Product Calibration Procedure for the ASAP 2020 APPROVALS:

Product Calibration Procedure for the APPROVALS: Director of Engineering Stefan Koch Product Integrity & Performance Manager Tony Thornton Director of Quality Assurance Andy Dovin International Service Manager Derrick McAdoo Director of Manufacturing Adrian Gibson Domestic Service Manager Kevin Fouquette Manufacturing Engineering Manager Dennis Pyle Project Engineer Danny Strickland Application Specialist Jeff Kenvin Responsible Engineer Graham Killip 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. GK/sv Document Number: 202/34000/76 December 2, 2009

Page: 2 of 82 REVISION HISTORY Rev. ECN # DESCRIPTION OF CHANGE CHK BY DATE - 020001 Formal Release Kim Massengill April 3, 2003 A 030167 Revised per ECN. Kim Massengill July 15, 2003 B 030534 Revised per ECN. Kim Massengill April 20, 2004 C 050223 Gas inlet leak tests expanded Kim Massengill May 20, 2005 D 080153 Elevator revision level required Kim Massengill April 23, 2008 E 090392 Vapor option test added

1.0 PURPOSE Page: 3 of 82 This document describes the process used to calibrate and test the assembly. This includes any of the various options that may be installed in a shippable instrument. 2.0 SCOPE This document is used in the Final Assembly area. 3.0 APPLICABLE DOCUMENTS Users Instruction Manual: 202-42801-00 (Physisorption) and 202-42808-00 (Chemisorption). 4.0 REQUIREMENTS 4.1 Calibration Tools 004-09814-00 Pressure Calibration Standard. (Paroscientific) 202-09801-00 Temperature Standard, 100 ohm RTD simulator 003-09601-00 Meter, Type K Thermocouple. (Two preferred) 003-09608-00 Digital Voltage Meter. 003-09623-10 Vacuum Calibration Standard. (Yellow Jacket) 003-09619-00* Vacuum gauge, 10 micron, (may share cabinet with 100 micron gauge) 900-62610-00* Vacuum gauge, 100 micron (may share cabinet with 10 micron gauge) * Only if Vacuum Calibration Standard (003-09623-10) is unavailable 4.2 Special Tools 202-29800-00 Reference Volume Chamber. (Two required). (Or one of 202-29800-00 and one of 004-29801-00). 202-09800-00 Heating Mantle Test Tool. (Two preferred) 4.3 Utilities Nitrogen gas 99.999% pure @ 10 psig, 2 stage regulated, metal supply lines Krypton gas 99.99% pure @ 10 psig, 2 stage regulated, metal supply lines Helium gas 99.999% pure @ 10 psig, 2 stage regulated, metal supply lines Hydrogen gas 99.999% pure @ 10 psig, 2 stage regulated, metal supply lines Carbon Monoxide 99.99% pure @ 10 psig, 2 stage regulated, metal supply lines Electrical: 115 or 208 Vac, 60 Hz, 1000VA. (If the end user s power is known, then every attempt shall be made to operate the instrument at the same voltage and frequency.) Liquid Nitrogen. Crushed Ice. 4.4 Environment special ventilation or temperature requirements. 4.5 Reference Materials Use the same reference material that is shipped in the standard accessory kit(s).

Page: 4 of 82 4.6 Computer / Network / Software A Windows based computer, operating with the current released version of the instrument operating program, and connected to the network is required. 5.0 CALIBRATION PROCEDURE This procedure should be followed in sequential order. Some steps are to be skipped when the affected option is not installed. Service Test Mode is required for calibration. From the Options menu, select Service Test Mode. Enter the password mic.key. Verify that the units of measurement have been selected to match those used in this procedure. Pull down the Options menu, select Data Presentation, then select Units. In the dialog box, select cm 3 /g STP for volume, select mmhg for pressure, and select C for Temperature Units. Make a copy of Appendix A, Data sheet. Make a copy of Appendix B, Checklist. For units in which one or more Alcatel Hybrid high vacuum pumps are installed, they must be runin before putting into full operation. Refer to Appendix F for details. Units with the vapor option must have the top cover in place. The manifold temperature must have had at least four hours to equilibrate at the current setpoint. The manifold temperature reading on the manual control screen must be between 45 C and 47 C. If the manifold temperature is not in this range, adjust the setpoint on the temperature controller and allow temperature to equilibrate for four hours. 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. Action: Analysis system: From the manual control screen, verify the operation of the instrument by toggling the valves and observing the pressure transducers readings for appropriate change. Actuate the elevator and observe that it will raise to the up position, stop during travel, and lower to the down position. Locate the label on the elevator which identifies its revision level. Write this on the data sheet. Degas system: Verify basic valve operation by toggling valves open and closed and observing changes in pressure readings. Test the heating mantle system by unplugging the thermocouple, then plugging it back in to observe the effect on the readings. Acceptance Criteria: This portion of the check-out will be considered complete when all of the valves have been cycled, heating mantle thermocouple system responds and the elevator has been actuated.

Page: 5 of 82 Outputs: The data sheet must be filled out verifying the observations. The Date Complete column must be marked on the checklist indicating that this step has been successfully completed. Background: 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 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. Action: 1. Remove the lower rear panel of the instrument. This allows you to check the voltages on the test points of the power distribution board. WARNING: THERE ARE LINE VOLTAGES ON POWER SUPPLIES AND CONNECTORS IN THE POWER MODULE. 2. Turn on the instrument power. 3. Use the black test point (TP3) for the negative lead of the DVM. Set the DVM to measure DC Volts. 4. Measure the voltages at each test point listed on the data sheet. Record the voltages. 5. Set the DVM to measure AC Volts. Locate UM&L connector J16. Measure the voltage between pin 4 and pin 6. (It is not necessary to remove the cable that is plugged into the connector.) Acceptance Criteria: The voltages of the supplies were at the required values. Outputs: Complete the data sheet and checklist.

