QUANTACHROME INSTRUMENTS MULTIPYCNOMETER User manual

MULTIPYCNOMETER
QUALITY ASSURANCE
AND
SERVICE
MANUAL
REVISION: K
MANUAL NUMBER: 05300-114
DATE OF LATEST REVISION: 03/24/14
ISSUE DATE: 7/18/16
©
COPYRIGHT (1997-2016) QUANTACHROME INSTRUMENTS

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TABLE OF CONTENTS
MULTIPYCNOMETER ................................................................................................ 1
1.0. PURPOSE ....................................................................................................... 3
2.0. SCOPE............................................................................................................ 3
3.0. DEFINITIONS ................................................................................................. 3
4.0. RESPONSIBILITIES ....................................................................................... 4
5.0. REQUIREMENTS ........................................................................................... 5
5.1. ELECTRICAL AND MECHANICAL INSPECTION ......................................... 5
5.2. POWER CHECKS .......................................................................................... 7
5.3. ALIGNMENTS ............................................................................................... 8
5.4. LEAK TEST .................................................................................................. 12
5.5. CALIBRATION .............................................................................................. 16
6.0. REFERENCES .............................................................................................. 26
APPENDIX A ............................................................................................................ 27
APPENDIX B ........................................................................................................... 28
APPENDIX B ........................................................................................................... 29
B.2. INSTRUMENT CALIBRATION SHEET FOR THE LARGE CELL .................... 29
B.3. INSTRUMENT CALIBRATION SHEET FOR THE SMALL CELL..................... 30
B.4. INSTRUMENT CALIBRATION SHEET FOR THE MICRO CELL ..................... 32
APPENDIX C ........................................................................................................... 34
C.1 SPHERE RUNS’ DATA SHEETS ...................................................................... 34
APPENDIX D ............................................................................................................ 35

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D.1. SPARE PARTS LIST .................................................................................... 35
D.2. ACCESSORY LIST ...................................................................................... 36
1.0. PURPOSE
1.1. THE REQUIREMENTS SPECIFIED HEREIN ARE INTENDED TO ASSURE
THAT MULTIPYCNOMETERS WITH MODEL NUMBER MVP-3 MEET OR
EXCEED THE REQUIRED MANUFACTURING AND QUALITY ASSURANCE
STANDARDS AS SPECIFIED IN THE COMPANY QUALITY MANUAL.
2.0. SCOPE
2.1. THIS PROCEDURE IS TO BE FOLLOWED BY ALL QUALITY
ASSURANCE PERSONNEL INVOLVED WITH MULTIPYCNOMETER TEST AND
CALIBRATION PROCEDURES.
2.2. THIS PROCEDURE CONTAINS CALIBRATION GUIDELINES THAT CAN
ALSO BE FOLLOWED BY QUALIFIED TECHNICIANS, INCLUDING
QUANTACHROME CUSTOMERS, AGENTS AND SALES PEOPLE.
2.3. THESE REQUIREMENTS APPLY TO OTHER MULTIPYCNOMETER MODELS WITH
MODIFICATIONS OUTLINED IN APPENDIX A.
3.0. DEFINITIONS
3.1. MULTIPYCNOMETER: APPARATUS DESIGNED TO MEASURE TRUE
SOLID VOLUMES BY A GAS EXPANSION TECHNIQUE KNOWN AS HELIUM
PYCNOMETRY [ 1 , 2 ].
3.2. QUALITY ASSURANCE: FULL COMPLIANCE WITH PROCEDURES AND
STANDARDS ITEMIZED IN THE COMPANY QUALITY MANUAL.
3.3. SERVICE: GUIDELINES PROVIDED TO ENABLE SERVICE
TECHNICIANS TO HANDLE INSTRUMENT TROUBLESHOOTING.
3.4. MVP - i : MULTIPLE VOLUME PYCNOMETER, MODEL -i .
3.5. VR : KNOWN MANIFOLD REFERENCE VOLUME IN CC’S [ 2 ].
3.6. VC : CELL VOLUME IN CC’S.
3.7. VP: SPHERE OR SAMPLE VOLUME IN CC’S.
3.8. PRESSURE: ALL PRESSURE READINGS ARE DISPLAYED ON THE
DIGITAL PANEL METER AND ARE GIVEN IN PSIG (POUNDS PER SQUARE
INCH GAUGE PRESSURE).

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3.9. SPHERES: STAINLESS STEEL BALLS OF VARIOUS SIZES ARE USED FOR
VOLUME CALIBRATIONS. ALL SPHERE VOLUMES ARE GIVEN IN CUBIC
CENTIMETERS (CC`S).
3.10. TOGGLE VALVE: TOGGLE VALVES ARE ON / OFF VALVES LABELED I, II,
GAS IN AND GAS OUT ON THE INSTRUMENT PANEL FACE. VALVES ARE
CLOSED WHEN THEIR HANDLES ARE PARALLEL TO THE CABINET FACE AND
OPEN WHEN PERPENDICULAR TO THE CABINET FACE.
3.11. NEEDLE VALVE: TWO ADJUSTABLE NEEDLE VALVES PERMIT FLOW
RATE CONTROL THROUGH GAS IN AND GAS OUT. TURNING THEIR KNOB
CLOCKWISE REDUCES THEIR RESPECTIVE FLOW RATES.
3.12. CORCOM: FUSED ELECTRICAL RECEPTACLE USED TO CONFIGURE THE
INPUT POWER FOR 100,120, 220, OR 240VAC. THE RECEPTACLE IS LOCATED ON
THE INSTRUMENT’S BACK PANEL.
3.13. SELECTOR VALVE: TWO - POSITION BALL VALVE LOCATED ON THE
MULTIPYCNOMETER’S CABINET FACE FOR SWITCHING BETWEEN POSITIONS
LABELED CELL AND REFERENCE.
4.0. RESPONSIBILITIES
4.1. THE FOLLOWING PROCEDURE SHALL BE PERFORMED ONLY BY
INDIVIDUALS TRAINED AS ELECTRICAL AND MECHANICAL TECHNICIANS.
4.2. QUANTACHROME TECHNICIANS SHALL BE FULLY TRAINED ON
ELECTRICAL PROCEDURES, MECHANICAL ASSEMBLY, AND GAS HANDLING
OPERATIONS AS OUTLINED IN THE COMPANY QUALITY MANUAL.
4.3. TECHNICIANS WILL HAVE AVAILABLE THE FOLLOWING
EQUIPMENT REQUIRED FOR TESTING.
4.3.1. CALIBRATED 4 1/2 DIGITAL VOLTMETER WITH OHMS, AC-
250VAC AND DC 24VDC.
4.3.2. ULTRA HIGH PURITY (99.999%) HELIUM WITH A TWO STAGE
REGULATOR SET TO DELIVER AT LEAST 25 PSIG OF PRESSURE.
4.3.3. 5/16 HEX ALLEN WRENCH.
4.3.4. STANDARD HAND TOOLS.
4.3.5. JEWELER’S SCREWDRIVER.
4.3.6. CALIBRATED PRESSURE GAUGE TO READ 25 +/- 0.25 PSIG.
4.3.7. BEAKER HALF FULL OF WATER.
4.3.8. TORQUE SEAL.

