Document Number: 239/34000/76 Revision: (-) 2009-Apr-13

Transcription

1 Product Calibration Procedure For APPROVALS: Director of Engineering Stefan Koch Product Integrity and Performance Manager Tony Thornton Senior project manager Patrick Wommack International Service Manager Derrick McAdoo Responsible Engineer Sam Varner Director of Quality Andy Dovin Manufacturing Engineering Manager Dennis Pyle Application Specialist Jeff Kenvin Director of Manufacturing Adrian Gibson Domestic Service Manager 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. SV/sv Document Revision: (-) 2009-Apr-13

2 Date: Page: 2 of 37 REVISION HISTORY Rev. ECN # DESCRIPTION OF CHANGE CHK BY DATE Formal Release

3 Date: Page: 3 of 37 1 PURPOSE SCOPE APPLICABLE DOCUMENTS REQUIREMENTS Calibration Tools Special Tools Utilities Environment Reference Materials CALIBRATION PROCEDURE Set Instrument Serial Number Test Serial Communication Manual Operation Check-out Check Voltages Initial Calibration Initial Manifold Clean-up and Leak Test Pressure Transducer Calibration Balance Port Volume Adjustment Quantity Adsorbed Calibration Final Leak Test Blank Sample Tube Runs Reference Chamber Analysis Po Measurement Reference Material Sample Run Adsorption/Desorption Run (t model only) Save Instrument Calibration Create Calibration/Program CD Documentation Reset to Defaults Deliverables Appendix A Data Sheet Set Instrument Serial Number Test Serial Communication Manual Operation Checkout Check Voltages Initial Calibration Initial Manifold Clean-up and Leak Test Pressure Transducer Calibration Transducer Zero Transducer Scaling Scaling accuracy test Dosing Servo Calibration Balance Servo Calibration Balance Port Volume Adjustment... 29

4 Date: Page: 4 of Point Balance Run Quantity Adsorbed Transducer Calibration Final Leak Test Blank Sample Tube Run Reference Chamber Analysis Po Measurement Reference Material Sample Runs Adsorption/Desorption Run (t model only Save Instrument Calibration Create Calibration/Program CD[ Documentation Reset to Defaults Deliverables Appendix B Checklist Appendix C Leak Test Calculations Appendix D PCP Author Completeness Checklist PURPOSE This document describes the process used to calibrate and test the Gemini , , or assembly. 2 SCOPE This document is used in the Final Assembly area. 3 APPLICABLE DOCUMENTS User s Instruction Manual Work Instructions, provided by the department manager in the Final Assembly area. 4 REQUIREMENTS 4.1 Calibration Tools Paroscientific Pressure Gauge or Crystal Pressure Gauge (if is not available) Vacuum Calibration Standard. (Super Bee) Reference Volume Chamber Kit. 2 kits required. 4.2 Special Tools Long slotted screwdriver Cable, 9 Pin F/F Null, Shield, 3M MULTIMETERS, GENERAL * CERT

5 Page: 5 of USB flash drive with embedded application software Personal computer with terminal software, a serial port, and appropriate cable 4.3 Utilities Electrical: 115 VAC, 60 Hz, 200VA. Nitrogen gas: % 15 psig, dual stage regulated, metal supply lines. Helium gas: % 15 psig, dual stage regulated, metal supply lines. Vacuum pump Liquid Nitrogen Crushed Ice 4.4 Environment No special ventilation or temperature requirements. 4.5 Reference Materials Carbon black reference material from the standard accessory kit Silica-alumina reference material from the standard accessory kit ( t model only). 5 CALIBRATION PROCEDURE This procedure should be followed in sequential order. Make copies of appendices A and B. Make a copy of appendix C, or use the spreadsheet. 5.1 Set Instrument Serial Number Purpose: To save the serial number in the instrument's electronics Inputs: Control box (keypad and display) The instrument's serial number : USB flash drive with embedded application software 1. Attach the control box. 2. Insert the USB flash drive into one of the USB sockets on the rear of the instrument. 3. Turn instrument on. 4. After about 45 to 60 seconds the bottom two lines of the display will say: Update Successful Remove USB Media Remove the USB drive.

6 Page: 6 of 37 If the message is not displayed then either the USB flash drive is defective or the CPU board is defective. 5. Verify that the instrument s LED is on and not blinking. 6. Verify that the display is illuminated. Adjust the contrast potentiometer if necessary. 7. Enter service mode by pressing Alt Enter Alt Clear quickly. Enter the password, and press Enter. 8. Press Enter to get to the Instrument S/N: entry field. 9. Type the serial number with no blanks. 10. Press Save 11. Ensure that the number that was typed in appears in the top line of the display. 12. Record the top line on the data sheet. The number that was typed in appears in the top line of the display. 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. Background: The serial number is used to identify the instrument to the Windows application. 5.2 Test Serial Communication Purpose: To verify proper functioning of the serial port on the CPU board. Inputs: Computer with Hyperterminal program null modem serial cable 1. Connect the instrument s serial port to the computer with the serial cable. 2. Start the Hyperterminal program and establish the connection. The serial parameters are N1 None. 3. Type Ctrl+D on the computer keyboard. Verify that the text on the instrument s keypad display was printed in the terminal window.

