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Installation Manual

Horiba MESA-6000Benchtop XRF Analyzer

Table of Contents
TOPIC

Pg

Tour

Setup

- Physical Planning

Safety Features &


Emergency Procedures

Sample Cup Preparation

Start Up & Login

Typical Work Flow

Testing

11

Results

12

Info

13

Admin

14

Admin > Calib

15

Admin > Config

16

Admin > Users

16

Logout & Shutdown

17

Instrument Radiation
Profile

18

Specifications

18

Kapton Window Maintenance


Clean Existing Window

19

Replace Existing Window

20

SUMMARY
SUMMARY
TheMESA-6000
MESA-6000X-ray
X-rayfluorescence
fluorescence(XRF)
(XRF)analyzer
analyzerisisdesigned
designedto
tosupport
supportseveral
severalkey
keymeasurements,
measurements,such
suchas:
as:
The
Sulfur in petroleum products
Chlorine in fuel oils or petroleum products
Oxygenated petroleum at low levels
Chlorine in presence of high sulphur
Traditionally, oxygen interferes with XRF analysis of sulfur. The MESA-6000 is the first XRF instrument that
can compensate for oxygen content in a sample. This enables accurate sulfur measurements of oxygenated
petroleum products (such as biodiesel and ethanol blended gasoline).
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Tour of the MESA-6000

Tour of the MESA-6000


The Horiba MESA-6000 XRF instrument resides in
a bench top cabinet that effectively supports:
1. Large-sized, radiation-safe Test Chamber, and
2. Touchscreen Computer for convenient input and
results display.

Embedded Application Software


Optimized for Sulfur and Chlorine analysis
Fast results display that can be exported
and printed

Instrument Features

1. Hinged Lid
2. Test Chamber
3. Measurement Window (Kapton)
4. X-Ray Indicator (Red LED)
5. Ventilation Slots
6. Touchscreen
7. Power Button w/Indicator (Blue LED)
8. Side Panel I/O (1 USB Port)

Rear Panel
1. Vacuum Valve
2. Fan w/Filter
3. Main Power Switch
4. Power Cord Socket
5. I/O Ports

3
4

Rear Panel I/O Ports


1. USB
2. 9-Pin Serial
3. RJ-45 Network
4. PS2 Keyboard/Mouse
5. 15-Pin Monitor

1
2

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MESA-6000 Benchtop XRF Analyzer

Setup the Analyzer


Physical PlanningThe MESA-6000 arrives ready to run as a stand-alone unit with an AC line cord. I/O ports support user cabling
options consisting of a serial cable, network cable (RJ45), USB cables (2), monitor cable, and PS2 Keyboard/Mouse.

Where will the instrument be used?


It weighs about 48.75 lbs. It can sit on a lab bench or table.
How much space (area) to allocate?

Use the dimensions shown below as your planning guide.


Ensure that the cooling vents on the rear and side panels are not obstructed.
Any special space issues for height?
Operator must be able to access the analyzers lid latch and test chamber comfortably.
Ensure that the lid can open without encountering an obstruction.
What are the electrical power requirements?
Minimal 3 Amp (Peak-to-Peak); less than 125 Watts draw; 100 - 240 VAC auto switching power adapter.

MESA-6000
Side View

Height - Closed

Height - Open

Dimensions in inches and millimeters

Instrument Dimension

inch

mm

Width

12.75

324

Depth

20.50

521

Height-Closed

16.25

413

Height-Open

23.00

584

Feet-Side-to-Side

10.75

273

Feet-Front-to-Back

13.00

330

Depth
Close-Up: Sample Test Chamber
View Looking Straight Down.

Width
MESA-6000
View Looking Straight Down

D-2

Dimensions in inches and millimeters

Width

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Rev 2: 7/2010

Depth

W-2

Chamber Dimensions

inch

mm

Width, Side Wall-to-Side Wall

7.00

178

Height, Internal, Lid Closed

2.09

53

Depth, Front-to-Back

7.00

178

D-2, W-2,Center
Window-to-Side Wall

3.40

86.6

Safety Features and Emergency Procedures

Safety Features and Emergency Procedures


Hardware Safety Features
[1]

X-Ray Indicator

Red LED glows when X-Ray tube is ON

[2]

Power Switch/Indicator

Blue LED glows when instrument power is ON

[3]

Interlock Switch

Ensures that lid is closed before turning X-Rays ON

[4]

Interlock Switch - Lid

Ensures that lid is closed before turning X-Rays ON

[5]

Shielded Test Chamber

Prevents X-Rays from escaping from the instrument during testing

[6]

Interlock Side Service


Panel(s)

Prevents removal of service panel during an X-Ray test

[7]

A/C Power Assembly (rear)

Recessed AC power socket and On/Off rocker switch

3
5

Emergency Shutoff Procedures


[2]

Power Switch/Indicator
Press the button; entire unit shuts OFF

[4]

Open Lid
During a test, opening the lid shuts
OFF X-Rays immediately.

