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VERTEX 70v

User Manual

1007253

1st edition 2007, publication date November 2007

2007 BRUKER OPTIK GmbH, Rudolf Plank Str. 27, D-76275 Ettlingen, www.brukeroptics.com

All rights reserved. No part of this manual may be reproduced or transmitted in any form or by any means including printing, photocopying, microfilm, electronic systems etc. without our prior written permission. Brand names, registered trademarks etc. used in this manual, even if not explicitly marked as such, are not to be considered unprotected by trademarks law. They are the property of their respective owner.

The following publication has been worked out with utmost care. However, Bruker Optik GmbH does not accept any liability for the correctness of the information. Bruker Optik GmbH reserves the right to make changes to the products described in this manual without notice.

This manual is the original documentation for the VERTEX 70v spectrometer.

T.ABLE . OF. .C.ONTENTS . . . . . . . . . . . . . . . . . ..... .. . .........


1 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 Warning Labels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 Safety Instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

2 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 3 Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 Delivery Scope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 Site Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9 Connecting VERTEX 70v to the Power Supply . . . . . . . . . . . . . . . . . . . 11 Connecting VERTEX 70v to a PC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 Connecting VERTEX 70v to the Vacuum Pump . . . . . . . . . . . . . . . . . . 13 Connecting VERTEX 70v to the Purge Gas Line . . . . . . . . . . . . . . . . . . 15

4 Overview. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . External Components. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Internal Components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Optical Path . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19 20 25 29

5 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Switching VERTEX 70v On and Off . . . . . . . . . . . . . . . . . . . . . . . . . . . . QuickLock. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Automatic Accessory Recognition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Performing a Measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Evacuating and Venting the Spectrometer. . . . . . . . . . . . . . . . . . . . . . . Optimizing the Vacuum Operation of the Spectrometer. . . . . . . . . . . . . Purging the Spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Exchanging the Beamsplitter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Exchanging the Detector . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Cooling an MCT Detector. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31 31 33 35 35 36 40 43 46 50 52

6 Maintenance and Repair . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57


General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Evacuating the MCT Detector Dewar. . . . . . . . . . . . . . . . . . . . . . . . . . . Replacing the Laser Module. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Replacing a defective IR Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Replacing the Fuses. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
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Ta b l e o f C o n t e n t s
Replacing the Sample Compartment Windows . . . . . . . . . . . . . . . . . . . 69 Cleaning the Instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73 Maintaining the Vacuum Pump . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

7 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75 Diagnostic Means. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 76 Problem - Possible Cause - Solution . . . . . . . . . . . . . . . . . . . . . . . . . . . 85

A Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101 B Consumable Spares . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103 C Default Parameter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 105 D Dimensional Drawings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 109 E Connecting VERTEX 70v to PC . . . . . . . . . . . . . . . . . . . . . . 115
General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Possible Connection Topologies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Selecting Network Addresses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Assigning Network Addresses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Checking the Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115 116 119 120 123

F Electronics and Power Supply . . . . . . . . . . . . . . . . . . . . . . . 125


Electronics Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125 Power Supply Panel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 128

G Firmware Update . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131


General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Updating the Firmware . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Restoring a previous Firmware Version . . . . . . . . . . . . . . . . . . . . . . . . Backing up the current Firmware Version . . . . . . . . . . . . . . . . . . . . . . 131 132 134 135

H Sample Preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137


General Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 137 Sample Preparation Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 139

Service Addresses. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 145

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VERTEX 70v User Manual

S. A.F. E.T. Y. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
GENERAL INFORMATION
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Read the following safety instructions carefully before putting the spectrometer into operation. Keep this manual in a suitable place for future reference. Always observe the instructions described in this manual to ensure user safety and to avoid property damage. Improper use or failure to follow these safety instructions can result in serious injuries and/or property damage. Any non-observance of the precautions will infringe the intended use (i.e. performing spectroscopic measurements) of the spectrometer. In this case Bruker Optik GmbH will not assume any liability. It is the operators duty to plan and implement all necessary safety measures and to supervise their observance. Moreover, the operator must ensure that the spectrometer is in proper functioning condition. A safe and faultless operation can only be guaranteed if the spectrometer is transported, stored, installed, operated and maintained properly according to the procedures described in this manual. Never remove or deactivate any supporting safety systems during spectrometer operation. Ensure that objects and/or material not required for the measurement is out of the spectrometer operating area. The spectrometer complies with the IEC/EN 61010-1 safety regulations.

Protective Earthing
To avoid personal injuries and/or property damage caused by electrical power, the spectrometer is equipped with a safety plug. Connect this plug only to a socket outlet with earthing contact. Make sure that the socket complies with IEC (International Electrotechnical Commission).

Qualified Personnel
Primary installation and all maintenance and repair works not described in this manual should only be performed by Bruker service personnel. Only authorized operating personnel that have been briefed about the spectrometer operation and all relevant safety aspects should operate and maintain (i.e. only maintenance works that are described in this manual) the spectrometer. All repairs, adjustments and alignments on any spectrometer component must be performed in accordance with the safety regulations and standards applied in the country in which the instrument is installed.
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Correct Usage

SAFETY Warning Labels

The spectrometer and its components should only be used according to the instructions described in the manual or advised by a Bruker engineer. In case of accessories or components made by other manufacturers and used in connection with the spectrometer, Bruker does not assume any liability for safe operation and proper functioning.

WARNING LABELS

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When operating the spectrometer you have to observe a number of safety instructions which are highlighted by various warning labels. This section describes the warning labels and explains their meaning. All warning labels on the spectrometer must always be kept legible. Immediately replace a worn or damaged label. The following warning labels indicate different dangerous situations which may be caused by improper use of the spectrometer.

Caut ion - Ge ne ral H azar d


This warning symbol indicates general hazard. Observe the safety instructions and follow the precautions described to avoid personal injury and/or property damage.

Caution - Electrical Shock


This warning symbol indicates electrical hazard. The symbol is located near live parts or on enclosures behind which are live parts that represent an accidental contact hazard. Never touch these parts. Before removing the corresponding compartment covers and beginning any maintenance or repair work, first turn off the mains switch and unplug the main power cable. Ensure that all live parts do not come into contact with a conductive substance or liquid. Non-observance of these safety instructions can cause severe personal injury and/or property damage.

Caution - Hot Surface


This warning symbol indicates components and surfaces which can become very hot during spectrometer operation. Do not touch these components and surfaces. Risk of skin burn! Be careful when operating near hot components and/or surfaces.

Caution - Laser Radiation


This warning symbol indicates the existence of laser radiation. Never look directly into the laser beam or use any kind of optical instruments to do so. Otherwise permanent eye damage can be the result.

VERTEX 70v User Manual

SAFETY Warning Labels

Caution - Frostbite
This warning symbol indicates cryogenic materials (e.g. liquid nitrogen) required to operate the spectrometer (e.g. cooling detector). Skin contact with these liquids or cooled components causes severe frostbite. Always handle the liquids with utmost care. Observe the safety instructions for handling of cryogenic liquids.

Caution - Ha rmful Material


This warning symbol indicates the existence of harmful or irritant material (e.g. the window material BaF2). Observe the safety instructions on the packaging, and the safety data sheets attached. Non-observance may cause personal injury.

Caution - Toxic Material


This warning symbol indicates the existence of toxic material (e.g. the window material KRS-5). Observe the safety instructions on the packaging, and the safety data sheets attached. Non-observance may cause severe personal injury or even death.

Besides the dangers described above, there can also be hazardous situations caused by the sample material. Depending on the type of hazardous substances you work with, you have to observe specific substance-relevant safety instructions. Put on the corresponding warning label on the appropriate spectrometer position. The label must be legible and permanently discernible. The following list contains some examples of hazardous substances:

Caution - Infectious Material


This warning symbol indicates the possible presence of bio-hazardous and infectious material. When working with this kind of material always, observe the prevailing laboratory safety regulations and take all necessary precautions and disinfection measures (e.g. wearing protective clothing, masks, gloves etc.). Failure to do so may cause severe personal injury or even death. (For information on how to use, dilute and efficiently apply disinfectants, refer to the Laboratory Biosafety Manual: 1993 by WHO - World Health Organization.)

Caution - Radioactive Material


This warning symbol indicates the possible presence of radioactivity. When working with radioactive material, always observe the safety regulations and take all necessary protective measures (e.g. wearing protective clothing, masks gloves etc.). Failure to do so may cause severe personal injury or even death.

VERTEX 70v User Manual

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SAFETY Safety Instructions

Caution - Corrosive Substance


This warning symbol indicates the possible presence of corrosive substances. When working with corrosive substances, always observe the laboratory safety regulations and take protective measures (e.g. wearing protective masks and gloves). Failure to do so may cause severe personal injury or even death.

Waste Disposal
Dispose all waste produced (chemicals, infectious and radioactively contaminated substances etc.) according to the prevailing laboratory regulations. Detergents and cleaning agents must be disposed according to the local waste regulations.

SAFETY INSTRUCTIONS

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The following chapters describe all relevant safety aspects of the spectrometer operation. Depending on the degree of hazard the safety instructions are classified as follows: Danger indicates that death, severe personal injury or substantial property damage WILL result if proper precautions are not taken. indicates that death, severe personal injury or substantial property damage CAN result if proper precautions are not taken. indicates that minor personal injury or property damage CAN result if proper precautions are not taken. draws your attention to particularly important information on the product, e.g. product operation or to a special part of the manual.

Warning

Caution

Note

The safety instructions Danger, Warning and Caution stand out by the corresponding warning labels.

VERTEX 70v User Manual

G. E .N. E.R. A.L. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

VERTEX 70v is an evacuable, fully digital FT-IR spectrometer for demanding R&D applications. The spectrometer is equipped with a number of features such as AAR (Automatic Accessory Recognition) ACR (Automatic Component Recognition) and PerformanceGuard that facilitate performing spectroscopic measurements and ensure reliable measurement results. The function AAR identifies automatically the accessory installed in the sample compartment, performs several tests and loads automatically the corresponding experiment file including the pre-defined measurement parameters. The feature ACR recognizes automatically the currently installed optical components like source, detector and beamsplitter. These components are electronically coded so that the spectrometer firmware can recognize them. This information is passed on to the application software OPUS. The purpose of ACR is to enable the user to select the right optics parameters in OPUS. In addition, the spectrometer components are monitored permanently to ensure that they operate within the specification range. This feature is called Performance Guard. Its purpose is to facilitate fault diagnostics and maintenance. The data acquisition is based on a free running delta-sigma, dual-channel A/D converter with 24-bit dynamic range. The A/D converter is integrated into the detector preamplifier electronics. The DigiTect technology ensures a signal transmission free from interferences and guarantees the highest signal-to-noise ratio. VERTEX 70v can be controlled by any data system (PC workstation, notebook etc.) on which the operating system Microsoft Windows and the spectroscopic software OPUS is installed. The Ethernet connection provides the possibility to control the spectrometer also via your intranet or the internet. The standard spectrometer configuration is designed for data acquisition in the mid IR region. Optionally, VERTEX 70v can be equipped with additional optical components to cover the whole spectral range - starting in the far infrared or THz region at 10cm-1 up to the ultraviolet region at 28,000cm-1. Due to the pre-aligned optical components and the permanently aligned RockSolid interferometer, the spectral range can be changed easily. If you work with the advanced spectrometer configuration (i.e. two detector positions and two source positions are available inside the spectrometer) you can select them using the software. Removable vacuum-tight covers provide access to the detector and beamsplitter if you want to exchange these components. VERTEX 70v has five IR-beam outlet ports (on the right, front and left side) and two IRbeam inlet ports (on the right and rear side) allowing the connection of a multitude of optional accessories and/or components like: TGA-coupling PMA 50 (Polarization Modulation Accessory for VCD and PM-IRRAS) HYPERION 1000/2000 IR microscope and HYPERION 3000 imaging microscope with FPA detector (Focal Plane Array detector system) IMAC module (Imaging Accessory with FPA detector)
VERTEX 70v User Manual 5

GENERAL

External sample compartment (XSA) HTS-XT module (High Throughput Screening Extension) Fiber optic coupling module with MIR or NIR fiber probes for solid and liquid samples FT Raman module (e.g. RAM II) FIR bolometer External, water-cooled sources There is also the possibility to connect several accessories simultaneously (e.g. a water-cooled Hg-arc source at the rear side, the RAM II FT-Raman module at the right side, a fibre optics coupling at the right front side, the HYPERION IR microscope at the left side and a bolometer detector at the front side). Diagnostic routines help to maintain optimum instrument status and performance. The internal validation unit (IUV) is located inside the spectrometer. It contains standards (test samples) used for the validation and testing of the instrument. Note: Depending on the spectrometer configuration you have ordered, your spectrometer may not include all options that are described in this manual. The evacuable VERTEX 70v spectrometer allows measurements under vacuum conditions, i.e. unwanted atmospheric interferents (e.g. water vapor or carbon dioxide) are eliminated nearly completely from the spectrometer interior. Evacuating the spectrometer is more efficient than purging it or using desiccant cartridges. The result of an optimal measurement under vacuum conditions is an IR spectrum in which no H2O or CO2 absorptions mask weak spectral features of the sample. The spectrometer design enables a separate evacuation of the spectrometer compartments, i.e. either the complete spectrometer interior (sample compartment plus the optical bench) or only the optical bench can be evacuated. Vacuum shutters (so called flaps), which can be equipped with optical or IR windows, allow a ventilation of only the sample compartment in order to preserve the vacuum in the rest of the optics compartment during a sample exchange or an accessory installation. Evacuating and venting the sample compartment and/or optics are computer-controlled. Moreover, the spectrometer is equipped with two pressure sensors providing for the display of the current pressure inside the spectrometer optics and/or sample compartment. VERTEX 70v is supplied with an efficient vacuum pump that can evacuate the spectrometer optics within a few minutes. The oil-free vacuum pump prevents the spectrometer optics from being contaminated by hydrocarbons.

VERTEX 70v User Manual

I.N .S. TA. L .L.A .T.I.O .N. . . . . . . . . . . . . . . . . . . . . . .. . . .


GENERAL INFORMATION
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Unpacking and initial installation of VERTEX 70v is done by Bruker service engineers. The operating company has to provide an installation site that meets the site requirements described in this chapter. (See also the technical document Installation Requirements for VERTEX 70v provided by Bruker Optik GmbH in advance.) This chapter contains a list of the standard as well as the optional spectrometer components and describes the procedures for connecting the spectrometer:

to the power supply, to a PC, to the vacuum pump and to the purge gas supply line, if necessary.

For detailed information about how to install the computer, refer to the PC manual.

DELIVERY SCOPE

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The basic instrument of VERTEX 70v allows upgrading with additional components and/ or accessories. The delivery scope depends on the spectrometer configuration you have ordered.

Standard Components
The basic instrument includes the following items:

VERTEX 70v spectrometer (including the user manual) Power cord PC compatible data system (if desired, the PC can also be provided by the
customer)

Data cable (Cat5, crossover cable for 10Base-T Ethernet standard) Purge gas hose (OD: 6mm, length: approx. 5m) Tool kit (slot-head screw driver, cross-head screwdriver and hex keys of several
sizes, sample preparation tools, 3x spare fuses, IR sensor card, metallic cap shown in fig. 28)

Software package OPUS/IR (including the OPUS Reference Manual)

VERTEX 70v User Manual

INSTALLATION Delivery Scope

For installing the vacuum pump, the following items are included:

Vacuum pump (including the user manual) Noise reduction hood Vibration absorber 2x flexible metal hoses 4x hose clamps 4x sealing rings

Optional Components
Depending on the ordered spectrometer configuration, the delivery scope can also include following optional components:

Optional spectrometer components (e.g. optional detectors) and/or accessories Optional OPUS software packages (e.g OPUS/STEP) including the corresponding
manuals

Inspecting the Packaging


After the receipt of the spectrometer, inspect the packaging for damages. If there are any signs of damage, contact your local shipping representative before opening the shipping box. Warning: Do not put a spectrometer into operation that shows signs of damage. Failure to do so may result in severe personal injuries and/or property damage.

Transportation
Due to its weight (about 105kg), VERTEX 70v has to be carried by at least four persons using the supplied transport handles. For transportation purposes, attach these handles properly to the right and left spectrometer side as shown in figure 1 using 12 screws (M5 x 16). Tighten the screws using a hex kex (size 4mm). After having transported the instrument to the desired place, you can remove the transport handles again. Alternatively, you can transport the instrument with a fork lifter. Warning: Due to the high instrument weight, improper transportation can lead to personal injuries and/or spectrometer damage.

VERTEX 70v User Manual

INSTALLATION Site Requirements

Transport Handles

Figure 1: Installing the Transport Handles

SITE REQUIREMENTS
Space Requirements

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The spectrometer dimensions are 85cm (w) x 71cm (d) x 32cm (h). (For exact spectrometer dimensions refer to appendix D.) At the rear side, the spectrometer requires a clearance of at least 25cm (10). The spectrometer should be placed on a stable and horizontal base. Note that the basic instrument has a weight of about 105kg. When preparing the installation location for the spectrometer, take into consideration that the mains power supply connection is easily accessible at any time. The mains power supply can be interrupted, for example, either by disconnecting the safety plug or switching off the mains switch on the spectrometer rear side or disconnecting the primary power receptacle.

Environmental Requirements
To ensure optimum spectrometer performance and long-term reliability the following environmental conditions are essential: Temperature Range: 18 - 35 C (64 - 95 F)

In case the vacuum pump is operated with installed noise reduction hood ensure the ambient temperature does not exceed 32C (90F). Humidity (non-condensing): 80% (relative humidity) Temperature variations can impair the results of long-term measurements. Therefore, the temperature variations should be less than 1C per hour and should not exceed 2C per day for this type of measurement.
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3
Vibration

INSTALLATION Site Requirements

Ideally, the spectrometer should not be installed near vibration sources (e.g. ventilation hoods, air conditioners, motors, elevator etc.) or in rooms with intense floor vibration.

Power Supply
The spectrometer power supply unit automatically adapts to the most common power sources. Valid voltage range: 100 V AC to 240 V AC Valid frequency range: 50 to 60 Hz VERTEX 70v is an instrument of the protection class I. Caution: To avoid personal injury and spectrometer damage, connect the spectrometer only to a socket outlet with earthing contact. To provide for good data quality and a long spectrometer service life, ensure that the following site requirements are met:

Do not install the spectrometer near sources of potential inductive electrical


interference (e.g. pumps, switching motors, microwave ovens etc.), sources of high energy pulses, and sources that might cause magnetic or radio frequency interference.

Do not place devices such as large electric motors, heaters, welding equipment,
radio transmitting equipment, units emitting pulsed NMRs, or high powered lasers in close vicinity to the spectrometer. These devices can interfere with the spectrometer and cause spectrometer malfunction. Ensure that these types of devices are not connected to the same electrical circuit as the spectrometer.

If a reliable mains power supply is a problem at your site (caused by brownouts,


power surges, frequent thunderstorms, for example), take precautions to ensure an uninterruptible power supply.

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VERTEX 70v User Manual

INSTALLATION Connecting VERTEX 70v to the Power Supply

CONNECTING VERTEX 70V TO THE POWER SUPPLY


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Pow er Cord
Before connecting the power cord, make sure that the spectrometer is switched off, i.e. the mains switch (B in figure 2) is in the O position. Connect the supplied power cord to the primary power receptacle (C in figure 2) as well as to the mains socket outlet. The power cord length should not exceed 3m. Depending on the local conditions, the original power cord may need to be exchanged for a power cord that complies with the standards of the country in question. The power cord must have approbation of at least your local authority, UL for US, CSA for Canada or VDE for Europe. The spectrometer power supply unit automatically adapts to the local voltage and frequency range. (See section Site Requirements.)

Figure 2: Spectrometer Rear Side - Connections for Power Supply and PC

Component A B C Ethernet port Mains switch Primary power receptacle (for connecting the power cord)

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INSTALLATION Connecting VERTEX 70v to a PC

CONNECTING VERTEX 70V TO A PC


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Data Cable
The data cable included in the spectrometer delivery scope is a CAT5 crossover cable (labelled Cross-over) with two RJ-45 plugs. This cable is only used for the direct connection of VERTEX 70v to a computer. If you intend to connect the spectrometer to a network, a different type of cable (i.e. non-crossover, CAT 5 cable for the 10Base-T Ethernet standard) is required. (See appendix E.) The data cable length should not exceed 100m (without repeater). Connect one end of the data cable to the Ethernet port (ETH) (A figure 2) and the other end of the data cable to the RJ-45 socket of the computer network interface card. (For detailed information refer to the computer manual.) After having set up the data cable connection, turn on the spectrometer using the mains switch. After a few seconds, the spectrometer beeps once and starts a self test. After the initialization has been completed successfully, the STATUS LED (figure 10) turns from red to green. Now switch on the computer and the monitor. (For information on how to install the computer and how to set up signal and power cable connections for the computer, monitor etc. refer to the computer manual.)