7 Page: 7 of After successful completion of this step, disconnect the control box and serial cable. They will not be needed for the remainder of the procedure. The lines printed in the Hyperterminal window match the display on the keypad. 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. Background: All of the instrument s input and output signals must be tested. The other signals (USB, Ethernet, etc.) are tested in other steps. 5.3 Manual Operation Check-out Purpose: To verify the basic operation of the unit. Inputs: Computer to actuate the various parts of the instrument application software Vacuum pump connected to the instrument. Gasses connected to the instrument. Data sheet to verify observations. 1. Connect the computer and start the 2390 application. The application will be used in most of the remaining steps. 2. Enter service test mode. 3. 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. 4. Click the Replace All button. Select the file SYSCHECK.SVT and then click OK. 5. 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. 6. 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)

8 Page: 8 of Locate the label on the elevator which identifies its revision level. Write this on the data sheet. This portion of the check-out will be considered complete when the word Failed does not appear on any of the tests. 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. Background: None 5.4 Check Voltages Purpose: To verify output voltages of the power supply are at their proper levels. Inputs: 003/09608/00 Digital Voltmeter (DVM) 3-1/2 or 4-1/2 digit. 1. Remove the top of the instrument, the lid supports and the metal shield over the circuit board. 2. Turn on the instrument power. 3. Measure the voltages between each pair of test point listed on the data sheet. Record the voltages. 4. Replace the shield, supports, and lid. All voltages are within the given limits. 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. Background: This test verifies the power supply provides the correct voltage to the electronics. If the voltages are too high or too low then the electronics may be unable to operate correctly, or may operate intermittently or in unpredictable ways. 5.5 Initial Calibration Purpose: To verify basic functionality. To calibrate the pressure transducers and servo valve for the subsequent leak test.

9 Page: 9 of 37 Inputs: Computer to actuate the various parts of the instrument Paroscientific Pressure Gauge or Crystal Pressure Gauge (if is not available) Vacuum Calibration Standard. (Super Bee) Null modem serial cable Because this is not a final calibration step, it is not necessary to record the serial numbers of the pressure and vacuum standard. 1. Attach nitrogen gas at 15 psig to adsorptive gas inlet port. 2. Attach helium gas at 15 psig to the helium inlet port. 3. Pressurize the ports if they are not at atmospheric pressure (about 740 mmhg). a. Enable manual control. b. Close all valves. c. Open valves 4-b and 4-s. Open valve 2 (adsorptive) for 15 seconds. Close all valves. d. Enable the balance servo. e. Set the sample servo target to increase to 780 mmhg and turn the servo on. f. Turn the servo off when sample pressure stabilizes. g. Disable manual control. 4. Install the vacuum gauge on the sample port. Attach the null modem cable between the gauge s cable and the RS-232 connector on the rear of the instrument. 5. Install an empty straight-wall tube or plug on the balance port. 6. Zero the pressure transducers. a. Enter service test mode. b. From the main menu for the unit number being operated, select Calibration Zero Pressure c. Select all transducers. d. Press the Start button to invoke the zero pressure transducers routine.

10 Page: 10 of 37 e. Click Next when the vacuum gauge reads less than 100 µmhg. f. Click No when asked whether to save the calibration as reference. g. If you encounter no error message, proceed to the next step. 7. Scale the pressure transducers. a. Enter service test mode. b. Pressurize the reservoirs and ports to 780 mmhg as in step #3. c. Remove the vacuum gauge and install the pressure gauge. Attach the null modem cable between the gauge and the RS-232 connector on the rear of the instrument. d. If the instrument has a Po transducer, establish a pressure a little above atmospheric in the manifold i. Close all valves. ii. Open the vacuum valve for five seconds then close. iii. Open valves 5-b, 5-s, and 6. iv. Turn the servo on until pressure stabilizes then turn off. e. Leave manual mode. f. From the main menu for the unit number being operated, select Calibration Pressure Scale g. Select Sample Transducer and Po Transducer (if present) and click Next. h. When pressure stabilizes, 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. i. Click close when the calibration terminates. 8. Calibrate the sample servo. a. Pressurize the ports to 780 mmhg as in step #3. b. Install empty straight-wall tubes on the ports. c. From the main menu for the unit number being operated, select Calibration Sample Servo

