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Micromeritics FlowSorb III 2305 Operator's Manual

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FlowSorb III 2305/2310
for determining
Single Point and Multipoint Surface Area
Operator's Manual
231-42801-01
March 2012

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Summary of Contents for Micromeritics FlowSorb III 2305

  • Page 1 FlowSorb III 2305/2310 for determining Single Point and Multipoint Surface Area Operator’s Manual 231-42801-01 March 2012...
  • Page 2 © Micromeritics Instrument Corporation, 2001-2012. All rights reserved. Printed in U.S.A.

  • Page 3: Table Of Contents

    FlowSorb III 2310 ......1-5 FlowSorb III 2305 ......1-6 Principle of Operation .
  • Page 4 Analysis ........3-7 FlowSorb III 2305 ......3-8 FlowSorb III 2310 .

  • Page 5: General Information

    CHAPTER 1 GENERAL INFORMATION Introduction • Conventions • Intended Use and Precautions • Description • Principle of Operation • Basic Construction • Components and Controls • Specifications •...
  • Page 7 FlowSorb III Introduction GENERAL INFORMATION Introduction This manual describes the installation and operation of the FlowSorb III; its con- tents are organized as follows: Chapter 1 General Information. Provides a general description of the FlowSorb III, its features, safety precautions, and specifications. Chapter 2 Installation.

  • Page 8: Intended Use

    BET technique (see Appendix A). The FlowSorb III 2310 is automatic and requires no operator intervention other than preparing, installing, and removing the sample. The FlowSorb III 2305 is manually operated. Both models measure with diminishing effectiveness the physical properties of ma- terials which have appreciable vapor pressures, i.e., materials which slowly evapo-...

  • Page 9: Precautions

    FlowSorb III Intended Use and Precautions Precautions Read all of the precautions contained in this section and observe them at all times when operating the FlowSorb III. General • Certain solids when heated give off corrosive vapors. Such vapors can damage instrument components.

  • Page 10: Dewar

    Intended Use and Precautions FlowSorb III Dewar Always handle dewars with care. Any product incorporating a vacuum is a potential safety hazard and should be treated with caution. Always observe the precautions listed below. We recommend the following be observed when handling dewars containing lique- fied gases: •...

  • Page 11: Description

    FlowSorb III Description Description The FlowSorb III is available in two models: the FlowSorb III 2305 and the FlowSorb III 2310. The FlowSorb III provides single-point and multipoint analy- ses, as well as the capability of reporting desorption isotherms. Adsorption iso- therms can also be reported if using the FlowSorb 2305.

  • Page 12: Flowsorb Iii 2305

    Dewar Platform Release Button The FlowSorb III 2305 reports adsorption and desorption measurements. This model requires the operator to place the Dewar on the Dewar tray and move it up about the sample for analysis to begin. After adsorption is complete, the opera- tor is required to remove the Dewar and warm the sample to room temperature, after which the desorption measurement is reported.

  • Page 13: Principle Of Operation

    FlowSorb III Principle of Operation Principle of Operation The surface area of granulated and powdered solids or porous materials is meas- ured with the FlowSorb III by determining the quantity of a gas that adsorbs as a single layer of molecules, a so-called monomolecular layer, on a sample. This ad- sorption is done at or near the boiling point of the adsorbate gas.

  • Page 14: Basic Construction

    Basic Construction FlowSorb III Basic Construction Functionally, the FlowSorbs III 2305 and 2310 are identical. The FlowSorb III 2305 requires the operator to submerge the sample in cryogenic liquid to induce adsorption, then to remove the cryogen and warm the sample for desorption. This operation is automatic when using the Flowsorb III 2310.
  • Page 15 FlowSorb III Basic Construction Electrical and electronic components include: (1) an on/off power switch, univer- sal power entrance, and fuse block; (2) a power supply; (3) a thermal conductiv- ity sensor and amplifier circuit; (4) a conductivity cell output linearization circuit; (5) a heating mantle temperature setting and feedback control system;...