[7]

Data is preserved.
This is the Recommended method

A/C Power Assembly


Press the Rocker switch to OFF

Data may not be preserved.

Data may not be preserved

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MESA-6000 Benchtop XRF Analyzer

Calibration Procedure - Prepare Sample Cups


Use these SEVEN steps:
STEP 1.
If using HORIBA 2 part cups, cells are
packaged with outer rings partially
assembled to cups.
Select an assembly and remove its
outer ring.
(See Figure 1 and Figure 2)
Figure 1

Figure 2

STEP 2.
Wipe the interior portion of the cell
with a Kimwipe. (See Figure 3)
NOTE: A Kimwipe is a particle free
tissue that comes in a small dust
resistant carton.
Figure 3

STEP 3.
Place the cell on a flat horizontal surface; fill
the cup using a fresh pipette for every sample.
Fill the sample cup to 5ml line. (See Figure 4)
Figure 4

STEP 4.
With the sample cup filled to
the 5 ml line, place a sheet of
Mylar over it.
NOTE: There are two types of
film in the Mylar box. Use only
the clear film, not the opaque
film which is used as a separator piece.
(See Figures 5 and 6)

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Rev 2: 7/2010

Figure 5

Figure 6

Handle the Mylar film by its edges only.


Never touch interior area where it is exposed to X-Rays.

Calibration Procedure - Prepare Sample Cup, continued

Calibration Procedure - Prepare Sample Cup, continued


STEP 5.
With film in place, gently locate the outer ring
portion over the film.
TIP: Angle the outer ring about 5 degrees with
the Jig Tool (See Figure 7).

Figure 7

STEP 6.
Locate the Jig on top of the sample cup with the slits facing down. (See Figure 8)
Using the palm of your hand, firmly press the Jig down until the film is tight.
Slowly remove the Jig; verify that the film has no bumps or wrinkles. (See Figures 9 and 10)

Figure 9

Figure 10

Figure 8

STEP 7.
When the sample cup is complete it
should be similar to the example in
Figures 11.

Figure 11

Technique for Testing Volatile Samples


If the sample is volatile such as gasoline, it is important to vent the Sample cup.
Turn the Sample cup into the Jig tool with the Mylar film portion facing down. This eliminates contact with dirty surfaces.
Using a needle or pin, pierce the top portion of the cup to vent the sample. This allows the film to remain flat and tight
without any bowing.
Check for leakage or any foreign substance on the film.

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MESA-6000 Benchtop XRF Analyzer

Start Up & Login


Start the MESA-6000

Apply AC power to the analyzer with the black rocker power switch (# 1)
located on the lower right side of the instruments back panel.
Turn on the computer with the front blue power switch (# 2)
located on the front of the instrument.

The touchscreen briefly shows a System Initialization display.


When the unit has successfully initialized, the Login screen is invoked.
We are now in the MESA-6000 User Interface.

#1

#2

Login

An on-screen keyboard allows


you to access the MESA-6000 UI
Username: Alphanumeric characters, no spaces; it is not case
sensitive.
Generic Username: Admin
Password: Alphanumeric characters.
This field is case sensitive.
Generic Password: 1234

Status field (text)

Progress Bar (real-time display)

The MESA-6000 touchscreen application software has a five tab User Interface design:

Testing
Results
Info
Admin (has three sub-tabs)

Calibration
Configuration
Users

Logout

Tabs are described on pages 11 through 17.


But first look at pages 8 through 10 which describe the analysis of work flow.

PN 103164
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Workflow for using the MESA-6000

r using the MESA-6000


Workflow for using the MESA-6000

1.0 After Login you will be on the Testing tab


1.1 Select Validate.
1.2 Press Measure button.

2.0 Select Admin tab,


then Configuration sub-tab
2.1 Select the Calibration curve you wish
to measure in from the drop-down list
box.