11 Page: 11 of 37 d. Press the Start button to invoke the calibration routine. e. If you encounter no error message, proceed to the next step. 9. Calibrate the balance servo. a. From the main menu, for the unit number being operated, select Calibration Balance Servo b. Press the Start button to invoke the calibration routine. c. If you encounter no error message, proceed to the next step. All steps complete. Outputs: The data sheet and checklist must be marked indicating that this step has been completed. Background: A reasonable calibration is required in order to perform the initial leak test. 5.6 Initial Manifold Clean-up and Leak Test Purpose: To measure the outgas rates of the manifolds. To perform a leak test of each valve in the system. To flush undesirable contaminants from the system. Inputs: Computer to actuate the various parts of the instrument Vacuum Calibration Standard (Super Bee). 1. Pressurize the ports if they are not at atmospheric pressure (about 740 mmhg). a. Enable manual control. b. Close all valves. c. Open valves 4-b and 4-s. Open valve 2 (adsorptive) for 15 seconds. Close all valves. d. Set the servo target to increase to 780 mmhg and turn the servo on. e. Turn the servo off when sample pressure stabilizes. 2. Disable manual control. 3. Install the vacuum gauge on the sample port. Attach the vacuum gauge interface cable to the appropriate connector on the rear of the instrument.

12 Page: 12 of Enter service test mode. 5. 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. 6. Click Replace All. If the external vacuum gauge is attached then select LEAKALL.SVT. 7. 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. 8. 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) 9. 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. 10. 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\2390\leakall Datasheets 11. After out of tolerance conditions are fixed, 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. All measured manifold outgas rates and valve leak rates are less than the maximum allowable rates shown on the data sheet. Output: The filled out Data Sheet and Checklist, or a printout of the spreadsheet. Background: The Background section in step 5.10 contains many topics that apply to this initial test. 5.7 Pressure Transducer Calibration Purpose: To set the zero point and scaling of all the pressure transducers. To verify pressure transducer linearity. Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations Pressure Calibration Standard

13 Page: 13 of Vacuum Calibration Standard. (Super Bee) Null modem serial cable ; Note that the pressure zero and pressure scale steps differ from those in the initial calibration section. 1. Pressurize the ports if they are not at atmospheric pressure (about 740 mmhg). a. Enable manual control. b. Close all valves. c. Open valves 4-b and 4-s. Open valve 2 (adsorptive) for 15 seconds. Close all valves. d. Enable the balance servo. e. Set the servo target to increase to 780 mmhg and turn the servo on. f. Turn the servo off when sample pressure stabilizes. g. Disable manual control. 2. Install the vacuum gauge on the sample port. Attach the null modem cable between the gauge s cable and the RS-232 connector on the rear of the instrument. 3. Install an empty straight-wall tube or plug on the balance port. 4. Zero the pressure transducers. a. Enter service test mode. b. From the main menu for the unit number being operated, select Calibration Zero Pressure c. Select all transducers. d. Press the Start button to invoke the zero pressure transducers routine. e. Click Next when the vacuum gauge reads less than 20 µmhg. f. Click Yes when asked whether to save the calibration as reference. g. If you encounter no error message, proceed to the next step. 5. Scale the pressure transducers. a. Enter service test mode.

14 Page: 14 of 37 b. Pressurize ports to 780 mmhg as in step #1. c. Remove the vacuum gauge and install the pressure gauge. Attach the null modem cable between the gauge and the RS-232 connector on the rear of the instrument. d. If the instrument has a Po transducer, establish a pressure a little above atmospheric in the manifold. i. Open the vacuum valve for five seconds then close. ii. Open valves 5-b, 5-s, and 6. iii. Turn the servo on until pressure stabilizes then turn off. e. Leave manual mode. f. From the main menu for the unit number being operated, select Calibration Pressure Scale g. Select Sample Transducer and Po Transducer (if present) and click Next. h. When pressure stabilizes, click the From Reference button to enter the pressure reading from the Paroscientific gauge, or type in the pressure reading from the pressure calibration standard. Press enter. i. Click close when the calibration terminates. j. Enable manual control and open valves 5-b and 5-s until the sample pressure is below 300 mmhg. Close all valves. k. Repeat step #5 but with a servo setting of 380 mmhg. l. Proceed if the values for the transducers are within 2 mmhg of the reading on the pressure gauge. 6. Calibrate the sample servo. a. Pressurize the ports to 780 mmhg as in step #1. b. Install empty straight-wall tubes on the ports. c. From the main menu for the unit number being operated, select Calibration Sample Servo d. Press the Start button to invoke the calibration routine. e. If you encounter no error message, proceed to the next step.

