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Product Calibration Procedure For

TriStar II 3020

APPROVALS: Director, Engineering Manager, Product Integrity and Performance Stefan Koch Tony Thornton Senior Project Manager Manager, International Service Patrick Wommack Derrick McAdoo Responsible Engineer Director, Quality Sam Varner Andy Dovin Manager, Manufacturing Engineering Application Specialist Dennis Pyle Jeff Kenvin Director, Manufacturing Manager, Domestic Service Adrian Gibson Kevin Fouquette This document, and specifications herein, is the property of Micromeritics.

Do not reproduce or use in whole or in part without written consent of Micromeritics.

Document Number: 302/34000/76 SV/sv Revision: (B) 2009/02/05

Title: Product Calibration Procedure for TriStar 3020

Date: 2009/02/05 Page: 2 of 38

Number: 302/34000/76 Revision: (B)

REVISION HISTORY

Rev.

ECN #

DESCRIPTION OF CHANGE

CHK BY

DATE

- 080001 Formal release K. Massengill 4/22/08 A 080365 Revised per ECN. K. Massengill 9/12/08 B 090021 Revised per ECN


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1.0 PURPOSE This document describes the process used to calibrate and test the TriStar 302/34000/00 or the 302-34000-01 assembly.

2.0 SCOPE This document is used in the Final Assembly area.

3.0 APPLICABLE DOCUMENTS 302-42801-00 User’s Instruction Manual Work Instructions, provided by the department manager in the Final Assembly area.

4.0 REQUIREMENTS 4.1 Calibration Tools

004-09814-00 Paroscientific Pressure Gauge or 004-09603-00 Crystal Pressure Gauge (if 004-09814-00 is not available) 003-09623-01 Vacuum Calibration Standard. (Yellow Jacket) 512-09800-00 Temperature Calibration Standard. 004-25538-00 1/2” gauge pins for sample port calibration, 3 required 236-09800-00 Reference Volume Chamber Kit. 2 kits required.

4.2 Special Tools

None

4.3 Utilities • Electrical: 115 Vac, 60 Hz, 200VA. • Nitrogen gas: 99.999% pure @ 15 psig, dual stage regulated, metal supply lines. • Helium gas: 99.999% pure @ 15 psig, dual stage regulated, metal supply lines. • Krypton gas: 99.99% pure @ 10 psig, dual stage regulated, metal supply lines • Dry high vacuum pump system • Liquid Nitrogen • Crushed Ice

4.4 Environment

No special ventilation or temperature requirements.

4.5 Reference Materials 004-16833-00 Carbon black reference material from the standard accessory kit.


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5.0 CALIBRATION PROCEDURE

This procedure should be followed in sequential order. Make copies of the appendices.

5.1 Manual Operation Check-out Purpose: To verify the basic operation of the unit.

Inputs: Computer to actuate the various parts of the instrument. Dry vacuum pump system connected to instrument. Gases connected to instrument. Data sheet to verify observations.

Action:

1. Enter service test mode.

2. From the main menu, for the unit number being operated, select “Service Test | Start…”. Enter the name SYSCXXXX.svt, where XXXX is the serial number of the instrument. Click OK, and then click the Yes button to create this file.

3. Click the Replace All button. Select the file SYSCHECK.SVT and then click OK.

4. Click the Next button. The service test will display several messages. Follow these instructions for each message then click OK. Take note of the amount of time the test will take.

5. When the test is complete a message is displayed. Click OK then click the Report button to produce reports on the screen. Click the “Save As” button to save an electronic copy of the report. The electronic report will have the same name as the service test file name with a file extension of “REP”. (i.e. SYSCXXXX.REP)

6. Locate the label on the elevator which identifies its revision level. Write this on the data sheet.

Acceptance Criteria: This portion of the check-out will be considered when the word “Failed” does not appear on any of the test reports.

Outputs: The data sheet must be filled out verifying the observations. The date completed column must be marked on the checklist indicating that this step has been successfully completed.


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Background: The dry vacuum pump system is used because when a TriStar is being

built and tested we do not know if the system will ship with a dry vacuum pump or an oil sealed vacuum pump. It is important to avoid oil vapor exposure which can coat the internal plumbing of the system.

The revision level of the elevator is recorded on both the data sheet and the serial number log book (or equivalent if we start a new record system) so that we can identify the elevator used in a particular instrument in the event of a failure at a customer’s location. This will enable us to quickly know if a particular elevator revision is causing any unexpected failures and allow us to make changes so that we can get the customer up and running as fast as possible.

5.2 Initial Calibration

Purpose: To verify basic functionality. To calibrate the pressure transducers and servo valve for the subsequent leak test.

Inputs: Computer to actuate the various parts of the instrument. 004-09814-00 Paroscientific Pressure Gauge or 004-09603-00 Crystal Pressure Gauge (if 004-09814-00 is not available) 003-09623-01 Vacuum Calibration Standard. (Yellow Jacket)

Action:

1. Because this is not a final calibration step, it is not necessary to record the serial numbers of the pressure and vacuum standard.

2. Attach nitrogen gas at 10 to 15 psig to gas inlet port for Valve 9.

3. Manually pressurize the system including the three sample ports (unless they are already open to the atmosphere) and Po port to 800 mmHg +/- 50 mmHg

4. Install the pressure calibration standard on sample port 1. If using the Paroscientific gauge connect it to the instrument’s RS-232 port. Removing the filter frit in the sample port is not required.