Computer Setup
VERTEX 70v and the delivered PC are already configured for the stand-alone operation. The spectrometer IP address is factory-set to 10.10.0.1. In case you have not purchased the computer together with the VERTEX 70v spectrometer, you have to assign an appropriate IP address to the computer to which you want to connect the spectrometer. For detailed information about how to assign an IP-address to the computer refer to appendix E.

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VERTEX 70v User Manual

INSTALLATION Connecting VERTEX 70v to the Vacuum Pump

CONNECTING VERTEX 70V TO THE VACUUM PUMP


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The attachment flange (NW25 flange) for connecting the vacuum pump is at the spectrometer rear side. Figure 3 shows the valve block with removed cover. Attachment Flange for the Vacuum Pump

Valve for evacuating the optical bench

Valve for evacuating the sample compartment Valve for venting the sample compartment Opening for venting the sample compartment
(Note: When purging the spectrometer this port is used as purge gas inlet for the sample compartment. Figure 3: Valve Block (Spectrometer rear Side)

Valve for venting the optical bench

Opening for venting the optical bench


(Note: When purging the spectrometer this port is used as purge gas inlet for the optical bench.

The vent openings are covered by a plug made from sintered-powder metal which is airpermeable (i.e. the spectrometer can be vented with the plugs installed on the vent opening). (See figure 8.) The plug functions like a filter preventing particles from entering the spectrometer together with the influent air. Note: For detailed information about the vacuum pump refer to the user manual provided by the vacuum pump manufacturer.

VERTEX 70v User Manual

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INSTALLATION Connecting VERTEX 70v to the Vacuum Pump

Installation Procedure
Remove the valve block cover shown in figure 4 by loosening the two Allen screws
using a hex key (size 3mm) and pulling off the cover. Allen Screws Valve Block Cover

Figure 4: Removing the Valve Block Cover

Install the supplied sealing ring at the attachment flange. See figure 5.
Attachment Flange Sealing Ring

Flexible Metal Hose

Figure 5: Connecting VERTEX 70v to Vacuum Pump - Step 1

Press the supplied flexible metal hose against the attachment flange (figure 6a)
and attach the hose to the flange using the supplied hose clamp (figure 6b). Secure the hose clamp by fastening the wing screw.

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INSTALLATION Connecting VERTEX 70v to the Purge Gas Line

Wing Screw

Hose Clamp

Figure 6: Connecting VERTEX 70v to Vacuum Pump -Step 2

During operation, the vacuum pump generates vibrations. In order to prevent these vibrations from being transferred to the spectrometer via the flexible metal hose, the supplied vibration absorber has to be installed between the vacuum pump and the spectrometer. The procedure for connecting the flexible metal hose to the vacuum pump and to the vibration absorber is identical to the procedure described above. Note: Make sure that the vibrating metal hoses do not come into contact with the table on which the spectrometer is placed.

During the operation, the vacuum pump produces an increased noise level. In order to reduce the noise level install the supplied noise reduction hood over the vacuum pump. For information about the noise reduction hood installation refer to instructions provided by the pump manufacturer.

CONNECTING VERTEX 70V TO THE PURGE GAS LINE


..........................................................
As an alternative to the vacuum operation, VERTEX 70v can be purged with either dry air or dry nitrogen gas. The spectrometer has two purge gas inlets; one for purging the sample compartment and the other for purging the optical bench. The purge gas inlets are at the spectrometer rear side. See figure 7.

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INSTALLATION Connecting VERTEX 70v to the Purge Gas Line

Purge gas inlet for optical bench.


(Note: In case of vacuum operation - vent opening for venting the optical bench.)

Purge gas inlet for sample compartment.


(Note: In case of vacuum operation - vent opening for venting the sample compartment.) Figure 7: Purge Gas Inlets

For detailed information about the required purge gas supply conditions refer to chapter Operation, section Purging the Spectrometer.

Installation Procedure
Note: In case the spectrometer is evacuated, first vent it before starting the installation procedure. Otherwise, a warning message regarding unstable pressure conditions inside the spectrometer will appear.

To connect the spectrometer to the purge gas supply you need a stiff hose with an
outer diameter of 6mm. Remove the plug (made from sintered-powder metal) from the purge gas inlet by pressing the lock ring inwards (figure 8) and pulling out the plug. Connect one end of the hose to your supply line for dry air or dry nitrogen gas and insert the other end of the hose into the purge gas inlet for either the sample compartment or optical bench.

If you want to purge both the sample compartment and the optical bench, you
need a T-shape connecting hose with two hose ends leading to the spectrometer. After having connected the main end of the hose to the supply line, insert one of the other two hose ends into the purge gas inlet for the sample compartment and the other hose end into the purge gas inlet for the optical bench.

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INSTALLATION Connecting VERTEX 70v to the Purge Gas Line

Lock Ring

Plug

Figure 8: Purge Gas Inlet with removed Plug

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INSTALLATION Connecting VERTEX 70v to the Purge Gas Line

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O. V .E. R.V. I. E .W . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
GENERAL INFORMATION
..........................................................

4
G H

This chapter describes all relevant external and internal spectrometer components. Note: The local indications right and left assume that the operator stands in front of the spectrometer. The indications forward and backward refer to the spectrometer front side and rear side, respectively.

A B C

E I F

Figure 9: General Overview

Compartment A B C D E F G H I Power Supply Connector Status Indicator Board Electronics Compartment Interferometer Compartment Detector Compartment Sample Compartment Laser Vacuum Pump Connection Port Beam Direction Control Compartment

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OVERVIEW External Components

The detector compartment, the interferometer compartment and the beam direction control compartment are not separated from each other but form one compartment. All spectrometer compartments are accessible by removing the corresponding cover.

EXTERNAL COMPONENTS
Status Indicator Board

..........................................................

The status indicator board is in the left rear corner of the spectrometer, more precisely, on the electronic compartment cover. (See figure 10.) The color of the LEDs gives a general indication of the operating status of the corresponding spectrometer component. Moreover, the color of the Vacuum LED indicates the current pressure situation inside the spectrometer compartments (i.e it shows whether a certain compartment is being evacuated/vented just now or is already evacuated/vented). In case one of these LEDs lights up red indicating a spectrometer problem refer to chapter Troubleshooting. This chapter shows possible causes of a problem and provides solutions.

Figure 10: Status Indicator Board

VACUUM The color of VACUUM LED depends on the current pressure situation inside the individual spectrometer compartments. The following table explains the meaning of the different LED colors:
LED is off. LED flashes green. LED lights up green. LED flashes yellow. Sample compartment and optical bench are vented. Sample compartment and optical bench are being either evacuated or vented. Sample compartment and optical bench are evacuated. The ultimate vacuum is achieved. Sample compartment is being either evacuated or vented. (In case the sample compartment is already vented, it flashes yellow also when the optical bench is being vented.) Sample compartment is vented. When the spectrometer is being evacuated, but a certain threshold pressure value is not reached within a certain period of time (i.e. the ultimate vacuum is not achieved). A red VACUUM LED indicates a problem. See chapter Troubleshooting, section Problem - Possible Cause - Solution, subsection Spectrometer problem indicated by spectrometer status indicator. VERTEX 70v User Manual

LED lights up yellow. LED lights up red.

20

OVERVIEW External Components LASER The LASER LED lights green when the laser is in operation and the laser signal is OK. The LASER LED lights up red if the laser power is too weak, the laser beam is blocked or if the laser module is defective or out of alignment. (See chapter Troubleshooting, section Problem - Possible Cause - Solution, subsection Spectrometer problem indicated by spectrometer status indicator.) This control lamp also lights up red during the spectrometer initialization phase. After the initialization is completed successfully, this LED turns to green. STATUS A green STATUS LED indicates that the spectrometer is in proper operating condition. The STATUS LED lights up red in case of a spectrometer malfunction or during the initialization phase. After the initialization is completed successfully, this LED turns to green. (See chapter Troubleshooting, section Problem - Possible Cause - Solution, subsection Spectrometer problem indicated by spectrometer status indicator.)

Sample Compartment
Normally, you gain access to the sample compartment from the spectrometer top side by removing the blue cover using the handle. See figure 11a. In exceptional cases, if your measurement accessory requires access from the spectrometer front side (e.g. for exchanging the sample), you can remove the blue front cover by loosening the six Allen screws using a hex key size 3mm. See figure 11b. Note: When performing measurements under vacuum condition do not forget to reinstall the sample compartment front cover. The sample compartment dimensions are 25.5cm (w) x 27cm (d) x 16cm (h). For more information about the sample compartment interior refer to chapter Operation, section QuickLock.

Sample Compartment Cover Handle

Allen Screws

Figure 11: a) Sample Compartment Top Cover

b) Sample Compartment Front Cover

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OVERVIEW External Components

IR Beam Ports
VERTEX 70v has seven IR beam ports (five outlet ports and two inlet ports) allowing the adaptation of external accessories and/or components (e.g. microscope, TG-IR coupling or external light source). The IR beam ports are at the front and rear side as well as at the left and right hand side of the spectrometer. For the exact dimensions of the IR beam port positions refer to appendix D. A B C

Figure 12: a) Front Side

b) Rear Side

Figure 12: c) Right Side

d) Left Side

IR Beam Ports A B C D E F G Outlet port for focussed beam (e.g. for connecting a bolometer) Outlet port for parallel beam (e.g. for connecting a fiber optic coupling module) Inlet port for connecting a light emission source (e.g. Hg source) Outlet port for parallel beam Outlet port for parallel beam (e.g. for connecting a microscope, PMA50, external sample compartment XSA) Inlet port for connecting a light emission source (e.g. FT-Raman module, water-cooled, high-power MIR source) Outlet port for parallel beam (e.g. for connecting a microscope) or focussed beam (e.g. for connecting a bolometer)
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OVERVIEW External Components The IR beam ports are vacuum-tight sealed by circular covers. To remove a cover loosen the six Allen screws using a hex key size 3mm. See figure 13. Note: External accessories are installed by the Bruker service technicians.

Allen Screws

Figure 13: Removing an IR Beam Port Cover

Spectrometer Rear Side


External Beam Port Attachment Flange for Vacuum Pump Electronics Panel CAN BUS Port

Vent Opening/ Purge Gas Inlet


Figure 14: Spectrometer Rear View

Primary Power Receptacle

Mains Switch

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OVERVIEW External Components

EXTERNAL BEAM PORT The inlet port is used for connecting a light source (e.g. Hg-Source) or an emission sample. VENT OPENING / PURGE GAS INLET Depending on whether you evacuate or purge the spectrometer, these two ports serve different purposes. In case of evacuating the spectrometer these ports serve as vent openings, whereas, when purging the spectrometer the purge gas supply lines are connected to these ports. (For detailed information about installing the purge gas connection refer to chapter Installation.) ELECTRONICS PANEL On the electronics panel are a number of ports (e.g. Ethernet port), the reset button as well as LEDs indicating, for example, the status of the interferometer. For a detailed description of the electronics panel refer to appendix F. MAINS SWITCH AND PRIMARY POWER RECEPTACLE The mains switch is used to turn the spectrometer on and off. The power supply socket is used to connect the power cord to the spectrometer. CAN BUS PORT The CAN bus port is primarily used to connect external automated units to the spectrometer. For more information refer to appendix F. ATTACHMENT FLANGE FOR VACUUM PUMP The vacuum pump can be connected to this attachment flange (NW25) using the supplied sealing ring, flexible metal hose and hose clamp. (For detailed information about how to connect the vacuum pump to the spectrometer refer to chapter Installation.)

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OVERVIEW Internal Components

INTERNAL COMPONENTS

..........................................................
The following figure identifies only the most important internal components and their location inside the spectrometer.

F G H

C I

Figure 15: Internal Spectrometer Components

Component A B C D E F G H I RockSolid interferometer (permanently aligned) DigiTect Detectors Sample holder for transmission measurements (exchangeable for other optional accessories with QuickLock baseplate) HeNe laser Two beamsplitters storage positions (optional) Beamsplitter (operation position) Optional NIR source (operating position) MIR source (operating position) QuickLock mechanism for accessories (including connectors)
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4
Light Source

OVERVIEW Internal Components

The basic instrument is equipped with a MIR source (H in figure 15). The MIR light source is a globar (i.e. an U-shaped silicon carbide piece) that emits mid-infrared light. Apart from the standard air-cooled MIR source, the following optional sources are available:

VIS/NIR source (tungsten halogen lamp), installed in the spectrometer (G in


figure 15), air-cooled

FIR source (mercury lamp), connected externally to the spectrometer, watercooled

UV/VIS/NIR source (tungsten lamp), connected externally to the spectrometer,


water-cooled

UV source (deuterium lamp), connected externally to the spectrometer, air-cooled High power MIR source (globar), connected externally to the spectrometer, watercooled All external sources can be connected to one of the two inlet ports (C in figure 12b or F in figure 12c). For the FIR source (mercury lamp), the preferred connection port is the inlet port at the spectrometer rear side, C in figure 12b.

Detector
The basic spectrometer configuration is equipped with a DigiTect DLaTGS detector with integrated preamplifier. This detector package contains an analog-to-digital-converter that converts the analog signal from the detector directly into a digital signal. This digital signal is transmitted to the data processing electronics unit of the spectrometer. The standard detector is a pyroelectric DLaTGS detector which covers a spectral range from 12,000 to 250cm-1, operates at room temperature and has a sensitivity of D*>4x108 cm Hz1/2 W-1. Apart from the standard detector, there is a large number of optional detectors. All detectors are mounted on dovetail slides which allow an easy exchange. The following optional detectors are available: Detector Mid-Infrared DLaTGS with KBr window DLaTGS with CsI window MCT narrow band, with BaF2 window
CAUTION - HARMFUL!

Spectral Range (cm-1)

Sensitivity

Operating Temperature

12,000 - 250 12,000 - 160 12,000 - 850

D*>4x108cm Hz1/2W-1 D*>4x108cm Hz1/2W-1 D*:>4x1010cm Hz1/2 W-1

Temperature-stabilized Room temperature Liquid N2 cooled

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OVERVIEW Internal Components

Detector MCT mid band, with ZnSe window


CAUTION - TOXIC!

Spectral Range (cm-1) 12,000 - 600

Sensitivity D*:>2x1010cm Hz1/2 W-1

Operating Temperature Liquid N2 cooled

MCT broad band, with KRS-5 window


CAUTION - TOXIC!

12,000 - 420

D*:>5x109cm Hz1/2W-1

Liquid N2 cooled

Photovoltaic MCT, with BaF2 window


CAUTION - HARMFUL!

12,000 - 850

D*:>2x1010cm Hz1/2 W-1

Liquid N2 cooled

MCT/InSb Sandwich, with ZnSe window


CAUTION - TOXIC!

10,000 - 600

D*:>2x1010 cm Hz1/2W-1 (MCT) D*:>1.5x1011cm Hz1/2W-1(InSb)

Liquid N2 cooled

Near-Infrared InSb InSb with cold filter Ge Detector (Raman) InGaAs Diode InGaAs Diode Ge Diode Far Infrared DLaTGS with PE window Silicon Bolometer Visible & UV Silicon Diode GaP Diode 25,000 - 9,000 33,000-18,000 NEP:<10-14 W Hz-1/2 No NEP available Room temperature Room temperature 700 - 10 600 - 10 D*>4x108cm Hz1/2W-1 NEP<10-13 W Hz-1/2 Room temperature Liquid He cooled 10,000 - 1,850 10,000 - 3,100 11,750 - 5,900 12,800 - 5,800 12,800 - 4,000 15,000 - 5,300 D*:>1.5x1011cm Hz1/2 W-1 D*>5x1011cm Hz1/2 W-1 NEP<10-15 W Hz-1/2 NEP:<2x10-14 W Hz-1/2 NEP:<2x10-13 W Hz-1/2 NEP:<5x10-12 W Hz-1/2 Liquid N2 cooled Liquid N2 cooled Liquid N2 cooled Room temperature Peltier cooled Room temperature

Warning: Some detectors are equipped with windows of which the material is harmful or (very) toxic. During normal spectrometer operation, these materials do not pose a health risk. However, should these windows break caused by mechanical impact, be extremely careful. Avoid generating dust. These materials are harmful or toxic if swallowed or inhaled. Also avoid skin and eye contact.

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4
Beamsplitter

OVERVIEW Internal Components

The standard KBr beamsplitter covers a spectral range from 8000 to 350cm-1. Apart from the standard beamsplitter, there are also optional beamsplitters. They allow data acquisition in wavelength ranges other than MIR (standard) when used in conjunction with the appropriate light source and detector. Note that the combination of light source, detector, beamsplitter and sample compartment window material defines the IR measurement range. The following optional beamsplitters are available: Beamsplitter Mid-Infrared KBr (standard) KBr (broad band) Csl Near-Infrared CaF2 CAUTION - HARMFUL! Visible & UV Quartz VIS/UV Far-Infrared Multilayer (far IR) Mylar 25m Mylar 50m Solid state Alignment Tool Glass For alignment purposes only! nickel-plated 680 - 30 120 - 20 50 - 10 600 - 30 *
* limited to a spectral resolution of 0.5cm-1

Spectral Range (cm-1)

Color Coding of the Beamsplitter Handle red red red black

7,500 - 370 10,000 - 400 5,000 - 210 15,500 - 1,200

25,000 - 9,000

white nickel-plated nickel-plated nickel-plated nickel-plated

Caution: The beamsplitter material CaF2 is harmful if inhaled or swallowed. Avoid also skin and eye contact.

Laser
VERTEX 70v is equipped with a HeNe laser (D in fig. 15) It emits red light with a wavelength of 633nm. The rated power output is 1mW. The laser controls the position of the moving interferometer mirror (also called scanner) and is used to determine the data sampling positions. The monochromatic beam produced by the HeNe laser is modulated by the interferometer to generate a sinusoidal signal. For information about how to replace a defective laser module, refer to chapter Maintenance and Repair.

Interferometer
VERTEX 70v is equipped with a high stability interferometer with ROCKSOLID permanent alignment. The ROCKSOLID interferometer incorporates dual retroreflecting cube corner mirrors in pendulum arrangement. The high throughput design ensures the highest possible signal-to-noise ratio.
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OVERVIEW Optical Path

OPTICAL PATH

..........................................................

Figure 16: VERTEX 70v - Optical Path

The beam path shown in figure 16 ist the beam path of the standard spectrometer configuration.

D1 D2 BMS APT OPF IN1 ... IN2 OUT1 ... OUT5

Standard detector Optional detector Beamsplitter Aperture wheel Optical filter wheel Beam inlet port 1 ... 2 Beam outlet port 1 ... 5

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OVERVIEW Optical Path

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O.PERATION . . . . . . . . . . . . . . . . . . . . . . . . . . ..........
GENERAL INFORMATION
..........................................................

After the spectrometer has been installed and connected to the power supply, the PC, and the vacuum pump, the spectrometer is ready for operation. VERTEX 70v is completely computer-controlled, i.e. operating the spectrometer (e.g. selecting the corresponding optical components) performing a measurement and evacuating/venting the spectrometer is done using the spectroscopic software OPUS. This chapter describes mainly the spectrometer related aspects of the operation. For detailed information about the OPUS software refer to the OPUS Reference Manual. The OPUS manual Getting Started explains step by step how to perform the first measurement after the spectrometer has been set up. The standard spectrometer configuration is designed for measurements in the mid infrared region. Optionally, the spectral region can be expanded by substituting the installed MIR components (source, detector, beamsplitter and sample compartment windows, if available) for the corresponding optical components that allow measurements in the far or near infrared as well as in the visible or ultraviolet region. (For information about the replacement procedure of these optional components refer to the corresponding sections in this chapter and in chapter Maintenance and Repair.)

SWITCHING VERTEX 70V ON AND OFF


..........................................................

General Information
The spectrometer is turned on and off using the mains switch at the spectrometer rear side (figure 14). After having switched on the spectrometer, it starts booting. The boot process takes about 30 seconds. As soon as this process is completed successfully, the STATUS LED (figure 10) turns from red to green. After having switched on the spectrometer wait at least ten minutes before starting the first measurement. This allows for the electronics and the light source to stabilize thermally. Caution: After having switched the spectrometer off, wait at least 30 seconds before switching the spectrometer on again. This measure avoids peaks in the initial current which could lead to fuse blowing and/or damaging the power switch.

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OPERATION Switching VERTEX 70v On and Off

Switch-on Procedure
To put the spectrometer into operation again, proceed as follows: 1 2 Switch on the PC. Switch on the spectrometer. The spectrometer begins to start up.