15 7. Calibrate the balance servo. Page: 15 of 37 a. From the main menu, for the unit number being operated, select Calibration Balance Servo b. Press the Start button to invoke the calibration routine. c. If you encounter no error message, proceed to the next step. All steps completed. The zero calibration has been saved as reference. The transducer reading at 380 mmhg (0.5 Po) is within 2.0 mmhg of the pressure gauge. 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. 5.8 Balance Port Volume Adjustment Purpose: To equalize the volumes of the sample and balance ports. Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations. Empty sample tube Slot screwdriver 1. Install empty sample tubes in both ports. 2. Enable manual control. 3. Turn the balance adjustment screw all the way in and then back out 10 turns. 4. Turn off the servo. Make sure the balance servo is enabled. 5. Open the vacuum, reservoir, and port valves and let the system evacuate for 10 minutes.

16 Page: 16 of Close the vacuum and port valves. 7. Open the adsorptive valve for 15 seconds, then close it. 8. Allow the quantity adsorbed (reservoir differential transducer) reading to stabilize for 10 seconds. 9. Close valves 4-b and 4-s. 10. Allow the quantity adsorbed reading to stabilize for 5 seconds. Make a note of this reading; it will be used in step Set the dosing servo to dose to 800 mmhg and turn the servo on. 12. Allow quantity adsorbed and balance transducer readings to stabilize. 13. If the quantity adsorbed reading is greater than the initial value, unscrew (CCW) the volume screw. If it is less, screw in (CW) the volume screw. NOTE: Every two turns of volume screw is approximately 0.01 cm3 STP quantity adsorbed. 14. Repeat Steps 5-13 until a quantity adsorbed reading within cm 3 STP of the initial reading is achieved. 15. Leave manual mode. 16. Place a Dewar of room-temperature water on the elevator. 17. Select "PCP Analysis" from the service test menu. 18. Select "2-Point Nitrogen Balance" in the wizard. 19. Start the sample run and wait for it to finish. 20. If the quantity adsorbed reading at 0.9 relative pressure is greater than the one at 0.1, unscrew (CCW) the volume screw. If it is less, screw in (CW) the volume screw. NOTE: Every 1/4 turn of volume screw changes the quantity adsorbed at 0.9 relative pressure by approximately 0.01 cm 3 STP. 21. Repeat the 2-point balance run as needed to fine-tune the balance volume adjustment. 22. Perform the 9-Point Nitrogen Balance PCP analysis. Quantities adsorbed are within the tolerances shown on the data sheet. Background: The Gemini requires identical conditions on the balance and sample sides. This step fine-tunes the volume in the balance port to match the volume in the sample port. This adjustment also compensates for other imbalances in the instrument.

17 Page: 17 of Quantity Adsorbed Calibration Purpose: To calibrate the reservoir differential transducer to read quantity adsorbed. Inputs: Computer to actuate the various parts of the instrument. Gemini volume chamber. Container for ice bath. Data sheet to verify observations. 1. Attach the volume chamber in ice bath to the balance and sample ports. 2. Invoke the quantity adsorbed calibration routine. 3. Enter the volume of the reference chamber. 4. Click Start. The automatic operation completed. Outputs: Background: The data sheet and checklist must be marked indicating that this step has been completed. None 5.10 Final Leak Test Purpose: To measure the outgas rates of the manifolds. To evacuate the system and perform a leak test of each valve in the system. Acceptable initial outgas and leak rates from these initial tests indicate, there are no large leaks into the system from atmosphere. Inputs: Computer to actuate the various parts of the instrument Vacuum Calibration Standard (Super Bee) to the sample port. Connect the interface cable to the RS232 port on the back of the instrument. 1. Pressurize the ports if they are not at atmospheric pressure (about 740 mmhg). f. Enable manual control. g. Close all valves. h. Open valves 4-b and 4-s. Open valve 2 (adsorptive) for 15 seconds. Close all valves.

18 Page: 18 of 37 i. Set the servo target to increase to 780 mmhg and turn the servo on. j. Turn the servo off when sample pressure stabilizes. k. Disable manual control. 2. Install the vacuum gauge on the sample port. Attach the vacuum gauge interface cable to the appropriate connector on the rear of the instrument. 3. Enter service test mode. 5. 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. 5. Click Replace All. If the external vacuum gauge is attached then select LEAKALL.SVT. 6. 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. 7. 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) 8. 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. 9. 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\2390\leakall Datasheets 10. After out of tolerance conditions are fixed, 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. 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: These service tests can be run by Final Assembly the same day the instrument is turned on and system vacuum levels are below 1 mmhg.