5. Install the vacuum gauge on sample port 2. Removing the filter frit in the sample port is not required.

6. Install a blank tube or plug on the other sample port.

7. Open valves 1, 2, 3, 4, 5, 6, and 10.

8. Wait until the vacuum gauge reads vacuum levels below 1000 µmHg.

9. Continue evacuation for 10 minutes.


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10. Zero the pressure transducers.

1. From the main menu, for the unit number being operated, select “Calibration | Zero Pressure…”

2. Select the Manifold Transducer, Port 1 Transducer, Port 2 Transducer, Port 3 Transducer, Po Transducer.

3. Press the Start button to invoke the zero pressure transducers routine.

4. Record the screen readings on the Data Sheet. If any transducers do not pass the Acceptance Criteria, you must identify and repair the problem before proceeding.

5. If you encounter no error message, proceed to the next step.

11. Scale the pressure transducers.

1. Pressurize the manifold, sample ports and Po port to 800–900 mmHg.

2. From the main menu, for the unit number being operated, select “Calibration | Pressure Scale…”


4. Click the “From Reference” button to enter the reading from the Paroscientific gauge, or type in the pressure reading from the pressure calibration standard. Press enter.

5. Reduce the system pressure to 380 mmHg +/- 20 mmHg.

6. Record the screen readings on the Data Sheet. If any transducers do not pass the Acceptance Criteria, you must identify and repair the problem before proceeding.

12. Scale the 10 mmHg pressure transducer (if installed).

1. Pressurize the manifold with the 10 mmHg valve open, to 7 to 9 mmHg.


3. Select the 10 mmHg Transducer.



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5. Reduce the system pressure to 5 +/- 1 mmHg.

6. Record the screen reading on the Data Sheet. If the 10 mmHg transducer fails the Acceptance Criteria, you must identify and repair the problem before proceeding.

13. Calibrate the servo valve.

1. From the main menu, for the unit number being operated, select “Calibration | Servo Valve…”

2. Press the Start button to invoke the Servo Valve Calibration routine.

3. If you encounter no error message, record your success on the Data Sheet.

Acceptance Criteria: All steps complete.

Outputs: The Data Sheet and Checklist are filled out indicating that this step is complete.

Background: This step is done to quickly confirm that the major components of the TriStar system are functional. It also helps subsequent steps to have the servo valve roughly calibrated so that achieving particular pressures is made easier.

5.3 Initial Manifold Clean-up Leak Test

Purpose: To measure the outgas rates of the analysis, dosing, gas inlet manifolds, and the 10-mmHg transducer manifold (if installed). To perform an exhaustive leak test of each valve in the system. To flush undesirable contaminates from the system.

Inputs: Computer to actuate the various parts of the instrument.

Action:


2. From the main menu, for the unit number being operated, select “Service Test | Start…”. Enter the name 1LEKXXXX.svt (where XXXX is the serial number of the instrument). Click the OK button, and then the Yes button to create this file.

3. Click Replace All. Select LEAKALL.SVT.


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4. Click the Next button. The service test will display several messages. Follow

these instructions for each message then press OK. Take note of the amount of time the test will take.

5. When the test is complete a message is displayed. Click OK then click the Report button to produce reports on the screen. Click “Save As” to save an electronic copy of the report. The electronic report will have the same name as the service test file name with a file extension of “REP”. (i.e. 1LEKXXXX.REP)

6. Use the data sheet in appendix C to record outgas rates, leak rates and other information from the report. Include out-of-tolerance or questionable results.

7. An Excel spreadsheet has been designed to simplify the recording of the INITIAL LEAK TEST results, data reduction, and printing the results. The spreadsheet also simplifies determining whether the results were; Passed, Check, or Failed. The Excel file is located in this location: \\me\manf\MANF_ENG\PROJECTS\3020\Leakall Datasheets

8. After out of tolerance conditions are fixed, repeat the automatic leak test can be repeated or measure the leak rate manually. Enter the Passed data on an additional data sheet or Excel file.

Acceptance Criteria: All measured manifold outgas rates and valve leak rates are less than the maximum allowable rates shown on the data sheet.

Output: The Data Sheet and Checklist are filled out indicating that this step is complete.

Background: The Background section in step 5.8 contains many topics that apply to this initial test.

5.4 Calibrate Pressure Transducers

Purpose: To set the zero point and scaling of all the pressure transducers. To verify pressure transducer linearity. To run the “match transducer” routine.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. 004-09814-00 Pressure Calibration Standard 004-09603-00 Crystal Pressure Gauge (if 004-09814-00 is not available) 003-09623-01 Vacuum Calibration Standard. (Yellow Jacket)


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Action:

1. Attach nitrogen gas at 10 to 15 psig to gas inlet port for Valve 9.

2. Manually pressurize the system including the three sample ports and Po port to 800 mmHg +/- 50 mmHg. If a 10mmHg transducer is installed, then you must also open valve 15.

3. Remove the sample port filter frits at ports 1 and 2.

4. Install the pressure calibration standard on sample port 1. If using the Paroscientific gauge connect it to the instrument’s RS-232 port.