  • Page 16: Components And Controls

    Components and Controls FlowSorb III Components and Controls This section provides a brief description of the use, manipulation, and function of major components and controls of the FlowSorb. Sample Tube Glass tubes in a variety of generally U-shaped configurations are used to hold the sample.

  • Page 17: Heating Mantle

    • FlowSorb III 2305: The Dewar is supported by a hinged platform. The platform hangs down when not in use. The Dewar is manually brought up around the sample and the platform swung upward where it locks into place.

  • Page 18: Instrument Display

    Clear SA Display pushbutton Not included on the FlowSorb III 2305 The signal chosen for display can be shifted at any time in any sequence without detriment to the other signals. Surface area information and gas volume data, whether displayed or not, are retained after a test is completed until the Clear SA Display button to the left of the meter is depressed.

  • Page 19: Threshold

    FlowSorb III Components and Controls Threshold Threshold indicator The Threshold indicator lamp to the left of the display meter flashes when the accumulated adsorption or desorption signal is greater than the threshold level. The more rapid the flashing, the greater the magnitude of the signal. This lamp is designed to begin indicating accumulation of signals as follows: •...

  • Page 20: Septum

    Specifications FlowSorb III Two gas flow paths, labeled Short and Long, are provided downstream of the sample Test position. The purpose of both is, upon removal of the liquid nitro- gen, to delay the arrival at the detector of the nitrogen-rich gas (created by sam- ple desorption) long enough for the flow rate to return to normal.

  • Page 21: Specifications

    FlowSorb III Specifications Specifications The FlowSorb III has been designed and tested to meet the specifications pro- vided below. Feature Specification ————— SAMPLE PARAMETERS ————— Surface Area Minimum 0.1 m Maximum 280 m Specific Surface Area Minimum: Approximately 0.01 m Maximum: Limited only by weighing accuracy of smallest sample...
  • Page 22 Specifications FlowSorb III Feature Specification ————— SUPPLIES ————— Gas: Mixtures, with helium, of nitrogen, argon, krypton, carbon dioxide, ethane, n-butane, and other non-corrosive gases. A mixture of 30% and 70% He is recommended for single- point analyses. Mixtures of He and approximately 5, 12, 18, and 24% N suggested for multipoint use.

  • Page 23: Installation

    CHAPTER 2 INSTALLATION • Unpacking and Inspecting the Equipment • Selecting the Location • Selecting the Input Power • Connecting the Gas Supply • Installing and Removing a Sample Tube • Installing a Heating Mantle • Using a Cold Bath...
  • Page 24 Specifications FlowSorb III 1-18 Aug 00...

  • Page 27: 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 28: Selecting The Location

    Reference the sales order or purchase order, and provide the date that the equipment was received. Notify the Micromeritics Service Department of the defect and request ship- ping instructions. The service department will assign a Returned Materials Authorization (RMA) number. Write the RMA number on the outside of the shipping carton.

  • Page 29: Selecting The Input Power

    FlowSorb III Selecting the Input Power Selecting the Input Power All instruments leave the factory set for 120 VAC and with the line fuse re- moved. The correct setting of the universal power entrance must be checked and the appropriate fuse installed before the FlowSorb can be operated. The FlowSorb is designed to operate with 100, 120, 220, or 240 VAC at 50 or 60 Hz.
  • Page 30 Selecting the Input Power FlowSorb III 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. Indicator Pin Voltage Insert the voltage selector card into the power connector housing with the edge containing the desired voltage first and with the printed side facing the power ON/OFF switch.
  • Page 31 FlowSorb III Selecting the Input Power Fuse the power line according to local safety practices. The double-fuse arrangement requires 20-mm fuses. Fuse Fuse Block Retaining Screw Cover Jumper Bar Fuses Fuse Block Fuse Block Fuse Cover Cover SINGLE-FUSE ARRANGEMENT DOUBLE-FUSE ARRANGEMENT The power cord must be disconnected from the analyzer when installing or replacing fuses.
  • Page 32 Selecting the Input Power FlowSorb III b. If the fuse block is positioned properly for the desired fusing, proceed to Step c. If the fuse block is not positioned properly: 1) Remove the fuse block retaining screw. 2) Lift the fuse block from the cover. 3) Rotate the fuse block.

