative pressures on the report options. The outlier points can be selected so that they will not be reported.

Delete

Clear

Use calculation assignments

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Pº and T

Displays the Pº and T dialog.

This dialog allows you to edit the Po measurement and analysis bath temperature.
Free Space

Displays the Free Space dialog, allowing you to edit freespace values.

This dialog also shows the isotherm for the analysis. The isotherm is redrawn each time values are edited. You can also customize parts of the isotherm plot, as well as zoom in for finer detail. Right-click in the graph area to display a shortcut menu displaying the options available. Refer to Shortcut Menus, page 7-24.

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Measured

Displays the Warm and Cold free-space values if Measured was chosen as the Free-space method for the analysis; these values cannot be edited.. Enables the Warm, Cold, and Non-ideality Factory fields so that you may enter the values manually. The warm free space is the sample tube gas capacity measured at room temperature. The cold free space is the sample tube gas capacity measured with the Dewar raised. The non-ideality factor compensates for the forces of attraction between molecules in a real gas.

Entered

Calculate

Select this option to have the free-space measurement calculated using the sample conditions and sample tube parameters. Displays the volume for the port used in the blank analysis.

Port volume

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Save

Save
Save enables you to save any changes you have made to the file in the active window. The file is saved under its current name.

Save As
Save As enables you to: • save a sample or parameter file in the active window under a different name. This option is useful for making a duplicate copy of a file that you can modify as desired without changing the original one. The original file remains open when you use this function, so be sure to open the new file before making any changes. • save a subset (parameter) of the sample file in the active window as a standalone parameter file. For example, select Analysis Conditions from the Save As menu to create a standalone parameter file of the analysis conditions portion of the active sample file. • save as an ASCII file the relative pressures and corresponding thicknesses (t-Curve). These data are derived by dividing the condensed volume of adsorptive by the selected surface area. The density conversion factor in the adsorptive properties file is used to convert quantity adsorbed to volume of condensed adsoptive. • save as an ASCII file the relative pressures and resulting quantities adsorbed (Alpha-S). These data are derived by dividing the isotherm by the quantity adsorbed at 0.4 relative pressure.

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Save As

TriStar II 3020

Sample and Parameter Files
A dialog similar to the one shown below is displayed when you select Sample Information, Sample Tube, Degas Conditions, Analysis Conditions, Adsorptive Properties, or Report Options.
Indicates the type of file being saved.

Enter a file name (up to eight characters) in the File name field; the appropriate extension is appended automatically when you click OK. The new file is saved as specified, but does not remain in the active window. Be sure to open the new file before making any changes to the file.

t-Curve and Alpha-S Files
The same type of dialog shown above is also displayed when you select t-Curve or Alpha-S. However, before you receive this dialog for t-Curve, the Save As t-Curve dialog is displayed. This dialog allows you to choose the surface area for the sample.

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Save All

Save All
Save All enables you to save all open files under their current names. This option provides a faster way to save all open files at one time and avoids having to perform a Save operation on each individual file.

Close
Close enables you to close the file in the active window. The following message is displayed if changes have been made to the file: (File name) has been changed. Save changes before closing? Yes No Cancel

Yes saves any changes and closes the active window. No discards any changes and closes the active window. Cancel returns you to the open file.

Close All
Close All enables you to close all open files under their current names. The following message is displayed for each file in which changes have been made: (File name) has been changed. Save changes before closing? Yes No Cancel

Yes saves any changes and closes the active window. No discards any changes and closes the active window;. Cancel returns you to the open file.

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Print

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Print
Print enables you to print the contents of one or more sample or parameter files to the printer, screen, or to a file. For example, if you choose Analysis Conditions, you will receive the parameters used for all analysis conditions associated with the file(s). The print dialog is common to all file types.
Indicates the type of file you are printing.

Does not display for parameter files.

File name

The name of the file you select from the Files list box is copied to this field. Enabled when Printer is selected as the print destination, allowing you to print up to four copies Select the destination. You may print to a printer, the screen, or to a file. Enabled when you select File as the destination. A default file name (the same name as the sample file) appears if you choose only one file; you can use the default name or enter another one. If you select multiple files, the default displays as *.RPT; each file will be exported as its original file name with the RPT extension.

Copies

Destination

File name

Refer to Selecting Files, page 2-11 for an explanation of the remaining fields on this dialog.

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List

List
List enables you to generate the following information on a selected sample or parameter file. • • • • • File name Date the file was last edited Time the file was last edited File identification File status

The List dialog is common to all file types.

Indicates the type of file on which statistics have been requested.

Does not display for parameter files.

The behavior of the List dialog is the same as the Print dialog; refer to Print, page 5-94 for an explanation of the fields on this dialog. You may request a list of multiple files by holding down Ctrl while selecting files. If no files are selected, a list is generated for all files.

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Export

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Export
Export allows you to copy the isotherm data in a sample information file and reformat it in an ASCII format acceptable to other programs, such as spreadsheets. The output file consists of four columns containing the elapsed time, absolute pressure, relative pressure, and specific quantity adsorbed (see example on next page).
You may export multiple files by holding Ctrl while selecting the files.

Select File > Export; the Export Sample File dialog is displayed.

File name

The name of the file you select from the Files list box is copied to this field. You can export data to a printer, to the screen, or to a File. • If you select Printer, the Copies field is enabled allowing you to print up to four copies. If you select File, the File Type and File name fields are enabled.

Destination

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File Type

You can export data in a spreadsheet format (XLS) or as a text file (TXT). Allows you to specify a name for your exported file, or you may accept the default. The default name is the name of the sample file appended with the appropriate extension.

File name

Refer to Selecting Files, page 2-11 for an explanation of the remaining fields on this dialog.

Format of Data Output
This example shows the format of the output file for exported data.

Description Operator Submitter Sample mass Type of Data*

Elapsed time

Absolute pressure

Relative pressure

Specific quantity adsorbed

*0 = automatically collected 1 = entered (relative pressures) 2 = entered (absolute pressures)

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Convert

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Convert
Convert enables you to convert StarDriver files (MGD extension) to a format compatible with the TriStar 3020 analysis program. The only files that will display in the Files window are those with the MGD extension.

Files window

Displays the StarDriver files in the current directory (the current directory is shown just above the Directories window). Refer to page 2-13 for information on navigating to other directories. Displays the current directory and the name of the selected file with an SMP extension. If you wish to save the file in a different directory, be sure to enter (or navigate to) the desired directory. You can choose multiple files by holding down Ctrl while selecting the files. These options are explained in Selecting Files on page 3-6.

Destination

Date Range

Files Directories

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Exit

Exit
Exit enables you to exit the TriStar analysis program. Select File > Exit from the main menu. If an analysis is in progress, it will continue until completion; analysis data are collected and stored in an embedded controller. • If a window containing a modified file is open, the following message is displayed: Modifications have been made to (file name). Do you want to save the modifications? Yes No Cancel

Yes saves any changes and exits the analysis program. No abandons any changes and exits the analysis program. Cancel returns you to the open file.

• If an analysis is in progress, the following message is displayed: CAUTION: Sample analysis is in progress. If you exit the program, analysis will continue to completion, but the data are not saved to disk until the program is restarted. Do you want to exit the program? Yes No

Yes exits the analysis program. No leaves the analysis program active and allows the analysis to finish. Although data are stored in an embedded controller when you exit the program, data are not saved to disk until you restart the program and save the data. If a power failure occurs and the analyzer does not have an Uninterruptible Power Supply (UPS), any unsaved data are lost.

• If a report is in progress, the following message is displayed: CAUTION: Reports are being generated. If you exit the program these reports will be canceled. Do you want to cancel reports and exit the program? Yes No

Yes cancels the reports and exits the analysis program. No leaves the analysis program active and allows the reports to finish.

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Description

6. UNIT MENU
The Unit menu contains the options for the operations which can be performed with the TriStar 3020. The main menu will contain a Unit menu for each attached analyzer. For example, if you have two attached analyzers, the main menu contains two Unit menus. The status displays associated with each unit are displayed in different colors. The unit number and the serial number also are displayed in the title bar of the operational windows. This is especially convenient if you have more than one analyzer attached to the same computer.
The Unit menu does not appear on the menu bar if the analysis program is being used for offline data operations on a computer other than the one controlling the analyzer.

Description

Listed below are brief descriptions of the Unit menu options. Detailed descriptions are found later in this chapter. Sample Analysis Allows you to perform up to three analyses using different analysis conditions. Page 6-3. Allows you to perform multiple sample analyses using the same analysis conditions, allowing you to create sample files at the time of analysis. Page 6-8.

QuickStart Analysis

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Description

TriStar II 3020

Krypton Analysis Blank Analysis Enable Manual Control Show Instrument Schematic Show Status Show Instrument Log

Enables you to perform a krypton analysis. Page 6-11. Enables you to perform a blank analysis. Page 6-12. Allows you to control the system manually. Page 6-14. Displays the analyzer’s schematic. Page 6-17.

Displays the status window. Page 6-19. Displays a log of recent analyses, calibrations, and error messages. Page 6-21. Displays software version, hardware configuration, and calibration information. Also allows you to enter mnemonic names for port gases. Page 6-23. Enables you to perform predefined diagnostics. Page 6-24. Enables you to perform certain instrument calibrations. The options on this menu are enabled only with the direction of a Micromeritics service representative. Page 6-27. Enables you to perform certain troubleshooting procedures. This option is enabled only with the direction of a Micromeritics service representative. Page 6-30.

Unit Configuration

Diagnostics Calibration

Service Test

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Sample Analysis

Sample Analysis
Use this mode of operation to schedule analyses which have different analysis conditions or report options. You can schedule up to three analyses at a time. You can continue to schedule analyses by clicking Next (appears after the first series of analyses are finished) on the analyzing view of the Analysis dialog. Samples cannot be removed from or added to ports until the full set of analyses has completed. Select Unit > Sample analysis; the Analysis dialog is displayed.

View

Allows you to choose the view you wish to display in the window. Operation displays the current mode of operation. Instrument Schematic displays a schematic of the TriStar system. Refer to Show Instrument Schematic, page 6-17 for additional information. Instrument Log displays a list of recent analyses, calibrations, and errors or messages. Refer to Show Instrument Log, page 6-21 for additional information.

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6-3

Sample Analysis

TriStar II 3020

Close Valves

Enabled when analysis is complete, allowing you to close all sample port valves immediately; otherwise the valves close in approximately five minutes. This field is blank until you choose a file to use for the analysis on this port. Click this push button to select a sample information file for the current; the Open Sample Information dialog is displayed. You can choose an existing file or accept the next sequenced number to create a new; default values will apply. Clears the information displayed for this port. Displays the identification of the selected sample file or the default description if creating a new one; this field may be edited if desired. Displays the value specified in the sample file; enter the mass for the current sample.. Displays the density of the sample specified in the sample information file; this, too, may be edited if needed. This value is applicable only when using the calculated free-space method. Enabled if you have selected Entered for the Po measurement for at least one file. Enter the Po value, or edit the current one. Enter the temperature for the analysis bath.

Port [n]

Browse

Clear

Sample

Mass

Density

Po

Bath temperature

6-4

Mar 08

TriStar II 3020

Sample Analysis

Report After Analysis

Allows you to have a report generated automatically after the analysis; displays the Report Settings dialog so that you may specify output options.

Export After Analysis

Allows you to have isotherm generated automatically after the analysis; displays the Export Settings dialog so that you may specify output options.

Start

Starts the analysis; displays an analyzing view of the Analysis dialog.

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6-5

Sample Analysis

TriStar II 3020

Port activity

Status window

This view also displays port activity as well as the status window.
Skip

Skips an analysis; visible only when an analysis is in progress. The Skip dialog is displayed so that you may choose the port(s) containing the analysis you wish to skip.

A check box is included for each port on which an analysis is being performed. This example shows only one port being used.
Suspend

Suspends an analysis; visible only when an analysis is in progress. A dialog similar to the one shown above is displayed so that you may choose the port(s) containing the analysis you wish to suspend.

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TriStar II 3020

Sample Analysis

Resume

Resumes a suspended analysis; visible only when an analysis is suspended. A dialog similar to the one shown above is displayed so that you may choose the port(s) containing the analysis you wish to resume. These push buttons allow you to generate reports on data collected at that time for the sample in the respective port. The reports are printed to the screen only. Cancels an analysis; enabled only when an analysis is in progress. A dialog similar to the one shown above is displayed so that you may choose the port(s) containing the analysis you wish to cancel. On this view of the Analysis dialog, this push button changes to Next when analyses are finished. Returns you to the first view of the Analysis dialog so that you may schedule additional analyses. Closes the Analysis dialog.

Report [n]

Cancel

Start

Next

Close

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QuickStart

TriStar II 3020

QuickStart
Use this mode of operation to analyze samples of the same type using the same analysis conditions, adsorptive properties, and report options. You may schedule up to three analyses at a time. You can continue to schedule analyses by clicking Next (appears after the first series of analyses are finished) on the analyzing view of the Analysis dialog. Select Unit > QuickStart analysis to display the QuickStart dialog.

View

Allows you to choose the view you wish to display in the window. Operation displays the current mode of operation. Instrument Schematic displays a schematic of the TriStar system. Refer to Show Instrument Schematic later in this chapter for additional information. Instrument Log displays a list of recent analyses, calibrations, and errors or messages. Refer to Show Instrument Log later in this chapter for additional information.

Close Valves

Allows you to ensure that all valves are closed before analysis is started. After analysis begins, this push button is disabled.

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Mar 08

TriStar II 3020

QuickStart

Sample ID Operator

Enables you to enter a name for the current series of samples. Enables you to enter the operator’s name, or some other appropriate identifier. This group box allows you to have a report generated automatically after each analysis. You can specify a destination and, when Printer is selected, the number of reports to be printed. If you choose File, the File name field is enabled. You can accept the default name or enter a new one.

Report Options

Export Options

Enables you to have isotherm data exported automatically after analyis. Advances you to the second view of the QuickStart dialog.

Next

This view of the QuickStart dialog allows you to specify sample information for the current set of samples.

The behavior of this dialog is the same as the Analysis dialog; refer to Sample Analysis, page 6-3 for a description of the fields on this dialog.

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6-9

QuickStart

TriStar II 3020

Port [n] Sample tube

Enables you to select the port(s) being used in the analyses. Enables you to select the sample tube file you wish to use; applicable only if you have selected the calculated method for measuring the free space. Starts the analysis; displays an analyzing view of the Analysis dialog. This view contains data collection for each analysis, as well as port information. Refer to the previous section for an explanation of the push buttons contained on this dialog. When analyses are complete, the second view of the dialog again is displayed, allowing you to quickly start the next set of samples.

Start

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Mar 08

TriStar II 3020

Krypton Analysis

Krypton Analysis
This option enables you to perform up to three krypton analyses at the same time. Use the following guidelines for performing krypton analyses: • All analyses must use krypton gas; if a gas other than krypton is specified, an error message is displayed. • From Psat tube must be selected as the Dosing Method (Adsorptive Properties dialog); an error message is displayed if this has not been selected. • Samples cannot be removed from or added to ports until the full set of analyses has completed.

The fields on this dialog are the same as for those on the Analysis dialog; refer to Sample Analysis, page 6-3 for a description of the fields on this dialog.

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6-11

Blank Analysis

TriStar II 3020

Blank Analysis
A blank analysis is used for obtaining sample tube parameters when using a calculated free space. A blank analysis can also be used for diagnostic purposes.

The behavior of this dialog is the same as the Analysis dialog; refer to Sample Analysis, page 6-3 for a description of the fields on this dialog. Port [n] Enables you to choose the port(s) you are using for a blank analysis. Displays the file name assigned to the blank analysis on the current port. File names are assigned automatically and contain appropriate conditions for performing a blank analysis. Click this push button to replace the values of the current file with those of an existing file. Appropriate default conditions for a blank analysis are contained in the assigned file. However, if you require a different set of conditions, you can use this push button to copy them into the assigned file.

Replace All

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TriStar II 3020

Blank Analysis

Sample

Enables you to enter an identification for the blank analysis. Use the dollar sign to have the automatically generated file name appear in the identification. For example, if you enter $ Blank Analysis Jan 2008 in the Sample field for Port 1 in the dialog shown above, BK1-000 Blank Analysis Jan 2008 will display as the identification in printed reports. The assigned file name will display wherever you place the $ sign within the identification.

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6-13

Enable Manual Control

TriStar II 3020

Enable Manual Control
Select this option to control certain components of your system manually. The instrument schematic must be visible to use this option. If it is not visible, select Unit [n] > Show Instrument Schematic.

Servo valve Elevator

When manual control is enabled, the valve symbols change color on the monitor screen to indicate their status. Green = open Yellow = closed

Each component that can be manually controlled has a shortcut menu displaying the operations available for that particular component. These menus may be accessed by selecting the desired component, then clicking the right mouse button once, or pressing Shift + F9. The options available for the components on the instrument schematic are: Valves 1 through 15 Open, Close, Pulse Open and Close open and close the valves. You may also open and close the valves by double-clicking on the valve or by pressing the Spacebar while the valve is selected. Pulse quickly turns the valve on and off, allowing the operation to proceed in small increments. You may also pulse the valve by pressing P while the valve is selected.

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TriStar II 3020

Enable Manual Control

Table 6-1. System Valves
Valve(s) Description

1 through 3 4 5 6 7 8 and 9 10 11 through 13 14 15 Unmarked

Sample ports Po port Isolation valve Isolation valve Helium port Analysis gas ports Vacuum Unrestricted vacuum for sample ports Analysis gas port 10-mmHg isolation valve (displays only if the Krypton option is installed). Servo

Servo Valve

Set, Close Set displays the Servo Valve Settings dialog so that you may choose to dose or evacuate and specify a target pressure. You may also display this dialog by pressing Spacebar while the servo valve is selected.

Close closes the servo valve. You may also close the servo valve by pressing Spacebar while the servo valve is selected.

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Enable Manual Control

TriStar II 3020

Elevator

Raise, Lower, Stop Raise and Lower raise and lower the elevator. You may also raise and lower the elevator by double-clicking in the elevator area or pressing Spacebar while the elevator area is selected. Stop stops the elevator at its current position. You may also stop the elevator by double-clicking in the elevator area or pressing Spacebar while the elevator area is selected.

These components are for informational purposes only; they cannot be controlled manually. Represents the sample tube.

Represents the pº (saturation pressure) tube.

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TriStar II 3020

Show Instrument Schematic

Show Instrument Schematic
Select this option to display a schematic of the analyzer. Refer to the previous section for an explanation of the components contained on the instrument schematic.
Displays only if the Krypton option is installed.

Even when manual control is not enabled, you still can determine the state of the valves by their color. Green = open White = closed

If you wish to change the state of a valve, you must enable manual control. A tool bar has been included on the instrument schematic, making it convenient and easy to perform commonly used operations.
Open Sample File

Displays the Open Sample Information dialog, enabling you to open and view or edit a sample file. Refer to Sample Information, page 5-4 for detailed information. Displays the Start Report dialog so that you can choose a sample file on which to generate report data. Refer to Start Report, page 7-3 for detailed information.

Start Report

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6-17

Show Instrument Schematic

TriStar II 3020

Start Analysis

Displays the Analysis dialog so that you can start an analysis, or analyses. Refer to Sample Analysis, page 6-3 for detailed information. Displays the QuickStart dialog so that you can begin a series of analyses. Refer to QuickStart, page 6-8 for detailed information. Displays the Control Chart dialog so that you can specify options for generating an SPC Control Chart report. Refer to Control Chart, page 7-11 for detailed information.

QuickStart Analysis

SPC Control Chart

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TriStar II 3020

Show Status

Show Status
Select this option to show only the status window of the analyzer.
If you have multiple instruments attached to your computer, the status bar for each instrument is displayed in a different color.

The status window shows the current status for each port. You may wish to use this option if: • You have an automatic operation in progress and you wish to edit a sample file. This way, you can keep up with the status of your operation while performing another task. • You have multiple units attached to your computer. You can select Show Status on each unit menu and have the status for all units displayed at one time. The Status window, like the instrument schematic, includes a tool bar of commonly used operations.
Open Sample File

Displays the Open Sample Information dialog, enabling you to open and view or edit a sample file. Refer to Sample Information, page 5-4 for detailed information. Displays the Start Report dialog so that you can choose a sample file on which to generate report data. Refer to Start Report, page 7-3 for detailed information. Displays the Analysis dialog so that you can start an analysis, or analyses. Refer to Sample Analysis, page 6-3 for detailed information.

Start Report

Start Analysis

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6-19

Show Status

TriStar II 3020

QuickStart Analysis

Displays the QuickStart dialog so that you can begin a series of analyses. Refer to QuickStart, page 6-8 for detailed information. Displays the Control Chart dialog so that you can specify options for generating an SPC Control Chart report. Refer to Control Chart, page 7-11 for detailed information.

SPC Control Chart

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TriStar II 3020

Show Instrument Log

Show Instrument Log
Displays a log of recent analyses, calibrations, and errors or messages. By default, this information is logged for a 7-day period for analyses and a 30-day period for messages and calibrations. You may change the time for which this information is retained in the Unit section of the WIN3020.INI file.

You can choose the type of information to display in the window by selecting only the desired item(s). For example, select only the Analysis option to display analysis information:

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6-21

Show Instrument Log

TriStar II 3020

Analysis Calibration Message
Add Log Entry

These options allow you to choose which entries to display in the window.

Enables you to make an entry in the instrument log that cannot be recorded automatically through the application software. For example, you may change the port filter. The field adjacent to the push button allows you to enter the operation; the push button is enabled when you make an entry in the field, allowing you to add the entry. Displays the Log Report Settings dialog so that you can specify report output options.

Report

Use the Start Date field to specify a date at which to start the printout. You can specify a date using one of the following methods: • • Press F2 to clear the field so that you can enter a date Double-click in the field (or press F4) to display a calendar to choose a date Press F3 to insert the current date

The Copies field is enabled when you select Printer as the destination, enabling you to print up to four copies. Choose the report destination in the Destination field. If you choose File as the destination, the File name field is enabled, allowing you to enter a name for the printed file (or you may accept the default).

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TriStar II 3020

Unit Configuration

Unit Configuration
Select this option to display hardware/software configurations, calibrations, and gas selections of the connected analyzer. When you select this option from the Unit menu, the Unit Configuration dialog is displayed.

Configuration

Displays the IP address used by the analysis program and the serial number of the selected analyzer. Also enables you to view details of the boards installed in the analyzer. Displays the software versions of the MICBIOS, controller, and TriStar 3020 analysis program. Enables you to specify the mnemonic names for the analysis gas(es). Gas inlet valves V8, V9, and V14 are designated for analysis gases; V7 is dedicated to the free-space measurement which uses Helium (He). You can enter up to three characters. Displays the date the servo valve was last calibrated. The remaining group boxes display calibration information for their respective component.

Software Versions

Gas Selections

Servo Valve Calibration group boxes

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6-23

Diagnostics

TriStar II 3020

Diagnostics
This option enables you to clean and verify gas lines when connecting or changing a gas (refer to Cleaning and Verifying the Gas Line, page 9-24 for step-by-step instructions). This option also allows you to perform diagnostic tests which your service representative may request. The data generated from these tests may be insignificant to you as a user, but can be very helpful to your service representative. Your service representative can view the results and may be able to resolve the problem, eliminating downtime and repair costs. These tests generate files to the 3020\Service\userdiag directory. Your service representative will request that you E-mail or fax the files to him so that he may examine them. When you select Unit [n] > Diagnostics, the Service Test dialog is displayed:

View

Allows you to view the current operation, the instrument schematic, or the instrument log in the Service Test dialog. Operation is the appropriate choice for tests. Contains a list of diagnostic tests. These tests will always include the latest revision letter at the end of the test name. Displays the test file number. This number is assigned automatically and incrementally sequenced by the software each time a test is performed. This also serves as the name of the file that is generated to the userdiag directory, and will be appended with SVT. For example, the name of the file for the test shown in the above dialog is 0006.SVT.

Test

Sequence

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Mar 08

TriStar II 3020

Diagnostics

Report after test

Select this option to have a report generated automatically after the test; page 6-9 provides an explanation of output options. If you do not select this option, you can still have a report generated from the report window.

Cancel

Cancels the test. Begins the test; displays the next view of the Service test dialog. The second view of the Service test dialog may contain a single pane or two panes, depending on the test selected.

Next

Report (field)

Contains a list of the reports that will be generated during this test. Lists the data in the two panes. Item 1 is the upper pane and Item 2, the lower pane. Enables you to generate a report. Cancels the test.

Item [n]

Report (push button)

Cancel

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Diagnostics

TriStar II 3020

The following push buttons become enabled when the test is complete.
Repeat

Repeats the test; not applicable for this test. Returns you to the first view of the Service Test window. Closes the dialog.

Next

Close

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TriStar II 3020

Calibration

Calibration
This option allows you to perform system calibrations. Some calibrations are disabled and can be accessed only when using the Service Test Mode with the assistance of your service representative. .

Zero Pressure
Use this option to evacuate the manifold and zero the selected transducers. The Calibrate Pressure Offset dialog is displayed.

Choose the transducer(s) you wish to have offset to zero. Be sure to install a sample tube on the selected ports. Click Start; a dialog indicating evacuation is in progress is displayed. When evacuation is complete, the dialog closes automatically.

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6-27

Calibration

TriStar II 3020

Match Transducers
Use this option to zero and match the selected transducers to the main manifold transducer.

Choose the transducer(s) you wish to have matched. Be sure to install a sample tube on the selected ports. Click Start; a progress dialog is displayed. When the operation is complete, a confirmation dialog is displayed; click OK to close the dialog.

Servo Valve
Use this option to calibrate the servo valve to the manifold pressure transducer. The servo valve should always be recalibrated after a pressure calibration has been performed. The Calibrate Servo Valve dialog is displayed.

The only action required here is to click Start. The servo valve is then used to fill and equilibrate the manifold, first to approximately 760 mmHg and then to approximately 50 mmHg. The pressure transducer readings (previously calibrated) at these points are used to calibrate the servo set point. Status messages are displayed during this procedure and a confirmation dialog is displayed when the operation is finished; click OK to close the dialog.

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TriStar II 3020

Calibration

Store Instrument Information
This option enables you to store calibration information in a text file, allowing you to view calibration parameters. When you select this option, the information is stored and a dialog giving the location of the saved file is displayed.

Make a note of the location, then use a utility such as Notepad to open the file.

Save to File
Use this dialog to save the current calibration settings to a file that you can reload; the Select Calibration File dialog is displayed.

File name

The default for naming calibration files is the serial number, then the next sequenced number. For example in the dialog shown above, the number has defaulted to 201-002.CAL, where 201 represents the instrument serial number and 002 represents the second calibration file saved. You can enter a different name if you wish; up to eight characters.

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Service Test

TriStar II 3020

Load from File
Displays the Select Calibration File dialog (shown above) so that you can load a different calibration file. When you choose a file and click OK, the following dialog is displayed.

This error message states that changing your calibration may affect the performance of your instrument. If you click Yes to continue, the selected file is loaded and a backup of the current calibration is saved as (SN)last.cal allowing you to reload the settings using the backup file. Although a backup file is created, it is recommended that you save the current calibration settings using the Save to File command before loading another file. A backup file is written over each time a new one is created. The Save to File function saves the file permanently.

Service Test
Certain service tests are included in the operating program, but can be performed only with the assistance of a trained Micromeritics service representative. These tests are designed to provide your service representative with instrument readouts, as well as to assist him in troubleshooting potential problems and, perhaps, eliminating unnecessary repair services. This service strategy allows you to conduct expert tests in less time than it would take to be properly trained in servicing the instrument. This option is enabled only when the analysis program is operating in Service Test mode (refer to Service Test Mode, page 8-15 for additional information).

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TriStar II 3020

Description

7. REPORTS MENU
This chapter describes the commands on the Reports menu; it also contains examples of reports. Reports can be generated for data: • collected on a sample that has completed analysis • collected on a sample that is currently being analyzed (includes only the information collected up to the time of the report) • that is manually entered

Description
Listed below are brief descriptions of the commands contained on the Reports menu. Detailed descriptions follow this section.

Start Report

Allows you to generate a report on a completed sample analysis or on the data collected thus far for an analysis in progress. Page 7-3. Closes all open report windows. Page 7-5. Enables you to open a report that was saved from the report window. Page 7-5. Allows you to specify the sample data to be included in SPC reports. Page 7-6.

Close Reports Open Report

SPC Report Options

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7-1

Description

TriStar II 3020

Regression Report Control Chart Heat of Adsorption

Allows you to generate a regression report. Page 7-7. Allows you to generate a control chart report. Page 7-11. Allows you to generate a heat of adsorption report. Page 7-15.

7-2

Mar 08

TriStar II 3020

Start Report

Start Report
Select this option to generate a report on a sample analysis; the Start Report dialog is displayed.

File name

The name of the sample file you select from the Files list window is copied to this field. If you select multiple files, the last one selected is displayed. If you have a sample file open, its name defaults to this field. • If you select multiple files on which to have reports generated, the reports specified in each sample file are printed to the output destination. If you choose a single file, the Select Reports dialog containing the available reports is displayed.

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7-3

Start Report

TriStar II 3020

Status

This drop-down list determines what type of sample files are displayed in the Files list window in the specified directory for all dates, or within the specified range of dates (using Date Range push button). Refer to Table 2-2. File Status and Description, page 2-12 for a description of status types. Displays the Select Dates dialog so that you may specify a range of dates. Refer to Selecting Files, page 2-11 for a description of this push button. Enabled when the Printer destination is chosen, enabling you to print up to four copies of the selected report(s). Enables you to print to a printer, to the screen, or to a file. If you select Screen, reports are displayed onscreen, allowing flexibility in manipulating and customizing reports. Refer to Printed Reports, page 7-19 for detailed information. If you select File, the tabular reports of the requested file are converted to a text file which can be viewed with a text editor or other text file manipulation tool.

Date Range

Copies

Destination

File name

Enabled when you select File as the destination. Allows you to enter a name, or you may accept the default. Displays a list of the available sample files for the choice shown in the Status field and within the range of dates specified in the Select Dates dialog. Displays a list of available drives and directories. The drive and directory last accessed is displayed immediately above the Directories list box.

Files list box

Directories

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TriStar II 3020

Close Reports

Close Reports
This option enables you to close all open report windows at one time. This avoids having to select close on each report window. This option is unavailable if reports are being generated.

Open Report
This option enables you to open a report that was saved from the Report window; the Report window opens with an Open dialog positioned on top.

Report Window

After you navigate to the desired directory, select your file, and click Open, your saved report is displayed in the Report window.

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7-5

SPC Report Options

TriStar II 3020

SPC Report Options
When you select SPC Report Options, the SPC Report Options dialog is displayed.