5. Install the vacuum gauge on sample port 2.

6. Install a blank tube or plug on sample port 3.

7. Open valves 1, 2, 3, 4, 5, 6, and 15 (if present).

8. Open valves 10, 11, 12, and 13.

9. Wait until the vacuum gauge reads vacuum levels below 20 µmHg.

10. Continue evacuation for 10 minutes.

11. Zero the pressure transducers.

1. From the main menu, for the unit number being operated, select “Calibration | Zero Pressure…”

2. Select the Manifold Transducer, Port 1 Transducer, Port 2 Transducer, Port 3 Transducer, Po Transducer and (if present) the 10mmHg transducer.

3. Press the Start button to invoke the zero pressure transducers routine.


12. Scale the pressure transducers.

1. Pressurize the manifold, sample ports and Po port to 800–900 mmHg.




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4. Click the “From Reference” button to enter the reading from the

Paroscientific gauge, or type in the pressure reading from the pressure calibration standard. Press enter.

5. Reduce the system pressure to 380 mmHg +/- 20 mmHg.

6. If the values for all 5 of the 1000-mmHg transducers are within the tolerances shown in the Data Sheet, proceed to the next step.

13. Match the pressure transducers.

1. From the main menu, for the unit number being operated, select “Calibration | Match Transducers…”


3. Press the Start button to invoke the match transducers routine.


5. If the system has a 10mmHg transducer proceed to the next step with the calibration standards attached to the system, otherwise remove the vacuum gauge and pressure calibration standards.

6. If the system has a 10mmHg transducer proceed to the next step with the filter frits removed, otherwise re-install the filter frits in the sample port 1 &2.

Acceptance Criteria: All steps completed, The transducer reading at 380 mmHg (0.5 Po) is within the acceptable limits shown on the Data Sheet.

Outputs: The data sheet and checklist must be marked indicating that this step has been completed

Background: Relative to the steps in the Pressure Transducer Scaling and Linearity Test; The transducer manufacturer specifies +/- 0.1% BFSL on the 30 psia (1550 mmHg) device. This equates to about 1.6 mmHg absolute error when we calibrate at zero and 850 mmHg. The Micromeritics published specification is +/- 0.5% of Full Scale for the 1000 mmHg range; which equates to +/- 5 mmHg at any point. The acceptance limits shown on the data sheet are between these two extremes.


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5.5 10-mmHg Pressure Transducer Scaling and linearity test (Krypton unit only)

Purpose: To set the scaling of the 10 mmHg transducer and to verify their linearity.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. 004-09814-00 Pressure Calibration Standard. 004-09603-00 Crystal Pressure Gauge (if 004-09814-00 is not available)

Action:

1. Install the pressure calibration standard on one of the sample ports. If using the Paroscientific gauge connect it to the instrument’s RS-232 port.

2. Manually pressurize the system including the one sample port to 9 mmHg +/- 0.5 mmHg.

3. From the main menu, for the unit number being operated, select “Calibration | Pressure Scale (10 mmHg)…”


5. Reduce the system pressure to 4.50 mmHg +/- 0.25 mmHg.

6. Record the value for the 10 mmHg transducer and the pressure calibration standard.

7. Calculate the differences between the pressure calibration standard and the instrument transducer.

8. Record the serial number of the pressure calibration standard on the data sheet.

9. Remove the vacuum gauge and pressure calibration standards.

10. Re-install the filter frits in the sample port 1 &2.

Acceptance Criteria: The automatic scaling operation completed. Error at 4.50 mmHg (half of full scale) is within the limits shown on the Data Sheet.

Outputs: The data sheet and checklist must be marked indicating that this step has been completed.

Background: None


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5.6 Servo Valve Calibration

Purpose: To calibrate the servo valve.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations.

Action: Invoke the servo valve calibration routine.

Acceptance Criteria: The automatic operation completed.


Background: This step teaches the software how to set the servo valve to the correct target value to achieve accurate pressures. If the master pressure transducer is later re-calibrated, then the servo calibration must be repeated.

5.7 Temperature Calibration

Purpose: To set the temperature of the dosing manifold.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. 512-09800-00 Temperature Calibration Standards (20 °C, 35 °C, 49 °C).

Action:

1. Remove the top panel of the instrument.

2. Locate the RTD connector at the front edge of the PCB. Disconnect the RTD cable. Insert one of the 35 °C simulators in the connector.

3. Invoke the temperature calibration routine.

4. Enter the calibration temperature corresponding to the resistor, 35.0.

5. Insert the calibration simulator for 20 °C. Record the reading on the data sheet.

6. Insert the calibration simulator for 49 °C. Record the reading on the data sheet.


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7. Record the serial numbers of each simulator.

8. Reinstall the RTD. Verify that the display shows a valid temperature so that you know the RTD is connected properly.

Acceptance Criteria: The automatic operation completed. Temperatures of the 20 °C and 49 °C are displayed within the acceptable limits shown on the Data Sheet.


Background: After calibration, this step verified that the temperature sensor was correctly functioning. Accuracy of the temperature reading is required for accurate analysis data. An error in temperature will cause an error in the calculation of gas uptake. It takes about 3 degrees error to cause 1% gas uptake error.

5.8 Final Automatic Leak Test

Purpose: Conduct a series of tests that first measures the outgas rates of the analysis, dosing, gas inlet manifolds, and the 10-mmHg transducer manifold (if installed). A second test evacuates the system and performs an exhaustive leak test of each valve in the system. Each system and gas inlet valve is leak tested. Acceptable initial outgas and leak rates from these initial tests indicate, there are no large leaks into the system from atmosphere. As test is run there is a gradual reduction of many undesirable contaminates in the system.

Inputs: Computer to actuate the various parts of the instrument.