Page: 6 of 82 Background: This test verified the correct voltages are present. If the AC voltage (tested in Action step 5) is significantly out of specification range, then the voltage setting at the power entrance may not have been set to match the incoming line voltage. 5.3 Analysis Vacuum Gauge Calibration and Verification Purpose: To calibrate the analysis vacuum thermocouple gauge system. Inputs: 003/09608/00 Digital Voltmeter (DVM) 3-1/2 or 4-1/2 digit Small Screwdriver for potentiometer adjustment. Reference Vacuum Gauge system Nitrogen connected to gas inlet port. Reference Pressure gauge (Paroscientific) Action: 1. Remove the analysis port sample frit and the frit opener before beginning the procedure. Failure to remove the frit may cause calibration errors. Install the reference vacuum gauge in the sample port. Connect the Paroscientific gauge to the vapor inlet. Open valve 8 to allow it to be evacuated while the following steps are completed. 2. Backfill the manifold to about 800 torr with nitrogen. Open valve 9. CAUTION: Use only nitrogen gas to backfill the analyzer. Use of helium may cause errors in the vacuum gauge readings. 3. Remove the Po tube from the analyzer. Open valves 7 and 11 to allow the analyzer to vent to atmosphere. 4. Connect the DVM to read the vacuum gauge voltage. DVM Black lead on the ANALOG GND test point TP 11, green). DVM Red lead on the VAC XDCR test point (TP 4, white) on the Transducer Interface PCB. Set the DVM to the 200 mv range. 5. Adjust the ATM (also called zero or offset ) potentiometer on the vacuum gauge thermocouple amplifier PCB fully counterclockwise. Then raise the value to be about 160mV (acceptable range is 90 to 200mV.) The setting should be very sensitive to potentiometer adjustment. However, if the potentiometer appears to have very little influence on the reading, then you are at a false setting. Turn the potentiometer several turns clockwise, until the value drops and then rises to the specified value. 6. Record the offset voltage in the appropriate place on the data sheet in Appendix A. 7. Close valves 7 and 11.

Page: 7 of 82 8. Evacuate the lower manifold and vacuum gauge by opening valves 1 and 9. 9. When the vacuum level has reached its lowest level observed on the reference vacuum gauge (this will be below 20 microns) and stabilized, adjust the VAC (also called GAIN ) potentiometer to obtain the correct voltage on the DVM (± 0.5V) for the vacuum level obtained. Vacuum readings versus voltages are as follows: Vacuum Voltage Vacuum Voltage Vacuum Voltage 9 microns 3.046 16 microns 2.796 50 microns 2.301 8 microns 3.097 15 microns 2.824 40 microns 2.398 7 microns 3.155 14 microns 2.854 30 microns 2.523 6 microns 3.222 13 microns 2.886 20 microns 2.699 5 microns 3.301 12 microns 2.921 19 microns 2.721 4 microns 3.398 11 microns 2.959 18 microns 2.745 3 microns 3.523 10 microns 3.000 17 microns 2.770 2 microns 3.699 1 microns 4.000 10. Record the voltage at lowest vacuum in the appropriate place on the Appendix data sheet. 11. Zero (Tare) the Paroscientific gauge. When the reading on the reference vacuum gauge is stable, use the pull down menu to select vacuum gauge calibration. 12. Enter the value from the reference vacuum gauge onto the computer and accept the value. Record the value on the data sheet in Appendix A 13. Close the vacuum valve and admit nitrogen to about 800 torr. Open valves 7 and 11 to vent to atmosphere. 14. Reset the ATM pot to give an atmospheric voltage the same as before (± 10mV). If no adjustment is needed, proceed to the next step, otherwise repeat the above steps (6 thru 14) until voltages are within ± 10mV at atmospheric pressure and within ± 0.5V at the vacuum reading. 15. Observing the Paroscientific gauge, set the instrument pressure to approximately 0.500 torr. (The actual value may be from 0.450 to 0.550 torr.) Adjust the ATM pot until the vacuum gauge reading on the computer screen matches the Paroscientific gauge. 16. Evacuate and verify that the screen matches the reference vacuum gauge. If it does not, then return to step 13. 17. Set the pressure to approximately 500 microns (0.500 torr) Record the Paroscientific gauge (P) reading and computer reading on the data sheet in Appendix A. The value in the Difference column must be within the limits specified on the data sheet. 18. Evacuate the manifold and reference gauges. The vacuum should pull below 10 microns. Record the reference vacuum gauge (V) reading and computer reading on the data sheet in Appendix A. The value in the Difference column must be within the limits specified on the data sheet. 19. If removing the reference gauges, you must backfill with nitrogen to 760 torr. Close valves before removing the gauges. Re-install port frit and frit opener. If you will be performing pressure transducer calibration, then leave the system evacuating.

