ASTM D5228-2016 Standard Test Method for Determination of Butane Working Capacity of Activated Carbon《测定活性炭丁烷工作容量的标准试验方法》.pdf

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1、Designation: D5228 92 (Reapproved 2015)D5228 16Standard Test Method forDetermination of Butane Working Capacity of ActivatedCarbon1This standard is issued under the fixed designation D5228; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev

2、ision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the butane working capacity (BWC) of new granular acti

3、vated carbon. TheBWC is defined as the difference between the butane adsorbed at saturation and the butane retained per unit volume of carbon aftera specified purge. The test method also produces a butane activity value that is defined as the total amount of butane adsorbed onthe carbon sample and i

4、s expressed as a mass of butane per unit weight or volume of carbon.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use.

5、 It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For a specific hazard statement, see 7.1.2. Referenced Documents2.1 ASTM Standards:2D2652 Terminology Relating to Activate

6、d CarbonD2854 Test Method for Apparent Density of Activated CarbonD2867 Test Methods for Moisture in Activated CarbonD3195 Practice for Rotameter CalibrationE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE300 Practice for Sampling Industrial ChemicalsE691 Practice for Cond

7、ucting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1 Definitions For definitions of terms used in this test method, refer to Terminology D2652.4. Summary of Test Method4.1 An activated carbon bed of known volume and mass is saturated with butane vapor. The mas

8、s adsorbed at saturation isnoted. The carbon bed is then purged under prescribed conditions with dry hydrocarbon free air. The loss of mass is the BWC andis expressed as mass of butane per unit volume of carbon.5. Significance and Use5.1 The BWC, as determined by this test method, is a measure of th

9、e ability of an activated carbon to adsorb and desorb butanefrom dry air under specified conditions. It is useful for quality control and evaluation of granular activated carbons that are usedin applications where the adsorption of butane and desorption with dry air are of interest. The BWC can also

10、 provide a relativemeasure of the effectiveness of the tested activated carbons on other adsorbates.5.2 The butane activity and retentivity can also be determined under the conditions of the test. The butane activity is anindication of the micropore volume of the activated carbon sample. The butane

11、retentivity is an indication of the pore structureof the activated carbon sample.1 This test method is under the jurisdiction of ASTM Committee D28 on Activated Carbon and is the direct responsibility of Subcommittee D28.04 on Gas PhaseEvaluation Tests.Current edition approved Oct. 1, 2015June 1, 20

12、16. Published October 2015July 2016. Originally approved in 1992. Last previous edition approved in 20102015 asD5228 92 (2010).(2015). DOI: 10.1520/D5228-92R15.10.1520/D5228-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. Fo

13、r Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may n

14、ot be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor

15、Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Apparatus6.1 Water Bath, capable of maintaining a temperature of 25 6 0.2C and of sufficient depth so the entire carbon bed in thesample tube is immersed in the water. A 6-mm OD copper tube with an immersed length of 1.9 m (Fig.

16、1) provides adequate heattransfer for gas temperature control.6.2 Sample Tube, as shown in Fig. 2. The glass plate with holes is preferred to a fritted disk to support the carbon, since fritteddisks can vary widely in pressure drop.6.3 Flow Meters, one capable of delivering air at 0 to 500 mL/min, a

17、nd one capable of delivering butane at 0 to 500 mL/min,both calibrated in accordance with Practice D3195.6.4 Balance, capable of weighing to within 60.01 g.6.5 Fill DeviceThe vibration feed device used in Test Method D2854, Figs. 1 through 4, is preferred.6.6 Buret, Class A, 25 mL capacity.6.7 Appar

18、atus Assembly shown in Fig. 1.7. Reagents7.1 n-Butane, C. P. Grade. (WarningButane is a flammable gas with a flash point of 138C and a boiling point of 0.5C.Its specific gravity is 2.046 relative to air. Butane may be narcotic in high concentrations and is considered a simple asphyxiant.If the entir