Action:


2. From the main menu, for the unit number being operated, select “Service Test | Start…”. Enter the name LEAKXXXX.svt (where XXXX is the serial number of the instrument). Click the OK button, and then the Yes button to create this file.

3. Click Replace All. Select LEAKALL.

4. Click the Next button. The service test will display several messages. Follow these instructions for each message then press OK. Take note of the amount of time the test will take.


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5. When the test is complete a message is displayed. Click OK then click the

Report button to produce reports on the screen. Click “Save As” to save an electronic copy of the report. The electronic report will have the same name as the service test file name with a file extension of “REP”. (i.e. LEAKXXXX.REP)

6. Use the data sheet in appendix D to record outgas rates, leak rates and other information from the report. Include out-of-tolerance or questionable results.

7. An Excel spreadsheet has been designed to simplify the recording of the FINAL LEAK TEST results, data reduction, and printing the results. The spreadsheet also simplifies determining whether the results were; Passed, Check, or Failed. The Excel file is located in this location: \\me\manf\MANF_ENG\PROJECTS\3020\Leakall Datasheets

8. After out of tolerance conditions are fixed, repeat the automatic leak test or measure the leak rate manually. Enter the Passed data on an additional data sheet or Excel file.

Acceptance Criteria: All measured manifold outgas rates and valve leak rates are less than the maximum allowable rates shown on the data sheet.

Output: The Data Sheet and Checklist are filled out indicating that this step is complete.

Background: In the production of TriStar 3000’s, the first day typically involved turning on the system, performing some simple tests and verification steps and having the instrument pump down overnight at the end of the first day. This initial evacuation of the analysis system removed many contaminates in the system, like water, atmospheric gases, and cleaning solvents.

Running the initial automatic service test for atmospheric and plunger leaks in the 3020 TriStar is more effective than the overnight, static, evacuation in the removal of contaminates because nitrogen gas is dosed into the system at the beginning of each test. The impact of nitrogen molecules on the internal walls causes molecules of contaminants to be released into the nitrogen and then evacuated from the system. This is more effective than simple evacuation.

These service tests can be run by Final Assembly on the same day that the instrument is turned on and system vacuum levels are below 1000 microns.


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Data obtained from this initial test indicates the analysis system has no large leak from atmosphere or the valves in the system

Each service test evacuates the system and performs an exhaustive test of the manifolds and components in the system.

5.9 System Volume Calibration

Purpose: To measure the system volume of the dosing manifold.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. Reference volume chamber kit Crushed ice

Action:

1. Connect the reference volume chamber to ports one and two of the TriStar under test (the volume ball must be on port 1)

2. Evacuate the chamber through valves 1 and 2. When the manifold pressure goes below 5 mmHg, open valves 11 and 12 and continue evacuation for 20 minutes.

3. Prepare an ice bath around the volume ball and allow it to equilibrate for ten minutes. Crushed ice must surround the volume ball. Do not add water.

4. Invoke the system volume calibration routine.

5. Select to run the volume calibration 3 times.

6. After all runs are complete; the average of the runs will be displayed on the computer screen. This value must be used as the system volume. Record this value on the data sheet. This value may also be recorded on the checklist (optional).

7. Record the serial number of the reference volume chamber kit on the data sheet.


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Outputs: The data sheet/checklist must be marked indicating that this step has been completed.

Background: System volume calibration is needed so that the instrument can quantify accurately the amount of gas that a real sample will adsorb.

5.10 Sample Port Volume Calibration

Purpose: To measure the volume of each sample port.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. 004-25538-00 1/2” gauge pins, 3 required

Action:

1. Install the plugs into the sample ports as snugly as possible pressing them all the way up into the sample ports.

2. Do not use a dewar.

3. Invoke the port volume calibration routine.

4. After all runs are complete; the averages of the runs will be displayed on the computer screen. Record the average port volumes on the data sheet.


Outputs: The data sheet/checklist must be marked indicating that this step has been completed. Record the average port volumes on the data sheet.

Background: Port volumes are expected to differ slightly due to manufacturing tolerances. Measuring the port volumes allows compensation for these differences when calculated free space is used.


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5.11 Blank Sample Tube Runs

Purpose: To verify the instrument’s ability to correctly measure free space.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. 302/61001/01, 3/8 tubes, quantity 3 302/61005/01, filler rod for 3/8 tube, quantity 3 302/25812/01, isothermal jacket, quantity 3

Action:

1. Attach a blank tube to each sample port.

2. Fill the Dewar with LN2. Verify the level using the dipstick.

3. Place the Dewar on the elevator.

4. Select “PCP Analysis” from the service test menu.

5. Select “Nitrogen Blank” in the wizard.

6. Start the sample runs and wait for them to finish.

7. Produce the nitrogen blank manufacturing report to the screen.

Acceptance Criteria: All points must lie between the blue lines on the nitrogen blank manufacturing report.

Outputs: The data sheet must be filled out and tolerances met. The data sheet and checklist must be marked indicating that this step has been completed. Print out the results and keep with the other documents.

Background: The long equilibration time simulates a long analysis which helps expose small leaks.


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5.12 Volume Chamber Analysis

Purpose: To verify the instrument’s ability to accurately meter nitrogen.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. Second reference volume chamber kit. Do not use the same chamber as used in step 5.8. Crushed ice.

Action:

1. Connect the reference volume chamber to ports one and two of the TriStar under test (the volume ball must be on port 1.

