PN 103164Rev 2: 7/2010

TOPIC Pg• Tour 2

• Setup 3

- Physical Planning 3

• Safety Features & Emergency Procedures

4

• Sample Cup Preparation 5

• Start Up & Login 7

• Typical Work Flow 8

• 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

— Table of Contents —

— SUMMARY —The MESA-6000 X-ray fluorescence (XRF) analyzer is designed to support several key measurements, such as:

• Sulfur in petroleum products• Oxygenated petroleum at low levels

• Chlorine in fuel oils or petroleum products• 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).

— SUMMARY —The MESA-6000 X-ray fluorescence (XRF) analyzer is designed to support several key measurements, such as:

Installation ManualHoriba MESA-6000™Benchtop XRF Analyzer

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

•

••

•

•

•

•

•

Rear Panel I/O Ports

1. USB 2. 9-Pin Serial 3. RJ-45 Network4. PS2 Keyboard/Mouse5. 15-Pin Monitor

Rear Panel

1. Vacuum Valve2. Fan w/Filter3. Main Power Switch4. Power Cord Socket 5. I/O Ports

Instrument Features

1. Hinged Lid2. Test Chamber3. Measurement Window (Kapton)4. X-Ray Indicator (Red LED)5. Ventilation Slots6. Touchscreen7. Power Button w/Indicator (Blue LED)8. Side Panel I/O (1 USB Port)

43

1

6

2

5

781

1

2

2

3

3

4

4

5

5

•

2 Rev 2: 7/2010PN 103164

MESA-6000™ Benchtop XRF Analyzer

Setup the Analyzer

Physical Planning-

The 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 analyzer’s 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.

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

Hei

ght

- C

lose

d

Depth

Hei

ght

- O

pen

Dimensions in inches and millimeters

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

MESA-6000View Looking Straight Down

Depth

Width

W-2

D-2

WidthClose-Up: Sample Test ChamberView Looking Straight Down.

MESA-6000Side View

PN 103164Rev 2: 7/2010 3

Safety Features and Emergency Procedures

Safety Features and Emergency Procedures

4

3 1

6

2

5

7

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

Emergency Shutoff Procedures[2] Power Switch/Indicator

Press the button; entire unit shuts OFF Data may not be preserved.

[4] Open LidDuring a test, opening the lid shuts OFF X-Rays immediately.

Data is preserved.This is the Recommended method

[7] A/C Power AssemblyPress the Rocker switch to OFF Data may not be preserved

4 Rev 2: 7/2010PN 103164

MESA-6000™ Benchtop XRF Analyzer

Calibration Procedure - Prepare Sample Cups

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)

Use these SEVEN steps:

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.

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)

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 separa-tor piece. (See Figures 5 and 6) Handle the Mylar film by its edges only.

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

Figure 1 Figure 2

Figure 3

Figure 4

Figure 5 Figure 6

PN 103164Rev 2: 7/2010 5

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).

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)

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

Figure 7

Figure 8Figure 9 Figure 10

Figure 11

6 Rev 2: 7/2010PN 103164

MESA-6000™ Benchtop XRF Analyzer

Start Up & Login

• Apply AC power to the analyzer with the black rocker power switch (# 1) located on the lower right side of the instrument’s 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.

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.

Username: Alphanumeric char-acters, no spaces; it is not case sensitive.

Generic Username: Admin

Password: Alphanumeric charac-ters. — This field is case sensitive.

Generic Password: 1234

An on-screen keyboard allows you to access the MESA-6000 UI

Start the MESA-6000

# 1

# 2

Login

Status field (text) Progress Bar (real-time display)

PN 103164Rev 2: 7/2010 7

Workflow for using the MESA-6000

Workflow for using the MESA-6000

1.0 After Login you will be on the Testing tab1.1 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.

r using the MESA-6000

8 Rev 2: 7/2010PN 103164

MESA-6000™ Benchtop XRF Analyzer

Workflow

3.0 Select Calibration sub-tab3.1 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 ID4.3 Press Next

PN 103164Rev 2: 7/2010 9

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.

4.11 Remove Sample after measurement is completed.

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.

10 Rev 2: 7/2010PN 103164

MESA-6000™ Benchtop XRF Analyzer

Testing Tab

Testing Tab.

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.

Testing

Action Buttons

Status Field

Sample Queue

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.

Deletes existing samples from the queue whether they are test samples or calibration samples. Deleted sam-ples remain in the Results tab.

Prints the sample information and average measurement results of the selected sample.

The queue lists the samples that may be measured. Validate, Quick Sample and Check Std are perma-nently in the queue.

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

Select Check Std to verify calibration.

Information for the selected sample

Displays validation and measured

Also shows evaluation progress for ongoing samples.

Aborts the test but results are still viewable.

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

When a sample has been evaluated, the superim-posed symbol becomes a green check mark.

This is the icon for calibration samples

If a sample being tested is interrupted, the superim-posed symbol becomes a yellow exclamation mark.

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

Progress Bar

Select Validate to confirm certain parameters in the X-ray detector. This is a hardware check.

use finger to move queueon touchscreen

samples. results for ongoing or finished

PN 103164Rev 2: 7/2010 11

Results Tab

Results TabThe Results tab organizes test sample results for:

• Inspection• Exporting• Printing

This screen has three types of function buttons:• Selection• Navigation• Action

Selection Navigation

Navigation

Action Buttons

Drop-down List Boxfor Calibrations

Time & Date

Sample ID Listing

ACTION Buttons

Deletes the selected test(s)

Saves the information and results of the

Prints the sample information and average

selected test(s) to an external file.

measurement results of the selected samples

Jump to the first or last page ofresults in the selected day.