Page: 8 of 82 Acceptance Criteria: The voltages were calibrated within limits as described. The instrument software was calibrated to match the reference gauge. The calibration was verified. Outputs: Record acceptance and the vacuum thermocouple offset voltage in the appropriate places on the data sheet in Appendix A. Record the reference gauge information on the data sheet. Background: This step set the voltages for the vacuum gauge electronics and stored the voltages to be converted to vacuum gauge readings by the software. te that the voltage recorded for the vacuum gauge at atmospheric pressure will usually be different when checked later. This is because the fine tuning which is done at 500 microns will change the voltage. The fine tuning is done to provide a more useful and accurate vacuum gauge reading. The initial voltage adjustment was simply to get close to the required value. If the voltage had not been within the acceptable limits, then this would indicate a possible fault in a component. The vacuum gauge is used to ensure that the pressure in the system is sufficiently low to know that the vacuum system is working. It is not used to make measurements of pressure for any calculations. It may be used, at micron levels, to observe outgas rate. The accuracy deteriorates at levels above 100 microns, due to the difference in thermal conductivity of the various gases that may be used in the instrument. The fundamental principle of the thermocouple vacuum gauge tube is loss of heat from a filament to the surrounding gas. As the number of gas molecules around the filament drops, the filament gets hotter. The thermocouple filament generates a voltage which rises as the vacuum (pressure) gets lower 5.4 Calibrating the Temperature Sensor Purpose: To calibrate the temperature sensor. Input: Either: Reference Temperature Gauge (Temperature calibration standard). All panels installed. Or: Temperature Standard, 100 ohm simulators (23, 28, 33, 50 C) (202-09801-00)

Page: 9 of 82 Action: 1. If using the Temperature Gauge, insert the thermocouple probe into the receiving hole on the bottom of the manifold. Select C and allow the temperature to equilibrate. 2. If using the reference standard, remove the top (roof) of the instrument, unplug the instrument RTD and insert the calibrated resistor (28 C) in connector J6. 3. From the Unit <n> menu, choose Calibrate then Calibrate Temperature. Enter either the reference temperature gauge reading, or the calibrated temperature corresponding to the resistor. 4. Record the temperature and which method was used in the Data Sheet of Appendix A. 5. If using the reference standard, insert the calibration resistor for 23 C, then 33 C, then 50 C. Record the readings on the data sheet. 6. Reinstall the RTD. Replace the top panel. Acceptance Criteria: This portion of the test shall be considered complete when the routine is complete. If using the calibration resistors, then the readings after calibration must be within the limits shown on the data sheet Outputs: The Data Sheet must be completed and the Checklist marked indicating this step is complete. Background: 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. 5.5 Calibrating and Verifying the Pressure Transducer(s) Purpose: To calibrate and verify the pressure transducer(s) at known vacuum and pressure levels. te that there is a Service Appendix for Field calibration of Pressure Transducers. Inputs: Gasses connected Reference Pressure Gauge (Paroscientific) 003/09608/00 Digital Voltmeter (DVM) 3-1/2 or 4-1/2 digit If the vapor option is to be installed it must be in place and the manifold must be at operating temperature before this calibration is done.

Page: 10 of 82 Action: te: The term Tare is used below to indicate the zeroing function of the Paroscientific gauge. (The reference vacuum gauge system may remain attached to the analysis port during the following steps, to avoid disturbing the system). 1. Record the serial number and calibration expiration date of the Paroscientific gauge. 2. Attach the Paroscientific gauge to the vapor inlet port. 3. From the manual control screen, open valves 1, 2, 7, 8 and 9. 4. Evacuate to below 20 microns. Continue to evacuate for 5 10 minutes. While evacuation continues, measure the transducer output voltage(s) at the test points on the transducer interface board. Set the DVM on the millivolt range. If any voltages are outside of the acceptable limits, the offsets must be adjusted to within 10mV of zero. 5. While valves 1, 2, 7, 8 and 9 are still open, tare (zero) the Paroscientific gauge. Then zero the pressure transducers in the instrument, using the pull down calibration menu. 6. Ensure that nitrogen is available above valves 4 and 5. Re-open valves 8 and 9. The next 2 steps are for units with a 1 torr transducer installed. If the unit does not have a 1 torr transducer, skip to step 9. If the unit does not have a 10 torr transducer, skip to step 11 7. Close valves 1 and 2. Open valve 4 (or pulse valve 4 using the P key) to 0.7 torr (+/- 0.05 torr). Use the uncalibrated reading on the screen to achieve the nominal 0.7 torr target pressure. 8. From the Unit menu in the tool bar, choose calibration, then Pressure Scale (1torr). Execute and follow the instructions. Use the reading from the Paroscientific gauge to enter the correct value. Record the value used on the data sheet in Appendix A. The next 2 steps are for units with a 10 torr transducer installed. If the unit does not have a 10 torr transducer, skip to step 11. 9. Close valves 1 and 2. Using valve 4 slowly dose nitrogen to 7 torr (+/- 0.5 torr). Use the uncalibrated reading on the screen to achieve the nominal 7 torr target pressure. 10. From the Unit menu in the tool bar, choose calibration, then Pressure Scale (10 torr). Execute and follow the instructions. Use the reading from the Paroscientific gauge to enter the correct value. Record the value used on the data sheet in Appendix A. 11. With valves 1 and 2 closed, open valve 4. Pressure should increase very slowly. Record that you observed slow pressure increase on the data sheet of Appendix A. 12. Open valve 5 and the rate of pressure rise should become faster. Record that you observed fast pressure increase on the data sheet of Appendix A. Close valves 4 and 5 at 760 torr (± 10 torr). Use the uncalibrated reading on the screen to achieve the nominal 760 torr target pressure. 13. From the Unit menu in the tool bar, choose calibration, then Pressure Scale (1000 torr). Execute and follow the instructions. Use the reading from the Paroscientific gauge to enter the correct value. Record the value used on the data sheet in Appendix A. 14. Build or reduce pressure as required to achieve targets listed on the data sheet of appendix A. The values shown are nominal values. It is only necessary to be within about 5% of each target pressure.

