product calibration procedure for the … calibration procedure for the asap 2020 ... 003-09619-00*...

Product Calibration Procedure for the

ASAP 2020

APPROVALS: Director of Engineering Product Integrity & Performance Manager Stefan Koch Tony Thornton Director of Quality Assurance International Service Manager Andy Dovin Derrick McAdoo Director of Manufacturing Domestic Service Manager Adrian Gibson Kevin Fouquette Manufacturing Engineering Manager Project Engineer Dennis Pyle Danny Strickland Application Specialist Responsible Engineer Jeff Kenvin 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 Revision: ( E ) December 2, 2009

Title: Product Calibration Procedure for the ASAP 2020

Date: December 2, 2009 Page: 2 of 82

Number: 202/34000/76 Revision: ( E )

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

This document describes the process used to calibrate and test the ASAP 2020 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

No special ventilation or temperature requirements.

4.5 Reference Materials Use the same reference material that is shipped in the standard accessory kit(s).




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 cm3/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 “run-in” 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.




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.




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.




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.




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. Note 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)




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. Note

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.




Action: Note: 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.




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

Note: 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. Note 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. Note 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.




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:

Note 1: If this system has a chemisorption option, then you may use the chemi software and perform PCP step 5.32 after this step. Note 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.




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. Note 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.

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. Action:

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.




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).




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.




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 0.1cm3/g The drops exceed the 0.05cm3/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 0.05cm3/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.




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.




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.




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.

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. Action:

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.




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.




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




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. Note: 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.




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). No 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).




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.




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.




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

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.




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. Note 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.




5.21 Degas Pressure Gauge and Servo Valve Calibration and Verification

Purpose:

To calibrate the Degas pressure transducer at known vacuum and pressure levels. Also to calibrate the Servo Valve.

Inputs:

Reference Pressure Gauge (Paroscientific) Nitrogen connected to degas inlet port. Reference vacuum gauge

Action: 1. Record the serial number and calibration expiration date of the Paroscientific gauge, if different

from the device used for the analysis system calibration. 2. 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. 3. Install the reference vacuum gauge in the right port, install the Paroscientific gauge in the left

port 4. From the manual control screen, open valves D1, D2 and D5 to evacuate the Paroscientific

gauge, reference vacuum gauge and the degas manifold. 5. Evacuate to below 20 microns, as shown on the reference vacuum gauge. Zero (Tare) the

Paroscientific gauge. 6. From the Unit menu in the tool bar, choose “degas”, then “Calibrate Pressure Zero” to zero the

screen reading. 7. Open valve D1, then admit nitrogen to about 760 torr (± 10 torr) as shown on the Paroscientific

gauge. 8. From the Unit menu in the tool bar, choose “degas”, then “Calibrate Pressure Scale”. Execute

and follow the instructions. Record the pressure used for this step on the datasheet. 9. Open valves D1,D2 and D5 and evacuate the manifold until the vacuum level is below 20

microns. The Paroscientific gauge should read zero. Observe the pressure reading on the computer screen (it should read zero ±1 torr). If it does not, then return to step 4.

10. From the Unit menu in the tool bar, choose “Degas”, then “Calibrate Servo”. 11. Click Start. Calibration data will appear on the screen during the automatic calibration process.

When the routine is complete, a message appears that verifies that the servo valve has been calibrated. The degas system will have been backfilled to an elevated pressure.

12. Open valve D1. 13. If the pressure is below 750 torr, then you must raise the pressure to about 800 torr before

proceeding. 14. Open valve D6, then double-click (or right click) the Servo valve to display the Servo Valve

Settings dialog. Enter 760 torr in the Target pressure field, and then click OK. (The set point is displayed below the Servo valve in the schematic.)

15. Observe the pressure reading on the schematic. When it reaches 760 torr, record the Paroscientific gauge reading and the computer reading on the data sheet in Appendix A.

16. Repeat steps 14 and 15 for each of the remaining target pressures: 550, 350, and 150 torr. Calculate the errors for the servo accuracy and for the calibration accuracy. The values in the “Error” columns must be within the limits specified on the data sheet in Appendix A.




17. If removing the reference gauges, you must backfill them to 760 torr. Close the port valves then

remove the gauges. Re-install the port frits and frit openers. If continuing with the next step (Vacuum gauge final calibration and verification) then you must leave the reference gauges installed.


The automatic Servo Valve calibration was successful, and the transducer readings showed that the calibration and the Servo system operates correctly.

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

The pressure calibration is required to allow controlled evacuation and controlled backfilling after degas. The transducer is not used for analysis data. The servo valve calibration is required for the controlled evacuation of samples. The software performs the calibration automatically.

5.22 Degas Vacuum Gauge Final Calibration and Verification

Purpose: To perform final calibration and verification of 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)

Action: 1. Evacuate the degas system and the attached vacuum gauge and Paroscientific gauge to below 20

microns, and then allow to evacuate for 10 more minutes. 2. Zero (Tare) the Paroscientific gauge. 3. When the reading on the reference vacuum gauge is stable, verify that the computer screen

reading of the degas vacuum gauge is within the limits shown in Appendix A. If it is acceptable, go on to step 4. If it is not, then 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. 4. Using the degas Servo valve system, set the target pressure to 1 torr. Adjust the ATM pot until the vacuum gauge reading on the computer screen matches the

Paroscientific gauge. 5. Evacuate and verify that the screen matches the reference vacuum gauge. If it does not, then

return to step 1. 6. Set the Servo target pressure to 1 torr. When the pressure is stable, record the Paroscientific

gauge (P) and computer readings in Appendix A.




7. Evacuate the degas system. When the pressure is stable, record the reference vacuum gauge (V)

and computer readings in Appendix A. The values in the Difference column must be within the limits specified on the data sheet. If they are not, return to step 1.

8. If removing the reference gauges, you must backfill them to 760 torr. Close the port valves then remove the gauges. Re-install the port frits and frit openers.


The voltages were calibrated within limits as described. The instrument software was calibrated to match the reference gauge. The calibration was verified at other pressures.

Outputs: Complete the appropriate places on the data sheet in Appendix A. Background:

The fine tuning is done to provide a more useful and accurate vacuum gauge reading. The fine tuning which is done at 1000 microns will change the voltages recorded earlier. The initial voltage adjustment was simply to get close to the required value and to allow the pressure gauge zeroing to be performed correctly.




5.23 Heating Mantle Test Purpose: To verify the degas heater system Inputs:

Temperature reference gauge (two preferred) 2 heating mantle test tools (202-09800-00) 2 heating mantles with clips

Action: 1. Install a test tool into each mantle. Insert the probe of the reference temperature meter into

the hole in the tool. (unless the thermocouple is already attached to the tool). If a second reference temperature meter is available, install it in the other mantle test tool. Use a mantle clip to close the mantle around the tool(s).

2. On the data sheet, record the ambient temperature reading of the meter and the mantle (from the screen).

3. Unplug the left port mantle’s thermocouple connector from the instrument. Observe the screen reading, and record the value on the data sheet. Then plug the connector back in.

4. Set the ramp rate at 10°C per minute, and the target temperature at 95°C for the left mantle, 105°C for the right.

5. After stabilization, record the reference meter reading and the screen reading. 6. Set the target temperature at 195°C for the left mantle, and 205°C for the right. 7. After stabilization, record the reference meter reading and the screen reading. 8. Set both mantles to 0°C. Remove the tools when cool.

Acceptance Criteria: The mantle readings were within the limits shown on the data sheet. Output: The Data Sheet and Checklist are filled out, indicating that this step is complete. Background:

The mantles must reach the setpoints and stabilize within the acceptable tolerances to ensure that samples are degassed correctly. The instrument specification for heating accuracy is stated as “Deviation less than +/- 10 ºC of set point at thermocouple”. This temperature is shown on the screen. This does NOT mean that the sample itself is +/-10°C of the set point. The mantle has to serve as an electrical insulator, which- unfortunately - also makes it a thermal insulator. Therefore there is an ever present gradient of temperature within the mantle system.




5.24 Verify Degas Manifold Outgas Rate

Purpose: To verify the vacuum integrity of the degas manifold. Inputs: Computer to actuate the various parts of the instrument. Action:

1. Thoroughly evacuate the degas manifold by opening valve D5. All other valves should be closed at this time.

2. Evacuate at least one hour after attaining pressure below 10 microns. Overnight evacuation is preferable, and will affect the outgas rate.

3. Close valves D5. 4. Record reading on degas vacuum gauge on datasheet in Appendix A. 5. Wait five (5) minutes. 6. Record reading again on degas vacuum gauge on datasheet in Appendix A. 7. Subtract first reading from second reading. 8. Divide result by five (5) to get the degas manifold outgassing rate in microns/min.

Acceptance Criteria: Degas manifold outgas rates are within limits shown on data sheet.