Note: After the spectrometer initialization is completed successfully, the STATUS LED turns to green. Now the spectrometer is ready for operation again. 3 Connect the the vacuum pump to the power supply.

Note: For information about how to operate the vacuum pump refer to the supplied user manual of the vacuum pump manufacturer.

Switch-off Procedure
Ideally, the spectrometer should uninterruptedly be kept under vacuum, even during times of nonuse. If, however, the circumstances require a switching-off of the vacuum pump and/ or the spectrometer the following procedure is recommended: 1 2 Evacuate the optical bench. As soon as the final pressure is reached, switch off the spectrometer.

Note: The evacuation will take about 5 minutes. In the electroless spectrometer state, all valves (for venting as well as for evacuating the spectrometer) are closed. 3 Disconnect the vacuum pump from the power supply.

In this state, the spectrometer interior is isolated from the laboratory environment and the optical spectrometer components are protected against air humidity and they are no longer current-carrying.

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OPERATION QuickLock

QUICKLOCK

..........................................................
The sample compartment is equipped with a locking mechanism, called QuickLock, for positioning and locking different measurement accessories. Therefore, you can use only accessories that are mounted on a QuickLock baseplate. The QuickLock mechanism enables a solid lock even for heavy and bulky accessories and allows a quick, easy and reproducible positioning of the measurement accessories in the sample compartment. When you insert and lock the accessory, all connections (purge gas connection and electrical connection) are established and the accessory is automatically recognized by the application software OPUS. This software feature is called AAR - Automatic Accessory Recognition. In addition, the recommended measurement parameters are selected automatically, provided that you have already stored the parameters for the accessory in question. (See OPUS Reference Manual.) QuickLock locking device Electronic connectors Purge gas connection port

Figure 17: a) Sample Compartment - QuickLock Holder

b) QuickLock Release Button

The QuickLock mechanism also allows purging the sample compartment with dry air or nitrogen gas. The purge gas enters the sample compartment via the gas diffusor (figure 18).

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OPERATION QuickLock

Purge gas diffusor Electronic connectors for AAR and CAN bus
Figure 18: Accessory with QuickLock Baseplate

To insert an accessory with QuickLock baseplate:


1 Hold the accessory with the QuickLock baseplate front edge slightly tilted upwards. Then, gently push the electrical connectors of the baseplate against their counterpart of the QuickLock holder. Put the baseplate down. Ensure that the baseplate is horizontally aligned to the QuickLock holder. Gently press the front edge of the baseplate downward until it snaps into place. To facilitate the insertion of the accessory, press the release button outside the sample compartment. (See figure 17b.)

To remove an accessory with QuickLock baseplate:


1 2 3 Press the QuickLock release button outside the sample compartment. (See figure 17b.) While pressing the QuickLock release button, lift the front edge of the QuickLock baseplate until the baseplate snaps free. Carefully lift the accessory off the QuickLock holder to avoid damages to the electrical connectors at the baseplate rear side.

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OPERATION Automatic Accessory Recognition

AUTOMATIC ACCESSORY RECOGNITION


..........................................................
As soon as an accessory is locked into the QuickLock holder, the OPUS/AAR software (Automatic Accessory Recognition) starts and recognizes automatically the accessory in question, provided you have activated the AAR function in the OPUS software. (For information about how to activate the AAR function refer to the OPUS reference manual, OPUS manual part Automatic Accessory Recognition). The OPUS/AAR software identifies the accessory, performs several tests, adapts the measurement parameters and opens the Measurement dialog window to start a measurement. If the automatic accessory recognition has been completed successfully, OPUS displays a corresponding message. Each time you start OPUS, the AAR program checks whether an accessory is installed into the sample compartment. If AAR detects an accessory, the corresponding dialog box is displayed. It also appears when the accessory is substituted by another one. Note: When installing a new accessory for the first time, it is not yet registered so that the OPUS/AAR software can not recognize it. In this case, you first have to register the new accessory in question. (See OPUS Reference Manual.)

PERFORMING A MEASUREMENT
..........................................................
The measurement procedure described in the following refers exclusively to measurements under vacuum conditions. In case you want to perform a measurement not under vacuum ignore the steps regarding evacuating and venting the spectrometer.

Specify the measurement parameters in the OPUS programme. To do this, select


in the OPUS Measure menu the Advanced Measurement function and select or enter the corresponding parameter values. (The standard parameter values are listed in appendix C.)

Evacuate the spectrometer as described in the following section. (Wait until the
ultimate vacuum is achieved.)

Acquire a background spectrum without the sample in the sample compartment by


clicking in OPUS on the Background Single Channel button. (See figure 19.)

Vent the sample compartment as described in the following section. Put the sample in the sample compartment. (For information about how to install a
QuickLock accessory into the sample compartment refer to the section QuickLock in this chapter. For information about sample preparation refer to appendix G.)

Evacuate the sample compartment again. (Wait until the ultimate vacuum is
achieved.)

Acquire a sample spectrum by clicking in OPUS on the Sample Single Channel


button (figure 19) and calculate the ratio (transmittance spectrum). Note: Use the same parameter values for the background and the sample measurement. Ensure that both measurements are performed under identical ambient conditions.
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OPERATION Evacuating and Venting the Spectrometer

Figure 19: OPUS Measurement Dialog Window

For detailed information about OPUS functions for data acquisition, manipulation and evaluation refer to the OPUS Reference Manual.

EVACUATING AND VENTING THE SPECTROMETER


..........................................................
VERTEX 70v is primarily designed for vacuum operation, but it can be purged as well. To activate the vacuum mode, select in the OPUS Measure menu the Optic Setup and Service function. Click on the Devices/Options tab and make sure that the Purge Mode check box is not ticked off. See figure 20.

With this checkbox being deactivated, the vacuum mode is activated.


Figure 20: Activating the Vacuum Mode

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OPERATION Evacuating and Venting the Spectrometer The flaps and the venting and evacuating valves are controlled automatically via the OPUS software. So evacuating and venting the sample compartment and/or optical bench is done using the OPUS software. The corresponding buttons are at the Basic page of the Measurement dialog window. See figure 21.

Command that can be executed next by clicking on this button. Current state in the individual compartments including the current pressure reading
Figure 21: Optical bench and sample compartment are vented.

Let us assume the following initial situation: both the sample compartment and the optical bench are vented. In this case, it is not possible to evacuate only the sample compartment. (The evacuation of only the sample compartment is not possible as in this case the pressure difference between the sample compartment and the optical bench would damage the flaps, i.e. the flaps are not designed for such an operation condition.) So, clicking on either button effects the evacuation of both compartments. The evacuation process is indicated by the message Sample / Optics Evacuating that appears in the fields below the buttons. The progress of the evacuation is shown by the permanently updated pressure readings in the lower fields. See figure 22. Note: After you have clicked on a button, the labeling of this button changes immediately showing the action that can be performed next (i.e. Evacuate... turns to Vent... and versa vice).

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OPERATION Evacuating and Venting the Spectrometer

Figure 22: Optical bench and sample compartment are being evacuated.

As soon as the evacuation process is completed, the message Sample / Optics Evacuated appears in the lower fields. See figure 23. Note: If the sample compartment is evacuated you can not open it.

Figure 23: Both compartments are evacuated.

Note: To prevent OPUS from starting a measurement while the spectrometer is being evacuated or vented proceed as follows: Click in the Measurement dialog window on the Optic tab and select in the Optical bench ready drop-down list the option Pressure stable. See figure 24.

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OPERATION Evacuating and Venting the Spectrometer

Figure 24: Defining the Measurement Start Precondition

When both compartments are evacuated you can vent the sample compartment separately (for example, if you want to open the sample compartment in order to exchange the sample) by clicking on the Vent Sample button.

Figure 25: Sample compartment is vented and optical bench is evacuated.

Note: When both compartments are evacuated, venting only the optical bench is not possible as the pressure ratio inside the spectrometer would damage the flaps. For safety reasons, the instrument does not perform this operation. In this case, clicking on the Vent Optics button effects the ventilation of the sample compartment as well. This precaution prevents the instrument from being operated wrongly.
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OPERATION Optimizing the Vacuum Operation of the Spectrometer

OPTIMIZING THE VACUUM OPERATION OF THE SPECTROMETER


..........................................................

General Information
To get optimum measurement results under vacuum conditions, there are some aspects that need to be taken into consideration:

The thermal conditions in an evacuated optics bench and in a purged optics bench
are completely different, i.e., under vacuum there is no thermal conduction at all due to the lack of the purge gas. This aspect has consequences on the reproducibility of the measurement results.

Water molecules are very polar. Due to this property, they tend to stick at the inner
wall of the optics compartment. For this reason, it takes time to get the water vapor pumped off completely. The purpose of the following advice is to help you in achieving optimum measurement results.

Reproducibility of the Results


After having evacuated the spectrometer, it is highly recommended that you allow the spectrometer to stabilize long enough. An optimally stabilized spectrometer is able to achieve an extreme high 100%-line stability in the sub-%-level with the standard optical components designed for MIR measurements. (Note: A precondition is that the room temperature does not vary by more than 1C per hour and 2C per day. Typically, this condition can be fulfilled in an air-conditioned environment.)

Recommendations: For demanding experiments, a stabilization period of at least 4 hours is


recommended. After this period, the maximum instrument stability is achieved.

For non demanding experiments, a stabilization time of 0.5 hour is sufficient. During a long-term experiment, it is recommended to repeat the background
measurement in regular interval, at least every hour.

Ideally, the spectrometer should be kept under vacuum overnight.

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OPERATION Optimizing the Vacuum Operation of the Spectrometer

Residual Water Vapor


Longer evacuation times will further reduce the residual water vapor concentration inside the spectrometer: Note: Besides the necessity of a water vapor concentration being as low as possible, there is another aspect regarding water vapor you have to take into consideration: The water vapor line intensity in the sample spectrum does not depend on the absolute residual water vapor concentration in the spectrometer but on the different water vapor concentrations during the background and the sample measurement. Therefore, it is of crucial importance that the residual water vapor concentration is (nearly) identical during both the background measurement and the sample measurement.

Evacuation Time
As mentioned above, water molecules are very polar. Due to this property, they tend to stick at the inner wall of the optics compartment, even under vacuum. For this reason, a long evacuation time is recommended. Ideally, the evacuation of the spectrometer should not be interrupted overnight. This action will further reduce the residual water vapor content.

Evacuation Procedure
Before acquiring a background spectrum, simulate a sample exchange in the same way as you will do it later for the real sample measurement: 1 2 Vent the sample compartment. Afterwards, evacuate the sample compartment for about 5 to 10 minutes. (An evacuation time longer than 10 minutes is not necessary because after that period, the final pressure of < 0.2hPa (< 0.2mbar) will be achieved.)

Note: As soon as the pressure falls below < 1hPa, the message Sample Evacuated, including the current pressure value, is displayed in the Measure dialog window (figure 26). The achievement of the final pressure is also indicated by the VACUUM LED at the spectrometer top side, i.e. this LED lights green.

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OPERATION Optimizing the Vacuum Operation of the Spectrometer

Current state inside the individual compartments, including the current pressure reading

Figure 26: OPUS dialog window Measurement - page Basic

Important Note:The evacuation times before the background measurement and before the sample measurement have to be more or less identical. To ensure reproducible evacuation times, specify in OPUS a Delay before Measurement. See the figure 27. 3 4 5 6 Acquire a single channel background spectrum. Afterwards, vent the sample compartment and place the sample in the sample compartment. Evacuate sample compartment for about 5 to 10 minutes. Acquire a single channel sample spectrum.

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OPERATION Purging the Spectrometer

Specifying the measurement delay time

Figure 27: OPUS Measurement dialog

Note: Take into account that the intensity of the water vapor band in the sample spectrum does not depend on the absolute residual water vapor concentration but results from a water vapor concentration difference during the background and the sample measurement. With the above described operation conditions and a spectral resolution of 4cm-1, typically a residual water vapor band intensity in the range of significantly less than 0.1%T can be achieved.

PURGING THE SPECTROMETER


..........................................................

General Information
Purging the spectrometer is not necessarily required, especially when you perform measurements under vacuum conditions. However, if the spectrometer is not evacuated, purging is recommended, especially when you frequently open the compartment covers (e.g. due to a detector or beamsplitter replacement or a sample substitution) or if the ambient air humidity content is too high because this measure reduces the level of water vapor, CO2 or other components of the ambient air inside the spectrometer. Note: Water vapor, CO2 and other atmospheric contaminants cause unwanted absorption. Therefore, open the sample compartment, the detector compartment and/or the interferometer compartment only if necessary in order to prevent water vapor, CO2 or other contaminants from entering the above mentioned compartments.

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OPERATION Purging the Spectrometer

Purge the spectrometer, for example, with dry air or low pressure nitrogen gas. Provide the following purge gas conditions:

Dry (dew point < -40C corresponds to a degree of dryness of 128ppm humidity),
oil-free and dust-free air or nitrogen gas

Maximum pressure of 2 bar (29 psi) Initial purge gas flow rate should not exceed 500 liters/hour Sustained purge gas flow rate should not exceed 200 liters/hour
Danger: Do not use flammable gases for purging the spectrometer. Some spectrometer components become very hot during operation. If flammable gases come in contact with hot components there will be the risk of fire and/or explosion! For information about how to connect the spectrometer to a purge gas supply line, refer to chapter Installation. Purge gas inlet for purging an enclosed accessory mounted on a QuickLock baseplate This opening is intended for evacuating, venting and purging the sample compartment.

Cap with screw thread

Figure 28: Sample Compartment

If you want to purge an enclosed accessory (e.g. micro ATR unit) you have to cover the opening, which is also intended for evacuating and venting the sample compartment (see figure 28), using the supplied cap in order to ensure a sufficient purge of the accessory. Put the cap over opening and screw on the cap. Attention: If you want to perform measurements under vacuum conditions do not forget to remove this cap again! Otherwise, the evacuation of sample compartment via the small purge gas inlet in the QuickLock clamping device (figure 28) will take too long causing a red VACUUM LED after a certain period of time.

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OPERATION Purging the Spectrometer

Controlling the Flaps


VERTEX 70v is primarily designed for vacuum operation, but it can be purged as well. To activate the purge mode, select in the OPUS Measure menu the Optic Setup and Service function. Click on the Devices/Options tab and make sure that the Purge Mode check box is activated. See figure 29.

Purge mode is activated.

Figure 29: Activating the Purge Mode

This operating mode allows you to control (open and close) the flaps in order to purge either the sample compartment or the optical bench or both. The flaps are controlled via the OPUS software. The corresponding buttons are at the Basic page of the Measurement dialog window. See the following figure.

Next possible action that can be performed by clicking on this button. Current state of the flaps

Figure 30: Controlling the Flaps

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OPERATION Exchanging the Beamsplitter

The flaps can be opened or closed only if the pressure difference between the sample compartment and the optical bench is below the threshold value of 5 hPa.

Special Case
Besides the normal purge mode in which the optical bench and/or the sample compartment are only purged, the following special case is also possible: the vented sample compartment is purged while the optical bench is evacuated. For the realization of this special case, the spectrometer needs to be equipped with windows mounted on either the sample compartment walls or the flaps which are closed in this case. To realize this special case, proceed as follows:

Make sure that the purge mode is deactivated in OPUS. (See figure 20.) Evacuate the optical bench and the sample compartment. (See chapter Operation, section Evacuating and Venting the Spectrometer.)

Afterwards, vent the sample compartment again. (In this condition, the flaps are
closed.)

Connect a hose to the purge gas inlet for the sample compartment. (The purge
gas inlet is at the spectrometer rear side. See chapter Installation, section Connecting VERTEX 70v to the Purge Gas Line, figure 7.)

Now start the purge gas supply.


Note: The flaps isolate the sample compartment hermetically from the optical bench.

EXCHANGING THE BEAMSPLITTER


..........................................................

General Information
The standard version and the optional version of VERTEX 70v differ from each other with regard to the interferometer compartment cover design (see fig. 33a and 33b) and the availability of the beamsplitter storage positions (see fig. 31) inside the interferometer compartment.

Feature Interferometer cover design compartment

Standard Version A beamsplitter exchange requires the removal of the complete interferometer compartment cover. No

Optional Version (S239/V) Wing-shaped cover provides for easy access to the beamsplitter.

Availability of the beamsplitter storage positions inside the interferometer compartment

Yes

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OPERATION Exchanging the Beamsplitter The standard spectrometer version is equipped with a MIR beamsplitter (made of KBr). If your measurement requires a different spectral range, you can exchange the beamsplitter manually. For a list with all available beamsplitters (including their spectral ranges) refer to chapter Overview, section Internal Components. Note: Make sure that the spectral ranges of the installed optical components (source, beamsplitter, detector and sample compartment windows, if installed) correspond with each other! Changing the beamsplitter is easy because a precise locking mechanism automatically fixes the beamsplitter at its pre-aligned position, as soon as you move the release lever (figure 34) into the locked position (i.e. backward). All beamsplitters for VERTEX 70v are electronically coded enabling the spectrometer firmware to auto-detect the beamsplitter type. The information about the component is passed on to the OPUS software. This feature is called ACR (Automatic Component Recognition)1. Its purpose is to prevent you from selecting a wrong component in OPUS when you set up a measurement. (Note: A wrongly selected component is indicated in OPUS by a red colored entry field of the corresponding drop-down list. See also the OPUS Reference Manual.) Beamsplitter (Operating position) Two additional Beamsplitters (Storage position)

Knob

Wing-shaped cover

Figure 31: VERTEX 70v - Beamsplitter Installation Positions (only In case of option S239/v)

1. ACR is restricted only to the optical components beamsplitter, detector and source.

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OPERATION Exchanging the Beamsplitter

Handling Instructions
Caution: The beamsplitter is a very delicate component. Handle it with utmost care and observe the following handling instructions to ensure a long service life.

Do not touch the beamsplitter surface as this will damage the surface and, as a
consequence, the beamsplitter may become useless. Hold the beamsplitter using always the handle (figure 32).

Some beamsplitter materials are hygroscopic. Never expose them to humidity or


water vapor. Store the beamsplitter either in a dry and sealed container (e.g. in the beamsplitter storage box) or inside the spectrometer (storage position, figure 31).

Do not try to loosen or fasten the screws as this will impair the optical quality of the
beamsplitter and lead to malfunctions.

Do not try to clean the beamsplitter. Do not expose the beamsplitter (especially beamsplitters made of KBr) to temperature changes.

Handle

Figure 32: Beamsplitter

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OPERATION Exchanging the Beamsplitter

Exchange Procedure
1 The procedure for gaining access to the beamsplitter depends on the interferometer compartment cover design. Standard cover (fig. 33a): Take off the complete cover. Optional cover (fig. 33b): Turn the knob counterclockwise until the stop and rotate the wing-shaped cover aside as shown in figure 31.

Figure 33: a) Standard Cover

b) Wing-shaped Cover (in case of option S239/V)

Caution: Class 2 laser radiation. When the cover is removed do not stare into the laser beam. 2 3 4 5 6 Move the release lever into the unlocked position (i.e. backward). Carefully pull the beamsplitter straight upwards without catching an edge. Take the other beamsplitter out of the storage position and insert it with the electrical contacts facing to the front side (figure 34). Push down the beamsplitter completely until you feel resistance. Move the release lever into the locked position, i.e. forward. (See figure 34.)

Note: A beep indicates that the beamsplitter has been recognized by the electronics. After a few seconds the spectrometer will start scanning. 7 8 Insert the beamsplitter, you have taken out of the operating position, either into the storage position holder (figure 31) or store it in the intended box. Standard cover: Place the cover on the interferometer compartment again. Optional cover: Rotate the wing-shaped cover over the openings and secure it by turning the knob clockwise. Check whether a signal is detected and the optics works correctly. (For detailed information refer to the OPUS reference manual.)
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OPERATION Exchanging the Detector

Beamsplitter handle

Release lever (in locked position)

Figure 34: Beamsplitter (Operating Position)

EXCHANGING THE DETECTOR


General Information

..........................................................

The basic spectrometer configuration is equipped with a DigiTect DLaTGS detector. If your measurement requires a different spectral range or another detector sensitivity you can install another detector into the second detector position, which is an optional spectrometer feature, or exchange the installed DigiTect DLaTGS detector for another DigiTect detector, such as a MCT with a higher sensitivity or a NIR detector. (For the list with all available detectors including their spectral ranges refer to chapter Overview, section Internal Components.) Note: Make sure that the spectral ranges of the installed optical components (source, beamsplitter, detector and sample compartment windows, if installed) correspond with each other! A removable cover provides access to the detector compartment. The dovetail detector mounting facilitates the exchange. A re-alignment is not necessary. All detectors for VERTEX 70v are electronically coded, enabling the spectrometer firmware to autodetect the type of detector currently installed. This information is passed on to the OPUS software. This feature is called ACR (Automatic Component Recognition)1. Its purpose is to prevent you from selecting a wrong component in OPUS when you set up a measurement. (Note: A wrongly selected component is indicated in OPUS by a red colored entry field of the corresponding drop-down list. See also the OPUS Reference Manual.)
1. ACR is restricted only to the optical components beamsplitter, detector and source.