  • Page 33: Connecting The Gas Supply

    Whatever the gas mixture or its source, it should be regulated to a pressure of at least 0.11 MPa (15 psig) by a reliable, leak-tested regulator. Suitable regulators are available from Micromeritics (refer to Chapter 5 for ordering information). Some commercial regulators incorporate internally a lubricant that can mi- grate and contaminate downstream systems.
  • Page 34 Connecting the Gas Supply FlowSorb III Bottle Shut-off Valve Two-Stage Pressure Reducing Regulator Shut-off Valve Nut Brass Reducer Fitting Gas Bottle Regulator Shut-off Valve Pressure Control Copper Tubing Knob Figure 2-1. Typical Gas Pressure Regulator Assembly Tighten the regulator shut-off valve nut. Do not over-tighten the fittings.

  • Page 35: Installing And Removing A Sample Tube

    FlowSorb III Installing and Removing a Sample Tube Attach the other end of the copper tubing to the gas fitting on the side of the instrument. Safety demands that pressurized gas cylinders be securely fastened to a rigid support. Installing and Removing a Sample Tube Glass, U-shaped sample tubes are used to hold the sample for analysis.

  • Page 36: Installing A Heating Mantle

    Installing a Heating Mantle FlowSorb III Installing a Heating Mantle A heating mantle is used on a sample tube to assist in maintaining a specified temperature. Heating mantles should be used only on samples being degassed (in the Degas position). Slide the heating mantle upward around the sample tube.

  • Page 37: Using A Cold Bath

    FlowSorb III Using a Cold Bath Using a Cold Bath Liquid argon, liquid oxygen, dry ice and acetone, ice water, and various other slush baths prepared from low melting point liquid solvents partially frozen by mixing with liquid nitrogen may be employed. Liquid nitrogen is most frequently employed.

  • Page 39: Operation

    CHAPTER 3 OPERATION • Preparing the FlowSorb for Operation • Degassing the Sample • Performing a Single-Point Surface Area Measurement • Performing a Multipoint Surface Area Measurement • Preparing the FlowSorb for Idle Periods...
  • Page 41 FlowSorb III Preparing the FlowSorb for Operation OPERATION Both FlowSorb III models permit the measurement of surface area by a single- point and multipoint determination. It is essential that you become familiar with the single-point test before attempting a multipoint analysis. Preparing the FlowSorb for Operation For best results, the FlowSorb should be free of air before performing analyses.
  • Page 42 Preparing the FlowSorb for Operation FlowSorb III Open the Toggle Switch on the lower right side of the FlowSorb to admit gas. Toggle Switch To Gas Source 6. Using the Flow Adjustment Valve Knob, adjust the flow until the float is centered on or near the calibration mark on the flowmeter tube.
  • Page 43 FlowSorb III Degassing the Sample Degassing the Sample Surface areas can be measured reliably with as little as 0.1 m of total sample sur- face or as much as 280 m . However, results are most accurately and quickly de- termined if sample quantity is adjusted to fall within 0.5 to 25 m range.

  • Page 44: Degassing Considerations

    (For further insight on establishing degassing parameters, con- tact your local Micromeritics sales engineer and request Application Note No. 121, Establishing Sample Degassing Conditions for the FlowSorb.)

  • Page 45: Performing A Single-Point Surface Area Measurement

    FlowSorb III Performing a Single-Point Surface Area Measurement Performing a Single-Point Surface Area Measurement Calibration The FlowSorb III should be calibrated at the start of each 8-hour operational period. Calibration is accomplished by injecting a precise volume of a gas mix- ture into the instrument through a septum using a syringe and needle.
  • Page 46 Performing a Single-Point Surface Area Measurement FlowSorb III FlowSorb 2310: Press the Reset button to lower the Dewar tray to its low- est postion FlowSorb 2305: Press the release tab to the right of the Dewar tray to allow the tray to hang down. Fill a 1-mL precision syringe to 1 mL with nitrogen gas: a.