19、e apparatus is not set up in a fume hood, provision must be made to vent the gas coming from the discharge stem ofthe sample tube.)7.2 Dry Air, free of organics, with a dew point no higher than 32C.8. Sampling8.1 For guidance in sampling granular activated carbon, refer to Practice E300.9. Calibrati

20、on of a Sample Tube9.1 Clean and dry the sample tube to prevent any water droplets from adhering to the inner surface of the tube.9.2 Using distilled water, carefully fill the sample tube through the narrow side stem to prevent the introduction of any airbubbles.9.2.1 Hold the sample tube upright wh

21、ile slowly introducing the distilled water. Air bubbles have a tendency to form directlybelow the retainer plate of the tube.9.3 Clamp the filled sample tube in an upright position to a ring stand and stopper the narrow side stem.FIG. 1 Butane Working Capacity Apparatus SchematicD5228 1629.4 Using a

22、 pipet, carefully remove the water from the sample tube to the top of the retainer plate. Caution must be taken sono water is removed from below the retainer plate creating air bubbles that would result in a spurious calibration of the sampletube. If this occurs, the tube must be refilled by repeati

23、ng 9.1 through 9.3.9.5 Using the buret, fill the sample tube with 16.7 6 0.05 mL of water, then etch the tube at the level of the meniscus.10. Maintenance of Bath Water10.1 In order to prevent mold formation, the bath water should be changed periodically.11. Procedure11.1 Dry an adequate sample as p

24、rescribed in Test Methods D2867, Section 4.11.2 Determine the apparent density in accordance with Test Method D2854 and record.11.3 Accurately weigh the empty, dry sample tube and stoppers to the nearest 0.01 g and record.11.4 Fill the adsorption tube with carbon to the etch mark at a rate of 0.35 t

25、o 1.0 mL/s using the vibrating feeder apparatusdescribed in Test Method D2854 with a funnel modified to accommodate the adsorption tube. Larger particles will require theslower fill rate to achieve the required packing density.11.5 Weigh the filled sample tube and stoppers to the nearest 0.01 g and

26、record.11.5.1 The sample packing density, carbon weight/16.7, must be equal to at least 94 % of its dry apparent density if the resultof the determination is to be reproducible. Otherwise, the ratio of purge air volume to sample volume will vary, and the quantityof butane purged will also vary from

27、one determination to the next. If the specified packing density is not achieved in the firstattempt, the filling procedure must be repeated until the tube is packed to the required density. If after several attempts the desiredpacking density cannot be achieved, the percentage should be noted and th

28、e procedure continued.11.6 Set the water bath control to maintain a temperature of 25 6 0.2C.11.7 Clamp the sample tube in a vertical position in the 25 6 0.2C water bath and attach the tube to the output of the flowmeter. If the entire apparatus is not in a hood, attach a short length of tubing fro

29、m the effluent side of the sample tube to an exhaustvent.11.8 Regulate the flow to pass butane through the carbon bed at 250 6 5 mL/min. Continue the flow of butane for at least 900s.1 Ground glass stopper, hollow, medium length, 14/20, from Kontes Catalog No. K-89100 Schwartz adsorption tube, or eq

30、uivalent.2 5-mm rod, brace.3 17-mm O.D. 1.2 mm standard wall tubing.4 Coors perforated porcelain disk or extra coarse fritted disk, or equivalent.5 10-mm O.D. 1.0 mm standard wall tubing.6 Right angle stopcock, Kontes Catalog No. K-84700, size 4, 10 mm O.D. stem, with Kontes Catalog No. K-89340 size

31、 B serrated hose connector, or equivalent.7 Dimension corresponding to a volume of 16.7 mL above the retainer plate.FIG. 2 Butane Working Capacity Sample TubeD5228 16311.9 Turn off the butane, disconnect the tubing, and immediately stopper the sample tube. Remove the sample tube from thewater bath,

32、dry the sample tube, and visually inspect the tube for any condensed water vapor. If any condensed water is observed,stop the testing and begin the test procedure again.11.10 Weigh the filled sample tube and its stoppers to the nearest 0.01 g and record.11.11 Reconnect the sample tube to the apparat