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4.4. THE QUALITY ASSURANCE MANAGER WILL CONFIRM THAT
QUANTACHROME TECHNICIANS FOLLOW ALL PROCEDURES IN
COMPLIANCE WITH THE GUIDELINES STATED IN THE COMPANY QUALITY
MANUAL.
4.5. THE PRODUCT MANAGER WILL EVALUATE ALL REVISIONS TO THIS
DOCUMENT TO ENSURE COMPLIANCE WITH ENGINEERING DESIGN
REQUIREMENTS.
5.0. REQUIREMENTS
5.1. ELECTRICAL AND MECHANICAL INSPECTION
5.1.1 ELECTRICAL
5.1.1.1 WIRING - VERIFY THAT ALL WIRING CONTINUITY CONFORMS TO THE
LATEST REVISION DRAWING
5.1.1.2. VISUALLY INSPECT THE DIGITAL PANEL METER CONNECTOR FOR
CORRECT WIRING AND ALL SOLDERING FOR COLD JOINTS.
5.1.1.3. VERIFY THAT TWO 2 AMP FUSES ARE INSTALLED IN THE CORCOM.
REMOVE THE FUSE BY SLIDING THE BLACK HANDLE IN THE CORCOM TO THE
LEFT. REINSTALL THE FUSES IF THE AMPERAGE IS CORRECT.
5.1.1.4. RECONFIGURE THE CORCOM TO MATCH THE VOLTGE REQUIRED FOR
THE CUSTOMER ORDER (FUSED ELECTRICAL RECEPTACLE) FOR 120 VAC.
PUSH THE PLASTIC SHIELD TO THE LEFT,
5.1.1.5. THE NEW CORCOM HAS A BARREL TYPE VOLTAGE ADJUSTMENT. DO
NOT SPIN THE BARREL OR YOU MAY DAMAGE THE CONTACTS. PULL OUT THE
BARREL AND ROTATE THE BARREL TO THE SPECIFIED CUSTOMER VOLTAGE
REQUIREMENT.

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5.1.2. MECHANICAL
5.1.2.1. VERIFY THAT ALL FRONT PANEL KNOBS ROTATE FREELY AND
THAT THE ZERO KNOB HAS A NYLON WASHER PLACED BEHIND IT.
5.1.2.2. VERIFY THAT THE SAMPLE CELL HOLDER COVER AND ITS RECEPTOR
IN THE INSTRUMENT’S COVER PANEL HAVE CLEARLY VISIBLE WHITE
ALIGNMENT LINES (FIDUCIARY MARKS). ALSO VERIFY THAT THE COVER
SCREWS FREELY ONTO THE RECEPTOR, AND THAT WHEN FULLY TIGHTENED
IT IS NOT IN CONTACT WITH THE BLACK BULKHEAD RETAINER.
5.1.2.3. REMOVE THE 2-INCH O-RING (PART NUMBER 51000-032) FROM
UNDER THE SAMPLE CELL HOLDER COVER. CLEAN THE COVER AND THE
BRASS CELL HOLDER SEAT. APPLY A VERY LIGHT COAT OF VACUUM
GREASE TO THE O-RING AND REINSTALL IT IN THE CELL COVER.
5.1.2.4. INSPECT THE SAMPLE CELL HOLDER TO MAKE SURE THAT IT HAS NO
SCRATCHES AND VERIFY THAT THE GAS INLET GROOVE IS CLEAN, FREE OF
DIRT AND THAT ITS FLOW PATH IS UNRESTRICTED.
5.1.2.5 VERIFY THAT ALL FITTINGS ARE SET ON TIGHTLY AND THAT ALL
SOLDER JOINTS ARE CLEAN, NOT COLD AND HAVE SHRINKABLE CLEAR
TUBING OVER THEM.
5.1.2.6. VERIFY THAT TWO PLASTIC TIES ARE WRAPPED AROUND BOTH THE
BIMBA BRAND AIR CHAMBER AND THE BRASS CELL HOLDER IN ORDER TO TIE
BOTH TOGETHER.
5.1.2.7. CLEAN ALL SPHERES, SAMPLE CELL CUPS AND SLEEVES WITH
ISOPROPYL AND A LINT-FREE TISSUE.
5.1.2.8. VERIFY THAT ALL THE SAMPLE CELL CUPS FIT SNUGLY INTO THEIR
SLEEVES AND THAT ALL SLEEVES FIT INTO THE BRASS SAMPLE CELL
HOLDER.

