QUANTACHROME INSTRUMENTS MVP-6DC User manual

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MULTIPYCNOMETER
Instrument Models:
MVP-6DC
MVP-D160E
OPERATING MANUAL
P/N 05034 Rev F
© Quantachrome Instruments, 2012-2014

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QUANTACHROME WARRANTY POLICY
Quantachrome Instruments warrants its instruments to be free from defects in material and workmanship for a
period of one year from date of shipment under normal use and conditions.
For the period commencing with the date of shipment and ending one year later, Quantachrome will, at its
option either repair or replace any part within an instrument that is found by us to be defective in material or
workmanship, without charge to the customer, at our facility or at a customer’s facility if the instrument
purchased is backed by Quantachrome’s on-site warranty as evidenced by the sales contract.
The customer is responsible for all transportation charges to our factory.
Damages during the warranty period resulting from unstable utilities, operator error or unauthorized repairs
will not be covered by this warranty.
Parts purchases are warranted to be free of defects for 90 days from shipping date.
The following limits apply to our warranty:
Glassware, including Dewar flasks, is not covered under this warranty except if damaged during shipment.
Claims for damage during shipping must be made in writing within 10 days of receipt of the goods.
Expendable items are warranted for 90 days for other than glassware breakage. Such items include, but are
not limited to, sample tubes, lamps, fuses, valve plungers, seals, o-rings & other seals, hoses, flexible tubing,
thermocouple vacuum tubes, filters, oils and other fluids.
Products sold by Quantachrome under their own brand name are not warranted by Quantachrome, but our best
effort will be made to secure repair or replacement if found to be defective.
Warranty becomes void in the event of modifications or repairs by persons other than Quantachrome’s service
personnel, unless permission is given in writing for such repairs or modifications. Warranty is also void in the
event of exposure to corrosive atmospheres of any kind.
Prior authorization must be obtained before returning any item to Quantachrome Instruments. Items must be
decontaminated before return to Quantachrome.
Any and all computer program(s), software, firmware, code, data acquisition and/or data reduction methods,
computations, graphical and/or tabular data reporting or presentation methods (collectively referred to as
software) provided with or in or loaded into any part of the instrument or a computer supplied as part of a
Quantachrome Instruments’ instrument are provided “as is”. Quantachrome Instruments warrants the
software will perform substantially in accordance with the accompanying materials for the period of this
warranty. All software is licensed and not sold. Quantachrome Instruments retains all rights to all software.
You may not reverse engineer, decompile, or disassemble the software. You may not distribute or copy the
software, except for the purpose of storing a back-up copy. The exclusive remedy for any software failing to
perform substantially in accordance with the accompanying materials shall be, at Quantachrome’s option, a)
repair or replacement of the software; b) return of the amount paid for the software. You are not entitled to
any damages, including but not limited to incidental, punitive, indirect or consequential damages including
but not limited to loss of profits, business interruption, personal injury, and other pecuniary losses.

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QUANTACHROME INSTRUMENTS’ TERMS AND CONDITIONS OF
SALE
Terms: Acceptance of this order is conditional on agreement by the Buyer to all terms herein.
Buyer’s agreement is assumed unless we are notified to the contrary prior to our invoicing. None of
the provisions, terms and conditions contained in this document may be added to, modified,
superseded or otherwise changed except by a written instrument signed by the Seller’s authorized
representative, regardless of any contrary or additional provisions contained in any purchase order or
other form from the buyer.
FOB Point: The FOB Point is Boynton Beach, FL unless otherwise indicated on our Quotation or
agreed to in writing by an authorized Seller representative.
Payment terms: Terms are net 30 days from date of invoice for established accounts where Seller
has received adequate financial information to warrant extending credit to Buyer. Purchase orders
from customers not meeting with Seller’s financial approval are not accepted under credit terms.
Delivery: Delivery dates are Seller’s best estimate of the time products will be shipped from our
factory and we assume no liability for loss, damage, or consequential damages due to delays. No
liability shall result from delay in performance or non-performance of this agreement, directly or
indirectly caused by fire, explosion, accidents, flood, labor trouble or shortage, war, act of God or
arising from contingencies, happenings, or causes beyond the control of the party affected.
Material Shortages: In the event of inability for any reason to supply the total demands for the
materials specified in this order, Seller may allocate its available supply among any or all
purchasers, as well as departments and divisions of the Seller, on such basis as it may deem fair and
practical, without liability for any failure or performance which may result there from.
Taxes: Buyer shall reimburse Seller for all taxes, excises or other charges which seller may be
required to pay to any government (National, State or Local) upon the sale, production or
transportation of the commodities sold hereunder and amended from time to time.
Proprietary Information: All specifications, data, drawings, designs and software are proprietary
information which are the sole and exclusive property of the Seller and purchaser agrees to retain
any and all such proprietary information as Seller may disclose to him in confidence and not disclose
it to other parties or use it except in inspection and evaluation purposes in connection with a contract
with Seller.

