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Micromeritics 1305 Operator's Manual

Multivolume pycnometer
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Model 1305
MultiVolume Pycnometer
(S/N: 801 and higher)
Operator's Manual
Part No. 135-42803-01
March 2001

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Summary of Contents for Micromeritics 1305

  • Page 1 Model 1305 MultiVolume Pycnometer (S/N: 801 and higher) Operator’s Manual Part No. 135-42803-01 March 2001...
  • Page 2 Swagelok is a registered trademark of Crawford Fitting Company. © Micromeritics Instrument Corporation, 2001. All rights reserved.
  • Page 3 MICROMERITICS shall not be liable for consequential or other type damages resulting from the use of any of its products other than the liability stated above. This warranty is in lieu of all other warranties, express or implied, including, but not limited to the implied warranties of merchantability or fitness for use.

  • Page 4: Table Of Contents

    Model 1305 MultiVolume Pycnometer Table of Contents TABLE OF CONTENTS 1. GENERAL INFORMATION Introduction ........1-1 Conventions .
  • Page 5 Table of Contents Model 1305 MultiVolume Pycnometer Pressure Indicator ....... . . 4-4 Fails to Illuminate .

  • Page 6: General Information

    CHAPTER 1 GENERAL INFORMATION • Introduction • Conventions • Equipment Description • Precautions and Intended Use • Specifications...
  • Page 7 Model 1305 MultiVolume Pycnometer Introduction GENERAL INFORMATION This manual describes how to install and operate the Model 1305 MultiVolume Pycnometer. Introduction This manual is divided into chapters and appendices as follows: Chapter 1 Provides a general description of the Model 1305 MultiVolume Pycnometer and its specifications.
  • Page 8 Conventions Model 1305 MultiVolume Pycnometer Conventions This manual uses the symbols shown below to identify notes of importance and warnings. Notes contain information pertinent to the subject matter. Warnings contain information to help you prevent actions which could cause personal injury.
  • Page 9 The sample chamber with the sample present is first charged to a gas pressure of about 20 psig (unit of measure for the Model 1305). Subsequent expansion of this gas charge into a second precisely measured volume which previously was at the same temperature and at zero psig results in a second pressure which be- comes progressively smaller for larger samples.
  • Page 10 Model 1305 MultiVolume Pycnometer Pressure Transducer Sample Chamber VENT FILL RATE VENT RATE Valve Valve Valve Gas In FILL Valve Filter PREP/TEST Valve Over-Pressure Relief Valve <5/>5 Valve <35/>35 Valve Figure 1-2. Schematic Diagram of the Model 1305 Jun 99...
  • Page 11 Precautions and Intended Use Precautions and Intended Use The Multivolume Pycnometer 1305 is designed to measure rapidly the skeletal volume of powders, granules, or any other solid objects having low vapor pres- sures and to permit computation of absolute density when weight information is supplied.

  • Page 12: Specifications

    Specifications Model 1305 MultiVolume Pycnometer Specifications The Model 1305 MultiVolume Pycnometer has been designed and tested to meet the specificaitons provided below. Characteristic Specification ————————— SAMPLE VOLUME ————————— 150 cm Range: Cylindrical sample chamber, 5.080 cm (2.000 in.) diameter x 7.620 cm (3.000 in.) usable depth;...
  • Page 13 Model 1305 MultiVolume Pycnometer Specifications Characteristic Specification ———————————— THROUGHPUT ———————————— Up to 15 samples per hour when sample preparation not required. Duplication of measurement requires less than two minutes for sample already in chamber. —————————— UTILITIES/SUPPLIES —————————— Accommodates to standard power mains worldwide.
  • Page 14 Specifications Model 1305 MultiVolume Pycnometer Characteristic Specification —————————————— CABINET —————————————— Physical: 31.1W x 18.7H x 38.1D cm (12.25W x 7.36H x 15.0D in.) Weight: 7.9 kg (17.4 lbs) Jun 99...

  • Page 15: Installation

    CHAPTER 2 INSTALLATION • Unpacking and Inspection • Selecting the Location • Selecting the Voltage • Gas Supply...

  • Page 16: Equipment Damage Or Loss During Shipment

    Equipment Return Micromeritics strives to ensure that all items arrive safely and in working order. Occasionally, due to circumstances beyond our control, equipment is received which is not in working condition. When it is necessary to return equipment...