The SPC Calculations dialog lists the variables available for SPC reporting. You can check as many as desired. However, for efficiency, it is best to select only the variables you actually intend to us. All variables selected must be computed for each sample file used in an SPC report. Click More on this dialog to display the SPC Calculations dialog.

The options on this dialog allow more detailed reports.

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TriStar II 3020

Regression Report

Regression Report
Select this option to generate a regression report. The regression report is used to determine the interdependency between two variables. Up to three dependent variables (Y-axis) may be plotted against a single independent variable (X-axis). The degree of correlation between the variables also is reported. The graphs for the regression report are scaled so that all three fit on a single page. If you choose less than three, the graphs are scaled to fill most of the page.

Show report title

Select this option to have a title display on your report. Accept the default or enter a new title. You can enter up to 40 alphanumeric characters. Deselect this option to omit the report title.

Show graphic

Select this option to have a graphic display above your report title. For example, you may wish to display your company logo. The graphic must be a bitmap (bmp) or enhanced metafile (emf). Click Browse to choose the file, then use the Height and Width fields to specify a size. This image can be edited in the report window (when printed to the screen), or removed if desired.

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7-7

Regression Report

TriStar II 3020

X- and Y-Axes Variable fields

Allows you to designate the X- and Y-axes variables. Click on the down arrow to display a list of variables. The variables in this list are the ones you specified in the SPC report options dialog. With this option, you can plot the regression of up to three Yaxis variables against the X-axis variable. The X-axis specifies the independent variable for the regression, while the Y-axes provide the dependent variables.

Axis Range

Enables you to specify the beginning and ending values for the X- and Y-axis ranges. Data collected outside these ranges are not included in the plot. These fields are disabled if you choose Autoscale. Allows you to have the X- and/or Y-axes scaled automatically. Select this option to have archived SPC values recalculated. This ensures that any changes made to the SPC Report Options are included in the new report; however, it does lengthen the time required to generate the report. Enables you to generate tabular, as well as graphical, data of the included samples. A tabular report contains the numeric values contributed by each sample. Allows you to label the points on the plot to correspond with the values in the sample files. Displays the Regression Report Sample Selection dialog, allowing you to choose the sample files you wish to have reported.

Autoscale

Recalculate archived SPC results

Tabular report

Label data

Samples

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TriStar II 3020

Regression Report

File name

Use this field to limit the files displayed in the Available Files pane. For example; enter g*.smp to display only the files beginning with a g. This drop-down list determines the type of sample files that display in the Available Files pane in the selected directory for all dates, or within the specified range of dates (using Date Range push button). Refer to Table 2-2. File Status and Description, page 2-12 for an explanation of the Status types. Displays the Select Dates dialog so that you can specify a range of dates. Refer to Selecting Files, page 2-12 for an explanation of this push button. Select this option to include all files from the selected directory in the report. Lists the current directory. Use the directory window to navigate to a different directory. Refer to Selecting Files, page 2-13 for information on selecting different directories.

Status

Date Range

Use all files in this directory Directories

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7-9

Regression Report

TriStar II 3020

Add

Moves the selected file in the Available Files pane to the Selected Files pane. Alternatively, you can simply doubleclick on the desired file(s). You can select multiple files by holding down Ctrl while making your selections. You can include up to 200 sample files. Removes the selected file from the Selected Files pane and places it back into the Available Files pane. Saves the current definition of the report as the default. The options in this group box enable you to choose output criteria. The Copies field is enabled when you choose Printer as the destination, enabling you to print up to four copies of the report.

Remove

Save As Default

Report Settings

Report

Generates the report.

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TriStar II 3020

Control Chart

Control Chart
This option enables you to generate a control chart report which plots the changes in a statistic.

Show report title

Select this option to have a title display on your report. Accept the default or enter a new title. You can enter up to 40 alphanumeric characters. Deselect this option to omit the report title.

Show graphic

Select this option to have a graphic display above your report title. For example, you may wish to display your company logo. The graphic must be a bitmap (bmp) or enhanced metafile (emf). Click Browse to choose the file, then use the Height and Width fields to specify a size. This image can be edited in the report window (when printed to the screen), or removed if desired.

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7-11

Control Chart

TriStar II 3020

X-axis Order By

Enables you to choose the order in which X-axis statistics are placed. You can have them placed by Time, File name, Date, Minutes, or Days. Time places the files on the graph at numerical points in the order of the date/time the files are analyzed. File name places the files on the graph at numerical points in alphanumeric order. Date places the files on the graph at points representing the actual date/time the files are analyzed. Minutes places the files on the graph at points representing the minutes that have elapsed from the first file placed on the list, which is the earliest-analyzed file. Days places the files on the graph at points representing the number of days that have elapsed from the first file placed on the list, which the earliest-analyzed file. Displays the Control Chart Graph [n] Options dialog, allowing you to define the Y-axis of each graph.

Graph [n]

Statistic

This drop-down list displays the SPC variables selected on the SPC Report Options dialog. The variable you choose will be plotted against time.

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TriStar II 3020

Control Chart

Autoscale

Allows you to have the Y-axis scaled automatically. If you wish to specify a range, deselect this option and enter a range in the From and To fields. Displays placement options for the variable’s optional value. Choose Entered to specify placement of the line. Displays the options available for limiting lines. You can have the lines placed at some multiple of the standard deviation or at specified positions (Entered). When you select Entered, the High limit and Low limit fields are enabled, allowing you to enter appropriate values.

Center Line

Limit Lines

Tabular report

Allows you to generate tabular, as well as graphical, data of the included samples. A tabular report contains the numeric values contributed by each sample. Select this option to have archived SPC values recalculated. This ensures that any changes made to the SPC Report Options are included in the new report. It also lengthens the time required to generate the report. Displays the Control Chart Sample Selection dialog, allowing you to choose the sample files on which you wish to report.

Recalculate archived SPC results

Samples

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7-13

Control Chart

TriStar II 3020

Samples

(continued)

This dialog functions in the same manner as the Regression Report Sample Selection Dialog explained earlier in this chapter. Refer to page 7-8 if you need assistance on the fields of this dialog. Saves the current definition of the report as the default. The options in this group box enable you to choose output criteria. The Copies field is enabled when you choose Printer as the destination, enabling you to print up to four copies of the report.

Save as Default

Report Settings

Report

Generates the report.

7-14

Mar 08

TriStar II 3020

Heat of Adsorption Report

Heat of Adsorption Report
The isosteric heat of adsorption is an important parameter for characterizing the surface heterogeneity and for providing information about the adsorbent and the adsorption capacity. Multiple adsorption isotherms are obtained on the same sample using the same adsorptive but at different temperatures to obtain the heat of adsorption. This option allows you to choose the sample files, define the quantities, and generate a Heat of Adsorption report; the Heat of Adsorption dialog is displayed.

Table

Contains the files you choose; also lists the quantity adsorbed. Displays the Select Samples dialog so that you can choose desired files. Removes the selected sample from the list. If no samples are selected, the last one is removed. Removes all samples from the list.

Add Samples

Remove Samples

Clear Samples

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7-15

Heat of Adsorption Report

TriStar II 3020

Edit Quantities

Displays the Edit Quantities Adsorbed dialog so that you can specify the range of surface coverage to include in the heat of adsorption report.

Quantity Adsorbed table
Insert Range

Allows you to enter the points.

Displays the Insert Quantity Range dialog. This dialog allows you to specify the starting and ending quantities adsorbed, as well as the number of points to insert within the specified range.

Insert

Inserts a row above the selected row. Deletes the selected row.

Delete

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Mar 08

TriStar II 3020

Heat of Adsorption Report

Clear

Clears the entire table of all entries except one; one is required. Allows you to import a previously saved table. Allows you to save the current table as a file (QNT extension). The options in this group box allow you to choose report criteria. Choose this option to have a title display in the header of your report; use the adjacent field to enter the title. This option allows you to have a graphic appear in your title; for example, you may wish to show your company logo. You can use a bitmap or an enhanced metafile. Use the Height and Width fields to define a size.

Load Table

Save Table

Report Settings

Show report title

Show graphic

Tabular report Isostere plot

Select this option to have data generated in a tabular format. Select this option to generate a graph showing quantities of gas adsorbed vs. the temperature. Select this option to generate the Heat of Adsorption data in a graphical format. Enabled when you choose Printer as the destination, allowing you to print up to four copies of your report(s). Enables you to choose a destination for your reports. Enabled when you choose File as the destination, allowing you to enter a name (or you can accept the default). Enables you to open a previously saved report.

Heat of adsorption plot Copies

Destination File name

Open

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Heat of Adsorption Report

TriStar II 3020

Save

Saves the current report. Generates the report. Closes the dialog.

Report

Close

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Mar 08

TriStar II 3020

Printed Reports

Printed Reports
Header
All printed reports (either to the screen or to a printer) contain a header displaying file statistics.

If specified, the report header can also contain a graphic (such as a company logo) and a title. • Tabular and graphical reports contain sample and instrument statistics such as date and time of analysis, analysis conditions, and so forth. The headers for these reports also contain notes of any changes to the sample file that occur after analysis. • Summary report headers contain the same type of information displayed in tabular and graphical reports with the exception of notes.

Onscreen Reports
The report window containing onscreen reports provides many options for customizing and manipulating reports: • • • • a tool bar shortcut menus zoom feature axis cross hairs

When reports are printed to the screen, they are printed in a window like the one shown below. Each requested report is listed in the Reports window on the tool bar; they are also indicated by selectable tabs across the top of the report header. To view a specific report, select its tab or select the report in the Reports window and click Show.

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Printed Reports

TriStar II 3020

Tabs display for each type of report you generate.

Header

List of reports requested.

Options or Tool Bar

Displays graphical (or tabular) data.

Tool Bar

Reports
Show

Contains a list of all requested reports. Shows the selected report in the report window. If the report has been hidden, it and its associated tab will become visible.

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TriStar II 3020

Printed Reports

Delete

Deletes the selected report. A deletion confirmation dialog is displayed since this function cannot be undone. The deleted report(s) will have to be regenerated if deleted in error. Hides (removes) the selected report from the report window. The report’s associated tab is also removed. Allows you to open a previously saved report file. Displays a print dialog so that you can choose an appropriate printer for report output. A list of available reports is displayed in the window on the right side of the dialog.

Hide

Open

Print

For convenience in selecting which reports to print, push buttons are provided beneath the report window. Or, you can make your selection by clicking on the desired reports.
Current selects the report displayed in the report window. Shown selects only the shown reports; any nonhighlighted

reports indicate they are hidden. You can still select hidden reports from this window to print.
All selects all reports, including those that may have been

hidden.
Clear clears all selections.

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Printed Reports

TriStar II 3020

Save

Saves all reports of the currently open file in a report format using the same name as the sample file, only with an rep extension. If you wish to specify a name and/or specific reports to save, use the Save As push button. Saves all or specified reports from the currently open file. The push buttons displayed on this dialog perform in the same manner as the print dialog (explained above). Reports can be saved in three different formats: Report system (*.rep): Saved in a format which allows you to reopen the file using the Open push button on the Report window tool bar. Spreadsheet (*.xls): Saved in a format which can be imported into most spreadsheet programs. Ascii Text (*.txt): Saved in ASCII text which can be imported into programs accepting this type of file. Displays the Default Style dialog so that you can specify default parameters for report fonts and curve properties.

Save As

Default Style

Font

Contains a list of report elements for which the font can be edited. Simply highlight the desired element and click Edit; a font dialog is displayed so that you can specify the desired font and attributes. The items in this group box enable you to specify a thickness for report curves and, when using histograms, the type of fill to apply.

Curve

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Mar 08

TriStar II 3020

Printed Reports

Graph border line thickness
Load

Enables you to specify a thickness for the border of the graph.

Loads the last saved defaults. Saves the changes as the defaults. If you do not click Save, the changes will apply to the current report set only. The next reports will revert to the defaults. Closes the dialog and applies the changes. If you clicked Save, the changes become the defaults. If you did not click Save, the changes apply to the current report only. Closes the report window.

Save

Close

Close

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Printed Reports

TriStar II 3020

Shortcut Menus Shortcut menus are accessed when you right-click on the tabular or graphical portion of a report. Tabular Reports

Resize column

Displays a dialog so that you can specify the width of the selected column (in inches). Displays a dialog so that you can edit the name of the selected column. Use to insert line feeds. Allows you to move the location of the selected column to the left or to the right. Enables you to right-align, left-align, or center the data in the selected column. Displays a list of all columns, enabling you to select the one you wish to hide. Displays a list of all hidden columns, enabling you to select the one you wish to have shown again. Displays a Font dialog, allowing you to change font attributes for the tabular data in the current report.

Rename column

Move column

Align column

Hide column

Show column

Column font

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Mar 08

TriStar II 3020

Printed Reports

Header font

Displays a Font dialog, allowing you to change font attributes for column headers in the current report. Allows you to edit the table title and font. Enables you to copy the entire table (column headers and data) and then insert it into another program. Columns are tab-delimited, allowing easy alignment.

Edit title Copy table as text

Graphs

Autoscale

Autoscales all axes of the graph. This function is useful for returning to a full view after having zoomed in. Shows any curve(s) that has been hidden. This option is disabled (greyed) if no curves have been hidden. Hides (removes from view) any unwanted curve(s)

Show curve

Hide curve

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Printed Reports

TriStar II 3020

Edit curve

Displays the Curve Properties dialog, allowing you to edit curve properties.

Title Style

Displays the title of the curve you are editing. Drop-down list containing styles in which collected data can be displayed. Choices: Curve, Histogram, Points, Curve and Points

Curve group box

Contains options for curves and points. You can edit the curve interpolation, the style of curve and/or points, as well as the pen color. The options in this group box are disabled if Histogram is chosen in the Style drop-down list. Allows you to specify the type of fill as well as the color if Histogram is chosen as the style for collected data.

Histogram group box

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Mar 08

TriStar II 3020

Printed Reports

Edit axis

Displays the Axis Properties dialog, allowing you to edit axis properties.

Edit legend

Displays the Legend Properties dialog, allowing you to edit the placement of the legend.

Edit title

Displays the Title Properties dialog, allowing you to edit the current graph’s title and font.

Copy as metafile

Copies the graph and places it on the clipboard, allowing you to paste it into other applications accepting Windows metafiles. Copies the data used to generate the graph as a series of tabdelimited columns of text.

Copy as text

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Printed Reports

TriStar II 3020

Zoom Feature A zoom feature is included with the report system so that you can zoom in to examine fine details. To use this feature, simply hold down the left mouse button and drag the mouse cursor (drawing a box) across the area you wish to view; then release the button. The enlarged area immediately fills the graph area. Right-click in the graph area and choose Autoscale from the shortcut menu to return to the normal view Axis Cross Hair A cross-hair function is available so that you can view axis coordinates. To use this feature, simply left-click in the desired area of the graph.

X-axis position

Point of coordination

Y-axis position

Right-click in the graph area and choose Autoscale or Redraw from the shortcut menu to remove cross-hair lines and return to the normal view. Alternatively, you can click outside of the graph area.

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TriStar II 3020

Report Examples

Report Examples
The remainder of this section contains samples of some of the reports which may be generated by the TriStarII 3020 Analysis Program. Most of the reports can be varied through entries on the report options dialogs.

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Report Examples

TriStar II 3020

Isotherm Plot

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Mar 08

TriStar II 3020

Report Examples

BET Surface Area Report

Mar 08

7-31

Report Examples

TriStar II 3020

BET Surface Area Plot

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Mar 08

TriStar II 3020

Report Examples

t-Plot Report

Mar 08

7-33

Report Examples

TriStar II 3020

BJH Adsorption: Cumulative Pore Area

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Mar 08

TriStar II 3020

Report Examples

BJH Desorption: Pore Volume Plot

Mar 08

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Report Examples

TriStar II 3020

Dollimore-Heal Desorption: Pore Volume/Area

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Mar 08

TriStar II 3020

Report Examples

Summary Report

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Report Examples

TriStar II 3020

Sample Log Report

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Mar 08

TriStar II 3020

Description

8. OPTIONS MENU
The commands on the Options menu allow you to configure the system to your laboratory’s requirements and specify defaults for sample and parameter files.

Description

Listed below are brief descriptions of the commands on the Options menu. Detailed descriptions follow this section. Option presentation Allows you to display the sample file dialog in either Basic, Advanced, or Restricted format. Page 8-2. Allows you to specify defaults for the parameters contained in the sample information and parameter files. Page 8-6. Allows you to choose the types of units to use for measurement, pressure, and temperature. Page 8-12. Enables you to choose the types of grid lines to display for the X- and Y-axes. Page 8-13. Enables you to choose the variable for the X-axis during data collection. Page 8-14. Allows you to specify a location for the predefined parameter files used by the Basic and Restricted formats. Page 8-15. Enables you to perform certain troubleshooting procedures under the direction of a Micromeritics service representative. Page 8-15.

Sample defaults

Units

Graph Grid Lines

Live Graph

Parameter files directory

Service Test Mode

Mar 09

8-1

Option Presentation

TriStar II 3020

Option Presentation
The sample editing dialogs for the TriStar 3020 analysis program may be presented in three different formats: Advanced, Basic, or Restricted.

Each format displays sample information and menu options differently. • Advanced: displays all parts of the sample information file in a tabbed dialog as in an index card file. Clicking on each tab opens an associated dialog. Use this format to edit parameter files or create customized sample files. • Basic: displays the sample file and parameter files in a single dialog. Use this format to create sample files using previously created parameter files. • Restricted: displays in the same manner as the Basic format. This format also is used to create sample files using previously created parameter files. However, you cannot switch to the Advanced format to edit parameters. You must also use a password for entering and exiting this format.

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TriStar II 3020

Option Presentation

Advanced
The Advanced format presents all parts of the sample information file in a tabbed dialog. For example, if you wish to open or create a sample file using the Advanced format, the following dialog is displayed.

If you are opening completed file, thisdialog also contains a tab for Collected Data.

The Advanced format is used to create customized sample files — easily and quickly. Simply click on the tabs to display its associated dialog. You can also switch to the Basic format, if desired, by clicking Basic. Refer to Advanced, page 5-5 for a detailed description of this dialog.

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8-3

Option Presentation

TriStar II 3020

Basic
The Basic format presents the sample information file and its parameter files in a single dialog. For example, if you wish to open or create a sample information file using the Basic format, the dialog is displayed in this manner.

The Basic format is used to create sample information files using previously defined parameter files. You can easily switch to Advanced format, if desired, by clicking Advanced. Refer to Basic, page 5-8 for a detailed description of this dialog.

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Mar 09

TriStar II 3020

Option Presentation

Restricted
The Restricted format is identical to the Basic format, except that certain menu options are disabled, and you cannot switch to the Advanced format. This format is password-protected and is typically used in laboratories where analysis conditions must remain constant, for example, in the pharmaceutical industry.

Does not contain the Advanced push button allowing access to parameter files.

When you select Restricted, a dialog requesting a password is displayed:

Any password (up to 31 characters) can be used to enable the Restricted format. The same password, however, must be used to exit the Restricted format. For example, if you enter “password” to enable the Restricted format, then you must use “password” to exit. If you forget the password, open the system INI file and navigate to the Private section. The current password will be shown immediately following “OptionPresentationPassword.” Make a note of the password, exit the INI file, and enter the password where requested. Do not attempt to delete the password in the INI file.

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8-5

Sample Defaults

TriStar II 3020

Sample Defaults
This option allows you to specify default parameters for sample information files and parameter files. You can specify default values using the Advanced or Basic format.

Advanced
When you select Sample Defaults while in the Advanced format, the Sample Defaults dialog is displayed. The values you specify for parameters of the Advanced sample information file serve as the parameter file defaults. For example, the values specified for the Analysis Conditions portion of the Advanced sample file display as the defaults for a newly created Analysis Conditions file..

Sequence

Specify a default sequence for the sample file name. The number you specify is sequenced incrementally each time you create a sample file. It is the number that appears in the File name field when you select File > Open > Sample information. • Use numbers, letters, or other printable characters, such as dashes. Do not use special characters such as * or ?. At least three numbers must be included. Use up to eight characters.

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Mar 09

TriStar II 3020

Sample Defaults

Sample

Allows you to enter an additional identification that provides more information than the sample file name alone. In the field on the left, edit the prompt for Sample if you wish. For example, you may prefer to use Test or Material. The maximum number of characters is 20. In the field on the right, specify a format for the sample identification. • Use numbers, letters, or other printable characters, such as dashes. Maximum number of characters is 42, plus the $ symbol. Include the automatically generated file name as part of the identification by using the $ symbol where you want the sequence number to appear. For example, if the sequence number is 000-001, enter the sample identification as follows: Lab #25 - $ The resulting sample identification for the first sample information file would be: Lab #25 - 000-001 and the second: Lab #25 - 000-002, and so on.

• •

Operator Submitter

Allow you to enter the name (or other identification) of the operator performing the analysis and the name of the person, department, customer, etc. that submitted the sample for analysis. The fields on the left can be edited to display something other than Operator and Submitter if you like. The fields on the right allow you to specify default names or titles. • Include the automatically generated file name as part of the identification by using the symbol $ where you want the sequence number to appear. Refer to the example in the previous section.

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8-7

Sample Defaults

TriStar II 3020

Operator Submitter (continued)

• •

Maximum number of characters for the prompt is 20. Maximum number of characters for the identification is 42, including the $ symbol. Omit this item entirely from the sample information file by selecting Omit.

Mass

You can choose to enter a sample mass or have the mass automatically calculated. Regardless of which option you choose for your default, you can change it in the sample file. Enables the Sample Mass field allowing you to enter a default value. Enables the Empty tube and Sample + tube fields, allowing you to enter default values. These values are used to calculate the mass of the sample,
Mass sample = Mass sample + tube – Mass tube

Enter

Calculate

Density

Enter a default density. If there is a material you analyze quite often, you may wish to use its default in this field. This value can be edited in the sample information file. Choose the manner in which you typically display data. The fields in this group box are used primarily for SPC (Statistical Process Control) reporting. They are used to specify characteristics of the sample or its manufacturing process. Once specified, these parameters display on the sample editor and in the SPC Sample Options dialog (accessed through the SPC Report Options dialog). These fields can also be used to record analysis conditions or sample information so that it can be printed on the Summary report. Select Omit if you do not wish to use these fields; this will prevent them from displaying on the sample information dialog.

Type of Data User Parameters

8-8

Mar 09

TriStar II 3020

Sample Defaults

Comments

Allows you to enter comments about the sample or its analysis conditions. Anything you enter in this window is printed in the report header. Allows you to enter comments about the sample or its analysis conditions. Anything you enter using this option appears in the Instrument Log Report; it does not display in the report header. Allows you to replace the contents of all parameter files contained in the current default sample file with those from an existing sample file. For example, you may have an existing sample file that contains most (or all) of the parameters that you wish to use. You can select this push button, choose the file, and then OK. All parameter files of the file you choose are copied into the sample defaults dialog. You can even change the values in these files (if needed) without affecting the file from which they were copied.

Add Log Entry

Replace All

Click on each remaining tab of the Advanced Sample dialog to complete sample defaults and establish parameter defaults. Refer to the following sections if you need assistance on the fields of these dialogs. • • • • • Sample Tube, page 5-11 Degas Conditions, page 5-13 Analysis Conditions, page 5-15 Adsorptive Properties, page 5-28 Report Options, page 5-31

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8-9

Sample Defaults

TriStar II 3020

Basic
When you select Sample Defaults while using the Basic format, the Sample Defaults dialog is displayed. The values you specify for the Basic format also apply to the Restricted format..

Sequence

Specify a default sequence for the sample file name. The number you specify is sequenced incrementally each time you create a sample file. It is the number that appears in the File name field when you select File > Open > Sample information. • Use numbers, letters, or other printable characters, such as dashes. Do not use special characters such as * or ?. At least three numbers must be included. Use up to eight characters.

• Sample

Allows you to enter an additional identification that provides more information than the sample file name alone. • In the field on the left, edit the prompt for Sample if you wish. For example, you may prefer to use Test or Material. The maximum number of characters is 20. In the field on the right, specify a format for the sample identification. Use numbers, letters, or other printable characters, such as dashes.

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Mar 09

TriStar II 3020

Sample Defaults

Sample (continued)

• •

Maximum number of characters is 42, plus the $ symbol. Include the automatically generated file name as part of the identification by using the $ symbol where you want the sequence number to appear. For example, if the sequence number is 000-001, enter the sample identification as follows: Lab #25 - $ The resulting sample identification for the first sample information file would be: Lab #25 - 000-001 and the second: Lab #25 - 000-002, and so on.

Mass

You can choose to enter a sample mass or have the mass automatically calculated. Regardless of which option you choose for your default, you can change it in the sample file. Enables the Sample Mass field allowing you to enter a default value. Enables the Empty tube and Sample + tube fields, allowing you to enter default values. These values are used to calculate the mass of the sample,
Mass sample = Mass sample + tube – Mass tube

Enter

Calculate

Density Sample tube Degas conditions Analysis conditions Adsorptive properties Report options

Enter the density of the material you are analyzing. Each parameter contains a drop-down list containing predefined parameter files, some of which were included with the software. Choose the file you wish to use as the default.

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8-11

Units

TriStar II 3020

Replace all

Allows you to replace all parameters of the default sample file you are creating with parameters from an existing sample file. For example, you may have an existing sample file that contains most (or all) of hte parameters that you wish to use. You can click this push button, choose the file, and then OK. All parameters ofthe file you choose are copied into thesample defaults dialog. You can edit the values if desired without changing the file from which they were copied. Saves the specified defaults. Closes the dialog.

Save

Close

Units
This menu command displays the Units Selections dialog which allows you to choose the manner in which to display data on reports.

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Mar 09

TriStar II 3020

Graph Grid Lines

Graph Grid Lines
Graph Grid Lines enables you to choose the type(s) of grid lines to show on your reports; the Graph Grid Lines dialog is displayed.

X-Axis Y-Axis

Enables you to choose Major and/or Minor lines to display in printed reports for the Logarithmic and Linear scales. If you deselect these items (remove the check marks), your report will not display grid lines.

Grid Line Style

Allows you to choose the type of grid line to display if grid lines are being shown.

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8-13

Live Graph

TriStar II 3020

Live Graph

This option enables you to choose the variable for the x-axis during data collection. You can also choose to correct for thermal transpiration which should always be selected for micropore analyses (refer to page 5-33 for additional information on thermal transpiration).

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Mar 09

TriStar II 3020

Parameter Files Directory

Parameter Files Directory
This option allows you to select the location for the predefined parameter files displayed in the drop-down lists on the Basic and Restricted Sample Information dialogs. The current directory specified for parameter files is displayed above the directory window. When you select this option, the Parameter File Directory Selection dialog is displayed.

The directory specified here is the one you should use when creating parameter files to be included in the drop-down lists on the Basic and Restricted sample information dialogs. It is where the software goes to obtain the files for the drop-down lists. The default directory is param and includes several parameter files supplied with the analysis program. If you specify a different directory, these files will not be included in the drop-down lists unless you copy (or move) them to the new directory. If you wish to continue to use the param directory for parameter files, it will display as the default when saving parameter files.

Service Test Mode
Certain service tests are included in the TriStar operating program. These tests, however, can be performed only with the assistance of a trained Micromeritics service representative. When you select Options > Service Test Mode, a dialog prompting you to enter a password is displayed. This password is supplied by your service representative. You will be unable to perform these tests without his guidance. After Service Test Mode has been enabled, the tests are accessible from the Unit menu.

Mar 09

8-15

TriStar II 3020

Troubleshooting

9. TROUBLESHOOTING AND MAINTENANCE
The TriStar system has been designed to provide efficient and continuous service. However, certain maintenance procedures should be followed to obtain the best results over the longest period of time. This chapter includes maintenance procedures and calibration procedures.

Troubleshooting
Most operational problems are caused by: • • • • • Leaks (commonly around the sample tube O-ring at the analysis port) Sample weighing errors Use of too much analysis bath fluid in the Dewar at the start of an analysis Entry of incorrect system volume for analysis Impure gas supply

Always check these first when expected analysis results are not obtained. Some common operational problems, which are not indicated on the video monitor screen, and their respective causes and solutions are provided in the following table.

What Happened

Why

What To Do

Analysis Dewar cannot Elevator that moves Dewar is be raised (or lowered). stuck. Vacuum pump is noisy. Sample tube connector is loose. Sample tube O-ring is worn or cracked. Sample tube is cracked. No sample tube loaded on a selected port. Gas inlet valve open while vacuum valve open.

Check for possible obstruction to elevator movement. Tighten fitting. Replace O-ring. Replace O-ring. Refer to Replacing the Sample Tube Oring, page 9-7 Replace with new sample tube. Install plug or empty sample tube. With manual control enabled, use the instrument schematic to close gas inlet valve. Make sure the cable is connected properly.

Analysis valves cannot Cable from computer to the be operated. instrument is loose.

Mar 08

9-1

Troubleshooting

TriStar II 3020

What Happened

Why

What To Do

Sample is not within specifications.

There may be a leak into or out of Refer to Performing a Leak the manifold. Test, page 9-16. Gas may be contaminated. Perform a blank analysis. If results are okay, perform a reference material analysis. Be sure your gas line is all metal; it is best to use the one shipped with the instrument. Do not use polymer gas lines or flexible gas lines that may be internally coated with a polymer. Contact your Micromeritics Service Representative.

Incorrect type of gas line.

Elevator is noisy.

The elevator screw may need greasing.

9-2

Mar 08

TriStar II 3020

Preventive Maintenance

Preventive Maintenance
The table below lists the preventive maintenance procedures you should complete to keep your analyzer operating at peak performance. Instructions for each procedure follow the table. Micromeritics also recommends that you have preventive maintenance procedures and calibration performed by one of our service representatives every 12 months.

Maintenance Required Check and clean Dewar, page 9-4 Replace port filters and O-rings, page 9-6 Replace sample tube O-ring, page 9-7 Inspect and change vacuum pump fluid*, page 9-8 Replace alumina in oil vapor traps*, page 9-11 Clean the outside of the analyzer, page 9-4 Test analyzer for leaks, page 9-16 Replace vacuum pump exhaust filter, page 9-15 Replace diaphragm in vacuum pump (if an oil-free pump is used)** *Oil-sealed vacuum pumps only. Weekly

Frequency

Every 3 to 6 months As required or every 3 to 6 months As required or every 3 to 6 months As required As required or every 6 months As required or every 12 months As required or every 12 months Every 12 months

**For oil-free pumps only: After 12 to 18 months of operation, the diaphragm in the pump will wear out and the pump becomes completely inoperable. To prevent any instrument downtime due to an inoperable pump, it is recommend that you have the diaphragm replaced by a Micromeritics Service Representative every 12 months.