Page: 11 of 82 15. Record those pressures from the computer display and from the reference gauge and check to make sure they are within specifications. 16. When complete, backfill the manifold to about 800 torr. 17. Remove pressure reference gauge and vacuum reference gauge (if still attached). Close valves 8 and 9, then open valves 1 and 2 to evacuate the system. Acceptance Criteria: This portion is considered complete when Steps 1-17 are successfully completed and all target pressures are within specifications. Output: The Data Sheet and Checklist are filled out, indicating that this step is complete. Background: Linearity of the 1000 torr transducer is important to achieve good free space measurements and good analysis data. The accuracy and linearity of all transducers allows accurate sample analyses to be attained. The pressure transducer calibration depends on temperature. If the vapor option is to be installed it must be in place and the manifold must be at operating temperature before this calibration is done. 5.6 Analysis Manifold Leak Test te: This step may not be needed if the manifold has been pre-tested on a manifold test cart. If so, proceed to the Action item 10, below. Purpose: To verify the vacuum integrity of the analysis manifold system. Inputs: Computer to actuate the various parts of the instrument. Action: 1. Thoroughly evacuate whole system with valves 1, 2, and 7 open. All other valves should be closed at this time. Gases may be connected to the physisorption gas inlet ports. 2. Evacuate at least two hours after attaining pressure below 10 microns. Overnight evacuation is preferable. 3. Close valves 1, 2, and 7. 4. te reading on the 1 torr transducer (first choice, if installed) or the 10 torr transducer (second choice, if installed) or the analysis vacuum gauge (if neither a 1 nor 10 torr transducer is installed). 5. Wait ten (10) minutes. 6. te the transducer reading again. 7. Subtract first reading from second reading. 8. Divide result by ten (10) to get lower manifold outgassing rate in microns/min. 9. Open valve 7 and repeat steps 4 through 8 for the combined upper and lower manifold outgassing rates.

Page: 12 of 82 10. Record the outgas rates on the data sheet. The rates may be derived from the previous steps or from the test cart report. Acceptance Criteria: Lower manifold and combined manifold acceptable leak rates are shown on data sheet. Outputs: The data sheet must be filled out with either the measured or the previously tested outgas rates. If the outgas rates are from the test cart report, then the report must be included with the other test documents. Background: Low outgas rate is essential for the instrument to perform an analysis. A high outgas rate could indicate a leak, or contamination. 5.7 Physi Gas Inlet Manifold Leak Test Purpose: To verify the vacuum integrity of the physi gas inlet manifold. Inputs: Computer to actuate the various parts of the instrument. Previous step completed. Action: te 1: If this system has a chemisorption option, then you may use the chemi software and perform PCP step 5.32 after this step. te 2: For pressure readings that are required in the following tests use the 1 torr transducer (if installed) or the 10 torr transducer (second choice, if installed) or the analysis vacuum gauge. 1. Close supply valves (i.e. Nupro valves) on lines attached to the physi gas inlet manifold. Install leak tight plugs in unused ports. 2. Open valves 1, 2, 7, PV, 4, 5 and PS. Evacuate the inlet ports by opening valves P1 to P6. 3. Evacuate at least 20 minutes. Overnight is preferred. 4. Close valves 1, 2 and PV, and record the pressure as the Initial Reading on the Data Sheet. 5. Wait three minutes, then record the pressure as the 3 Minute Reading on the data sheet. 6. Subtract the two readings and record on the Difference column on the Data Sheet. This indicates if any gas inlet valve, inlet plug or gas line is leaking from atmosphere. 7. Close all gas inlet manifold valves (P1 to P6). 8. Record the pressure as the Initial Reading then begin timing as soon as you complete the next step. 9. Pressurize the inlet to valve P1 by opening the supply valve or removing the port plug. This allows gas or air to pressurize the inlet valve above the seat. 10. After 3 minutes record the pressure as the 3 Minute Reading. Subtract the first reading from the second and record in the Difference column on the Data Sheet.

Page: 13 of 82 11. Repeat steps 8 to 10 for the inlet valves P2 to P6. Acceptance Criteria: Physi inlet manifold outgas rate is within acceptable limits shown on the datasheet. Physi gas inlet valves have outgas or leak rates within acceptable limits. Outputs: The data sheet must be filled out verifying the observations and that this step has been successfully completed. Background: Low outgas rates confirm that no gas inlet valves or interconnecting tubing are leaking. 5.8 System Volume Calibration Purpose: To measure the system volume of the dosing manifold. te that there is a Service Appendix for field re-calibration of system volume, which allows a modified procedure. Inputs: Reference volume chamber. Crushed ice, in suitable dewar. Port frit removed from sample port fitting. If the vapor option is to be installed it must be in place and the manifold must be at operating temperature before this calibration is done. Action: NOTE: The reference chamber must be free of internal water vapor. If you are not sure, then it must be baked and flushed with pure nitrogen. 1. Connect the reference volume chamber the analysis port. Connect the solenoid valve coil to the calibration valve cable, located under the access plate beneath the elevator. 2. Submerse the volume ball into an ice bath and allow it to equilibrate for ten minutes. Crushed ice must surround the volume ball. Add a little water to cause a thick slush to surround the volume ball. 3. Invoke the system volume calibration routine. 4. Select to run the volume calibration 3 times. 5. After all runs are complete, the average of the runs will be displayed on the computer screen. These values must be used as the system volume. Record the values on the data sheet. These values may also be recorded on the checklist (optional). 6. Record the serial number of the reference volume chamber on the data sheet.

