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QUANTACHROME INSTRUMENTS MULTIPYCNOMETER Manual

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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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Summary of Contents for QUANTACHROME INSTRUMENTS MULTIPYCNOMETER

  • Page 1: Multipycnometer

    MULTIPYCNOMETER QUALITY ASSURANCE 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...

  • Page 2: Table Of Contents

    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.

  • Page 3: Purpose

    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 ].

  • Page 4: Responsibilities

    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.

  • Page 5: Requirements

    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.
  • Page 6 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).

  • Page 7: Power Checks

    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.

  • Page 8: Alignments

    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”...
  • Page 9 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 set bri to 5.
  • Page 10 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;...
  • Page 11 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.

  • Page 12: Leak Test

    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.
  • Page 13 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.
  • Page 14 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.
  • Page 15 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.

  • Page 16: Calibration

    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.
  • Page 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.
  • Page 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.
  • Page 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 ×...
  • Page 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.
  • Page 21 5.5.7. VCd SMALL CALIBRATION ( NO SPHERES, SMALL CELL) 5.5.7.1. INSTALL ONE SMALL SLEEVE AND ITS SAMPLE CELL CUP INTO THE CELL HOLDER. PERFORM THE STEPS LISTED IN SECTION 5.5.1. ( THE PURGE ROUTINE ) WITH THE CELL EMPTY. 5.5.7.2. CLOSE VALVES I AND GAS IN. OPEN VALVE II. 5.5.7.3.
  • Page 22 5.6.3. SMALL SPHERE RUN 5.6.3.1. INSTALL ONE SMALL SPHERE (7.0699 cc) AND TWO MICRO SPHERES (2.145 cc) IN THE SAMPLE CELL CUP. ( THIS IS EQUIVALENT TO FILLING THE SMALL CUP WITH THE SPHERE INDICATED AS THE SAMPLE.) PLACE THE SAMPLE CELL CUP INTO ITS SLEEVE AND THEN THE SLEEVE INTO THE CELL HOLDER.
  • Page 23 5.6.4. VRe MICRO CALIBRATION (NO SPHERES, MICRO CELL & MICRO SLEEVE) 5.6.4.1. PERFORM THE STEPS LISTED IN SECTION 5.4.1. ( THE PURGE ROUTINE ) WITH THE EMPTY MICRO CELL IN PLACE. 5.6.4.2. CLOSE ALL THE TOGGLE VALVES . 5.6.4.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE.
  • Page 24 5.7.3. TURN THE SELECTOR VALVE ON THE FRONT PANEL TO THE CELL POSITION AND THEN OPEN THE GAS OUT TOGGLE VALVE. 5.7.4. 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.
  • Page 25 5.9. MICRO SPHERE RUN 5.9.1. INSTALL TWO MICRO SPHERES, EACH WITH A VOLUME OF 1.0725 cc IN THE CELL CUP. (THIS IS EQUIVALENT TO FILLING THE MICRO CUP WITH THE SPHERE INDICATED AS THE SAMPLE.) PERFORM THE STEPS LISTED IN SECTION 5.6.1.

  • Page 26: References

    6.0. REFERENCES 6.1. S. LOWELL AND J.E. SHIELDS, “ POWDER SURFACE AREA AND POROSITY”, 3RD ED., CHAPMAN AND HALL, NY (1991). 6.2. QUANTACHROME MULTIPYCNOMETER OPERATION MANUAL, PART NUMBER 05034. 6.3. MECHANICAL ASSEMBLY DIAGRAM BM114-1618-2 ( THREE SHEETS). 6.4. ELECTRICAL ASSEMBLY DIAGRAM BM114-1618-1 (ONE SHEET).
  • Page 27 APPENDIX A A.1. MODIFICATIONS AND REVISIONS. A.1.1. MODIFICATIONS FOR USE WITH ALL MULTIPYCNOMETER MODELS ARE LISTED BELOW. DATE MODEL MODIFICATION APPROVED BY 6/20/95 MVP-2 DIGITAL FRONT PANEL METER D.J.S CHANGED , ONLY AFFECTED THE MODEL 10/29/96 MVP-3 CUT AWAY CELL, ONLY AFFECTED...
  • Page 28 APPENDIX B B.1. INSTRUMENT CHECK SHEET B.1.1 . THIS INSTRUMENT CHECK SHEET IS TO BE FILLED COMPLETELY BY THE TECHNICIAN OR OPERATOR INVOLVED WHEN FULLY TESTING THE MULTIPYCNOMETER. B.1.2.1. OPERATOR B.1.2.2. DATE B.1.2.3. MODEL B.1.2.4. SERIAL NUMBER B.1.3. ADD TICK MARKS TO CONFIRM THAT THE STEPS OUTLINED IN THE SECTIONS INDICATED BELOW HAVE BEEN CARRIED OUT SATISFACTORILY.