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Software License: Title to all software provided as separate modules or embedded in the Products
("Software") shall remain the property of Quantachrome or Quantachrome's licensors.
Quantachrome grants to Buyer a non-exclusive, limited license to use the Software together with the
Products. Buyer shall not decompile, disassemble or otherwise reverse engineer the Software, and
may create derivative works only to the extent permitted by Quantachrome. Buyer shall not
sublicense, assign, copy, distribute or disclose any portion of the Software to a third party without
the express written consent of Quantachrome. Buyer may transfer or sell its license rights to use the
Software only together with the Products to a transferee, which has accepted this provision of
Quantachrome’s Terms and Conditions of Sale in writing.
Changes: Orders accepted by the Seller cannot be changed or modified in whole or part, except with
the written consent of Seller.
Return Policy: Prior approval must be obtained from an authorized Seller representative to return
any Product. Seller will assign a return authorization number and record the reason for return. Seller
will examine returned part to determine the actual cause, if any, leading to Buyer’s return. If Product
has a manufacturing defect Seller will, at its discretion, repair or replace with like product.
Restockingcharges: Product purchased, under the sole discretion of the Seller, may be returned for
a 20% restocking fee and must be returned within 90 days of date of delivery. Product cannot be
returned if used or modified.
Claims: Claims for shortages or damage must be reported within 10 business days after receipt of
shipment. All claims for loss or damage in transit must be made against the carrier.
Warranty:Quantachrome Instruments warrants all instruments that it manufactures for a period of
twelve months from the date of delivery. This warranty includes all parts and labor. Quantachrome
does not warrant any product against damage from corrosion, contamination, misapplication,
improper specification, or wear and tear and operational conditions beyond the Seller’s control. This
warranty excludes all glassware and expendable items associated with each instrument. Repairs
made during the warranty period are guaranteed until the end of the warranty period or 90 days,
whichever is greater.

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TABLE OF CONTENTS
I. INTRODUCTION 7
II. INSTALLATION AND COMPONENTS 9
Location 9
Mains Power 9
Gas Tank Connections 10
Sample Cells and Sample Cell Holder 10
Toggle Valves 11
Needle Valves 11
Selector Valve 11
Pressure Display and Transducer 11
Pressure Relief Valve 12
Calibration Status 12
RS232 Port 12
III. SAMPLE PREPARATION 13
Purging Method 13
Vacuum Method 13
IV. SAMPLE ANALYSIS 14
Stepwise measurement instructions 14
Density Worksheet 15
V. CALIBRATION 16
Recalibration 16
Calibration Spheres 19
VI. SOURCES OF ERROR 20
Non-ideal gas behavior 20
Diffusion/Absorption 20
Impure gases 20
Insufficiently prepared samples 20
The size of the gas molecule 20

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MULTIPYCNOMETER
CALIBRATION VALUES
LARGE CALIBRATION SPHERE Vcal large = 56.5592 cm3
MICRO CALIBRATION SPHERES (2) 1.0725 cm3each Vcal micro = 2.145 cm3
LARGE SAMPLE CELL VOLUME Vc large = __________cm3
LARGE REFERENCE VOLUME VRef large = __________cm3
SMALL SAMPLE CELL VOLUME Vcsmall = __________cm3
SMALL REFERENCE VOLUME VRef small = __________cm3
MICRO CELL VOLUME Vcmicro = __________cm3
MICRO REFERENCE VOLUME VRef micro = ___________cm3
Model Number ______________ Serial Number ______________

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I. INTRODUCTION
“Pycnometer” is derived from the Greek word pyknos which has long been identified with volume
measurements. The MULTIPYCNOMETER is an instrument specifically designed to measure the
true volume of a variety of solid materials by employing Archimedes’ principle of fluid
displacement and Boyle’s Law of gas expansion. The displaced fluid is a gas which can penetrate the
finest pores to assure maximum accuracy. For this reason helium is recommended since its small
atomic dimension assures penetration into crevices and pores approaching two Ångströms (2 x 10-
10m). Its behavior as an ideal gas is also desirable. Other gases such as nitrogen can also be used,
often with no measurable difference.
It is used to determine the true volume of solid or powder samples by measuring the pressure
difference when a known quantity of gas under pressure is allowed to expand from a precisely
known reference volume into a sample cell holder, also of known volume, containing the sample cell
with sample.
Figure 1 is a flow diagram of the MULTIPYCNOMETER. The shaded area represents the known
reference volume(s) VR. After the system is purged with analysis gas, the valve that admits gas in to
the system is closed, the selector valve between VRand the cell holder VCis turned to connect them,
and the vent valves are opened. The system is now at ambient pressure Paand the state of the sample
cell with sample is defined by
(
)
RT
n
=
V V
Pa
aSC
a
−
(1)
where nais the number of moles of gas occupying the calibrated cell volume (VC) with sample
present of volume (Vs), R is the gas constant and Tais ambient temperature in kelvin.
When the reference volume alone is pressurized above ambient (after isolating it from the sample
cell holder), the state of the reference volume (VR) can be expressed as
RT
n
=
V
Pa
1R
1(2)
where P1represents a pressure above ambient (17 psig, ~120kPa, for example) and n1is the total
number of moles of gas in the reference volume (VR).
When the selector valve is turned again to connect the reference volume to the sample cell holder,
the pressure will fall to a lower pressure P2, given by
(
)
RT
n
+
RT
n
=
V
+
V V
Pa
1
a
aRSC
2
−
(3)