Page: 14 of 82 Acceptance Criteria: The automatic operation completed. 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. Due to temperature gradients produced by the manifold heater, the system volume will change with temperature. If the vapor option is to be installed it must be in place and the manifold must be at operating temperature before this calibration is done. 5.9 Blank Tube Test (Nitrogen) Purpose: Test the sample manifold assembly during an automatic nitrogen analysis. The analysis conditions for this test are chosen to closely approximate the full pressure range and long run times of a full adsorption/desorption isotherm. The test typically takes between 11 to 15 hours to complete. Inputs: Sample tube (240-61003-00) Filler Rod (240-61016-00) Isothermal Jacket (202-25903-00) The instrument must be fully calibrated. All instrument panels should be installed. All gas inlet valves should have between 10 to 18 psig of gas pressure applied. Action: 1. Re-install the frit opener and port filter disk. 2. Attach the sample tube with isothermal jacket to the analysis port. 3. Evacuate analysis manifold, sample tube, Po tube and the N2 gas line for at least 1 hour. 4. Place the sample tube dewar cover over the sample tube stem just above the isothermal jacket. 5. Install the cold trap and analysis dewar filled to the correct level with liquid nitrogen and verified with the dipstick. 6. Begin evacuation of the sample tube. 7. Create a Sample Information File (see appendix C) 8. Verify that the correct sample information is displayed and selected (should be a file created and named as Nitrogen Blank). Do not select Report After Analysis. 9. Install the safety shields on the analyzer cold trap and analysis ports, then start the analysis. 10. Allow the run to complete before reviewing and printing data. Store completed sample file in permanent location. (See Output section, below, for file name information).

Page: 15 of 82 Acceptance Criteria: The acceptable tolerances are shown on the data sheet. Outputs: The data sheet must be filled out and tolerances met. The checklist must be marked indicating that this step is complete. Print out the results and keep with the other operational verification documents. The sample file is to be named PNBsn.SMP, where sn is the serial number of the instrument. Background: The long run time for this test is achieved thru the use of a 100-second equilibration interval, and a relative pressure table with 40 to 45 target pressures. With the 100 second equilibration interval, each relative pressure point in the pressure table will add a minimum of ((100 x 10) + 100) = 1,100 seconds (each pressure point takes approx. 18 min 20 sec). o This test is useful in detecting leaks into the analysis manifold from a gas supply valve or other valve that has pressure on it. The test can also detect atmospheric leaks into the analysis manifold from leaking plugs. It can also detect the resulting loss of gas that occurs when gas leaks out of the analysis manifold thru vacuum valves 1, and 2. o When using the results of this test for ascertaining the presence of a leak or high outgas rate, primary focus should be given to the first and last points. A line drawn between the first and last points can best illustrate the effect of a leak or high outgas rate. o The results from this test can provide useful insight into other aspects of the instruments performance. Volume adsorbed data that ends below 0.15 cc/g, indicate that gas is leaking into the manifold from a source of higher pressure. Sources of higher pressure include: gas inlet valves, Valves 8, 9, 10, & 11 as well as leaks from atmosphere at any of the manifold plugs, transducer connections, or associated interconnecting tubing.

Page: 16 of 82 Volume adsorbed data that ends above +0.15 cc/g, indicate that gas is leaking out of the manifold to a source of lower pressure. (i.e. Valve 1 or Valve 2). In this example, there are two unusual events. On the adsorption branch, there is a sudden drop of measured adsorption. The second event occurs during desorption, where the isotherm drops by about 0.1cm 3 /g The drops exceed the 0.05cm 3 /g limit specified in the Appendix, and require diagnostic work to identify the cause. It may be a leak or transducer defect. If the drops were less than 0.05cm 3 /g, they would be acceptable. If another test is done, and the event does not recur, then the system is considered acceptable without repair. However, if the step still occurs, then diagnostic work is needed to identify the cause and fix it.

Page: 17 of 82 The upper and lower limits established for this test take into account the maximum allowable upper and lower limits for freespace error. When these upper and lower limits are plotted, the V shape of the unfolded isotherm illustrate how any freespace error will be added to and then taken away from the 0.0 m2/g volume adsorbed base line. Freespace errors can sometimes be traced to contamination in the helium gas supply, leaks into the manifold that mix with helium during freespace measurement, overfilling the analysis dewar with LN2, the lack of a filler rod, or the lack of an isothermal jacket. Sometimes there will be a noticeable spike in the isotherm, close to a relative pressure of 1.0. This spike does not indicate a problem. The spike is usually cause by a insignificant difference in the measured saturation pressure in the Po tube, and the sample tube. This difference in saturation pressure will cause a spike when the sample file has a relative pressure point greater than 0.99. This spike can sometimes be avoided if the pressure table omits relative pressures greater than 0.985.

Page: 18 of 82 System Component(s) Being Targeted for Testing: 1000 torr, 10 torr, & 1 torr Transducers o As the test takes place, each of these transducers and associated electronics are tested. o Relative pressure points have been chosen to collect multiple data points over a significant range for each transducer. o 1 torr (relative pressures of: 0.00026 will take data at 0.2 torr, 0.00065 will take data at 0.5 torr, 0.00105 will take data at 0.8 torr) o 10 torr (relative pressures of: 0.0026 will take data at 2 torr, 0.0065 will take data at 5 torr, 0.0105 will take data at 8 torr) o 1000 torr (40 relative pressure points, 20 adsorption, 20 desorption) Sample Manifold Assembly o The port plugs and interconnecting tubing of this assembly are tested. Sample Manifold Valves V1 - V5, V7, V9, V10 & V11. o All of the active valves in the sample manifold are tested, to one degree or another, during this test. o Some valves are tested more that others. o Inactive valves include V6, & V8. Physi Gas Inlet Manifold Valves PV, PS, P1, P2, P3, P4, P5, P6. o In order for gas inlet valves to be tested there must be gas pressure on each gas inlet valve. Chemi Gas Inlet Manifold Valve CS, o The following valves (CV, C1, C2, C3, C4, C5, C6) are not tested during this test because they are isolated by valve CS. Vacuum Gauge Assembly o The vacuum gauge transducer and associated electronics are used during this test to measure when the manifold pressure is at any number of select set points. Elevator Assembly o The elevator is raised and lowered during this test.