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5.2. POWER CHECKS
5.2.1. AC CHECKS
5.2.1.1. CAUTION -THESE CHECKS MUST BE PERFORMED WITH THE POWER
SWITCH TURNED OFF AND WITH THE POWER CORD UNPLUGGED. THESE
INSTRUCTIONS SHOULD ONLY BE PERFORMED BY TRAINED PERSONNEL AND
THEN ONLY AFTER TAKING ALL PERTINENT SAFETY PRECAUTIONS.
5.2.1.2. SET THE POWER SWITCH TO THE OFF POSITION AND CONFIGURE THE
CORCOM FOR 120 VAC OR TO THE SPECIFIED CUSTOMER VOLTAGE
REQUIREMENT. THE CORCOM CARD IS LOCATED BEHIND THE CLEAR PLASTIC
SLIDE DOOR NEXT TO THE POWER SOCKET. TO CHANGE THE VOLTAGE
SETTINGS, SLIDE THE DOOR AND REMOVE THE CARD USING PLIERS. HOLD
THE CARD SO THAT THE VOLTAGE YOU ARE CONFIGURING THE UNIT FOR
FACES YOU, AND SLIDE THE CARD BACK IN THE SLOT.
5.2.1.3. USING AN OHM METER, TEST FOR CONTINUITY ACROSS THE LINE
INPUT TERMINALS. THE READING SHOULD BE INFINITY (OPEN CIRCUIT).
5.2.1.4. USING AN OHM METER, TEST FOR CONTINUITY BETWEEN THE INPUT
LINE TERMINALS AND THE CHASSIS GROUND. THE READING SHOULD BE
INFINITY (OPEN CIRCUIT).
5.2.1.5. USING AN OHM METER, TEST FOR CONTINUITY BETWEEN THE INPUT
GROUND TERMINALS AND THE CHASSIS GROUND. VERIFY A READING OF
CONTINUITY INDICATING A SHORT CIRCUIT.
5.2.1.6. SET THE POWER SWITCH TO ON. USING AN OHM METER, TEST ACROSS
THE LINE INPUT TERMINALS. THE READING SHOULD BE AROUND 17 OHMS. IF
A SHORT IS READ THE SWITCH MAY BE WIRED INCORRECTLY.
THE READING SHOULD BE AROUND 68 OHMS IF THE VOLTAGE IS 220V-240V.

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5.3.2.2. DC POWER -ON CHECKS
5.2.2.1. REMOVE THE PRESSURE TRANSDUCER CONNECTOR FROM THE SMALL
PRINTED CIRCUIT BOARD (PART NUMBER 00003) LOCATED INSIDE ON THE
LEFT BULKHEAD.
5.2.2.2. CONNECT THE INSTRUMENT TO THE 120 VAC SUPPLY OUTLET (OR TO
THE CUSTOMER REQUIRED VOLTAGE) AND TURN THE POWER SWITCH TO THE
“ON” POSITION.
5.2.2.3. USING A CALIBRATED DIGITAL VOLT METER, CHECK AND ADJUST THE
POWER SUPPLY FOR DC OUTPUT VOLTAGE SUPPLIED TO THE CIRCUIT CARD.
THE READINGS ARE TAKEN AT THE POWER SUPPLY TERMINALS AND ARE
REFERENCED TO THE NEUTRAL POST. THESE READINGS SHOULD BE +24.00 
0.01VDC AT THE POST RED & YELLOW AND + 5.00  0.01VDC AT THE POST
COM. & ORG.
5.2.2.4. CONNECT THE VOLTMETER LEADS TO THE PRESSURE TRANSDUCER
PLUG ON THE SMALL PRINTED CIRCUIT BOARD AND VERIFY THAT +24 
0.01VDC ARE MEASURED ACROSS PINS 4 AND 6.
5.2.2.5. TURN THE POWER SWITCH TO OFF AND THEN RECONNECT THE
PRESSURE TRANSDUCER CONNECTOR TO THE SMALL PRINTED CIRCUIT
BOARD.
5.3. ALIGNMENTS
5.3.1. DIGITAL PANEL METER
5.3.1.1. TURN THE INSTRUMENT’S POWER SWITCH TO ON. VERIFY THAT THE
DIGITAL PANEL DISPLAYS NUMBERS THAT ARE BRIGHT AND CLEAR.
5.3.1.2. TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL FROM
STOP TO STOP SLOWLY AND VERIFY THAT SMOOTH DIGITAL CHANGES OCCUR
AND THAT ALL SEGMENTS OF EACH DIGIT ILLUMINATE.
5.3.1.3. TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL TO THE
MID-RANGE POSITION (5 TURNS FROM THE STOP FOR A TYPICAL 10 TURN
POTENTIOMETER).
5.3.1.4. TURN THE SELECTOR VALVE TO THE CELL POSITION AND OPEN THE
GAS OUT TOGGLE VALVE TO VENT THE CELL. AFTER 5 MINUTES OF WARM UP
TIME ADJUST RESISTOR R1 LOCATED ON THE SMALL PRINTED CIRCUIT
BOARD FOR A READING OF 0.000 PSIG ON THE DIGITAL PANEL METER. THIS IS
PERFORMED BY PLACING A JEWELER’S SCREWDRIVER THROUGH THE HOLE IN
THE BACK PANEL AND TURNING THE POTENTIOMETER UNTIL THE DIGITAL
PANEL METER READING DISPLAYS 0.000 PSIG.
5.3.1.5. PLACE A SMALL AMOUNT OF TORQUE SEAL BETWEEN THE
ADJUSTMENT KNOB AND THE BODY OF THE POTENTIOMETER R1 TO INSURE
THAT IT REMAINS UNCHANGED DURING SHIPMENT.