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MESA-6000 Benchtop XRF Analyzer

Workflow

3.0 Select Calibration sub-tab


3.1 Select the same Calibration Curve
from the drop-down list box.

4.0 Choose Testing tab.


Note: Active Calibration has changed
4.1 Press New Sample

4.2 Type a Sample ID


4.3 Press Next

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Workflow

Workflow

4.3 Enter Comments, if needed.


4.4 Press Next.

4.4 Press OK.


This sends the newly created sample
to the Measure Queue.

4.5 Open Sample Lid.


4.6 Make a Sample cup with 5ml of Sample.
4.7 Load onto measurement position.
4.8 Close Sample Lid.
4.9 Select the Sample.
4.10 Press Measure.

4.11 Remove Sample after measurement


is completed.

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MESA-6000 Benchtop XRF Analyzer

Testing Tab
Testing Tab.
Testing
By default, the Testing tab is
the initial screen presented by
the UI.
The following button actions
assume you have:
(1) completed the calibration
processes,
and
(2) selected the appropriate
calibration.

Displays validation and measured


results for ongoing or finished
samples.
Also shows evaluation progress
for ongoing samples.
Information for the selected sample

Sample Queue
use finger to move queue
on touchscreen
Action Buttons

Status Field

Defines new sample and places it onto the queue. During


the sample definition process the (a) Sample ID, (b)
length of measurement time, (c) the number of repeats,
and (d) sample comments are entered.

Progress Bar
The queue lists the samples that may be measured.
Validate, Quick Sample and Check Std are permanently in the queue.

Deletes existing samples from the queue whether they


are test samples or calibration samples. Deleted samples remain in the Results tab.

Select Validate to confirm certain parameters in the


X-ray detector. This is a hardware check.

Aborts the test but results are still viewable.

Selects a Quick Sample. Evaluates a sample using one repetition of the current selected default settings without
invoking the New Sample wizard.

Prints the sample information and average measurement


results of the selected sample.

Select Check Std to verify calibration.

Fluid in a sample cup is icon for a defined test sample.


When testing is in progress, the sample being evaluated
has a radiation symbol superimposed over the icon.
For example, shown below are testing-in-progress for
the following:

Check Std

Quick Sample

Test Sample

This is the icon for calibration samples

When a sample has been evaluated, the superimposed symbol becomes a green check mark.

If a sample being tested is interrupted, the superimposed symbol becomes a yellow exclamation mark.

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Results Tab

Results Tab
The Results tab organizes test sample results for:
Inspection
Exporting
Printing
This screen has three types of function buttons:
Selection
Navigation
Action

Results

Navigation
Buttons

Selection
Buttons

Time & Date

Navigation
Buttons
Sample ID Listing

Drop-down List Box


for Calibrations

Action Buttons

INSTRUCTIONS for Using the RESULTS Screen


Use the List Box to choose the appropriate calibration.
Use the Selection Buttons to define and narrow
the results to examine.
As an example, group the results by Day.
NAVIGATION Buttons

SELECTION Buttons
Displays all results within the
selected calibration.
Group the results by the
corresponding time period.

Jump to the first or last day of results.


Move forward or backward in
increments of one day where data
is available.

12

ACTION Buttons
Deletes the selected test(s)

Jump to the first or last page of


results in the selected day.

Saves the information and results of the


selected test(s) to an external file.

Scroll up or down in the result


rows of the selected day in
increments of one page.

Prints the sample information and average


measurement results of the selected samples

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MESA-6000 Benchtop XRF Analyzer

Info(rmation) Tab
Info

The Info tab displays information specific to this instrument:


Version of Application Software
Identification of Firmware
Hardware operating conditions
List of Errors and warnings

Messages

Messages reported in this box can include errors, warnings,


and informational items.
The Navigation Buttons on the right
are used to get to the event of interest.

Displayed Hardware Information


Parameter

Acceptable Values

Detector Temp Variation

2 C of detector set temperature

Set Tube Voltage

10.5 kV (when sample being evaluated)


0.0 kV (after interlocks disengaged)

Monitor Tube Voltage

Set Tube Voltage 0.5 kV (when sample being evaluated)


0.5 kV 0.5kV (after interlocks disengaged)

Set Tube Current

2000 uA (when sample being evaluated)


0 uA (when no sample being evaluated)

Monitor Tube Current

Set Tube Current 100 uA

Vacuum Pressure

less than 40 mB

X-ray Count Rate

10,000 - 30,000 counts per second (typical)

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Admin Tab

Admin Tab
Admin

Admin tab contains privileged features and functions which are accessible
only to instrument administrators. It consists of three sub-tabs:
Calibration
Configuration
Users
The MESA-6000 must be calibrated in order to translate the X-ray data from a test
sample into measurement readings. Customer options include:
Measure sulfur with the option of oxygen correction
or
Measure chlorine with the option of sulfur co-measurement.