2. Evacuate the chamber through valves 1 and 2. When the manifold pressure goes below 5 mmHg, open valves 11 and 12 and continue evacuation for 20 minutes.

3. Prepare an ice bath around the volume ball and allow it to equilibrate for ten minutes. Crushed ice must surround the volume ball. Do not add water.

4. Select “Volume Ball” in the PCP analysis wizard.

5. Start the analysis and wait for it to finish.

6. Record the serial number of the reference volume chamber kit on the data sheet.

7. Enter the volume of the chamber on the data sheet.

8. Enter the volume of the chamber in the report editor for the manufacturing reports. Produce the report to the screen.

Acceptance Criteria: The measured volumes must be within the blue lines shown on volume chamber manufacturing report.

Outputs: The data sheet must be filled out and tolerances met. The data sheet/checklist must be marked indicating that this step has been completed. Print out the results and keep with the other documents.

Background: The second reference volume is used as a cross check that the chamber used on step 5.8 gave a good calibration value for the system manifold volume.


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The pressure table uses 0.9 as the highest point, and the run conditions

use 844.444 mmHg as saturation pressure. Multiplying 0.9 by 844.444 gives the highest equilibration pressure as 760 mmHg. The reason for not using an entered saturation pressure of 760, with a target of 1.0 is that the TriStar software interprets 1.0 relative pressure as a trigger to cause special pressure dosing that searches for saturation equilibration. This will not work during volume verification with nitrogen at ice bath temperatures.

5.13 Reference Material Sample Runs

Purpose: To verify the instruments ability to correctly measure surface area.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. Carbon black reference material (004-16833-00) from accessory kit. Sample tubes called out in the reference material data sheet.

Action:

1. Prepare three reference material samples as outlined in the data sheet included with the reference material.

2. Select “Nitrogen Reference” in the PCP analysis wizard.

3. Fill the dewar with LN2. Verify the level using the dipstick.

4. Place the dewar on the elevator.


6. Record the name, part number, lot number, multipoint surface area and area tolerance of the reference material on the data sheet.

Acceptance Criteria: The acceptable tolerances are shown on the sample data sheet.

Outputs: The data sheet must be filled out with the expected value and the measured value. The data sheet and checklist must be marked indicating that this step has been completed. Print out the results and keep with the other documents.

Background: Successfully running a sample material verifies that the instrument correctly measures helium and nitrogen.


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5.14 Kr Blank Sample Tube Runs (Krypton unit only)

Purpose: To verify the instrument’s ability to correctly measure free space.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. Blank 3/8 tubes with isothermal jackets. No filler rods.

Action:

1. Make sure krypton is properly attached to the instrument.

2. Attach a blank tube to each sample port.

3. Select “Krypton Blank” from the PCP analysis wizard.

4. Fill the Dewar with LN2. Verify the level using the dipstick.

5. Place the Dewar on the elevator.


Acceptance Criteria: All points must lie between the blue lines on the nitrogen blank manufacturing report.

Outputs: The data sheet must be filled out and tolerances met. The data sheet and checklist must be marked indicating that this step has been completed. Print out the results and keep with the other documents.

Background: The long equilibration time simulates a long analysis which helps expose small leaks.


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5.15 Kr Reference Material Sample Runs (Krypton units only)

Purpose: To verify the instruments ability to correctly measure surface area.

Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. Reference material. 3/8 sample tubes with isothermal jackets. No filler rods.

Action:

1. Prepare three reference material samples as outlined in the data sheet included with the reference material.

2. Select “Krypton Reference” in the PCP analysis wizard.

3. Fill the dewar with LN2. Verify the level using the dipstick.

4. Place the dewar on the elevator.


6. Record the name, part number, lot number, multipoint surface area and area tolerance of the reference material on the data sheet.

Acceptance Criteria: The acceptable tolerances are shown on the sample data sheet.

Outputs: The data sheet must be filled out with the expected value and the measured value. The data sheet / checklist must be marked indicating that this step has been completed. Print out the results and keep with the other documents.

Background: Successfully running a sample material verifies that the instrument correctly measures helium and krypton.


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5.16 Save Instrument Calibration

Purpose: Save calibration data and copy calibration files to network.

Inputs: Networked computer terminal

Action:

1. Select Unit x from pull down menu (where x is the unit number being worked on).

2. Select “Calibration Data”, click on “Save to file”.

3. Edit the suggested name of the file: remove the dash and all numbers after it so that the name is the serial number of the instrument and the extension is .CAL.

4. Click OK.

5. Click Accept.

6. Select Unit x from pull down menu (where x is the unit number being worked on).

7. Select “Calibration Data”, click on “Store Instrument Information…”.

8. Click OK.

9. Exit the 3020 application program.

10. Select “Product Info. Transfer” icon from the desktop. Select the 3020 model.

11. Enter or select the instrument’s serial number, press Enter.

Acceptance Criteria: Calibration data were saved and transferred to the network.

Outputs: Calibration files saved on network.

Background: In order to create a Calibration CD for this instrument the calibration files must be saved to the network.


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5.17 Create Calibration/Program CD

Purpose: Create Calibration/Program CD to be shipped with instrument.

Inputs: Personal computer with Lotus Notes e-mail, or verbal method of requesting CD creation.

Action: E-mail (or verbally tell) the Final Assembly supervisor the instrument model number and serial number, ask them to create Calibration/Program CD and to send the CD to Final Assembly.