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9-3

Preventive Maintenance

TriStar II 3020

Lubricating Elevator Drive Assembly
The elevator screw should not require lubricating; it is lubricated before it leaves the factory. If your elevator starts to vibrate or become noisy when traveling, contact your Micromeritics Service representative for disposition.

Cleaning the Analyzer
The exterior casing of the analyzer may be cleaned using a clean cloth, dampened with isopropyl alcohol (IPA), a mild detergent, or a 3% hydrogen peroxide solution. Do not use any type

of abrasive cleaner.
Do not allow liquid to penetrate the casing of the analyzer. Doing so could result in damage to the unit.

Cleaning the Analysis Dewar
When handling Dewars, be sure to observe the Dewar precautions outlined in Installing the Analysis Dewar, page 3-25.

Ice and suspended frost particles may accumulate in the bottom of an analysis port Dewar. Particles or deposits exceeding 1/4 in. (0.64 cm) in depth may jam between the bottom of the sample tubes and the bottom of the Dewar, causing the Dewar not to raise fully. Accumulations of fine particles impede liquid nitrogen circulation around the bottom of the sample tubes. This causes the sample temperature to be slightly higher which, in turn, can cause pore volume measurement errors in those samples exhibiting high isotherm slope above 0.97 relative pressure. Accumulated ice is likely to melt and form a pool of water in the Dewar if all liquid nitrogen evaporates. The water must be removed; otherwise it will solidify when liquid nitrogen is added and could press on the bottom of the sample tube causing breakage. To ensure problems do not develop due to ice accumulation, check the Dewar after each use. Clean the Dewar on a weekly basis. 1. Remove the sample tubes from the analysis ports. 2. Select Unit [n] > Show Instrument Schematic to display the instrument schematic, then Unit [n] > Enable Manual Control.

9-4

Mar 08

TriStar II 3020

Preventive Maintenance

3. Right-click on the elevator icon and select Lower to lower the elevator to its lowest position.

4. Remove the Dewar and pour the liquid nitrogen from the Dewar into an appropriate cryogenic container.
Do not pour liquid nitrogen directly into a sink. Doing so may cuase drain pipes to burst.

5. Rinse the Dewar with warm water to melt any ice accumulation which may remain in the Dewar, then dry thoroughly.

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9-5

Preventive Maintenance

TriStar II 3020

Replacing Port Filter and O-ring
A 20-µm filter (frit) is located in each analysis port. If the filter is contaminated, the contaminant may adsorb or desorb during analysis, affecting the results. A contaminated filter on the analysis port may be indicated by a leak or by a free-space reading much lower than normal. A contaminated filter should be replaced as follows: 1. Select Unit [n] > Show Instrument Schematic, then Unit [n] > Enable Manual Control. 2. Right-click on the valve for the desired port and choose Close to close the valve. 3. Using a wrench, remove the sample tube fitting from the port. Pry out the filter and O-ring.
20-µm filter (frit) O-ring

Sample Tube fitting

To avoid degassing problems, the filter and O-ring should be clean and should not be touched with bare hands.

4. Replace the filter and O-ring. Carefully reassemble the sample tube fitting and reinstall on the sample port. Tighten by hand, then with a wrench to prevent leaks.

9-6

Mar 08

TriStar II 3020

Preventive Maintenance

Replacing the Sample Tube O-ring
It is important to maintain a vacuum-tight seal near the top of the sample tube stem. If an Oring becomes worn or cracked, it does not provide a good seal and will need to be replaced.
Before removing (or installing) a sample tube, ensure that the port valve is closed. Observe the instrument schematic to verify valve status.

1. Holding the sample tube firmly with one hand, loosen the sample tube connector nut by turning counterclockwise.
Be careful not to let the sample tube connector nut drop onto the bottom of the tube as it may break the tube.

2. Carefully pull the sample tube down until it is free from the port. You may have to grasp the sample tube with both hands.

O-ring

Ferrrule

3. Remove the O-ring from the top of the sample tube and replace it with a new one.
If the O-ring remains inside the sample port, you may use a pair of tweezers or needlenose pliers to remove it.

4. After the new O-ring is in place, insert the sample tube back into the sample port until it is fully seated. 5. Slide the sample tube connector nut up the tube (the ferrule and O-ring will move along with the connector nut). Then, turning clockwise, hand-tighten the connector nut to the sample connector.

Mar 08

9-7

Preventive Maintenance

TriStar II 3020

Inspecting and Changing Vacuum Pump Oil
This procedure is also shown in one of the How-To videos located on the Help menu.

The oil in the vacuum pump should be changed every three months, when the efficiency of the vacuum pump declines (requiring increased time to reach vacuum levels), or if it becomes discolored. The oil is easily inspected to determine if a change is necessary. Inspecting the Oil View the vacuum pump oil through the oil-level window. The oil level should be midway between the indicators on the oil-level window. Oil in good condition is clean, clear or light in color, and transparent.

Oil-level window

• Change the oil if it has darkened • Add oil if it is below the midway level Changing or Adding Oil
Always drain the vacuum pump while the pump is warm and disconnected from the power source.

Use oil supplied by Micromeritics, or refer to the vacuum pump manual for other acceptable oils. 1. Unplug the vacuum pump from the power source.

9-8

Mar 08

TriStar II 3020

Preventive Maintenance

2. Loosen the wing nut on the clamp at the top of the oil vapor trap. Swing the clamp open and remove the trap from the hose.

3. Grasp the handle on top of the vacuum pump and place it on a work table.

4. Drain the used oil:
If you are adding oil, skip this step and continue with Step 5.

a. Place a waste container under the drain spout. b. Remove the plug from the drain spout; allow the oil to drain into the waste container.

d. Replace the drain plug.

Mar 08

9-9

Preventive Maintenance

TriStar II 3020

5. Remove the plug from the oil-fill port.

Oil-fill port

6. Slowly add oil to the port until the level is midway between the indicator lines in the oillevel window.

Midway level

Do not allow oil to rise above the midway position. Doing so may cause oil to splash into the oil filter and contaminate it.

7. Check the washer or O-ring used at the oil-filling port; replace if necessary. 8. Insert the oil-fill plug and turn counterclockwise to tighten. 9. Check the alumina in the oil vapor trap. If most of the pellets are no longer white, replace the alumina in the oil vapor trap before reattaching the vacuum pump. Refer to Replacing the Alumina in the Oil Vapor Trap, page 9-11 for instructions. 10. Reconnect the vacuum pump hose. 11. Reconnect the power cord to the power source. 12. Allow the pump to run a few hours (overnight if possible) to eliminate air and moisture from the fresh fluid and to produce efficient vacuum operations.

9-10

Mar 08

TriStar II 3020

Preventive Maintenance

Replacing the Alumina in the Oil Vapor Trap
The activated alumina in the oil vapor trap becomes saturated during use. The alumina should be inspected periodically and replaced when most of the alumina pellets are no longer white.
Do not perform the following procedure on used alumina. The resultant oil vapors may cause a fire or an explosion.

1. Loosen the wing nut on the clamp at the bottom of the oil vapor trap. Swing the clamp open and remove the trap.

2. Remove one end fitting from the trap body; dispose of the used alumina in an appropriate manner. 3. Wash the trap body with a detergent-based soap. Rinse with water, then with isopropyl or ethyl alcohol. Set the trap aside and allow to dry thoroughly.
Exposure of the trap body to oil vapor may cause small cracks on the inside surface of the trap body. Under normal circumstances, these cracks will not cause problems or leaks.

Mar 08

9-11

Preventive Maintenance

TriStar II 3020

4. Prepare fresh alumina as follows: a. Preheat the oven to 300 °C. b. Pour approximately 180 grams of fresh alumina into a glass or metal container for (approximately 250 mL if a graduated beaker is used). Place the container in the oven. c. Bake the alumina for two hours. d. Remove the baked alumina from the oven and allow it to cool until luke warm. A desiccator may be used to speed the cooling process. 5. Using a small spatula, gently pry the O-ring from the end fittings of each end of the trap body.

6. Inspect the O-rings. • If dusty, clean with a lint-free tissue. • If damaged, replace with a new O-ring. 7. Screw one of the end fittings onto the trap body.

9-12

Mar 08

TriStar II 3020

Preventive Maintenance

8. Be sure the trap body is dry and the alumina is lukewarm; pour the alumina pellets into the trap until they are level with the top of the trap body.

9. Screw the other end fitting back onto the trap and tighten securely by hand. 10. Lightly tap both ends of the trap body on the work surface. This will remove any remaining dust from the pellets.

11. Make sure the centering ring is in place on the intake port. 12. Place the trap on the centering ring.

Centering Ring

Mar 08

9-13

Preventive Maintenance

TriStar II 3020

13. Open the clamp and place it around the flange of the intake port and the flange of the trap. Swing the clamp fastening screw toward the intake port until it fits into the slot in the other half of the clamp. Tighten the wing nut securely by hand.

14. Reconnect the hose from the analyzer to the oil vapor trap. a. Place the clamp around the flange of the vacuum pump hose and vapor trap.

b. Swing the cslamp fastening screw around until it fits into the slot on the other half of the clamp. Tighten the wing nut securely by hand.

15. Plug the pump power cord into the power source. 16. Allow the pump to run a few hours (overnight if possible) to eliminate air and moisture from the fresh oil and to produce efficient vacuum operations.

9-14

Mar 08

TriStar II 3020

Preventive Maintenance

Changing the Vacuum Pump Exhaust Filter
The gases used by the TriStar 3020 are exhausted by the vacuum pump. An exhaust filter is installed on the exhaust port of oil-filled pumps. The filter minimizes the release of oil vapor and should be replaced when it becomes so saturated with oil that it is ineffective.
Exhaust filters are used to minimize the release of oil vapors. The gases are diluted substantially upon release from the vacuum pump. However, it may be desirable in some locations to provide a fume hood for protection from hazardous gases and vapors released into the work area.

1. Loosen the wing nut of the clamp at the vacuum pump exhaust port. Swing the clamp away from the exhaust port and remove it.

2. Remove and discard the exhaust filter; do not remove the centering ring. 3. Make sure the centering ring is in place on the exhaust port. 4. Place the new filter on the centering ring. 5. Open the clamp and place it around the flange of the exhaust port and the flange of the exhaust filter. Swing the clamp fastening screw toward the exhaust port until it fits into the slot in the other half of the clamp. Tighten the wing nut securely by hand.

Mar 08

9-15

Preventive Maintenance

TriStar II 3020

Performing a Leak Test
Your service representative may request that you perform a leak test to determine if there is a leak in your system. This test generates a report that your service representative will request that you send to him for observation. The following types of information are displayed during the test: • Prompts on preparing the instrument for the test • Approximate time period of the test • Prompts in which an operator response is required 1. Select Unit [n} > Diagnostics; the Service Test dialog is displayed.

2. Click the down arrow to the right of the Test field and select System Leak Test Rev. [latest revision letter]. 3. Ensure that Report after test is selected and that Screen is chosen as the destination.

9-16

Mar 08

TriStar II 3020

Preventive Maintenance

4. Click Next; the second view of the Service Test dialog is displayed.

Data will be inserted into the pane as collected. 5. After the test is finished, a dialog stating the test is complete is displayed. 6. Click OK to close the dialog, then click Close on the test dialog to close the test. 7. When you close the test, a report is generated automatically to the screen.

Mar 08

9-17

Preventive Maintenance

TriStar II 3020

8. Click Save as; the Save As dialog is displayed.

9. Accept the default name displayed in the File name field, then click Save to return to the report window. 10. Click Close to close the report window. 11. E-mail the report file to your service representative.

9-18

Mar 08

TriStar II 3020

Connecting Gases

Connecting Gases
This procedure is also shown in one of the How-To videos located on the Help menu.

Guidelines for Connecting Gases to the Analyzer
Use these guidelines when installing regulators and gas lines: • Place gas bottles close to the analyzer. Using gas line extenders on gas bottles located in remote areas may degrade gas quality and reduce pressure. • Use a retaining strap (or other appropriate tether) to secure the gas bottle. • Carefully route the gas lines from the bottle to the analyzer, avoiding overlapping or entangling gas lines. • Label the gas line at the instrument inlet for proper identification and maintenance. • Ensure that the gas bottle is closed before connecting to the analyzer. The instructions below describe a typical installation. Some configurations require additional components, such as regulator expansion kits, when one gas source will be used for several operations or when the gas bottle cannot be located close to the analyzer.
In order to use oxygen with the TriStar, your analyzer must be equipped with an oxygen-compatible vacuum pump that uses Fomblin® (or a suitable equivalent) pump oil, or a dry pump. Failure to use the proper vacuum system could result in hazardous conditions including fire and personal injury.

Disconnecting the Depleted Bottle
1. Close the gas bottle shut-off valve, then open the regulator shut-off valve.

Gas Bottle shut-off valve

Regulator shut-off valve

Mar 08

9-19

Connecting Gases

TriStar II 3020

2. Both gauges should read at or near zero; if not, disconnect the gas line from the regulator and allow the pressure to purge from the lines. 3. Use an appropriate wrench to loosen the nut at the regulator/gas bottle connection, then remove the regulator from the bottle.

You do not have to disconnect the gas line from the regulator or the instrument. 4. Replace the protective cap on the depleted bottle, disconnect the retaining strap, and remove the bottle from its current location.

9-20

Mar 08

TriStar II 3020

Connecting Gases

Connecting a Replacement Gas Bottle
Move the replacement bottle close to the instrument and tether it into place.
When connecting hazardous gases, be sure to vent properly and follow the safety procedures established for your lab.

A power failure or loss of cryogen can result in dangerous pressures in the sample tube. The TriStar uses pressure relief valves to vent this pressure into the instrument cabinet and return the instrument to a safe condition. When using toxic or flammable gases, additional venting of the cabinet may be required.

1. Use an appropriate cylinder wrench to remove the protective cap from the replacement bottle.

2. Attach the gas regulator to the connector on the gas bottle. Hand-tighten the nut, then use an appropriate wrench to tighten an additional 3/4 turn.
Do not overighten the fitting; doing so may cause a leak.

3. Check for leaks at the high-pressure side of the regulator and in the connector.
HIgh-pressure Gauge

Gas Bottle Shut-Off valve

Regulator Control knob

Regulator connector nut

Mar 08

9-21

Connecting Gases

TriStar II 3020

a. Turn the regulator control knob fully counterclockwise. b. Slowly open the gas bottle shut-off valve, then close it. c. Observe the pressure on the high-pressure gauge. • If the pressure is stable, proceed with the next step. • If the pressure decreases, tighten the regulator connector nut until it becomes stable. 4. Purge the air from the lines.

Gas Bottle Shut-Off valve

Regulator Shut-Off valve

a. Turn the regulator shut-off valve counterclockwise to open. b. Open the gas bottle shut-off valve to flow gas. c. Close the regulator shut-off valve to stop flow. d. Close the gas bottle valve. 5. Set the instrument pressure.
Low-pressure Gauge

Regulator Shut-Off valve

Gas Bottle Shut-Off valve

Regulator Control knob

a. Turn the regulator control knob clockwise until the low-pressure gauge reads 15 psig (103 kPag). b. Open the regulator shut-off valve.

9-22

Mar 08

TriStar II 3020

Connecting Gases

c. Open the gas bottle shut-off valve and flow gas for 10 to 30 seconds. d. Close the gas bottle shut-off valve. 6. If you disconnected the gas line to the instrument inlet, reconnect it now. 7. Verify that the line for the newly connected gas is clean; refer to Cleaning and Verifying the Gas Line, page 9-24. 8. If you connected the same gas as the one you removed, you are ready to resume operation. If you connected a different gas than the one you removed, you must specify the change; refer to Specifying Gas Ports, page 9-28.

Mar 08

9-23

Connecting Gases

TriStar II 3020

Cleaning and Verifying the Gas Line
You should always clean the gas lines and verify there are no leaks at the connections after you connect a gas bottle. This test examines the gas line from the instrument to the gas bottle, then from the instrument to the regulator shut-off valve. A report is generated at the completion of the test verifying that it has passed or failed. Causes and corrective action for a failure are provided. Before beginning, confirm that the state for valves and the low-pressure gauge are as follows:

Low-pressure gauge

14 - 15 psig
Gas Bottle Shut-Off valve

CLOSED

Regulator Control knob Regulator Shut-Off valve

OPEN

OPEN

1. Select Unit [n} > Diagnostics; the Service Test dialog is displayed. 2. Click the down arrow to the right of the Test field and select Clean and Verify Gas Line [port number] Test Rev. [latest revision letter]. 3. Ensure that Report after test is selected and that Screen is chosen as the destination.

Be sure Report after test is selected and Screen is the destination.

9-24

Mar 08

TriStar II 3020

Connecting Gases

4. Click Next; the second view of the Service Test dialog is displayed. On this dialog a series of messages is displayed. These messages are of the following types: • Informative; for example, advising how long the test will take or how long before you will be required to open or close a valve. Read the message and click OK to proceed. • Operator response; for example, you will be asked to open and close regulator and gas bottle valves (depicted below). Perform the task first, then click OK.
Low-pressure gauge Gas Bottle Shut-Off valve

Regulator Control knob Regulator Shut-Off valve

5. After the test is finished, a dialog stating the test is complete is displayed; click OK to close the dialog. 6. A report is generated automatically to the screen.

Observe the Slope field on the Instrument to Regulator Shut-off Valve -1 report; it should display Passed, indicating that the gas line from the instrument to the regulator is clean and leak-free. If Failed is shown, a leak is indicated between this connection. Check the connections from the instrument to the gas regulator valve. Tighten as necessary, then try the test again.

Mar 08

9-25

Connecting Gases

TriStar II 3020

7. Click the Instrument to Gas Bottle Shut-off Valve - 2 tab to display its report.

Observe the Slope field; it should display Passed, indicating that the gas line from the instrument to the gas bottle is clean and leak-free. If Failed is shown, a leak is indicated between this connection. Check the connections from the regulator shut-off valve to the gas bottle shut-off valve. Tighten as necessary, then try the test again. 8. Click the Gas Pressure Test - 3 tab to display its report.

9-26

Mar 08

TriStar II 3020

Connecting Gases

Passed should display in the Minimum field, indicating that all valves are in the proper state for operation. If Failed is shown, one or more valves is not in the proper position; set the valves as shown below and ensure the appropriate pressure is displayed on the low-pressure gauge.

Low-pressure gauge

14 - 15 psig
Gas Bottle Shut-Off valve

OPEN

Regulator Control knob Regulator Shut-Off valve

OPEN

OPEN

If you wish to run the test again, be sure to close the gas bottle valve before starting the test. 9. Click Close to close the test report. 10. Click Close on the test dialog to close the test.

Mar 08

9-27

Specifying Gas Ports

TriStar II 3020

Specifying Gas Ports
The TriStar 3020 has gas inlets for up to three analysis gases and a dedicated inlet for helium. The gases you connect to the inlets must be specified in the analysis program. If you change gases on one of the inlets, be sure to access the Unit Configuration dialog and make the change there as well. It is very important that the analysis program be kept informed of any change in gases. 1. Select Unit [n] > Unit Configuration; the Unit Configuration dialog is displayed.

2. In the Gas Selections group box, enter the mnemonic for the gas(es) you have attached to the gas inlets. 3. Click OK to save the selections and close the Unit Configuration dialog.

9-28

Mar 08

TriStar II 3020

Calibrating the System

Calibrating the System
A calibration file was created specifically for your analyzer and included with your accessories. Reinstalling Calibration Files, page 4-19 describes how to install this file. It is not necessary to recalibrate your system unless you suspect that it may be out of calibration. Certain calibrations are not allowed unless performed under the direction of a Micromeritics service representative; those calibrations are greyed on the Calibration menu. You can review calibration details of your analyzer by selecting Unit > Unit configuration. The following calibrations can be performed without the assistance of a service representative: • Zero pressure • Match transducers • Servo valve

Zero Pressure
This command enables you to evacuate the system and zero the transducers. 1. Install a blank sample tube on each applicable port. 2. Select Unit [n] > Calibration > Zero pressure; the Calibrate Pressure Offset dialog is displayed.

3. Ensure that all transducers are selected, then click Start. The dialog closes automatically when calibration is complete.

Mar 08

9-29

Calibrating the System

TriStar II 3020

Match Transducers
This command enables you to zero and match the selected transducers to the main manifold transducer.

Be sure that a sample or Po tube is installed on each selected port before clicking Start.

Servo valve
Make sure the pressure transducer has been calibrated before performing this procedure. Select Unit > Unit configuration and view the calibration information. Contact your service representative if calibration dates are not listed.

1. Select Unit [n] > Calibration > Servo valve; the Calibrate Servo Valve dialog is displayed.

2. Click Start; the dialog closes when calibration is complete.

9-30

Mar 08

TriStar II 3020

Ordering Information

10. ORDERING INFORMATION
The TriStar 3020 Analysis System components and accessories can be ordered using one of the following methods: • Call our Customer Service Department at (770) 662-3636 • Access our web site at www.micromeritics.com • Contact your local sales representative When ordering, please use the information provided below to place your order.
Part Number Item and Description

065-00000-00 060-00030-00 061-00030-00

SmartPrep 065, Windows interface allowing programmable ramp and soak rates; degasses up to six samples with flowing gas FlowPrep 060, degasses up to six samples at up to 400 ºC with flowing gas VacPrep 061, degasses up to six samples at up to 400 ºC; uses flowing gas or evacuation by vacuum (evacuation requires a vacuum pump and a regulator) Krypton Option; adds 10-mmHg transducer and high-vacuum pump, enabling you to perform krypton analyses (service-installed). Vacuum pump with built-in anti-suckback valve, 100/120 VAC, includes hose kit Vacuum pump with built-in anti-suckback valve, 220/240 VAC, includes hose kit Oil Vapor Trap; includes alumina and instructions Activated alumina, 500 grams; for oil vapor trap Valve, solenoid, 24 VDC 10-32 Mt, 0.025-in. orifice, for standard evacuation (Valves 1 through 10) Valve, solenoid, 24 VDC 10-32 Mt, 0.060-in. orifice, for fast evacuation (Valves 11, 12, and 13) CGA 580 fitting, 30 psig (He, N2) CGA 320, 30 psig (CO2) Expansion Kit; adds an additional outlet to the gas regulator Pressure Relief Kit; prevents excessive gas pressure in the event of regulator failure (not to be used with toxic gases) Reference Material, Carbon black, ~ 30.6 m2/g, 10 g Reference Material, Silica alumina, ~ 215 m2/g,10 g

302-33002-00 062-00000-11 062-00000-23 062-33002-00 004-16830-00 003-22617-00 003-22626-00 004-62230-58 004-62230-32 004-33601-00 004-33602-00 004-16833-00 004-16821-00

Jul 09

10-1

Ordering Information

TriStar II 3020

Part Number

Item and Description

004-16818-00 004-16816-00 003-63801-01 004-25549-00 290-25846-00 290-25846-01 240-14855-00 240-25853-00 240-25901-00 302 -33601-00

Reference Material, Glass, ~ 5.8 m2/g, 10 g Reference Material, Alumina, ~ 0.25 m2/g, 15 g; for krypton analysis Cable, ethernet straight-thru Reducer, 1/8-in. tube x 1/4-in. tube Gas inlet line, 1/8 in. x 6 ft long, copper Gas inlet line, 1/8 in. x 16 ft long, copper Rack, sample tube Funnel, sample tube Dip stick; for checking liquid nitrogen level in Dewar Sample Tube Kit, 1/4-in; includes six each sample tubes, O-rings, and plastic caps; three each isothermal jackets, filler rods, and ferrules; and a Dewar cover Sample Tube Kit, 3/8-in; includes six each sample tubes, O-rings, and stoppers; three each isothermal jackets, filler rods, and ferrules; one sample tube brush; and a Dewar cover Sample Tube Kit, 1/2-in; includes six each sample tubes, O-rings, and stoppers; three each isothermal jackets, filler rods, and ferrules; one sample tube brush; and a Dewar cover Sample tube, 1/4-in. stem OD; for analyzing powdered samples where free-space management (with a filler rod inserted) is critical Sample tube, 3/8-in. stem OD; for analyzing any type of sample Sample tube, 1/2-in. stem OD; for analyzing larger pieces of granular or pelleted samples Sample tube, 1/4-in. stem OD, flat bottom Sample tube, 3/8-in. stem OD, flat bottom Sample tube, 1/2-in. stem OD, flat bottom Isothermal jacket, for 1/4-in sample tube Isothermal jacket, for 3/8-in. sample tube Isothermal jacket, for 1/2-in. sample tube Hanging filler rod, for 1/4-in. sample tube Hanging filler rod, for 3/8-in. sample tube Hanging filler rod, for 1/2-in. sample tube Filler rod, for 1/2-in. sample tube when using the Seal Frit O-Ring, Buna-N size 010; for sample port and 1/4-in. sample tube O-Ring, Buna-N size 012; for 3/8-in. sample tube O-Ring, Buna-N size 014; for 1/2-in. sample tube

302 -33602-00

302 -33603-00

302-61001-00 302-61001-01 302-61001-02 302-61002-00 302-61002-01 302-61002-02 302-25812-00 302-25812-01 302-25812-02 302-25821-00 302-25821-01 302-25821-02 302-61005-02 004-25466-00 004-25022-00 004-25469-00

10-2

Jul 09

TriStar II 3020

Ordering Information

Part Number

Item and Description

300-31802-02 300-31802-03 004-54104-00 300-25825-00 300-25826-00 260-25843-00 004-27046-00 004-32004-00 004-32604-08 302-33607-00 260-25890-00 300-32800-00 300-25861-20 004-27040-00 004-16003-01 200-25879-00 302-42801-00 202-33024-00

Dewar cover, for 1/4-in. and 3/8-in. sample tubes Dewar cover, for 1/2-in. sample tube Brush, for cleaning sample tubes Ferrule, for 1/4-in. sample tube Ferrule, for 3/8-in. sample tube Ferrule, for 1/2-in. sample tube Frit, 40 µm, for sample port Stopper, rubber, for 3/8- and 1/2-in. sample tubes Cap, plastic, for 1/4-in. sample tube Seal Frit Kit; includes three seal frits, nine openers, three filler rods, installation tool and instructions Seal Frit assembly Support, sample weighing Dewar, 2.75 liters Filter, for vacuum pump exhaust Oil, vacuum pump, 1 Liter Funnel, for filling vacuum pump with oil Operator’s manual, TriStar 3020 DataMaster Program; allows you to generate classical or micropore data reductions

Jul 09

10-3

TriStar II 3020

Appendix A

A. FORMS
This appendix contains the following form: • Sample Data Worksheet Copy and use this form as needed.

Mar 08

A-1

Sample Data Worksheet
Use this worksheet to record the values necessary to calculate the sample mass. Sample Tube Identification:_________________________________

Sample Mass

NOTE: Record all values in grams. Before Degas A. Mass for empty sample tube set: B. Sample tube set plus sample mass: C. Sample mass (B - A): ____________ ____________ ____________ _____________ _____________ ____________ ____________ After Degas After Analysis

Degas Information

Degas apparatus: Temperature (ºC): Time (hours): Actual time started: Actual time finished:

____________________________________________ ____________________________________________ ____________________________________________ ____________________________________________ ____________________________________________

Degas notes: ________________________________________________________________________ ___________________________________________________________________________________ ___________________________________________________________________________________ ___________________________________________________________________________________ ___________________________________________________________________________________

TriStar II 3020

Appendix B

B. ERROR MESSAGES
Error messages for the are listed numerically. If the Action response instructs you to contact your service representative, record the error message and make backup copies of any files involved in the operation.
The 1000-series error message, used primarily for software testing, are not included in this appendix. These errors should not occur during normal operation. If you receive a 1000-series message, contact your service representative after making backup copies of nay files involved in the operation.

2400 Series
2401FATAL ERROR: (error message)

Cause:

An internal processing and/or hardware error has occurred during communication with the analyzer. Contact your service representative if you continue to receive this message.

Action:

2430-

Error accessing file (file name), error code = (number).

Cause A: Action A:

Media may be damaged. Clean the media drive. If this does not eliminate the problem, attempt operation using a backup copy of the file.

Cause B: Action B:

Hard disk may be damaged. Contact your service representative.

Cause C: Action C:

A software error occurred when the file was accessed. Contact your service representative.

Cause D: Action D:

The name specified contains one or more invalid characters. Enter a valid filename (refer to your operating systems manual).

Mar 08

B-1

Appendix B

TriStar II 3020

2431-

Error writing file (file name), error code = (number).

Cause:

The hard disk does not have enough space left to perform the operation. Copy files not used regularly from the hard disk to diskette, delete them from the hard disk, and then try the operation again

Action:

2432-

Invalid response from MMI ‘FILE_READ’ request.

Cause: Action:

An internal processing and/or hardware error has occurred. Contact your service representative if you continue to receive this error message.

2433-

New entries have been found in this directory. Refresh the directory information?

Cause:

Several TriStar 3020 files (sample information, analysis conditions, adsorptive properties, or report options) have been added to this directory by some function other than the TriStar 3020 program. Select Yes to update the directory information with data from each new file. This operation may take a minute. Select No if you do not want to spend the time updating the directory information. This option may be feasible if a large number of files have been copied into the directory and you know the name of the file you wish to access.

Action:

2434-

File (file name) — Subset # (number) wrote wrong amount of data.

Cause: Action:

An internal processing and/or hardware error has occurred. Contact your service representative if you continue to receive this error message.

B-2

Mar 08

TriStar II 3020

Appendix B

2436-

Path specification (path name) is invalid.

Cause: Action:

You entered an invalid path name and/or extension. Type a valid path name (including the proper extension) and press
Enter.

2437-

File (file name) does not exist.

Cause: Action:

You entered a file specification that does not exist. Enter an existing file specification or select a file name from the list box.

2438243924402441244224432444244524462447-

Disk drive (letter): is inaccessible. Could not register file. Subset not found. Seek within file failed. Bad header in subset file. Subset owner denied access. Not a valid file format. Subset wrote the wrong amount of data. Error reading data. Error writing data.

Cause: Action:

An unexpected error occurred when you tried to access a data file. Contact your service representative.

2448-

File directory (path name) is invalid. Resetting to the installation directory.

Cause:

A working directory specified in the .INI file is invalid. The directory may have been deleted or moved to a different location. The installation directory will be substituted. The next time you open a file, use the Directories list to move to the correct directory.

Action:

2449-

This field does not contain a valid file specification.

Cause: Action:

You entered an invalid file name. See the description of file naming conventions in your Windows manual and re-enter the name.

Mar 08

B-3

Appendix B

TriStar II 3020

2450-

Sample Defaults may not be edited while this operation is in progress. Do you wish to save and close the Sample Defaults edit session?