Outputs:


Background: Low outgas rates confirm that no degas valves or manifold components are leaking. The outgas rate is affected by how recently the manifold was exposed to air, water vapor in the air, and any other gas. Prolonged evacuation, such as overnight, will help to remove such gases and water vapor from the elastomer seals and the surface of the manifold itself. A high outgas rate after overnight evacuation suggests that a leak is present. It may be from the gas inlet valve or it may be across a seal to atmosphere.

The section numbers jump to 5.30 for the chemisorption system This is to allow adding more steps while minimizing editing chores




5.30 Chemisorption Initial Installation

Purpose: To verify that the Chemisorption port and furnace system fit correctly.

Inputs: Chemisorption port assembly Chemisorption furnace assembly Chemisorption sample tube (004/61701/00) with filler rod (004/61701/02)

CAUTION Do not touch the sample tube or filler rod with bare skin. Oils from your skin will be left upon the quartz tubes and will cause etching of the quartz when subjected to high temperatures. Always use gloves to handle the quartz tubes. The quartz tubes must be wiped with alcohol to remove oils.

Action: 1. Install the chemisorption port assembly onto the panel above the elevator. It will be

necessary to rotate the Po tube to the left and back towards the instrument front panel. Connect the D connector to the chemisorption front panel. Connect the sample thermocouple extension cable to the front panel. Connect the exhaust gas hose to the inlet on the front panel.

2. Place the furnace on the elevator. Center it on the elevator. Connect the furnace power cable to the connector on the lower front of the chemisorption front panel. Connect the thermocouple extension cable to the furnace thermocouple connector on the lower front of the same panel. Connect the furnace cooling gas supply hose to the connection on the front panel.

3. Connect a hose with cooling air or nitrogen to the furnace cooling gas inlet on the right side chemisorption accessory panel. The supply pressure is to be as specified in the instruction manual (nominally 3 to 6 psig). Connect an exhaust hose to the outlet on the same accessory panel. The exhaust must vent safely to an exhaust hood or equivalent.

4. NOTE: Do not touch the quartz sample tube with your fingers. Finger moisture and grease will poison the quartz. At high temperatures, the poisoned quartz will disintegrate. Install a chemisorption sample tube onto the port. Lightly grease the O-Rings with Dow Corning Vacuum Grease. Open valves 9 and 1 to allow the sample tube to pump out for at least 10 minutes to eliminate any out-gassing.

5. If not already running, start the 2020 Chemisorption software. Verify that the screen shows the chemisorption furnace icon and the chemisorption inlet valves.

Acceptance Criteria: The chemisorption furnace and port fit correctly onto the instrument. The software shows the presence of the furnace and inlet valves.

Outputs: Complete the Data Sheet and the checklist showing completion of this step.

Background: This step verified that the chemisorption option installs correctly.




5.31 Sample Temperature Thermocouple Calibration and Verification

Purpose: To calibrate the sample thermocouple to a known reference and to verify that the furnace can achieve 1100 °C.

Inputs:

Chemisorption furnace assembly on elevator and connected Sample tube installed Temperature Calibration Standard

Action:

1. Install the probe for the temperature calibration standard so that the tip is as close as possible to the tip of the sample thermocouple. The metal sheaths should touch within 1/8 inch of the tips to ensure that the two thermocouples are sensing the same temperature.

2. Allow the reading on the reference meter to stabilize. 3. From the Unit menu in the tool bar, choose “Calibration”, then “Sample Temperature

Offset”. Enter the value from the reference standard into the dialog field. Record this value on the data sheet in Appendix A.

4. Raise the elevator. Ensure that the thermocouples remain in contact. Evacuate the sample tube using valves 1 and 9. (This is to avoid pressure rise while heating the sample tube). When the elevator stops, place the furnace insulator halves around the sample tube neck. Set the furnace temperature to 750 °C, and a ramp rate of 50 °C per minute. Wait for the temperature to stabilize.

5. From the Unit menu in the tool bar, choose “Calibration”, then “Sample Temperature Scale”. Enter the value from the reference standard into the dialog field. Record this value on the data sheet.

6. Set the furnace temperature to 1100°C at a ramp rate of 50°C per minute. Wait for the temperature to stabilize. Record the temperature of the furnace thermocouple, sample thermocouple, and reference temperature gauge on the check sheet in Appendix A.

7. Calculate, record and verify that the difference between the sample thermocouple and the reference temperature gauge is within the allowable limits stated in Appendix A.

8. Verify and record on the check sheet in Appendix A that the furnace thermocouple is hotter than the sample thermocouple.

9. Repeat steps 7, 8, and 9 for the target temperatures of 800°C, 600°C, and 100°C. 10. Cool the furnace below 50°C and remove the reference temperature gauge thermocouple

from the furnace. Acceptance Criteria: The temperature values recorded must be within the tolerances listed in the appendix. Output: The Data Sheet and Checklist are filled out, indicating that this step is complete.




Background:

The sample temperature thermocouple is at a different location from the furnace thermocouple. The sample thermocouple requires calibration with the instrument electronics, while the furnace controller calibration is built into the purchased furnace controller. The highest required temperature for the furnace is 1100°C so this value is also verified.

5.32 Chemi Gas Inlet Manifold Leak Test

Purpose: To verify the vacuum integrity of the chemi gas inlet manifold. Inputs: Computer to actuate the various parts of the instrument. Action:

1. Close supply valves (i.e. Nupro valves) on lines attached to the chemi gas inlet manifold. Install leak tight plugs in unused ports.

2. Open valves 1, 2, 7, CV, CS, 4, 5, PV and PS. Evacuate the inlet ports by opening valves C1 to C6.

3. Evacuate at least 20 minutes. Overnight is preferred. 4. Close valves PV, PS, 1, 2 and CV, 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 reading 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 (C1 to C6). 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 C1 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. 11. Repeat steps 8 to 10 for the inlet valves C2 to C6.

Acceptance Criteria: Chemi inlet manifold outgas rate is within acceptable limits shown on the datasheet. Chemi gas inlet valves have outgas or leak rates within acceptable limits. Outputs:


Background: Low outgas rates confirm that no gas inlet valves or interconnecting tubing are leaking.




5.33 Chemisorption Blank Run Purpose: Verify blank runs give acceptably small uptake of gas. Inputs:

Empty sample tube with filler rod Furnace with top insulators

Action:

1. Create a sample information file. (See Appendix C).

CAUTION Do not touch the sample tube or filler rod with bare skin. Oils from your skin will be left upon the quartz tubes and will cause etching of the quartz when subjected to high temperatures. Always use gloves to handle the quartz tubes. The quartz tubes must be wiped with alcohol to remove oils.

2. Load the sample tube with filler rod onto the sample port. The sample thermocouple must be located in the small loop of quartz near the bottom.

3. Raise the elevator with the oven installed, ensuring that the sample tube enters the oven at the center. Install the top insulators around the furnace opening.

4. Start the blank analysis run. 5. Allow the run to complete before reviewing and printing data. 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 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 CBsn.SMP, where sn is the serial number of the instrument.

Background:

The blank tube test helps to identify leaks and furnace performance. If any positive gas uptake was measured, then the two isotherms (first and repeat runs) should be parallel after the first few points. The lines should be fairly straight, which indicates good temperature control, and lack of leaks. If there was no positive gas uptake, then the isotherms will not be useful. In such cases the values shown on the report must be used to verify that the uptake is within acceptable limits.




5.34 Chemisorption Sample Run

Purpose: Verify sample runs give acceptable results. Inputs:

Empty sample tube with filler rod Furnace with top insulators Reference material, as shipped with the instrument.

Action: 1. Create a sample information file. (See Appendix C).

CAUTION

Do not touch the sample tube or filler rod with bare skin. Oils from your skin will be left upon the quartz tubes and will cause etching of the quartz when subjected to high temperatures. Always use gloves to handle the quartz tubes. The quartz tubes must be wiped with alcohol to remove oils.

2. Weigh the empty tube with filler rod, then load the sample tube with 21 pellets of the reference material. This is about 1 gram. Do not use broken pellets. Place the filler rod into the sample tube.

3. Load the tube onto the sample port. The sample thermocouple must be located in the small loop of quartz near the bottom.

4. Raise the elevator with the oven installed, ensuring that the sample tube enters the oven at the center. Install the top insulators around the furnace opening.

5. Start the sample analysis run. 6. Allow the run to complete then weigh the sample. Enter the weight into the sample file and

generate a report. 7. 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 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 CRsn.SMP, where sn is the serial number of the instrument.

Background:

The sample run helps to verify correct valve operation and the ability of the system to measure the amount of gas which chemically adsorbs to the surface of the reference material. Furnace stability is confirmed by the relative straightness of the “difference” isotherm, verified by the calculation of Standard Deviation for the points in the last part of the isotherm.