Acceptance Criteria: CD received from Final Assembly supervisor.

Outputs: Record acceptance in the appropriate places on the checklist in Appendix A.

Background: The Calibration/Program CD is needed to be shipped with the instrument. It contains the current operating program and the calibration files.

5.18 Documentation

Purpose: To combine the Data Sheet, the Checklist, and all of the reports for the instrument history file. To record the elevator’s revision level wherever serial numbers of instruments are kept.

Input: Completed Data Sheet(s), completed checklist, and all reports.

Action: Place all the reports, the completed Data Sheets, the completed checklist, together as a package. This package will be placed in the instrument history file. Ensure that the elevator’s revision level is recorded in the instrument serial number repository.

Acceptance Criteria: The operator has completed this step.

Outputs: The checklist must be marked indicating that this step has been completed.

Background: None


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5.19 Deliverables

Purpose: To combine the calibration diskette(s), and all of the other loose items for shipment.

Input: The calibration/program CD(s), and all loose items that were tested with the instrument.

Action: Collect the parts, per the checklist. Bag and label them. These parts are to leave the floor with the instrument and will be shipped with the instrument.

Acceptance Criteria: The operator has completed this step.

Outputs: The checklist must be marked indicating that this step has been completed.

Background: The hardware items on the checklist are tested with the instrument to verify that they function correctly.


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APPENDIX A TriStar II 3020 Data Sheet (Page 1 of 7)

Date Core Part Number Serial Number

Operator(s)

Part Number Description Serial # Cal. Due Date 512-09800-00 Temperature Calibration Standard 004-09814-00 or 004-09603-00

Pressure Calibration Standard (Paroscientific or Crystal. Identify which was used)

003-09623-01 Vacuum Calibration Standard (Yellow Jacket) 236-09800-00 First Reference Volume Chamber Kit 236-09800-00 Second Reference Volume Chamber Kit

5.1 Manual Operation Checkout OK? Did the Application program start successfully? Test passed? (attach report) Report filed syscXXXX.svt and syscXXXX.rep (stored in \\mic\products\3020\Calibration Data), where XXXX is the serial number of the instrument.

Was the temperature reading within 5 °C of ambient? Record Revision level of elevator 300-34005-00 Rev


Date: 2009/02/05 Page: 26 of 38


APPENDIX A

TriStar II 3020 Data Sheet (Page 2 of 7)

5.2 Initial Calibration Pre-test Verification Screen Reading Acceptance Limit OK? Best vacuum level achieved microns Below 1000 microns

Observe transducer readings after zeroing (no recording needed) Master < 0.5 mmhg Port 1 < 0.5 mmhg Port 2 < 0.5 mmhg Port 3 < 0.5 mmhg Po < 0.5 mmhg 10 mmHg (if installed) Write N/A if not applicable < 0.5 mmhg

Transducer readings at 360 to 400 mmHg Reference Reading mmHg Master mmHg +/- 50 mmHg Port 1 mmHg +/- 50 mmHg Port 2 mmHg +/- 50 mmHg Port 3 mmHg +/- 50 mmHg Po mmHg +/- 50 mmHg

10 mmHg scaling test (if installed) at 4 to 6 mmHg (If not installed, write N/A on the “OK?” lines) Reference Reading mmHg 10 mmHg reading mmHg +/- 1 mmHg

Servo Valve Calibration No error message

5.3 Initial Manifold Clean-up and Leak Test

Automatic leak test for TriStar 3020 OK? Create and run the appropriate service test file named 1LEKxxxx.svt, where

XXXX is the instrument serial number

Create electronic copy of service test named 1LEKxxxx.rep, where XXXX is the instrument serial number

Record the outgas, leak rate and other information from the report on the data sheet. Perform the necessary calculations.

All automatic or manually measured test results are within allowable limits on data sheet for initial data.


Date: 2009/02/05 Page: 27 of 38


APPENDIX A



Transducer Zero OK? Verify vacuum is less than 20 microns. No error message?

Transducer Scaling OK? Verify transducer scaling has been completed. No error message? Scaling accuracy test at 0.5 Po (380 +/- 20 mmHg) Sensor Reference

(mmHg) Computer reading

(mmHg) Difference from Reference

(mmHg) OK?

Master Port 1 Port 2 Port 3

Po Difference must be less than 2.0 mmHg

5.5 10 mmHg Transducer Scaling (if installed) Scaling accuracy test (at 4.5 +/- 0.25 mmHg). Write N/A if not applicable Reference (mmHg) Computer reading (mmHg) Difference from Reference(mmHg) OK? Difference must be less than 0.02 mmHg

5.6 Servo Valve OK? No error message?


Date: 2009/02/05 Page: 28 of 38




OK? Reference (°C) Computer reading (°C) Difference from Reference (°C)

20 49

Differences must be less than 0.1 °C


Automatic leak test for TriStar 3020 OK? Create and run the appropriate service test file named LEAKxxxx.svt, where

XXXX is the instrument serial number

Create electronic copy of service test named LEAKxxxx.rep, where XXXX is the instrument serial number

Record the outgas, leak rate and other information from the report onto the Appendix D data sheet. Perform the necessary calculations.

All automatic or manually measured test results are within allowable limits on the Appendix D data sheet for initial data.