Scroll up or down in the result rows of the selected day in increments of one page.

NAVIGATION Buttons

Jump to the first or last day of results.

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

SELECTION Buttons

As an example, group the results by “Day.” Displays all results within the

• Use the Selection Buttons to define and narrow

• Use the List Box to choose the appropriate calibration.

the results to examine.

Group the results by the corresponding time period.

selected calibration.

— INSTRUCTIONS for Using the RESULTS Screen —

Buttons Buttons

Buttons

Results

12 Rev 2: 7/2010PN 103164

MESA-6000™ Benchtop XRF Analyzer

Info(rmation) Tab

The Info tab displays information specific to this instrument:• Version of Application Software• Identification of Firmware• Hardware operating conditions• List of Errors and warnings

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)

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

Messages

“Messages” reported in this box can include errors, warnings,and informational items.

Info

PN 103164Rev 2: 7/2010 13

Admin Tab

Admin Tab

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

Measure chlorine with the option of sulfur co-measurement.— or —

When the Admin tab is selected, the Calibration sub-tab is invoked initially.

calibration, select “New” from the drop-down List Box.

Assign a name to the new calibration, This calls a unique screen available only during calibration which requires you to: If you want to create a new

Select the type of calibration from four available alternatives (see a - d selection high lights).— and —

2

1

1

2

Sulfur measurement without oxygen correction

a

b

c

d

b

c

d

Selection• Working with only one fuel blend.

Sulfur measurement with oxygen correction • 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

Chlorine measurement without sulfur correction

Chlorine measurement with sulfur correction

• Measuring Chlorine in a fluid not expected to contain significant sulfur.

• Measuring Chlorine in a fluid that may containsignificant sulfur.

After choosing your calibration type, tap OK to return to the main Calibration sub-tab. You can now specify the calibration parameters.

Applicationa

or biofuels.

Admin

Continue Calibration Procedure on the next page

14 Rev 2: 7/2010PN 103164

MESA-6000™ Benchtop XRF Analyzer

Admin > Calibration Sub-tab

31 52 4 6

7

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

PN 103164Rev 2: 7/2010 15

Admin > Configuration Sub-tab}

Admin > Configuration Sub-tab}

A

2

4

1

3

5

Admin > Configuration

[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.

ACTION Buttons for Admin > Calibration Sub-tab

Admin > Calibration continued

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 haven’t 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.

16 Rev 2: 7/2010PN 103164

MESA-6000™ Benchtop XRF Analyzer

2

1

3

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.

Logout

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.

A new user is saved only after all his perti-nent details are entered.

The Delete button removes a user.

Generic Username: AdminGeneric Password: 1234

Admin > Users

Operators with Groupaccess level of “User”cannot view “Manager”passwords.

PN 103164Rev 2: 7/2010 17

Instrument Radiation Profile

Instrument Radiation Profile

Specifications

Notes:1. “No Sample” - System over-ridden to permit continuous air shot2. Background reading (BK) = < 0.5 ìSv/h (varied 0 to 0.45 ìSv/h)

RESULT: Maximum leakage acceptable on design tested (random prototype production sample).

Measured Dose Rate (ìSv/h)

LOCATION TOP RIGHT SIDE LEFT SIDE FRONT REAR BOTTOM

SAMPLE

STD 316 Sample < 0.5 (BK)* < 0.5 (BK)* < 0.5 (BK)* < 0.5 (BK)* < 0.5 (BK)* < 0.5 (BK)*

Plastic SampleCarrier 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)*

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

MESA 6000 Unit configuration – 10.5 kV @ 2.0mASurvey Instrument: Ludlum Model 3 - 44-7 Detector

Component DescriptionEnclosure • 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: -25°to +40°C • Humidity: 0 - 95% Relative Humidity, non-condensing

Storage Environment • Temperature: -30°to +45°C

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

18 Rev 2: 7/2010PN 103164

MESA-6000™ Benchtop XRF Analyzer

Kapton Window Maintenance

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. 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.

3. Turn Vacuum Release Valve to its closed position.

OPEN

Vacuum Release Valve

1

Upper left rear corner of MESA-6000

CLOSED

3

2

Maintenance: Two Levels

1. Clean Existing Window

Cleaning Procedure

Tools Required

• Philips head screw driver• Isopropanol (IPA)• Particle free tissue

• Nitrile gloves• Can of compressed air

PN 103164Rev 2: 7/2010 19

• Philips head screw driver• Isopropanol (IPA)• Particle free tissue• Nitrile gloves,• Can of compressed air

Key Parts •

•

•Kapton Window FrameHas 7.5 micron Kapton film.fused to an aluminum ring-disk.

Assembly Screws (3)# 4 x 6mm flat head Philips head screws

Remove Old Window

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.Don’t over-tighten them; this can strip the threads.

Remember to turn the Vacuum Release Valve to its CLOSED position (See page 19).

CAUTION

•

2. Replace Existing Window

Tools Required

20 Rev 2: 7/2010PN 103164