19 Page: 19 of 37 Data obtained from this initial test indicates the analysis system has no large leak from atmosphere or the valves in the system. As test is run there is a gradual reduction of many undesirable contaminates in the system 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. Empty sample tubes 1. Attach an empty straight-wall tube to the sample and balance ports. 2. Place a Dewar of room-temperature water on the elevator. 3. Purge the helium line. a. Ensure that the helium line shut-off valve is open. b. Enter manual mode. c. Close all valves except for vacuum. d. Open the helium valve for 30 seconds, then close. e. Leave manual mode. 4. Select PCP Analysis from the service test menu. 5. Select 9-Point Nitrogen Blank in the wizard. 6. Start the sample runs and wait for them to finish. 7. Produce the nitrogen blank manufacturing report. The acceptable tolerances are shown on the data sheet. No jumps of 0.01 cm 3 STP or more. Outputs: The nitrogen blank manufacturing report or the filled-in table on the data sheet. 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.

20 Page: 20 of 37 Background: A flat blank isotherm ensures that systematic errors in the instrument are small. A blank that is not flat may indicate a leak. Large jumps may indicate a noisy transducer. The helium line is closed and evacuated for the leak test. Purging ensures that pure helium is used for the free-space measurement Reference Chamber Analysis Purpose: To verify the instrument s ability to accurately measure amount of gas adsorbed. 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 for the quantity adsorbed transducer calibration. Crushed ice. 1. Remove the Dewar from the elevator. 2. Connect the reference volume chamber to the sample and balance ports. 3. Evacuate the chamber under manual control until the sample transducer reads less than 10 mmhg. Leave manual control. 4. Select Volume Chamber 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. Produce the volume chamber manufacturing report or fill out the table in the data sheet. The acceptable tolerances are shown on the data sheet. The calculated volume must be between the limits calculated for the reference chamber used in this test. Outputs: The volume chamber manufacturing report or the filled-in table on the data sheet. 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 to check the calibration obtained with the other chamber Po Measurement Purpose: To determine the saturation pressure for the reference material analysis.

21 Page: 21 of 37 Inputs: Computer to actuate the various parts of the instrument. 1. Ensure that blank tubes are on the sample and balance ports. 2. Fill the Dewar with liquid nitrogen and allow to equilibrate for 30 minutes. 3. Select Po Measurement from the Unit menu. 4. For p and t models, select measurement in the Po tube. For the a model, the measurement will be done in the sample tube. 5. Start the measurement. 6. Enter the measured saturation pressure (from the Unit X Unit Configuration dialog), and the current atmospheric pressure into the data sheet. The analysis completes without error. Measured Po is within the limits on the data sheet. Background: The p and t models can measure Po during an analysis, but the a model can not. Performing the Po measurement before the analysis allows all instruments to use the same conditions for the sample runs Reference Material Sample Run Purpose: To verify the instrument s ability to measure surface area accurately. Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations carbon black reference material. Straight-wall sample tubes. 1. Prepare the reference material sample as outlined in the data sheet included with the reference material. 2. Fill the Dewar with liquid nitrogen and allow to equilibrate for 30 minutes. 3. Select Nitrogen Reference in the PCP analysis wizard. 4. Start the sample run and wait for it to finish. 5. Record the name, part number, lot number, multipoint surface area and area tolerance of the reference material on the data sheet.

22 Page: 22 of 37 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 meters helium and nitrogen Adsorption/Desorption Run (t model only) Purpose: To verify the instrument s ability to measured adsorption and desorption accurately. Inputs: Computer to actuate the various parts of the instrument. Data sheet to verify observations silica alumina reference material. Straight-wall sample tubes. 1. Prepare the reference material sample as outlined in the data sheet included with the reference material. 2. Fill the Dewar with liquid nitrogen and allow to equilibrate for 30 minutes. 3. Create a new file in the PCP directory. Use the name DNNN-0.SMP, where NNN is the instrument s serial number. Increment the number after the dash for repeat runs. Replace All with the file sialfull.smp in the data directory (one directory up). 4. Start the sample run and wait for it to finish, about 15 hours. 5. Record the name, part number, lot number, surface area and quantity adsorbed at 0.3 relative pressure of the reference material on the data sheet. 6. If the difference at 0.3 relative pressure exceeds the tolerance on the data sheet, the Vads transducer will need to be replaced. The discarded transducer may have acceptable performance in an a or p model. The acceptable tolerances are shown on the sample data sheet. Outputs: The data sheet must be filled out with the expected values and the measured values. 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.