When the Admin tab is selected, the Calibration sub-tab is invoked initially.
If you want to create a new calibration, select New from the drop-down List Box. 1
This calls a unique screen available only during calibration which requires you to:
Assign a name to the new calibration, 2
and
Select the type of calibration from four available alternatives (see a - d selection high lights).

2
a

c
d

Selection

Sulfur measurement without oxygen correction

Sulfur measurement with oxygen correction

c
d

Application
Working with only one fuel blend.
Working with various blends of two fuels, one is
oxygenated and the other is non-oxygenated;

for example, ethanol and gasoline mixed in different ratios


or biofuels.

Chlorine measurement without sulfur correction Measuring Chlorine in a fluid not expected to
contain significant sulfur.
Chlorine measurement with sulfur correction
Measuring Chlorine in a fluid that may contain
significant sulfur.
After choosing your calibration type, tap OK to return to the main Calibration sub-tab.
You can now specify the calibration parameters.

Continue Calibration Procedure on the next page

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MESA-6000 Benchtop XRF Analyzer

Admin > Calibration Sub-tab


Admin > Calibration

Field and Settings Definitions


[1]

Standard Name

Assigned name for each calibration standard.

[2]

Assayed levels

Each featured element for each calibration standard


Note: Calibration standards without assayed entries or with incomplete entries
will NOT be used.

[3]

Num

Number of repeats.

[4]

Measured

Indicates if the standard has been run.

[5]

Exclude

Allows user to remove outliers from calibration curve.

[6]

Cal settings

Cal time(s) duration that each calibration sample will be evaluated.

[7]

Sample settings

Test time(s) and Repeats - default duration and number of repeats that test samples shot
with this calibration should match calibration settings and repeats. See # 3 and #4.

Go to next page for description of the ACTION buttons

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Admin > Configuration Sub-tab}

Admin > Configuration Sub-tab}


Admin > Calibration

continued
ACTION Buttons for Admin > Calibration Sub-tab

Delete Cal

Removes calibrations from the calibration list

Export

Exports data to user specified export path

Copy Cal

Allows user to copy an existing calibration

Delete Std

Removes standards from the calibration standards list.


Calibration standards cannot be removed from the list until the completed calibration has
been used to evaluate a test sample.

Expand Std

Allows user to view all standards prior to queueing

Queue

Sends the completed standards list to the testing queue for evaluation.
If standards are added to the calibration standards list, queueing again sends only the
samples that havent already been queued.
Note that once you initially queue the calibration samples, you cannot change the time
intervals for evaluating calibration samples and test samples.

Spectrum

Displays visual spectrum for standard

Calculate

Computes the calibration factors for evaluating test samples with this calibration.
To use all available data, perform calibration factor computation after all calibration
samples have been shot. Click the appropriate Exclude column checkbox to keep that
particular calibration sample from being included in the subsequent computation.

Admin > Configuration

1
2
3
4
5
[1] Use the Active Calibration drop-down list box to select the desired profile.
Test samples are evaluated on the basis of this choice.
[2] Use the Export Path to define where results can be exported.
[3] This feature allows user to specify or modify the testing time and repeats within
the Testing tab.
[4] Turns automatic printing capabilities On or Off.
[5] Service mode feature for instrument troubleshooting.
A

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MESA-6000 Benchtop XRF Analyzer

Admin > Users


The Users sub-tab manages user access to
the instrument. It lists the User name,
Password, and access level for each user.
Username and Password are entered or
changed by typing into the appropriate
box. The access level is selected from the
drop-down list box in the Group column.

Operators with Group


access level of User
cannot view Manager
passwords.

A new user is saved only after all his pertinent details are entered.
The Delete button removes a
user.
Generic Username: Admin
Generic Password: 1234

Logout

Normal Shutoff Procedure

1.

Press the Logout tab from the UI.


Goes to the Login screen.
2. Press Exit button.
Goes to Shell screen.
3. Press Shutdown button.
Screen goes to neutral-blank.
4. After 15 seconds the unit turns OFF.