  • Page 17: Selecting The Location

    Model 1305 can be operated. The Model 1305 is designed to operate with either 100, 120, 220 or 240 VAC at 50 or 60 Hz. Voltage selection and fusing are made at the power connector which is lo- cated on the right side panel of the unit.
  • Page 18 Model 1305 MultiVolume Pycnometer Selecting the Voltage Pull the voltage selector card straight out of the power connector housing. Figure 2-2. Removing Voltage Selector Card Orient the voltage selector card so that the desired voltage is indicated at the bottom. Orient the indicator pin so that it points upward as shown in the fol- lowing illustration.
  • Page 19 Selecting the Voltage Model 1305 MultiVolume Pycnometer Fuse the input power line according to local safety practices. The input power connector can be used with either a single-fuse arrangement or a dou- ble-fuse arrangement, as shown in the following illustration.
  • Page 20 Model 1305 MultiVolume Pycnometer Selecting the Voltage The fuses used in the pycnometer must be identical in type and rating to that specified. Use of other fuses could result in electrical shock and/or damage to the pycnometer. c. Insert appropriate fuse(s) for the input power source. Refer to the chart below for the appropriate fuse rating.

  • Page 21: Gas Supply

    The regulator outlet should be attached with metal tubing to the MultiVolume Pycnometer 1305 on the righthand side of the instrument to the fitting closest to the power entranc; a roll of copper tubing with fittings is sup- plied in the accessory kit for this purpose.

  • Page 22: Operation

    CHAPTER 3 OPERATION • Controls and Components • Startup • Preparing and Weighing the Sample • Performing an Analysis • Calculating the Sample Volume, Density, and Specific Volume • Verifying Calibration • Calibrating the Analyzer • Turning Off the Analyzer...

  • Page 23: Controls

    Controls and Components Before operating the Model 1305 Pycnometer, you should become familiar with its controls and components. All operating controls for the Model 1305 Pycnome- ter are on the front panel (shown in the following illustration). The gas, vacuum, and power connections are located on the right side panel.
  • Page 24 Controls and Components Model 1305 MultiVolume Pycnometer ZERO adjustment Allows you to zero the pressure reading following the knob venting of the internal volumes to the atmosphere This control is a 10-turn precision potentiometer allow- ing you to set the zero to the nearest 0.001 psig with a range of more than ±...
  • Page 25 Model 1305 MultiVolume Pycnometer Controls and Components FILL RATE Controls the rate of pressure build when charging the control valve sample chamber or the flow rate when purging a sam- ple during preparation. A judicious balance of the ap- plied pressure (say, 22 psig) along with this setting...

  • Page 26: Components

    120 cm since it must be smaller than the chamber diameter. Sample chamber Accuracy of the MultiVolume Pycnometer 1305 tends insert to be a fixed fraction of the maximum sample cham- ber volume whether filled with sample or not. Sample...
  • Page 27 This transducer type has been chosen for its excellent linearity, a factor es- sential to the accurate operation of the Model 1305 MultiVolume Pycnometer. Jun 99...
  • Page 28 Controls and Components Model 1305 MultiVolume Pycnometer Overpressure Relief Provided for protection against damage to the instru- Valve ment. The overpressure relief valve is connected di- rectly at the gas input connection and is set at the factory to open when the pressure reaches 25 ±1 psig.
  • Page 29 Model 1305 MultiVolume Pycnometer Controls and Components DC power supply The DC power supply is located in the electronics compartment and is accessible by removing the rear panel (detach power cord first). It is a standard OEM open-frame unit wired to deliver +24 VDC and +5 VDC to power the transducer and pressure display, re- spectively.

  • Page 30: Startup

    Startup Model 1305 MultiVolume Pycnometer Startup The following procedure should be followed when the Multivolume Pycnometer 1305: • is being used for the first time • has not been used for several days Before beginning this procedure, ensure that the gas supply has been con- nected and that the proper voltage is being supplied to the analyzer.
  • Page 31 Model 1305 MultiVolume Pycnometer Startup If analysis is to be performed in the 150-cm range and an insert is in the chamber, perform the following steps to remove it: a. Place the VENT valve in the OPEN position, then turn the VENT RATE control several turns counterclockwise to open it.
  • Page 32 Startup Model 1305 MultiVolume Pycnometer Insert in Sample Nominal Sample Chamber Valve Orientation Volume (cm3) Under 5 5 to 35 35 to 150 Figure 3-1. Pycnometer Settings for Optimum Results 17. Place the PREP/TEST valve in the PREP position. The instrument is now ready to run samples.