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Substituting into equation (3) Pa(VC– VS)and P1VRfor naRTaand n1RTa, respectively, gives
()
(
)
V
P
+
V V
P
=
V
+
V V
PR
1
SC
a
RSC
2
−
−
(4)
or
()
(
)
(
)
V
P P
=
V V
P P
R
21
SC
a2
−
−
−(5)
Then
V
P PP
P
=
V VR
a2
21
SC −
−
−(6)
Since Pais made to read zero on the digital meter, that is, all pressure measurements are relative
to Pa, equation (6) becomes
V
PP
P
=
V VR
2
21
SC
−
−(7)
or
(
)
[
]
-
P
/
P
V
-
V
=
V21
RCS 1(8)
Equation (8) is the working equation employed with the MULTIPYCNOMETER.

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II. INSTALLATION AND COMPONENTS
Location
Place the MULTIPYCNOMETER on a level surface away from sources of heat and cold such as
radiators, air conditioning vents, direct sunlight, etc.
Mains Power
Ensure that the voltage selector at the rear of the unit matches your local mains supply. The
MULTIPYCNOMETER is designed for operation on 100V, 120V, 220V or 240V, 50/60 Hz. It was
shipped from the factory set for the voltage according to the purchase order which should match the
voltage on the serial number plate at the rear of the unit. If the selector needs to be changed refer to
the diagram below and carefully follow these steps:
1. Make sure the unit is switched OFF and unplug the power cord from its socket on the unit.
2. Pry open the plastic cover by inserting a screwdriver behind the tab on the side away from the
socket.
3. Using long-nosed pliers, gently pull out the wheel located behind the plastic cover.
4. The 4 voltages are printed on the wheel. Re-insert the wheel with the voltage required facing out,
towards you. Then close the plastic cover. Ensure that the voltage visible in the opening in the
plastic cover matches your local mains supply before reconnecting the power cord.

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Gas Tank Connections Tools required: 7/16” wrench (not supplied).
Attach a dual stage gas regulator to a cylinder of analysis gas, usually ultra-high purity helium or
nitrogen. Connect the output of the regulator to the compression fitting on the right side of the
cabinet using the 1/8” copper tubing and nut & ferrule set supplied.
Do not use plastic tubing. If you need to extend the gas supply line always use clean copper (or
stainless steel) tubing with appropriate metal compression fittings.
It will be necessary to obtain an adapter to connect the tubing to the regulator if it does not have a
1/8” Swagelok® brand fitting. A suitable regulator assembly (P/N 01207) complete with shut-off
valve, CGA580 cylinder connector and 1/8” Swagelok® brand outlet fitting is available from
Quantachrome.
Adjust the pressure regulator to slightly above 20 psig (140 kPa). Pressures above 25 psig could
potentially damage the MULTIPYCNOMETER’s pressure transducer.
Check all connections for leaks using soap solution.
Sample Cells and Sample Cell Holder
Three sample cells (stainless steel cups) and two adapter sleeves are supplied with the
MULTIPYCNOMETER. Sample cells are placed in the chamber with the screw cap - the sample
cell holder. To open the sample cell holder, rotate the cap’s outer ring counter-clockwise until it can
be lifted off. To remove the sample cell insert the lift out tool into one of the holes near the top of the
cell and lift it out of the holder.
Sample cells should be removed from the unit before being filled with sample or adding calibration
spheres. Use the largest amount of sample available for best accuracy. If you do not have enough
sample material to fill the large cell (135 cm3) to at least 50% of its volume, use the small cell (20
cm3) and the micro cell (4.5 cm3) for even smaller quantities. The small and micro cells are always
used with the appropriate adapter sleeve.
When calibrating a cell, especially the large cell, do not simply drop the large sphere into the cell but
turn the cell sideways and roll the sphere into it to prevent deforming the cell.
When using the large sample cell, ensure that the horizontal slit(s) near the top of the cell line up
with the vertical groove(s) machined into the cell holder. This ensures that the gas has a free path
into and out of the cell.
Before replacing the cell holder cap make sure that its O-ring1is undamaged, clean, lightly greased2
and is secured in the groove inside the cap. Align the fiduciary mark on the cap with the line on the
cabinet ring; a locating pin on the bottom side of the cap slots into a hole in the top edge of the
sample cell holder. Then rotate the outer ring of the cap clockwise (on the threads of the cell holder)
until metal to metal contact is made.
1 Spare O-rings are sold in packs of two, p/n 51000-032.
2 Use Vacuum Grease P/N 91000-.25 to lubricate O-ring, never petrolatum.