5.40 Save Instrument Calibration

Purpose: Save calibration data and copy calibration files to network. Inputs: Networked computer terminal Action:

1. Select Unit x from pull down menu (where x is the unit number being worked on). 2. Select Instrument 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 on OK. 5. Click on Accept. 6. Exit the 2020 application program. 7. Select “Product Info. Transfer” icon from the desktop. Select the appropriate 2020 model

(the choices are "2020 Nitrogen", "2020 Krypton", and "2020 Chemisorption"). 8. Enter or select the instrument’s serial number, press <ENTER>. 9. If the 2020 application referred to in step 6 was the Chemisorption application then launch

the 2020 Physisorption application and perform steps 1 through 8. Acceptance Criteria: Calibration data must be saved and transferred to the network. Outputs: Calibration files saved on network. Background:

In order to create a Calibration CD for this instrument the calibration files must be saved to the network. The Degas calibration (if a degas system is installed) is stored on the degas circuit board. If this is a physisorption system, then all of the relevant calibration files (such as transducer scaling, system volume etc.) are stored using this procedure. If the instrument also has the chemisorption option installed, then the chemisorption calibration files (such as thermocouple scaling) are also stored. This can be done in either the physisorption program or the chemisorption program, so there is no need to switch applications.




5.41 Create Calibration / Program CD

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

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

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

Acceptance Criteria: CD received from Final Assembly supervisor. Outputs: Record acceptance in the appropriate places on the checklist in Appendix A. Background: The Calibration / Program CD is needed to be shipped with the instrument. It contains the

current operating program and the calibration files. 5.42 Documentation

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

Input: Completed data sheet(s), completed checklist, and all reports. Action:

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

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




Background: No further information.

5.43 Deliverables

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

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

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


The operator has completed this step. Outputs:

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

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




APPENDIX A

ASAP 2020 DATA SHEET (Page 1 of 10)

Date Core Part Number Serial Number

Operator(s)

Part Number Description Serial # Cal. Due Date 003-09601-00 Meter, Type K Thermocouple

202-09801-00 Temperature Standard, 100 ohm RTD simulator

004-09814-00 Pressure Calibration Standard

202-29800-00 1st Ref. Volume Chamber

202-29800-00 or 004-29801-00

2nd Ref. Volume Chamber

003-09608-00 Digital Voltmeter

003-09623-10 or 003-09619-00 & 900-62610-00

Vacuum Gauge Calibration Standard (identify which standard was used)

PCP Step OK ? 5.1 Manual Operation Checkout

Did the Application program boot up successfully? Did all the analysis valves operate properly? Did all the degas valves operate properly? Did the analysis transducer readings show pressurization and vacuum? Did the degas transducer readings show pressurization and vacuum? Did the elevator raise and lower and stop correctly?

Did the degas mantle thermocouples cause correct display responses? Record Revision level of elevator 300-34005-00 Rev 5.2 Check Voltages. (TP 3 / black is reference ground for DC readings) Voltage to test Measured value Acceptable range +5 Volt, TP4 / red +5.10 to 5.25 VDC +15 Volt, TP5 / blue +14 to +16 VDC -15 Volt, TP 6 / yellow -14 to -16 VDC + 24 Volt, TP7 / white +23 to +25 VDC + 24 Volt valve, TP1 / white +23 to +25 VDC Degas AC, J16 pin 4 to 6 26 to 32 VAC




APPENDIX A

ASAP 2020 DATA SHEET (Page 2 of 10) Serial Number

5.3 Analysis Vacuum Gauge Calibration and Verification

Measured value Acceptable range OK? Voltage at Atmospheric Pressure before

final adjustment mV 90 to 200mV

Voltage used for Calibration at lowest vacuum V 2.699 to 4.000 V

Vacuum used for software calibration microns 1 to 30 microns Target

Pressure Computer Display Reference

Gauge (P or V)

Difference (microns)

Limits (microns)

OK?

~500 microns P= ± 200 <10 microns V= ± 5 5.4 Calibrating the Temperature Sensor Fill out the appropriate section for the method used (Resistors or gauge). Write N/A in the unused section. Resistance Temperature Standard

Simulator Value Simulator serial # Displayed Temp Acceptable Value 28 °C n/a n/a 23 °C 22.8 to 23.2 °C 33 °C 32.8 to 33.2 °C 50 °C 49.6 to 50.4 °C Temperature Gauge Temperature used for software calibration °C 5.5 Calibrating and Verifying the Pressure Transducer(s)

Limits OK?

1 torr transducer offset (if present) (gnd TP24 gray, + TP20 blue) mV +/-30mV 10 torr transducer offset (if present) (gnd TP25 gray, + TP21 blue) mV +/-30mV 1000 torr transducer offset (gnd TP26 gray, + TP15 blue) mV +/-30mV 1 torr range (if present) Calibration point (reference gauge reading) torr 10 torr range (if present) Calibration point (reference gauge reading). torr Valve 4 shows pressure increase when opened? Valve 5 shows even faster pressure increase when opened? 1000 torr range calibration point (reference gauge reading) torr




APPENDIX A


Verifying the 1000 torr Pressure Transducer

Target Pressure (torr)

Computer Display

Reference Gauge

Difference

~850 (804 – 893) ~760 (722 – 798) ~650 (617 – 683) ~550 (522 – 578) ~450 (427 – 473) ~350 (332 – 368) ~250 (237 – 263) ~150 (142 – 158) All values in “Difference” column less than 1.5 torr? Verifying the 10 torr Pressure Transducer Pressure (torr) 1000 torr

screen value * 10 torr screen value

Reference Gauge Difference

~8 (7.6 - 8.4) ~5 (4.7 - 5.3) ~3 (2.8 - 3.2) Calculate difference between “10 torr screen” and “Reference Gauge” values. All

values in “Difference” column must be less than +/-0.03 torr

* 1000 torr screen value is for historical interest only, and is not used to judge the calibration. Verifying the 1 torr Pressure Transducer Pressure (torr) 10 torr screen

value ** 1 torr screen value

Reference Gauge Difference

~0.8 (.76 - .84) ~0.5 (.47 - .53) ~0.3 (.28 - .32) Calculate difference between “1 torr screen” and “Reference Gauge” values. All

values in “Difference” column less than +/-0.005 torr?

** 10 torr screen value is for historical interest only, and is not used to judge the calibration.




APPENDIX A


5.6 Analysis Manifold Leak Test

Measured Outgas Rate (microns/minute) ***

Maximum rate (Microns/minute)

Lower Manifold 0.5 microns/min Upper & Lower 0.7 microns/min *** If data is from test cart report, attach the report with this data sheet, and check here 5.7 Measure Physi Gas Inlet Manifold Leak Test Test Initial Reading 3 Minute

Reading Difference Limits OK?

Inlet Ports 30microns (.03 torr)

Valve P1 2.1 microns (0.0021 torr)






5.8 System Volume Calibration

Reference Volume = cc S/N = Run Upper & Lower

Manifolds Volume Lower Manifold Volume

Average Volume Standard Deviation (SD) Max allowable SD 0.05 0.02




APPENDIX A


5.9 Blank Tube Test (Nitrogen). Fill in values, or attach graph showing compliance.

P/Po Range Volume Adsorbed (cc) Max Allowable 0.0 - 0.1 (Ads) +/- 0.075 0.1 - 0.2 (Ads) +/- 0.100 0.2 - 0.3 (Ads) +/- 0.125 0.3 - 0.4 (Ads) +/- 0.150 0.4 - 0.5 (Ads) +/- 0.175 0.5 - 0.6 (Ads) +/- 0.200 0.6 - 0.7 (Ads) +/- 0.225 0.7 - 0.8 (Ads) +/- 0.250 0.8 - 0.9 (Ads) +/- 0.275 0.9 - 0.98 (Ads) +/- 0.295 0.98 Ads to 0.98 Des No limit 0.98 Des to 0.0 Des +/- 0.150 All OK? No steps larger than 0.05 cm3/cc from point to point Sample file named PNBsn.SMP, where sn is the instrument serial number.

5.10 Reference Chamber Analysis Reference Volume cc Measured Volume Difference Max Difference = +/- 0.5% Sample file named PRCsn.SMP, where sn is the instrument serial number. 5.11 Nitrogen Standards Test (N2) Lot Number Expected Surface Area Measured Area +/- Sample file named PNRsn.SMP, where sn is the instrument serial number.




APPENDIX A ASAP 2020 DATA SHEET (Page 6 of 10)

Serial Number 5.12 Krypton Blank Tube Test (Units with 10 torr transducer)

Fill in values, or attach graph showing compliance

P/PO Approx

Volume Adsorbed (cc)

Max Allowable Buna-N Version

Max Allowable Kalrez Version

.06 -0.0005 to +.0022 -0.0015 to +.0066

.12 -0.0006 to +.0027 -0.0018 to +.0081

.18 -0.0007 to +.0031 -0.0021 to +.0093

.24 -0.0010 to +.0035 -0.0030 to +.0105

.30 -0.0012 to +.0039 -0.0036 to +.0117

All in limits

Sample file named PKBsn.SMP, where sn is the instrument serial number. 5.13 Krypton Standards Test (Units with 10 torr transducer) Lot Number Expected Surface Area Measured Area +/- Sample file named PKRsn.SMP, where sn is the instrument serial number. 5.14 Vapor Option Test (Units with the vapor option)

Measured value (°C)

Acceptable range (°C)

OK?