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5.3.2 Texmate DI-50E Panel Meter Setup
STEP A CODE SETUP: Instrument Model No. MVP-DI50E (Multi- Pycnometer)
5.3.2.1 Press Program and Up-arrow at the same time:
This enters the main programming mode. Display toggles between [bri]
and [5].
Press Program to set bri to 5. If bri is not set to 5 then use up/ down arrow
and
set bri to 5.
5.3.2.2 Press Program button
Display toggles between [CAL] and [000].
5.3.2.3 Press Program button again
Display toggles between [Cod_1] and [000].
Change Cod_1 to 001 for model#24000-2-0-D. Enter 061 for
model#20033-1
5.3.2.4 Press Program button
Display toggles between [DiSP] and [003].
Change DiSP to 004. (This will move the decimal)
5.3.2.5 Press Program button
Display toggles between [Cod_1] and [061]
Change Cod_1 to 000.
5.3.2.6 Press Program button
Display toggles between [Cod_2] and [XXX]
Change Cod_2 to 001.
5.3.2.7 Press Program button
Display toggles between [Cod_3] and [XXX]
Change Cod_3 to 000.
5.3.2.8 Press Program button
Display toggles between [Cod_4] and [XXX] Note: Set Cod_4 to 000 for
60 Hz
Change Cod_4 to 000. Set Cod_4 to 001 for
50 Hz
5.3.2.9 Press Program button
Display toggles between [Cod_5] and [XXX]
Change Cod_5 to 000.
5.3.2.10 Press Program button until you have reached Cod_8.
Display toggles between [Cod_8] and [XXX]
Change Cod_8 to 002.
5.3.2.11 Press Program button
Display toggles between [Cod_9] and [XXX]
Change Cod_9 to 000.
5.3.2.12 Press Program button
Display will indicate instrument’s current pressure.
Verify the decimal is set as XX.XXX

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5.3.2.13 Press Program and Down-arrow at the same time:
This enters the setpoint-programming mode.
Display toggles between [SP_1] and [50000]. 18.xxx for the new model
5.3.2.14 Press the Program button repeatedly until the
Display toggles between [SP_5] and [30000],10000 for the new model.
Change SP_5 to 1.000
Note: If SP_5 is unavailable, perform the next step (SPC_5) then come back
to this step; Ensure SPC_5 is set to [000].
You should now be able to set up SP_5 to 1.000. Continue and perform the
next step before locking the meter.
5.3.2.15 Press Program button repeatedly until the
Display toggles between [SPC_5] and [000].
Change SPC_5 to 46.
5.3.2.16 Check all the setting before lock
STEP B LOCK CODE SETUP:
5.3.2.17 Loosen the meter from cabinet.
5.3.2.18 Remove black face meter bezel.
5.3.2.18 Set both DIP Switches from OFF to ON position.
5.3.2.20 Reinstall the bezel and secure the meter.

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5.3.3. PRESSURE RELIEF VALVE
5.3.3.1. USING 1/8 INCH COPPER TUBING, CONNECT THE CALIBRATED
PRESSURE GAUGE BETWEEN THE HELIUM TANK AND THE GAS INPUT
SWAGELOCK CONNECTION LOCATED ON THE SIDE OF THE
STEREOPYCNOMETER .
5.3.3.2. THE PRESSURE RELIEF VALVE IS LOCATED IMMEDIATELY BEFORE THE
INPUT FLOW CONTROL NEEDLE VALVE INSIDE THE STEREOPYCNOMETER.
ADJUSTMENTS WILL BE MADE SO THE PRESSURE IS RELIEVED IF THE TANK
PRESSURE EXCEEDS 25 PSIG. AT 25 PSIG THE RELIEF VALVE WILL ACTUATE
AND THE GAS WILL BE VENTED, AFTER WHICH REMOVE THE GAS INPUT LINE
MOMENTARILY TO ALLOW THE PRESSURE RELIEF VALVE TO RESET
5.3.3.3. USING A 5/16 HEX ALLEN WRENCH, SET THE RELIEF VALVE TO JUST
STOP AT 25 PSIG. CHECK THE SETTING BY SUBMERGING THE END OF THE
RELIEF VALVE IN A BEAKER OF WATER, IN ORDER TO VERIFY THAT NO
BUBBLES ARE FORMED AT 25 PSIG. INCREASE THE TANK PRESSURE AS
DISPLAYED ON THE CALIBRATED PRESSURE GAUGE TO 26 PSIG AND VERIFY
THAT BUBBLES APPEAR IN THE BEAKER.
5.3.3.4. TIGHTEN THE OUTER LOCKING NUT UNTIL IT MEETS THE INNER NUT.
APPLY A MODERATE AMOUNT OF TORQUE SEAL TO THE OUTER NUT. NOTE
THAT AN EXCESSIVE AMOUNT OF TORQUE SEAL WILL BLOCK THE RELIEF
VALVE.
5.3.3.5. ADJUST THE TANK PRESSURE REGULATOR TO DELIVER SLIGHTLY
ABOVE 20 PSIG.