  • Page 47: Analysis

    FlowSorb III Performing a Single-Point Surface Area Measurement 15. Inject the gas at a moderate rate. Withdraw the needle when the syringe is completely discharged. After approximately one minute (five minutes for Long Path), the Thresh- old light begins to flash and the indicator starts to accumulate surface area information.

  • Page 48: Flowsorb Iii 2305

    FlowSorb III 2310 or 2305; advance to the appropriate set of instructions and proceed accordingly. FlowSorb III 2305 Raise the Dewar of liquid nitrogen about the sample and lift up on the Dewar tray until it locks into position; this starts the analysis.

  • Page 49: Flowsorb Iii 2310

    FlowSorb III Performing a Single-Point Surface Area Measurement Special sample tubes such as those having ground glass joints must be warmed with care as they are more subject to stress development which can lead to breakage. Continue the warming procedure until the flowmeter float returns to its nor- mal level.
  • Page 50 Performing a Single-Point Surface Area Measurement FlowSorb III Record the desorption value along with other sample information. This value represents the sample surface area. The indicated number divided by the sam- ple weight (in grams) is the sample specific surface area in square meters per gram.

  • Page 51: Performing A Multipoint Surface Area Measurement

    FlowSorb III Performing a Multipoint Surface Area Measurement Performing a Multipoint Surface Area Measurement The startup and sample preparation for multipoint analysis procedures are identi- cal to the single-point method except that a multigas manifold is needed to facili- tate shifting among different gas mixtures. Calibration Calibration should be performed at the start of each 8-hour operational period.
  • Page 52 Performing a Multipoint Surface Area Measurement FlowSorb III Use the Coarse and Fine Zero knobs to zero the instrument. Observe the display for a few minutes to establish system stability. A change of no more than 0.01 should be achieved. The two primary factors leading to excessive instability are: •...
  • Page 53 FlowSorb III Performing a Multipoint Surface Area Measurement 10. Record the reading for subsequent use. Each valve on the Multigas Manifold has its own erasable tab for recording its calibration information. It is also recommended that you record the nitro- gen composition of the gas bottle connected to each valve on the tab so that it is readily available when needed.

  • Page 54: Analysis

    A multipoint analysis can be conducted as a series of single-point steps using either the FlowSorb III 2305 or 2310, progressing from lower to higher nitrogen gas concentrations. After each concentration is established in the FlowSorb, the in- strument is adjusted appropriately for the new gas mixture, and the adsorbed gas volume is measured.

  • Page 55: Calculating The Result

    FlowSorb III Performing a Multipoint Surface Area Measurement Calculating the Result Appendix A gives the basic theory and pertinent equation of the multipoint calcu- lation. Table 3.3 formalizes the procedure beginning on the left and proceeding to the right using the experimental data in Table 3.2. Table 3.3.
  • Page 56 Performing a Multipoint Surface Area Measurement FlowSorb III For purposes of comparison, a single-point specific surface area of 73.8 m /g was obtained for this same material using a gas composition of 30.017% N and the remainder helium. Figure 3.2. Example Plot 3-16 Mar 2012...

  • Page 57: Preparing The Flowsorb For Idle Periods

    FlowSorb III Preparing the FlowSorb for Idle Periods Preparing the FlowSorb for Idle Periods If the FlowSorb is to be inoperative or unattended for a period long enough for the liquid nitrogen in the Cold Trap Dewar to evaporate (or the dry ice to evapo- rate from the dry ice acetone slurry), remove the Dewar and U-tube so that impu- rities are not released into the system.

  • Page 59: Troubleshooting And Maintenance Troubleshooting

    CHAPTER 4 TROUBLESHOOTING AND MAINTENANCE Troubleshooting • Replacing the Septum •...