Page: 19 of 82 5.10 Reference Chamber Analysis Purpose: The reference chamber test is used to verify that the scale factor accuracy and linearity of the instrument are within specifications. The reference chamber test confirms that the instrument accurately measures pressures and volume. The test is performed after temperature and pressure transducers are calibrated and the nitrogen blank tube run indicates that the instrument is free of gas leaks and other gas accounting errors. The test typically takes between 2 to 3 hours to complete. Inputs: Second reference volume chamber kit. Do not use the same chamber as used in step 5.9. Crushed ice, in suitable dewar. The instrument must be fully calibrated up to this step. All instrument panels installed. Nitrogen Blank Tube Test must have passed successfully. Action: NOTE: The reference chamber must be free of internal water vapor. If you are not sure, then it must be baked and flushed with pure nitrogen. 1. Connect the reference volume chamber to the sample port. Connect the solenoid valve coil to the calibration valve cable, located under the access plate beneath the elevator. The valve must be actuated via the manual mode screen and commands. Evacuate the chamber while preparing the test. You may also use a reference volume chamber with a manual valve. 2. Submerse the volume ball into an ice bath and allow to equilibrate for ten minutes. Crushed ice must surround the volume ball. Add a little water to cause a thick slush to surround the volume ball. 3. Set up a sample file for the volume chamber run using the analysis conditions in Appendix C. 4. Close the solenoid valve, then disconnect it. Start the analysis run and wait for the first point to be taken. Reconnect the solenoid valve, and open it. Then disconnect the solenoid connector for the rest of the analysis. You may open the valve before the first point, or you may allow up to three points to be taken. Then wait for the run to finish. 5. Record the serial number of the reference volume chamber kit on the data sheet. 6. Store completed sample file in permanent location. (See Output section, below, for file name information). Acceptance Criteria: The acceptable tolerances are shown on the data sheet. 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. The sample file is to be named PRCsn.SMP, where sn is the serial number of the instrument.

Page: 20 of 82 Background: The second reference chamber is used as a cross check that the reference chamber used on step 5.9 gave a good calibration value for the system manifold volume. Gas adsorption instruments indirectly determine surface area and pore volume by changing the pressure on a sample and then measuring the number of standard cubic centimeters of gas missing from the free space in the sample tube and that part of the instrument below the sample valve. This quantity of missing gas, plotted against pressure and measured at constant temperature, is called an isotherm. Surface area and pore volume can then be calculated from the isotherm data. If an instrument is not properly calibrated, the isotherm will contain errors. Undetected errors can disproportionately affect the BET calculation, t-plots, and calculation of BJH pore volumes. Often these computational variations are magnified over those in the original isotherm. o The reference chamber test verifies that the instrument accurately measures pressure, volume, and temperature. o The reference chamber test uses the definition of a standard cubic centimeter of gas to verify the accuracy of an instrument. During the test, the reference chamber is immersed in a Dewar filled with ice and water to maintain a temperature of 0ºC (the standard temperature). The reference chamber then extracts from the instrument a known gas (nitrogen) which fills the known volume of the reference chamber. If the instrument does not report (within specified limits) the amount of gas missing from the free space, the instrument is not properly calibrated. o The volume of a reference chamber itself is determined using a simple laboratory procedure. The empty chamber is weighed and then filled with a fluid (water or mercury) of known density. The volume of the chamber is then calculated based on the weight and density of the fluid. The procedure is repeated and the results are averaged. Using these methods, Micromeritics has attained an accuracy of chamber measurement better than ±0.1%. o The results of tests which rely upon the use of reference or standard materials may vary because of differences in how samples are handled, prepared and weighed. The reference chamber test removes these variables and may also be performed more quickly than tests using reference or standard materials. Micromeritics has established the reference chamber test as one of the pass/fail criteria for its gas adsorption instruments.

Page: 21 of 82 o The Calibration Volume Plot, shown in this section, is the graphic report produced by the instrument software when Service Test Mode is used. o The Volume of the reference chamber in the illustrated test was 407.690 cc. o This value was entered into the software and the upper and lower limits displayed in this report were automatically calculated. o The upper and lower limits for this test were calculated by adding and subtracting 0.5 % from the known volume of the reference chamber. o The 407.690 cc chamber would have an upper limit of 409.73 cc and a lower limit of 405.65 cc. o The calculated data from the test is determined by taking the reported Volume Adsorbed, and Pressure data reported between 0.5 Relative Pressure and performing the following calculation: Calculated Volume = Volume Adsorbed X (760/Pressure) o The data in the table below shows how this formula manually calculates the results of the test. Relative Pressure Pressure Volume Adsorbed Calculated Data 0.4941 375.53290 201.1775 407.1411 0.7328 556.96051 298.3848 407.1607 0.8949 680.16858 364.4257 407.1983 0.9783 743.56476 398.3550 407.1599 0.9039 686.98627 368.1434 407.2701 0.7054 536.13306 287.1431 407.0421 0.5056 384.26898 205.6367 407.7044