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5.4. LEAK TEST
5.4.1. PURGE
5.4.1.1. THE PROCEDURE TO PURGE THE INSTRUMENT (BY FLOWING HELIUM
TO REMOVE CONTAMINANTS) NEEDS TO BE PERFORMED PRIOR TO TESTING
NEW INSTRUMENTS AND INSTRUMENTS THAT HAD BEEN TURNED OFF FOR
MORE THAN ONE DAY. THERE IS NO NEED TO REPEAT THIS PROCEDURE
BETWEEN THE CELL AND REFERENCE CALIBRATIONS.
5.4.1.2. INSTALL THE TWO MICRO STAINLESS STEEL BALLS INTO THE SAMPLE
CELL AND THEN THE SAMPLE CELL INTO THE MICRO SLEEVE. PLACE THE
FILLED SLEEVE INTO THE CELL HOLDER AND THEN CLOSE THE CELL HOLDER
COVER. SET GAS IN NEEDLE VALVE TO 0 BY ADJUSTING KNOB AND SET
SCREW.
5.4.1.3. OPEN THE GAS OUT TOGGLE VALVE AND THE GAS OUT NEEDLE
VALVE.
5.4.1.4. SET THE SELECTOR VALVE TO THE CELL POSITION.
5.4.1.5. OPEN BOTH TOGGLE VALVES I AND II ON THE FRONT PANEL.
5.4.1.6. OPEN THE GAS IN TOGGLE VALVE AND ADJUST THE GAS IN NEEDLE
VALVE FOR A 1 PSIG PURGE RATE AS DISPLAYED ON THE DIGITAL PANEL
METER.
5.4.1.7. PURGE THE MULTIPYCNOMETER FOR 30 MINUTES BEFORE
CONTINUING TO STEP 5.4.2. CLOSE THE GAS IN TOGGLE VALVE WHEN THE
PURGE TIME IS COMPLETED.

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5.4.2. MICRO REFERENCE
5.4.2.1. FOLLOWING A SUITABLE PURGE (SEE ITEM 5.4.1.1), INSTALL THE
MICRO SAMPLE CELL AND SLEEVE WITH TWO MICRO STAINLESS STEEL
BALLS INTO THE CELL HOLDER AND CLOSE THE COVER. PURGE THE
INSTRUMENT FOR AN ADDITIONAL MINUTE TO REMOVE ALL AIR WITHIN IT.
5.4.2.2. CLOSE THE TOGGLE VALVES I, II AND GAS IN.
5.4.2.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
5.4.2.4. TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL UNTIL A
0.000 PSIG READING IS DISPLAYED ON THE DIGITAL PANEL METER.
5.4.2
.
5. TURN THE SELECTOR VALVE TO THE REFERENCE POSITION AND
CLOSE THE GAS OUT TOGGLE VALVE.
5.4.2.6. OPEN THE GAS IN TOGGLE VALVE AND, WHEN THE DIGITAL PANEL
METER READS 19.0 PSIG, CLOSE THE GAS IN TOGGLE VALVE.
5.4.2.7. RECORD THE FIRST STABLE READING AS THE STARTING PRESSURE
AND ENTER THAT READING ON THE INSTRUMENT CHECK SHEET IN APPENDIX
B.1, ITEM B.1.3.7. AS THE STARTING PRESSURE FOR MICRO. THIS WILL SIGNAL
THE BEGINNING OF A 1 MINUTE LEAK TEST.
5.4.2.8. AFTER 1 MINUTE HAS ELAPSED, RECORD THE READING AS DISPLAYED
ON THE DIGITAL PANEL METER AND ENTER THAT READING AS PRESSURE
AFTER 1 MINUTE FOR MICRO ON THE INSTRUMENT CHECK SHEET IN
APPENDIX B.1, ITEM B.1.3.7. THE CALCULATED LEAK RATE MUST BE NO
GREATER THAN 0.004 PSIG IN ONE MINUTE BEFORE PROCEEDING.

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5.4.3. SMALL REFERENCE
5.4.3.1. FOLLOWING A SUITABLE PURGE (SEE ITEM 5.4.1.1), INSTALL THE
MICRO SAMPLE CELL AND SLEEVE WITH TWO MICRO STAINLESS STEEL
BALLS INTO THE CELL HOLDER AND CLOSE THE COVER. PURGE THE
INSTRUMENT FOR AN ADDITIONAL MINUTE TO REMOVE ALL AIR WITHIN IT.
5.4.3.2. CLOSE ALL THE TOGGLE VALVES ON THE INSTRUMENT ‘S FRONT
PANEL. THEN, OPEN TOGGLE VALVE II.
5.4.3.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
5.4.3.4 TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL UNTIL A
0.000 PSIG READING IS DISPLAYED ON THE DIGITAL PANEL METER.
5.4.3.5. TURN THE SELECTOR VALVE TO THE REFERENCE POSITION AND
CLOSE THE GAS OUT TOGGLE VALVE.
5.4.3.6. OPEN THE GAS IN TOGGLE VALVE AND, WHEN THE DIGITAL PANEL
METER READS 19.0 PSIG, CLOSE THE GAS IN TOGGLE VALVE.
5.4.3.7. RECORD THE FIRST STABLE READING AS THE STARTING PRESSURE
AND ENTER THAT READING ON THE INSTRUMENT CHECK SHEET IN APPENDIX
B.1, ITEM B.1.3.7. AS THE STARTING PRESSURE FOR SMALL. THIS WILL SIGNAL
THE BEGINNING OF A 1 MINUTE LEAK TEST.
.
5.4.3.8. AFTER 1 MINUTE HAS ELAPSED, RECORD THE READING AS DISPLAYED
ON THE DIGITAL PANEL METER AND ENTER THAT READING AS PRESSURE
AFTER 1 MINUTE FOR SMALL ON THE INSTRUMENT CHECK SHEET IN
APPENDIX B.1, ITEM B.1.3.7. THE CALCULATED LEAK RATE MUST BE NO
GREATER THAN 0.004 PSIG IN ONE MINUTE BEFORE PROCEEDING.
5.4.4. LARGE REFERENCE
5.4.4.1. FOLLOWING A SUITABLE PURGE (SEE ITEM 5.4.1.1), INSTALL THE
MICRO SAMPLE CELL AND SLEEVE WITH TWO MICRO STAINLESS STEEL
BALLS INTO THE CELL HOLDER AND CLOSE THE COVER. PURGE THE
INSTRUMENT FOR AN ADDITIONAL MINUTE TO REMOVE ALL AIR WITHIN IT.
5.4.4.2. OPEN BOTH TOGGLE VALVES I AND II. CLOSE THE GAS IN TOGGLE
VALVE.
5.4.4.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
5.4.4.4. TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL UNTIL A
0.000 PSIG READING IS DISPLAYED ON THE DIGITAL PANEL METER.