Manifold temperature (from temperature controller)

55 to 59

Vapor temperature 38 to 42 Manifold temperature (from instrument) 45 to 47 Manifold temperature varies by less than 0.5 °C over 1 minute?

5.20 Degas Vacuum Gauge Calibration

Measured value Acceptable range OK? Voltage at Atmospheric Pressure before final adjustment

mV 90 to 200mV

Voltage used for Calibration at lowest vacuum

V 2.699 to 4.000 V

Vacuum used for software calibration microns 1 to 30 microns




APPENDIX A


5.21 Degas Pressure Gauge and Servo Valve Calibration and Verification

Pressure at which calibration was done = torr Servo

Target Computer

Display Servo Error

Reference Gauge

Calibration Error

A B A-B C B-C 760 torr 550 torr 350 torr 150 torr Max +/- 5 torr Max +/- 5 torr OK? All values in “Error” columns less than limits shown?

5.22 Degas Vacuum Gauge Final Calibration and Verification Target

Pressure Computer Display

(microns) Reference Gauge

(P or V)* Difference (microns)

Limits (microns

)

OK?

1 torr P= ± 200 <20 microns V= ± 5

*Convert Paroscientific gauge readings from torr to microns by multiplying by 1000 5.23 Heating Mantle Test

Left Mantle Test Screen Value Acceptance OK ? Reference Meter Acceptance OK? Amb N/A N/A +/- 10 °C Open N/A N/A N/A >495 °C 95°C 90 - 100 85 - 105 195°C 190 - 200 175 - 215

Right Mantle Test Screen Value Acceptance OK ? Reference Meter Acceptance OK? Amb N/A N/A +/- 10 °C Open N/A N/A N/A >495 °C 105°C 100 - 110 95 - 115 205°C 200 - 210 185 - 225




APPENDIX A


5.24 Verify Degas Manifold Outgas Rate Measure and Record Combined and Lower Outgas Rates

Manifold Computer Display Reading 1 Reading 2

(Reading 2 minus Reading 1) Result divided by 5

___________ ___________ =___________ ___________ /5 =___________

Maximum Rate = 10 microns/ min. (.01 torr/min.) after overnight evac. 5.30 Chemisorption Initial Installation

Chemi port fits front panel correctly Software shows chemi furnace and valves

5.31 Sample Temperature Thermocouple Calibration and Verification

Temperature at which “Offset” value was recorded °C Temperature at which “Scale” value was recorded °C

Target Temp.

Computer Display Furnace

TC*

Computer Display Sample

TC*

Reference Temp. meter

Acceptance Value Sample

TC* - Ref. Temp. Meter

Difference OK?

Furnace TC* is hotter than Sample TC*?

1100°C ±10°C 800°C ± 5°C 600°C ± 5°C 100°C ± 5°C




APPENDIX A


5.32 Chemi Gas Inlet Manifold Leak Test Test Initial Reading 3 Minute

Reading Difference Limits OK?

Inlet Ports 30microns (.03 torr)

Valve C1 2.1 microns (0.0021 torr)






5.33 Chemisorption Blank Run

1 Measured Free Space cc 2 Multiply Measured Free Space (line 1) by

0.005(this is 1/2% of free space)

cc

3 Maximum reported quantity adsorbed (1st run)(Largest number, ignoring minus signs)

cc

Value in line 3 must be smaller than value in line 2. Submit printed report with this sheet.

Sample file named CBsn.SMP, where sn is the instrument serial number.

5.34 Chemisorption Sample Run Sample Run (Difference Results) Reported Values Slope between -0.00008 and +0.00008 Calculated Standard Deviation ≤ 0.011 %Metal Dispersion: Expected Value = _________+/- _________ Sample file named CRsn.SMP, where sn is the instrument serial

number.




APPENDIX A


5.40 Save Instrument Calibration Calibration data saved to network?

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

5.42 Documentation To be compiled in this order:

Appendix A, data sheet Appendix B, checklist Manifold Outgas and Leak Check report or section 5.6 completed Nitrogen Blank Run report Reference chamber report Nitrogen sample run report Krypton blank run report (if applicable) Krypton sample run report (if applicable) Chemisorption blank run report (if applicable) Chemisorption sample run report (if applicable) All items present Have you recorded the elevator revision level in the serial number log?

5.43 Deliverables (Loose items that are tested and then delivered to stock with the instrument)

All units Qty Po Tube 200/25840/00 1 Analysis Dewar 202/25850/00 1 Cold Trap Dewar 202/25849/00 1 CD, Physi, with cal data 202/20801/99 1 Units with the Vapor Option Temperature Controller 202/34150/03 1 Vapor Enclosure 202/34150/00 1 Units with Degas system Heating mantles 003/26043/00 2 Units with Chemisorption Chemi Port assembly 202/34021/00 1 Furnace 202/34011/00 1 Cable, furnace TC 202/63801/00 1 Cooling hose for furnace 202/32802/00 1 CD, Chemi, with cal data 202/20808/99 1

All items present




APPENDIX B

ASAP 2020 CHECKLIST

Date Core Part Number Serial Number

Operator(s) PCP step Step Description Date Complete

5.1 Manual Operation Checkout 5.2 Check Voltages 5.3 Analysis Vacuum Gauge Calibration and Verification 5.4 Calibrating the Temperature Sensor 5.5 Calibrating and Verifying the Pressure Transducer(s) 5.6 Analysis Manifold Leak Test 5.7 Physi Gas Inlet Manifold Outgas Rate 5.8 System Volume Calibration 5.9 Blank Tube Test (N2) 5.10 Reference Chamber Analysis 5.11 Nitrogen Standards Test (N2) 5.12 Krypton Blank Tube Test (10 torr and 1 torr units only) 5.13 Krypton Standards Test (10 torr and 1 torr units only) 5.14 Vapor Option Test (Units with the vapor option) 5.20 Degas Vacuum Gauge Calibration 5.21 Degas Pressure Gauge and Servo Valve Calibration and Verification 5.22 Degas Vacuum Gauge Final Calibration and Verification 5.23 Heating Mantle Test 5.24 Verify Degas Manifold Outgas Rate 5.30 Chemisorption Initial Installation 5.31 Sample Temperature Thermocouple Calibration and Verification 5.32 Chemi Gas Inlet Manifold Outgas Rate 5.33 Chemisorption Blank run 5.34 Chemisorption Sample run 5.40 Save Instrument Calibration 5.41 Create Calibration / Program CD 5.42 Documentation 5.43 Deliverables




APPENDIX C

ANALYSIS CONDITIONS Nitrogen Blank Analysis Conditions Description: Run Conditions Collect ROA Data: No Pressure Table Relative BET Surf. Lang. Surf. Freund. Temkin t-Plot Alpha-S Pressure (p/p°) Area Area

1 0.000260000 2 0.000650000 3 0.001050000 4 0.002600000 5 0.006500000 6 0.010500000 7 0.050000000 8 0.100000000 9 0.150000000 10 0.200000000 11 0.250000000 12 0.300000000 13 0.350000000 14 0.400000000 15 0.450000000 16 0.500000000 17 0.550000000 18 0.600000000 19 0.650000000 20 0.700000000 21 0.750000000 22 0.800000000 23 0.850000000 24 0.900000000 25 0.950000000 26 0.995000000 27 0.950000000 28 0.900000000 29 0.850000000 30 0.800000000 31 0.750000000 32 0.700000000 33 0.650000000 34 0.600000000 35 0.550000000 36 0.500000000 37 0.450000000 38 0.400000000 39 0.350000000 40 0.300000000 41 0.250000000 42 0.200000000 43 0.150000000 44 0.100000000




Preparation Fast evacuation: Yes Vacuum setpoint: 1.3 Pa (10 microns) Evacuation time: 0.20 h Leak test: No Use TransSeal: No Free Space Free-space type: Measured Lower dewar for evacuation: No Evacuation time: 0.30 h Outgas test: No p° and Temperature p° and T type: Measure p° at intervals during analysis. Enter the Analysis Bath Temperature below. Measurement interval: 120 min Temperature: 77.300 K Dosing Use first pressure fixed dose: No Use maximum volume increment: No Absolute pressure tolerance: 0.6666 kPa (5 torr) Relative pressure tolerance: 5.0% Low pressure dosing: No Equilibration Equilibration interval: 100 s Minimum equilibration delay at p/p° >= 600 s 0.995: Sample Backfill Backfill at start of analysis: Yes Backfill at end of analysis: Yes Backfill gas: N2




Report Options Description: Report Options Show report title: Yes Report title: Show bitmap: Yes Bitmap file: Micro.bmp Bitmap width: 2.000 in. Bitmap height: 0.250 in. Smooth pressures below 0.10 p/p°: No Apply thermal transpiration correction: No Isotherm: Yes Tabular Report Selected: Yes Plot Adsorption Branch: Yes Plot Desorption Branch: Yes Linear Plot Selected: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Logarithmic Plot Selected: No BET Surface Area: No Langmuir Surface Area: No Freundlich: No Temkin: No t-Plot: No Alpha-S Method: No f-Ratio Method: No BJH Adsorption: No BJH Desorption: No Horvath-Kawazoe: No Dubinin: No MP-Method: No Options: Yes Summary: No Sample Log: Yes Manufacturing: Yes