Cause:

You are in the process of initiating an automatic analysis (an analysis in which sample files are created using the defaults) while editing the defaults. Finish your edit session of the defaults and close the dialog. Then restart the automatic analysis.

Action:

24522453-

Attempt to write MICATTR.DIR in read only mode. (file name) Attempt to append MICATTR.DIR in read only mode. (file name)

Cause:

The Read-Only attribute is turned on in the application’s MICATTR.DIR file (this file exists in each folder containing sample or parameter files). Use Windows Explorer to access the folder containing the MICATTR.DIR file and disable the Read-Only option.

Action:

24542455-

Too many selections for a print-to-file operation. Only the first (number) selections will be processed. Please reselect the remainder. Too many selections for an export-to-file operation. Only the first (number) selections will be processed. Please reselect the remainder.

Cause: Action:

You selected too many files for this operation. Select only the number of files specified in the message.

2456-

Insufficient file handles available. Application cannot continue.

Cause: Action:

You have more than 50 files open at the same time. Refer to the manual for your operating system and set the limit for open files to 50 or greater.

B-4

Mar 08

TriStar II 3020

Appendix B

2457-

Results cannot be displayed. More than (number) windows are currently displaying or printing results.

Cause: Action:

You have too many windows open in the application. Close some of the open windows.

2458-

An instrument is performing a critical operation. Wait a few moments before exiting the application.

Cause:

You are attempting to exit the application while the instrument is performing a critical operation. This operation must be completed before the application can be stopped. Wait a short time and attempt to stop the application again.

Action:

2459-

An instrument is busy. A delay in restarting this application could result in loss of new data. Continue with program Exit? (Yes, No)

Cause:

You are attempting to exit the application while an analysis is in progress. While this is possible, the data collected while the application is inactive will not be permanently recorded until the application is restarted. A power failure to the instrument could cause some data to be lost. If you are not concerned with the potential for loss of data should a power failure occur, click Yes to continue; otherwise click No.

Action:

2460-

Fatal Communications error on (Unit n - S/N: nnnn)

Cause:

There was a fatal error in communication between the application and the software in the instrument. All displays for that instrument will be closed. Ensure that the analyzer is connected to the computer on the communications port configured in the Setup program. Stop the TriStar 3020 software and then restart it. If this error persists, contact your service representative.

Action:

Mar 08

B-5

Appendix B

TriStar II 3020

2461-

No instruments are in operation. This application will unconditionally terminate.

Cause:

At least one instrument must be active for the application to operate. The initialization of all of the instruments configured with the Setup program has failed. The application stops. Usually this message is preceded by another message giving the reason for the instrument’s failure to initialize. See the instructions for that message. Ensure that the instrument is attached to the computer on the communications port configured with the Setup program. Verify that the instrument has the power switch in the ON position and that the light on the front panel is illuminated. If the application continues to fail in its attempts to initialize the instrument, contact your service representative.

Action A:

Action B:

2477-

Unit n - S/N: nnnn did not properly initialize.

Cause:

The software was unable to initialize this instrument; this is usually caused by one of the conditions listed in the error messages above. Correct the problem as described above, then restart the application.

Action:

2478-

Error copying sequential data segment.

Cause:

An internal processing and/or hardware error occurred while accessing a portion of a sample file. Confirm that the media being accessed does not contain errors; for example, you may wish to use a utility such as ScanDisk. Contact your service representative if you continue to receive this error message.

Action:

B-6

Mar 08

TriStar II 3020

Appendix B

2479-

(Unit n; Serial nn) The instrument is busy performing an operation of which this application is unaware. Do you want to cancel? (Yes, No)

Cause:

During initialization of the application, the status of the analyzer was found to be in a different state than expected. Click Yes to cancel the operation in process, allowing the analyzer to reset and continue with initialization. Click No to cancel the initialization process. If you continue to get this message, verify that files in the application directory structure are not being changed or removed.

Action:

2480-

File <name> cannot be analyzed. It is currently being edited.

Cause: Action:

You are trying to start an analysis using a file that is open for editing. Finish editing the file, save and close it, then start the analysis.

2481-

Error accessing the sample information file <name>.

Cause: Action:

An unexplained error prevents you from accessing this file. The hard disk drive may be corrupt. Run diagnositics.

2482-

File cannot be opened for writing. It is already in use.

Cause:

You attempted to open a file that is currently being used (either by this application or another). Locate the application using the file (in the Micromeritics application, use the Windows menu item to get a list of all windows, one of which may contain this file).

Action:

Mar 08

B-7

Appendix B

TriStar II 3020

2483-

An analysis cannot be performed on (file name). It is open for editing and contains errors.

Cause:

You attempted to use a sample file containing errors that is currently open. Go to the window containing the file, correct the errors, and save it.

Action:

2484-

The edit session for <name> must be saved before the analysis. Save changes and continue with the analysis? (yes, no)

Cause:

You are trying to start an analysis using a file that contains unsaved changes and is open for editing. Select Yes to save the changes and proceed with the analysis; select No to cancel the analysis and continue editing the Sample Information file.

Action:

2485-

The service test file has an invalid status and cannot be used for this analysis.

Cause: Action:

The selected service test file has a status other than No Analysis. Select a different service test file or create a new one and use Replace All to copy parameters from the file you originally selected.

2486-

Could not construct (name) report type. Program will terminate.

Cause A: Action A:

You may not have full rights to the application’s folders and files. Contact your system administrator to have full rights granted.

Cause B: Action B:

An internal processing and/or hardware error has occurred. Contact your service representative if you continue to receive this error message.

B-8

Mar 08

TriStar II 3020

Appendix B

2487-

Could not start report generator. Error code (number). Program will terminate.

Cause: Action:

An internal processing and/or hardware error has occurred. Contact your service representative if you continue to receive this error message.

2488-

File (file name) cannot be opened for editing. It is already in use.

Cause: Action:

The file you specified is being used in another edit operation. Check the Windows list to locate the other edit session.

2489-

File (file name) cannot be opened for writing. It is already in use.

Cause: Action:

The file you specified in a Save As operation is already open for edit. Select a different file for the Save As operation.

2490-

No ‘.INI’ file present. Application will terminate.

Cause:

The ASCII file containing initialization information and system options information used during program startup does not exist. Run the TriStar 3020 Setup program, select Change analyzer setup, and create the control file used by the TriStar 3020.

Action:

2491-

Highlighted fields contain errors. Please correct the errors before closing dialog box.

Cause:

The highlighted fields contain invalid entries. You will not be able to close the dialog box until you correct the errors. Check the entries, correct the errors, and close the dialog box.

Action:

2492-

This field’s entry is invalid.

Cause: Action:

The highlighted field contains an invalid entry. Check the entry and correct the error.

Mar 08

B-9

Appendix B

TriStar II 3020

2493-

An entry is required for this field.

Cause: Action:

This field requires a valid entry for you to proceed. Enter or select an appropriate value.

2494-

Value is out of the valid range.

Cause:

The value you entered in the highlighted field is outside the valid range of values. Check the entry and enter or select an appropriate value.

Action:

2495-

Value is out of the valid range. Enter a value between (value) and (value).

Cause:

The value you entered in the highlighted field is outside the valid range of values. Check the entry and enter or select a value within the indicated range.

Action:

2496-

Invalid number.

Cause: Action:

The number you entered in the highlighted field is invalid. Check the entry and enter or select a valid number.

2497-

This field contains an invalid character.

Cause: Action:

You entered an invalid character in the highlighted field. Check the entry and enter valid characters.

2498-

The requested change to the Sample’s status is invalid at this time.

Cause:

A request to change the file’s status (for example, from automatically collected to manually entered) could not be done. Contact your service representative if you continue to receive this error message. Record the name of the sample file in which the problem occurred.

Action:

B-10

Mar 08

TriStar II 3020

Appendix B

2499-

Sequence number must contain at least 3 digits.

Cause:

You tried to enter a sequence number that did not contain at least three digits. Enter a sequence number that contains at least three digits.

Action:

Mar 08

B-11

Appendix B

TriStar II 3020

2500 Series
2500All sample file names that can be created using the sequence number pattern already exist. You may want to modify the next sequence number.

Cause:

No more sample information files can be created using the currently entered file name sequence number. Select Options > Sample defaults and enter another sequence number.

Action:

2501-

System resources have reached a dangerously low level. Please close some windows to avoid the loss of data.

Cause:

A large number of windows are open and consuming the system resources available to all applications. Close one or more windows on the screen. Contact your service representative if you continue to receive this error message.

Action:

2502-

Error writing to file (name) during print. Error code: (number).

Cause: Action:

An error occurred in the file being written to during a print operation. Ensure that there is sufficient space on the drive containing the file.

2503-

Error converting file (file name). Could not create DIO intermediate file.

Cause A:

Insufficient space is available on the hard disk. The DIO file is placed in the directory specified by the TEMP environment variable. Determine if there is sufficient space on the drive where the TEMP directory is located.

Action A:

Cause B: Action B:

An internal processing and/or hardware error has occurred. Contact your service representative if you continue to receive this error message.

B-12

Mar 08

TriStar II 3020

Appendix B

2504-

Cannot create output file for sample (sample name).

Cause: Action:

Insufficient space may be available on the hard disk. Ensure that sufficient space is available. Contact your service representative if you continue to receive this error message.

2506-

(sample file) Output device (name) is not installed. Printing cannot be accomplished.

Cause: Action:

The selected output device is not installed in Windows. Select a different output device in the System Configuration dialog box. Install the device using the Control Panel - Printers operation.

2508-

(sample file) Overlay file (name) was not found. It will not be included in the reports.

Cause: Action:

The specified overlay file could not be found. Ensure that the file specified as an overlay does exist.

2509-

(sample file) Error opening file (name): (error). Reports cannot be produced.

Cause:

An error occurred while the program was opening a file necessary to the report operation. Use the name given in the error message to investigate. Contact your service representative if you continue to receive this error message.

Action:

Mar 08

B-13

Appendix B

TriStar II 3020

2510-

(sample file) Error parsing reports from file (name). Reports cannot be produced.

Cause A:

One or more data entry fields in the sample file may contain an invalid character (such as a single quote or double quotes). Review the data entry fields and remove the invalid character.

Action A:

Cause B:

The system was unable to create the usual temporary files during the report, possibly due to insufficient disk space. Check the space available on the hard disk.

Action B:

Cause C: Action C:

An internal processing error occurred. Contact your service representative.

2511-

Print job (name) has been cancelled due to insufficient disk space. Delete unnecessary files and restart the report.

Cause:

The disk drive does not have enough space for the temporary file required by the Windows Print Manager. Therefore, printing of the requested report has been canceled. Delete unnecessary files from the disk. You will require at least five megabytes of free space for normal operation.

Action:

2512-

Print job (name) cancelled.

Cause: Action:

The requested print job was canceled at your request. None required.

2513-

Unable to read the calibration file (file name).

Cause: Action:

You selected an invalid calibration file or one that cannot be read. Be sure the media containing the calibration file has no problems.

B-14

Mar 08

TriStar II 3020

Appendix B

2514-

Unable to write the calibration file (file name).

Cause:

An attempt to Save calibration data has failed due to possible media problems. Be sure the media you want to Save the file to has no problems. Choose an alternate media to Save the calibration data.

Action A: Action B:

2515-

Warning: Changing the calibration information will affect the performance of the instrument. Only qualified service personnel should do this. Do you wish to proceed?

Cause: Action:

You have started the process of performing a calibration operation. Calibration operations should only be done by or under the direction of qualified service personnel.

2516-

Warning: Keeping a backup copy of the calibration data is recommended by Micromeritics. Would you like to do so now?

Cause:

You have performed a calibration operation; a backup copy is recommended. Perform a calibration Save operation.

Action:

2517-

Canceling this dialog will reset the calibration state to what it was when this dialog was first opened. Are you sure you want to cancel?

Cause: Action:

You have not accepted the calibration you performed. If the calibration operation was successful, press Accept.

2521-

Unable to program controller.

Cause: Action:

A hardware malfunction has occurred. Contact your local Micromeritics service representative.

Mar 08

B-15

Appendix B

TriStar II 3020

2522-

Invalid controller application file.

Cause: Action:

The application’s control file has been corrupted or deleted. Reinstall the TriStar analysis program.

252325242525252625272528252925302531-

Programming the controller failed. CRC check failed on programming controller. Unknown error programming controller. Controller download was not successful. Controller CRC error on boot block. Controller DRAM error. Controller Com1: error. Controller Com2: error. Controller debug port error.

Cause: Action:

An internal processing and/or hardware error has occurred. Contact your service representative if you continue to receive this error message.

2532-

The instrument contains a different software version. Do you want to reset it?

Cause:

The application has discovered a different version of software operating in the analyzer. If there are no analyzers other than the TriStar connected to the computer, select Yes and allow the updated software to load.

Action:

2533-

Analyzer initialization failed.

Cause: Action:

An internal processing and/or hardware error has occurred. Contact your service representative if you continue to receive this error message.

B-16

Mar 08

TriStar II 3020

Appendix B

2534-

Error opening file (name) for printing. Error code: (number).

Cause: Action:

An error occurred in the selected file for print output. Ensure that sufficient space is available on the drive containing the file.

2548-

System status (n)

Cause: Action:

There was a problem establishing communication with the analyzer. Ensure that the communications cable is seated firmly in the ethernet slot at the analyzer connection and the computer connection. If you continue to get this message, contact your Micromeritics service representative.

2549-

Error accessing online manual file (code #).

Cause: Action A: Action B:

The operator’s manual file could not be located. Reinstall the application. Copy the contents of the manual folder on the setup CD to the application directory.

2550-

Attempts to acquire the instrument’s status timed out.

Cause: Action:

There was a problem establishing communication with the analyzer. Ensure that the communications cable is seated firmly in the ethernet slot at the analyzer connection and the computer connection. If you continue to get this message, contact your Micromeritics service representative.

Mar 08

B-17

Appendix B

TriStar II 3020

4000 Series
40004001Memory Allocation Error. Error Smoothing Data.

Cause:

An internal processing and/or hardware error occurred during report generation. Contact your service representative if you continue to receive this error message.

Action:

4002-

Thermal Transpiration correction had no effect.

Cause:

The Thermal transpiration correction option was selected on the Report Options dialog. However, the correction did not change any pressure by more than one percent. Deselect this option to disable this message. This correction is only meaningful for very low pressures.

Action:

40034004-

Error Converting Pressures. Error Computing Volume Adsorbed.

Cause:

An internal processing and/or hardware error occurred during report generation. Contact your service representative if you continue to receive this error message.

Action:

4005-

Pressures were not smoothed. Not enough pressures below 0.10 P/Po.

Cause:

The Smooth pressures below 0.10 P/Po option was selected on the Report Options dialog. There must be at least 10 pressures within this range for smoothing to occur. Deselect this option to disable this message.

Action:

B-18

Mar 08

TriStar II 3020

Appendix B

40064007-

Report Type Not Found. Error Processing Report.

Cause:

An internal processing and/or hardware error occurred during report generation. Contact your service representative if you continue to receive this error message.

Action:

4008-

Report requested on sample file with no data points.

Cause: Action:

You selected a file for reporting which contains no collected data. Select another file which contains collective data and restart the report.

4010-

Summary Report was not included in the Selected Reports.

Cause:

You did not select a plot or a table for any of the Selected Reports in the Report Options dialog; you selected the reports only to generate an entry in the summary. However, the Summary was not included in the Selected Reports. Select a plot or table in one or more of the Selected Reports, and/or add the Summary to the Selected Reports.

Action:

4014-

File (name) is not a valid file for conversion.

Cause: Action:

The file selected for conversion is not a valid file. Select only files that have been created by TriStar 3000 or Gemini programs.

4015-

Error creating export file for sample <sample file name>.

Cause: Action:

A file error occurred during creation of an export output file. The output file name may be invalid. Ensure that the target directory exists. Ensure that the target diskette is not full or write protected. The target disk drive may be damaged or inoperative. Verify that other files may be created on the same drive. Contact your service representative if you continue to receive this error message.

Mar 08

B-19

Appendix B

TriStar II 3020

4016-

Sample <sample file name> has no data for export to ISO/DFT.

Cause:

The file selected for export has a status of No Analysis. No export file will be created. Select a file which contains analysis data.

Action:

4017-

Damage to the instrument will result if the sample has not been manually evacuated. Have you evacuated the sample?

Cause:

You did not select Backfill sample at start of analysis on the Sample Backfill Options dialog. The sample tube is normally at atmospheric pressure when an analysis is started, and it must be backfilled before the analysis begins to prevent sample material from being drawn into the manifold. If you have manually evacuated the sample tube, select Yes. If you have not, select No and then either perform a manual evacuation or go to the Sample Backfill Options dialog and select Backfill sample at start of analysis.

Action:

4020-

Disabling this option may damage the instrument. Are you sure that the sample should not be backfilled?

Cause:

You did not select Backfill sample at start of analysis on the Sample Backfill Options dialog. The sample tube is normally at atmospheric pressure when an analysis is started; it must be backfilled before the analysis begins to prevent sample material from being drawn into the manifold. If you want to manually evacuate the sample prior to the start of the analysis, select Yes. Otherwise, select No, go to the Sample Backfill Options dialog, and select Backfill sample at start of analysis.

Action:

4023-

The file <name> cannot be prepared for analysis. It is open for editing and contains errors.

Cause:

You are trying to start an analysis using a file that contains errors and is open for editing. Finish editing this file, save and close it, then start the analysis.

Action:

B-20

Mar 08

TriStar II 3020

Appendix B

4026- Cannot calculate Dubinin-Astkahov: bad least squares data.

Cause: Action:

Less than two selected data points are within the fitted pressure range. Edit the calculation assignments on the Collected Data dialog, or change the fitted pressure range on the Dubinin report options dialog.

4027-

Fewer than two sample files have data suitable for heat of adsorption reports.

Cause:

Less than two of the sample files you selected for heat of adsorption reports contain appropriate data. Edit the Quantity Adsorbed table, or select other sample files.

Action:

4028-

Dubinin calculations cannot be performed because the affinity coefficient of the analysis gas is zero.

Cause:

Dubinin values could not be calculated because the affinity coefficient of the analysis gas is zero. Access the Dubinin Report Adsorptive options in the sample file and enter an appropriate value for the analysis gas.

Action:

4029-

At least two fitted data points are needed for Alpha-S calculations.

Cause: Action:

Fewer than two data points fall within the selected Alpha-s range. Edit the calculation assignments or the fitted Alpha-s range, or use a different reference curve.

4030-

Preparations failed in primary data.

Cause: Action:

Appropriate data were not available to generate the report. This message was preceded by a different error message; refer to the cause/action of the preceding message.

Mar 08

B-21

Appendix B

TriStar II 3020

4031-

Not enough points with a relative pressure in the range (n,n)

Cause:

Fewer than two data points selected for the Dubinin report falls within the selected relative pressure range. Edit the calculation assignments or the fitted relative pressure range.

Action:

4032-

Some summary reports could not be produced because they require the Micropore option.

Cause:

Some of the summary reports you requested were not produced because you do not have the micropore option installed. Edit the summary report and deselect the micropore options.

Action:

4033-

Not enough points to generate Dubinin Tabular Report.

Cause:

There are fewer than two valid data points available for the Dubinin tabular reports. Examine the calculation assignments in the Collected Data dialog of the sample file. You must have at least two micropore pressures selected for inclusion in the Dubinin report.

Action:

4034-

Fewer than 2 points available for Dubinin calculations.

Cause:

There are fewer than two valid data points available for Dubinin reports in one of the sample files selected for overlaying. Examine the calculation assignments in the Collected Data dialog of the sample file. You must have at least two micropore pressures selected for inclusion in the Dubinin report.

Action:

B-22

Mar 08

TriStar II 3020

Appendix B

4035-

Cannot calculate optimized Astakhov exponent: Not enough points with a relative pressure in the range [(pressure), (pressure)].

Cause:

There are fewer than two valid data points in the relative pressure range specified. Astakhov reports will not be produced. Examine the calculation assignments in the Collected Data dialog for the sample file. You must have at least two pressures in the given range selected for inclusion in the Dubinin report.

Action:

4036-

Fewer than 2 points available for Horvath-Kawazoe calculations.

Cause:

You must select at least two data points for inclusion in the HorvathKawazoe analysis on the Collected Data dialog. No report will be produced. From the Collected Data dialog, select the data points to be analyzed.

Action:

4037-

Computations failed while processing the primary data set. No reports will be produced.

Cause:

The preparation of data for reporting could not be successfully completed. No Horvath-Kawazoe reports will be produced. This message will always be preceded with another one containing additional information. Refer to the number of the error message which preceded this one for an explanation.

Action:

4038-

Fewer than 2 points available for the Langmuir Qm computation. Cheng/Yang correction will not be applied.

Cause:

The Cheng/Yang correction to the Horvath-Kawazoe equation requires the value of the monolayer volume as calculated from the Langmuir equation. The isotherm must include at least two points above 0.02 relative pressure for the Langmuir equation to be applied. The analysis will be performed without the Cheng/Yang correction. Deselect Apply Cheng/Yang correction on the Horvath-Kawazoe Report Options dialog to prevent this message from appearing on future reports.

Action:

Mar 08

B-23

Appendix B

TriStar II 3020

4039-

The isotherm does not meet the constraints of the Cheng/Yang assumption. Cheng/Yang correction will not be applied.

Cause:

The Cheng/Yang correction to the Horvath-Kawazoe equation requires the value of the monolayer volume as calculated from the Langmuir equation. The isotherm does not correlate to the Langmuir assumption with a coefficient of 0.98 or more. The correction is not applicable to this isotherm or to the range of the data points selected. The analysis will be performed without the Cheng/Yang correction. Deselect Apply Cheng/Yang correction on the Horvath-Kawazoe Report Options dialog to prevent this message from appearing on future reports.

Action A:

Action B:

Generate the Langmuir report for the same data points selected for the Horvath-Kawazoe report. If the Langmuir correlation coefficient can be brought above 0.98 by removing some points at high relative pressure, remove them and reproduce the Horvath-Kawazoe reports.

4040-

The value of Qm computed from the Langmuir equation is too low. The pore size will not be computed for all data points.

Cause:

The Cheng/Yang correction to the Horvath-Kawazoe equation requires the value of the monolayer volume as calculated from the Langmuir equation. The computed value is less than the volume adsorbed at the largest relative pressure included in the analysis. The correction is not applicable to this isotherm or to the range of the data points selected. The analysis will be performed and the Cheng/Yang correction will be applied to all points with a volume adsorbed less than the value of Vm. The pore size will not be calculated for data points with an invalid volume adsorbed. Deselect Apply Cheng/Yang correction on the HorvathKawazoe Report Options dialog to clear this message.

Action:

B-24

Mar 08

TriStar II 3020

Appendix B

4041-

Cheng/Yang correction is inappropriate for some P/Po.

Cause:

The Cheng/Yang correction is usually inappropriate for any P/Po above the isotherm knee. In some instances, the computed pore sizes may decrease above the knee. While it is possible to include these relative pressures (usually above 0.1 P/Po) in the analysis, the computed pore sizes for these pressures are usually meaningless. Change the data points selected for the Horvath-Kawazoe report to include only relative pressures at or below the knee of the isotherm, or change the Horvath-Kawazoe report options so that the Cheng/Yang correction is not applied.

Action:

4042-

0.0 cannot be a starting or ending pressure for a geometric progression from low pressure.

Cause:

You selected to generate a pressure table from a geometrically progressing range. Change the 0.0 entered value.

Action:

4043-

1.0 cannot be a starting or ending pressure for a geometric progression toward saturation.

Cause:

You selected to generate a pressure table from a geometrically progressing range. Change the 1.0 entered value.

Action:

4044-

Points in the Langmuir report pressure table lie outside the collected data.

Cause:

Calculation assignments are not being used and more than one of the report pressure table points is above the range of the collected data, and more than one is below. Change the report pressure table to be more consistent with the collected data.

Action:

Mar 08

B-25

Appendix B

TriStar II 3020

4045-

Points in the report pressure table lie outside the collected data.

Cause:

Calculation assignments are not being used and more than one of the report pressure table points is above the range of the collected data, and more than one is below. Change the report pressure table to be more consistent with the collected data.

Action:

4046- (file name) could not be opened for reading.

Cause: Action:

A thickness curve file could not be opened. If the problem persists, restart your computer and optionally perform a media integrity check (using ScanDisk).

4047-

Warning: An error occurred while reading (file name).

Cause: Action:

An error happened during a read operation of a thickness curve file. If the problem persists, restart your computer and optionally perform a media integrity check (using ScanDisk).

4048-

Warning: An error occurred while restoring the heat of adsorption report editor.

Cause:

The state of the heat of adsorption report editor could not be restored. Default settings will be used. No action.

Action:

4049-

The sample (file name) does not have enough data. A minimum of two adsorption points is required.

Cause:

A sample file has been included in the Heat of Adsorption report that does not have enough data. Remove the file from the selected file list.

Action:

4050-

None of the requested quantities adsorbed is within the range of the collected

B-26

Mar 08

TriStar II 3020

Appendix B

data of more than one sample file.

Cause:

The Heat of Adsorption report failed because the specified quantities are not within the range of the collected data. Edit the quantities adsorbed so that they are within the range of the collected data, or select other sample files.

Action A:

4051-

The sample (file name) does not have any data in the range of the requested quantities adsorbed.

Cause:

The sample’s data cannot be interpolated to any of the quantities adsorbed. Edit the quantities adsorbed so that they are within the range of the collected data.

Action:

4052-

Fewer than two points are selected for this report.

Cause: Action:

At least two points are required for the BET calculations. Edit the calculation assignments for the BET report.

4053-

At least two data points must be selected for t-Plot calculations.

Cause: Action:

At least two points are required for the t-Plot calculations. Edit the calculation assignments for the t-Plot report.

4054-

Fewer than two data points are inside the fitted thickness range.

Cause:

At least two points must be within the fitted thickness range for the tPlot calculations. Edit the calculation assignments for the t-Plot report.

Action A:

Action B:

Edit the fitted thickness range in the t-Plot report editor.

Mar 08

B-27

Appendix B

TriStar II 3020

4055-

A positive BET surface area was not calculated.

Cause:

Fewer than two points were assigned to the requested surface area calculation in the collected data table. Assign more points to the surface area calculation.

Action A:

Action B:

Select a different surface area in the t-Plot report editor.

4056-

A positive Langmuir surface area was not calculated.

Cause:

Fewer than two points were assigned to the requested surface area calculation in the collected data table. Assign more points to the surface area calculation. Select a different surface area in the t-Plot report editor.

Action A: Action B:

4057-

At least two data points are needed for Freundlich calculations.

Cause:

Less than two data points have been selected for the Freundlich report; at least two are required. Select Freundlich points on the Collected Data dialog. If calculation assignments are not being used, edit the Freundlich Report options, Absolute pressure range in the sample file.

Action:

4058-

At least two data points are needed for Temkin calculations.

Cause:

Less than two data points have been selected for the Temkin report; at least two are required. Select Temkin points on the Collected Data dialog. If calculation assignments are not being used, edit the Temkin Report options, Absolute pressure range in the sample file. You have selected at least one point with a negative pressure value to include in the Temkin report. Negative pressure points void Temkin calculations. Open the sample file and click the Collected Data tab. Locate the negative value(s) in the Temkin column and deselect it(them).

Action:

Cause:

Action:

B-28

Mar 08

TriStar II 3020

Appendix B

4059-

Fewer than 2 points available for MP-Method calculations.

Cause: Action:

At least two points are required for the MP-Method calculations. Edit the calculation assignments for the MP-Method report.

4060-

Sample (file name) contains no data points.

Action:

An attempt was made to save a sample without collected data as a tcurve or alpha-S curve. Repeat the save as t-curve or save as alpha-S operation after opening a sample that has collected data.

Cause:

4061-

The t-curve must contain at least 2 points.

Cause: Action:

At least two points are required in a thickness curve definition. Edit the thickness curve.

4062-

Error during report generation.

Cause: Action:

An internal processing error has occurred. Contact your Micromeritics service representative.

4063-

The data requested on this report are not available.

Cause: Action:

There is no information in the sample log to report. You selected a sample file for which no instrument operations have been used. Select a sample file with a status of Prepared, Preparing, Analyzing, or Complete to obtain a valid sample log report.

Mar 08

B-29

Appendix B

TriStar II 3020

4067-

No data points are within the range of pressures in the reference isotherm.

Cause:

Thre are no collected data points within the range of pressures in the reference isotherm. Select data points that are in the range of the reference isotherm, or select a more appropriate reference isotherm.

Action:

4068-

No points were selected for the f-Ratio report.

Cause:

The collected data column for the f-Ratio report does not have any points selected. Edit the collected data dialog and select points for the f-Ratio report.

Action:

4070-

Unable to load deconvolution model (name).

Cause:

For some reason, the list of available models was corrupted, therefore, the model selected could not be loaded for the deconvolution. Exit the program and reinstall the software, then try again.

Action:

4071-

The selected pressures points do not form a valid set for deconvolution.

Cause:

The data points selected for analysis do not contain enough information to allow a DFT data reduction. Edit data points in the table of the Collected Data dialog, or select another sample file. At least two points with strictly increasing pressures and volumes adsorbed are required for a DFT Plus data reduction. Edit the pressure range on the DFT report options dialog.

Action A:

Action B:

B-30

Mar 08

TriStar II 3020

Appendix B

4072-

The range of pressures selected is too small to deconvolute using this model.

Cause: Action:

A null result was found using the selected model. Edit data points in the table of the Collected Data dialog, or select another sample file. At least two points with strictly increasing pressures and volumes adsorbed are required for a DFT data reduction.

4073-

The analysis gas (name) does not match the model gas (name).

Cause:

The model assumes a specific gas and the sample file uses a different one. Select a model that assumes the same gas.

Action:

4074-

The analysis temperature (nn) does not match the model temperature (nn).

Cause:

The temperature for the selected model did not match the analysis temperature. Select a different model.

Action:

4075-

The models cannot be located in the models folder. Reinstall the software.

Cause:

The models could not be located. They may have been inadvertently deleted or moved. Reinstall the software.

Action:

Mar 08

B-31

Appendix B

TriStar II 3020

4077-

Cannot get surface area for: (file name)

Cause:

The Isotherm report for the named overlay file has Per gram selected for the Volume Adsorbed, and the Isotherm report for the primary file has a surface area option selected for the Volume Adsorbed. Edit the Isotherm report for the named overlay file and select a surface area option for Volume Adsorbed. Click Overlays on the Report options dialog of the primary file and remove the named overlay file from the list.

Action A:

Action B:

4078-

Slope and Y-Intercept cannot be determined from the selected points.

Cause: Action:

The Langmuir report cannot be generated from the selected points. Edit the calculation assignments in the Langmuir column on the Collected Data dialog.