23 Page: 23 of 37 Background: At 0.3 relative pressure, the quantity adsorbed on the desorption branch should match that on the adsorption branch. Non-linearity in the volume adsorbed transducer could cause the gap to be unacceptably large Save Instrument Calibration Purpose: Save calibration data and copy calibration files to network. Inputs: Networked computer terminal 1. Select Unit x from pull down menu (where x is the unit number being worked on). 2. Select Calibration, 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. Exit the 2390 application program. 6. Select Product Info. Transfer icon from the desktop. Select the model: 2390 short for models a and p, or 2390 tall for the t model. 7. Enter or select the instrument s serial number, press Enter. Calibration data were saved and transferred to the network. Outputs: Calibration files saved on network. The data sheet must be filled out and the checklist must be marked indicating that this step has been completed. Background: In order to create a Calibration CD for this instrument the calibration files must be saved to the network Create Calibration/Program CD Purpose: Create Calibration/Program CD to be shipped with instrument. Inputs: Personal computer with Lotus Notes , or verbal method of requesting CD creation.

24 Page: 24 of 37 (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. CD received from Final Assembly supervisor. Outputs: The data sheet must be filled out and the checklist must be marked indicating that this step has been completed. Background: The Calibration/Program CD is needed to be shipped with the instrument. It contains the current operating program and the calibration files Documentation Purpose: To combine the Data Sheet, the Checklist, and all of the reports for the instrument history file. Input: Completed Data Sheets, completed checklist, and all reports. 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. The operator has completed this step. Outputs: The data sheet must be filled out and the checklist must be marked indicating that this step has been completed. Background: None 5.19 Reset to Defaults Purpose: To delete data generated by analyses performed in the calibration procedure. Input: Computer Open the unit configuration dialog (Unit X Unit Configuration ) and click the Restore Factory Defaults button. Click Yes in the confirmation dialog. The operator has completed this step. Outputs: The checklist must be marked indicating that this step has been completed. Background: Analysis data must be removed from the instrument before shipment.

25 Page: 25 of Deliverables Purpose: To combine the calibration disk and all of the other loose items for shipment. Input: The calibration and program CDs, and all loose items that were tested with the instrument. 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. The operator has completed this step. Outputs: The data sheet must be filled out and 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.

26 Page: 26 of 37 Appendix A Data Sheet (page 1 of 6) Start Date: Core Part #: S/N: Operator(s): Part Number Description Serial # Cal. Due Date Pressure Calibration Standard or Vacuum Calibration Standard (Super Bee) First Reference Volume Chamber Kit Second Reference Volume Chamber Kit Multimeter 5.1 Set Instrument Serial Number Top line of control box display Typed-in serial number is displayed 5.2 Test Serial Communication Contents of display were printed 5.3 Manual Operation Checkout Did the Application program start successfully? Test passed? (attach report) Report filed sysc.svt and sysc.rep (stored in \\mic\products\2390\calibration Data) OK? OK? OK? 5.4 Check Voltages +TP -TP Acceptable Range Measured Voltage Within Tolerance? 18 (red) 14 (green) 4.75 to 5.25 VDC 28 (blue) 29 (black) 14 to 16 VDC 27 (yellow) 29 (black) -14 to -16 VDC 7 (white) 5 (black) 23 to 26 VDC

27 5.5 Initial Calibration No error messages Page: 27 of 37 OK?

28 Page: 28 of 37 Appendix A (page 2 of 6) 5.6 Initial Manifold Clean-up and Leak Test 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 (spreadsheet Appendix C). Perform the necessary calculations. All automatic or manually measured test results are within allowable limits on data sheet for initial data. OK? 5.7 Pressure Transducer Calibration Transducer Zero Verify vacuum gauge reads less than 20 µmhg. No error message? Transducer Scaling Verify transducer scaling has been completed. No error message? OK? OK? Scaling accuracy test Reference (mmhg) Sample Po Dosing Servo Calibration No error message? Balance Servo Calibration No error message? Displayed Pressure (mmhg) Difference less than 2.0 mmhg? OK? OK?

29 Page: 29 of 37 Appendix A (page 3 of 6) 5.8 Balance Port Volume Adjustment Point Balance Run Tolerance: Quantity adsorbed must be within the bounds marked on the nitrogen blank manufacturing report. The isotherm must show a fairly smooth trace with no sudden peaks. If the manufacturing report is not available, fill in the table below. PCP Analysis report OK? File: 9 -.SMP Relative Pressure Tolerance (cm3 STP) Nitrogen balance is within tolerances? 5.9 Quantity Adsorbed Transducer Calibration No error message? OK? OK? 5.10 Final Leak Test 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 on the data sheet (spreadsheet or Appendix C). Perform the necessary calculations. All automatic or manually measured test results are within allowable limits on data sheet for initial data. OK?