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OPERATION Exchanging the Detector

MCT detector

DLaTGS detector Locking screw of the detector installed in position 2 Locking screw of the detector installed in position 1
Figure 35: Detector Compartment

Fixed mirror Moveable mirror

Exchange Procedure
1 Take off the detector compartment cover (E in figure 9).

Caution: If there is a MCT detector installed in the detector compartment (including a vacuum-tight closure at the filling hole in the detector compartment cover) the detector compartment cover can not be taken off. In this case, do not try to remove the cover forcibly as this may cause a spectrometer damage! Therefore, first screw off the sealing adapter mating part (figure 39) before you take off the detector compartment cover. (See chapter Operation, section Cooling an MCT Detector, subsection Detector Compartment Cover Preparation Procedure.) 2 Loosen the locking screw (allen screw) that secures the detector using a hex key (size 6mm). See figure 35. Depending on which detector you want to remove, the allen screw is on the left or right side of the detector. Pull the detector straight upwards out of the dovetail guide.

Caution: Remove the detector carefully in order not to damage the detector and/or the mirrors. 4 Insert the other detector precisely into the dovetail guide and push the detector downwards until you feel a resistance.

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OPERATION Cooling an MCT Detector

Note: A beep indicates that the detector has been recognized by the electronics. The electrical connections are established automatically. 5 6 Fasten the allen screw slightly using a hex key (size 6mm). Place the cover on the detector compartment. Make sure that the four plastic pins in the corners at the bottom side of the detector compartment cover engage into the corresponding hole of the spectrometer case.

Note: If there is a MCT detector in the detector compartment do not forget to reinstall the vacuum-tight closure at the filling hole in the detector compartment cover. For information about it refer to chapter Operation, section Cooling an MCT Detector, subsection Detector Compartment Cover Preparation Procedure.) 7 Check whether a signal is detected and the optics works correctly (For detailed information refer to the OPUS reference manual).

COOLING AN MCT DETECTOR


General Information

..........................................................

To ensure operating ability, MCT detectors have to be cooled regularly with liquid nitrogen. The typical hold time depends on the detector. There are MCT-detectors with a hold time of 8, 12 or 24 hours. To fill the detector with liquid nitrogen you need neither to remove the detector from the spectrometer nor even open the detector compartment. The supplied funnel facilitates the filling in of the liquid nitrogen in the detector. See figure 40.

D e t e c t o r C o m p a r t m e n t C o v e r Preparation Procedure
In case the MCT detector has been delivered together with VERTEX 70v, the detector compartment cover is already prepared for the funnel insertion. If you have ordered the MCT detector at a later date you need to prepare the cover as described in the following. In accordance with the number of detectors that can be installed in the VERTEX 70v detector compartment, there are two filling holes in the cover. See figure 36. These holes are intended to accommodate the funnel. Upon delivery, these holes are closed vacuum-tightly by a cap plus O-ring.

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OPERATION Cooling an MCT Detector

Filling holes closed by caps

Figure 36: Detector Compartment Cover (Top Side)

Proceed as follows: 1 2 Take off the detector compartment cover and turn it upside down. Remove the cap from the filling hole that corresponds with the position of the MCT detector you want to cool. To do this, loosen the nut using a wrench (size 24mm) and remove the O-ring and the cap. See figure 37.

Open filling hole

Closed filling hole

Figure 37: Detector Compartment Cover (Bottom Side)

By default, the sealing adapter is already factory-mounted on the MCT detector. If not, screw the sealing adapter on the MCT detector filling piece. See figure 38.

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OPERATION Cooling an MCT Detector

Sealing adapter

MCT detector

Figure 38: Detector Compartment

4 5

Put the cover on the detector compartment again. Screw the white sealing adapter mating part on the threaded end fitting of the sealing adapter. See figure 39. Threaded end fitting of the sealing adapter

Sealing adapter mating part

Figure 39: Installing a vacuum-tight closure

Note: When you perform a measurement in vacuum, the sealing adapter and its mating part ensure a vacuum-tight closure at the filling hole in the detector compartment cover. Caution: With the installed vacuum-tight closure at filling hole, the detector compartment cover can not be removed. In this case, do not try to remove the cover forcibly as this may cause a spectrometer damage. 6 Insert the funnel as shown in figure 40.

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OPERATION Cooling an MCT Detector

Safety Notes
MCT detectors have to be cooled with liquid nitrogen. The temperature of liquid nitrogen is minus 196C (minus 320.8F). Therefore, handling liquid nitrogen requires the observance of the following safety notes: Warning: Handle liquid nitrogen always with utmost care. Due to its extremely low temperatures, skin contact can cause severe frostbites! Also the gases escaping from the liquid nitrogen are extremely cold and can cause frostbite. The delicate eye tissue can be damaged if exposed to this cold gas even for a short time. Protect your eyes by wearing a face shield or safety goggles! Note that goggles without side shields do not provide adequate protection! Warning: High nitrogen gas concentrations in an enclosed area can cause asphyxiation! Use liquid nitrogen only in well-ventilated areas. Nitrogen gas is colorless, odorless and tasteless. Therefore, it can not be detected by human senses and will be inhaled as if it were normal air.

Cooling Procedure
1 Fill in slowly liquid nitrogen. See figure 40. At first the liquid nitrogen evaporates and streams out again.

Warning: Liquid nitrogen boils and splashes when it is filled a warm container. Therefore, fill in the liquid nitrogen slowly to minimize boiling and splashing. Stand clear of boiling and splashing liquid nitrogen and its issuing gas.

Figure 40: Filling in liquid Nitrogen

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5
2

OPERATION Cooling an MCT Detector

Wait until the funnel is empty before refilling. When the liquid nitrogen stops streaming out the dewar has reached liquid nitrogen temperature. Then, fill the funnel again with liquid nitrogen. Avoid spilling the liquid on the housing. Repeat this procedure until the detector dewar has been filled to maximum. (As a rough rule of thumb for the standard MCT detector: the maximum dewar capacity is about the quantity of two to three funnel fillings. Note that the first two funnel filling will evaporate almost completely.) Avoid overfilling. In this case the liquid flows out of the filling port. After having filled in sufficient liquid nitrogen, remove the funnel and insert the supplied plug instead. See figure 41. Wait about 20 minutes before starting the measurement to allow the detector to stabilize.

4 5

Plug

Figure 41: Closed Filling Hole

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M. AINTENANCE . AND. R. EPAIR . . . . . . . . . ............. .... . ......


GENERAL INFORMATION
..........................................................

VERTEX 70v is a low-maintenance instrument equipped with easy-to-replace components. The operator can replace components with a limited service life (e.g. IR source) without requiring the assistance of the Bruker service personnel. The following maintenance and repair procedures are described in this chapter:

Evacuating a MCT detector dewar Replacing a defective laser module Replacing a defective IR source Replacing fuses Replacing the sample compartment windows Cleaning the instrument Maintaining the vacuum pump

Perform only the maintenance and repair works which are described in this manual. Adhere strictly to the described procedures and observe all relevant safety precautions. Otherwise, personal injury and/or spectrometer damage can be the result. In this case, Bruker does not assume any liability. Maintenance and repair works that are not described in this manual should only be performed by Bruker service personnel. (For service addresses and telephone numbers refer to appendix I.) Caution: Avoid electrostatic discharges (ESD) to prevent ESD sensitive electronic components from being damaged. Electronic components (like semiconductor chips and boards) are very susceptible to electrostatic discharges caused by the operator. Even the slightest electrostatic discharge that is imperceptible to the operator can damage electronic components. Therefore, it is of crucial importance that you are connected to ground with respect to the spectrometer before you touch any electronic component inside the spectrometer. Electrical grounding can be accomplished either by using a grounded wrist strap or touching a grounded object (e.g. radiator). The grounded wrist strap is the most effective (and the preferred) grounding method. Note: After having exchanged a defective optical component e.g. laser unit, light source we recommend running the OQ test using the OVP software to check the spectrometer performance. (For the test procedure refer to the OPUS Reference Manual.)

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MAINTENANCE AND REPAIR Evacuating the MCT Detector Dewar

EVACUATING THE MCT DETECTOR DEWAR


..........................................................

General Information
Most liquid nitrogen cooled detectors are mounted in re-pumpable vacuum dewars (except for those which are sealed permanently). Evacuating the detector dewar becomes necessary if the hold time decreases considerably (i.e. a hold time of less than four hours). The existence of condensation water on the detector outside indicates that the dewar must be evacuated soon. If there is frost on the detector outside the dewar must be evacuated immediately. Before evacuating the dewar, the detector must be removed from the spectrometer. To evacuate the dewar the following evacuating equipment is required:

turbo molecular pump / oil-free high-vacuum pump (that generates an vacuum of


at least < 10-5mbar)

vacuum adapter
Note: Bruker offers suitable evacuating equipment (# S105-V). In case you do not want to purchase this equipment, Bruker also offers the service of evacuating the MCT detector (# D128). So, alternatively you can send the complete MCT detector in to Bruker. A B C D

Figure 42: a) Vacuum Adapter

b) Vacuum Adapter with flexible Metal Hose and Flange

Component A B C D
58

Vacuum Adapter (D126) Flange Flexible Metal Hose NW 25 Flange


VERTEX 70v User Manual

MAINTENANCE AND REPAIR Evacuating the MCT Detector Dewar

Evacuation Procedure
1 2 3 4 Remove the MCT detector from the spectrometer. See chapter Operation, section Exchanging the Detector. Connect the connecting piece of the vacuum adapter (E in figure 43) to the vacuum pump. (The connecting piece has an OD of 9.7mm.) Pull the knob (H in figure 43) to the open position and loosen the coupling nut (A in figure 43). Push the vacuum adapter carefully over the connection nozzle of detector dewar and fasten the coupling nut finger-tight. Additional tightening is not necessary. Push the knob in the closed position until the threaded rod (D in figure 43) of the vacuum adapter is in contact with the dewar evacuation valve. Screw the threaded rod in the evacuation valve closure of the dewar by turning the knob clockwise; 2 to 3 rotations are sufficient. Evacuate the vacuum adapter using the vacuum pump.

5 6 7

Note: The dewar should not contain any liquid nitrogen and should be at or slightly above room temperature (max. 60C). 8 Pull the knob to the open position in order to open the dewar evacuation valve. Evacuate the detector dewar using the vacuum pump.

Note: Evacuating the dewar takes several hours. Therefore, it is recommendable to evacuate the dewar overnight. The final pressure in the dewar should be less than 10-5 mbar. 9 10 11 When the desired vacuum is achieved, push the knob to the closed position in order to close the dewar evacuation valve. Vent the section between vacuum pump and vacuum adapter. Rotate the knob several turns counterclockwise in order to screw the threaded rod off the dewar evacuation valve. Be careful not to vent the dewar. Pull the knob to the open position, loosen the coupling nut and remove the vacuum adapter from the connection nozzle of the dewar. Reinstall the MCT detector in the spectrometer.

12 13

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MAINTENANCE AND REPAIR Evacuating the MCT Detector Dewar

A B

C D F G

closed open
Figure 43: Vacuum Adapter - Cross Section

Component A B C D E F G H Coupling nut O-ring retainer O-ring Threaded rod (to remove the valve closure of the detector dewar) Connecting piece for vacuum pump (OD = 9,7mm) Vacuum adapter Washer and O-ring packing Knob

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MAINTENANCE AND REPAIR Replacing the Laser Module

REPLACING THE LASER MODULE


..........................................................

General Information
The laser module needs to be replaced only if it is defective. A defective laser is indicated by a red LASER LED (fig. 10). For detailed information about fault diagnosis refer to chapter Troubleshooting, section Diagnostic Means. The replacement laser module consists of the laser tube and the laser power supply unit, i.e. in case of a defective laser you have to replace both components. For the order number of the replacement laser module refer to appendix B.

Safety Notes
The interferometer is equipped with a HeNe laser. This laser emits red light with a wavelength of 633nm. The rated power output is 1mW. According to EN 60825-1/ 10.2003, the laser is laser class 2 product. Laser class 2 means that the accessible laser radiation can cause eye injuries. Therefore, when replacing the laser, observe the following safety notes: Caution: Do not stare into the beam! A long-standing exposure to laser class 2 radiation can lead eye injuries. Always switch off the spectrometer and disconnect the power plug before beginning the laser removal. Be aware of the fact that the laser is active as soon as the spectrometer is switched on. Do not put the spectrometer into operation if the covers are removed or show signs of damage.

Replacement Procedure
The laser module is accessible from the spectrometer rear side. For the exact location of the laser, see to chapter Overview, section Internal Components, fig. 15. Proceed as follows: 1 2 3 4 In case the spectrometer is evacuated, vent it first Switch off the spectrometer using the mains switch at the spectrometer rear side and unplug the power cord. See chapter Installation, fig. 2. Remove the interferometer compartment cover. Remove the valve block cover shown in fig. 44 by loosening the two Allen screws (using a hex key, size 3mm) and pulling off the cover.

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MAINTENANCE AND REPAIR Replacing the Laser Module

Allen Screws

Valve Block Cover

Figure 44: Removing the Valve Block Cover

Disconnect the laser power supply cable from the laser module by loosening the two slotted screws at the green plug shown in figure 45 and pulling off the plug.

2 slotted screw (at the green plug)

Laser power supply cable

Figure 45: Disconnecting the Laser Power Supply Cable

Loosen the Allen screw (A in fig. 46) using the supplied hex key (size 3mm) and rotate the holding plate (B fig. 46) aside.

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MAINTENANCE AND REPAIR Replacing the Laser Module

Figure 46: Laser module - Top view

Grasp the laser module with both hands as shown in fig. 47 and pull it out of the holder. (Note: To do this, you have to apply some force in order to overcome the holding force of the fixing pins.)

Fixing pins

Figure 47: Removing the Laser Module

Install the replacement laser module and connect the laser power supply cable. (See step 3 to 4.)

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MAINTENANCE AND REPAIR Replacing the Laser Module

Important: When inserting the replacement laser module in the spectrometer pay attention to the following potential installation errors: Insert the laser module in such a way that the white labels at both laser tube ends (fig. 48a) do not come in contact with the two locking pins. Otherwise, the laser beam will be out off alignment. Make sure that the outlet of the black cable is orientated as shown in fig. 48b.

White labels

Laser tube

Cable outlet

Figure 48: a) Replacement Laser Module (side view)

b) Laser Module (front view)

9 10

Reinstall the valve block cover. (See step 2.) Reconnect the spectrometer to the power supply and switch on the spectrometer. (See step 1.)

Laser Parameter Reset


After having replaced the laser, do not forget to reset the laser parameters (operating time and laser dropouts, if necessary) using the OPUS software. To do this, proceed as follows:

Select in the OPUS Measure menu the Optic Setup and Service function. A dialog
window opens. Click on the Service tab and then on the Laser Replaced (Rest Parameters) button. (See fig. 49.) Alternatively, either click on the green status light (at the right end of the status bar) or select in the Measure menu the Optics Diagnostics function. The Instrument Status window opens. Click the on HeNe laser icon and then on the Service Info button. The diagnostics page of the HeNe laser opens. (See chapter Troubleshooting, fig. 60.) Click on the Reset button.

If the previous laser has shown sporadic power fluctuations, these fluctuations
have been recorded automatically by an internal counter. After having replaced the laser, reset this counter to 0 by clicking on the Reset Laser Dropouts button, OPUS dialog window Optic Setup and Service page Service. (See fig. 49.)
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MAINTENANCE AND REPAIR Replacing the Laser Module

Laser parameters Source parameters

Figure 49: OPUS dialog window - Optic Setup and Service

Note: After a laser replacement, it is highly recommended to perform an OQ test using OVP. For detailed information about this topic refer to the OPUS Reference Manual.

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MAINTENANCE AND REPAIR Replacing a defective IR Source

REPLACING A DEFECTIVE IR SOURCE


..........................................................

General Information
The basic spectrometer configuration is equipped with a MIR source (standard). Optionally, a NIR source can be installed inside the spectrometer. The replacement procedure is identical for both IR sources. The IR sources are pre-aligned and electrically coded enabling the spectrometer firmware to auto-detect the source type. This information is passed on to the OPUS software. This feature is called ACR (Automatic Component Recognition)1. Its purpose is to prevent you from selecting a wrong component in OPUS when you set up a measurement. (Note: A wrongly selected component is indicated in OPUS by a red colored entry field of the corresponding drop-down list. See also the OPUS Reference Manual.)

Safety Notes
During the spectrometer operation, the IR source becomes very hot. Therefore, after having switched off the spectrometer, wait until the IR source has cooled down sufficiently before you remove it. Caution: Avoid any skin contact with a hot IR source. Risk of skin burn!

Replacement Procedure
The IR sources are situated in the interferometer compartment. See chapter Overview, figure 15. The replacement procedure is identical for both IR source types, MIR and NIR source. 1 2 3 Switch off the spectrometer. Take off the interferometer compartment cover. Wait until the IR source has cooled down sufficiently. Loosen the knurled thumb screw of the release lever (approx. one turn). See figure 50.

1. ACR is restricted only to the optical components beamsplitter, detector and source.

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MAINTENANCE AND REPAIR Replacing a defective IR Source

Release levers

Knurled thumb screws

Figure 50: IR Sources

4 5 6

Press the IR source slightly downwards while swiveling the release lever aside. Take out the IR source. Insert the replacement IR source into the seating hole. Note that the two pins shown in figure 51 have to snap in the corresponding holes at the IR source bottom side to ensure the correct position of the source.

Pins

Source seating hole

Figure 51: Installing a MIR Source

Gently press the IR source downwards and swivel the release lever over the source to secure it. A beep indicates that the source has been recognized by the electronics. Tighten the knurled thumb screw of the release lever. Place the cover again on the interferometer compartment. Switch on the spectrometer. Check whether a signal is detected and the optics works correctly using the OPUS software.

8 9 10 11

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MAINTENANCE AND REPAIR Replacing the Fuses

Source parameter Reset


After having replaced the source, reset the operating hour meter. Proceed as follows:

Select in the OPUS Measure menu the Optic Setup and Service function. The
corresponding dialog window opens. Click on the Service tab and then on the Source Replaced (Rest Parameters) button. (See figure 49.)

Alternatively, either click on the green status light (at the right end of the status
bar) or select in the Measure menu the Optics Diagnostics function. The Instrument Status window opens. Click the on source icon and then on the Service Info button. The diagnostics page of the source opens. (See figure 61.) Click on the Reset button. Note: After a source replacement, it is highly recommended to perform an OQ test using OVP. For detailed information about this topic refer to the OPUS Reference Manual.

REPLACING THE FUSES


General Information

..........................................................

If the voltage status LEDs (A in fig. 83) at the spectrometer rear side do not light, although the spectrometer is switched on (assuming sufficient power is supplied to the spectrometer), a blown fuse of the spectrometer mains power supply can be the cause. The fuse box is at the spectrometer rear side below the mains switch. (See figure 52a.)

Replacement Procedure
1 2 Switch off the spectrometer by turning the mains switch to the O position (figure 52a) and unplug the spectrometer power cable. Open the fuse box flap by inserting a small flat-ended screwdriver into the groove and gently prying out the fuse block flap. (See figure 52b.) Turn the fuse box downwards. (See figure 52c.) The fuse box contains two fuses. Replace both fuses with 5x20 mm fuses with a rated current of 4A, slow blow (according to IEC 60 127-2).

Note: We recommend fuses of the manufacturer WICKMANN. (See www.wickmannusa.com). Alternatively, you can order single fuses at BRUKER. 4 5 6
68

Close the fuse box by turning the box upwards and pressing it against the housing until the spring clip engages. Reconnect the spectrometer to the mains. Switch on the spectrometer.
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MAINTENANCE AND REPAIR Replacing the Sample Compartment Windows

Mains Switch Fuse Box

Figure 52: a) Fuse Box

b) Opening the Fuse Box

c) Opened Fuse Box

REPLACING THE SAMPLE COMPARTMENT WINDOWS


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General Information
Provided the sample compartment of your spectrometer is equipped with windows, they are mounted either on the sample compartment walls or on flaps which can be move in and out of the beam path. With the flaps in the beam path, the windows separate the sample compartment from the detector compartment and the beam direction control compartment. The flap movement is computer-controlled. In the course of time, the opaqueness of the windows can reach such a degree that the transparency (infrared transmittance) is seriously reduced. If this is the case, the windows need to be replaced. Note: When installing new windows, make sure that their transmission range corresponds with the spectral range of the other installed components (detector and beamsplitter). For information about the transmission range of the available window materials refer to the table below. The spectral range of the available detectors and beamsplitters is listed in the corresponding tables in chapter Overview, section Internal Components.