Volume Chamber Run Analysis Conditions

Description: Run Conditions Collect ROA Data: No Pressure Table Relative BET Surf. Lang. Surf. Freund. Temkin t-Plot Alpha-S Pressure (p/p°) Area Area

1 0.100000000 2 0.200000000 3 0.500000000 4 0.700000000 5 0.800000000 6 0.900000000 7 0.980000000 8 0.900000000 9 0.700000000 10 0.500000000

Preparation Fast evacuation: Yes Vacuum setpoint: 1.33 Pa (10 microns) Evacuation time: 0.10 h Leak test: No Use TransSeal: No Free Space Free-space type: Measured Lower dewar for evacuation: No Evacuation time: 0.10 h Outgas test: No p° and Temperature p° and T type: Enter p° below.(Use 760 torr) Enter the Analysis Bath Temperature below. Temperature: 273.150 K (0°C) Dosing Use first pressure fixed dose: No Use maximum volume increment: No Absolute pressure tolerance: 0.6666 kPa (5 torr) Relative pressure tolerance: 5.0% Low pressure dosing: No Equilibration Equilibration interval: 10 s Minimum equilibration delay at p/p° >= 600 s 0.995: Sample Backfill Backfill at start of analysis: No Backfill at end of analysis: Yes Backfill gas: N2 ------------------------------------------------------------------------------------




Report Options Description: Report Options Show report title: Yes Report title: Volume Chamber Run Show bitmap: Yes Smooth pressures below 0.10 p/p°: No Apply thermal transpiration correction: No Isotherm: Yes Tabular Report Selected: Yes Plot Adsorption Branch: Yes Plot Desorption Branch: Yes Linear Plot Selected: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Logarithmic Plot Selected: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes BET Surface Area: No Langmuir Surface Area: No Freundlich: No Temkin: No t-Plot: No Alpha-S Method: No f-Ratio Method: No BJH Adsorption: No BJH Desorption: No Horvath-Kawazoe: No Dubinin: No MP-Method: No Options: Yes Summary: No Sample Log: Yes Manufacturing: Yes




Nitrogen Sample Analysis Conditions Description: Nitrogen Standard Collect ROA Data: No Pressure Table Relative BET Surf. Pressure (p/p°) Area 1 0.060000000 x 2 0.080000000 x 3 0.120000000 x 4 0.160000000 x 5 0.200000000 x Preparation Fast evacuation: Yes Vacuum setpoint: 1.33 Pa (10 microns) Evacuation time: 0.50 h Leak test: Yes Leak test duration: 120 s Use TransSeal: No Free Space Free-space type: Measured Lower dewar for evacuation: No Evacuation time: 0.50 h Outgas test: No p° and Temperature p° and T type: Measure p° at intervals during analysis. Calculate the Analysis Bath Temperature from these values. Measurement interval: 120 min Dosing Use first pressure fixed dose: No Use maximum volume increment: No Absolute pressure tolerance: 0.6666 kPa (5 torr) Relative pressure tolerance: 5.0% Low pressure dosing: No Equilibration Equilibration interval: 10 s Minimum equilibration delay at p/p° >= 600 s 0.995: Sample Backfill Backfill at start of analysis: Yes Backfill at end of analysis: Yes Backfill gas: N2 ------------------------------------------------------------------------------------




Report Options Description: Report Options Show report title: Yes Report title: Show bitmap: Yes Bitmap file: Micro.bmp Bitmap width: 2.000 in. Bitmap height: 0.250 in. Smooth pressures below 0.10 p/p°: No Apply thermal transpiration correction: No Isotherm: Yes Tabular Report Selected: Yes Plot Adsorption Branch: Yes Plot Desorption Branch: Yes Linear Plot Selected: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Logarithmic Plot Selected: No BET Surface Area: Yes Tabular Report Selected: Yes Transform Plot Selected: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Isotherm Plot Selected: Yes Overlay Samples: Yes Autoscale X Axis: Yes Autoscale Y Axis: Yes Langmuir Surface Area: No Freundlich: No Temkin: No t-Plot: NO Alpha-S Method: No f-Ratio Method: No BJH Adsorption: No Horvath-Kawazoe: No Dubinin: No MP-Method: No




Summary: Yes Surface Area Single-point BET: Yes Multi-point BET: Yes Langmuir: No t-Plot Micropore: No t-Plot External: No BJH Cumulative Adsorption: No BJH Cumulative Desorption: No Pore Volume Adsorption Total: No Desorption Total: No t-Plot Micropore: No BJH Cum. Adsorption: No BJH Cum. Desorption: No Pore Size Average pore diameter: No BJH adsorption avg.: No BJH desorption avg.: No Freundlich No Temkin No Alpha-S method No Horvath-Kawazoe Maximum pore volume: No Median pore width: No Dubinin-Radushkevich Micropore surface area: No Monolayer capacity: No Dubinin-Astakhov Micropore surface area: No Limiting micropore volume: No MP-Method Cumulative surface area: No Cumulative pore volume: No Average pore hydraulic radius: No Sample Log: Yes Manufacturing: No




Krypton Blank Analysis Conditions Description: KRYPTON MULTIPT SA Collect ROA Data: No Pressure Table Relative BET Surf. Lang. Surf. Freund. Temkin t-Plot Alpha-S Pressure (p/p°) Area Area 1 0.060000000 x 2 0.070000000 x 3 0.085000000 x 4 0.100000000 x 5 0.120000000 x 6 0.140000000 x 7 0.180000000 x 8 0.240000000 x 9 0.300000000 x Preparation Fast evacuation: Yes Vacuum setpoint: 1.3 Pa (10 microns) Evacuation time: 0.50 h Leak test: Yes Leak test duration: 120 s Use TransSeal: No Free Space Free-space type: Measured Lower dewar for evacuation: Yes Evacuation time: 0.50 h Outgas test: Yes Outgas test duration: 120 s p° and Temperature p° and T type: Measure Psat of a gas. Calculate p° of the adsorptive from the measured Psat. Calculate the Analysis Bath Temperature using the Adsorptive Properties temperature data. Measurement gas: Nitrogen @ 77.35 K (N2) Max Man Press: 123.3232 kPa (925 torr)

Dosing Use first pressure fixed dose: No Use maximum volume increment: No Absolute pressure tolerance: 0.0007 kPa (.005 torr) Relative pressure tolerance: 5.0% Low pressure dosing: No Equilibration Equilibration interval: 10 s Minimum equilibration delay at p/p° >= 0 s 0.995: Sample Backfill Backfill at start of analysis: Yes Backfill at end of analysis: Yes Backfill gas: N2 ------------------------------------------------------------------------------------




Report Options Description: MULTIPOINT N2 & KR Show report title: Yes Report title: MICROMERITICS INSTRUMENT CORPORATION Show bitmap: No Smooth pressures below 0.10 p/p°: No Apply thermal transpiration correction: No Isotherm: Yes Tabular Report Selected: Yes Plot Adsorption Branch: Yes Plot Desorption Branch: Yes Linear Plot Selected: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Logarithmic Plot Selected: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes BET Surface Area: No Langmuir Surface Area: No Freundlich: No Temkin: No t-Plot: No Alpha-S Method: No f-Ratio Method: No BJH Adsorption: No BJH Desorption: No Horvath-Kawazoe: No Dubinin: No MP-Method: No Options: Yes Summary: No Sample Log: Yes Manufacturing: Yes




Krypton Sample Analysis Conditions Description: KRYPTON MULTIPT SA Collect ROA Data: No

Pressure Table Relative BET Surf. Lang. Surf. Freund. Temkin t-Plot Alpha-S Pressure (p/p°) Area Area 1 0.060000000 x x 2 0.070000000 x 3 0.085000000 x 4 0.100000000 x x 5 0.120000000 x 6 0.140000000 x 7 0.160000000 x x 8 0.180000000 x 9 0.200000000 x x Preparation Fast evacuation: Yes Vacuum setpoint: 1.3 Pa (10 microns) Evacuation time: 0.10 h Leak test: Yes Leak test duration: 120 s Use TransSeal: No Free Space Free-space type: Measured Lower dewar for evacuation: Yes Evacuation time: 0.10 h Outgas test: Yes Outgas test duration: 180 s p° and Temperature p° and T type: Measure Psat of a gas. Calculate p° of the adsorptive from the measured Psat. Calculate the Analysis Bath Temperature using the Adsorptive Properties temperature data. Measurement gas: Nitrogen @ 77.35 K (N2) Max Man Press: 123.3232 kPa (925 torr) Dosing Use first pressure fixed dose: No Use maximum volume increment: No Absolute pressure tolerance: 0.0007 kPa (0.005 torr) Relative pressure tolerance: 5.0% Low pressure dosing: No Equilibration Equilibration interval: 10 s Minimum equilibration delay at p/p° >= 0 s 0.995: Sample Backfill Backfill at start of analysis: Yes Backfill at end of analysis: Yes Backfill gas: N2