Page: 22 of 82 o Data is not typically used below relative pressures of 0.5. o The reason for this is the slow gas flow into and out of the reference chamber, thru the narrow tubing, at increasing lower pressures sometimes causes the reported calculated volume data to curve downward. o This false indication is eliminated by only using data above 0.5 relative pressure. o The falling slope towards the end of the runs is attributed to unknown causes. System Component(s) Being Targeted for Testing: 1000 torr Transducer o As the test takes place, this transducer and its associated electronics are tested. Temperature RTD o Data is taken from this device throughout this test. te: Errors in Manifold Temperature will cause the results of this test to be out of spec. If the calculated results of this test are too high, the manifold calibrated temperature may need to be raised, (if the entered manifold temperature is determined to have been too low). Likewise, if the calculated results of this test are too low, lowering the manifold temperature will raise subsequent test results. 5.11 Nitrogen Standards Test (N2) Purpose: To describe the procedures for performing the reference sample analysis using nitrogen. Inputs: Sample tube (240-61003-00) Filler Rod (240-61016-00) Isothermal Jacket (202-25903-00) Reference Material (as shipped with the accessories) Balance Port frit installed in sample port Action: 1. Degas reference material as per reference material data sheet. The weight of the degassed sample must be obtained. The degassing may be done on a 2020 or other degas system. 2. Evacuate analysis manifold, Po tube and the N2 gas line for approximately 1hr. 3. Install the sample tube and isothermal jacket. 4. Place the sample tube dewar cover over the sample tube stem just above the isothermal jacket. 5. Install the cold trap and analysis dewars filled to the correct level with liquid nitrogen and verified with the dipstick. 6. Create a Sample Information File (see appendix c) 7. Verify that the correct sample information is displayed and selected (should be file created and named as Nitrogen Standard). Do not select Report After Analysis. 8. Install safety shields on the cold trap and sample port then start the analysis. 9. Allow the run to fully complete before reviewing and printing data.

Page: 23 of 82 10. Store completed sample file in permanent location. (See Output section, below, for file name information). Acceptance Criteria: The acceptable tolerances are shown on the data sheet of the reference material. Outputs: The data sheet must be filled out and tolerances met. The checklist must be marked indicating that this step is complete. Print out the results and keep with the other operational verification documents. The sample file is to be named PNRsn.SMP, where sn is the serial number of the instrument. Background: This step verified that the instrument could measure freespace and nitrogen uptake accurately. 5.12 Performing a Krypton Blank Tube Test (Units with 10 torr transducers) Purpose: Test the sample manifold assembly during an automatic krypton analysis. The analysis conditions for this test are chosen to closely approximate the low pressures of a krypton surface area analysis. This test also tests the instrument s ability to store and purify krypton in the Po Tube. The test typically takes between 2 to 6 hours to complete. Inputs: Sample tube (240-61003-00). filler rod. Isothermal Jacket (202-25903-00) Action: 1. Attach the sample tube and isothermal jacket to the analysis port. 2. Evacuate analysis manifold, Po tube and the Kr gas line to the regulator for approximately 2 hr. 3. Install the sample tube and isothermal jacket. 4. Place the sample tube dewar cover over the sample tube stem just above the isothermal jacket. 5. Install the cold trap and analysis dewar filled to the correct level with liquid nitrogen and verified with the dipstick. 6. Begin evacuation of the sample tube. Then continue to enter the parameters while the sample tube is being evacuated. 7. Create a Sample Information File (see Appendix c) 8. Verify that the correct sample information is displayed and selected (should be file created and named as Krypton Blank). Do not select Report After Analysis. 9. Install safety shields on the cold trap and sample port then start the analysis. 10. Allow the run to fully complete before reviewing and printing data. 11. Store completed sample file in permanent location. (See Output section, below, for file name information).

Page: 24 of 82 Acceptance: The acceptable tolerances are shown on the isotherm graph, and on the Data Sheet (Appendix A). Outputs: The data sheet must be filled out and tolerances met. The checklist must be marked indicating that this step is complete. Print out the results and keep with the other operational verification documents. The sample file is to be named PKBsn.SMP, where sn is the serial number of the instrument. Background: This test verifies that very small leaks do not affect the ability to run low surface area samples. This test also verifies that the Krypton purification step works correctly. o The krypton blank tube test plot shown to the right is the graphic report produced by the instrument software when Service Test Mode is used. o The seemingly steep slope of the upper limit allows for some adsorption that may occur on the walls of the sample tube.

Page: 25 of 82 5.13 Krypton Standards Test (Units with 10 torr transducer) Purpose: To describe the procedures for performing analysis of a low surface area material. Inputs: Sample tube (240-61003-00) Filler Rod (240-61016-00) Isothermal Jacket (202-25903-00) Reference Material (as shipped with the accessories) Balance Action: 1. Degas sample as per reference material data sheet. The weight of the degassed sample must be obtained. 2. Attach the degassed sample and isothermal jacket to the analysis port. 3. Evacuate analysis manifold, Po tube and the Kr gas line to the regulator for approximately 2 hr. 4. Install the sample tube and isothermal jacket. 5. Place the sample tube dewar cover over the sample tube stem just above the isothermal jacket. 6. Install the cold trap and analysis dewar filled to the correct level with liquid nitrogen and verified with the dipstick. 7. Create a Sample Information File (see Appendix C) 8. Verify that the correct sample information is displayed and selected (should be file created and named as Krypton Standard). Do not select Report After Analysis. 9. Install safety shields on the cold trap and sample port then start the analysis. 10. Allow the run to fully complete before reviewing and printing data. 11. Store completed sample file in permanent location. (See Output section, below, for file name information). Acceptance: The acceptable tolerances are shown on the reference material data sheet. Outputs: The data sheet must be filled out and tolerances met. The checklist must be marked indicating that this step is complete. Print out the results and keep with the other operational verification documents. The sample file is to be named PKRsn.SMP, where sn is the serial number of the instrument. Background: This test verifies that the system can accurately measure the uptake of Krypton gas and not become contaminated by leaky nitrogen or helium gas inlet valves.