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Handling Instructions
The windows are very fragile. Moreover, contaminations on the window surface can decrease the transparency significantly. Therefore, follow the following instructions: Caution: Handle the windows with great care because they are made of fragile material that cracks under influence of mechanical pressure. Do not touch the window surface. This may lead to irreversible contamination.

Safety Notes
Some window materials are harmful or (very) toxic. (See the following table.) During normal operation, these window materials do not pose a health risk. However, should these windows break, be extremely careful. Avoid generating dust. Warning: Observe the safety instructions on the packaging, and the safety data sheets attached. Non-observance may cause serious health problems or even death. The following table lists the available window materials including their transmission range, refraction index and chemical properties. Material Quartz (Infrasil) SiO2 Silicon Si Calcium Fluoride CaF2 Barium Fluoride BaF2
CAUTION - HARMFUL!

Transmission Range (cm-1)* 57,000 - 2,800 10,000 - 100 66,000 - 1,000

Refraction Index n (at 2000cm-1) 1.46 3.42 1.40

Chemical Properties Insoluble in water; soluble in HF Insoluble in most acids and bases; soluble in HF and HNO3 Insoluble in water; resistant to most acids and bases; soluble in NH4 salts Low water solubility; soluble in acid and NH4Cl Hygroscopic; slightly soluble in alcohol and NH3 Soluble in strong acids and in HNO3 Insoluble in water; soluble in NH4OH Soluble in water, alcohol, and glycerine; hygroscopic

50,000 - 800

1.45

Sodium Chloride NaCl Zinc Selenide ZnSe


CAUTION - TOXIC!

28,000 - 580 20,000 - 500

1.50 2.43

Silver Chloride AgCl


CAUTION - HARMFUL!

23,000 - 400

2.00

Potassium Bromide KBr

33,000 - 280

1.54

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MAINTENANCE AND REPAIR Replacing the Sample Compartment Windows Transmission Range (cm-1)* 33,000 - 180 Refraction Index n (at 2000cm-1) 1.74

Material Cesium Iodide CsI


CAUTION - HARMFUL!

Chemical Properties Soluble in water and alcohol; hygroscopic Soluble in warm water and bases; insoluble in acids Resistant to most solvents Soft crystal; insoluble in water; darks upon exposure to UV radiation

KRS-5 (TIBr/I thallium bromide-iodide)


CAUTION - VERY TOXIC!

16,000 - 250

2.38

Polyethylene PE (high density) Silver bromide AgBr


CAUTION - HARMFUL!

600 - 10 22,000 - 300

1.52 2.22

* 50% value at a window thickness of 4mm

Replacement Procedure for Windows mounted on Flaps:


1 2 Take off the sample compartment cover. To gain access to the flaps, first remove the cover by loosening the two Allen screws using a hex key (size 2mm). See figure 53.

Cover Allen screws

Figure 53: Removing the Cover

3 4 5 6

Remove the window retaining ring by loosening the three slotted screws. See figure 54. Take out the window and install the new one. Attach the window retaining ring by fastening the three slotted screws. See figure 54. Reinstall the cover using the two Allen screws. See figure 53.
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Retaining ring

Slotted Screws

Window

Figure 54: Replacing a Window

Replacement Procedure for Windows mounted on the Sample Compartment Walls:


1 2 Take off the sample compartment cover. Remove the complete window assembly by loosening the three Allen screws using the hex key (size 2mm) See figure 55. (The window assembly consists of the retaining ring, the window and the flange ring. See figure 56b)

Allen screws

Figure 55: Removing the Window Assembly

3 4

Loosen the three slotted screws shown in figure 56a and remove the retaining ring. Take the window out of the flange ring and insert a new one.

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Slotted screws

Retaining ring

Flange ring

Figure 56: Window Assembly (a) assembled

(b) disassembled

Reassemble the window assembly and attach it to the sample compartment wall. (Note: While reassembling the window assembly, tighten the slotted screws alternately.)

CLEANING THE INSTRUMENT

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Only the outer surface of the spectrometer can be cleaned with a dry or damp cloth. Do NOT use detergents with organic solvents, acid or base! Warning: Do not clean the spectrometer interior. This may lead to serious spectrometer damage.

MAINTAINING THE VACUUM PUMP


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The vacuum pump needs to be maintained regularly. For detailed information about the maintenance procedure and service intervals refer to the supplied vacuum pump user manual.

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T.ROUBLESHOOTING. . . . . . . . . . . . . . . . . . ..................
GENERAL INFORMATION
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This chapter describes the most common potential spectrometer problems, their possible causes and recommended solutions.1 Depending on how a spectrometer problem becomes apparent, they are subdivided into the following categories:

Spectrometer problem indicated by the spectrometer status indicator Spectrometer problem indicated by an instrument status message in OPUS or
other OPUS messages

No interferogram displayed in the OPUS dialog Check Signal A failed OVP test Spectrometer problem indicated by various diagnostic LEDs at the spectrometer
rear side (e.g. ERR LED, voltage status LEDs)

No data transfer between spectrometer and computer


The available diagnostic means (e.g. spectrometer status indicator, error messages in OPUS, diagnostics pages of the firmware) enable the operator to identify and solve many spectrometer problems without requiring the support of the Bruker service, or at least to narrow down a problem. If the solutions listed below do not solve a problem contact the Bruker service. (For service addresses and telephone numbers refer to appendix I.) With OPUS version 6 or higher, it is possible to send the complete spectrometer status report by e-mail to the Bruker service. This report allows the Bruker service technician a first remote fault diagnostics. To do this, proceed as follows: 1 Click on the OPUS status light. (The status light is in the lower right corner of the OPUS interface.) The Instrument Status dialog window opens. Click on the Send Report button. (See figure 58.) The report is sent by e-mail to opusreports@brukeroptics.de.

Note: This function requires an e-mail program installed on your computer and a set-up mail account. In addition, your spectrometer needs to be connected to a network computer.

1. Not all possible spectrometer problems and causes are listed in this chapter. If the recommended solutions do not solve the problem, contact your local Bruker service. For service addresses and telephone numbers refer to appendix I.

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DIAGNOSTIC MEANS

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For a spectrometer fault diagnosis, the following diagnostic means are available: Spectrometer status indicator on the spectrometer top side OPUS dialog window Instrument Status Instrument status messages in OPUS Diagnostics pages for the following spectrometer components: laser, source, interferometer1, electronic, automation and detector

Several diagnostic LEDs at the spectrometer rear side

Spectrometer Status Indicator Board


The status indicator board (figure 57) is in the left rear corner on the spectrometer top side.

Figure 57: Status Indicator Board

These LEDs can light up in different colors. Depending on the LED in question, they indicate the following status/condition: VACUUM LED The color of VACUUM LED depends on the current pressure situation inside the individual spectrometer compartments. LED is off. LED flashes green. LED lights up green. LED flashes yellow. Sample compartment and optical bench are vented. Sample compartment and optical bench are being either evacuated or vented. Sample compartment and optical bench are evacuated. The ultimate vacuum is achieved. Sample compartment is being either evacuated or vented. (In case the sample compartment is already vented, it flashes yellow also when the optical bench is being vented.)

1. The terms Interferometer and Scanner are used synonymously.

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TR O U B L E S H O O T I N G Diagnostic Means LED lights up yellow. LED lights up red. Sample compartment is vented. When the spectrometer is being evacuated, but a certain threshold pressure value is not reached within a certain period of time (i.e. the ultimate vacuum is not achieved). A red VACUUM LED indicates a problem. LASER LED LED lights green. LED lights up red. Laser is OK. Possible causes are: Laser power is too weak. Laser beam is blocked. Laser module is defective. Laser tube is out of alignment. STATUS LED LED lights green. LED lights up red. Spectrometer is OK. Possible causes are: Spectrometer is still initializing. There is a general spectrometer problem (e.g. a defective spectrometer component).

Note: The diagnostic LED Status corresponds for the most part with the instrument status indicator in OPUS. (The difference between both is that the spectrometer Status LED does not light up yellow whereas the instrument status indicator in OPUS does.) The instrument status indicator is in lower right corner of the OPUS user interface. For detailed information about it, refer to the OPUS Reference Manual. For detailed information about the diagnostic LEDs of the status indicator board refer to chapter Overview, section External Components.

OPUS Dialog Window Instrument Status


The OPUS dialog window Instrument Status allows you to diagnose which spectrometer component has caused the failure or to find out whether an OVP test1 has expired or failed. To perform a fault diagnosis, proceed as follows:

1. OVP test is a collective term for all tests (e.g. OQ, PQ, PHEUR2240) that can be performed with OVP. OVP (OPUS Validation Program) is part of OPUS. The general purpose of these OVP tests is to check whether the spectrometer system achieves the specified performance. For detailed information about OVP refer to the OPUS Reference Manual.

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TR O U B L E S H O O T I N G Diagnostic Means

Either click on the OPUS status light or select in the OPUS Measure menu the Optics Diagnostics function. The following dialog window opens:

Figure 58: Optics Diagnostics - Instrument Status dialog

A The status of the hardware components, e.g. source, laser, interferometer etc. is displayed in the upper icon line. The status can be as follows:

Green check mark: Component is okay.

WARNING (light blue): The exact meaning of a warning depends on the component in question. For example, in case of the source, a warning means: End of the specified lifetime of the component is nearly reached. In this case, measuring is still possible. ERROR (red): Component is defective. In this case, measuring is no longer possible.

B The second row of icons refer to the possible active test channel and indicates the result of the last OVP test performed. The results can be as follows:

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PASSED (green): OVP test passed. Test is still valid.

EXPIRED (light blue): The validity period of an OVP test has expired. What to do in this case? Perform the OVP test in question. (See OPUS Reference Manual.) FAILED (red): OVP test failed. What to do in this case? Try to find out the cause of a failed OVP test by performing a systematic fault diagnosis. Solve the problem and then repeat the OVP test in question.

To perform a fault diagnosis of a particular spectrometer component click on the respective icon in the first row of the Instrument Status dialog. The Instrument Status Message dialog opens. (See figure 59.)

Instrument Status Messages in OPUS


Some spectrometer problems are indicated additionally by a corresponding instrument status message displayed in OPUS. (See fig. 59) These messages appear when you click on the icon of the optical component in question in the Diagnose window.
Status indication for the component in question (green: OK, yellow: warning, red: error)

Component in question

Status message for the component in question

Figure 59: Instrument Status Message in OPUS indicating a Source Problem

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Diagnostics Pages
When you click on the Service Info button (figure 59), the diagnostics page for the component in question opens. The diagnostics pages of the spectrometer firmware contain all relevant information about the current operating state of the respective spectrometer component. In the following figures, the information important for fault diagnostics are highlighted by a rectangle. The following figures show the diagnostics pages of the spectrometer components listed above. These pages provide information relevant to fault diagnostics.

Current reading of the laser operating hour counter

Date of initial laser operation

Figure 60: Laser Diagnostics Page

Figure 61: Source Diagnostics Page

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Figure 62: Scanner Diagnostics Page

Figure 63: Electronics Diagnostics Page

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e.g. Flaps

Note: A missing cross indicates a disconnected flap.

Figure 64: Automation Diagnostics Page

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Figure 65: Detector Diagnostics Page

Voltage Status LEDs


The voltage status LEDs (A in figure 83) are at the spectrometer rear side, labeled +5V, +12V and -12V. These diagnostic LEDs indicate the state of the secondary voltages of the electronics unit.

Diagnostic LEDs RX and TX


These LEDs (S and T in figure 82) indicate the data transfer direction between the spectrometer and the data system via the Ethernet connection. In case of the standalone configuration, the green RX LED signals that the spectrometer receives data. In case the spectrometer is connected to an Ethernet network, the green RX LED indicates that a data packet is transmitted on the Ethernet. (It does not necessarily mean that the data packet is destined for the spectrometer!) The yellow TX LED lights when the spectrometer transmits a data packet. This indicates that the spectrometer is accessed by a computer.

Diagnostic LEDs SR and SG


These two LEDs (red SR LED and green SG LED, P and Q in figure 82) indicate the internal operating state of the spectrometer communication processor. (The abbreviation SR stands for Status Red and SG for Status Green.) If the SR LED lights up the spectrometer is busy and not ready for communication.

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Diagnostic LED ERR


The red ERR LED (K in figure 82) indicates an interferometer error (e.g. a missing laser signal). As long as this LED lights, data acquisition is not possible.

Diagnostic LED CR, CY and CG


These LEDs (D, E and F in figure 82) are status and diagnose LEDs for the step scan option. They indicate the status of the controlling device. (The abbreviation CR stands for Controller Red, CY for Controller Yellow and CG for Controller Green.) (For detailed information refer to the Step Scan Manual.)

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PROBLEM - POSSIBLE CAUSE - SOLUTION


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Spectrometer problem indicated by spectrometer status indicator.


RED VACUUM LED During a spectrometer evacuation, a red VACUUM LED indicates that the ultimate vacuum inside the spectrometer is not reached (i.e it lights up red if a certain threshold pressure value is not reached within a certain period of time). Possible causes There is a leakage that allows air to enter the spectrometer. During the evacuation, a leakage may become apparent by a hiss. Possible leakages are: sample compartment cover has not been placed correctly on the spectrometer, flaps do not close properly, the wing-shaped cover is not secured properly (after the beamsplitter has been exchanged), a beam port cover is not reinstalled properly (after an accessory has been removed from an IR beam port). Vacuum pump is defective. Vacuum pump is not connected properly. Solutions Find the leakage and close it. (In case of defective flaps contact the Bruker service. See appendix I.)

See the user manual of the vacuum pump. Check the vacuum pump connection. (For information about how to connect the vacuum pump to the spectrometer refer to chapter Installation, section Connecting the Vacuum Pump.) Contact the Bruker service. (See appendix I.)

Venting valve(s) do(es) not close. This problem is accompanied by a hissing sound at the spectrometer rear side.

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RED LASER LED Possible causes Spectrometer is still initializing. (In this case, there is no spectrometer problem.) Laser beam inside the interferometer compartment is blocked.
Note: This problem is indicated by the following instrument status message HeNe-Laser is off or no laser signals.

Solutions Wait until the spectrometer has completed the initialization successfully (i.e. the LED turns to green). Contact the Bruker service. (See appendix I.)

After a laser replacement, the laser beam is out of alignment due to the white labels at both laser tube ends (fig. 48a) being in contact with the fixing pins (fig. 47). Laser tube is not orientated correctly.

Install the laser correctly as described in chapter Maintenance and Repair, section Replacing the Laser Module. Correct the laser tube orientation as shown in fig. 48b. (See chapter Maintenance and Repair, section Replacing the Laser Module.) Have a look at the laser diagnostic page. (See section Diagnostics Pages.) In case of a defective laser: order a replacement laser module (For the order number of the spare part, refer to appendix B.) replace the laser module as described in chapter Maintenance and Repair, section Replacing the Laser Module. If the average laser lifetime is exceed (significantly) the laser module needs to be replaced. To do this: order a replacement laser module (For the order number of the spare part, refer to appendix B.) replace the laser module as described in chapter Maintenance and Repair, section Replacing the Laser Module.

Laser is defective.
Note: This problem is indicated by the following instrument status message HeNe-Laser is off or no laser signals.

Laser signal is too weak because the average laser lifetime is nearly over.
Note: In this case, the OPUS message End of average life time is nearly reached, spare part will be required appears.

RED STATUS LED A red STATUS LED indicates a spectrometer problem which can be caused by a number of spectrometer components (e.g. laser, source, detector). In order to be able to narrow down the problem, it is highly recommended to open the OPUS dialog window Instrument Status. See figure 58.
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Possible causes Spectrometer is still initializing. (In this case, there is no spectrometer problem.) If the laser is the cause of the problem either: the laser beam is blocked or the laser tube is not orientated correctly or the laser is defective.
Note: These causes are also indicated by a red LASER LED.

Solutions Wait until the spectrometer has completed the initialization (i.e. the LED turns to green). Blocked laser beam: Contact the Bruker service. (See appendix I.) Incorrect laser tube orientation: Correct the laser tube orientation as shown in fig 48. See chapter Maintenance and Repair, section Replacing the Laser Module. Defective laser: Order a replacement laser. (For the order number of the spare part, refer to appendix B.) Replace the laser as described in chapter Maintenance and Repair, section Replacing the Laser Module. Check whether the source is installed properly. If the source is defective it needs to be replaced. Proceed as follows: order a replacement source (For the order number of the spare part, refer to appendix B.) replace the source as described in chapter Maintenance and Repair, section Replacing a defective IR Source. Cool down the MCT detector by filling liquid nitrogen into the detector dewar. (See chapter Operation, section Cooling an MCT Detector.) Check whether the detector is installed correctly. (See chapter Operation, section Exchanging the Detector.) To narrow down the cause of the problem, see section below Spectrometer Problem indicated by an Instrument Status Message, messages regarding the interferometer. If an unlocked beamsplitter is the cause of the problem lock it. See chapter Operation, section Exchanging the Beamsplitter. Check whether the voltage status LEDs labeled +5V, +12V and -12V (A in fig. 83) at the spectrometer rear side are on. (See also section Voltage Status LEDs below in this chapter.) In case of a defective power supply unit contact the Bruker service. (See appendix I.)
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If the source is the cause of the problem it is either not installed or defective.
Note: This problem is indicated by the following instrument status message Source is broken or not connected.

If the detector is the cause of the problem it is either not cooled down (instrument status message: Detector not ready) or it is not installed correctly (instrument status message: Device not connected. No analog board selected). If the interferometer is the cause of the problem there are a number of possible causes. For example, the beamsplitter is not locked. This problem is also indicated by the instrument status message BMS door is open in OPUS.
(Note: In case there is no beamsplitter installed at all, also the LASER LED is red.)

If the electronics is the cause of the problem the electronics unit is defective or there is a short circuit, for example.

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Possible causes

TR O U B L E S H O O T I N G Problem - Possible Cause - Solution

Solutions To narrow down the cause of the problem, open the Automation Diagnostics Page (figure 64) in OPUS. See also section Spectrometer Problem indicated by an Instrument Status Message below in this chapter; Instrument status messages regarding the automation. If you can not solve the problem contact the Bruker service. (See appendix I.)

If the automation is the cause of the problem there are a number of possible causes.

Spectrometer Problem indicated by an Instrument Status Message


INSTRUMENT STATUS MESSAGE REGARDING THE LASER Instrument status message HeNe laser is off or no laser signal. Possible causes Laser tube is not orientated correctly. OR Power supply to the laser is interrupted because the green plug of the laser power supply cable is not plugged in at all or not secured properly. (See fig. 45.) OR Laser is defective. Order a replacement laser module and replace the defective laser module as described in chapter Maintenance and Repair, section Replacing the Laser Module. (For the order number of the replacement laser refer to appendix B.) Solutions Correct the laser tube orientation as shown in fig. .48. (See chapter Maintenance and Repair, section Replacing the Laser Module.) Plug in the green plugs and secure them properly by fastening the two slotted screws. See chapter Maintenance and Repair, section Replacing the Laser Module.

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Instrument status message End of average lifetime is nearly reached, spare part will be required.

Possible causes The end of the specified lifetime of the laser is nearly reached.

Solutions Order a replacement laser module. (For the order number refer to appendix B.) After the receipt, replace the laser module. (See chapter Maintenance and Repair, section Replacing the Laser Module.)
Note: Despite this warning message, measuring is still possible. To turn the OPUS status light green again click on the Ignore button in the Instrument Status Message dialog (fig. 59). The message will be repeated in certain intervals until you have replaced the laser module.

INSTRUMENT STATUS MESSAGE REGARDING SOURCE Instrument status message Source is broken or not connected. Possible causes Source is not installed at all or not installed properly. OR Solutions Install the source as described in chapter Maintenance and Repair, section Replacing a defective IR Source. Order a replacement source and replace the defective source as described in chapter Maintenance and Repair, section Replacing a defective IR Source. Order a spare source. (For the order number refer to appendix B.) After the receipt, replace the laser module. (See chapter Maintenance and Repair, section Replacing a defective IR Source..)
Note: Despite this warning message, measuring is still possible. To turn the OPUS status light green again click on the Ignore button in the Instrument Status Message dialog (fig. 59). The message will be repeated in certain intervals until you have replaced the source.

Source is defective (e.g. burnt out).