4079-

Points found with negative pressure values will not appear on the graph.

Cause: Action:

Collected data contains negative pressure values. Negative pressure points are automatically removed from isotherm graphs. If you wish to have negative pressure values appear on the graph: Open the sample file and click the Collected Data tab. Deselect Use calculation assignments and then select the points with negative pressures as Outliers.

4400-

The communications port specified for the SmartPrep(s) is not physically installed in the Control Module. Cannot initialize.

Cause: Action:

The communications port associated with this unit was not valid. Run the setup program and set up the unit on a valid port.

B-32

Mar 08

TriStar II 3020

Appendix B

4401-

The communications port specified for the SmartPrep(s) is already in use. Cannot initialize.

Cause:

The communications port associated with this instrument is in use by some other program in the system. Close the other program to release the port. Restart the TriStar 3020 application.

Action:

44024403-

The communications port specified for the SmartPrep(s) cannot be accessed. Cannot initialize. Cannot communicate with SmartPrep Unit n - S/N: nn.

Cause: Action:

The communications port associated with this unit was not valid. Run the setup program and set up the unit on a valid port.

4404-

The application version of the SmartPrep Unit n - S/N: nn is invalid.

Cause:

The controller software running on the designated instrument is invalid. Use the SmartPrep setup program to download the proper controller software to the instrument, or contact a service representative if unavailable.

Action:

4405-

Fatal communications error with SmartPrep Unit n - S/N: nn.

Cause:

There was a fatal error in the serial communications between the application and the SmartPrep Instrument Controller. All displays for that SmartPrep will be closed. Ensure that the SmartPrep is properly chained to the computer on the communications port configured in the Setup program. Stop and restart the application. If this error persists, contact your service representative.

Action:

Mar 08

B-33

Appendix B

TriStar II 3020

6000 Series
6000An error occurred while loading the application control information. Data entry cannot be performed. (Code number)

Cause:

An error occurred accessing the control information disk file required by this application. The disk drive may have failed or be corrupt. Run diagnostics on the disk drive.

Action:

6002-

File cannot be opened for writing.

Cause:

You attempted to save to a file that is marked as “read-only.” Files can be marked automatically as read-only when they are transferred from a CD to the application directory. Use Windows Explorer to access the folder containing the file and disable the Read-Only option. Enter a different name to save the file.

Action A:

Action B:

6003-

Unable to read the calibration file (number).

Cause:

Your attempt to load a previously saved calibration file was unsuccessful. Make sure the file exists, and that you have entered the file name correctly, then try again.

Action:

6004-

Unable to write the calibration file (number).

Cause: Action:

Your attempt to save the calibration to a separate file was unsuccessful. Make sure that the disk is not full or write-protected, then try again.

B-34

Mar 08

TriStar II 3020

Appendix B

6005-

The sample has an invalid status and cannot be used for this analysis.

Cause:

You selected a sample file with a status other than No Analysis or Prepared. Select a sample file with a status of No Analysis or Prepared.

Action:

6008-

At least one sample must be selected to proceed.

Cause: Action:

You attempted to start an analysis without selecting any sample files. Select at least one file, then start the analysis.

6010-

This sample requires a different adsorptive and cannot be analyzed at the same time as the other samples.

Cause:

You selected a sample file for analysis that requires a different adsorptive gas than the sample files selected for the other ports. Select only sample files to be analyzed with the same adsorptive and perform the analysis. Then perform the analysis with the other adsorptive.

Action:

6011-

The adsorptive required by this analysis is not available on this instrument.

Cause:

You attempted to start an analysis with an adsorptive that is not connected to the instrument, or has not been designated in the software. Make sure that the adsorptive is connected to the instrument. Then select Unit [n] > Unit configuration to tell the application that the gas is connected. Select only sample files for which the analysis gas is available.

Action A:

Action B:

6015-

Cannot read the sample tube properties parameter file.

Cause:

The sample tube file you selected on the QuickStart screen cannot be read. Select a different file.

Action:

Mar 08

B-35

Appendix B

TriStar II 3020

6016-

Dosing manifold from valve (number) failed.

Cause A:

The maximum time was exceeded before the target pressure point was reached. The nitrogen regulator may be set too low or turned off. Set the analysis gas regulator to 10 psig (0.7 bar), then resume the analysis.

Action A:

Cause B: Action B:

The analysis gas bottle is empty. Connect a new analysis gas bottle, then resume the analysis.

6017-

Leak test failed on port (number).

Cause:

With the sample port valve closed, the sample pressure increased by 0.15 mmHg before the leak test duration was completed. Check sample tube fitting and ensure that it is securely attached to the port, then restart the analysis.

Action:

6018-

Volume dosed exceeded 1000 cm3 STP. Analysis is canceled.

Cause: Action:

There is a problem with the analyzer’s calibration. Use the Setup program to reinstall the calibration files. If the problem persists, contact y our Micromeritics service representative.

6019-

Elevator failed to reach upper/lower limit switch.

Cause A: Action A: Cause B:

There is an obstruction in the elevator path. Clear all obstructions and restart the analysis. Ice is present in the bottom or the neck of the Dewar, preventing the elevator from rising completely. Check the Dewar; remove ice and restart the analysis.

Action B:

Action C:

Contact your service representative if results for Actions A and B failed.

B-36

Mar 08

TriStar II 3020

Appendix B

6020-

Warning, servo valve performance is out of specification.

Cause:

The servo valve tried to dose to a pressure but was unable to reach it within specification. The analysis will continue. At the next appropriate time, calibrate the servo valve to bring it back within specification (refer to Chapter 9).

Action:

6021-

Servo calibration failed.

Cause A:

The maximum time was exceeded before the target pressure point was reached. The nitrogen regulator may be set too low or turned off. Set the analysis gas regulator to 10 psig (0.7 bar), then resume the analysis.

Action A:

Cause B: Action B:

The analysis gas bottle is empty. Connect a new analysis gas bottle, then resume the analysis.

6022-

This file already selected for the analysis.

Cause:

You tried to choose a file for the analysis on this port which has been selected for another port. Choose a different file.

Action:

6023-

The instrument (number) is not calibrated.

Cause:

The TriStar application is in the process of initializing the instrument and is unable to locate the calibration files. Click OK. Select Unit [n] > Calibration > Load from File and select a file containing calibration data.. Click OK. Close the application and use the Setup program to reinstall calibration files.

Action A:

Action B:

Mar 08

B-37

Appendix B

TriStar II 3020

6024-

Evacuation failed.

Cause:

While attempting to zero the pressure transducers, the instrument was unable to evacuate to a pressure of less than 1 mmHg. This may be due to a leak or a bad calibration. Check the sample tube fitting and ensure that it is securely attached to the port. Use the Setup program to reinstall the calibraiton files..

Action A:

Action B:

6026-

Psat gas is not condensing.

Cause A: Action A:

The working Dewar does not contain enough bath liquid. Refill the Dewar and try the operation again.

Cause B: Action B:

The Psat gas is contaminated. Replace the Psat gas supply.

Cause C: Action C:

The Psat tubing from the regulator to the instrument is contaminated. Pump out the tubing.

6027-

There is no nitrogen attached to the unit.

Cause:

You attempted a calibration requiring nitrogen, but the software does not recognize that nitrogen is attached. Be sure that a nitrogen gas bottle is installed at one of the analysis ports, then Select Unit > Unit configuration and enter N2 for the appropriate valve.

Action:

B-38

Mar 08

TriStar II 3020

Appendix B

60286029-

The backfill gas required by this analysis is not available on this instrument. The Po gas required by this analysis is not available on this instrument.

Cause:

You attempted to start an analysis with a gas that is not connected to the instrument, or has not been designated in the software. Make sure the gas is connected to the instrument. Then select Unit [n] > Unit configuration to tell the application that the gas is connected.

Action A:

6030-

Dosing method choice is invalid. The Krypton analysis requires that Adsorptive Properties “Dosing Method” is set to “From Psat tube.”

Cause:

You selected a file for a krypton analysis that has Normal selected for the Dosing Method. Normal is for standard analyses only. Open the sample file and change the Dosing Method to From Psat tube or select a different file for the analysis.

Action:

6031-

Dosing method choice is invalid. The analysis requires that Adsorptive Properties “Dosing Method” is set to “Normal.”

Cause:

You selected a file for a standard analysis that has From Psat tube selected for the Dosing Method. From Psat tube is for krypton analyses only. Open the sample file and change the Dosing Method to Normal or select a different file for the analysis.

Action:

6038-

At least one report item must be selected. Press Cancel if you do not want a report.

Cause:

You selected a sample file on which to generate reports but there were no reports selected. Open the file and select at least one report.

Action:

Mar 08

B-39

Appendix B

TriStar II 3020

6040-

Failed to reach pressure dosing through servo. Calibration canceled.

Cause A:

There was insufficient gas pressure to calibrate for matching transducers. The gas is not connected or the tank is almost empty. Be sure the gas is connected properly and assigned correctly in the Unit Configuration dialog. Replace the tank if necessary.

Action A:

Cause B: Action B:

The gas valve is not working properly. Contact your Micromeritics service representative.

604160426043604460456047604860496050605160526053-

Servo Calibration failed. Master pressure transducer calibration failed. Offset is out of range. Port 1 pressure transducer calibraiton failed. Offset is out of range. Port 2 pressure transducer calibration failed. Offset is out of range. Port 3 pressure transducer calibration failed. Offset is out of range. 10-torr pressure transducer calibration failed. Offset is out of range. Master pressure transducer calibration failed. Scale is out of range. Port 1 pressure transducer calibration failed. Scale is out of range. Port 2 pressure transducer calibration failed. Scale is out of range. Port 3 pressure transducer calibration failed. Scale is out of range. Po pressure transducer calibration failed. Scale is out of range. 10-torr pressure transducer failed. Scale is out of range.

Cause: Action:

There is a problem with the analyzer’s calibration. Use the Setup program to reinstall the calibration files. If the problem persists, contact your Micromeritics service representative.

B-40

Mar 08

TriStar II 3020

Appendix C

C. CALCULATIONS
This appendix contains the calculations used in the TriStar program.

Saturation Pressure
Saturation pressure (Po) is selected on the Po and Temperature Options dialog. It may be entered or measured in the Po tube or on port 3. • If entered, Po = user-entered value • If measured, Po = equilibrated pressure reading after saturating Po tube or the sample tube

Relative Pressure Calculations
If Po was measured at intervals in the Po tube and several data points were collected in the interval: • For points taken before the previous Po measurement, ( Po 2 – Po 1 ) × ( T I – To 1 ) Po I = Po 1 + ----------------------------------------------------------( To 2 – To 1 ) • For points taken after the previous Po, use the previous Po: PoI = Po1 If Po was entered, use the entered Po: PoI = PoE Calculate relative pressure for the Ith data point: P1 P rel1 = ------Po I

Mar 08

C-1

Appendix C

TriStar II 3020

where PoI Po1 Po2 PoC PoE TI To1 To2 PrelI PI = saturation pressure for the Ith data point (mmHg) = most previous measured saturation pressure before Ith data point (mmHg) = first measured saturation pressure after the Ith data point (mmHg) = calculated Po = entered saturation pressure (mmHg) = time when the Ith data point was taken (minutes) = time when Po1 was measured (minutes) = time when Po2 was measured (minutes) = relative pressure for the Ith data point (mmHg) = absolute pressure for the Ith data point, taken at equilibrium (mmHg)

C-2

Mar 08

TriStar II 3020

Appendix C

Volume Adsorbed Calculations
Free Space

Measured Measured free-space volumes are calculated using the following equations: P1 V MAN - × ---- – 1 × T STD V FW = ----------T MAN P2 P 2⎞ V FC = V FW ⎛ ----⎝ P 3⎠ V FC – V FW V BATH = ----------------------T BATH 1 – ------------T AMB where: P1 P2 P3 TSTD TAMB TMAN VMAN VFC VFW VBATH TBATH = = = = = = = = = = system manifold pressure before dosing helium onto sample (mmHg) system manifold pressure after dosing helium onto sample (mmHg) sample pressure after raising Dewar and equilibrating with helium (mmHg) standard temperature (273.15 K) approximate room temperature (298 K) system manifold temperature before dosing helium onto sample (K) manifold volume (cm3) volume of free space, cold (cm3 at standard temperature) volume of free space, warm (cm3 at standard temperature) portion of cold free space at analysis bath temperature: used in non-ideality correction (cm3 at standard temperature) = analysis bath temperature (K)

Mar 08

C-3

Appendix C

TriStar II 3020

Calculated The calculated free space is determined by subtracting the gas capacity of the volume occupied by the sample from the measured free space of the empty tube. T STD V FW = V WB + ∆ V – V S × ----------T AMB T STD V FC = V CB + ∆ V – V S × ------------T BATH where VFW VFC VWB VCB ∆V VP VPB VS = = = = = = = = calculated warm free space calculated cold free space warm free space of the empty tube cold free space of the empty tube VP - VPB volume of the port used for analysis volume of the port used for the blank analysis sample mass/density

C-4

Mar 08

TriStar II 3020

Appendix C

Equilibration
Equilibration is reached when the pressure change per equilibration time interval (first derivative) is less than 0.01% of the average pressure during the interval. Both the first derivative and average pressure are calculated using the Savitzky-Golay1 convolution method for polynomial functions. The equations below are those used to compute weighted average and first derivative, respectively, for the 6th point of an 11-point window. – 36 ( P 11 + P 1 ) + 9 ( P 10 + P 2 ) + 44 ( P 9 + P 3 ) + 69 ( P 8 + P 4 ) + 84 ( P 7 + P 5 ) + 89 ( P 6 ) P AVG = ------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------429 5 ( P 11 – P 1 ) + 4 ( P 10 – P 2 ) + 3 ( P 9 – P 3 ) + 2 ( P 8 – P 4 ) + ( P 7 – P 5 ) P CHG = ---------------------------------------------------------------------------------------------------------------------------------------------------------110 P CHG P PCPI = 100% ----------P AVG where the numerical constants are from the Savitzky-Golay convolution arrays, and PAVG PCHG PPCPI PI = = = = average pressure (mmHg) change in pressure (mmHg) percent change per interval Ith pressure reading taken at equilibrium intervals (mmHg)

If a non-zero value that is too small is entered for the maximum equilibration time, the points are collected before equilibration is reached.

If PAVG is greater than 0.995 times the current Po, equilibration will not take place until the Minimum equilibration delay for P/Po 0.995 has expired, in addition to the standard equilibration criteria.

Mar 08

C-5

Appendix C

TriStar II 3020

Thermal Transpiration Correction
During data reduction, thermal transpiration correction is applied to the data if the user selected Thermal transpiration correction from the Report Options dialog. Starting with the first collected pressure, the following calculations are performed until the pressure ratio (PC/ P) is greater than or equal to 0.99. P × SD × MD 3 Y = ----------------------------------- × 10 2.33 × T
2

+G×Y ---------------------µ = 1 1+H×Y 1 F = ----------------------------------------------------2 (α × Y ) + (β × Y) + µ T ABT⎞ 0.5⎞ ⎫ ⎧ PC = ⎨ 1 – F – ⎛ F ⎛ ---------×P ⎝ ⎝ T RM ⎠ ⎠ ⎬ ⎩ ⎭ where: P SD MD T α β G H TABT TRM PC F,Y,µ = equilibrated collected pressure measured by gauge at temp TRM (mmHg) = inside diameter of sample tube (mm), from the Report Options dialog = thermal transpiration hard sphere diameter of gas (Å), from the Adsorptive Properties dialog = average temperature [TABT + TRM] / 2 (K) = Weber’s coefficient, 0.033 = Weber’s coefficient, 0.245 = Weber’s coefficient, 2.5 = Weber’s coefficient, 2 = analysis bath temperature (K), from the Po and Temperature Options dialog = room temperature (298 K) = corrected equilibrated pressure at temperature TABT (mmHg) = intermediate values for subsequent calculations

C-6

Mar 08

TriStar II 3020

Appendix C

BET Surface Area
For each point designated for surface area calculations, the BET2 transformation is calculated as follows: P rel1 B 1 = --------------------------------------------( 1.0 – P rel1 ) × N ads1 where BI is in units of g/cm3 STP. A least-squares fit is performed on the (PrelI ,BI) designated pairs where PrelI is the independent variable and BI is the dependent variable. The following are calculated: a. Slope (S g/cm3 STP) b. Y-intercept (YINT g/cm3 STP) c. Error of the slope (SERR g/cm3 STP) d. Error of the y-intercept (YIERR g/cm3 STP) e. Correlation coefficient (Cc) Using the results of the above calculations, the following can be calculated: BET Surface Area (m2/g): CSA × ( 6.023 × 10 ) SA BET = -------------------------------------------------------------------------------------------------------------------3 18 2 2 ( 22414 cm STP ) × ( 10 nm / m ) × ( S + Y INT )
23

where CSA = analysis gas molecular cross-sectional area (nm2), user-entered on the Adsorptive Properties dialog

BET C value: S + Y INT C = -----------------Y INT

Mar 08

C-7

Appendix C

TriStar II 3020

Volume of the Monolayer (cm3/g STP): 1 1 - = -----------------V M = ------------------S + Y INT C × Y INT Error of the BET Surface Area (m2/g): SA BET × ( S ERR + YI ERR ) BET ERR = -------------------------------------------------------------------Y INT + S
2 2 0.5

C-8

Mar 08

TriStar II 3020

Appendix C

Langmuir Surface Area
For each point designated for surface area calculations, the Langmuir3 transformation is calculated as follows: P relI L I = ---------N adsI where LI is in units of g/cm3 STP A least-squares fit is performed on the (PrelI, LI) designated pairs where PrelI is the independent variable and LI is the dependent variable. The following are calculated: a. Slope (S g/cm3 STP) b. Y-intercept (YINT g/cm3 STP) c. Error of the slope (SERR g/cm3 STP) d. Error of the y-intercept (YIERR g/cm3 STP) e. Correlation coefficient (Cc) Using the results of the above calculations, the following can be calculated: Langmuir Surface Area (m2/g): CSA × ( 6.023 × 10 ) SA LAN = ----------------------------------------------------------------------------------------------3 18 2 2 ( 22414 cm STP ) × ( 10 nm / m ) × S
23

where CSA = analysis gas molecular cross-sectional area (nm2), user-entered on the Adsorptive Properties dialog

Volume of the Monolayer (cm3/g STP): 1 V M = -S Langmuir b Value: b = ( Y INT ) ( V M ) Error of the Langmuir Surface Area (m2/g): SA LAN × S ERR LAN ERR = ------------------------------S

Mar 08

C-9

Appendix C

TriStar II 3020

t-Plot
For each point designated for t-Plot4 calculations, the following calculations are done: Thickness for the Ith point (Å): HP 2 t I = HP 1 × ------------------ln ( P relI ) or HJP 1 t I = -----------------------------------------HJP 2 – log ( P relI ) or t I = STSA 1 ( P rel1 ) + STSA 2 ( P rel1 ) + STSA 3
2 HJP 3 HP 3

(Halsey5)

(Harkins and Jura6)

where: tI HP1 HP2 HP3 HJP1 HJP2 HJP3 STSA1 STSA2 STSA3 PrelI = = = = = = = = = = = thickness for Ith point Halsey parameter #1 Halsey parameter #2 Halsey parameter #3 Harkins and Jura parameter #1 Harkins and Jura parameter #2 Harkins and Jura parameter #3 statistical thickness surface area parameter #1 statistical thickness surface area parameter #2 statistical thickness surface area parameter #3 relative pressure for the Ith point (mmHg)

A least-squares analysis fit is performed on the (tI, NadsI) data pairs where tI is the independent variable and NadsI is the dependent variable. Only the values of tI between tMIN and tMAX, the minimum and maximum thickness, are used. The following are calculated: a. Slope (S cm3/g-Å STP) b. Y-intercept (YINT cm3/g STP) c. Error of the slope (SERR cm3/g-Å STP)

C-10

Mar 08

TriStar II 3020

Appendix C

d. Error of the Y-intercept (YIERR cm3/g STP) e. Correlation coefficient (Cc) Using the results of the above calculations, the following can be calculated: External Surface Area (m2/g): ( S cm / g – A STP ) × ( 10 A / m ) × ( D cm liquid / cm STP ) SA EXT = ------------------------------------------------------------------------------------------------------------------------------------------------------6 3 3 F × ( 10 cm / m )
3 10 3 3

where F D = surface area correction factor, user-entered on the t-Plot Report Options dialog = density conversion factor, user-entered on the Adsorptive Properties dialog

Micropore Surface Area (m2/g): SA µ P = SA TOT + SA EXT where SATOT is the BET surface area if the user enabled the BET report exclusively, or Langmuir surface area if the user enabled the Langmuir report exclusively. If neither report has been selected, SATOT is the BET surface area value calculated using a set of default parameters. Micropore Volume (cm3 liquid/g): V µ P = ( Y INT cm / g STP ) × ( D cm liquid / cm STP )
3 3 3

Mar 08

C-11

Appendix C

TriStar II 3020

BJH Pore Volume and Area Distribution
For adsorption data, the relative pressure and volume adsorbed data point pairs collected during an analysis must be arranged in reverse order from which the points were collected during analysis. All calculations are performed based on a desorption model, regardless of whether adsorption or desorption data are being used. The data used in these calculations must be in order of strictly decreasing numerical value. Points which do not meet this criterion are omitted. The remaining data set is composed of relative pressure (Pr), volume adsorbed (Va) pairs from (Pr1, Va1) to (PrN, VaN) where (PrN = 0, VaN = 0) is assumed as a final point. Each data pair represents an interval boundary (or desorption step boundary) for intervals i=1 to i=N-1 where N = total number of (Pr, Va) pairs. Generally, the desorption branch of an isotherm is used to relate the amount of adsorbate lost in a desorption step to the average size of pores emptied in the step. A pore loses its condensed liquid adsorbate, known as the core of the pore, at a particular relative pressure related to the core radius by the Kelvin7 equation. After the core has evaporated, a layer of adsorbate remains on the wall of the pore. The thickness of this layer is calculated for a particular relative pressure from the thickness equation. This layer becomes thinner with successive decreases in pressure, so that the measured quantity of gas desorbed in a step is composed of a quantity equivalent to the liquid cores evaporated in that step plus the quantity desorbed from the pore walls of pores whose cores have been evaporated in that and previous steps. Barrett, Joyner, and Halenda8 developed the method (known as the BJH method) which incorporates these ideas. The algorithm used on the TriStar 3000 is an implementation of the BJH method.

Explanation of Terms
A pore filled with condensed liquid nitrogen has three zones: a. The core - evaporates all at once when the critical pressure for that radius is reached; the relationship between the core radius and the critical pressure is defined by the Kelvin equation. b. The adsorbed layer - composed of adsorbed gas that is stripped off a bit at a time with each pressure step; the relationship between the thickness of the layer and the relative pressure is defined by the thickness equation.

C-12

Mar 08

TriStar II 3020

Appendix C

c. The walls of the cylindrical pore - the diameter of the empty pore is required to determine the pore volume and pore area. End area is neglected.
pore

a d s o r b e d l a y e r

c o r e

wall

Insignificant compared to core length

Calculations
The volumes adsorbed (Va) are converted to the liquid equivalent volumes (V1, cm3/g): VI I = ( Va I ) ( D ) where D is the Density Conversion Factor from the Adsorptive Properties dialog. The relative pressure (Pr1) is assumed to be close to unity so that substantially all the pores in the sample are filled. The corresponding Kelvin core radius is calculated. Only pores smaller than this size will be included: –A Rc I = ---------------------------------------( 1 + F ) [ ln ( Pr I ) ] where A F = adsorbate property factor (the BJH Adsorptive Options dialog) = fraction of pores open at both ends (from the BJH Adsorption Report Options dialog or the BJH Desorption Report Options dialog); assumed to be zero for desorption

This radius will be adjusted for the thickness of the adsorbed layer during subsequent calculation steps.

Mar 08

C-13

Appendix C

TriStar II 3020

The thickness of the remaining adsorbed layer at this relative pressure is calculated: HP 2 Tw 1 = HP 1 -----------------ln ( Pr 1 ) where HP1, HP2, and HP3 are Halsey Parameters 1, 2, and 3 (respectively) from the Halsey Thickness Equation dialog. These calculations illustrate the use of the Halsey thickness equation. If the Harkins/Jura equation was selected, substitute the following wherever the thickness equation appears: HJ 1 Tw 1 = ------------------------------------HJ 2 – log ( Pr 1 ) where HJ1, HJ2, and HJ3 are Harkins-Jura Parameters 1, 2, and 3 (respectively) from the HarkinsJura Thickness Equation dialog. The following calculations (a-c) are made for each relative pressure interval based on the increment of volume desorbed during that interval. The variable I refers to the interval number, that is I=1 for the first interval from Pr1 to Pr2, and so on. J refers to each previous interval during which new pores were found. K refers to the total number of intervals in which new pores have been found. K is also the number of lines reported on the BJH table for collected data. a. The thickness of the adsorbed layer at the end of the interval is calculated as follows: HP 2 Tw I + 1 = HP 1 ----------------------ln ( Pr I + 1 )
HP 3 HJ 3 HP 3

(For the last pressure interval from the lowest PrI to zero relative pressure, TwI+1 = 0.) For the first pressure interval, there are no previously opened pores so the volume desorbed from walls of previously opened pores is zero (Vd1 = 0), and the remainder of Step (a) is skipped. The change in thickness of the wall layer due to desorption from previously opened pores is calculated: ∆ Tw = Tw 1 – Tw I + 1

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Appendix C

The annular cross-sectional area of the wall layer desorbed is calculated for all previously opened pores: CSA J = π [ ( Rc j + ∆ Tw ) – Rc j ] ( 10
2 2 – 16

cm / A )
2 2

The total volume of gas desorbed from walls of previously opened pores is calculated: Vd I =

∑ ( Lp J ) ( CSAaJ )

for all previously opened pores

where LPJ = length of previously opened pores as calculated in Step b(2). b. The physical processes occurring for this pressure interval are determined as follows: (1) If VdI is greater than the current increment of volume desorbed (VlI - VlI+1), desorption from walls only is occurring. Total surface of walls exposed thus far (cm2/g) is calculated as follows: SA W =

∑ π ( LPJ ) ( Davg ) ( 10
J

–8

cm / A ) for all previously opened pores

where DavgJ = weighted average pore diameter calculated below in Step b(2). A new layer thickness (∆Tw) that will not overcompensate for the actual volume desorbed in this interval is calculated: ( V 1 I – V 1 I + 1 ) ( 10 A / cm ) ∆ Tw = -------------------------------------------------------------SAw I
8

Since no cores are evaporated in this pressure interval, no new pores are revealed. Thus no ending Kelvin radius and average pore diameter are calculated for this interval. Note that this means the report may have fewer tabulated intervals on the collected data report than experimental pressure intervals. (2) If VdI is less than the volume increment desorbed during this interval ( Vl 1 – Vl l + 1 ) , the remaining volume is due to new pores with core evaporation taking place in this interval. K, the number of intervals with new pores exposed, is increased by 1. (For the interval from the lowest Pr1 to zero relative pressure, no new pore volume is calculated and the rest of Step b is skipped.)

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Appendix C

TriStar II 3020

The volume desorbed from newly opened pores in this interval is calculated as follows: Vc I = ( VI I – VI I + 1 ) – Vd I The Kelvin radius for the end of the interval is calculated as follows: –A Rc K + 1 = ---------------------------------------------( 1 + F ) [ ln ( Pr I + 1 ) ] All new pores opened in this interval are represented by one pore having a length-weighted average pore diameter and a corresponding length sufficient to account for the required volume of adsorbate. The weighted average pore diameter is calculated as follows: ( 2 ) ( Rc K + Rc K + 1 ) ( Rc K ) ( Rc K + 1 ) D avgK = -----------------------------------------------------------------------------2 2 Rc K + Rc K + 1 DavgK is the diameter of a pore which would have a surface area that is the average of the areas for pores radius RcK and RcK+1, if its length was the mean of the lengths at those radii. The relative pressure corresponding to is calculated as follows: P avgK = ln
–1

–2 A ---------------------------------( 1 + F ) ( D avgK )

The thickness of the adsorbed layer at this pressure is calculated as follows: HP 2 Tw avgK = HP 1 --------------------ln ( P avgK )
HP 3

The decrease in thickness of the wall layer by desorption from the walls of new pores during the lower portion of the pressure interval is calculated as follows: ∆ Td = Tw avgK – TW I + 1 The cross-sectional area of the newly opened pores is calculated as follows:
2 Davg K – 16 2 2 + ∆ Td ( 10 cm / A ) CSAc K = ---------------2

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Appendix C

The length of the newly opened pores is calculated as follows: Vc I LP K = ---------------CSAc K c. Pore diameters and radii are adjusted for the change in thickness of the adsorbed wall layer during this interval. If new pores were opened during this interval, the average diameter is adjusted by the change in layer thickness during the second portion of the desorption interval as follows: D avgKnew = D avgKold + 2 ( ∆ Td ) The layer thickness change during the whole interval is added to diameters of previously opened pores as follows: D avgJnew = D avgJold + 2 ( ∆ Tw ) (not including DavgK) The layer thickness change desorbed during this interval also is added to the radii corresponding to the ends of the pressure intervals as follows: Rc Jnew = Rc Jold + ∆ Tw for all except RcK+1. Steps a to c are repeated for each pressure interval. After the above calculations have been performed, the diameters corresponding to the ends of the intervals are calculated as follows: Dp J = 2 ( Rc J ) for all RcJ including RcK+1. The remaining calculations are based on DP(I), Davg(I), and LP(I). These calculations are only done for Davg(I) values that fall between the Minimum BJH diameter and the Maximum BJH diameter specified by the operator on the BJH Adsorption Report Options dialog or the BJH Desorption Report Options dialog. 1) Incremental Pore Volume (VpI, cm3/g): D avgI 2 16 - 10 cm 2 / A 2 Vp I = π ( Lp I ) ---------2

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Appendix C

TriStar II 3020

2) Cumulative Pore Volume (VpCUM(1), cm3/g): VP CUM( 1 ) =

∑ VpJ for ( J ≤ 1 )

3) Incremental Surface Area (SAI, m2/g): SA I = π ( LP I ) ( 10
–2

m / cm ) ( D avgI ) ( 10

– 10

m/A)

4) Cumulative Surface Area (SACUM(I), m2/g): SA CUM10 =

∑ SAJ for J ≤ 1

5) dV/dD pore volume (dV/dDI, cm3/g-A): VP I dV / dD I = ----------------------------Dp I – Dp I + 1 6) dV/dlog(D) pore volume (dV/dlog(D)I, cm3g): Dp I ⎞ dDv / d log ( D ) I = VP I / log ⎛ -------------⎝ Dp I + 1⎠ 7) dA/dD pore area (dA/dDI, m2/g-A): SA I dA / dD I = ----------------------------Dp I – Dp I + 1 8) dA/dlog(D) pore area [dA/dlog(D)I, m2/g]: Dp I ⎞ dA / d log ( D ) I = SA I / log ⎛ -------------⎝ Dp I + 1⎠

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Appendix C

For fixed pore size tables (if selected), the following calculations are performed: 1) Average Fixed Pore Size (DFavgJ, A): Dp FJ + Dp FJ + 1 DF avgJ = --------------------------------2 calculated for all intervals in the fixed pore size table. For the intervals with between the Minimum BJH diameter and the Maximum BJH diameter. 2) Cumulative Pore volume (VpFCUMI, cm3/g): VpF CUMI = INTERP ( DpF I + 1 ) where INTERP(x) is the value interpolated from the function X = DpJ+1 and Y = VPCUMJ, using an AKIMA semi-spline interpolation. 3) Incremental Pore Volume (VpFI, cm3/g): VpF I = VpF CUMI – VpF CUMI – 1 where VpFCUM0 = 0. 4) Cumulative Surface Area (SAFCUMI, m2/g): SAF CUMI = INTERP ( DpF I + 1 ) where INTERP(x) is the value interpolated from the function X = DpJ+1 and Y = SACUMJ. 5) Incremental Surface Area (SAFI, m2/g): SAF I = SAF CUMI – SAF CUMI – 1 where SAFCUM0 = 0.