  • Page 33: Preparing And Weighing The Sample

    Model 1305 MultiVolume Pycnometer Preparing and Weighing the Sample Preparing and Weighing the Sample Sample preparation consists of: • obtaining a representative sample of the material • removing any vapors (especially water) which would interfere with the pressure ratios measured by the instrument •...

  • Page 34: Performing An Analysis

    Performing an Analysis Model 1305 MultiVolume Pycnometer Performing an Analysis The following step-by-step procedure assumes that the >5/<5 valve and the >35/<35 valve have been set to the desired range, that the matching insert is in place or available, and that the matching sample cup contains the sample to be analyzed.
  • Page 35 Model 1305 MultiVolume Pycnometer Performing an Analysis 14. Place the PREP/TEST valve in the TEST position. 15. Allow the pressure to fall to zero and stabilize, correcting the pressure dis- play with the ZERO control as necessary. 16. Place the PREP/TEST valve in the PREP position, ensuring that the zero does not shift.

  • Page 36: Calculating The Sample Volume, Density, And Specific Volume

    Calculating the Sample Volume, Density, and Specific Volume Model 1305 MultiVolume Pycnometer Calculating the Sample Volume, Density, and Specific Volume The general equation for computing the sample volume is − ⁄ P − 1 SAMP CELL where = the sample volume to be found,...

  • Page 37: Verifying Calibration

    Model 1305 MultiVolume Pycnometer Verifying Calibration Specific volume is defined as the volume per unit weight and is computed as SAMP SAMP ρ SAMP SAMP where = sample specific volume. SAMP Verifying Calibration Two quick checks may be made to determine if the instrument needs to be recali- brated.

  • Page 38: Calibrating The Analyzer

    Model 1305 MultiVolume Pycnometer Calibrating the Analyzer Definition of Volumes to be Calibrated Illustrated here is a schematic diagram of the Multivolume Pycnometer 1305 with labels added to facilitate the discussion which follows. Refer to it as the follow- ing is read.
  • Page 39 Model 1305 MultiVolume Pycnometer Calibrating the Analyzer The following six calibrated volumes must be known for each instrument before sample runs can be made: The sample cell and void volume between the FILL valve and the CELL5 VENT valve when the PREP/TEST valve is in the PREP position,...

  • Page 40: Calibration Procedure

    Calibrating the Analyzer Model 1305 MultiVolume Pycnometer Calibration Procedure This procedure measures V , and V CELL5 CELL35 CELL150 EXP5 EXP35 EXP150 as the average of three repeated determinations. A data sheet is provided in Ap- pendix B from which results can be computed by using the calculator workshee also provided in Appendix B.

  • Page 41: Turning Off The Analyzer

    Turning Off the Analyzer Perform the following steps to properly shut down the Model 1305 Pycnometer: Remove any sample from the sample chamber and replace the sample cap. Place the >5/<5 valve in the >5 position and the >35/<35 valve in the >35 position.

  • Page 42: Troubleshooting

    CHAPTER 4 TROUBLESHOOTING • Unstable Pressures • Nonreproducible Results • Incorrect Results • Pressure Indicator • Slow Return to Zero Pressure Upon Venting...

  • Page 43: Falling Pressures

    Model 1305 Multivolume Pycnometer Unstable Pressures TROUBLESHOOTING Perform the checks and tests described in this section before seeking further assis- tance. Contact your local service representative or the factory when unsuccessful in resolving the difficulty. Unstable Pressures Falling Pressures Falling temperatures or rising ambient pressure can cause the indicated pressure to continue to fall beyond the expected transients following filling and expansion.

  • Page 44: Rising Pressures

    Nonreproducible Results Model 1305 Multivolume Pycnometer Many samples such as organic materials or closed cell foam plastics allow helium or other gases in the initial gas charge to slowly diffuse into the interior of the sample. To determine whether the sample is responsible for any discrepancy, re- move the sample and re-test with the chamber empty.

  • Page 45: Incorrect Results

    Model 1305 Multivolume Pycnometer Incorrect Results Purging is important to remove all air following opening and reclosing of the sam- ple chamber. Air, especially moist air, behaves differently than helium or dry ni- trogen and will cause the sample results to vary.

  • Page 46: Pressure Indicator

    Pressure Indicator Model 1305 Multivolume Pycnometer Samples of high specific surface area may contribute an error due to a layer near the surface that is partly depleted of gas molecules termed the annulus volume. Volume errors in the range of 0.005 cm...