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5.4.4.5. TURN THE SELECTOR VALVE TO THE REFERENCE POSITION AND
CLOSE THE GAS OUT TOGGLE VALVE.
5.4.4.6. OPEN THE GAS IN TOGGLE VALVE AND, WHEN THE DIGITAL PANEL
METER READS 19.0 PSIG, CLOSE THE GAS IN TOGGLE VALVE.
5.4.4.7. RECORD THE FIRST STABLE READING AS THE STARTING PRESSURE
AND ENTER THAT READING ON THE INSTRUMENT CHECK SHEET IN APPENDIX
B.1, ITEM B.1.3.7. AS THE STARTING PRESSURE FOR LARGE. THIS WILL SIGNAL
THE BEGINNING OF A 1 MINUTE LEAK TEST.
.
5.4.4.8. AFTER 1 MINUTE HAS ELAPSED, RECORD THE READING AS DISPLAYED
ON THE DIGITAL PANEL METER AND ENTER THAT READING AS PRESSURE
AFTER 1 MINUTE FOR LARGE ON THE INSTRUMENT CHECK SHEET IN
APPENDIX B.1, ITEM B.1.3.7. THE CALCULATED LEAK RATE MUST BE NO
GREATER THAN 0.004 PSIG IN ONE MINUTE BEFORE PROCEEDING.
5.4.5. CELL SECTION
5.4.5.1. FOLLOWING A SUITABLE PURGE (SEE ITEM 5.4.1.1), INSTALL THE
MICRO SAMPLE CELL AND SLEEVE WITH TWO MICRO STAINLESS STEEL
BALLS INTO THE CELL HOLDER AND CLOSE THE COVER. PURGE THE
INSTRUMENT FOR AN ADDITIONAL MINUTE TO REMOVE ALL AIR WITHIN IT.
5.4.5.2. CLOSE ALL THE TOGGLE VALVES.
5.4.5.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
5.4.5.4. TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL UNTIL A
0.000 PSIG READING IS DISPLAYED ON THE DIGITAL PANEL METER. CLOSE THE
GAS OUT TOGGLE VALVE. TURN THE SELECTOR VALVE TO REFERENCE.
5.4.5.5. OPEN THE GAS IN TOGGLE VALVE AND, WHEN THE DIGITAL PANEL
METER READS 19.0 PSIG, CLOSE THE GAS IN TOGGLE VALVE.
5.4.5.6. RECORD THE FIRST STABLE READING AS THE STARTING PRESSURE
AND ENTER THAT READING ON THE INSTRUMENT CHECK SHEET IN APPENDIX
B.1, ITEM B.1.3.7. AS THE STARTING PRESSURE FOR CELL. THIS WILL SIGNAL
THE BEGINNING OF A 1 MINUTE LEAK TEST.
5.4.5.7. AFTER 1 MINUTE HAS ELAPSED, RECORD THE READING AS DISPLAYED
ON THE DIGITAL PANEL METER AND ENTER THAT READING AS PRESSURE
AFTER 1 MINUTE FOR CELL ON THE INSTRUMENT CHECK SHEET IN APPENDIX
B.1, ITEM B.1.3.7. THE CALCULATED LEAK RATE MUST BE NO GREATER
THAN 0.004 PSIG IN ONE MINUTE BEFORE PROCEEDING.
5.4.6. FOUR WAY VALVE SECTION

16
5.4.6.1. FOLLOWING A SUITABLE PURGE (SEE ITEM 5.4.1.1), INSTALL THE
MICRO SAMPLE CELL AND SLEEVE WITH TWO MICRO STAINLESS STEEL
BALLS INTO THE CELL HOLDER AND CLOSE THE COVER. PURGE THE
INSTRUMENT FOR AN ADDITIONAL MINUTE TO REMOVE ALL AIR WITHIN IT.
5.4.6.2. CLOSE ALL THE TOGGLE VALVES.
5.4.6.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
5.4.6.4 TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL UNTIL A
0.000 PSIG READING IS DISPLAYED ON THE DIGITAL PANEL METER.
5.4.6.5. TURN THE SELECTOR VALVE TO THE REFERENCE POSITION AND
CLOSE THE GAS OUT TOGGLE VALVE.
5.4.6.6. OPEN THE GAS IN TOGGLE VALVE AND, WHEN THE DIGITAL PANEL
METER READS 19.0 PSIG, CLOSE THE GAS IN TOGGLE VALVE.
5.4.6.7. RECORD THE FIRST STABLE READING AS THE STARTING PRESSURE
AND ENTER THAT READING ON THE INSTRUMENT CHECK SHEET IN APPENDIX
B.1, ITEM B.1.3.7. AS THE STARTING PRESSURE FOR FOUR WAY. THIS WILL
SIGNAL THE BEGINNING OF A 1 MINUTE LEAK TEST.
5.4.6.8. AFTER 1 MINUTE HAS ELAPSED, RECORD THE READING AS DISPLAYED
ON THE DIGITAL PANEL METER AND ENTER THAT READING AS PRESSURE
AFTER 1 MINUTE FOR FOUR WAY ON THE INSTRUMENT CHECK SHEET IN
APPENDIX B.1, ITEM B.1.3.7. THE CALCULATED LEAK RATE MUST BE NO
GREATER THAN 0.004 PSIG IN ONE MINUTE BEFORE PROCEEDING.
5.5. CALIBRATION
5.5.1. PURGE
5.5.1.1. INSTALL THE SAMPLE CELL YOU ARE INTENDING TO CALIBRATE
(LARGE, SMALL OR MICRO CELL) AND CLOSE THE CELL HOLDER COVER.
5.5.1.2. OPEN THE GAS OUT TOGGLE VALVE AND THE GAS OUT NEEDLE
VALVE.
5.5.1.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION.
5.5.1.4. OPEN BOTH TOGGLE VALVES I AND II.
5.5.1.5. OPEN THE GAS IN TOGGLE VALVE AND ADJUST THE GAS IN NEEDLE
VALVE FOR A 1 PSIG PURGE RATE AS DISPLAYED ON THE DIGITAL PANEL
METER.
5.5.1.6. PURGE THE MULTIPYCNOMETER FOR 5 MINUTES BEFORE
CONTINUING. CLOSE THE GAS IN TOGGLE VALVE WHEN THE PURGE
TIME IS COMPLETED.