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Instrument Radiation Profile

Instrument Radiation Profile


Measured Dose Rate (Sv/h)
LOCATION

TOP

RIGHT SIDE

LEFT SIDE

FRONT

REAR

BOTTOM

STD 316 Sample

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

Plastic Sample
Carrier w/ Film

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

No Sample
(Open Beam)

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

< 0.5 (BK)*

SAMPLE

* All Meter Readings No Different than Background No High Spots Found

MESA 6000 Unit configuration 10.5 kV @ 2.0mA


Survey Instrument: Ludlum Model 3 - 44-7 Detector
Notes:
1. No Sample - System over-ridden to permit continuous air shot
2. Background reading (BK) = < 0.5 Sv/h (varied 0 to 0.45 Sv/h)
RESULT: Maximum leakage acceptable on design tested (random prototype production sample).

Specifications
Component

Description

Enclosure

Analyzer is housed in a rugged enclosure with hinged lid protected by a gas shock
absorber
Dimensions: Closed 16.25 H x 12.75 W x 20.50 D mm [See Page 3 for outline]
Weight: 48.75 lbs.

Sample Test Chamber

Dimensions: 7.0 W x 7.0 D x 2.1 H


Lid has a safety interlock that create a closed beam system

Power Requirements

100 - 240 VAC, 50-60 Hz, auto-switching adapter; maximum draw less than 150 Watts

Fuse Rating

6.3 A - 250V 5 x 20 mm Slow Blow

Operating Environment

Temperature: -25to +40C


Humidity: 0 - 95% Relative Humidity, non-condensing

Storage Environment

Temperature: -30to +45C

X-Ray Tube

Power: (Maximum) 50 kV, 3.3 mA, up to 50 W


(Operating conditions in MESA-6000) 10.5 kV, 2 mA, maximum draw 10 W

Computer

These are nominal specs:


Intel Pentium processor running Microsoft Windows XP
RAM: 512 MB
Local Disk: 80 GB
Ports: Serial I/O, USB (2) and network (RJ-45)
Peripheral connections available: keyboard, mouse, video display, printer

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MESA-6000 Benchtop XRF Analyzer

Kapton Window Maintenance


Maintenance: Two Levels
1. Clean existing window -(a) when obvious extraneous material (fluid or solid) is evident on the film, or
(b) when contamination from previously leaked samples causes shifted measurement readings.

2. Replace existing window -(a) when a tear or puncture prevents creating a vacuum in the chamber, or
(b) when the cleaning procedure does not help with shifted measurement readings.

1. Clean Existing Window


Tools Required

Philips head screw driver


Isopropanol (IPA)
Particle free tissue

Nitrile gloves
Can of compressed air

Cleaning Procedure
1. Ensure that the Vacuum Release Valve is open;
arrow/knob pointing down.
2. Wearing Nitrile gloves, clean top of window (the film surface)
with IPA and particle free tissue. Use this technique:
a. Wipe from the center-out to drag contaminants away
from the window.
b. Dispose of tissue immediately after use since it is now
contaminated also.

Upper left rear corner of MESA-6000

OPEN

3. Turn Vacuum Release Valve to its closed position.

Vacuum Release Valve

3
CLOSED

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19

2. Replace Existing Window

Tools Required

Philips head screw driver


Isopropanol (IPA)
Particle free tissue
Nitrile gloves,
Can of compressed air

Kapton Window Frame


Has 7.5 micron Kapton film
.fused to an aluminum ring-disk.

Key Parts

Assembly Screws (3)

# 4 x 6mm flat head Philips head screws

Remove Old Window


CAUTION

Keep dust or foreign material out of the vacuum chamber.


Take care to have clean hands; wear Nitrile gloves if possible.
1. Make certain that the instrument is powered off.
2. Ensure that the Vacuum Release Valve is OPEN (See page 19)
3. Use the philips head screwdriver to remove the three screws;
carefully store these small parts away from the vacuum chamber opening.
4. Lift out the old Kapton window frame and discard.

Install New Window


1. Remove new window frame from shipping envelope.
2. Apply canned compressed air to both sides to clear any contaminants from the surfaces.
3. Lay the replacement window frame into place with the Kapton window facing up.
4. Insert the three screws; tighten only to snug.
Dont over-tighten them; this can strip the threads.
Remember to turn the Vacuum Release Valve to its CLOSED position (See page 19).

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