5.9 System Volume Calibration Reference S/N Average Manifold Volume Average Manifold + 10-mmHg volume (10-mmHg

only) Write N/A if not applicable

cm3 cm3

5.10 Sample Port Volume Calibration Record Average Port Volume (cm3)

Port 1 Port 2 Port 3


Date: 2009/02/05 Page: 29 of 38



5.11 Blank Runs Tolerances for 3/8 tubes: All quantities adsorbed must be within +/-( 0.017 + 0.56 P/Po) cm3 STP. These limits are printed on the nitrogen blank manufacturing report.. The isotherm must show a fairly smooth trace with no sudden peaks, except at saturation. OK? All points are within tolerance lines on the nitrogen blank manufacturing report? Port Filename

1 1B_______-___.SMP

2 2B_______-___.SMP

3 3B_______-___.SMP

5.12 Volume Chamber The measured volume must be within 0.5% of the chamber’s volume for relative pressures above 0.5. These limits are shown on the volume chamber manufacturing report

Reference Chamber Volume cm3 Serial # OK? Data points are within the limits on the volume chamber manufacturing report? Port Filename

1 1V_______-___.SMP

2 2V_______-___.SMP

5.13 Reference Material Type of material Part Number Lot Number Multipoint S/A from ref. material label

m2/g Tolerance +/- m2/g

Port Filename Reported Surface Area Within Tolerance?

1 1N_______-___.SMP m2/g

2 2N_______-___.SMP m2/g

3 3N_______-___.SMP m2/g


Date: 2009/02/05 Page: 30 of 38


APPENDIX A


5.14 Krypton Blank Tube Test (Units with 10 mmHg transducer) Attach graphs showing isotherm within limits. Write N/A if not applicable. Required? Yes ____ No _____ Port Filename Ok?

1 1A_______-___.SMP

2 2A_______-___.SMP

3 3A_______-___.SMP Positive acceptable limits are defined by an adsorption line drawn on the isotherm starting at 0.0022cm3/g at P/Po of 0.06 and ending at 0.0039cm3/g at P/Po of 0.30. Negative acceptable limits are defined by an adsorption line starting at –0.0005cm3/g at P/Po of 0.06 and ending at –0.0012cm3/g at P/Po of 0.30. These limits are printed on the krypton blank manufacturing report.

5.15 Krypton Standards Test (Units with 10 mmHg transducer) Attach reports

Port Expected Surface Area Measured Area Filename OK?

1 +/- 1K_______-___.SMP

2 +/- 2K_______-___.SMP

3 +/- 3K_______-___.SMP

5.16 Save Instrument Calibration Calibration data saved to network?

5.17 Create Calibration/Program CD CD created and labeled for shipping with instrument?


Date: 2009/02/05 Page: 31 of 38



5.18 Documentation To be compiled in this order; write N/A if not applicable.

Appendix A, Data Sheet Appendix B, Checklist Appendix C, Data Sheet Appendix D, Data Sheet Transducer Service Test report (if used) Nitrogen Blank Run report Reference chamber report Nitrogen sample run report Krypton blank run report (if applicable) Krypton sample run report (if applicable) All items present?

5.19 Deliverables Loose items that are tested and then delivered to stock with the instrument.

All units Qty Analysis Dewar 300-25861-20 1 CD, with calibration data 302-20800-99 1 All items present?

(Po tube remains installed on the instrument)


Date: 2009/02/05 Page: 32 of 38


Appendix B

TriStar II 3020 Checklist (Page 1 of 1) Date Core Part Number Serial Number

Operator(s) PCP step Step Description Date Complete

5.1 Manual Operation Checkout

5.2 Initial Calibration

5.3 Initial Manifold Cleanup and Leak Test


5.5 10-mmHg Transducer Scaling and Linearity (10-mmHg units only)

5.6 Servo Valve Calibration



5.9 System Volume Calibration

5.10 Sample Port Volume Calibration

5.11 Blank Tube Test (N2)

5.12 Reference Chamber Analysis

5.13 Nitrogen Standards Test (N2)

5.14 Krypton Blank Tube Test (10-mmHg units only)

5.15 Krypton Standards Test (10-mmHg units only)

5.16 Save Instrument Calibration

5.17 Create Calibration/Program CD

5.18 Documentation

5.19 Deliverables


Date: 2009/02/05 Page: 33 of 38


Appendix C (1 of 3) TriStar II 3020

Data Sheet for Initial Automatic Leak Test a Service Test Information Serial Number

Service Test File Name LEAKALL Rev Level Run Date b Manifold and Valve Leak Test data on this report came from (check which type of system)

1000 mmHg Transducer System (no 10 mmHg)

10 mmHg Transducer System

Test

Measured Outgas Rates.

Enter slope from service tests (umHg/min)

Leak Rates. Enter slope from

service tests (umHg/min)

Base or OGR Rate Enter slope from


Difference Leak Rate – Base Rate

(umHg/min)

Preliminary Limits

Maximum rate (umHg/min)

Pass

Check

Fail

Sample Manifold OGR

(1000t)

Sample Manifold OGR

< 50.0 Good 50.1 to 75.00 Investigate > 75.1 Bad

10 mmHg Manif OGR (if installed)

10 mmHg Manifold OGR


Samp & 10 mmHg OGR (if installed)