End of average lifetime is nearly reached, spare part will be required.

The end of the specified lifetime of the source is nearly reached.

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INSTRUMENT STATUS MESSAGE REGARDING THE INTERFEROMETER Instrument status message Scanner initialization mode. Possible causes This error message appears only if you try to start a measurement while the spectrometer is still initializing.
Note: Also other error messages can be displayed. As in this case there is not a spectrometer problem you can ignore them.

Solutions Before starting a measurement, wait until the spectrometer has completed the initialization successfully.

BMS door is open.

Beamsplitter is not installed properly (i.e. the beamsplitter release lever is not in the locked position). Interferometer is out of adjustment caused by strong vibrations, for example.

Put the beamsplitter release lever in the locked position. (See chapter Operation, section Exchanging the Beamsplitter.) Contact the Bruker service. (See appendix I.)

Laser-A timing error / Laser-B timing error OR Laser-A modulation too small / Laser-B modulation too small OR Laser signals modulation too small OR Laser period too slow or modulation too small

INSTRUMENT STATUS MESSAGE REGARDING DETECTOR Instrument status message Detector not ready. Possible causes The MCT detector is not cooled down to its operating temperature. Solutions Cool down the MCT detector by filling liquid nitrogen into the detector dewar. (See chapter Operation, section Cooling an MCT Detector.) Install the detector as described in chapter Operation, section Exchanging the Beamsplitter.

Device not connected. No analog board selected. OR No analog board found.

Detector is not installed.

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TR O U B L E S H O O T I N G Problem - Possible Cause - Solution INSTRUMENT STATUS MESSAGE REGARDING AUTOMATION Instrument status message Pressure in interferometer compartment is unstable. / Pressure in sample compartment is unstable.
Note: These messages are displayed if the defined ultimate pressure is not reached in the compartment in question when evacuating or venting it.

Possible causes A valve jams. OR Vacuum pump is defective / does not work properly. OR There is a leakage that allows air to enter the interferometer compartment. During the evacuation, a leakage may become apparent by a hissing sound. Possible leakages are: detector compartment cover / sample compartment cover has not been placed correctly on the spectrometer or the flaps do not close properly or the wing-shaped cover is not secured properly (after the beamsplitter has been exchanged) or an beam port cover is not reinstalled properly (after an accessory removal).

Solutions Contact the Bruker service. See appendix I. See the user manual of the vacuum pump. Find the leakage and close it. (In case of defective flaps contact the Bruker service.)

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OTHER ERROR MESSAGES IN OPUS Error message Error message from Optical Bench. Should this message be ignored? Fatal 50200 Flaps Device error.
Note: As a flap malfunction leads to unstable pressure conditions inside the spectrometer during venting or evacuating it, this kind of problem is also indicated by a red VACUUM LED and a red STATUS LED. Moreover, the instrument status message Pressure in interferometer compartment / sample compartment is unstable is displayed in OPUS as well. (See section Diagnostic Means.)

Possible causes Upon closing the flaps, a flap is blocked by an object. (For example, an object has got in the opening while you have worked in the sample compartment.) OR Flaps malfunction (i.e. one or both flaps do not open / close properly.) OR One or both flaps are not connected.

Solutions Check whether there is something that blocks the flaps. If so, remove it.

Contact the Bruker service. (See appendix I.)

To find out whether a disconnected flap is the cause of the problem, consult the automation diagnostics page. See fig. 64. If so, Contact the Bruker service.

If an error message appears which is not listed above contact the Bruker service. See appendix I.

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T h e r e i s n o I n t e r f e r o g r a m d is p l a y e d i n O P U S D i a l o g Check Signal
Assuming that, firstly, the computer can access the spectrometer and secondly, there is an optical connection between the interferometer outlet and the detector inlet, this problem can have the following possible causes: Possible Causes Optical path is blocked. Detector is not cooled down at operating temperature.
Note: This problem is indicated by the instrument status message Detector not ready.

Solutions Check whether the accessory in the sample compartment blocks the IR beam. Cool down the detector. In case of a liquid nitrogen cooled detector, fill liquid nitrogen into the dewar. (See chapter Operation, section Cooling an MCT Detector.) Manually Changed Detectors: Check whether the detector is inserted properly in its holder. (See chapter Operation, section Exchanging the Detector.) External detectors: Examine the cable connection at the detector as well as at the spectrometer rear side. Check whether the IR source is installed properly or replace the IR source, if it is defective. (See chapter Maintenance and Repair, section Replacing a defective IR Source.) Check whether the beamsplitter is properly installed. (See chapter Operation, section Exchanging the Beamsplitter.) Replace the beamsplitter and check the signal. (See chapter Operation, section Exchanging the Beamsplitter.)
Note: If a replacement beamsplitter is not available, you need to order a new one.

Detector is not or incorrectly installed.


Note: This problem is indicated by the instrument status message Device not connected. No analog board selected.

Defective or not correctly installed IR source.


Note: This problem is indicated by the instrument status message Source is broken or not connected.

Beamsplitter is not properly installed.


Note: This problem is indicated by the instrument status message BMS door is open.

Beamsplitter has become opaque or is damaged.

The red ERR LED on the spectrometer rear side lights up, i.e. there is a spectrometer error, for example, strong mechanical shocks have caused a temporary or permanent optics misalignment or the laser is defective. (In case of a defective laser, the LASER LED lights up red.)

In case of an optics misalignment, contact the Bruker service. In case of a defective laser order a replacement laser module. (For the order number refer to appendix B.) After the receipt, replace the laser module. (See chapter Maintenance and Repair, section Replacing the Laser Module.)

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Possible Causes

TR O U B L E S H O O T I N G Problem - Possible Cause - Solution

Solutions Check the voltage status LEDs on the spectrometer rear side. If none of the LEDs lights, the power supply unit probably needs to be replaced. Contact the Bruker service. See appendix I. Either reduce the light source intensity by using a smaller aperture or reduce the gain settings.

Defective power supply unit.

Detector oversaturation or ADC overflow

A failed OVP test


OVP test is a collective term for all tests (e.g. OQ test, PQ test, PHEUR2240) that can be performed with OVP (OPUS Validation Program). The general purpose of these OVP tests is to check whether the spectrometer system achieves the specified performance. For detailed information about OVP refer to the OPUS Reference Manual. Possible causes There is a sample in the spectrometer sample compartment which blocks the IR beam. Source performance has decreased because the end of its service lifetime is nearly reached.
Note: This problem is indicated by the following message End of average lifetime is nearly reached, spare part will be required. Note: To find out of which component - either laser or source - the end of the average lifetime is nearly reached, open in OPUS the Instrument Status dialog window (fig. 58) The component in question has the status WARNING.

Solutions Take the sample out of the sample compartment and repeat the OVP test. Order a replacement source. (For the order number refer to appendix B.) After receipt, replace the source as described in chapter Maintenance and Repair, section Replacing a defective IR Source.

Sample compartment windows are dirty or have become opaque.

Order new windows and replace them as described in chapter Maintenance and Repair, section Replacing the Sample Compartment Windows. Replace the beamsplitter as described in chapter Operation, section Exchanging the Beamsplitter. Install windows made from a material that corresponds with the spectral range of the other selected components. See chapter Maintenance and Repair, section Replacing the Sample Compartment Windows.

Beamsplitter is dirty, opaque or damaged.

Regarding the spectral range of the selected optical components source, beamsplitter and detector, the wrong sample compartment windows are installed in the sample compartment.

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TR O U B L E S H O O T I N G Problem - Possible Cause - Solution

Possible causes The spectral ranges of the selected optical components - source, beamsplitter and detector - do not correspond with each other.

Solutions Check whether the spectral ranges of the selected optical components correspond with each other. (For information about the spectral range of the available detectors and beamsplitters refer to chapter Overview, section Internal Components.) Evacuate the MCT detector dewar as described in chapter Maintenance and Repair, section Evacuating the MCT Detector Dewar. Reduce the air humidity content inside the spectrometer by either evacuating the spectrometer or purging it with dry air or nitrogen gas. See chapter Operation, section Evacuating and Venting the Spectrometer or section Purging the Spectrometer. Save the new peak position using the OPUS software. Proceed as follows: Select in the Measure menu the Advance Measurement function, click on the Check Signal tab. (Ensure that the option button Interferogram is activated.) If the peak position is constant save it by clicking on the Save Peak Position button. ... contact appendix I.) the Bruker service. (See

Ice formation in the MCT detector dewar.


Note: This problem becomes apparent by a failed ice band test. This test is part of the PQ test procedure.

Air humidity content inside the spectrometer is too high.


Note: This problem becomes apparent by a failed water vapor test. This test is part of the OQ test procedure.

Peak position has shifted.

If a failed OVP test has a different cause (e.g. detector sensitivity has weakened or interferometer is out of adjustment due to shock etc.) ...

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Voltage Status LEDs


ALL VOLTAGE STATUS LEDS ARE OFF Possible causes Spectrometer is not turned on. Power cord is not connected. No voltage is applied. Solutions Turn on the spectrometer using the mains switch. Connect the power cord to the power outlet as well as to the appliance inlet connector. Check whether the proper voltage is applied at the outlet to which the spectrometer is connected. Replace the fuse as described in chapter Maintenance and Repair, section Replacing the Fuses. Typically, a short circuit is accompanied by a ticking sound in the power supply unit. Disconnect the power supply unit immediately. If there are additional external circuitry connected to the CAN bus or the MPE port, disconnect them and try it again. If this measure solves the problem the external circuitry has caused the short circuit. Otherwise, it is an internal problem of the spectrometer electronics. Contact the Bruker service. (See appendix I.) If the voltage status LEDs do not light correctly, probably the power supply unit needs to be replaced. If they do not light at all, contact the Bruker service. (See appendix I.)

Defective fuse.

Short circuit in the power supply unit.

Defective power supply unit.

ONE VOLTAGE STATUS LED IS OFF Possible causes An external device shortens the power supply unit. Temporary short circuit in the spectrometer. Solutions Disconnect all external devices from the CAN bus or the MPE port and try it again. Switch off the spectrometer, wait about 30 seconds and switch it on again. After the initialization cycle the STATUS LED will turn to green.

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TR O U B L E S H O O T I N G Problem - Possible Cause - Solution

Possible causes A defective LED.

Solutions In this case, there is no spectrometer malfunction and the spectrometer operates properly. Only the defective LED needs to be replaced.

E R R L ED
Generally, a red ERR LED indicates a scanner malfunction, i.e. all components and/or conditions that are involved in the scanner functioning (laser, beamsplitter, air bearing pressure etc.) can cause a red ERR LED. Possible causes If the laser is the cause of the problem either the laser beam is blocked or the laser tube is not orientated correctly or the laser is defective.
Note: These causes are also indicated by a red LASER LED.

Solutions Blocked laser beam: Contact the Bruker service. (See appendix I.) Incorrect laser tube orientation: Correct the laser tube orientation as shown in fig. 48. See chapter Maintenance and Repair section Replacing the Laser Module. Defective laser: Order a replacement laser module. (For the order number refer to appendix B.) After the receipt, replace the laser module. (See chapter Maintenance and Repair, section Replacing the Laser Module.) Install a beamsplitter in the operating position or check whether the beamsplitter is locked properly (i.e. the release lever (fig. 34) has to be in the front position. (See chapter Operation, section Exchanging the Beamsplitter.) In case of an opaque or damaged beamsplitter replace it as described in chapter Operation, section Exchanging the Beamsplitter.
Note: Probably you need to order a replacement beamsplitter.

In case the beamsplitter is the cause of the problem either: no beamsplitter is installed in the operating position or the beamsplitter is not locked properly or it is damaged or has become opaque.
Note: The second cause is also indicated by the instrument status message BMS door is open.

Strong mechanical shocks have caused a permanent optics misalignment.

Contact the Bruker service. (See appendix I.)

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TR O U B L E S H O O T I N G Problem - Possible Cause - Solution

The SR LED lights permanently


The SR LED indicates whether the instrument is busy and not available for communication. Possible causes Spectrometer is still in the initialization phase. (In this case, there is no spectrometer problem.) Spectrometer control hangs. Solutions After having switched on the spectrometer wait about one minute until the initialization procedure is completed. Reset the spectrometer using the reset button (R in fig. 82) at the spectrometer rear side and wait for initialization to terminate. If this measure does not solve the problem, contact the Bruker service. (See appendix I.)

No Data Transfer between Spectrometer and Computer


In this case the troubleshooting procedure depends on the connection topology. The default connection (stand-alone configuration) is established using a crossover cable between the PC and the spectrometer 10Base-T Ethernet port (see appendix E, figure 79). Alternatively, the spectrometer can be connected directly to an Ethernet network using the 10Base-T port. The direction of the data transfer is indicated by the RX and TX LEDs on the spectrometer rear side. The TX LED lights during the spectrometer sends data and the RX LED lights during the spectrometer receives data. THE GREEN RX LED DOES NOT LIGHT AT ALL This indicates a problem with regard to the physical connection between the spectrometer and the PC or the network. Possible causes Wrong cable type is used. Solutions To connect the spectrometer directly to the PC use a CAT 5 crossover cable for the 10Base-T Ethernet standard. To connect the spectrometer to an existing network use a regular CAT-5 10Base-T cable (ask your network administrator). Check the RJ-45 connection to the Ethernet port (ETH) and at the other end of the cable. Replace the cable, if necessary. Check the main power supply. At least the voltage status LEDs +5V, +12V and -12V must light when the spectrometer is switched on.
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Defective cable or unstable connection.

Spectrometer does not start up.

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TR O U B L E S H O O T I N G Problem - Possible Cause - Solution DURING THE CONNECTION ESTABLISHMENT THE GREEN RX LED LIGHTS BUT THE YELLOW TX LED DOES NOT There is no logical connection between the spectrometer and network or computer. Possible causes Wrong IP address has been assigned to the spectrometer. Solutions Assign the correct IP address to the spectrometer. You find the correct IP address on a label on the spectrometer rear side. (See figure 82.) For detailed information refer to appendix E. Refer to appendix E.

TCP/IP settings mismatch between spectrometer and computer/network.

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S.PECIFICATIONS. . . . . . . . . . . . . . . . . . . . . ...............
Spectrometer
Parameter
Weight Dimension Power Consumption

Specification
approx. 105kg (depends on the individual instrument configuration) 85cm (W) x 71cm (D) x 32cm (H) Spectrometer: 100 - 240 VAC 10%; 50 - 60 Hz; 80W typical, 180 W max. Vacuum pump: approx. 500 W Complete power consumption (but without data station): ca. 700 W VERTEX 70v is a protection class I product. standard: With the standard optical components (KBr beamsplitter, DLaTGS detector and MIR source) the following spectral range is achieved: Middle IR: 8,000 to 350cm-1 optional: With the corresponding optional optical components, the following spectral ranges can be achieved: Far IR/THz: 680 to 10cm-1 Near IR: 15,500 to 4,000cm-1 UV/VIS: 28,000 to 9,000cm-1

Spectral Range

Spectral Resolution

standard: better than 0.4cm-1 (apodized) optional: better than 0.2cm-1 (apodized) better than 0.01cm-1 @ 2,000cm-1 better than 0.1% T

Wavenumber Accuracy Photometric Accuracy Scan Speed

standard: 0.1 to 3.75 cm/sec (opd - optical phase difference) optional: 0.1 to 10 cm/sec (opd - optical phase difference)
Operational temperature range of VERTEX 70v: 18 - 35C (64 - 95F)

Environmental Conditions

In case the vacuum pump is operated with installed noise reduction hood ensure the ambient temperature does not exceed 32C (90F).
Temperature variation: max. 1C per hour and max. 2C per day Humidity (non condensing): 80% (relative humidity) Installation site: in a closed room, max. 2000m above sea level Overvoltage category: II Degree of pollution: 2

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A
Parameter
Detector

SPECIFICATIONS

Specification
standard: High sensitivity DLATGS detector with KBr window optional: various detectors for measurements in the NIR, MIR, FIR, UV and VIS region (See also chapter Overview.) VERTEX 70v is a laser class 2 product containing a laser class 2 laser according to EN 60825-1/10.2003. Divergence angle: 1.77 mrad 5% Permanently aligned RockSolid interferometer 25.0cm (W) x 27.0cm (D) x 16.0cm (H) Optionally, the evacuable and purgeable sample compartment can be separated from the optical bench by KBr windows mounted on either the flaps or the sample compartment walls. Microprocessor-controlled optics bench with digital speed control, system diagnostics, advanced system check, 80 kHz A/D converter with 24 bit dynamic range. Industry standard Ethernet connection Vacuum-tight cast aluminum housing Evacuable below 0.2mbar

Laser

Interferometer Sample Compartment

Electronics

Housing Vacuum

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C.ONSUMABLE. .S. PARES. . . . . . . . . . . . . . . ............ ......


Spare Parts - Standard Components

Part # Q 328/7 Q 101/B

Description MIR source, mounted, 12 V, replacement unit HeNe laser module (laser tube plus laser power supply unit)

Spare Parts - Optional Components

Part # Q 428/7 Q 402 Q 302 Q 202/6

Description NIR source with QuickSwitch mount, 12 V average lifetime > 9000 hours NIR source (24V, 150W), connected externally and water-cooled MIR source (24V, 150W), connected externally and water-cooled FIR source (Hg-arc), connected externally and water-cooled

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CONSUMABLE SPARES

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D.EFAULT. .P ARAMETER. . . . . . . . . . . . . . . ....... ............

Note that depending on the spectrometer configuration, different default parameter sets may apply. In the following table you will find a list of the measurement parameters that apply to the standard spectrometer configuration (MIR). Select in the OPUS Measure menu the Select Measurement Parameters function and enter following measurement parameters.
Advanced Parameters Resolution Sample/Background Scan Time Save Data Result Spectrum Data Blocks to be saved Optics Parameter Source Setting Beam splitter Optical Filter Setting Aperture Setting Sample/Background Measurement Channel Detector Setting Scanner Velocity Sample Signal Gain Background Signal Gain Delay after Device Change Delay before Measurement Acquisition Parameters Wanted High Frequency Limit Wanted Low Frequency Limit Settings 4 6 scans from 7500 to 400cm-1 Transmittance Transmittance and Single Channel Settings MIR source (#1) KBr open 6mm Sample Compartment RT-DLaTGS (#1) 10 kHz automatic automatic 3 0 Setting 15.500cm-1 0cm-1

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DEFAULT PARAMETER

Advanced Parameters High Pass Filter Low Pass Filter Acquisition Mode Correlation Mode FT-Parameters Phase Correction Phase Correction Mode Apodization Function Zerofilling Factor

Settings open 10kHz Double Sided - Forward/Backward OFF Settings 32cm-1 Power Spectrum Blackman-Harris3-Term 2

The OPUS software provides the option to set the optics parameters Source Setting, Detector Setting and Measurement Channel also interactively using the schematic presentation of the beam path. To do this, click in the Setup Measurement Parameters dialog box on the Beam Path tab. The following window opens:

Figure 66: OPUS Dialog Window - Beam Path

To select the detector position 2, for example, place the cursor on this detector so that the label Detector 2 occurs and double-click on this position. The setting will switch to detector 2. See figure 67. As soon as you click on the Check Signal tab the spectrometer implements the settings.

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DEFAULT PARAMETER

Figure 67: Changing the Detector Position interactively

In this way, you can also change the Source Setting and Measurement Channel. Note: The parameters you have set in the schematic presentation of the beam path are realized automatically by the software also in the corresponding fields on the Optics page and vice versa.

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DEFAULT PARAMETER

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D.IMENSIONAL. D. RAWINGS. . . . . . . . . . . . ............ . .........

Figure 68: VERTEX 70v - Isometric View

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DIMENSIONAL DRAWINGS

Figure 69: VERTEX 70v - Top View

Figure 70: VERTEX 70v - Top View Showing Sample Compartment Dimensions

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DIMENSIONAL DRAWINGS

Figure 71: VERTEX 70v - Right Side View

Figure 72: VERTEX 70v - Left Side View

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DIMENSIONAL DRAWINGS

Figure 73: VERTEX 70v - Front View

Figure 74: VERTEX 70v - Rear View

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DIMENSIONAL DRAWINGS

Figure 75: VERTEX 70v - Sample Compartment Interior (Right Side View)

Figure 76: VERTEX 70v - Sample Compartment Interior (Front View)

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DIMENSIONAL DRAWINGS

Figure 77: VERTEX 70v - Sample Compartment Interior (Top View)

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C.ONNECTING. .VERTEX. .70 V. TO. .PC . ........... ......... ... .. ...