17
5.5.2. VRa LARGE CALIBRATION (NO SPHERES, LARGE CELL)
5.5.2.1. PERFORM THE STEPS LISTED IN SECTION 5.5.1 (THE PURGE ROUTINE)
WITH THE LARGE SAMPLE CELL IN THE CELL HOLDER.
5.5.2.2. OPEN THE TOGGLE VALVES I AND II AND CLOSE THE GAS IN
TOGGLE VALVE.
5.5.2.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
5.5.2.4. TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL UNTIL A
0.000 PSIG READING IS DISPLAYED ON THE DIGITAL PANEL METER.
5.5.2.5. TURN THE SELECTOR VALVE TO THE REFERENCE POSITION AND
CLOSE THE GAS OUT TOGGLE VALVE.
.
5.5.2.6. OPEN THE GAS IN TOGGLE VALVE AND, WHEN THE DIGITAL PANEL
METER READS 17.0 PSIG, CLOSE THE GAS IN TOGGLE VALVE.
5.5.2.7. VERIFY THAT THE PRESSURE DISPLAYED ON THE DIGITAL PANEL
METER DOES NOT CHANGE DURING A 10-SECOND PERIOD. TAKE THE aP1
PRESSURE READING ON THE DIGITAL PANEL METER AND ENTER THAT
NUMBER ON THE INSTRUMENT CALIBRATION SHEET IN APPENDIX B.2, ITEM
B.2.3., AS aP1.
5.5.2.8. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION.
5.5.2.9. VERIFY THAT THE NEW PRESSURE DISPLAYED ON THE DIGITAL PANEL
METER DOES NOT CHANGE DURING A 10-SECOND PERIOD. TAKE THE aP2
PRESSURE READING ON THE DIGITAL PANEL METER AND ENTER THAT
NUMBER ON THE INSTRUMENT CALIBRATION SHEET IN APPENDIX B.2, ITEM
B.2.3, AS aP2.
5.5.2.10. CALCULATE THE RATIO aP1/aP2 = aP AND ENTER THIS VALUE AS aP
ON THE INSTRUMENT CALIBRATION SHEET IN APPENDIX B.2, ITEM B.2.3.
5.5.2.11. REPEAT THE STEPS IN SECTIONS 5.5.2.2 TO 5.5.2.11 UNTIL FIVE
CONSECUTIVE aP VALUES FALL WITHIN +/-0.0005 OF EACH OTHER.
NOTE: THE RATIOS CAN BE CALCULATED TO 4 DECIMAL PLACES AND ARE
DIMENSIONLESS, NOT IN PSIG.

18
5.5.3. VCb LARGE CALIBRATION (56.5592 cc SPHERE)
5.5.3.1. INSTALL ONE LARGE 56.5592 cc SPHERE IN THE SAMPLE CELL AND
PLACE THE SAMPLE CELL INTO THE SAMPLE CELL HOLDER. PERFORM THE
STEPS LISTED IN SECTION 5.5.1. (THE PURGE ROUTINE) WITH THE LARGE
CELL CONTAINING THE LARGE SPHERE.
5.5.3.2. OPEN THE TOGGLE VALVES I AND II, AND CLOSE THE GAS IN
TOGGLE VALVE.
5.5.3.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
5.5.3.4. TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL UNTIL A
0.000 PSIG READING IS DISPLAYED ON THE DIGITAL PANEL METER.
5.5.3.5. TURN THE SELECTOR VALVE TO THE REFERENCE POSITION AND
CLOSE THE GAS OUT TOGGLE VALVE.
5.5.3.6. OPEN THE GAS IN TOGGLE VALVE AND, WHEN THE DIGITAL PANEL
METER READS 17.0 PSIG, CLOSE THE GAS IN TOGGLE VALVE.
5.5.3.7. VERIFY THAT THE PRESSURE DISPLAYED ON THE DIGITAL PANEL
METER DOES NOT CHANGE DURING A 10-SECOND PERIOD. TAKE THE bP1
PRESSURE READING ON THE DIGITAL PANEL METER AND ENTER THAT
NUMBER ON THE INSTRUMENT CALIBRATION SHEET IN APPENDIX B.2, ITEM
B.2.7., AS bP1.
.
5.5.3.8. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION.
5.5.3.9. VERIFY THAT THE NEW PRESSURE DISPLAYED ON THE DIGITAL PANEL
METER DOES NOT CHANGE DURING A 10-SECOND PERIOD. TAKE THE bP2
PRESSURE READING ON THE DIGITAL PANEL METER AND ENTER THAT
NUMBER ON THE INSTRUMENT CALIBRATION SHEET IN APPENDIX B.2, ITEM
B.2.7, AS bP2.
5.5.3.10. CALCULATE THE RATIO bP1/bP2 = bP AND ENTER THIS VALUE AS bP
ON THE INSTRUMENT CALIBRATION SHEET IN APPENDIX B.2, ITEM B.2.7.
5.5.3.11. REPEAT THE STEPS IN SECTIONS 5.5.3.2 TO 5.5.3.11 UNTIL FIVE
CONSECUTIVE bP VALUES FALL WITHIN +/-0.0005 OF EACH OTHER.