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Appendix C

TriStar II 3020

6) dV/dD pore volume (dV/dDpFI, cm3/g-A)): dV / dDpF I = INTERP ( DpF I + 1 ) where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dV/dDJ. 7) dV/dlog(D) pore volume [dV/dlog(DpF)I, cm3/g]: dV / d log ( D pF I ) = INTERP ( DpF I + 1 ) where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dV/dlog(D)J. 8) dA/dD pore area (dA/dDpFI, m2/g-A): dA / dDpF I = INTERP ( DpF I + 1 ) where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dA/dDJ. 9) dA/dlog(D) pore area [dA/dlog(DpFI), m2/g]: dA / d log ( D pF I ) = INTERP ( DpF I + 1 ) where INTERP(x) is the value interpolated from the function X = DavgJ and Y = dA/dlog(D)J.

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Appendix C

Compendium of Variables
Va Vl D Pr Dp Rc A F ∆Tw Tw = quantity adsorbed expressed as a volume (cm3/g STP) = liquid equivalent volume of volume adsorbed (cm3/g) = density conversion factor from the Adsorptive Properties dialog (cm3/cm3 STP) = relative pressure = pore (or core) diameter (A) = Kelvin radius (A) of core = adsorbate property factor; from the BJH Adsorptive Options dialog = fraction of pores open at both ends; from the BJH Adsorption Report Options dialog or the BJH Desorption Report Options dialog = thickness of adsorbed layer desorbed during interval (A) = thickness of remaining adsorbed wall (A)

HP1, HP2, and HP3 are Halsey Parameters from the Halsey Thickness Equation dialog. HJ1, HJ2, and HJ3 are Harkins and Jura Parameters from the Harkins/Jura Thickness Equation dialog. STSA1, STSA2, and STSA3 are STSA parameters from the STSA Thickness Equation dialog. Vd Davg CSAa CSAc SAw ∆Td Vc Lp = = = = = = = = volume of gas desorbed from walls of previously opened pores (cm3/g) average pore diameter (A) annular cross-sectional area of the desorbed layer (cm2) cross-sectional area of opening of newly opened pores (cm2) total surface area of walls exposed (cm2/g) thickness of layer desorbed from walls of newly opened pores (A) volume desorbed from cores of newly opened pores (cm3/g) length of pore (cm/g)

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Appendix C

TriStar II 3020

Horvath-Kawazoe
A relative pressure lower limit is determined such that L-d0 never equals zero. All pressure points less than this limit are discarded. For each collected relative pressure point, values of L are chosen in an iterative manner, and the relative pressure (P/Po) determined by solving one of the following equations: • Slit Pore Geometry (original Horvath-Kawazoe) • Cylinder Pore Geometry (Saito/Foley) • Sphere Pore Geometry (Cheng/Yang)

Slit Pore Geometry (original HK)
When you use the original Horvath-Kawazoe9 method, the following equation is solved for each value of P. The value of L is determined when the solved-for relative pressure is within 0.1% of the collected absolute pressure.
4 10 4 10 K IP × 10 JA / J cm σ P σ σ σ - × ------------------------------------------------ln ------ = -----× ----------------------------– ----------------------------– -------------+ -------------4 3 9 3 9 RT Po σ × ( L – 2 × d0 ) 3 × ( L – d0 ) 9 × ( L – d0 ) 3 × d0 9 × d0 32 4 4

where K R T σ = Avogadro’s number (6.023 x 1023) = gas constant (8.31441 x 107 ergs/mole K) = analysis bath temperature (K), from an entered or calculated value on the Po and Temperature Options dialog ZS + ZA = gas solid nuclear separation at zero interaction energy (Å), ---------------2 where: ZS = sample equilibrium diameter at zero interaction energy (Å) from the Horvath-Kawazoe Physical Properties dialog ZA = zero interaction energy diameter from the Horvath-Kawazoe Physical Properties dialog d0 DA + DS ( A ) = ----------------------------2 where: DA = molecular diameter (Å) from the Horvath-Kawazoe Physical Properties dialog DS = diameter of sample atom (Å) from the Horvath-Kawazoe Physical dialog L = pore width (nucleus to nucleus) (Å)

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Appendix C

P Po IP

= equilibrium pressure (mmHg) = saturation pressure (mmHg) = interaction parameter (10-43 ergs-cm4) from the Horvath-Kawazoe Report Options dialog

Cylinder Pore Geometry (Saito/Foley)
When you use the Saito-Foley10 method, the following equation is solved for each value of P. The value of L is determined when the solved-for relative pressure is within 0.1% of the collected absolute pressure. P⎞ 3 π K IP × 10 JA / J cm - = -- ------ × -------------------------------------------------× ln ⎛ -----4 ⎝ Po⎠ 4 RT d0
32 4 4 ∞


k=0

d 0⎞ 4 ⎫ d 0⎞ 2 k ⎧ 21 ⎛ d 0⎞ 10 1 ⎛ ----------- 1 – ---- α k ---- – β k ⎛ ---- × ⎨ ----⎝ rp ⎠ ⎝ rp⎠ ⎬ k + 1⎝ rp⎠ ⎩ 32 ⎭

where K R T L P Po IP = Avogadro’s number (6.023 x 1023) = gas constant (8.31441 x 107 ergs/mole K) = analysis bath temperature (K), from an entered or calculated value on the Po and Temperature Options dialog = pore width (nucleus to nucleus) (Å) = equilibrium pressure (mmHg) = saturation pressure (mmHg) = interaction parameter (10-43 ergs-cm4) from the Horvath-Kawazoe Report Options dialog DA + DS ( A ) = --------------------------2 where: DA = molecular diameter (Å) from the Horvath-Kawazoe Physical Properties dialog DS = diameter of sample atom (Å) from the Horvath-Kawazoe Physical dialog αk βk rp = = 4.5 – k⎞ ⎛– ------------------- α , α = 1.0 ⎝ k ⎠ k–1 0 1.5 – k⎞ ⎛– ------------------- β , β = 1.0 ⎝ k ⎠ k–1 0
2 2

d0

L = radius of the cylindrical pore, -2

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Appendix C

TriStar II 3020

Sphere Pore Geometry (Cheng/Yang)
When you use the Cheng/Yang11 method, the following equation is solved for each value of P. The value of L is determined when the solved-for relative pressure is within 0.1% of the collected absolute pressure. 6 ( N 1 ε 12 + N 2 ε 22 ) L × 10 J A / J cm P-⎞ ln ⎛ -----= --------------------------------------------------------------------------------------------------3 ⎝ Po⎠ RT ( L – d )
* * 3 32 4 0 12 d 0⎞ 6 ⎛ 1 1 ⎞ ⎛ d 0⎞ ⎛ 1 1 ⎞ - T 1 + -- T 2 + -------- T + ----- -----T – ⎛ ---⎝ L ⎠ ⎝ 12 8 ⎠ ⎝ L ⎠ ⎝ 90 3 80 4⎠ 4

where R T = gas constant (8.31441 x 107 ergs/mole K) = analysis bath temperature (K), from an entered or calculated value on the Po and Temperature Options dialog DA + DS ( A ) = --------------------------2 where: DA = molecular diameter (Å) from the Horvath-Kawazoe Physical Properties dialog DS = diameter of sample atom (Å) from the Horvath-Kawazoe Physical dialog pore width (nucleus to nucleus) (Å) equilibrium pressure (mmHg) saturation pressure (mmHg) 4π L2 NS, where NS = number of sample atoms/cm2 at monolayer 4π (L - d0)2 NA, where Ns = number of gas molecules/cm2

d0

L P Po N1 N2 e*12

= = = = =

2 AS 6 × MC × α S × α A A = -------------------------------------------= ----------, where S 6 αS αA 4 dS ----- + ----χS χA 2 AA 3 × MC × α A × χ A A = ------------, where = -------------------------------------------A 6 2 4 DA

ε*22 T1

=

1 1 -----------------– -----------------3 3 (1 – S) (1 + S) 1 1 - – ----------------------------------2 2 (1 + S) (1 – S)

T2

=

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Appendix C

T3 T4

= =

1 1 - – ----------------------------------9 9 (1 – S) (1 + S) 1 1 - – ----------------------------------8 8 (1 + S) (1 – S) L – d0 where S = ------------L

Cheng/Yang Correction
This factor corrects for the nonlinearity of the isotherm. It adds an additional term to the equations for the different geometrics: P⎞ 1 ⎛ 1 ⎞ - ln ----------- = G ( L ) – 1 – -ln ⎛ -----⎝ Po⎠ θ ⎝ 1 – θ⎠ where G(L) θ = one of the Horvath-Kawazoe equations given above = degree of void filling; θ is estimated by first computing the monolayer capacity (Vm) with the Langmuir equation over the range of data points from relative pressure 0.02 to 0.2 or the maximum relative pressure included in the Horvath-Kawazoe analysis. θ is computed as the volume adsorbed over Vm.

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Appendix C

TriStar II 3020

Interaction Parameter
The interaction parameter (IP) results from the following calculations: The Kirkwood-Muller dispersion coefficients 6 × MC × α S × α A A S = -------------------------------------------αS αA ----- + ----χS χA
2

3 × MC × α A × χ A A A = -------------------------------------------2
2

where MC2 αS αA χS χA = = = = = kinetic energy of electron (0.8183 x 10-6 erg) polarizability of sample atoms (cm3) polarizability of gas molecule (cm3) diamagnetic susceptability of sample atom (cm3) diamagnetic susceptability of gas molecule (cm3)

IP = ( N A × A A ) + ( N S × A S ) where: NA NS = number of gas molecules/cm2 at monolayer from the Horvath-Kawazoe Physical Properties dialog = number of sample atoms/cm2 from the Horvath-Kawazoe Physical Properties dialog

Refer to Interaction Parameter Components later in this Appendix for recommended values.

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Appendix C

Additional Calculations Based on the previous calculations, the following can be calculated: Adjusted Pore Width (Å):
(Shell to Shell)

AL I = L I – DS Cumulative Pore Volume (cm3/g): V CUMI = V I × D where D = density conversion factor (cm3 liquid/cm3 STP) on the Adsorptive Properties dialog

dV/dD Pore Volume (cm3/g-Å): V CUMI – V CUMI – 1 dV -------- = ------------------------------------dD I AL I – AL I – 1

Median Pore Width (Å): V CUMN V HALF = -------------2 log ( D G ) – log ( D L ) D MED = 10 log ( D L ) + [ log ( V HALF ) – log ( V L ) ] × --------------------------------------------log ( V G ) – log ( V L ) where VCUMN = total cumulative pore volume (VCUMI) for points designated for HorvathKawazoe calculations VHALF = 50% of total cumulative pore volume VL = cumulative pore volume (VCUMI) for first point less than VHALF VG = cumulative pore volume (VCUMI) for first point greater than VHALF DL = pore width (LI) that corresponds to VL DG = pore width (LI) that corresponds to VG

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Appendix C

TriStar II 3020

Interaction Parameter Components
Table C-1. Interaction Parameters
Interaction Parameter Calculated Value*

Gas

Bath Temperature (K)

Sample Type

Argon

87.3

Carbon (Ross/Olivier value) Carbon (Horvath/Kawazoe value) Zeolite Carbon (Ross/Olivier value) Carbon (Horvath/Kawazoe value) Zeolite Carbon (Ross/Olivier value) Carbon (Horvath/Kawazoe value) Zeolite Carbon (Ross/Olivier value) Carbon (Horvath/Kawazoe value) Zeolite Carbon (Ross/Olivier value) Carbon (Horvath/Kawazoe value) Zeolite

2.61 5.89 3.19 4.20 9.20 5.08 4.34 9.35 5.22 4.72 9.72 5.60 2.84 6.53 3.49

Carbon Dioxide

298.15

273.15

194.65

Nitrogen

77.15

*The interaction parameter is entered in the Horvath-Kawazoe Report Options dialog in the following field: Interaction parameter: (calculated value) x 10-43 ergs-cm4 The following values were used to calculate the values in Table C-1.

Carbon-Graphite

Zeolite

DS = 3.40 NS = 3.845 x 1015 χS = 1.05 x 10-29 (Ross/Olivier) 13.5 x 10-29 (Horvath/Kawazoe, implicit) αS = 1.02 x 10-24
Nitrogen

DS NS χS αS

= = = =

3.04 3.75 x 1015 1.94 x 10-29 0.85 x 10-24

Argon

DA ΝA χA αA

= = = =

3.00 6.71 x 1014 3.6 x 10-29 1.76 x 10-24

DA ΝA χA αA

= = = =

2.95 7.608 x 1014 3.22 x 10-29 1.63 x 10-24

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Appendix C

Carbon Dioxide

DA = 3.23 NA = 4.567 x 1014 (25 ºC) 5.45 x 1014 (0 ºC) 7.697 x 1014 (-78 ºC) χA = 5.0 x 10-29 αA = 2.7 x 10-24

DA values are from van der Waal’s constant. NA values are from liquid densities. χ and α values are derived from data found in Ross and Olivier12.

The physical parameters referenced in Saito/Foley are as follows:

Aluminophosphate

Aluminosilicate

DS NS χS αS

= = = =

2.60 1.48 x 1015 1.3 x 10-29 2.5 x 10-24

DS Ns χS αS

= = = =

2.76 1.31 x 1015 1.3 x 10-29 2.5 x 10-24

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Appendix C

TriStar II 3020

Dubinin-Radushkevich
The Dubinin-Radushkevich13 equation is as follows: B × T× log Po -----log ( V ) = log ( Vo ) – -------------β P
2 2

where: V Vo Po P B β T = = = = = = volume adsorbed at equilibrium pressure (cm3/g STP) the micropore capacity (cm3/g STP) saturation vapor pressure of gas at temperature T (mmHg) equilibrium pressure (mmHg) a constant the affinity coefficient of analysis gas relative to Po gas (for this application β is taken to be 1) = analysis bath temperature (K), from the Po and Temperature Options dialog

For each point designated for Dubinin-Radushkevich calculations, the following calculations are done: LV = log (V) Po⎞ LP = log ⎛ -----⎝ P⎠
2

The intercept, log(Vo) can be found by performing a least-squares fit on the (LP,LV) designated pairs where LP is the independent variable and LV is the dependent variable. Assuming the adsorption of gas is restricted to a monolayer, Vo is the monolayer capacity. Based on this assumption, the following are calculated: a. Slope (S cm3/g STP) b. Y-intercept (YI cm3/g STP) c. Error of the slope (SERR cm3/g STP) d. Error of the y-intercept (YIERR cm3/g STP) e. Correlation coefficient (Cc)

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Appendix C

Using the results of the above calculations, the following can be calculated: Monolayer Capacity (cm3/g STP): Vo = 10YI Error of Monolayer Capacity (cm3/g STP): VoERR = Vo x (10YIERR - 1.0) Micropore surface area (m2/g): σ × Vo × ( 6.023 × 10 ) SDP = -------------------------------------------------------------------3 18 2 2 22414 cm × ( 10 nm / m )
23

where σ = molecular cross sectional area of gas (nm2) from the Adsorptive Properties dialog

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Appendix C

TriStar II 3020

Dubinin-Astakhov
The Dubinin-Astakhov equation is a follows: RTlog ( V ) = log ( Vo ) – -------β E0 where V Vo Po P T R E0 N β = = = = = = = = volume adsorbed at equilibrium pressure (cm3/g STP) the micropore capacity (cm3/g STP) saturation vapor pressure of gas at temperature T (mmHg) equilibrium pressure (mmHg) analysis bath temperature (K) the gas constant (0.0083144 kJ/mol) characteristic energy (kJ/mole) Astakhov exponent, may be optimized or user entered from the Dubinin Report Options dialog = the affinity coefficient of the analysis gas relative to the Po gas, from the Dubinin Adsorptive Options dialog
N

Po × log -----P

N

For each point designated for Dubinin-Astakhov calculations, the following calculations are done: LV = log(V) Po LP = log -----P
N

A least-squares fit is performed on the (LP,LV) designated pairs where LP is the independent variable and LV is the dependent variable. If the user selected Yes for the Optimize Astakhov Exponent prompt, a systematic search for the optimum value of N is conducted by recalculating the linear regression and selecting the value of N that gives the smallest standard error of the y-intercept. The exponent N is optimized to within 10-4. If the optimum value for N is not found in this range, an exponent of 2 is used. The following are calculated: a. Slope (S cm3/g STP) b. Y-intercept (YI cm3/g STP) c. Error of the slope (SERR cm3/g STP) d. Error of the y-intercept (YIERR cm3/g STP) e. Correlation coefficient (Cc) f. Optimized Astakhov exponent (N)

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Appendix C

Using the results of the above calculations, the following can be calculated: Monolayer Capacity (cm3/g STP): V0 = 10YI Micropore Volume (cm3/g): WI = (VI x D) where D = density conversion factor (cm3 liquid/cm3 STP) from the Adsorptive properties dialog

Limiting Micropore Volume (cm3/g): W0 = (V0 x D) where D = density conversion factor (cm3 liquid/cm3 STP) from the Adsorptive Properties dialog

Error of Limiting Micropore Volume (cm3/g): W0ERR = W0 x (10YIERR - 1.0) Characteristic Energy (KJ/mole): 2.303 × R × T E = -----------------------------------1/ N β ( 2.303 × S ) Modal Equivalent Pore Diameter (Å): D MODE where β = affinity coefficient of the analysis gas relative to the Po gas from the Dubinin Adsorptive Options dialog ⎧ 3N = 2 × ⎨ --------------⎩ 3N + 1
1/ N 3 3 3 10 nm /A ⎫ - ⎬ × --------------------------β ⋅ Eo ⎭ 1/3

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Appendix C

TriStar II 3020

Maximum Differential Pore Volume (cm3/g-Å): This value is also known as frequency of the mode12 3N + 1 dV ---------------Max = 0.5 × ( 3 N + 1 ) × W o × --------------3N dD mode Mean Equivalent Pore Width (Å): 10 nm /A --------------------------β ⋅ E0 = 2 × -------------------------------------3 N + 1 ⎛ ⎞ Γ --------------⎝ 3N ⎠
3 3 3 1/3 1/3N

β ⋅ E0 × --------------------------3 3 3 10 nm /A

1/3

3N + 1 - ⎞ × exp ⎛ – --------------⎝ 3N ⎠

D MEAN

Micropore surface area (m2/g): E0 SDA = 1000 × 2.0 × W 0 × ----k
1/3

3 N + 1⎞ × Γ ⎛ --------------⎝ 3N ⎠

Γ is calculated by a polynomial approximation over the domain 0 ≤ x ≤ 1 as follows: Γ(x+1) = 1+b1x + b2x2 + b3x3 + b4x4 + b5x5 + b6x6 + b7x7 + b8x8 + ε(x) | ε(x) | ≤ 3 x 10-7 where b1 b2 b3 b4 b5 b6 b7 b8 and where 3N + 1 -⎞ x + 1 = ⎛ --------------⎝ 3N ⎠ = = = = = = = = -0.57719 1652 0.98820 5891 -0.89705 6937 0.91820 6857 -0.75670 4078 0.48219 9394 -0.19352 7818 0.03586 8343

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Appendix C

Equivalent Pore Diameter (Å): 10 nm /A ⎞ – ⎛ --------------------------⎝ β ⋅ E0 ⎠ D i = 2 × ---------------------------------------ln ( W i ) – ln ( W 0 )
3 3 3 N 1/3N

dV/dD Pore Volume (cm3/g-Å): 10 nm /A dV -------- = 0.5 × W 0 × 3 N × --------------------------β ⋅ E0 dD i
3 3 3 N 3 3 3 N D i⎞ –( 3 N + 1 ) D i⎞ –3 N 10 nm /A ⎞ - × ⎛ ---× ⎛ ---× exp – ⎛ --------------------------⎝ β ⋅ E0 ⎠ ⎝ 2⎠ ⎝ 2⎠

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Appendix C

TriStar II 3020

MP-Method
For each point designated for MP-method14 calculations, the following calculations are done: Thickness for the Ith point (Å): HP 2 t I = HP 1 × ------------------ln ( P relI ) or HJP 1 t I = -----------------------------------------HJP 2 – log ( P relI ) where: tI HP1 HP2 HP3 HJP1 HJP2 HJP3 PrelI = = = = = = = = thickness for Ith point Halsey parameter #1 Halsey parameter #2 Halsey parameter #3 Harkins and Jura parameter #1 Harkins and Jura parameter #2 Harkins and Jura parameter #3 relative pressure for the Ith point (mmHg)
HJP 3 HP 3

(Halsey5)

(Harkins and Jura6)

With the (tI,VI) data pairs, the Akima semi-spline interpolation method is used to interpolate volume adsorbed values based on thickness values that are evenly spaced 0.2 Angstrom apart starting at the first outlier point. Outliers are defined as those points have the maximum instantaneous slope within an iteratively shrinking subset of all points. The remaining pore surface area calculation result is the slope of the line defined by two consecutive interpolated points. The slopes of each pair of consecutive points from the origin to the last point must be monotonically decreasing and non-negative. With the interpolated points set the following can be calculated: Average pore hydraulic radius (Å): tI + tI – 1 R I = ----------------2

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Appendix C

Remaining pore surface area for the Ith point (m2/g): ( V I – V I – 1 ) × ( D × 10 m / cm ) S I = -----------------------------------------------------------------------------– 10 ( t I – t I – 1 ) × 10 m / A
–6 3 3

where D = density conversion factor (cm3 liquid/cm3 STP) on the Adsorptive Properties dialog

Incremental pore surface area occluded for the Ith point (m2/g): S INCI = S I – 1 – S I Cumulative pore surface area occluded for the Ith point (m2/g): S CUMI = S INCI + S INCI – 1 + … + S INC1 dA/dR pore surface area for the Ith point (m2/g-Å): S INCI dA ------- = ----------------dR I tI – tI – 1 Incremental pore volume occluded for the Ith point (cm3/g): V INCI = ( S INCI × 10 cm / m ) × ( R I × 10
4 2 2 –8

cm /Å )

Cumulative pore volume occluded for the Ith point (cm3/g): V CUMI = V INCI + V INCI – 1 + … + V INC 1 dV/dR pore volume for the Ith point (cm3/g-Å): V INCI dV ------- = ----------------dR I tI – tI – 1

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Freundlich Isotherm
The Freundlich isotherm has the form:
1/ m Q ------ = CP Qm

where Q Qm C m = = = = quantity of gas adsorbed quantity of gas in a monolayer temperature-dependent constant temperature-dependent constant

The pressure is absolute; typically, m > 1. In terms of quantity adsorbed, Q = Q m CP
1/ m

Taking the log of both sides yields: 1 - log P log Q = log Q m C + --m

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Appendix C

Temkin Isotherm
The Temkin isotherm has the form, RTQ ------ = -------ln ( A 0 P ) q0 α Qm where Q Qm q0 A = = = = quantity of gas adsorbed quantity of gas in a monolayer the differential heat of adsorption at zero surface coverage a0 exp {-q0/RT}, where α0 and a0 are adjustable constants

In terms of quantity adsorbed, RTQ S P⎞ - ln A 0 + ln ⎛ -----Q = ------------⎝ Po⎠ q0 α Thus, the plot of the natural log of absolute pressure vs. quantity adsorbed yields a straight line with slope RTQm/q0 and intercept (ln A) RTQm/q0α.

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DFT (Density Functional Theory)
The adsorption isotherm is known to convey a great deal of information about the energetic heterogeneity and geometric topology of the sample under study. The data of physical adsorption have been used for many years as the basis for methods to characterize the surface area and porosity of adsorbents. Real solid surfaces rarely approach ideal uniformity of structure. It is accepted that in general, the surface of even a nonporous material presents areas of greater or lesser attraction for adsorbed molecules. This energetic heterogeneity greatly affects the shape of the adsorption isotherm with the result that simple theories such as the Langmuir and BET formulas can, at best, give only approximate estimates of surface area. Porous solids virtually are never characterized by a single pore dimension, but instead exhibit a more or less wide distribution of sizes. The observed adsorption isotherm for a typical material is therefore the convolution of an adsorption process with the distribution of one or more properties which affect that process. This was first stated mathematically by Ross and Olivier12 for the case of surface energy distribution and has become known as the integral equation of adsorption.

The Integral Equation of Adsorption
In a general form for a single component adsorptive, the integral equation of adsorption can be written as Q ( p ) = ∫ da db dc … q ( p, a, b, c … ) f ( a, b, c … ) where Q(p) a,b,c,... f(a,b,c,...) q(p,a,b,c,...) = = = = the total quantity adsorbed per unit weight at pressure p, a set of distributed properties, the distribution function of the properties, and the kernel function describing the adsorption isotherm on unit surface of material with fixed properties a,b,c,... (1)

Equation (1), a Fredholm integral of the first kind, is a member of a class of problems known as ill-posed, in that there are an infinite number of functional combinations inside the integral that will provide solutions. Even when the kernel function is known, experimental error in the data can make solving for even a single distribution function a difficult task. Solving for multiple distribution functions requires more data than provided by a single adsorption isotherm.

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Appendix C

Application to Surface Energy Distribution Under certain conditions, an energetically heterogeneous surface may be characterized by a distribution of adsorptive energies. The conditions are that the sample is not microporous, i.e., that adsorption is taking place on essentially a free surface with no pore filling processes at least to about 0.2 relative pressure. Secondly, that each energetically distinct patch contributes independently to the total adsorption isotherm in proportion to the fraction of the total surface that it represents. This condition is satisfied if the patches are relatively large compared to an adsorptive molecule, or if the energy gradient along the surface is not steep. In mathematical terms, this concept is expressed by the integral equation of adsorption in the following form. Q ( p ) = ∫ dε q ( p, ε ) f ( ε ) where Q(p) q(p,e) f(e) = = = the experimental quantity adsorbed per gram at pressure p, the quantity adsorbed per unit area at the same pressure, p, on an ideal free surface of energy e, and the total area of surface of energy e in the sample. (2)

The exact form of the energy-dependent term depends on the form of the model isotherms expressed in the kernel function and is provided in the model description. Application to Pore Size Distribution Similarly, a sample of porous material may be characterized by its distribution of pore sizes. It is assumed in this case that each pore acts independently. Each pore size present then contributes to the total adsorption isotherm in proportion to the fraction of the total area of the sample that it represents. Mathematically, this relation is expressed by Q ( p ) = ∫ dH q ( p, H ) f ( H ) where Q(p) q(p,H) f(H) = = = the experimental quantity adsorbed at pressure p, the quantity adsorbed per unit area at the same pressure, p, in an ideal pore of size H, and the total area of pores of size H in the sample. (3)

Numerical values for the kernel functions in the form of model isotherms can be derived from modern statistical mechanics such as density functional theory or molecular simulations, or can be calculated from one of various classical theories based on the Kelvin equation. Several types are found in the models library.

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Performing the Deconvolution
The integrations in equations (2) and (3) are carried out over all surface energies or pore sizes in the model. The functions q(p,e) and q(p,H), which we call the kernel functions, are contained in numeric form as model isotherms. Because, in general, there is no analytic solution for equation (1), the problem is best solved in a discrete form; the integral equation for any distributed property Z becomes a summation: Q(p) =

∑ q ( p, Z i ) f ( Z i )
i

(4)

Given a set of model isotherms, q(p,Z), from a model chosen from the models library and an experimental isotherm, Q(p), contained in a sample information file, the software determines the set of positive values f(Z) that most nearly, in a least squares sense, solves equation (4). The distributed property, surface energy or pore size, is then displayed on the Report Options dialog as a selection of tables or graphs. Regularization DFT allows a selectable regularization (also referred to as smoothing) constraint to be applied during the deconvolution process to avoid over-fitting in the case of noisy data or ill-fitting models. The method used is based on co-minimization of the second derivative of the distribution. The relative weight given to this term is determined by the value of the regularization parameter, which is set on the DFT Pore Size or Surface Energy dialog and also is shown in the header of reports. The value of the regularization parameter varies from zero (for no second derivative constraint) to ten (indicating a weight equal to minimizing the residuals), or even larger. When the distribution and residuals obtained change little with the value of the regularization parameter, it indicates that the chosen model provides a good representation of the data. Conversely, a large sensitivity to the regularization parameter might indicate inadequate data or a poor choice of model to represent the data.

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Appendix C

SPC Report Variables
Regressions Chart Variables
The line of best fit for the Regression Chart is calculated by the usual Least Squares methd. (Refer to BASIC Scientific Subroutines Vol II, by F.R. Ruckdeschel, Copyright 1981 BYTE Publications/McGraw Hill, p. 16.) If there is only a single point or all N points have the same x-value, there can be no line of best fit in the standard form. Σ xi XAve = -------N Σ yi YAve = -------N Σ ( x i – XAve ) ( y i – YAve ) Slope = -------------------------------------------------------------2 Σ ( x i – XAve ) The coefficient of Correlation for this line is also calculated in the usual way. (Refer to Mathematical Handbook for Scientists and Engineers, by Granino A. Korn and Theresa M. Korn, Copyright 1961, 1968 McGraw Hill, Sec. 18.4.)