Report Options Description: MULTIPOINT N2 & KR Show report title: Yes Report title: MICROMERITICS INSTRUMENT CORPORATION Show bitmap: No Smooth pressures below 0.10 p/p°: No Apply thermal transpiration correction: No Isotherm: Yes Tabular Report Selected: Yes Plot Adsorption Branch: Yes Plot Desorption Branch: Yes Linear Plot Selected: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Logarithmic Plot Selected: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes BET Surface Area: No Langmuir Surface Area: No Freundlich: No Temkin: No t-Plot: No Alpha-S Method: No f-Ratio Method: No BJH Adsorption: No BJH Desorption: No Horvath-Kawazoe: No Dubinin: No MP-Method: No Options: Yes Summary: Yes




Surface Area Single-point BET: Yes Multi-point BET: Yes Langmuir: No t-Plot Micropore: No t-Plot External: No BJH Cumulative Adsorption: No BJH Cumulative Desorption: No Pore Volume Adsorption Total: Yes Relative Pressure: 0.010000000 Desorption Total: Yes Relative Pressure: 0.900000000 t-Plot Micropore: No BJH Cum. Adsorption: No BJH Cum. Desorption: No Pore Size Average pore diameter: Yes BJH adsorption avg.: No BJH desorption avg.: No Freundlich No Temkin No Alpha-S method No Horvath-Kawazoe Maximum pore volume: No Median pore width: No Dubinin-Radushkevich Micropore surface area: No Monolayer capacity: No Dubinin-Astakhov Micropore surface area: No Limiting micropore volume: No MP-Method Cumulative surface area: No Cumulative pore volume: No Average pore hydraulic radius: No Sample Log: Yes Manufacturing: No




Chemi Blank Analysis Conditions Description: CO blank Cool sample at termination: Yes Backfill sample at termination: Yes Backfill gas: Nitrogen Task Summary Task Task Temp Rate Time Pressure Number Name Gas (°C) (°C/min) (min) (kPa) 1 Evacuation 350 20.0 10 2 Evacuation 35 20.0 10 3 Leak Test 35 10.0 4 Analysis CO 35 10.0 Analysis Task 1 - Evacuation Backfill gas: Fast evacuation: Yes Unrestricted evac. pressure: 3.999672 kPa (30 torr) Vacuum setpoint: 1.3 Pa (10 microns) Evacuation time: 10 min Temperature: 350 °C Heat rate: 20.00 °C/min Analysis Task 2 - Evacuation Backfill gas: Fast evacuation: Yes Unrestricted evac. pressure: 3.999672 kPa (30 torr) Vacuum setpoint: 1.3 Pa (10 microns) Evacuation time: 10 min Temperature: 35 °C Heat rate: 20.00 °C/min Analysis Task 3 - Leak Test Temperature: 35 °C Heat rate: 10.00 °C/min Outgas rate: 1.3 Pa/min (10 microns/min) Analysis Task 4 - Analysis Adsorptive: Carbon Monoxide Temperature: 35 °C Heat rate: 10.00 °C/min Equilibration interval: 10 s Relative target tolerance: 5.0% Absolute target tolerance: 0.666 kPa (5.0 torr) Repeat analysis: Yes Fast evacuation: Yes Unrestricted evac. pressure: 4.00 kPa (30 torr) Vacuum Setpoint: 1.3 Pa (10 microns) Evacuation time: 60 min Free space group: Measured Estimated free space: 6.9500 cm³ Incremental dosing: No




Pressure Table Absolute Include in Lang. Surf. Freund. Temkin Pressure (torr) Line Fit Area 1 60 2 70 3 90 4 110 5 130 6 150 7 170 8 190 9 210 10 230 11 250 12 275 Report Options Report Options ID: Chemi Report Report Title: Smooth Pressure Data: No Isotherm: Yes Tabular Report Selected: Yes Plot Report Selected: Yes X Axis Scale: Linear Plot Analysis: Yes Plot Repeat Analysis: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Analysis: Yes Summary Report Selected: Yes Tabular Report Selected: Yes Plot Report Selected: Yes Report Differences: Yes Report Analysis: Yes Plot Analysis: Yes Plot Repeat Analysis: Yes Plot Difference: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Langmuir Surface Area: No Freundlich: No Temkin: No Options: Yes Sample Log: Yes




Chemi Sample Analysis Conditions Description: CO Analysis of Platinum Cool sample at termination: Yes Backfill sample at termination: Yes Backfill gas: Nitrogen Task Summary Task Task Temp Rate Time Pressure Number Name Gas (°C) (°C/min) (min) (kPa) 1 Evacuation HE 110 10.0 30 2 Flow H2 100 10.0 10 3 Flow H2 350 10.0 120 4 Evacuation 350 10.0 120 5 Evacuation 35 10.0 10 6 Leak Test 35 10.0 7 Evacuation 35 10.0 8 Analysis CO 35 10.0 Analysis Task 1 - Evacuation Backfill gas: Helium Fast evacuation: Yes Unrestricted evac. pressure: N/A Vacuum setpoint: 1.3 Pa (10 microns) Evacuation time: 30 min Temperature: 110 °C Heat rate: 0.50 °C/min Analysis Task 2 - Flow Gas: Hydrogen Temperature: 100 °C Heat rate: 10.00 °C/min Time: 10 min Analysis Task 3 - Flow Gas: Hydrogen Temperature: 350 °C Heat rate: 10.00 °C/min Time: 120 min Analysis Task 4 - Evacuation Backfill gas: Fast evacuation: Yes Unrestricted evac. pressure: N/A Vacuum setpoint: 0.6 Pa (5 microns) Evacuation time: 120 min Temperature: 350 °C Heat rate: 10.00 °C/min Analysis Task 5 - Evacuation Backfill gas: Fast evacuation: Yes Unrestricted evac. pressure: N/A Vacuum setpoint: 0.6 Pa (5 microns) Evacuation time: 10 min Temperature: 35 °C Heat rate: 10.00 °C/min Analysis Task 6 - Leak Test Temperature: 35 °C Heat rate: 10.00 °C/min Outgas rate: 1.3 Pa/min (10 microns/min) Analysis Task 7 - Evacuation Backfill gas: Fast evacuation: Yes Unrestricted evac. pressure: 3.999672 kPa (30 torr) (N/A) Vacuum setpoint: 1.3 Pa (10 microns) Evacuation time: 20 min Temperature: 35 °C Heat rate: 10.00 °C/min Analysis Task 8 - Analysis Adsorptive: Carbon Monoxide Temperature: 35 °C Heat rate: 10.00 °C/min Equilibration interval: 20 s Relative target tolerance: 5.0%




Absolute target tolerance: 5.000 kPa (37.5 torr) Repeat analysis: Yes Fast evacuation: Yes Unrestricted evac. pressure: N/A Vacuum Setpoint: 1.3 Pa (10 microns) Evacuation time: 60 min Free space group: Measured Estimated free space: 6.8500 cm³ Incremental dosing: No

Pressure Table Absolute Include in Lang. Surf. Freund. Temkin Pressure (torr) Line Fit Area 1 100 x 2 150 x 3 200 x 4 250 x 5 300 x 6 350 x 7 400 x 8 450 x Report Options Report Options ID: chemi report Report Title: Smooth Pressure Data: No




Active Metals Table

Element Atomic Atomic Cross. % of Sample Density (g/cm³) Weight Sect. Area Weight platinum 195.0900 0.0800 0.500 21.4500 Stoichoimetry Factor Hydrogen 1.000 Oxygen 1.000 Carbon Monoxide 1.000 Helium 1.000 Isotherm: Yes Tabular Report Selected: Yes Plot Report Selected: Yes X Axis Scale: Linear Plot Analysis: Yes Plot Repeat Analysis: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Analysis: Yes Summary Report Selected: Yes Tabular Report Selected: Yes Plot Report Selected: Yes Report Differences: Yes Report Analysis: Yes Plot Analysis: Yes Plot Repeat Analysis: Yes Plot Difference: Yes Plot Curve: Yes Plot Points: Yes Overlay Samples: No Autoscale X Axis: Yes Autoscale Y Axis: Yes Langmuir Surface Area: No Freundlich: No Temkin: No Options: Yes Sample Log: Yes




APPENDIX D

(deleted by ECN 050223) APPENDIX E

(deleted by ECN 050223)

APPENDIX F Alcatel pump conditioning

For units in which one or more Alcatel Hybrid high vacuum pumps are installed, they must be “run-in” before putting into full operation. Use the following procedure.

Note: this procedure does not apply to Edwards or Pfeiffer hybrid high vacuum pumps.

The Alcatel pump uses bearings which are lubricated with grease. When the pump is unused for 30 days or more, the grease settles and must be redistributed before full speed operation is allowed.

FAILURE TO CONDITION THE BEARINGS CORRECTLY MAY DAMAGE THEM.