33、us and flow butane for an additional 600 s and weigh and record. Repeat toconstant weight.11.12 Reconnect the saturated carbon and sample tube and purge with dry organic free air for 2400 6 20 s at 300 6 5 mL/min.11.13 Turn off the purge flow, disconnect tubing, install stoppers, remove the sample t

34、ube from the water bath, and dry.11.14 Weigh to the nearest 0.01 g and record.12. Calculation12.1 The calculations described in this section are based upon the following determinations made during the course of theprocedure:A = Apparent density from 11.2,B = Weight of sample tube and stoppers,C = We

35、ight of carbon sample, sample tube, and stoppers,D = Weight of saturated carbon, sample tube, and stoppers, andE = Weight of purged carbon, sample tube, and stoppers.NOTE 1A sample data and calculations sheet for BWC determinations is given in Annex A1.12.2 Calculate the BWC on weight and volume bas

36、es as follows:BWC,W/W%5D 2E!C2B! 3100 (1)BWC, W/Vg/100 mL5D 2E!C2B! 3A 3100 (2)12.3 Calculate the butane activity on weight and volume bases as follows:Butane activity,W/W%5D 2C!C2B! 3100 (3)Butane activity,W/Vg/100 mL5D 2C!C2B! 3A 3100 (4)12.4 Calculate the butane retentivity on weight and volume b

37、ases as follows:Butane retentivity,W/W%5E 2C!C2B! 3100 (5)Butane retentivity,W/Vg/100 mL5E 2C!C2B! 3A 3100 (6)13. Report13.1 The analysis report shall include the following information:13.1.1 Name of activated carbon supplier,13.1.2 Grade designation of the sample,13.1.3 Nominal partialparticle size

38、 range,13.1.4 Butane working capacity,13.1.5 Butane activity,13.1.6 Butane retentivity,13.1.7 Name of the agency and technician running the test,13.1.8 Identification number and date of the test, and13.1.9 Lot number from which the sample was taken.14. Precision and Bias14.1 An interlaboratory study

39、 of this test method was conducted in 1990.3 Each of eight laboratories tested three randomlydrawn test specimens from each of three different activated carbons. Practice E691 and its computer software were followed forthe design of the study and the data analysis.3 Supporting data have been filed a

40、t ASTM International Headquarters and may be obtained by requesting Research Report RR:D28-1003. Contact ASTM CustomerService at serviceastm.org.D5228 16414.2 95 % Limit on Repeatability (within Laboratory) in Percent:Activated CarbonA B CActivity %, weight/weight 1.95 2.34 .97Retentivity %, weight/

41、weight 2.52 1.80 1.77Working capacity %, weight/weight 2.05 3.14 2.19Activity g/100 mL, weight/vol 0.68 0.70 0.40Retentivity g/100 mL, weight/vol 0.72 0.52 0.95Working capacity g/100 mL, weight/vol0.51 0.92 1.0414.3 95 % Limit on Reproducibility (between Laboratories) in Percent:Activated CarbonA B

42、CActivity %, weight/weight 3.57 3.15 1.05Retentivity %, weight/weight 3.75 3.79 3.79Working capacity %, weight/weight 5.06 4.70 3.83Activity g/100 mL, weight/vol 0.91 1.08 0.57Retentivity g/100 mL, weight/vol 1.05 1.22 1.84Working charge g/100 mL, weight/vol1.41 1.51 2.0614.4 Apparent Densitys 95 %

43、Repeatability and Reproducibility Limits:Activated CarbonA B CRepeatability g/100 mL 0.012 0.004 0.008Reproducibility g/100 mL 0.019 0.021 0.025NOTE 2The terms repeatability and reproducibility limit are used as specified in Practice E177.ANNEX(Mandatory Information)A1. DATAAND CALCULATIONS SHEET FO

44、R BWC DETERMINATIONSA1.1 See Fig. A1.1:D5228 165ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights,

45、 and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn.Your comments are invited either for revi

46、sion of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you

47、shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be o

48、btained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ A1.1 Data and Calculations Sheet for BWC DeterminationsD5228 166

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