σx =

Σ ( x i – XAve ) ----------------------------------N

2

σy =

Σ ( y i – YAve ) ----------------------------------N

2

Σ ( x i – XAve ) ( y i – YAve ) Cov ( x, y ) = -------------------------------------------------------------N ( x, y ) Correlation Coefficient = Cov ----------------------σx σy

Control Chart Variables

Σ yi Mean = -------N StdDev = Σ ( y – Mean ) ----------------------------------N–1
2

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-----------------CoefVar = StdDev Mean PlusNSig = Mean + n ⋅ StdDev MinusNSig = Mean – n ⋅ StdDev

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Appendix C

Summary Report
The following calculations and the results of previous calculations (as noted) are used to generate the summary report: a. Single-point Surface Area (m2/g) [ Va × ( 1 – Pr ) ] × CSA × ( 6.023 × 10 ) S 1 PT = -----------------------------------------------------------------------------------------------3 18 2 2 22414 cm STP × 10 nm / m
23

where Pr = pressure closest to 0.3 of the relative pressure points designated for surface area calculations. Va = volume corresponding to Pr b. Multipoint Surface Area See BET Surface Area Calculations c. Langmuir Surface Area See Langmuir Surface Area Calculations d. t-Plot Micropore Surface Area See t-Plot calculations e. t-Plot External Surface Area See t-Plot calculations f. BJH Cumulative Adsorption

g. BJH Cumulative Desorption h. Adsorption Total Pore Volume i. j. Desorption Total Pore Volume t-Plot Micropore Pore Volume See t-Plot calculations k. Dubinin-Radushkevich Micropore Surface Area See Dubinin-Radushkevich calculations

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l.

Dubinin-Radushkevich Monolayer Capacity See Dubinin-Radushkevich calculations

m. Dubinin-Astakhov Micropore Surface Area See Dubinin-Astakhov calculations n. Dubinin-Astakhov Micropore Volume See Dubinin-Astakhov calculations o. MP-Method Cumulative Surface Area of Pores MPSTOT = SCUMI, (see MP-method Calculations) for the last collected data point used in the MP-method Calculations, and the range of hydraulic pore radii over which the cumulative surface area was computed. p. MP-Method Cumulative Pore Volume of Pores MPVTOT = VCUMI, (see MP-method calculations) for the last collected data point used in the MP-method calculations, and the range of hydraulic pore radii over which the cumulative pore volume was computed. q. Average Pore Hydraulic Radius (A) MPV TOT –6 3 10 MP DAVER = -------------------× 10 m / cm × 10 Å/ m MPS TOT

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Appendix C

References
1. Savitzky, A. and Golay, M.J.E., Anal. Chem. 36, 1627 (1964). 2. Brunauer, S.; Emmett, P.H.; and Teller, E., J. Am. Chem. Soc. 60, 309 (1938). 3. Langmuir, I., J. Am. Chem. Soc. 38, 2267 (1916); J. Am. Chem. Soc. 40, 1361 (1918); Phys. Rev 8, 149 (1916). 4. deBoer, J.H., et al, J. Catalysis 3, 32, 38, 44, 268 (1964); J. Catalysis 4, 319, 643, 649 (1965); Cranston, R. and Inkley, F., Adv. Catalysis 9, 143 (1957). 5. Halsey, G., J. Chem. Phys. 16, 931-937 (1948). 6. Harkins, W.D. and Jura, G., J. Chem. Phys. 11, 431 (1943). 7. Kelvin, J. (published under the name of Sir William Thomson), Phil. Mag. 42, 448-452 (1871). 8. Barrett, E.P.; Joyner, L.S.; and Halenda, P.P., J. Am. Chem. Soc. 73, 373-380 (1951). 9. Horvath, G. and Kawazoe, K., J. Chem. Eng. Japan 16(6), 470 (1983). 10. Saito, A. and Foley, H.C., AlChE Journal 37(3), 429 (1991). 11. Cheng, Linda S. and Yang, Ralph T., Chemical Engineering Science 49(16), 2599-2609 (1994). 12. Ross and Olivier, J.P., “On Physical Adsorption,” J. Wiley and Sons, New York (1964). 13. Dubinin, M., Carbon 21, 359 (1983); Dubinin, M., Progress in Surface and Membrane Science 9, 1, Academic Press, New York (1975); Dubinin, M. and Astakhov, V., Adv. Chem. Ser. 102, 69 (1971); Lamond, T. and Marsh, H., Carbon 1, 281, 293 (1964); Medek, J., Fuel 56, 131 (1977); Polanyi, M., Trans. Faraday Soc. 28, 316 (1932); Radushkevich, L., Zh. fiz. Kemi. 33, 2202 (1949); Stoeckli, H., et al, Carbon 27, 125 (1989). 14. Mikhail, R., Brunauer, S. and Bodor, E., J. Colloid and Interface Sci. 24, 45 (1968).

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Appendix D

D. FREE-SPACE CORRECTION
Free space is that volume of the sample tube which is unoccupied by the sample. The quantity of gas dosed into the sample tube is calculated from the difference in pressures in the manifold before and after the dose is delivered. The quantity of gas adsorbed by the sample is calculated by subtracting the quantity of gas remaining in the free space of the sample tube after equilibrium is established from the quantity of gas originally dosed into the sample tube. Free space must be determined accurately to obtain a precise value for quantity adsorbed. Static-volumetric systems such as the TriStar consist basically of a gas manifold joined to a sample tube by an isolation valve. The manifold section has connections for an absolute pressure transducer, a temperature gauge, and a vacuum system. It also has inlets for the adsorptive gas and helium. A Dewar flask containing a cryogenic liquid (usually LN2 at approximately 77 K) is situated so that it can be raised to immerse most of the sample tube. Two temperature zones exist within the sample tube when immersed in the cryogenic bath: a warm zone (the volume above the liquid level and near ambient temperature) and a cold zone (the volume below the liquid level at cryogenic temperature). Not only must the total free-space volume be determined, but it also is necessary to determine the quantity of gas residing within the “cold” zone since a nonideality correction must be applied to only that quantity of gas. The total quantity of gas in the partly immersed sample holder cannot simply be determined using n = PV/RT because temperature is not constant over the total volume, but instead is distributed as two temperature zones with a steep temperature gradient between them. A convenient method for resolving this problem is to derive two factors which, for the existing temperature profile, can be multiplied by the prevailing pressure to reveal the molar volume of gas contained in the cold zone and the total quantity residing in the free volume of the immersed sample holder (the cold free space). The TriStar system provides the following methods for free-space determination: • Measure • Calculate • Enter

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Measure
Generally, this method, although requiring a little more time (approximately 10 minutes) is the most preferred one for determining free space. It is simple, automatic, requires very little information, and essentially is error-proof. With this method, the instrument first evacuates the manifold and sample tube (containing sample), then isolates the sample tube by closing the valve. Then the manifold is charged with helium, the pressure measured, and the valve opened allowing the helium to expand into the sample tube at ambient temperature. Again the pressure is measured. The Dewar is raised and the sample tube is cooled to cryogenic temperature. Again pressure drops; when pressure has equilibrated, the value is recorded. Warm and cold free spaces are calculated from (1) system volume, (2) system, ambient, and bath temperatures, and (3) measured pressures. From these, the value of the portion of cold free space at cryogenic temperature which requires correction for nonideality can be determined. This method may be undesirable if: • Helium is unavailable; free-space determination by the TriStar requires the use of helium • Analysis speed is a major factor; a helium free-space measurement of 10 to 15 minutes is required • Your sample tends to absorb and retain helium for a prolonged period of time or if it adsorbs helium

Calculate
This method is the most rapid and efficient way of compensating for free space. You must ensure the following is accomplished: • • • • • Perform a blank analysis on the sample tube Load the blank analysis file data into the sample tube file Indicate whether a filler rod is being used (found on the Sample Tube dialog) Enter the analysis bath temperature (foudn on the Po and Temperature dialog) Enter the sample mass and density (found on the Sample Information dialog)

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Appendix D

Enter
This method allows you to enter predetermined values for the warm and cold free spaces. The values to enter may be obtained in one of two ways: • A pre-analysis free-space calibration of the sample tube containing sample • The total free space of an empty sample tube is measured and the displacement of the sample calculated from its mass and density and subtracted from the total free space In either procedure, ensure that the level (or, in cases where the Isothermal Jacket is used, the effective level) of the cryogen bath on the sample tube is the same when the analysis is performed as it was when gathering data for free-space calculations.

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Appendix E

E. ETHERNET CONFIGURATION
Your computer and analyzer communicate by means of an ethernet connection. This appendix contains instructions for ensuring that the ethernet connection operates properly.
The sample screens shown in this appendix are Microsoft operating system screens, which may be subject to change. The screens are included for reference purposes only.

Configuring the Ethernet Port
This section contains instructions for configuring an ethernet port in either Microsoft® Windows XP Professional or Windows Vista. The instructions do not apply to any other operating system.
Depending on your desktop settings, you may have to access the dialogs in this procedure in a different manner. Refer to your Windows help system if you need assistance.

Windows XP Professional
1. Select Start > Settings > Network Connections from the Status bar at the bottom of the screen; the Network Connections dialog is displayed.

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2. Double-click the appropriate Local Area Connection, which is actually the ethernet port; the Local Area Connection Status dialog is displayed.

If no Local area connections are displayed, Windows did not detect an ethernet port. Contact your system administrator.

3. Click Properties; the Local Area Connection Properties dialog is displayed. 4. Scroll to Internet Protocol (TCP/IP) and make sure a check mark appears in the box to the left of the item. If it does not, click on the box to insert a check mark.

Make sure Internet Protocol (TCP/IP) is checked

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Appendix E

5. Select Internet Protocol (TCP/IP) to highlight it, then click Properties; the Internet Protocol dialog is displayed. 6. Click Use the following IP address, then enter the following in the IP address fields: 192 168 77 100.

After entering 77 in this field, use the right arrow key on your keyboard to advance to the next field.

7. The following numbers should display in the Subnet mask field: 255.255.255.0. If these numbers are not displayed, enter them. 8. Leave all other fields in the dialog blank. 9. Click OK to return to the Local Area Connection Properties dialog, then OK on this dialog to return to the Local Area Connection Status dialog. 10. Click Close to close the Local Area Connection Status dialog.

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Windows Vista
Depending on your desktop settings, you may have to access the dialogs in this procedure in a different manner. Refer to your Windows help system if you need assistance.

1. Select the Windows icon from the Status bar at the bottom of the screen, then select Control Panel. 2. Double-click on Network and Sharing Center; a dialog similar to this one is displayed.

Click here

3. Click Manage network connection from the Tasks list on the left side of the window, then click Local Area Connection for your analyzer on the dialog that displays. You should see a dialog similar to this one.

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Appendix E

4. Click Properties; the Local Area Connection Properties dialog is displayed.

5. Highlight Internet Protocol Version 4, then click Properties; the Internet Protocol Version 4 Properties dialog is displayed. 6. Click Use the following IP address, then enter the following in the IP address field: 192 168 77 100. Use the right arrow key to advance to the fourth field.

After entering 77 in this field, use the right arrow key on your keyboard to advance to the next field.

7. The following numbers should display in the Subnet mask field: 255.255.255.0. If these numbers are not displayed, enter them. 8. Leave all other fields in the dialog blank.

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9. Click OK to close the Internet Protocol Version 4 dialog. 10. Then click OK or the X in the upper right-hand corner of the remaining dialogs and windows to close them.

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Appendix E

Configuring the Firewall Setting
An ethernet firewall typically is enabled by default for the Windows XP and Windows Vista operating systems. Windows operating systems prior to these versions did not have firewalls. To prevent an initialization failure when running the Micromeritics software, you must turn off the firewall option between your computer and the analyzer. You must also do this for any third-party firewalls you may have installed (refer to the firewall software manual or contact your system administrator for instructions).
Depending on your desktop settings, you may have to access the dialogs in this procedure in a different manner. Refer to your Windows help system if you need assistance.

Windows XP Professional
Perform the following steps to disable the ethernet firewall for the instrument connection: 1. Select Start > Settings > Control Panel from the Status bar at the bottom of the screen; the Control Panel window is displayed. 2. Double-click the Windows Firewall icon; the Windows Firewall dialog is displayed. 3. Click the Advanced tab; a list of network connections is displayed.

4. Click the check box next to the connection assigned to your analyzer to clear the check mark, then click OK.

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Windows Vista
1. Select the Windows icon from the Status bar at the bottom of the screen, then select Control Panel. 2. Double-click on Network and Sharing Center.

Click here

3. Double-click Windows Firewall; the Windows Firewall dialog is displayed.

Highlighted green when on and red when off.

Note that the Windows Firewall statement is highlighted with green, indicating the Firewall is turned on.

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Appendix E

4. Click Change Settings; a dialog requesting permission to continue is displayed. Click Continue; the Windows Firewall Settings dialog is displayed.

5. Click the Advanced tab, then OK; a list of network connections is displayed.

6. Click the check box next to the connection assigned to your analyzer to clear the check mark, then click Apply. Click OK to close the dialog. 7. Click the X in the upper right-hand corner of the remaining associated windows to close them.

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Appendix F

F. DFT MODELS
Theories are developed by scientists in an attempt to explain a class of observed behavior. In the experimental physical sciences, theories are often expressed in terms of a model that can be visualized and described mathematically. Early models of physical adsorption were quite simple, both conceptually and mathematically, for very practical reasons — hand computations were required. Today we can explore complex models that describe adsorption systems on the atomic scale of size and sub-picosecond time frame. This is not because scientists are smarter, but because of available tools. The DFT models are created by classical approaches to adsorption as well as models based on modern statistical thermodynamics.

Models Based on Statistical Thermodynamics
Included in this group are methods that model the adsorption system in terms of forces acting between individual molecules.

Theoretical Background
Traditional adsorption theories attempt to describe experimental adsorption isotherms with an isotherm equation containing a small number of parameters. At a minimum, these parameters include the extent of the surface, such as the monolayer capacity (Vm), and the molar intensity of the gas-surface interaction, such as the Langmuir “K” constant or the BET “C” constant. In some equations, additional parameters take into account the lateral interaction of adsorbed molecules with each other. Other theories, such as the Dubinin-Astakhov approach, also include parameters for the effect of adsorbent porosity. Instead of this classical kinetic or phenomenological approach, we can use a molecular-based statistical thermodynamic theory that allows us to relate the adsorption isotherm to the microscopic properties of the system: the fluid-fluid and fluid-solid interaction energy parameters, the pore size, the pore geometry, and the temperature. The following example is given so that you may understand how such a theory is constructed. A clean sample of a solid material containing slit-shaped pores of a single width is placed in an evacuated space. It is kept at a fixed temperature as a known quantity of pure argon gas is admitted into the space surrounding the sample. The pressure within the space is recorded over time. In this situation, the pressure falls rapidly from its initial value and gradually approaches a steady reading, called the equilibrium pressure. The amount adsorbed corresponds to the quantity of gas effectively removed from the gas phase by the solid surface. A graph that plots amount adsorbed versus equilibrium pressure is called an adsorption isotherm. Under such conditions, the argon atoms that randomly enter the pore space feel the presence of the solid surface as the action of an external attractive force (the dispersion forces or Van der Waal’s forces) and spend more time near the surface. As a result, the space near the surface acquires a greater average density of argon atoms than regions farther removed.

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If the equilibrium distribution of the gas atoms near the surface could be described as a function of pressure and the molecular properties of the components of the system, then a model could be constructed for the adsorption isotherm for the system. Modern physical chemistry provides several ways to calculate this distribution. All these methods are based on the fundamental thermodynamic law that such a system adopts a configuration of minimum free energy at equilibrium. Also needed is a description of the pairwise interaction energy between atoms, U(s), commonly given by a Lennard-Jones potential:
σ -⎞ U ( s ) = ⎛ -⎝ s⎠
12 6 σ -⎞ – ⎛ -⎝ s⎠

where ε σ s = a characteristic energy of the adsorptive, = the diameter of the adsorptive molecule, and = the separation distance.

Molecular Simulation Methods
Two simulation techniques are commonly used to determine the distribution of gas molecules in a system in equilibrium: the molecular dynamics method and the Monte Carlo method. Both of these are used as reference methods because their results are considered exact. Molecular Dynamics Method In the molecular dynamics method, the position and velocity of individual gas particles are calculated over time at very short intervals. This method takes into account both the forces acting between the gas particles themselves and those acting between the gas particles and the atoms of the simulated surface. As the simulated particles collide with each other and with the surface, the average concentration of particles in the space near the surface is calculated; this calculation yields the amount of gas adsorbed. This method can be thought of as a way to determine the chronological record of the movement of each particle in the system using time steps of 10-14 seconds. Although the mathematics are simple, the number of calculations required for a system of even a few hundred particles is astronomical and challenges even the fastest computers. Monte Carlo Method In the Monte Carlo method, determination of the system equilibrium distribution begins with an assumption (which may be only approximate) about the initial configuration of particles in the system. The system is “equilibrated” through a process of randomly selecting one particle and conditionally moving it a random distance in a random direction. If the move results in a configuration of lower total energy, then the move is completed and another particle is randomly selected to be moved.

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Appendix F

If the move results in a configuration of higher energy, a probability for that event is calculated, and a random number between zero and one is generated. If the generated number is smaller than the probability of the event, then the move is accepted; otherwise, another particle is selected and the process is repeated. This process continues until the average total energy of the system no longer decreases; at this point, average configuration data are accumulated to yield the mean density distribution of particles in the system. Monte Carlo simulations require considerable less computation time than molecular dynamic simulations and can yield the same results; however, neither method provides a really practical way to calculate complete isotherms.

Density Functional Formulation
Density functional theory offers a practical alternative to both molecular dynamic and Monte Carlo simulations. When compared to reference methods based on molecular simulation, this theory provides an accurate method of describing inhomogeneous systems yet requires fewer calculations. Because the density functional theory provides accuracy and a reduced number of calculations, it is the basis embodied in the DFT models. The system being modeled consists of a single pore represented by two parallel walls separated by a distance H. The pore is open and immersed in a single component fluid (adsorptive) at a fixed temperature and pressure. Under such conditions, the fluid responds to the walls and reaches an equilibrium distribution. In this condition (by the definition of equilibrium), the chemical potential at every point equals the chemical potential of the bulk fluid. The bulk fluid is a homogenous system of constant density; its chemical potential* is determined by the pressure of the system using well-known equations. The fluid near the walls is not of constant density; its chemical potential is composed of several position-dependent contributions that must total at every point to the same value as the chemical potential of the bulk fluid. As noted previously, at equilibrium, the whole system has a minimum (Helmholtz) free energy, known thermodynamically as the grand potential energy (GPE). Density functional theory describes the thermodynamic grand potential as a functional of the single-particle density distribution; therefore, calculating the density profile that minimizes the GPE yields the equilibrium density profile. The calculation method requires the solution of a system of complex integral equations that are implicit functions of the density vector. Since analytic solutions are not possible, the problem must be solved using iterative numerical methods. Although calculation using these methods still requires supercomputing speed, the calculation of many isotherm pressure points for a wide range of pore sizes is a feasible task. The complete details of the theory and the mathematics can be found in the papers listed under References at the end of this appendix. The following graphs and accompanying text illustrate the results of using density functional theory to predict the behavior of a model system.

*Chemical potential may be thought of as the energy change felt by a probe particle when it is inserted into the system from a reference point outside the system. It can also be defined as the partial derivative of the grand potential energy with respect to density (or concentration).

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Appendix F

TriStar II 3020

Figure F-1 shows the density profile for argon at a carbon surface as calculated by density functional theory for a temperature of 87.3 K and a relative pressure of about 0.5.

Figure F-1. Density Profile for Argon on Carbon at 87.3 K and a Relative Pressure of 0.5 This figure represents a cross-section of the region near the surface. Note the layerwise distribution of adsorbate; the first monolayer is sharply defined and a third layer can be distinguished. The area under the profile curve represents the amount adsorbed per unit area at this pressure. The positions of the maxima are separated by a distance determined by the size of the adsorptive atom. Given the density profile, the amount adsorbed at the stated pressure can be easily calculated as the integral over the profile. Repeating this calculation over a range of pressures yields the adsorption isotherm for the model. If the value of H is very large, the isotherm obtained corresponds to that of an external, or free, surface. If H is smaller, a range of pressures is reached where two minima exist for the grand potential, showing the presence of two metastable phases having different density distributions but the same chemical potential. The phase with the lower GPE is the stable one. As the pressure is increased, a point is reached where the other phase becomes the stable one. This phase transition reflects condensation of adsorbate in the pore; the pressure at which it occurs is called the critical pore-filling pressure. This pressure is analogous to the condensation pressure predicted by the Kelvin equation in the classical model of pore filling. Figure F-2 shows how the profiles change with pressure for a model pore with H = 40 Angstroms. The insets show the density profiles for the corresponding points of the isotherm.

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TriStar II 3020

Appendix F

Figure F-2. Model Isotherm for Argon at 87.3 K in a 40 Å Slit in a Carbon Substrate The profiles show the density distribution from one wall to the center of the slit; the other half of the distribution is a mirror image of the profile shown. As the pressure is first increased from zero, almost all the adsorbed atoms occupy a position close to the surface. • Inset a shows the profile corresponding to point a on the isotherm where the surface is about half covered. • At point b, the first layer is so full that it is more favorable for atoms to start a new layer. • At point c, a third layer is forming. Point c, for this size slit, is the critical pore-filling pressure. In inset c, the profile shows the density decreasing to near zero (actually the bulk gas density) at 4 or 5 molecular diameters from the surface. • Inset d shows the profile converging on a density similar to that of bulk liquid argon in the center of the pore, indicating a phase transition. Note that the adsorption isotherms for pores larger than the one shown in Figure F-2 is identical up to point c. The lower branch of the isotherm simply continues to a higher pressure for larger pores. This trend is illustrated in Figure F-3, where isotherms for some larger size pores are shown. It is clear that pore size is uniquely characterized by a corresponding critical porefilling pressure. At large pore sizes, density functional theory produces results for the critical filling pressures that are in good agreement with those produced by the Kelvin equation.

Mar 09

F-5

Appendix F

TriStar II 3020

Figure F-3. Model Isotherms for Some Larger Pore Widths Argon on Carbon at 87.3 K Figure F-4 shows model isotherms for pores in the micropore size range. Note the logarithmic scale for pressure.

Figure F-4. Model Isotherms in the Micropore Size Range of Pore Width Argon on Carbon at 87.3 K

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Appendix F

Pores of 4 Å width, barely larger than the argon atom (3.38 Å), fill at pressures below 1 millitorr. Pores below 15 Å fill before a monolayer is completed on the surface of the larger pores. In the micropore size range, the pore volume fills more gradually with pressure and the total shape of the isotherm is important in characterizing the pore size.

Models Included

Non-Local Density Functional Theory with Density Independent Weights N2 - DFT Model AR - DFT Model Geometry: Substrate: Category: Method: Slit Carbon (graphite) Porosity Nitrogen at 77 K; Argon at 87 K

Using the methods of non-local density functional theory, two sets of isotherms have been calculated to serve as kernel functions for the characterization of porous solids from adsorption data. The model isotherms are stored in binary format files. These models assume a slitlike pore geometry. The pore size range from 4.0 to 4000 Å is covered in 91 classes in a geometric progression. The class intervals are rounded to the nearest 0.02 molecular diameters. A model for the free or external surface is included to account for unfilled pores. Each of the 92 model isotherms has been calculated at 181 pressure points from near 1x10-6 to near 1.00 relative pressure. These models are identical to those supplied with the original DOS version of DFT software. Some slight difference from the DOS results may be noted when they are applied to the same data due to improvements in the deconvolution algorithm and better regularization of the current software. Modified Non-Local Density Functional Theory with Density-Dependent Weights N2 - Modified Density Functional Geometry: Substrate: Method: Free surface Surface energy Nitrogen at 77K

Using the modified Tarazona prescription described by Olivier (refer to References, references 3 and 4), model isotherms were calculated for a wide range of adsorptive energies to a relative pressure of 0.6. The model makes no provision for pore filling in the micropore region. If the sample solid contains small mesopores, the isotherm data should be truncated (using the Select Data Points dialog box) to a suitably low relative pressure to avoid trying to fit this region; mesopore filling reports as a large area of low energy in the calculated distribution of adsorptive potential.

Mar 09

F-7

Appendix F

TriStar II 3020

The surface energy is reported in terms of the effective Lennard-Jones interaction parameter, e, for the adsorptive/adsorbent pair divided by Boltzmann’s constant. The units are therefore degrees Kelvin. N2 - Cylindrical Pores - Oxide Surface AR - Cylindrical Pores - Oxide Surface Geometry: Substrate: Category: Method: Cylinder Oxide Porosity Nitrogen at 77 K; Argon at 87 K

Model isotherms were calculated using a combination of statistical mechanical calculations and experimental observations for macroporous silicas and MCM-41 mesoporous silicas as well as zeolites. The pore-filling pressures were determined as a function of the pore size from adsorption isotherms on MCM-41 materials characterized by X-ray and other techniques. The variation of the pore fluid density with pressure and pore size has been accounted for by density functional theory calculations. The N2 model reports pore sizes ranging from 3.8 to 387 Angstroms and the AR model from 3.8 to over 500 Angstroms. Reference: M. Jaroniec, M. Kruk, J.P. Olivier, and S. Koch, “A New Method for the Accurate Pore Size Analysis of MCM-41 and Other Silica-Based Mesoporous Materials,” Proceedings of COPS-V, Heidelberg, Germany (1999)

N2 – Cylindrical Pores – Pillared Clay Surface (Montmorillionite) Geometry: Substrate: Category: Method: Cylinder Crystalline Silicate Porosity Nitrogen at 77 K

Model isotherms were calculated using a combination of statistical thermodynamic NonLocal Density Functional Theory (NLDFT) calculations and experimental isotherms for reference samples of montmorillionite.The construction method for the hybrid models was analogous to that described in the first reference below (Jaroniec et al,1999). The additional references add additional theoretical details as well as examples of the application of the model to pillared clay catalysts.This model reports pore widths from 3.8 to 387 Angstroms.

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Appendix F

References:

Mietec Jaroniec, Michal Kruk, James P. Olivier and Stefan Koch, “A New Method for the Characterization of Mesoporous Silicas,” Proceedings of COPS-V, 1999, Studies in Surface Science, Vol 128, Characterization of porous Solids V , Unger, et al, Eds, Elsevier, Amsterdam, 2000. James P. Olivier and Mario L. Occell, “Surface Area and Microporosity of a Pillared Interlayered Clay (PILC) from a Hybrid Density Functional Theory (DFT) Method,” The Journal of Physical Chemistry B; 2001, 105(3), 623-629. M. L. Occelli, J. P. Olivier, J. A. Perdigon-Melon, and A. Auroux, “Surface Area, Pore Volume Distribution, and Acidity in Mesoporous Expanded Clay Catalysts from Hybrid Density Functional Theory (DFT) and Adsorption Microcalorimetry Methods,” Langmuir 2002, 18, 9816-9823.9b James P. Olivier, “The Importance of Surface Heterogeneity in Developing Characterization Methods.” 6th International Symposium on the Characterization of Porous Solids, Studies in Surface Science and Catalysis 144, Elsevier, 2002. James P. Olivier and Mario L. Occelli, “Surface Area and Microporosity of Pillared Rectorite Catalysts from a Hybrid Density Functional Theory Method,” Microporous and Mesoporous Materials 2003, 57, 291-296.

C02 - DFT Model Geometry: Substrate: Category: Method: Slit Carbon Porosity Carbon dioxide at 273 K

Model isotherms were calculated, using the non-local prescription of Tarazona, employing molecular parameters derived from the known bulk properties of carbon dioxide.

AR - Modified Density Functional Model Geometry: Substrate: Category: Method: Free Surface Any Surface energy Argon at 87 K

This model was produced in the same manner as the N2 Modified Density Functional model listed earlier, except applicable to argon adsorbed at 87.3 K.

Mar 09

F-9

Appendix F

TriStar II 3020

N2 - Tarazona NLDFT, Esf = 30.0K Geometry: Substrate: Category: Method: Cylinder Oxide Porosity Nitrogen at 77 K

Model isotherms were calculated using the prescriptions of Tarazona for density dependent weighting functions and a cylindrical pore geometry. The wall potential used is /k = 30 K, typical for a silica or alumina surface. This model file is particularly useful for sizing zeolites or zeolite containing materials that have substantial micropore volume. The reported pore size range is 3.8 to 387 Angstroms. Reference: P. Tarazona, Phys. Rev. A 31: 2672 (1985). Idem, Phys. Rev. A 32: 3148 (1985). P. Tarazona, U. M. B. Marconi, and R. Evans, Mol. Phys. 60: 573 (1987).

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Appendix F

Models Based on Classical Theories
Both surface energy distribution and pore size distribution may be evaluated using classical approaches to model kernel functions for use with equation (1) of the DFT Theory in the calculations appendix. Be aware that the deconvolution method only provides a fitting mechanism; it does not overcome any inherent shortcomings in the underlying theory.

Surface Energy
The use of classical theories to extract adsorptive potential distribution is mostly of historical interest. At a minimum, the equation must contain a parameter dependent on adsorption energy and another dependent on monolayer capacity, or surface area. This is sufficient to permit the calculation of the set of model isotherms that is used to create a library model. The Langmuir equation has been used in the past, as have the Hill-deBoer equation and the Fowler-Guggenheim equation. All of these suffer from the fact that they only describe monolayer adsorption, whereas the data may include contributions from multilayer formation.

Pore Size
It is well established that the pore space of a mesoporous solid fills with condensed adsorbate at pressures somewhat below the prevailing saturated vapor pressure of the adsorptive. When combined with a correlating function that relates pore size with a critical condensation pressure, this knowledge can be used to characterize the mesopore size distribution of the adsorbent. The correlating function most commonly used is the Kelvin equation. Refinements make allowance for the reduction of the physical pore size by the thickness of the adsorbed film existing at the critical condensation pressure. Still further refinements adjust the film thickness for the curvature of the pore wall. The commonly used practical methods of extracting mesopore distribution from isotherm data using Kelvin-based theories, such as the BJH method, were for the most part developed decades ago and were designed for hand computation using relatively few experimental points. In general, these methods visualize the incremental decomposition of an experimental isotherm, starting at the highest relative pressure or pore size. At each step, the quantity of adsorptive involved is divided between pore emptying and film thinning processes and exactly is accounted for. This computational algorithm frequently leads to inconsistencies when carried to small mesopore sizes. If the thickness curve used is too steep, it finally will predict a larger increment of adsorptive for a given pressure increment than is actually observed; since a negative pore volume is non-physical, the algorithm must stop. Conversely, if the thickness curve used underestimates film thinning, accumulated error results in the calculation of an overly large volume of (possibly nonexistent) small pores. The use of equation (1) represents an improvement over the traditional algorithm. Kernel functions corresponding to various classical Kelvin-based methods have been calculated for differing geometries and included in the list of models.