30 Page: 30 of 37 Appendix A (page 4 of 6) 5.11 Blank Sample Tube Run Tolerance: Quantity adsorbed must be within the bounds marked on the nitrogen blank manufacturing report. The isotherm must show a fairly smooth trace with no sudden peaks. If the manufacturing report is not available, fill in the table below. PCP Analysis report OK? File: B -.SMP Relative Tolerance (cm 3 STP) Pressure Nitrogen blank is within tolerances? Actual (cm 3 STP) OK? 5.12 Reference Chamber Analysis Tolerance: Volume must be within the bounds marked on the volume chamber manufacturing report. If the manufacturing report is not available, fill in the table below. Reference Chamber Volume (V) cm 3 Upper Limit = V 1.01 cm 3 Lower Limit = V 0.99 cm 3 Pressure nearest 760 mmhg (P) mmhg Quantity adsorbed at P (V P ) cm 3 STP Measured Volume = 760 V P /P cm 3 PCP Analysis report File: V -.SMP OK? Measured volume is between the upper and lower limits?

31 5.13 Po Measurement Measured Po Current atmospheric pressure Page: 31 of 37 Appendix A (page 5 of 6) mmhg mmhg Measured Po is within 25 mmhg of the current atmospheric pressure? No error message? 5.14 Reference Material Sample Runs Type of Material Part Number Lot Number Multipoint S/A from ref. material label m 2 /g Tolerance +/- m 2 /g PCP Analysis report File: N -.SMP OK? OK? 5.15 Adsorption/Desorption Run (t model only) Type of Material Part Number Lot Number Multipoint S/A from label m 2 /g OK? S/A Tolerance +/- m 2 /g Q a = Quantity adsorbed at 0.3 Po (adsorption) cm 3 /g STP Q d = Quantity adsorbed at 0.3 Po (desorption) cm 3 /g STP Q max = Maximum quantity adsorbed cm 3 /g STP (Q a Q d ) / Q max OK? Tolerance +/ Save Instrument Calibration Calibration data saved to network? 5.17 Create Calibration/Program CD CD created and labeled for shipping with instrument?

32 Page: 32 of 37 Appendix A (page 6 of 6) 5.18 Documentation To be compiled in this order; write N/A if not applicable. Appendix A, Data Sheet Appendix B, Checklist Appendix C, Leak Test Calculations Nitrogen blank run report Volume chamber report Reference sample run report All items present? 5.19 Reset to Defaults OK? 5.20 Deliverables Loose items that are tested and then delivered to stock with the instrument. Qty Analysis Dewar CD with calibration data (Po tubes remain installed on the instrument) All items present?

33 Page: 33 of 37 Appendix B Checklist (page 1 of 1) Start Date: Core Part #: S/N: Operator(s): PCP step Step Description Date Complete 5.1 Set Instrument Serial Number 5.2 Test Serial Communication 5.3 Manual Operation Checkout 5.4 Check Voltages 5.5 Initial Calibration 5.6 Initial Manifold Cleanup and Leak Test 5.7 Pressure Transducer Calibration 5.8 Balance Port Volume Adjustment 5.9 Quantity Adsorbed Calibration 5.10 Final Leak Test 5.11 Blank Sample Tube Runs 5.12 Reference Material Analysis 5.13 Po Measurement 5.14 Reference Material Analysis 5.15 Adsorption/Desorption Run (t model only) 5.16 Save Instrument Calibration 5.17 Create Calibration/Program CD 5.18 Documentation 5.19 Reset to Defaults 5.20 Deliverables

34 Page: 34 of 37 Appendix C Leak Test Calculations (page 1 of 2) a Service Test Information Serial Number Service Test File Name Test Rev Level Run Date b Manifold and Valve Leak Test data on this report came from an External Vacuum Gauge: Yes No Test Vacuum Level After Initial Evacuation Balance & Sample Port Outgas Rates (Sample Port) Balance & Sample Port Outgas Rates (balance xdcr) Manifold and Sample Port Outgas Rate Balance Port Outgas Rate (w/prior ogr) Measured Outgas Rates. Enter slope from service tests (umhg/min) Leak Rates. Enter slope from service tests (umhg/min) Manifold and Sample Port Outgas Rate Base or OGR Rate Enter slope from service tests (umhg/min) SYS OGR during test Difference Leak Rate Base Rate (umhg/min) Manifold and Outgas Rate Balance Port Outgas Rate SYS OGR during test Balance Port Outgas Rate Preliminary Limits Maximum rate (umhg/min) < 30.0 Good 30.1 to 70.0 Investigate > 70.1 Bad < 9.0 Good 9.1 to 14.0 Investigate > 14.1 Bad 6.00 to Good to Investigate < Bad > 6.01 Bad < 11.0 Good 11.1 to 25.0 Investigate > 25.1 Bad < 9.0 Good 9.1 to 14.0 Investigate > 14.1 Bad Po Port OGR Po Port OGR SYS OGR during test Po Outgas Rate < 9.0 Good 9.1 to 14.0 Investigate > 14.1 Bad Sample Reservoir OGR SYS OGR during Sample OGR Balance Reservoir OGR SYS OGR during Balance OGR Sample Port OGR (vac gauge) < 5.0 Good 5.1 to 9.0 Investigate > 9.1 Bad < 11.0 Good 11.1 to 25.0 Investigate > 25.1 Bad < 5.0 Good 5.1 to 9.0 Investigate > 9.1 Bad < 11.0 Good 11.1 to 25.0 Investigate > 25.1 Bad < 9.0 Good 9.1 to 14.0 Investigate > 14.1 Bad P a s s C h e c k F a i l