  • Page 29: Instrument Calibration Sheet For The Large Cell

    APPENDIX B B.2. INSTRUMENT CALIBRATION SHEET FOR THE LARGE CELL B.2.1. THIS INSTRUMENT CALIBRATION SHEET IS TO BE FILLED COMPLETELY BY THE TECHNICIAN OR OPERATOR INVOLVED WHEN FULLY CALIBRATING THE MULTIPYCNOMETER. B.2.2.1. OPERATOR B.2.2.2. DATE B.2.2.3. MODEL B.2.2.4. SERIAL NUMBER B.2.3.

  • Page 30: Instrument Calibration Sheet For The Small Cell

    VR LARGE × B.3. INSTRUMENT CALIBRATION SHEET FOR THE SMALL CELL B.3.1. THIS INSTRUMENT CALIBRATION SHEET IS TO BE FILLED COMPLETELY BY THE TECHNICIAN OR OPERATOR INVOLVED WHEN FULLY CALIBRATING THE MULTIPYCNOMETER. B.3.2.1. OPERATOR B.3.2.2. DATE B.3.2.3. MODEL B.3.2.4. SERIAL NUMBER B.3.3.
  • Page 31 B.3.5. TOTALc IS THE SUM OF FIVE CONSECUTIVE cP READINGS. ENTER THE SUM AS TOTALc IN SECTION B.3.3. B.3.6. c IS THE AVERAGE OF FIVE CONSECUTIVE cP VALUES. B.3.7. VCd SMALL’S dP1 AND dP2 ARE THE PRESSURES BEFORE AND AFTER EXPANSION RESPECTIVELY.

  • Page 32: Instrument Calibration Sheet For The Micro Cell

    B.4. INSTRUMENT CALIBRATION SHEET FOR THE MICRO CELL B.4.1. THIS INSTRUMENT CALIBRATION SHEET IS TO BE FILLED COMPLETELY BY THE TECHNICIAN OR OPERATOR INVOLVED WHEN FULLY CALIBRATING THE MULTIPYCNOMETER. B.4.2.1. OPERATOR B.4.2.2. DATE B.4.2.3. MODEL B.4.2.4. SERIAL NUMBER B.4.3. VCe MICRO’S eP1 AND eP2 ARE THE PRESSURES BEFORE AND AFTER...
  • Page 33 B.4.7. VCf MICRO’S fP1 AND fP2 ARE THE PRESSURES BEFORE AND AFTER EXPANSION (SECTION 5.5.9.), RESPECTIVELY. ÷ ÷ ÷ ÷ ÷ ÷ f = TOTALf ÷ 5 = B.4.8. COLUMN fP LISTS FIVE CONSECUTIVE PASSES OF ITEMS IN SECTION 5.5.9. THE fP RATIO MUST FALL WITHIN +/-0.0005 OF EACH OTHER BEFORE THEIR SUM CAN BE AVERAGED.

  • Page 34: Sphere Runs' Data Sheets

    COMPLETELY BY THE TECHNICIAN OR OPERATOR INVOLVED AFTER FULLY CALIBRATING THE MULTIPYCNOMETER. NOTE THAT THE WORKING EQUATION FOR THE MULTIPYCNOMETER IS VP = VC-VR [P1/P2], WHERE VP IS THE SPHERE OR SAMPLE VOLUME. C.1.2. LARGE SPHERE RUN (SAMPLE VOLUME VP = 56.5592 cc). DATA ARE TO BE TAKEN FROM SECTION 5.6.2.
  • Page 35 APPENDIX D D.1. SPARE PARTS LIST D.1.1. THIS LIST IS PROVIDED TO ASSIST IN THE ORDERING OF REPLACEABLE PARTS FOR THE MULTIPYCNOMETER. PART NUMBER DESCRIPTION 00131 MVP TRANSDUCER 49077 BALL VALVE 50021 RELIEF VALVE 50045 TOGGLE VALVE 00003 PRINTED CIRCUIT BOARD...
  • Page 36 D.2. ACCESSORY LIST 2.1. THIS LIST IS PROVIDED TO ASSIST IN THE ORDERING OF ACCESSORY PARTS THAT CAN BE USED WITH A MULTIPYCNOMETER. PART NUMBER DESCRIPTION 01500-NIST-LG LARGE CALIBRATION SPHERE MEASURED BY NIST 01500-NIST-SM SMALL CALIBRATION SPHERE MEASURED BY NIST...

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