Page: 26 of 82 5.14 Vapor Option Test (Units with the vapor option) Purpose: To check the operation of the heated manifold cover and vapor box. Inputs: Vapor option (202-33054-00) Action: 1. Install the heated manifold cover and its cabling. The vapor enclosure need not be mounted to the instrument. 2. Install the instrument s top cover. 3. Connect the controller to the vaporizer and to the connector for the heated duct (mounted on the rear of the instrument, at the top of the vacuum pump cave). 4. Set the controllers to 57 C (manifold) and 40 C (vaporizer). 5. Wait four hours for the manifold to warm up. 6. Perform the instrument calibration procedure starting from section 5.0 of this document. 7. Record setpoints and temperature readings on the data sheet. Acceptance: The acceptable tolerances are shown on the data sheet. Outputs: The data sheet must be filled out and tolerances met. The checklist must be marked indicating that this step is complete. Background: This test verifies that the temperatures are properly controlled for vapor analyses. Pressure transducers and system volume calibrations need to be performed after the temperature stabilizes. The section numbers jump to 5.20 for the degas system This is to allow adding more steps while minimizing editing chores.

5.20 Degas Vacuum Gauge Calibration Page: 27 of 82 Purpose: To calibrate the degas vacuum thermocouple gauge system. Inputs: 003/09608/00 Digital Voltmeter (DVM) 3-1/2 or 4-1/2 digit, with small hook probes or clip leads to attach to scope probe test hooks Small Screwdriver for potentiometer adjustment Reference Vacuum Gauge system Reference Pressure gauge (Paroscientific) Nitrogen connected to degas inlet port Action: 1. Unless already done, you must remove the sample frit and the frit opener from both degas ports before beginning the procedure. Failure to remove the frits may cause calibration errors. 2. Install the reference vacuum gauge in the right port. 3. Install the Paroscientific gauge in the left port. 4. Backfill the manifold to about 760 torr with nitrogen. CAUTION: Use only nitrogen gas to backfill the analyzer. Use of helium will cause errors in the vacuum gauge readings. 5. On the Degas Control PCB, connect the DVM to read the vacuum gauge voltage, guided by the following chart: Circuit Board Number Analog ground test hook VAC XDCR test hook 202/17710/011 TP 10, green TP 15, gray 202/17720/011 TP 8, green TP 10, gray Set the DVM to the 200 mv range. 6. Adjust the ATM (also called zero or offset ) potentiometer on the vacuum gauge thermocouple amplifier PCB fully counterclockwise. Then raise the value to be about 100mV (acceptable range is 90 to 200mV). The setting should be very sensitive to potentiometer adjustment. However, if the potentiometer appears to have very little influence on the reading, then you are at a false setting. Turn the potentiometer several turns clockwise, until the value drops and then rises to the specified value. 7. Record the offset voltage in the appropriate place on the data sheet in Appendix A. 8. Evacuate the both ports by opening valves D1, D2 and D5.

Page: 28 of 82 9. When the vacuum level has reached its lowest level observed on the reference vacuum gauge (this will be below 20 microns) and stabilized, adjust the VAC (also called GAIN ) potentiometer to obtain the correct voltage on the DVM (± 0.5V) for the vacuum level obtained. Vacuum readings versus voltages are as follows: Vacuum Voltage Vacuum Voltage Vacuum Voltage 9 microns 3.046 16 microns 2.796 50 microns 2.301 8 microns 3.097 15 microns 2.824 40 microns 2.398 7 microns 3.155 14 microns 2.854 30 microns 2.523 6 microns 3.222 13 microns 2.886 20 microns 2.699 5 microns 3.301 12 microns 2.921 19 microns 2.721 4 microns 3.398 11 microns 2.959 18 microns 2.745 3 microns 3.523 10 microns 3.000 17 microns 2.770 2 microns 3.699 1 microns 4.000 10. Record the voltage used in the appropriate place on the data sheet in Appendix A. 11. Close the vacuum valve and admit nitrogen to about 760 torr. (700 to 800 torr). 12. Reset the ATM pot to give an atmospheric voltage the same as before (± 10mV). If no adjustment is needed, proceed to the next step, otherwise repeat the above steps (6 thru 12) until voltages are within ± 10mV at atmospheric pressure and within ± 0.5V at the vacuum reading. 13. Evacuate the vacuum gauge to the below 20 microns, and then allow it to evacuate for 10 more minutes. 14. When the reading on the reference vacuum gauge is stable, use the pull down menu to select degas vacuum gauge calibration. Enter the value from the reference vacuum gauge onto the computer and accept the value. 15. Record the value on the data sheet in Appendix A. Acceptance Criteria: The voltages were calibrated within limits as described. The instrument software was nominally calibrated to match the reference gauge. (The calibration will be verified at other pressures in a later step). Outputs: Complete the appropriate places on the data sheet in Appendix A. Record the reference gauge information on the data sheet. Background: This step set the voltages for the vacuum gauge electronics and stored the voltages to be converted to vacuum gauge readings by the software. te that the voltage recorded for the vacuum gauge at atmospheric pressure will usually be different when checked later. This is because the fine tuning which is done at 1000 microns will change the voltage. The fine tuning is done to provide a more useful and accurate vacuum gauge reading. The initial voltage adjustment was simply to get close to the required value. If the voltage had not been within the acceptable limits, then this would indicate a possible fault in a component.