GENERAL INFORMATION
..........................................................
The connection of the spectrometer to a PC involves the following steps: 1 2 3 4 Defining a connection topology Defining the corresponding network addresses Assigning the network addresses Checking the connection

Depending on the connection typology, two different data cable types are required:

Data cable type

For realizing the following connection topology 1. Stand-alone topology, i.e. spectrometer is connected to a stand-alone PC. See fig. 79. 2. Spectrometer is connected to a network computer. See fig 81. 1. Spectrometer and PC are connected to a network. See fig. 80. 2. Spectrometer is connected to a network computer. See fig 81.

Included in the delivery scope

crossover cable

Yes (1 piece)

No
Note: A straight data cable, category 5, with RJ45 plugs for the Ethernet standard 10Base10 is required.

straight through cable

1 2 3

1 2 3

1 2 3

1 2 3

6
Straight through cable

6
Crossover cable

Figure 78: Schematic presentation of the different data cable types

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C O NN E CT I NG VE RT E X 7 0 V TO P C Possible Connection Topologies

POSSIBLE CONNECTION TOPOLOGIES


..........................................................
Basically, the following connection topologies are possible:

Connecting the spectrometer directly to a stand-alone PC (It is the standard


connection topology.) See fig. 79. Connecting both the spectrometer and PC to a network. See fig. 80. Connecting the spectrometer to a network computer. See fig. 81.

a) Configuration for stand-alone Operation (Standard)

Spectrometer
10.10.0.1 Crossover cable

PC
OPTIC CONNECTOR

10.10.0.100

Figure 79: Stand-alone Configuration of the Spectrometer

The spectrometer is connected directly to the standalone computer, i.e. neither the PC nor the spectrometer is connected to a network. By default, the supplied PC is equipped with two network interface cards labelled OPTIC CONECTOR and LAN. For the stand-alone configuration, connect the crossover cable to the OPTIC CONNECTOR at the PC rear side. See figure 79. Advantages:

Easy to install. Full bandwidth available for data transfer between the spectrometer and PC. No access conflicts with other PCs that try to access the spectrometer as well. No data transfer rate problems.

Disadvantages:

No remote access to the spectrometer from other PCs on which OPUS is


installed. No computer network connection. A local printer is required to print out the measurement results.

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C O N N E CT I N G V E RT E X 7 0 V T O P C Possible Connection Topologies

b ) C o n n e c t i n g b o t h S p e c t r o me t e r a n d P C t o a N e t w o r k :

Hub
Straight through Cables

Spectrometer

PC 1
LAN

PC 2
LAN

Figure 80: Integration of the Spectrometer into a 10Base-T Ethernet Network

Both the spectrometer and the PC, on which the OPUS software is installed, are connected directly to the network. By default, the supplied PC is equipped with two network interface cards labelled OPTIC CONECTOR and LAN. For this connection topology, connect the straight through cable(s) to the LAN connector at the PC rear side. See figure 80. Advantages:

Remote access to the spectrometer via the internet or the intranet is possible. The PC can access to all network resources (provided that you have the
corresponding access right). Disadvantages:

Data cables are required which are not included in the delivery scope of the
spectrometer. They have to be provided by your network administrator.

Only a fraction of the bandwidth is available for the data transfer between the
spectrometer and the PC. Due to data transmission delays, the measurement time may increase.

Access conflicts caused by other PCs that try to access the spectrometer as well. Your network administrator must be involved in configuring the connection.

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C O NN E CT I NG VE RT E X 7 0 V TO P C Possible Connection Topologies

c) Connecting the Spectrometer to a Network Computer:

Hub
Straight through cable

Spectrometer
LAN

PC 1
OPTIC CONNECTOR

Crossover cable
Figure 81: Integration of the Spectrometer into a 10Base-T Ethernet Network via a PC

This topology combines the advantages of the other two connection topologies, but it requires additional hardware (straight trough cable). By default, the supplied PC is equipped with two network interface cards labelled OPTIC CONECTOR and LAN. For this connection topology, connect the crossover cable to the OPTIC CONNECTOR and the straight through cable to the LAN connector at the PC rear side. See figure 81. Advantages:

Full bandwidth is available for the data transfer between the spectrometer and PC. Remote access to the spectrometer via internet or intranet is possible (provided
that you have the corresponding access rights).

The PC has access to all network resources (provided that you have the
corresponding access rights).

Different data transfer rates for the data exchange between the spectrometer
(10Base-T) and the network (no restriction) are possible. Disadvantages:

For connecting the PC to a hub, a straight through data cable is required which is
not included in the delivery scope of the spectrometer. It has to be provided by your network administrator.

Your network administrator must be involved in configuring the connection.

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C O N N E CT I N G V E RT E X 7 0 V T O P C Selecting Network Addresses

SELECTING NETWORK ADDRESSES


..........................................................
Depending on the connection topology, use the following network addresses:

a) Network Addresses for the Stand-alone Operation:


Spectrometer: IP-address Subnet Mask Gateway IP-address Subnet Mask Gateway 10.10.0.1 255.255.255.0 0.0.0.0 (no entry in case of Windows 2000 or XP) 10.10.0.100 255.255.255.0 0.0.0.0 (no entry in case of Windows 2000 or XP)

PC:

The delivered spectrometer and the delivered PC are factory-configured for the stand-alone operation, i.e. all network addresses for a stand-alone operation are already assigned, provided that you have acquired the PC by Bruker.

b) Network Addresses for connecting both Spectrometer and PC to a Network:


For this connection topology, both the spectrometer and the PC must have a unique IP address. These addresses depend on your intranet and have to be assigned by your network administrator. To ensure that the spectrometer can be accessed via internet also a gateway address has to be assigned. The gateway links your intranet domain to other domains (e.g. domains being part of the internet). Otherwise, set the gateway address to 0.0.0.0. In case of the operating system Windows 2000 or XP do not specify a Gateway. Note: A wrong IP address can cause problems with other devices connected to the network.

c ) N e t w o r k A d d r e s s e s f o r C o n ne c t i n g t h e S p e c t r o m e t e r t o a Network Computer
This connection topology requires two network interface cards and three addresses sets: the first set for the spectrometer, the second for the network interface card communicating with the spectrometer and the third for the network interface card linking the computer to the intranet.
Spectrometer: IP-address Subnet Mask Gateway 10.10.0.1 255.255.255.0 0.0.0.0 (no entry in case of Windows 2000 or XP)

PC and network interface card connected to the spectrometer: IP-address 10.10.0.100 Subnet Mask 255.255.255.0 Gateway 0.0.0.0 (no entry in case of Windows 2000 or XP) PC and network interface card connected to the network/hub: IP-address assigned by your network administrator Subnet Mask assigned by your network administrator Gateway assigned by your network administrator VERTEX 70v User Manual 119

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C O NN E CT I NG VE RT E X 7 0 V TO P C Assigning Network Addresses

ASSIGNING NETWORK ADDRESSES


..........................................................
This section describes how to assign an IP address to an instrument, not yet configured, using the FCONF program (Firmware Configuration). The program is part of the OPUS software. You will find it in the OPUS directory or directly on the OPUS CD. Note: Among other things, the FCONF program also allows for updating the spectrometer firmware. These program options are described in detail in appendix G.

Start the FCONF program.

Select the option Modify IP settings and click on the Next button.

Accept the settings by clicking on the Next button.


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Activate the radio button Assign a new address to the spectrometer and click on
the Next button.

The IP address assignment window opens:

Specify the MAC address (Media Access Control), the IP address and the
gateway address. The Help buttons provide information on what to enter in the different lines.

The MAC address is the unique hardware name of the network interface adapter
installed inside the spectrometer. You will find this address on the label at the spectrometer rear side (see the above figure.). In this example, the MAC address is 00 00 AD 02 AC 11. Enter this code into the first line of the IP assignment window.
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C O NN E CT I NG VE RT E X 7 0 V TO P C Assigning Network Addresses

If this label is missing or the MAC address proves to be incorrect, you will find this
address also on a label inside the electronics unit. It is placed on the black 26-pole connector at the EWS15-board. Note: Always keep the MAC address on the label at the spectrometer rear side up to date! Ensure that the MAC address on the label is legible.

The entries for the remaining three lines depend on the chosen connection
topology. For more information see section Selecting Network Addresses. The default entries are shown in the above figure. Use them for the direct connection of the spectrometer to the PC. After entering all addresses, click on the Next button.

Now you are asked to set the spectrometer into BootP-mode. Follow the
instructions on the screen.

Note: The reset button (R in figure 82) is on the spectrometer rear side.

When the spectrometer is in BootP mode, click on the Next button to start the
procedure. Otherwise, the BootP-mode will be canceled automatically after 2 minutes.

The assigning process starts immediately and may take several minutes. After a successful completion, a message appears and the spectrometer reboots
automatically.

Now the spectrometer starts up with the newly assigned IP setting and can be
accessed by the computer.

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C O N N E CT I N G V E RT E X 7 0 V T O P C Checking the Connection

CHECKING THE CONNECTION

..........................................................
To check the connection you can use either the internet explorer provided as part of Windows or any other internet browser program installed on your PC. Proceed as follows: 1 2 3 4 Switch on the spectrometer. Wait about one minute to allow the spectrometer to boot. A dark SR LED (P in figure 82) indicates that the spectrometer is ready. Start your internet browser. Check that the internet browser is not in offline mode. In case of the Microsoft Internet Explorer, the offline mode is indicated by a tick in front of Offline Mode in the File menu of the browser. Ensure that the internet browser does not use a proxy server, or at least not for addresses of direct access in the 10.10.x.x.-range. In case of the Microsoft Internet Explorer, you can check this by selecting the Internet Options function in the Extra browser menu. Click on the Connections tab. Then, click in the LAN-Settings group field on the Settings button. Enter the IP address of the spectrometer in the corresponding browser entry field (for stand-alone configuration: 10.10.0.1). Press the enter button.

6 7

Now the Internet Explorer should display the home page of your spectrometer. In case the Internet Explorer shows a blank page and is not able to access the instrument home page, check the IP address you have just assigned for correct spelling. If the problem is persistent, refer to chapter Troubleshooting.

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E.LECTRONICS. .AND. .P .OWER. .S. UPPLY . ............ ... . ..... ......


ELECTRONICS PANEL
..........................................................

The electronics panel at the spectrometer rear side includes cable connections (e.g. Ethernet connection) and LEDs. The LEDs serve for instrument diagnostics purposes. Each LED indicates a specific operating state (e.g. interferometer mirror movement, data transfer).

A B C D E

J K L M N O P

Q R

H I

T U V

Figure 82: Electronics Panel

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F
TRG PORT

ELECTRONICS AND POWER SUPPLY Electronics Panel

The 15-pin TRG port (A in figure 82) is intended for the connection of a triggering device. This port is only used in conjunction with the Step Scan option for step scan and time-resolved measurements. (The abbreviation TRG stands for Trigger.) (For detailed information refer to the Step Scan Manual.) EDIS PORT The EDIS port (B in figure 82) has no function at the moment. (The abbreviation EDIS stands for External Display.) PORT DDC 1/2/3/4 The ports DDC 1 to 4 (C, G, I and N in figure 82) are versatile ports to connect external optical modules and detectors. These ports include a complete CAN-Bus, transmits all required remote trigger signals and establishes a complete connection to DDC (Digital Detector Connection) compatible detectors. (Note that the DDC 4 port can not be used if a detector is connected to the DDC 4 port inside the spectrometer. In this case, a cap is fixed to the DDC 4 port.) CR, CY AND CG LEDS These LEDs (D, E and F in figure 82) are status and diagnose LEDs for the step scan option. They indicate the status of the controlling device. (The abbreviation CR stands for Controller Red, CY for Controller Yellow and CG for Controller Green.) (For detailed information refer to the Step Scan Manual.) LAS TEST The port LAS TEST (H in figure 82) is intended for service and diagnostic purposes only. Do not connect a device to this port! COM1 PORT The COM1 port (J in figure 82) is technically similar to a conventional, PC-compatible serial port, however, it does not have the complete functionality like serial port of a PC. It is only used for special applications. ERR LED The red ERR LED (K in figure 82) indicates an interferometer error (e.g. a missing laser signal). As long as this LED lights, data acquisition is not possible. See chapter 7 for troubleshooting. FWD LED The yellow FWD LED (L in figure 82) indicates the current interferometer mirror movement. As long as the interferometer mirror moves forward this yellow LED lights. During the backward movement the LED does not light. Thus, the LED flashes in the rhythm of the interferometer mirror forward and backward movement. This rhythm depends on the chosen measurement parameters (e.g. resolution and velocity). (The abbreviation FWD stands for forward.)
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ELECTRONICS AND POWER SUPPLY Electronics Panel TKD LED The green TKD LED (M in figure 82) indicates that the interferometer mirror is within the data acquisition range. Typically, it flashes with twice the frequency and synchronous to the FWD LED. During data acquisition the light intensity changes to bright green. (The abbreviation TKD stands for take data.) LPT1 PORT This parallel port (O in figure 82) is reserved for diagnostic purposes. Do not connect any device to this port! (The abbreviation LPT stands for Line Printer.) SR LED AND SG LED These 2 LEDs (red SR LED and green SG LED, P and Q in figure 82) indicate the internal operating state of the spectrometer communication processor. See also chapter 7. (The abbreviation SR stands for Status Red and SG for Status Green.) RES BUTTON The spectrometer is equipped with a reset button (R in figure 82) similar to the one you know from a PC. Pressing this button longer than 1 second resets the spectrometer without the need to turn it off. The effect is identical to switching the spectrometer off and on again. In addition, this button can be used to assign an IP address to the spectrometer. Refer to appendix E. TX LED AND RX LED These LEDs (S and T in figure 82) indicate the data transfer between the spectrometer and the data system via the Ethernet connection. In case of the stand-alone configuration, the green RX LED signals that the spectrometer receives data. In case the spectrometer is connected to an Ethernet network, the green RX LED indicates that a data packet is transmitted on the Ethernet (this does not necessarily mean that the data packet is destined for the spectrometer!) The yellow TX LED lights if the spectrometer transmits a data packet. This indicates that the spectrometer is accessed by a computer. Note: Use these LEDs to test the operational reliability of the Ethernet connection. 10BASE-T ETHERNET PORT The ETH port (U in figure 82) is primarily used to connect the spectrometer to a computer on which the application software (e.g. the OPUS software) is installed. The spectrometer can be connected either to a 10Base-T intranet or directly to the computer using a crossover cable (stand-alone configuration). This is a standard cable in which the TX and RX lines are cross-linked.

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ELECTRONICS AND POWER SUPPLY Power Supply Panel

VERTEX 70v is factory-configured for stand-alone operation. The IP address is on a label on the spectrometer rear side. The Ethernet port (ETH) is designed for RJ-45 plugs and complies with the 10Base-T standard. Use a CAT 5 cable (SSTP) to realize the connection; the cable length should not exceed 100 meters. Alternatively, a gateway can be used to connect the spectrometer to the internet. In this case a unique IP address must be assigned to the spectrometer. For detailed information on how to assign an IP address refer to appendix E. Note: Keep in mind that the interface speed is 10 Mbit/s. In this case a 100BASE-T connection does not work!

POWER SUPPLY PANEL

..........................................................

Figure 83: Power Supply Panel

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ELECTRONICS AND POWER SUPPLY Power Supply Panel VOLTAGE STATUS LEDS (+5V, +12V, -12V) These LEDs (A in figure 83) indicate the state of the secondary voltages of the electronics unit. Note: A dark power supply LED indicates a major electronics problem. CAN BUS PORT The CAN bus port (B in figure 83) is primarily used to connect external automated units (e.g. sample changer, moving mirror unit, etc.) to the spectrometer. The CAN bus also provides power to these units. Thus, most external units can be operated without connecting them to the power supply. Furthermore, the CAN bus can be used as a communication link to control these external units via the spectrometer. (The abbreviation CAN stands for Controller Area Network.) MAINS SWITCH The mains switch (C in figure 83) is used to switch the spectrometer on and off. This switch interrupts the primary voltage supply. PRIMARY POWER RECEPTACLE Connect the supplied power cord to the primary power receptacle at the spectrometer rear side (D in figure 83) as well as to the mains socket outlet. POWER CORD Replace the power cord if there are any visible signs of insulation, connectors or cable damage. Do not repair it! Replace the power cord only with cords rated for at least 250VAC, 10A. The cord must have approbation of at least your local authority, UL for US, CSA for Canada or VDE for Europe.

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F.IRMWARE . U.PDATE. . . . . . . . . . . . . . . . . . ......... . ......


GENERAL INFORMATION
..........................................................

The spectrometer firmware needs to be updated in order to make new features (e.g. a higher scanner velocity) available. It is updated using the FCONF program (Firmware Configuration Tool). This program performs automatically all the necessary actions. The FCONF program facilitates:

updating the firmware, restoring a previous firmware version, backing up the current firmware version, initializing the firmware (For service purposes only!), modifying IP settings (See appendix E, section Assigning Network Addresses.), running a custom script (For service purposes only!).

Firmware updates are typically delivered on CD or by e-mail. If the firmware update has been delivered on a CD start the FCONF program directly from the CD by double-clicking on the fconf.exe file and proceed as described below. If the firmware update has been delivered via e-mail, store the delivered files into a temporary directory, start the FCONF program by double-clicking on the fconf.exe file and proceed as described below. After having double-clicked on the fconf.exe file, the following window appears:

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FIRMWARE UPDATE Updating the Firmware

UPDATING THE FIRMWARE


To update the firmware, proceed as follows:

..........................................................

Activate the Update firmware option button and click on the Next button. The following window appears:

If there is no reason why another directory (run folder) than the displayed default
directory should be specified, accept the default directory by clicking on the Next button. The following window appears:

In this window you have to specify the spectrometer of which the firmware is to be
updated. To do this, activate the Enter custom address option button and enter the corresponding IP address in dotted notation. Note: In case of a stand-alone operated instrument, the default IP address is 10.10.0.1. If the spectrometer is integrated into a network and therefore the operating company has assigned a different than the default IP address you will find it at the spectrometer rear side. In this case, it is the operating companys duty to inscribe the IP address on the provided label at the spectrometer rear side.
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After having entered the IP address, check whether the intended spectrometer is
addressed by clicking on the Beep button. The addressed spectrometer will beep shortly three times.

Click on the Next button. The following window will appear:

Press the Finish button to start the update procedure.


Note: The update procedure may take several minutes, depending on the available bandwidth and the amount of files to be updated. During the update procedure, a log window is displayed showing all actions performed by the FCONF program. (The log-file is stored in the same directory as the backup files.)

At the end of the update procedure, the FCONF program resets the spectrometer (telling it in the log window: Resetting the spectrometer... done.). After a successful spectrometer initialization, the firmware version is displayed in the log window.
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FIRMWARE UPDATE Restoring a previous Firmware Version

After the firmware updating has been completed successfully, the following message appears:

Click on the OK button of the message window and on the Close button of the log
window. Note: The delivered Firmware update performs automatically all the actions necessary to properly replace the existing firmware version by the new one. It also generates automatically backup information to allow the restoration of the previous firmware version, in case the new firmware version does not ensure a trouble-free operation. For information on how to restore a previous firmware version refer to the next section. Note: In case of error during the update procedure, the FCONF program terminates the procedure and proposes to restore the previous firmware version.

RESTORING A PREVIOUS FIRMWARE VERSION


..........................................................
Restoring a previous firmware version is only possible if an update has been performed from that PC before. To restore the previous firmware version, proceed as follows:

Activate the Restore previous firmware option button and click on the Next button.
The following window appears:

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FIRMWARE UPDATE Backing up the current Firmware Version

The FCONF program asks you to select the directory containing the backup
information of the last firmware version (previous run folder). By default, this directory is displayed automatically. Note: If you click on the View Log button a log window appears displaying detailed information about the last update including errors, warnings or other irregularities.

Press on the Next button. In the next window you are asked to specify a directory for the backup files of the
restoration procedure. It is recommended to accept the directory proposed by the FCONF program.

The rest of the restoration procedure is identical to the update procedure


described above.

BACKING UP THE CURRENT FIRMWARE VERSION


..........................................................
To backup the current firmware version, proceed as follows:

Activate the Backup current firmware option button and click on the Next button. The following backup procedure is identical to the update procedure described
above.

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S.AMPLE. .P. REPARATION. . . . . . . . . . . . . . ...... .............


GENERAL INFORMATION
..........................................................

Proper sample preparation is crucial to obtain good and meaningful spectra. This section describes several sample preparation technique that cover a wide range of samples. It will give you some help in choosing the most suitable sample preparation technique for a given sample. The adequate sample preparation technique depends on the state of aggregation and the spectral absorptivity of the sample. Regardless of the state of aggregation, the sample material has to be homogeneous because variations in concentration or composition within the sample area to be analyzed can result in misleading or erroneous data. Sometimes the trial-and-error procedure is required to obtain an acceptable spectrum.