This procedure also must be followed when the pump (or the instrument in which it is installed) is transported in any way, G forces, even light G forces, will distribute the grease unevenly. The following steps are then required to return the pump to operational condition. Turn off the power to the instrument. Turn off the forepumps connected to the high vacuum pump. Turn off the power to the high vacuum pump, using the breaker which is located beneath the cover plate under the elevator. If it was running, wait for the high vacuum pump to stop; about 30 minutes. Remove the connecting hose that connects the forepump to the instrument. This will prevent the high vacuum pump from attaining full speed. Apply power to the high vacuum pump, by turning on the high vacuum pump breaker and then the instrument power. The high vacuum pump will begin to turn, but will never reach full speed. The bearings will warm up, and the grease will be gently redistributed. Run the pump for 10 minutes. Do not exceed 15 minutes. Turn off the high vacuum pump breaker, so that the pump slows down and comes to a complete stop. (Since there is no forepump, this should take only a few minutes. Wait 15 minutes to be sure. You can listen closely to the pump and you may be able to hear it slowing down).. Reconnect the forepumps. Turn them on. Turn on the power to the high vacuum pumps.




SERVICE APPENDIX

(Page 1 of 9)

5.5 Service Field calibration of Pressure Transducers Justification The transducer calibration in the first section of this procedure is centered on the use of a full range transfer pressure standard. This standard was not available to all field locations when revision A of this procedure was released. The following steps are included here to allow an alternate method of calibration when the recommended transfer standard is unavailable.

5.5.1 Service Calibrating and Verifying the 1000 torr Pressure Transducer

Purpose: To calibrate and verify the 1000 torr pressure transducer at known vacuum and

pressure levels.

Inputs: Gasses connected. Reference Pressure Gauge (003-09603-00, Crystal Gauge)

Action:

1. The sample frit and frit opener must be removed from the analysis. Failure to remove the frit may cause calibration errors.

1. It is extremely important to properly zero the reference pressure gauge. 2. Record the serial number and calibration expiration date of the reference pressure gauge. 3. Attach the reference pressure gauge to the analysis port. 4. If Manual Mode is not enabled, select Unit 1 > Enable Manual Mode to enable it. Open

valves 1, 2, 7, and 9. From the manual control screen, open valves 1, 2, 7, and 9. 5. Evacuate to below 20 microns. Continue to evacuate for 5 – 10 minutes. 6. While valves 1, 2, 7, and 9 are still open, zero the reference pressure gauge as follows:

a. Rotate the range selector knob on the gauge to 100mmHgA setting. b. Use a small screwdriver to adjust the ZERO potentiometer until the display reads 00.00

(± 0.05 torr). c. Record the zero reading for the reference pressure gauge on the data sheet at the end of

this section. d. Set the selector knob to 1000mmHgA. e. Use a small screwdriver to adjust the zero potentiometer until the display reads 000.0 (±

0.05 torr). f. Record the zero reading from the reference pressure gauge on the data sheet at the end of

this section. 7. Ensure that nitrogen is available above valves 4 and 5. With valves 1 and 2 closed, open

valves 4 and 9. Pressure should increase very slowly. Record slow pressure increase on the data sheet.

8. Open valve 5 and the rate of pressure rise should become faster. Record fast pressure increase on the data sheet. Close valves 4 and 5 at 760 torr (± 10 torr) as shown on the reference pressure gauge.




SERVICE APPENDIX

(Page 2 of 9) Field calibration of Pressure Transducers

9. From the Unit menu in the tool bar, choose “calibration”, then “Pressure Scale (1000 torr)”.

Execute and follow the instructions. 10. Open valves 1 and 2 and evacuate the manifold until the vacuum level is below 20 microns.

The reference pressure gauge should read zero. Observe the pressure reading on the computer screen. (It should read zero ± 0.05 torr. If there is a 10 torr transducer and if there is also a 1 torr transducer, then their readings should also be ± 0.05 torr).

11. Zero the pressure gauge as per Step 7. 12. Indicate that you have calibrated the 1000 torr transducer on the datasheet. 13. With valves 1 and 2 closed, open valves 4, 5 and 9 and build pressure to 760 (± 10) torr.

The reference gauge and the analyzer reading on the computer screen must not differ by more than ± 0.1 torr. If greater than ± 0.1 torr repeat Steps 7 - 12 until successful.

14. Build or reduce pressure as required to achieve targets listed on the data sheet. The values shown are nominal values. It is only necessary to be within 5% of each target pressure.

15. Record those pressures from the computer display and from the reference gauge and check to make sure they are within specifications.

16. If you will not be calibrating the 10 torr transducer, backfill the manifold to 800 torr. Close valve 9. Remove the reference gauge, and re-install the port frit and the frit opener.

17. If you are going to calibrate the 10 torr transducer, evacuate the manifold by opening valves 1 and 2.

Acceptance Criteria: This portion is considered complete when Steps 1-16 are successfully

completed and all target pressures are within specifications. Output: The Data Sheet is 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. Calibration of 1000 torr is very important because it will be used as a standard to calibrate the 10 torr transducer, if installed.

5.5.2 Service Calibrating the 10 torr Pressure Transducer. (If applicable, 10 torr equipped units.)

Purpose To calibrate the 10 torr pressure transducer. Inputs The 1000 torr transducer will be used as a pressure standard for the 10 torr

transducer.




SERVICE APPENDIX


Action: 1. The 1000 torr transducer accuracy must be verified before performing this step. 2. With valves 1, 2, and 7 open, evacuate the manifold to a pressure of 10 microns or less.

Allow the system to pump for an additional 30 minutes before zeroing the pressure reading. 3. Close valves 1 and 2. Using valve 4 slowly dose nitrogen until the 1000 torr pressure

reading on the computer display reads 7 torr (± 0.5 torr). 4. From the Unit menu in the tool bar, choose “calibration”, then “Pressure Scale (10 torr)”.

Execute and follow the instructions. 5. Record the values shown on the screen from the 10 and 1000 torr transducers immediately

after the calibration dialog closes, on the data sheet at the end of this section. 6. In preparation for the next step (either verifying the 10 torr calibration, or calibrating a 1 torr

transducer), evacuate the manifold by opening valves 1 and 2.

Acceptance Criteria: This portion is considered complete when the 10 torr transducer is calibrated at ~7 torr.

Outputs: Data sheet must be completed indicating this step is complete.

Background: This test was conducted to calibrate the 10 torr transducer. This calibration technique of using one transducer to calibrate another compensates for any slight scaling error of the transducer or the electronics

5.5.3 Service Calibrating the 1 torr Pressure Transducer. (If applicable, 1 torr equipped units.)

Purpose: To calibrate the 1 torr pressure transducer.

Input: The 10 torr transducer will be used as a pressure standard for the 1 torr transducer.

Action: 1. The 10 torr transducer accuracy must be verified before performing this step. 2. With valves 1, 2, and 7 open, evacuate the manifold to a pressure of 10 microns or less.

Allow the system to pump for an additional 30 minutes before zeroing the pressure reading. 3. Close valves 1 and 2. 4. Open valve 4 (or pulse valve 4 using the “P” key) to 0.7 torr (+/- 0.05 torr). Use the 10 torr

transducer reading to set this pressure. 5. From the Unit menu in the tool bar, choose “calibration”, then “Pressure Scale (1 torr)”.

Execute and follow the instructions. 6. Record the values shown on the screen from the 1 and 10 torr transducers immediately after

the calibration dialog closes, on the data sheet at the end of this section. 7. In preparation for the next step, evacuate the manifold by opening valves 1 and 2.




SERVICE APPENDIX


Acceptance Criteria: This portion is considered complete when the 1 torr transducer is

calibrated at ~0.7 torr. Outputs: Data sheet must be completed indicating step is complete. Background: This test was conducted to calibrate the 1 torr transducer. This calibration

technique of using one transducer to calibrate another compensates for any slight scaling error of the transducer or the electronics.

5.5.4 Service Verifying the 10 torr Pressure Transducer. (If applicable, 10 torr equipped

units.) Purpose To verify the accuracy of the 10 torr pressure transducer. Inputs Step F.2 completed. Action:

1. Open valves 1, 2, and 7 and evacuate to below 10 microns. 2. With valves 1, 2, and 7 open, evacuate the manifold to a pressure of 10 microns or less.

Allow the system to pump for 5 minutes before zeroing the pressure reading. 3. Close valves 1 and 2. Using valve 4 slowly dose nitrogen until the 1000 torr pressure

reading on the computer display reads ~ 8 torr (7.6 – 8.4 torr). 4. Record the values on the data sheet. 5. Using valve 2, slowly reduce the manifold pressure until the 1000 torr pressure reading on

the computer display reads ~ 5 torr (4.7 – 5.3 torr). 6. Record the values on the data sheet. 7. Using valve 2, slowly reduce the manifold pressure until the 1000 torr pressure reading on

the computer display reads ~ 3 torr (2.8 – 3.2 torr). 8. Record the values on the data sheet 9. If you will not be verifying the 1 torr transducer, backfill the manifold to 800 torr. Close

valve 9. Remove the reference gauge, and re-install the port frit and the frit opener. 10. If you are going to verify the 1 torr transducer, evacuate the manifold by opening valves 1

and 2. Acceptance Criteria: This portion is considered complete when the 10 torr transducer

accuracy has been verified at ~8 torr, ~5 torr, and ~3 torr.