Sample & 10 mmHg OGR


Sample, 10 mmHg & Inlet

OGR

Sample 10T & Inlet OGR


Sample Port 1

Port One OGR

System OGR During Port 1

< 10.00 Good 10.01 to 15.00

Investigate > 15.01 Bad

Sample Valve 1

Leak Test

Valve 1 Leak Rate Valve 1 Base Rate

< 5.00 Good 5.01 to 12.00 Investigate

> 12.01 Bad

Valve 1Leak Rate: Max Pressure > 500 Good

<499 Investigate Sample Port 1

Valve 11

Valve 11 Leak Rate: Greatest Range Per 6 min

< 0.500 Good 0.501 to 1.000


Sample Port 2

Port Two OGR


< 10.00 Good 10.01 to 15.00


Sample Valve 2

Leak Test



> 12.01 Bad

Form Rev 03-25-08


Date: 2009/02/05 Page: 34 of 38







Test

Measured Outgas Rates. Enter slope from service

tests (umHg/min)






(umHg/min)

Preliminary Limits


Pass

Check

Fail

Valve 2 Leak Rate Max Pressure > 500 Good


Valve 12


< 0.500 Good 0.501 to 1.000


Sample Port 3

Port Three OGR


< 10.00 Good 10.01 to 15.00


Sample Valve 3

Leak Test



> 12.01 Bad

Valve 3 Leak Rate: Max Pressure > 500 Good


Valve 13


< 0.500 Good 0.501 to 1.000


Po Tube Port 4

Po Port OGR

System OGR During Po Port

< 10.00 Good 10.01 to 15.00


Po Port Valve 4

Leak Test

Valve 4 Leak Rate Valve 4 Base Rate < 5.00 Good 5.01 to 12.00 Investigate

> 12.01 Bad

Valve 7 Gas Line

OGR

Valve 7 Gas Line OGR

System OGR During Valve 7 Gas Line

< 10.00 Good 10.01 to 20.00


Gas Inlet Valve 7

Leak Test


< 10.00 Good 10.01 to 15.00


Form Rev 03-25-08


Date: 2009/02/05 Page: 35 of 38







Test



Leak Rates. Enter slope from service

tests (umHg/min)



Difference Leak Rate – Base Rate (umHg/min)

Preliminary Limits


Pass

Check

Fail




< 10.00 Good 10.01 to 20.00


Gas Inlet Valve 8

Leak Test


< 10.00 Good 10.01 to 15.00





< 10.00 Good 10.01 to 20.00


Gas Inlet Valve 14 Leak Test

Valve 14 Leak Rate

Valve 14 Base Rate

< 10.00 Good 10.01 to 15.00


Valve 5n6 Base Rate

Valve 5n6 Base Rate

< 40.00 Good 40.01 to 65.00


Valve 6 Leak Test

Valve 6 Leak Rate Valve 5n6 Base Rate


> 10.01 Bad

Valve 5 Leak Test



> 10.01 Bad




< 10.00 Good 10.01 to 20.00


Gas Inlet Valve 9

Leak Test


< 10.00 Good 10.01 to 15.00


Form Rev 03-25-08


Date: 2009/02/05 Page: 36 of 38


Appendix D (1 of 3) TriStar II 3020

Data Sheet for Final Automatic Leak Test a Service Test Information Serial Number




Test





Base or OGR Rate


Difference Leak Rate – Base Rate (umHg/min)

Preliminary Limits


Pass

Check

Fail

Sample Manifold OGR

(1000t)

Sample Manifold OGR


10 mmHg Manif OGR (if installed)

10 mmHg Manifold OGR


Samp & 10 mmHg OGR (if installed)

Sample & 10 mmHg OGR


Sample, 10 mmHg & Inlet

OGR

Sample 10T & Inlet OGR


Sample Port 1

Port One OGR



> 10.01 Bad

Sample Valve 1

Leak Test



Valve 1Leak Rate:

Max Pressure

> 500 Good <499 Investigate

Sample Port 1

Valve 11


< 0.500 Good 0.501 to 1.000


Sample Port 2

Port Two OGR



> 10.01 Bad

Sample Valve 2

Leak Test



Form Rev 03-25-08


Date: 2009/02/05 Page: 37 of 38







Test








(umHg/min)

Preliminary Limits


Pass

Check

Fail

Valve 2 Leak Rate

Max Pressure > 500 Good


Valve 12


< 0.500 Good 0.501 to 1.000


Sample Port 3

Port Three OGR



> 10.01 Bad

Sample Valve 3

Leak Test



Valve 3 Leak Rate: Max Pressure

> 500 Good


Valve 13


< 0.500 Good 0.501 to 1.000


Po Tube Port 4

Po Port OGR

System OGR During Po Port


> 10.01 Bad

Po Port Valve 4

Leak Test

Valve 4 Leak Rate Valve 4 Base Rate < 3.00 Good 3.01 to 7.00 Investigate > 7.01 Bad





> 15.01 Bad

Gas Inlet Valve 7

Leak Test



Form Rev 03-25-08


Date: 2009/02/05 Page: 38 of 38







Test



Leak Rates. Enter slope from service

tests (umHg/min)




(umHg/min)

Preliminary Limits

Maximum rate

(umHg/min)

Pass

Check

Fail





> 15.01 Bad

Gas Inlet Valve 8

Leak Test







> 15.01 Bad

Gas Inlet Valve 14 Leak Test

Valve 14 Leak Rate

Valve 14 Base Rate


Valve 5n6 Base Rate

Valve 5n6 Base Rate

< 10.00 Good 10.01 to 25.00


Valve 6 Leak Test



Valve 5 Leak Test







> 15.01 Bad

Gas Inlet Valve 9

Leak Test



Form Rev 03-25-08

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