  • Page 61: Detector Drift

    • how you can resolve them • instructions on replacing the septum Contact your local Micromeritics service representative if additional assistance is required. Troubleshooting Detector Drift Some detector drift when first turning on the power is normal and to be ex- pected.

  • Page 62: Low Results On X10 Range

    Troubleshooting FlowSorb III Incompletely degassed samples cause detector drift and offset because contaminants can still be flushed from the sample at room temperature. Such drift and offset will cease once the sample is immersed in liquid nitrogen. Leaks caused by a worn septum; always use a good septum. Replace the septum periodically;...

  • Page 63: Non-Reproducible Calibrations

    FlowSorb III Troubleshooting Non-Reproducible Calibrations A damaged and leaking septum should be eliminated as the first possible cause of non-reproducible calibrations. Replace the septum with a new one if there is any doubt as to its integrity. (Refer to Replacing the Septum in this chapter.) The knurled nut which retains the septum should be finger-tightened.

  • Page 64: Surface Area Display Not Clearing To Zero

    Troubleshooting FlowSorb III Surface Area Display Not Clearing to Zero Temperature changes and aging of components may cause the surface area dis- play to register a number slightly different from zero when it is cleared. To cor- rect this condition: Remove the instrument rear panel, being careful not to contact any of the electrical leads in the lower portion of the instrument.

  • Page 65: Display And Indicators Fail To Illuminate

    Lodged Flowmeter Float Fine particles that escape filter entrapment, as well as accumulated vapor deposi- tion can cause the ball float to become lodged in the glass tube of the flowmeter. Contact your local Micromeritics service representative if this occurs. Aug 00...

  • Page 66: Replacing The Septum

    Replacing the Septum FlowSorb III Replacing the Septum The septum is installed at the Inject port and is held into place by a knurled nut. A septum usually requires replacing after approximately 100 injections when us- ing the 1-mL syringe and approximately 20 injections when using the 10-mL syr- inge.