  • Page 47: Slow Return To Zero Pressure Upon Venting

    Model 1305 Multivolume Pycnometer Slow Return to Zero Pressure Upon Venting Slow Return to Zero Pressure Upon Venting The VENT RATE control may be set too far clockwise. Increase the flow rate by turning it counterclockwise one or more turns.

  • Page 48: Ordering Information

    CHAPTER 5 ORDERING INFORMATION...
  • Page 49 Model 1305 MultiVolume Pycnometer Ordering Information ORDERING INFORMATION Accessories for the Model 1305 MultiVolume Pycnoemter can be ordered through our Customer Order Entry Department, (707) 662-3636. Please use the informa- tion provided below. Part Number Description 004-16006-00 Vacuum grease, 25 grams 003-51135-00 Fuse, 3 AG, 0.5 A, Slow-Blow, for 100/120 V mains...
  • Page 50 APPENDIX A THEORY...
  • Page 51 Appendix A THEORY The Multivolume Pycnometer 1305 is a gas displacement pycnometer, a type of instrument which measures the volume of solid objects of irregular or regular shape whether powdered or in one piece. A greatly simplified diagram of the in- strument is shown in Figure A1-1.
  • Page 52 Appendix A Model 1305 MultiVolume Pycnometer When the valve is opened, the pressure will fall to an intermediate value, P2, and the mass balance equation becomes ) = n CELL SAMP Substituting from equations (1) and (2) into (3): ) = P...
  • Page 53 SAMP CELL −1 Equation (12) then becomes the working equation for the MultiVolume Pycnome- ter 1305. Calibration procedures are provided to determine V and V CELL the pressures are measured by a gauge pressure transducer. Provisions are made for conveniently charging and discharging gases at controlled rates, for optimizing...
  • Page 54 APPENDIX B FORMS...
  • Page 55 MultiVolume Pycnometer 1305 Sample Data Sheet Sample Identification: __________________________________________________________________ ____________________________________________________________________________________ Gross Weight: ______________ Full Scale Range: ______________ Cup Weight: ______________ Minutes Purge: ______________ Net Weight: ______________ Minutes Vacuum: ______________ ______________ ______________ CELL − SAMP CELL − 1 SAMP ______________ _______________...
  • Page 56 Data Sheet for Internal Volume Calibration MultiVolume Pycnometer 1305 Pressures = psig; Volumes = cm 5-cm Range (empty sample cup) in place) CALIB5 ____________ ___________ P2 ____________ _________________ ___________ P1 ___________ P2 ____________ _________________ ___________ P1 ___________ P2 ____________ _________________...
  • Page 57 MultiPycnometer 1305 Calibration Worksheet for Calculator Page 1 of 1...
  • Page 58 APPENDIX C SAMPLE RESULTS COMPUTATION PROGRAM...
  • Page 59 Model 1305 MultiVolume Pycnometer Appendix C SAMPLE RESULTS COMPUTATION PROGRAM Jun 99...
  • Page 60 APPENDIX D DERIVATION OF CALIBRATION EQUATIONS...
  • Page 61 Appendix D DERIVATION OF CALIBRATION EQUATIONS Prior to running samples on the MultiVolume Pycnometer 1305, the volume of the sample cell and the expansion volume must be known. The derivation that fol- lows permits these internal volumes to be measured with respect to a removable, accurately known standard volume.
  • Page 62 Appendix D Model 1305 MultiVolume Pycnometer Substitution of equation (3) into equation (2) yields  − P  − V ) = P ∗ (V − V ∗ (V ) + P ∗ V   CELL CELL CALIB CALIB CELL ...
  • Page 63 INDEX...
  • Page 64 Model 1305 MultiVolume Pycnometer Index INDEX >35/<35 valve, 3-2 FILL RATe valve, 3-3 >5/<5 valve, 3-2 FILL valve, 3-2 Filter, 3-6 Forms, A-3 Accessories, ordering, 5-1 Analysis performing, 3-12 theory, A-1 regulator, 2-6 Analyzer regulator, attaching to analyzer, 2-6 calibrating, 3-16, 3-17, 3-18...
  • Page 65 Index Model 1305 MultiVolume Pycnometer Reproducibility, 4-2 Warnings, 1-2 Sample Zero cup, 3-4 adjustment, 3-2 preparation, 3-11 offset, 3-15 results computation, C-1 pressure, 4-5 volume, specifications, 1-6 Sample chamber, 1-3, 3-4 cap, 3-5 cleaning, 3-8 insert, 1-6, 3-4 insert, installing, 3-8...

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