Mar 09

F-11

Appendix F

TriStar II 3020

Models Included

Kelvin Equation with Halsey Thickness Curve

N2 - Halsey Thickness Curve Geometry: Substrate: Category: Method: Slit Average Porosity Nitrogen at 77 K

The kernel function is calculated using the Halsey equation with standard parameters:
– 5.00 ⎞ 1/3 ---------------------t = 3.54 ⎛ ⎝ ln ( P /Po )⎠

The nitrogen properties used in the Kelvin equation are: Surface tension = 8.88 dynes cm-1 Molar density = 0.02887 g cm-3

N2 - Halsey Thickness Curve Geometry: Substrate: Category: Method: Cylinder Average Porosity Nitrogen at 77 K

The calculation is the same as above except that cylindrical geometry is assumed. Reference: G. Halsey, J. Chem. Phys 16, 931 (1948)

Kelvin Equation with Harkins and Jura Thickness Curve

N2 - Harkins and Jura Thickness Curve Geometry: Substrate: Category: Method: Slit Average Porosity Nitrogen at 77 K

The kernel function is calculated using the Harkins and Jura equation with standard parameters:

F-12

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TriStar II 3020

Appendix F

1/2 13.99 -⎞ t = ⎛ -------------------------------------------⎝ 0.034 – log ( P / Po )⎠

The nitrogen properties used in the Kelvin equation are: Surface tension = 8.88 dynes cm-1 Molar density = 0.02887 g cm-3

N2 - Harkins and Jura Thickness Curve Geometry: Substrate: Category: Method: Cylinder Average Porosity Nitrogen at 77 K

The calculation is the same as above except that cylindrical geometry is assumed. References: W. D. Harkins and G. Jura, J.A.C.S. 66, 1366 (1944) J. H. DeBoer et al., J. Colloid and Interface Sci. 21, 405 (1966) Kelvin Equation with Broekhoff-de Boer Thickness Curve

N2 - Broekhoff-de Boer Model Geometry: Substrate: Category: Method: Slit Average Porosity Nitrogen at 77 K

The kernel function is calculated using the Broekhoff-de Boer equation with standard parameters: The nitrogen properties used in the Kelvin equation are: Surface tension = 8.88 dynes cm-1 Molar density = 0.02887 g cm-3

N2 - Broekhoff-de Boer Model Geometry: Substrate: Category: Method: Cylinder Average Porosity Nitrogen at 77 K

Mar 09

F-13

Appendix F

TriStar II 3020

The calculation is similar to the above except that cylindrical geometry is assumed, and the film thickness depends on pore size (see reference). Reference: Specifically, equations 20 and 21 in: J.C.P. Broekhoff and J.H. de Boer, “The Surface Area in Intermediate Pores,” Proceedings of the International Symposium on Surface Area Determination, D.H. Everett, R.H. Ottwill, eds., U.K. (1969)

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TriStar II 3020

Appendix F

References
The papers listed below provide additional information on DFT models: 1. “Determination of Pore Size Distribution from Density Functional Theoretic Models of Adsorption and Condensation within Porous Solids,” J.P. Olivier and W.B. Conklin, Micromeritics Instrument Corp; presented at the International Symposium on the Effects of Surface Heterogeneity in Adsorption and Catalysts on Solids, Kazimierz Dolny, Poland (July 1992). 2. “Classification of Adsorption Behavior: Simple Fluids in Pores of Slit-shaped Geometry,” Perla B. Balbuena and Keith E. Gubbins, Fluid Phase Equilibria, 76, 21-35, Elsevier Science Publishers, B.V., Amsterdam (1992). “Modeling Physical Adsorption on Porous and Nonporous solids Using Density Functional Theory,” J.P. Olivier, Journal of Porous Materials, 3, 9-17 (1995). “The Determination of Surface Energetic Heterogeneity Using Model Isotherms Calculated by Density Functional Theory,” J.P. Olivier; presented at the Fifth International Conference on the Fundamentals of Adsorption, Pacific Grove, CA (1995).

3.

4.

Mar 09

F-15

TriStar II 3020

Appendix G

G. MAINTAINING HIGH PURITY GASES
The TriStar was designed to measure accurately the surface area of all types of materials. It is important that the gases (nitrogen or helium) used for these measurements be of highest purity, especially when analyzing low surface area samples. Three ways to ensure high purity gases are to always maintain: • thoroughly purged gas pressure regulators • non-permeable gas lines • leak-free connections Impure gas is strongly indicated, for example, if a series of measurements on a low surface area material yields decreasing specific surface areas with decreasing quantities of sample. The TriStar uses very small amounts of helium; therefore any residual air in the regulator can distort results of subsequent analyses for quite some time. Micromeritics offers the following suggestions to assist you in maintaining high purity gases (particularly helium) for the TriStar. • Use metal gas lines only • Remove trapped air from the regulator and gas lines

Using Metal Gas Lines
You should always use metal gas lines which have been carefully cleaned of any oils and greases used in the manufacturing process. Do not use plastic or rubber gas lines. When these types of permeable, nonmetallic gas lines are used with helium, contaminants accumulate at a much faster rate. This causes errors in analysis results and can also contaminate a clean sample.

Removing Trapped Air
When connecting the regulator to the gas bottle, air is unavoidably trapped on the high- and low-pressure sides of the regulator, as well as in the gas lines. You should remove as much of this air as is possible before opening the gas bottle valve. If this air is allowed to remain in the regulator, it will mix with the helium and cause inaccurate results in subsequent analyses. Or if the valve is open for any length of time, the air trapped on the high pressure side may diffuse back into the gas bottle and contaminate its entire contents. There are two methods for removing trapped air from the regulator lines: the Purge Method and the Evacuation Method.

Mar 08

G-1

Appendix G

TriStar II 3020

Purge Method This is the preferred method for removing trapped air. 1. Select Unit > Enable manual control (if the instrument schematic is not displayed, select Show
instrument schematic). If you have multiple TriStars installed, make sure you choose the correct Unit menu.

2. Close all valves.

3. Open the regulator Shut-off valve. 4. Open the gas bottle valve briefly and allow the regulator to be charged with gas until the highpressure gauge reads just over half the tank pressure; then quickly close the valve.
High-Pressure gauge Regulator Shut-off valve Gas Bottle valve

Pressure Control knob

5. Using the Pressure Control knob, set the output pressure (gas bottle pressure gauge) to 15 psig. 6. Loosen the fitting at the helium inlet (on the rear panel of the TriStar) until the low pressure side drops to approximately 3 psig (0.02 MPa), then tighten the fitting.

G-2

Mar 08

TriStar II 3020

Appendix G

7. Repeat steps 4, 5, and 6 three times. 8. Briefly open the gas bottle valve; then, using the Pressure Control knob, reset the regulator output pressure to 15 psig. 9. After the pressure has stabilized (indicating there are no leaks), open the gas bottle valve. Evacuation Method
To use this method, your gas tank must be within 10 feet of the instrument.

1. Do one of the following:
If... Then...

The regulator has not Close the gas bottle valve. been filled with gas and Open the regulator Shut-off valve. the gas line is attached to the instrument: The regulator is filled with gas: Close the gas bottle valve. Open the regulator Shut-off valve. Loosen the helium inlet fitting (or nut) on the rear panel of the instrument. Allow all of the gas in the regulator to expel from the line (pressure reading will be zero). Retighten the helium inlet fitting (or nut). 2. Select Unit > Enable manual control (if the instrument schematic is not displayed, select Show
instrument schematic). If you have multiple TriStars installed, make sure you choose the correct Unit menu.

Mar 08

G-3

Appendix G

TriStar II 3020

3. Close all valves; then open valves 6, 7, and 10.

Open valves 6, 7, and 10

4. Allow evacuation to continue for 20 minutes. This pulls a vacuum on the helium line to the gas bottle. The manifold pressure transducer should fall close to zero.
Be sure to allow evacuation for a full 20 minutes. If evacuation time is too short, trapped air may remain in the lines.

5. Close valves 6, 7, and 10.

G-4

Mar 08

TriStar II 3020l

Index

INDEX

$ symbol, 8-11

A
Absolute pressure dosing, 5-22, 5-28 Absolute pressure tolerance, 5-20 Accessories, ordering, 10-1 Add log entry, 8-9 Add Log Entry push button, 5-7 Adding an analyzer, 4-9 Adsorbate property factor, 5-59 Adsorption isotherm, F-1 Adsorptive properties file, 5-28 creating, 3-10 listing statistics, 3-33 printing contents, 3-31, 5-94 Adsorptive push button BJH report, 5-58 Dubinin report, 5-76 Advanced format, 5-5, 8-2 sample defaults, 8-6 sample information file, 3-14, 8-3 All file status, 2-12 Alpha-S curve, 5-92 Alpha-S report, 5-52 Alumina, replacing in oil vapor traps, 9-11 Analysis Dewar, 3-25 Dewar, checking, 9-4 performing, 3-27, 6-3 QuickStart method, 3-29, 6-8 Analysis conditions file, 5-15 creating, 3-9 listing statistics, 3-33 printing contents, 3-31, 5-94 Analysis Preparation dialog, 5-22 Analysis program, 1-5 exiting, 5-99 installing upgrade, 4-8 installling, 4-1 uninstalling, 4-20 using, 2-6 Analyzer adding another, 4-9 changing ethernet connection, 4-17 cleaning, 9-4 configurations, 6-23 electrical, 1-9 maintaining, 9-3

moving from one computer to another, 4-11 physical dimensions, 1-9 removing from computer, 4-16 schematic, 6-14 turning on/off, 2-5 weight and dimensions, 1-9 Analyzing file status, 2-12 AR Cylindrical Pores - Oxide Surface model, F-8 AR DFT model, F-7 AR Modified Density Functional Model, F-9 Astakhov report, 5-75 Autoscale, 5-63 Autoscale x- and y-axis, 5-43 Avogadro's number, C-22 Axis coordinates, viewing, 7-28 properties, editing, 7-27 Axis Properties dialog, 7-27

B
Backfill gas, 5-27 options, 5-27 Basic format, 8-4 sample file defaults, 8-10 sample information file, 3-16, 5-8 BET surface area report, 5-39 calculations, C-7 example of, 7-31 BJH Adsorption/Desorption report, 5-57 calculations, C-12 examples of, 7-34 plot options, 5-62 tabular options, 5-60 BJH Adsorptive Options dialog, 5-58 Blank analysis, 5-11, 6-12 Boltzmann’s constant, F-8 Bookmarks tab, 2-17 Broekhoff-de Boer thickness curve, 5-49 Browse push button, 2-10

C
Calibrate Pressure Offset dialog, 6-27 Calibration, 6-27, 9-29 information, 6-23 match transducers, 6-28, 9-30

Jul 09

Index-1

Index

TriStar II 3020

servo valve, 6-28, 9-30 zero pressure, 6-27, 9-29 Calibration command, 6-27 Calibration file loading, 6-30 reinstalling, 4-19 saving, 6-29 Cancel push button, 6-7 Carbon Black STSA thickness curve, 5-49 Catalysts, 5-19 Cautions, defined, 1-3 Check box, 2-10 Chemical potential, F-3 Cheng/Yang calculations, C-25 correction, 5-65 Pore Geometry, C-24 Cleaning analyzer, 9-4 Dewars, 9-4 Close All command, 5-93 Close command, 5-93 Close push button, 2-11 Close Reports command, 7-5 CO2 DFT Model, F-9 Cold free space, 5-11, 5-24 Collected data, 5-87 Columns, editing on onscreen reports, 7-24 Comments window, 8-9 Complete file status, 2-12 Components and Connectors, 2-1 front panel, 2-1 rear panel, 2-4 sample compartment, 2-2 side panel, 2-3 Computer requirements, 1-9 Control Chart command, 7-11 Control Chart dialog, 7-11 Control Chart Graph Options dialog, 7-12 Control Chart report, 7-11 defining the Y-axis, 7-12 recalculating archived results, 7-13 Control Chart Sample Selection dialog, 7-13 Conventions, used in operator’s manual, 1-3 Convert command, 5-98 Convert StarDriver Sample Files dialog, 5-98 Cross hair, axis, 7-28 Cross-references, 2-20 Curve Properties dialog, 7-26

D
Data collected, 5-87

entered, 5-87 exported, 5-96 selecting display options, 8-12 Date Range push button, 2-12 Defaults for sample information files, 8-6 parameter files, 8-6 Restricted sample information file, 8-6 Degas Conditions dialog, 5-13 Degas conditions file, 5-13 defining, 3-8 listing statistics, 3-33 printing contents, 3-31, 5-94 Degassing units, 1-6 ordering, 10-1 Density conversion factor, 5-29 Density Functional theory, F-3 Destination, 5-94 Dewar checking, 9-4 cleaning, 9-4 installing, 3-25 precautions, 3-25 DFT models, F-1 See Models DFT Pore Size Report Options dialog, 5-71 DFT report Pore size, 5-71 surface energy, 5-74 DFT Surface Energy Report Options dialog, 5-74 Diagnostics gas line test, 9-24 leak test, 9-16 Diagnostics command, 6-24 Dialog boxes, using, 2-8 Directory navigating to a different, 2-13 parameter files, 8-15 Dollimore-Heal Adsorption/Desorption report, 5-64 example of, 7-36 Dose increment, 5-20, 5-21 Dose Increment Edit dialog, 5-21 Dose Increments dialog, 5-21 Drop-down list, 2-10 Dubinin Adsorptive Options dialog, 5-76 Dubinin report, 5-75 calculations, C-30 pore volume options, 5-79 tabular options, 5-77 Transformed isotherm plot, 5-78 types available, 5-76 Dubinin Report Options dialog, 5-79 Dubinin Tabular Report Column Options dialog, 5-77 Dubinin Transformed Isotherm Plot Options dialog, 5-78

Index-2

Jul 09

TriStar II 3020l

Index

Dubinin-Astakhov calculations, C-32 Dubinin-Radushkevich calculations, C-30

E
Edit push button, 5-46 Edit Quantities Adsorbed dialog, 7-16 Elevator manual control options, 6-16 screw, 9-2 Enable Manual Control command, 6-14 Entered data, 5-87 Entered file status, 2-12 Entered Pressures dialog, 5-16 Environment conditions, 1-9 Equation Broekhoff-de Boer, 5-49 Carbon Black STSA, 5-49 Halsey, 5-48 Harkins and Jura, 5-49 Kruk-Jaroniec-Sayari, 5-48 Equation push button, 5-81 Equilibration calculations, C-5 interval, 5-27 push button, 5-26 Error messages, B-1 2400 series, B-1 2500 series, B-12 4000 series, B-18 6000 series, B-34 Ethernet configuring port for Vista, E-4 configuring port for XP, E-1 disabling a firewall, E-7 switch, connecting, 4-9 Evacuation options, 5-22 Exit command, 5-99 Exiting the analysis program, 5-99 Export format, 5-97 Export command, 5-96 Export Sample File dialog, 5-96 Export Settings dialog, 6-5 Exporting sample files, 3-34, 5-96

File menu, 5-1 Close All command, 5-93 Close command, 5-93 Convert command, 5-98 Exit command, 5-99 Export command, 5-96 List command, 5-95 Open command, 5-3 Print command, 5-94 Save All command, 5-93 Save command, 5-91 File name default extensions, 2-14 included as part of ID, 8-7 sequence, 8-10 Filler rod, 5-12, 5-33 cleaning, 3-18 Find command, 2-21 Firewall disabling for Windows Vista, E-8 disabling for Windows XP, E-7 Fixed dose, 5-19 Format of exported data, 5-97 Forms, A-1 f-Ratio report, 5-55 Free space, D-1 calculated method, 5-24, D-2 calculations, C-3 cold, 5-24 entered method, 5-24, D-3 measured method, D-2 warm, 5-24 Free Space dialog, 5-23 Freundlich report, 5-42 calculations, C-38 Freundlich Report Options dialog, 5-42 Front Panel, 2-1 Function keys See Shortcut keys

G
Gas, 1-8 connecting, 9-19 disconnecting depleted bottle, 9-19 guidelines for connecting to analyzer, 9-19 hazardous, 9-19 line, clean and verify, 9-24 maintaining high purity, G-1 selecting, 6-23 specifying port location, 9-28 toxic, 9-21

F
File printing to, 7-4 selecting, 2-11 statistics, 3-33 status, 2-12

Jul 09

Index-3

Index

TriStar II 3020

Graph copying as metafile, 7-27 editing onscreen, 7-25 grid lines, 8-13 legend, editing, 7-27 Graph Grid Lines command, 8-13 Graph Grid Lines dialog, 8-13 Graph overlay, 3-35 for multiple graphs, 3-38 for multiple samples, 3-35 Graph Overlay Samples dialog, 5-33 Graphic, appearing in report title, 5-32 Grid lines, 8-13

data, exporting, 5-96 report options, 5-37 Isotherm collection dose increments, 5-20 target pressures, 5-16 Isotherm report, 5-37 example of, 7-30 Isothermal jacket, 5-12

K
Kernel function, F-11, F-12 Kruk-Jaroniec-Sayari Thickness Equation, 5-48

H
Halsey thickness curve, 5-48 Harkins and Jura thickness curve, 5-49 Heat of Adsorption dialog, 7-15 Heat of Adsorption report, 7-15 Help menu, 2-24 How-To videos, 2-15 Horvath-Kawazoe calculations Cylinder pore geometry (Saito/Foley), C-23 Slit pore geometry (original HK), C-22 Sphere pore geometry (Cheng/Yang), C-24 Horvath-Kawazoe Physical Properties dialog, 5-66 Horvath-Kawazoe Plot Options dialog, 5-69 Horvath-Kawazoe report, 5-65 calculations, C-22 plot options, 5-69 tabular options, 5-69 Horvath-Kawazoe Report Options dialog, 5-65 How-To videos, 2-15

L
Langmuir surface area report, 5-39 calculations, C-9 Leak test, 5-23 performing, 9-16 Legend Properties dialog, 7-27 Lennard-Jones, F-2, F-8 Links, 2-19 List command, 5-95 List, generating, 5-95 Live Graph command, 8-14 Local area connection, E-2 Log entry, 5-7 Log Report settings, 6-22 Low surface area sample, analyzing, G-1

M
Maintenance, system, 9-1 Manual control, 6-14 accessing shortcut menu, 6-14 enabling, 6-14 Maximum BJH diameter (or radius), 5-58 Maximum volume increment, 5-19 MCM-41 materials, F-8 Menu bar, 2-23 Menu structure, 2-23 Mesoporous materials, 5-19 Metafile, copying graphs as, 7-27 Minimum BJH diameter (or radius), 5-58 Models, F-1 AR Cylindrical Pores - Oxide Surface, F-8 AR DFT model, F-7 AR Modified Density Functional, F-9 based on classical theories, F-11 based on statistical thermodynamics, F-1 CO2 DFT Model, F-9 N2 Broekhoff-de Boer Model, F-13

I
Increment, maximum volume, 5-19 Index, online, 2-20 Insert Predefined Pressures dialog, 5-18 Insert Pressure Range dialog, 5-17 Insert Quantity Range dialog, 7-16 Installation videos, 2-15 Instrument log, 6-2, 6-21 Instrument schematic manual control, 6-14 showing, 6-17 Interaction parameter, C-26 IP address entering, Windows Vista, E-5 entering, Windows XP, E-3 Isosteric heat of adsorption, 7-15 Isotherm, F-1 collecting, 5-15

Index-4

Jul 09

TriStar II 3020l

Index

N2 Cylindrical Pores - Oxide Surface, F-8 N2 Cylindrical Pores - Pillared Clay Surface, F-8 N2 DFT model, F-7 N2 Halsey Thickness Curve, F-12 N2 Harkins and Jura Thickness Curve, F-12, F-13 N2 Harkins and Jura Thickness Curve model, F-12 N2 Modified Density Functional, F-7 N2 Tarazona NLDFT, Esf = 30.0K, F-10 Molecular dynamics, F-2 Molecular simulation methods, F-2 Monolayer capacity, 5-42 Monte Carlo, F-2 Montmorillionite, F-8 Moving an analyzer to another computer, 4-11 MP-Method report, 5-80 calculations, C-36 plot options, 5-83 tabular options, 5-82 types available, 5-81 MP-Method Tabular Report Column Option dialog, 5-82

Options menu, 8-1 Graph Grid Lines command, 8-13 Live Graph command, 8-14 Option presentation command, 8-2 Parameter Files Directory command, 8-15 Sample Defaults command, 8-6 Service Test Mode command, 8-15 Units command, 8-12 Options report, 5-85 Ordering information, 10-1 O-ring, replacing port, 9-6 Outgas test, 5-24 Overlay samples, 5-39 Overlays push button, 5-33

P
Parameter File Directory Selection dialog, 8-15 Parameter files, 5-4 default values, 3-1 defining, 3-6 listing statistics, 3-33 printing contents, 3-31, 5-94 specifying location, 8-15 Parameter Files Directory command, 8-15 Parameters, user, 8-8 Parts, ordering, 10-1 Pass/Fail Options dialog, 5-36 Password, restricted format, 8-5 Po and T dialog, 5-25 collected data, 5-89 Po and T push button, 5-25 Po and Temperature Options dialog, 5-25 Po tube, on schematic, 6-16 Po value, 6-4 Pore filling pressure, F-4 Pore Geometry cylinder (Saito-Foley), C-23 slit (original Horvath-Kawazoe), C-22 sphere (Cheng/Yang), C-24 Pore size, F-11 Preparation push button, 5-22 Prepared file status, 2-12 Preparing file status, 2-12 Presentation options, 8-2 Pressure offset, 6-27 relative, calculations, C-2 table, 5-16 target, 5-16 tolerance, 5-20 Preventive maintenance schedule, 9-3 Print command, 5-94 Printing file contents, 3-31

N
N2 Broekhoff-de Boer model, F-13 N2 Broekhoff-de Boer Model model, F-13 N2 Cylindrical Pores - Oxide Surface model, F-8 N2 Cylindrical Pores - Pillared Clay Surface model, F-8 N2 DFT model, F-7 N2 Halsey Thickness Curve model, F-12 N2 Harkins and Jura Thickness Curve model, F-13 N2 Modified Density Functional model, F-7 N2 Tarazona NLDFT, Esf = 30.0K model, F-10 Next push button, 6-7 nk, 5-11 No analysis file status, 2-12 Non-ideality factor, 5-12, 5-29 Notes, defined, 1-3

O
Oil vapor trap, replacing alumina, 9-11 Online manual cross references, 2-20 index, 2-20 printing options, 2-22 using, 2-17 See also Operator’s manual Open command, 5-3 Open Report command, 7-5 Operator, specifying, 8-7 Operator’s manual conventions, 1-3 online, 2-17 Option Presentation command, 8-2

Jul 09

Index-5

Index

TriStar II 3020

Psat vs t push button, 5-29 Push button, 2-9 Browse, 2-10 Close, 2-11 Date Range, 2-12 Equilibration, 5-26 Free Space, 5-23 Overlays, 5-33 Po and T, 5-25 Preparation, 5-22 Psat vs t, 5-29 Replace, 2-10 Save, 2-10 Skip, 6-6 Suspend, 6-6

Q
QuickStart command, 6-8

R
Radio button, 2-10 Radushkevich report, 5-75 Ramp rate, 5-14 Ranges, valid, 2-9 Rear panel, 2-4 Reference thickness curve, 5-47 Regression report, 7-7 recalculaing SPC values, 7-8 selecting X- and Y-Axes variables, 7-8 Regression Report command, 7-7 Regression Report dialog, 7-7 Regression Report Sample Selection dialog, 7-8 Regularization, 5-72 Relative pressure tolerance, 5-20 Removing an analyzer, 4-16 Replace All pushbutton, 5-7 Replace push button, 2-10 Report Alpha-S method, 5-52 BET Surface Area, 5-39 BJH Adsorption/Desorption, 5-57 closing, 7-5 Control Chart, 7-11 displaying company logo in title, 5-32 Dollimore-Heal, 5-64 Dubinin, 5-75 examples, 7-29 f-Ratio method, 5-55 generating, 7-3 graphs, editing onscreen, 7-25 header, 7-19 Heat of Adsorption, 7-15

Isotherm, 5-37, 7-30 Langmuir surface area, 5-39 legend, editing, 7-27 onscreen, 7-19 onscreen, shortcut menus for, 7-24 opening, 7-5 Options, 5-85 Regression, 7-7 Sample log, 5-85 saving in other formats, 7-22 selecting, 2-13 Statistical Process Control (SPC), 7-6 Summary, 5-35 Tabular options, 5-60 Tabular, editing onscreen, 7-24 Tool bar, 7-20 t-Plot, 5-46 types available, 5-34 Validation, 5-86 zoom feature, 7-28 Report button, 7-10 Report options file, 5-31 creating, 3-12 listing statistics, 3-33 printing contents, 3-31, 5-94 Report Relative Pressure Table dialog, 5-40 Reports menu, 7-1 Close Reports command, 7-5 Control Chart command, 7-11 Open report command, 7-5 Regression Report command, 7-7 SPC Report Options command, 7-6 Start Report command, 7-3 Restricted format, 8-5 Sample information file, 3-16, 5-10 Resume push button, 6-7

S
Saito-Foley calculations, C-23 Pore Geometry, C-23 Sample degassing, 3-23 entering density, 8-11 low surface area, G-1 weighing, 3-21 Sample Analysis command, 6-3 Sample Backfill Options dialog, 5-27 Sample compartment, 2-2 Sample defaults, 8-6 Advanced format, 3-1, 8-6 Basic format, 3-4, 8-10 Sample Defaults command, 8-6

Index-6

Jul 09

TriStar II 3020l

Index

Sample Defaults dialog Advanced format, 8-6 Basic format, 8-10 Sample file name, specifying default sequence, 8-6 Sample information dialog Advanced format, 5-5 Basic format, 5-8 Restricted format, 5-10 Sample information file, 5-4 Advanced format, 5-5 Basic format, 5-8 creating in Advanced format, 3-14 creating in Basic format, 3-16 defaults, restricted format, 8-10 exporting, 3-34, 5-96 listing statistics, 3-33, 5-95 printing contents, 3-31, 5-94 Restricted format, 5-10 Sample log report, 5-85 example of, 7-38 Sample ports location, 2-2 replacing O-rings, 9-6 Sample tube cleaning and labeling, 3-18 file, 5-11 installing, 3-24 on schematic, 6-16 replacing O-ring, 9-7 Sample Tube dialog, 5-11 Sample tube file, 5-11 creating, 3-6 listing statistics, 3-33 printing contents, 3-31, 5-94 Save All command, 5-93 Save As command, 5-91 Save as Default push button, 7-14 Save command, 5-91 Save push button, 2-10 Schematic, 6-14 Select Calibration File dialog, 6-29 Select Dates dialog, 2-12 Selecting files, 2-11 reports, 2-13 Service Test command, 6-30 Service Test mode, 8-15 Servo valve calibrating, 6-28 settings, 6-15 Servo Valve dialog, 6-28 Setup program, 4-6 adding an analyzer, 4-9 moving an analyzer to another computer, 4-11

reinstalling analysis program, 4-8 reinstalling calibration files, 4-19 removing an analyzer from the computer, 4-16 uninstalling software, 4-20 Shortcut keys, 2-6 for Select Dates dialog, 2-12 list of, 2-7 Shortcut menu, 2-6 for graphs, 7-25 for instrument schematic, 6-14 for tabular reports, 7-24 Show Instrument Log command, 6-21 Show Instrument Schematic command, 6-17 Show Status command, 6-19 Side panel, 2-3 Skip push button, 6-6 SmartPrep, 3-23 SmartPrep Degasser, 1-6 Soak temperature, 5-14 time, 5-14 Software installing, 4-1 installing upgrade, 4-8 uninstalling, 4-20 using, 2-6 using for other functions, 4-6 SPC report, 7-6 Control chart, 7-11 Regression, 7-7 user parameters, 5-6, 8-8 SPC Report Options command, 7-6 SPC Report Options dialog, 7-6 Specifications, 1-8 Spreadsheet format exporting isotherm data, 5-96 saving reports, 7-22 StarDriver files, converting, 5-98 Start push button, 6-7 Start Report command, 7-3 Start Report dialog, 7-3 Status list, 7-4 Status window, 6-19 STSA thickness curve, 5-49 Submitter, specifying, 8-7 Subnet mask entering, Windows Vista, E-5 entering, Windows XP, E-3 Summary report, 5-35 calculations, C-45 example of, 7-37 Surface area correction factor, 5-50 Surface Energy, F-11 Surface Energy report, 5-74

Jul 09

Index-7

Index

TriStar II 3020

Suspend push button, 6-6 System installation videos, 2-15 System valves, 6-15

T
Table of Contents, online, 2-19 Tarazona, F-7 Target pressure, 5-16 Temkim Report Options dialog, 5-44 Temkin report, 5-44 calculations, C-39 Temperature soak, 5-14 specifications, 1-9 Text, copy graph data as, 7-27 Thermal transpiration correction, 5-33 calculations, C-6 Thermodynamic law, F-2 Thickness curve, 5-46, 5-57 Broekhoff-de Boer, 5-49 Carbon Black STSA, 5-49 Halsey, 5-48 Harkins and Jura, 5-49 Reference, 5-47 user-defined, 5-47 Thumbnails tab, 2-22 Title Properties dialog, 7-27 Tool bar, reports window, 7-20 t-Plot report, 5-46 calculations, C-10 example of, 7-33 Transducer match, 6-28 offset, 6-27 TriStar description, 1-4 specifications, 1-8 See also Analyzer Troubleshooting, 9-1

Unit Configuration command, 6-23 Units command, 8-12 Units Selections dialog, 8-12 Units, selecting, 8-12 Use calculation assignments, 5-88 User parameters, 5-6 specifying, 8-8

V
Vacuum seal type, 5-12 Vacuum pump, 1-5 changing or adding oil, 9-8 inspecting oil level, 9-8 replacing alumina in oil vapor trap, 9-11 replacing exhaust filter, 9-15 Validation report, 5-86 Valves failure, 9-1 system, 6-15 Van der Waal force, F-1 Videos, 2-15

W
Wall potential, F-10 Warm free space, 5-11, 5-24 Warnings, defined, 1-3 Weighing sample, 3-21 Windows tile and cascade, 2-24 Windows menu, 2-24

X
X-axis order by, 7-12

Z
Zero pressure calibration, 6-27 Zoom feature, 7-28

U
Unit configuration, 6-23 Unit menu, 6-1 Calibration command, 6-27 Diagnostics, 6-24 Enable Manual Control command, 6-14 QuickStart command, 6-8 Sample Analysis command, 6-3 Service Test command, 6-30 Show Instrument Log command, 6-21 Show Instrument Schematic command, 6-17 Show Status command, 6-19

Index-8

Jul 09

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