  • Page 67: Ordering Information

    CHAPTER 5 ORDERING INFORMATION...
  • Page 69 ORDERING INFORMATION Components and accessories can be ordered by: • contacting our Customer Service Department at 770/662-3636 • accessing our web site at http://www.micromeritics.com When ordering, please use the information provided below. Part Number Description 230-62804-00 Multigas Manifold, allows attachment of multiple gases for multipoint analysis.
  • Page 71 APPENDIX A THEORY...
  • Page 73 FlowSorb III Appendix A THEORY One form of the well-known BET equation* that describes the adsorption of a gas upon a solid surface is (P/P )/V[1-(P/P )] = 1/(V C)+[(C-1)/(V C)]P/P where = the volume (at standard temperature and pressure, STP) of gas adsorbed at pressure P = the saturation pressure which is the vapor pressure of liquified gas at the adsorbing temperature...
  • Page 74 Appendix A FlowSorb III which rearranges to = V[1-P/P Another way of arriving at the same result is by recognizing that the term 1/(V C) of equation 1 is generally small. Taking it as insignificant changes the slope, and hence the value of V and the sample surface area as calculated by equation 2, only a small amount.
  • Page 75 FlowSorb III Appendix A The result for a 30% N /70% He mixture adsorbed at liquid nitrogen temperature when room temperature is 22 C and atmospheric pressure is 760 mmHg is the expression  Atm.Press.  6.023x10 x16.2x10   ⁄...
  • Page 76 Appendix A FlowSorb III Multipoint Surface Area A straight line usually results between P/P values from about 0.05 to 0.25 when experimental data are plotted as (P/P )/V[1-(P/P )] on the ordinate against P/P the abscissa. Relative pressures within this prescribed range are typically obtained with gas compositions between about 5% and 25% N with the remainder He.
  • Page 77 APPENDIX B OTHER GASES AND COMPOSITIONS...
  • Page 79 FlowSorb III Appendix B OTHER GASES AND COMPOSITIONS Although nitrogen in helium (30/70) with liquid nitrogen as the cold bath pro- vides the most frequently used conditions, there are occasions where it may be de- sirable to employ a different set of circumstances. For example, some investi- gators favor a 20/80 nitrogen-in-helium mixture when analyzing carbon blacks;...
  • Page 80 Appendix B FlowSorb III The FlowSorb III may require other adjustments to render it applicable under the new conditions. Contact your service representative or the factory for further information. Table B.1. Physical Property Data Area Occupied by Vapor Pressure at Gaseous Bath Temperature Adsorbed Molecule at...
  • Page 81 APPENDIX C SPECIALTY GAS SOURCES...
  • Page 83 Appendix FlowSorb Ill SPECIALTY GAS SOURCE 404/451-2711 P. 0. Box 80563 ATLANTA,GA.30341 DOMESTIC SPECIALTY GAS FACILITIES TAMAQUA, PA (HOMETOWN) MOUNTAIN VIEW, CA Air Products and Chemicals, Inc. Air Products and Chemicals, Inc. Specialty Gas Department Specialty Gas Department P. 0. Box 351 465 N Hhisman Road R .D.
  • Page 84 Appendix FlowSorb Ill ATLANTA, GA. 30341 P. 0. Box 80563 404/451-2711 SOUTH AFRICA KOREA Air Products South Africa (Pty) Limited Korea Industrial Gases Ltd. Private Bag 2, Kempton Park 1620 Chung Mu Ro 2Ka 64-5, Chung Ku Transvaal, South Africa Han II Bldg., Room 907 Phone: 36-6686 Seoul, Korea...
  • Page 85 FlowSorb Ill Appendix C Air Products Sales Offices MISSOURI ALABAMA Kansas City ..... (913) 492-1550 Birmingham ....(205) 87Q-5603 Earth City ...... (314) 739-6211 Dothan ......(205) 794-5422 Mobile ......(205) 433-6512 NEBRASKA Muscle Shoals ....(205) 381-0542 Grand Island ....
  • Page 87 APPENDIX D SAMPLE TUBES...
  • Page 89 FlowSorb III Appendix D SAMPLE TUBES Tube 1 (see Figure D-1) primarily is used as the cold trap tube. It also can be used for sample quantities up to a bulk volume of 0.1 cm . Because its use in- creases the gas velocity across the sample, it minimizes the creation of thermal gradients.
  • Page 90 Appendix D FlowSorb III P/N: 230-61002-00 P/N: 230-61001-00 P/N: 230-61003-00 P/N: 230-61005-00 P/N: 230-61004-00 Figure D-1. Sample Tubes Aug 00...
  • Page 91 INDEX...
  • Page 93 INDEX sample, 3-3 Detector, 1-12 Adsorbed gas volume, 3-12, 3-14 drift, 3-4, 4-1 signal, 1-12 purging from system, 3-1 Dewar, 1-11 Analysis cold trap, 1-13 multipoint surface area, 3-14 precautions, 1-4 single-point surface area, 3-7 support, 1-11 Analyzer Display meter, 1-12 See Instrument Erratic results, 4-2 BET equation, A-1...
  • Page 94 Index FlowSorb III Instrument Parts, ordering, 5-1 description, 1-7 Path leaks, 4-2 See Gas location, selecting, 2-2 Potentiometer adjustment, 3-5 precautions, 1-2 Power, input, 2-3 preparing for idle periods, 3-17 Precautions, 1-2 preparing for operation, 3-1 Purging air from system, 3-1 returning, 2-1 schematic, 1-8 specifications, 1-15...
  • Page 95 FlowSorb III Index detector drift, causes for, 4-1 erratic high results, 4-2 Flowmeter float lodged, 4-5 indicators fail to illuminate, 4-5 instrument display not clearing to zero, 4-4 non-reproducible calibrations, 4-3 sample holder, hard to release, 4-5 X10 range, low results on, 4-2 Unpacking instrument, 2-1 Voltage, selecting, 2-3 Warnings, 1-2...

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Flowsorb iii 2310

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