SERVICE APPENDIX


Outputs: Data sheet must be completed indicating this step is complete. Background: This test was conducted to verify the accuracy of the 10 torr transducer. This

calibration technique of using one transducer to calibrate another compensates for any slight scaling error of the transducer or the electronics.

5.5.5 Service Verifying the 1 torr Pressure Transducer. (If applicable, 1 torr equipped units.) Purpose To verify the accuracy of the 1 torr pressure transducer. Inputs Step F.3 completed. Action:

1. With valves 1, 2, and 7 open, evacuate the manifold to a pressure of 10 microns or less. Allow the system to pump for 5 minutes before zeroing the pressure reading.

2. Close valves 1 and 2. Using valve 4 slowly dose nitrogen until the 10 torr pressure reading on the computer display reads ~ 0.8 torr (.76 - .82 torr).

3. Record the values on the data sheet. 4. Using valve 2, slowly reduce the manifold pressure until the 10 torr pressure reading on the

computer display reads ~ 0.5 torr (.47 - .53 torr). 5. Record the values on the data sheet. 6. Using valve 2, slowly reduce the manifold pressure until the 10 torr pressure reading on the

computer display reads ~ 0.3 torr (.28 - .32 torr). 7. Record the values on the data sheet. 8. Backfill the manifold to 800 torr. Close valve 9. Remove the reference gauge, and re-install

the port frit and the frit opener. Acceptance Criteria: This portion is considered complete when the 1 torr transducer

accuracy has been verified at ~0.8 torr, ~0.5 torr, and ~0.3 torr. Outputs: Data sheet must be completed indicating this step is complete. Background: This test was conducted to verify the accuracy of the 1 torr transducer. This

calibration technique using one transducer to calibrate another compensates for any slight scaling error of the transducer or the electronics.

The accuracy comparisons are based on a worst case error analysis of the transducer readings at the overlapping regions where the 1000 torr transducer is compared o the 10 torr transducer, and where the 10 torr transducer is compared to the 1 torr transducer. The following table shows how this error budget was derive.




SERVICE APPENDIX


Error budget, comparing installed 2020 transducers Assumes perfectly zeroed transducers

1000 torr transducer

transducer error, % of reading

screen resolution error

(+/-), torr max error

rounded to display resolutio

n

min displayed value

max displayed value

pressure 0.15% 0.01 +/- +/- 8 0.012 0.022 0.02 7.98 8.02 5 0.0075 0.0175 0.02 4.98 5.02 3 0.0045 0.0145 0.01 2.99 3.01

10 torr transducer





n

min displayed value

max displayed value

max possible difference

pressure 0.15% 0.0001 +/- +/- max 1000 - min 10

8 0.012 0.0121 0.0121 7.9879 8.0121 0.03 5 0.0075 0.0076 0.0076 4.9924 5.0076 0.0251 3 0.0045 0.0046 0.0046 2.9954 3.0046 0.0191

1 torr transducer





n

min displayed value

max displayed value

pressure 0.12% 0.00001 +/- +/- 0.8 0.00096 0.00097 0.00097 0.79903 0.80097 0.5 0.0006 0.00061 0.00061 0.49939 0.50061 0.3 0.00036 0.00037 0.00037 0.29963 0.30037

10 torr transducer





n

min displayed value

max displayed value

max possible difference

pressure 0.15% 0.0001 +/- +/- max 10 - min 1

0.8 0.0012 0.0012 0.0012 0.7988 0.8012 0.00217 0.5 0.00075 0.00075 0.0008 0.49925 0.50075 0.00136 0.3 0.00045 0.00045 0.0005 0.29955 0.30045 0.00082




SERVICE APPENDIX


Data Sheet for Field Calibration and Verification of Pressure Transducers

Part Number Description Serial # Cal. Due Date

003-09603-00 Pressure Calibration Standard

5.5.1 Service Calibrating and Verifying the 1000 torr Pressure Transducer Reference Pressure Gauge OK ? Record zero reading for 100mmHgA setting Record zero reading for 1000mmHgA setting Valve 4 shows pressure increase when opened? Valve 5 shows even faster pressure increase when opened? Software calibration routine completed at 760 torr?

Target Pressure (torr)

Computer Display

Reference Gauge

Difference

~760 (722 – 798) ~850 (804 – 893) ~650 (617 – 683) ~550 (522 – 578) ~450 (427 – 473) ~350 (332 – 368) ~250 (237 – 263) ~150 (142 – 158) All values in “Difference” column less than 1.5 torr?

5.5.2 Service Calibrating the 10 torr Pressure Transducer

Software calibration routine completed? (Computer readings) Pressure 10 torr 1000 torr ~7 (6.5 – 7.5)

5.5.3 Service Calibrating the 1 torr Pressure Transducer

Software calibration routine completed? (Computer readings) Pressure 1 torr 10 torr ~.7 (.65 – .75)




SERVICE APPENDIX


Serial Number

5.5.4 Service Verifying the 10 torr Pressure Transducer (Record values from the computer screen) Pressure 10 torr 1000 torr Difference ~8 (7.6 – 8.4) ~5 (4.7 – 5.3) ~3 (2.8 – 3.2) All values in “Difference” column less than +/-0.03 torr? 5.5.5 Service Verifying the 1 torr Pressure Transducer (Record values from the computer screen) Pressure 1 torr 10 torr Difference ~0.8 (.76 - .84) ~0.5 (.47 - .53) ~0.3 (.28 - .32) All values in “Difference” column less than +/-0.005 torr?




SERVICE APPENDIX

(Page 9 of 9) Serial Number

5.8 Service Field calibration of System Volume

Justification The system volume calibration and verification in the first section of this procedure uses two reference volume chambers; one with a solenoid valve and one with a manual valve. Carrying both chambers in field service kits is impractical in most locations. The following steps are provided as a means of verifying the existing volume calibration, and making adjustments if the measurement indicates that the stored system volume is incorrect.

5.8.1 Service Verifying the system volume The 1000 Torr transducer must be correctly calibrated. The manifold temperature must be correctly calibrated. The vacuum gauge must be correctly calibrated. The system must be leak free. A blank sample tube run is the best indicator that the system is leak free. Perform step 5.10 (Reference Chamber Analysis) using chamber 004/29801/00. This chamber has a manual valve above the chamber. Fill out this worksheet. Reference Volume cc Measured Volume Difference Max Difference = +/- 0.5%

If the difference is larger than the maximum difference allowed, then perform the following calculations.

5.8.2 Service Adjusting the volume values Reference Volume / Measured Volume = Correction Value = K = From the Unit menu, select Calibration, and then select Volume. Copy the existing (old) values for the System Volume and for the Lower Volume into the following worksheet to calculate new values. New System Volume = Old value x K = cc New Lower Volume = Old value x K = cc On the calibration screen, select the “Entered” button, and then type the new values in the appropriate boxes. Accept the new values and close the screen.

5.8.3 Service Verifying the new values Repeat step 5.10. Complete the following worksheet to confirm that the new system volume calibration values provide the correct measured volume. Reference Volume cc Measured Volume Difference Max Difference = +/- 0.5%




PCP AUTHOR COMPLETENESS CHECKLIST

This section was completed by the author of the PCP to satisfy the requirements of the Micromeritics Procedure for Creating and Maintaining Product Calibration Procedures (001/42036/00). No further action is necessary.

[x] Check power level in all important places. Sections: 5.2 [x] Initialize non-volatile memory: Programmable parts loaded. Board IDs set up properly. Confirm versions of all software used in system. Sections: 4.6 [x] Prepare (clean/set up) instrument before any tests are done. Sections: 5.0, 5.6 [x] Test both actuation and status of all items that can be actuated Sections: 5.1 [x] Calibrate and check all analog signals. Sections: 5.3, 5.4, 5.5, 5.20, 5.21, 5.22, 5.31 [x] Ensure all hardware adjustments done. Pots Restrictions Sections: 5.3, 5.20 [x] Test subsystem performance independently of analyses. Leak rates, outgas rates Flow rates Sections: 5.23, 5.24 [x] Calibrate all subsystems that need it Volume calibration Normalization Sections: 5.8 [x] Confirm proper operation and results with analyses. Sections: 5.9, 5.10, 5.11, 5.12, 5.13, 5.30, 5.32, 5.33, 5.34 [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 [x] Ensure enough time on the instrument to overcome initial component failures Burn in of heaters General components initial failure Sections: 5.6, 5.7, 5.24, 5.32 [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




Checklist Sections: 5.40, 5.41, 5.42

product calibration procedure for the … calibration procedure for the asap 2020 ... 003-09619-00*...

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