35 Page: 35 of 37 Test Sample & Balance Port OGR (balance xdcr) 5-s - Sample Valve Plunger Leak Test 5-b - Balance Valve Plunger Leak Test Valve 6 Plunger Leak Test Valve 4-s Plunger Leak Test Valve 4-b Plunger Leak Test Sample Servo Plunger Leak Test Balance Servo Plunger Leak Test 4-s Leak Rate with Sample Servo Leak 4-b Leak Rate Taken with Balance Servo Leak 5-b 5-s Leak Rate (during V 6 leak tst) 4-s 4-b leak (during V 6 leak) Helium Gas Line Leak Test Helium Gas Valve Leak Test Nitrogen Gas Line Leak Test Nitrogen Gas Valve Leak Test Measured Outgas Rates. Enter slope from service tests (umhg/min) Leak Rates. Enter slope from service tests (umhg/min) Appendix C Leak Test Calculations (page 2 of 2) Base or OGR Rate Enter slope from service tests (umhg/min) Difference Leak Rate Base Rate (umhg/min) Preliminary Limits Maximum rate (umhg/min) 6.00 to Good to Investigate < Bad > 6.01 Bad < 9.0 Good 9.1 to 14.0 Investigate > 14.1 Bad 6.00 to Good to Investigate < Bad > 6.01 Bad < 9.0 Good 9.1 to 14.0 Investigate > 14.1 Bad < 5.0 Good 5.1 to 9.0 Investigate > 9.1 Bad 6.00 to Good to Investigate < Bad > 6.01 Bad < 9.0 Good 9.1 to 14.0 Investigate > 14.1 Bad 6.00 to Good to Investigate < Bad > 6.01 Bad < 11.0 Good 11.1 to 25.0 Investigate > 25.1 Bad < 11.0 Good 11.1 to 25.0 Investigate > 25.1 Bad < 9.0 Good 9.1 to 14.0 Investigate > 14.1 Bad < 9.0 Good 9.1 to 14.0 Investigate > 14.1 Bad < 10.0 Good 10.1 to 20.0 Investigate > 20.1 Bad < 2.0 Good 2.1 to 7.0 Investigate > 7.1 Bad < 10.0 Good 10.1 to 20.0 Investigate > 20.1 Bad < 2.0 Good 2.1 to 7.0 Investigate > 7.1 Bad P a s s C h e c k F a i l

36 Page: 36 of 37 Appendix D PCP Author Completeness Checklist [x] Check power level in all important places. Sections: 5.4 [x] Initialize non-volatile memory: Programmable parts loaded. Board IDs set up properly. Confirm versions of all software used in system. Sections: 5.1 [x] Prepare (clean/set up) instrument before any tests are done. Sections: 5.5, 5.6 [x] Test both actuation and status of all items that can be actuated Sections: 5.3 [x] Calibrate and check all analog signals. Sections: 5.7 [x] Ensure all hardware adjustments done. Pots Restrictions Sections: 5.8 [x] Test subsystem performance independently of analyses. Leak rates, outgas rates Flow rates Sections: 5.6, 5.10 [x] Calibrate all subsystems that need it Volume calibration Normalization Sections: 5.7, 5.9 [x] Confirm proper operation and results with analyses. Sections: 5.12, 5.14, 5.14, 5.15 [x] Test all I/O devices on the instrument LEDs Computer and peripheral connections: RS-232, USB, Analog I/O Digital I/O Sections: 5.1, 5.2, 5.3 [x] Ensure enough time on the instrument to overcome initial component failures Burn in of heaters General components initial failure Sections: 5.6, 5.10 [x] Ensure that instrument information properly filed at end of PCP. Product Info Transfer has been updated (all files identified) Calibration and verification results to network. /99 CD made Data Sheet

37 Checklist Sections: 5.16, 5.17, 5.18 Page: 37 of 37