State of Aggregation
Depending on the state of aggregation of the sample, there are different sample preparation and measurement techniques. If you have to analyze a solid sample you can either prepare a solution, a Nujol mull or a KBr pellet. Liquid samples can be analyzed either as a thin film between plates or in a liquid cell. Gaseous samples require dedicated cells with different path lengths.

Absorptivity
The absorptivity of the sample is a critical factor in choosing a suitable sample preparation method. To get a meaningful spectrum of a strongly absorbing sample, the sample has to be either:

very thin or diluted by a solvent or powder that is not strongly absorbing.


According to Beers Law, the absorbance (i.e. peak intensity) in an absorbance spectrum is directly proportional to the component concentration in the sample, pathlength of the sample and the absorptivity.

A = bC

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SAMPLE PREPARATION General Information

Symbol A b C

Description Absorbance at a given wavelength Molar absorptivity (a proportionality constant) Pathlength of the sample (cell length for samples in a cell or sample thickness for films, pressed pellets) Component concentration in the sample

Typical Units None l . mol-1. cm-1 cm mol/l)

If the absorbance A (i.e. peak intensity) is too strong, decrease the sample concentration C by diluting it or diminish the pathlength b by reducing the sample thickness. If the absorbance A (i.e. peak intensity) is too weak, increase the sample concentration C or the pathlength b correspondingly to obtain a reasonable peak intensity. To find out whether a sample is strongly absorbing in the wavelength range of interest or not you have to acquire a test transmission spectrum. The figure below shows a transmission spectrum of a strongly absorbing sample.

Regions of total Absortion

Figure 84: Transmission Spectrum of a strongly absorbing Sample

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SAMPLE PREPARATION TECHNIQUES


..........................................................
There is a large number of possible sample preparation techniques. For lack of space, however, not all possible techniques can be described in detail in this chapter. Therefore, we restrict our explanations only to the most common techniques. (For more detailed information about this topic refer to the relevant specialist literature1.) Moreover, we give you a general guideline for choosing the adequate sample preparation technique. To find the most adequate method we recommend trying several sample preparation techniques and acquiring spectral data. On the basis of these data, you can assess which sample preparation technique is the most suitable one for your application. In case of doubt ask your application specialist. Some of the most common sample preparation techniques are:

No sample preparation (e.g. self supporting film or measurement using a microATR accessory)

Thin film of liquid sample solution between two IR-transparent2 plates Preparing a solution Preparing a Nujol mull3 Pressing a KBr pellet Liquid cell and gas cell

Note: Most of the described sample preparation techniques involve the use of hygroscopic materials (such as NaCl or KBr), i.e. if these materials come in contact with water or alcoholic solvents, they begin to dissolve or become cloudy and thus, impair the measurement results. Therefore, avoid all sources of water and even alcohols (ethanol and methanol).

No Sample Preparation
The easiest samples to analyze are film and polymer samples with a thickness of less than approx. 100 micrometers. They can be simply placed in a magnetic holder and immediately scanned. The same procedure can be used for samples which can be sliced to an appropriate thickness. A large number of solid and liquid samples can also be analyzed without requiring a preparation using a micro-ATR accessory. Attenuated Total Reflectance (ATR) units are a very versatile accessory for FT-IR measurements. In many cases, the micro-ATR unit can be used for liquid and semi-liquid materials instead of the constant path transmis1. e.g. Gnzler, Helmut / Gremlich, Hans-Ulrich (2002): IR Spectroscopy - An Introduction. Weinheim: WILEY-VCH Verlag. 2. i.e. IR-transparent within the frequency range of interest 3. A mull is a mixture (more precisely a suspension) of two substances, one of which (i.e. the sample) is finely divided and dispersed in the other (e.g. the paraffin oil Nujol). VERTEX 70v User Manual 139

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SAMPLE PREPARATION Sample Preparation Techniques

sion cells and the salt plates. In addition, this measurement accessory can also be used for analyzing polymer films, pastes and powders. Due to the reproducible effective pathlength, they are well suited for both qualitative and quantitative analyses. Depending on the sample material and the objective of the analysis, there are different ATR-crystal materials (e.g. ZnS, ZnSe, Ge and diamond). The sample penetration depth ranges between 0.1 and 2m and depends on the wavelength, the refractive index of the ATRcrystal material and the incidence angle of the beam. (For more information about attenuated total reflectance refer to the respective specialist literature.)

Thin Film between two Plates


Preparing a thin film of a liquid sample between two IR-transparent plates is an easy sample preparation method. Choose this method if your sample is either a liquid or an oil. An advantage of this method is that only a small amount of the sample is required.

Apply a drop of the sample on one of the plates using a pipet. Place a second plate on the top and make a quarter turn to obtain a nice even film
of the liquid sample. Sandwich the plates carefully together to remove all air bubbles. Note that these plates are very fragile and can break easily. (The space between the two plates is very small (typically < 0.01mm).

If the sample amount proved to be too much, separate the plates, wipe one side
clean and fit the plates together again.

Slot the plates in the sample holder of the spectrometer and start the
measurement. Note: The plates (made of NaCl or KBr) are extremely moisture sensitive. Therefore, do not use samples that contain water, keep the plates always dry, clean them only with chloroform or high purity acetone and polish them carefully after each use. In the course of time they will absorb moisture from the atmosphere and deteriorate. Therefore, proper storage (e.g. in an exicator) is extremely important.

Solid Sample as Solution


Use this sample preparation method if your sample is a soluble solid (e.g. a soluble powder). To obtain an IR spectrum, you have to prepare a concentrated solution of your sample using a suitable solvent. The concentration of the solution needed for a good spectrum depends on the sample.

Dissolve the sample or sample powder in a solvent and apply the sample solution
between two support plates, as described above. Depending on the available amount of sample material you can either apply a small amount of your sample powder directly on the plate and add one drop of the solution or dissolve the sample in a test tube and apply the solution with a pipet on the plate.

A second variant is to apply the sample solution on an IR-transparent plate and


allow the solvent to evaporate leaving a thin sample film on the plate. Then, slot the plate in the sample holder of the spectrometer and start the measurement.
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A third variant is to fill the sample solution in a liquid cell and acquire a sample
spectrum. To acquire a background spectrum measure the liquid cell containing only the solvent. The volumes of these liquid cells are between 0.1 and 1ml. Microcells with a much lower capacity are also available.

Do not forget to acquire a background spectrum from the solvent as well.


Note: The plates (made of NaCl or KBr) are extremely moisture sensitive. (See above.) The major problem in preparing a solution is choosing an appropriate solvent. Most solvents have a strong absorptivity and so their absorption bands will superimpose those of the solute. Therefore, you have to ensure that the used solvent is not strongly absorbing in the wavelength range of interest. Use only spectrophotometrically pure solvents and solvents that are not infrared active in the spectral region of interest. No solvent is perfect but if some information about the sample is known, the solvent can be chosen accordingly. Commonly used solvents are carbon tetrachloride, carbon disulphide, chloroform, cyclohexane, acetonitrile, and tetrachloroethylene. Never use water as solvent because, firstly, it will dissolve the salt plates and secondly, it exhibits a broad OH-peak. Consult the relevant reference books for the absorptivity of the various solvents.

Preparing a Mull
This sample preparation method is suitable if the solid sample can be ground into fine particles but a suitable solvent is not available. In this case the sample powder is suspended in a mulling agent (i.e. a liquid in that the solid is not soluble). A suitable mulling agent is Nujol, a paraffin oil, which is transparent in the infrared region, except for narrow bands at 2900, 1450 and 1375cm-1. (An alternative mulling agent, which does not absorb in these regions, is a perfluorokerosene, such as Fluorolube.) The advantage of this technique is that it is a relatively quick and simple procedure. The disadvantage is the interference resulting from the absorption bands of the mulling agent. (Both Nujol and Fluorolube have characteristic spectral features and in most cases have to be used as a pair in order to generate a complete MIR spectrum. Nujol is used below 1330cm-1, Fluorolube above 1330cm-1.)

Put a small amount of your solid sample in an agate mortar. Grind the sample thoroughly into fine powder (particles smaller than 500 mesh)
using a pestle. Note: A common mistake when preparing a Nujol mull is to spend too little time grinding the powder. Note that a mull prepared from a coarsely ground solid will yield only a poorly resolved spectrum. Grinding the sample into very fine particles is also important to reduce light scattering and salt plate scratching.

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SAMPLE PREPARATION Sample Preparation Techniques

Add 1 or 2 drops of Nujol. Be careful not to add too much Nujol. Mix the ground sample with the mulling agent until a uniform paste with a
vaseline-like consistency is formed.

Apply some mull on the surface of a NaCl plate using a suitable tool (e.g. a small
spatula or a rubber policeman). Be careful not to scratch the plate.

Place the second plate over the mull. To ensure an even and thin sample
thickness between the plates, rotate and press the plates together in order to squeeze out the excess of the paste. Exclude also air bubbles.

Slot the plates in the plate holder installed in the spectrometer sample
compartment and start the measurement.

Do not forget to acquire also a background spectrum of the pur Nujol.

Pressing a KBr Pellet


This sample preparation technique is very suitable for solid samples in terms of the information yield from an IR spectrum because KBr is significantly more IR transparent than most solvents or Nujol oil. KBr has no absorption in the region 4000cm-1 to 250cm-1 so that a good sample spectrum (i.e. a spectrum that does not contain spectral information about the dispersing agent) is obtained. The success of this technique strongly depends on the grain size of the ground sample. Grind the sample as fine as possible (particle size of at least 200 mesh, better 500 mesh) to minimize the infrared light scattering on the particle surface, also called Christiansen effect. This effect is caused by a refraction index mismatch between the salt (KBr) and the sample powder that leads to reflections at the salt-sample interface. Therefore, proper grinding is required to ensure a good contact between KBr and sample powder and to minimize the portion of the reflected light. Another important factor in this technique is to keep everything moisture free as the KBr material is hygroscopic. To prevent the KBr material from absorbing moisture, keep the KBr material and the die in a drying oven at a temperature of 50 to 60C. Failure to do so will result in cloudy pellets that yield distorted spectra. A correctly prepared KBr pellet will be transparent to IR light. To sum it up, the KBr-pellet technique yields good quality spectra with a wide spectral range and no interfering peaks. Disadvantages include tedious and time consuming sample preparation and cleanup, interference of water bands (3,960 to 3,480cm-1 and 1,950 to 1,300cm-1 and below 500cm-1) and in same cases structural changes caused by high pressure applied to the KBr/sample mix.

Put a small amount of the sample in an agate mortar and grind it up as fine as
possible.

Add a spatula full of oven-dry KBr material to the ground sample and mix it until a
uniform mixture is obtained. Do not grind the mixture as this may increase the absorption of water by KBr.

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SAMPLE PREPARATION Sample Preparation Techniques Note: A common mistake is to use to much sample. The concentration of the sample in KBr should be in the range of 0.2% to 1% (i.e. typically a 300:1 dilution by mass).

Transfer the mixture into a die of a hydraulic or hand press and subject it to very
high pressure (ca. 20,000 psi) for a few minutes (2 to 5 minutes). The result should be a translucent pellet with an ideal thickness of 0.5 to 1mm.

Carefully remove the pellet from the die, place it in the pellet holder and put the
pellet holder in the spectrometer sample compartment. Note: The KBr pellet is very hygroscopic and fragile. Handle it with care and use gloves to avoid contact with moisture from your hands. Measure the KBr pellet immediately after removing it from the press as the pellet will fairly rapidly begin to absorb moisture from the air and becomes cloudy.

Liquid Cell
Liquid cells produce excellent results for most liquids. Especially for liquid samples that are very volatile, using a liquid cell is highly recommended. A liquid cell consists of two IR transparent windows with a precision spacer in between. One of the windows has two drilled holes for the introduction and evacuation of the liquid. A large number of cell options are available including permanently sealed cells, demountable cells with different window material and a wide selection of spacers. Note: Take into consideration that KBr is hygroscopic and the pathlength of the KBr cell will change when exposed to a wet sample (this may affect quantitative results). In addition, water will reduce the cell throughput by clouding the windows. Note that many liquid cells contribute a fringe pattern to the spectrum. Matching the refraction index of the window material with that of the sample can minimize this effect.

Gas Cell
To obtain an infrared spectrum of a gaseous sample a gas cell with windows at each end is required. It is important to select a suitable window material (e.g. KBr, NaCl, or CaF2) that does not absorb infrared light. The cell usually has an inlet and outlet port with a tap to facilitate the filling with the gas to be analyzed. Simple demountable cells (50 mm to 100 mm) are recommended for samples in a 5 - 10% concentration range. For diluted samples (ppm to ppb concentrations) a long path cell should be used. The long path cell reflects the IR beam several times through the sample using a set of mirrors positioned on the opposite ends of the cell. Note that the cell thickness, the pressure of the gas (proportional to concentration) inside the cell, and the molar absorptivity determine the peak intensity.

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S.ERVICE . A.DDRESSES. . . . . . . . . . . . . . . . ....... . ..........

Bruker Optik has an international network of branch offices and representations to ensure worldwide a competent customer service. Below the addresses of the Bruker headquarters are listed. For a complete list with the addresses and telephone numbers of the Bruker branch offices and representations worldwide refer to the internet: http://www. brukeroptics.com/contacts/worldwide.html

North America
Bruker Optics Inc 19 Fortune Drive Billerica, MA 01821 USA Phone: +1-978-439-9899 (ext. 5227) Fax: +1-978-663 9177 www.brukeroptics.com info@brukeroptics.com

Europe
Bruker Optik GmbH Rudolf-Plank-Str. 27 76275 Ettlingen Germany Phone: +49 7243/504-619 / -600 Fax: +49 7243/504-698 www.brukeroptics.de ir_service@brukeroptics.de

Asia
Bruker Optik Asia Pacific Ltd. Unit 505, 6/F, Tower III Enterprise Square No. 9 Sheung Yuet Road Hong Kong Phone: +852 2796 6100 Fax: +852 2796 6109 asiapacific@brukeroptics.com.hk
No responsibility can be taken for the correctness of this information. Subject to change.

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SERVICE ADDRESSES

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I. NDEX. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .....
Numerics
10Base-T Ethernet network 117, 118 10Base-T Ethernet port 98, 127 10Base-T Ethernet standard 7, 12, 98

D
Data cable 7, 12, 115 DDC ports 126 Detector 25, 26, 28, 29, 50, 87, 90, 93, 102 Exchange procedure 51 Operating temperature 26 Sensitivity 26 Spectral range 26 Detector compartment 19, 50, 52 Detector dewar 56 Detector diagnostics page 83 Diagnostic LEDs 75 Diagnostics page 75, 80 DLaTGS detector 26, 51

A
AAR 5, 33, 35 ACR 5, 47, 50, 66 Air humidity content 43, 95 Aperture wheel 29 Automatic accessory recognition 5, 35 Automatic component recognition 5, 47, 50, 66 Automation diagnostics page 82, 88

B
Beam direction control compartment 19 Beam path 106 Beamsplitter 25, 28, 29, 47, 50, 90, 93, 94, 97 Color coding of the handle 28 Exchange procedure 49 Handling instructions 48 Operating position 47 Spectral range 28 Storage position 47

E
EDIS port 126 Electronics 87, 102 Electronics compartment 19 Electronics diagnostics page 81 Electronics panel 23, 24, 125 Electronics unit 129 Electrostatic discharges 57 ERR LED 84, 93, 97, 126 Ethernet 24, 98 Ethernet connection 5 Ethernet network 83, 127 Ethernet port 11, 98, 127, 128 Evacuating valve 13, 37 Evacuation time 41

C
CAN bus port 23, 24, 96, 129 CAT 5 cable 98, 128 CG LED 84, 126 COM1 port 126 Computer network interface card 12 Connection topology 116 Connecting VERTEX 70v and PC to a network 117 Connecting VERTEX 70v to a network computer 118 For stand-alone operation 116 CR LED 126 Crossover cable 7, 12, 98, 127 CY LED 84, 126

F
FCONF program 120, 131 FIR source 26 Firmware 120, 131 Backing up the current version 135 Modifying IP settings 120 Restoring a previous version 134 Updating the firmware 132 Flaps 6, 37, 45, 69, 71, 85, 91 Controlling 45

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Index
Fuses Replacement procedure 68 FWD LED 126 Mains switch 11, 23, 24, 31, 68, 96, 129 MCT detector 26, 51, 52, 53, 55, 56, 87, 90, 95 Cooling procedure 55 Evacuation procedure 59 Measurement parameters 105 MIR source 25, 26, 66, 103 MPE port 96

G
Gas cell 139, 143 Gaseous sample 137 Globar 26

H
HeNe laser 103

N
Network 116 Network interface card 118, 119 NIR source 25, 26, 66, 103 Noise reduction hood 8, 15 Nujol mull 137, 139, 141

I
Inlet port 5, 22, 24, 26, 29 Instrument status message 75, 79, 88 Interferogram 75 Interferometer 28, 87, 90, 102 Interferometer compartment 19 Internet 117 Intranet 117 IP address 12, 99, 123, 127, 128 IP addresses for the stand-alone configuration 119 IR beam port 22, 23, 85 IR-transparent plate 139, 140

O
Optical path 29 OQ test 57, 94 Outlet port 5, 22, 29 OVP 94 OVP software 57 OVP test 75, 77, 78, 94

P
Peak position 95 Photometric accuracy 101 Power 101 Power cord 7, 11, 96, 129 Power supply Frequency range 10 Voltage range 10 Power supply connector 19 Power supply panel 128 Power supply unit 94, 96 PQ test 94 Pressure sensor 6 Primary power receptacle 11, 23, 24, 129 Primary voltage supply 129 Purge gas 33 Degree of dryness 44 Flow rate 44 Maximum pressure 44 Purge gas connection 33 Purge gas hose 7 Purge gas inlet 15, 16, 24

K
KBr pellet 137, 139, 142, 143

L
LAS TEST port 126 Laser 19, 25, 28, 61, 86, 88, 93, 97, 102 Parameter reset 64 Replacement procedure 61 Safety notes 61 Laser beam 86, 87, 97 Laser diagnostics page 64, 80 Laser LED 21, 61, 77, 86, 87, 93, 97 Laser power supply unit 61 Laser tube 86, 87, 97 Liquid cell 139, 143 Liquid nitrogen 52, 55, 93 Safety notes 55 Liquid sample 137 LPT1 Port 127

M
MAC address 121

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I. NDEX. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .....
Q
QuickLock 25, 33, 34 Inserting a QuickLock accessory 34 Removing a QuickLock accessory 34 Source diagnostics page 68, 80 Spectral range 101 Spectral resolution 101 Spectrometer Connecting the vacuum pump 13 Connecting to a PC 12 Connecting to the power supply 11 Connecting to the purge gas supply 15 Evacuating procedure 36 Initialization 21, 77, 86, 87, 96, 98 Purging 43 Rear side 23 Switching-on/off-procedure 31 Venting procedure 36 Spectrometer status indicator 75 SR LED 83, 98, 123, 127 Stand-alone configuration 123, 127 Status indicator board 19, 20, 76 Status LED 12, 21, 31, 32, 77, 86, 96 Step scan option 126

R
Reset button 24, 98, 127 Residual water vapor 41 RJ-45 connection 98 RX LED 83, 98, 127

S
Sample compartment 19, 21, 33, 102 Dimensions 110 Sample compartment windows 28, 50, 69, 94 Chemical properties 70 Handling instructions 70 Refraction index 70 Replacement procedure 71 Safety notes 70 Transmission range 70 Sample holder 25 Sample preparation 137 Sample preparation techniques 139 Sample spectrum 141 Sanner diagnostics page 81 Scan speed 101 SG LED 83, 127 Site requirements Environmental requirements 9 Humidity 9 Power supply 10 Space requirements 9 Temperature range 9 Vibration 10 Solid sample 137, 140 Source 26, 28, 31, 89, 93, 94 Parameter reset 68 Replacement procedure 66 Safety notes 66

T
Temperature range 101 Time-resolved measurement 126 TKD LED 127 Tool kit 7 Transport handles 8 TRG port 126 TX LED 83, 98, 127

U
UV source 26

V
Vacuum 102 Vacuum LED 20, 76, 85 Vacuum pump 6, 8, 9, 13, 15, 32, 73, 85 Vacuum pump connection port 13, 19, 23, 24 Valve block 13 Vent opening 13, 23, 24

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Index
Venting valve 13, 37, 85 Vibration absorber 8, 15 VIS source 26 Voltage status LED 68, 83, 87, 94, 96, 98, 129

W
Wavenumber accuracy 101

VERTEX 70v User Manual

VERTEX 70v User Manual

VERTEX 70v User Manual