19
5.5.4. CALCULATION OF VR LARGE AND VC LARGE VOLUMES
5.5.4.1. FILL IN THE CORRESPONDING CALCULATION SHEET ON
APPENDIX B.2., ITEMS B.2.11. AND B.2.12.
VR LARGE = 56.5592 cc [V SPHERE] = 56.5592
(a - 1) - (b - 1) ( a - b )
VC LARGE = VR LARGE × ( a - l )
5.5.5. LARGE SPHERE RUN
5.5.1. INSTALL ONE LARGE 56.5592 cc SPHERE IN THE SAMPLE CELL CUP AND
PLACE BOTH INTO THE CELL HOLDER. ( THIS IS EQUIVALENT TO FILLING THE
LARGE CUP WITH THE SPHERE INDICATED AS THE SAMPLE.) PERFORM THE
STEPS LISTED IN SECTION 5.6.1. (THE PURGE ROUTINE ) WITH THE LARGE CELL
FILLED.
5.5.2. OPEN THE TOGGLE VALVES I AND II AND CLOSE THE GAS IN
TOGGLE VALVE.
5.5.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
5.5.4. TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL UNTIL A
0.000 PSIG READING IS DISPLAYED ON THE DIGITAL PANEL METER. CLOSE THE
GAS OUT TOGGLE VALVE.
5.5.5. TURN THE SELECTOR VALVE TO THE REFERENCE POSITION AND
CLOSE THE GAS OUT TOGGLE VALVE.
5.5.6. OPEN THE GAS IN TOGGLE VALVE AND, WHEN THE DIGITAL PANEL
METER READS 17.0 PSIG, CLOSE THE GAS IN TOGGLE VALVE.
5.5.7. VERIFY THAT THE PRESSURE DISPLAYED ON THE DIGITAL PANEL
METER DOES NOT CHANGE DURING A 10-SECOND PERIOD. TAKE THE P1
PRESSURE READING ON THE DIGITAL PANEL METER AND ENTER THAT
NUMBER ON THE LARGE SPHERE RUN DATA SHEET (APPENDIX C, ITEM C.1.2.).
.
5.5.8. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION.
5.5.9. VERIFY THAT THE NEW PRESSURE DISPLAYED ON THE DIGITAL PANEL
METER DOES NOT CHANGE DURING A 10-SECOND PERIOD. TAKE THE P2
PRESSURE READING ON THE DIGITAL PANEL METER AND ENTER THAT
NUMBER ON THE LARGE SPHERE RUN DATA SHEET (APPENDIX C, ITEM C.1.2.).
5.5.10. CALCULATE VP = VC - VR × ((P1/P2) -1), WITH NUMBERS FOR VC AND
VR TAKEN FROM THE CALIBRATION SECTION. VERIFY THAT THE
CALCULATED VALUES ARE WITHIN 0.4 % OF THE EXPECTED VOLUME OF
56.5592 cc. THE UPPER LIMIT IS 56.7854 cc AND THE LOWER LIMIT IS 56.3330 cc.

20
5.5.6. VRc SMALL CALIBRATION (NO SPHERES, LARGE CELL)
5.5.6.1. PERFORM THE STEPS LISTED IN SECTION 5.5.1 (THE PURGE ROUTINE)
WITH THE LARGE SAMPLE CELL IN THE CELL HOLDER.
5.5.6.2. CLOSE TOGGLE VALVES I AND GAS IN. OPEN VALVE II.
5.5.6.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
5.5.6.4. TURN THE ZERO ADJUSTMENT KNOB ON THE FRONT PANEL UNTIL A
0.000 PSIG READING IS DISPLAYED ON THE DIGITAL PANEL METER. CLOSE THE
GAS OUT TOGGLE VALVE.
5.5.6.5. TURN THE SELECTOR VALVE TO THE REFERENCE POSITION AND
CLOSE THE GAS OUT TOGGLE VALVE.
5.5.6.6. OPEN THE GAS IN TOGGLE VALVE AND, WHEN THE DIGITAL PANEL
METER READS 17.0 PSIG, CLOSE THE GAS IN TOGGLE VALVE.
5.5.6.7. VERIFY THAT THE PRESSURE DISPLAYED ON THE DIGITAL PANEL
METER DOES NOT CHANGE DURING A 10-SECOND PERIOD. TAKE THE cP1
PRESSURE READING ON THE DIGITAL PANEL METER AND ENTER THAT
NUMBER ON THE INSTRUMENT CALIBRATION SHEET IN APPENDIX B.3, ITEM
B.3.3., AS cP1.
5.5.6.8. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL
POSITION.
5.5.6.9. VERIFY THAT THE NEW PRESSURE DISPLAYED ON THE DIGITAL PANEL
METER DOES NOT CHANGE DURING A 10-SECOND PERIOD. TAKE THE cP2
PRESSURE READING ON THE DIGITAL PANEL METER AND ENTER THAT
NUMBER ON THE INSTRUMENT CALIBRATION SHEET IN APPENDIX B.3, ITEM
B.3.3, AS cP2.
5.5.6.10. CALCULATE THE RATIO cP1 / cP2 = cP AND ENTER THIS VALUE AS cP
ON THE INSTRUMENT CALIBRATION SHEETS IN APPENDIX B.3, ITEM B.3.3.
5.5.6.11. REPEAT THE STEPS IN SECTIONS 5.5.5.2 TO 5.5.5.11 UNTIL FIVE
CONSECUTIVE cP VALUES FALL WITHIN +/-0.005 OF EACH OTHER.