1、Designation: D 3467 04Standard Test Method forCarbon Tetrachloride Activity of Activated Carbon1This standard is issued under the fixed designation D 3467; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.
2、A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.INTRODUCTIONCarbon tetrachloride is classified as a class I ozone depleting substance by the U.S. EnvironmentalProtection Agency. Therefore, use
3、 of this test method is discouraged.Instead, the use of Test Method D 5742 is recommended. The correlation obtained between n-butaneactivity values and carbon tetrachloride activity values is contained in that test method.21. Scope1.1 This test method covers the determination of the acti-vation leve
4、l of activated carbon. Carbon tetrachloride (CCl4)activity is defined herein as the ratio (in percent) of the weightof CCl4adsorbed by an activated carbon sample to the weightof the sample, when the carbon is saturated with CCl4underconditions listed in this test method.1.2 This standard does not pu
5、rport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Sec
6、tion 7.2. Referenced Documents2.1 ASTM Standards:3D 2652 Terminology Relating to Activated CarbonD 2854 Test Method for Apparent Density of ActivatedCarbonD 2867 Test Method for Moisture in Activated CarbonD 5742 Test Method for the Determination of Butane Ac-tivity of Activated CarbonE 300 Practice
7、 for Sampling Industrial ChemicalsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 DefinitionsTerms relating to this test method aredefined in Terminology D 2652.4. Summary of Test Method4.1 Activity is determined by flowing CCl4-lade
8、n airthrough a sample of carbon of known weight, under specifiedconditions, until there is no further increase in the weight of thesample, then determining the weight of the CCl4adsorbed. Theapparatus required for the test consists essentially of means tocontrol the supply air pressure, to remove oi
9、l and water in bothliquid and vapor states from the supply air, to produce thespecified concentration of CCl4in the air flowed through thecarbon sample, and to control the flow rate of the gas (air +CCl4) mixture through the sample.5. Significance and Use5.1 Activity as measured by this test method
10、is basically ameasure of the pore volume of the activated carbon sample.This test method is therefore a means of determining the degreeof completion of the activation process, hence a useful meansof quality control for gas-phase activated carbons. This activitynumber does not necessarily provide an
11、absolute or relativemeasure of the effectiveness of the tested carbon on otheradsorbates, or at other conditions of operation.6. Apparatus and Materials6.1 Carbon Tetrachloride, reagent grade.6.2 Supply of Clean, Dry, Oil-Free AirThe air must bepassed through a HEPA filter and a bed of activated car
12、boncontaining at least 500 mL of carbon per 1670 mL/min of airflow. Relative humidity of the air must be less than 5 % at25C.1This test method is under the jurisdiction of ASTM Committee D28 onActivated Carbon and is the direct responsibility of Subcommittee D28.04 on GasPhase Evaluation Tests.Curre
13、nt edition approved August 1, 2004. Published September 2004. Originallyapproved in 1976. Last previous edition approved in 2003 as D 3467 99 (2003).2The data for this correlation is available from ASTM International Headquar-ters. Request RR: D 281000.3For referenced ASTM standards, visit the ASTM
14、website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United
15、States.6.3 Balance, capable of weighing to within 610 mg.6.4 Pressure Regulator.6.5 CCl4Gas-Generating Device, capable of maintaining aCCl4concentration of 250 6 10 mg/L in the air stream at atemperature of 25 6 1C, equivalent to a relative saturation of27.5 %. A typical generation device, shown in
16、Fig. 1, consistsof a gas-washing bottle and a refrigerated bath capable ofmaintaining a bath temperature of 0C. See also Table 1.6.6 Stopcock, three-way.6.7 Regulating Valve, needle valve, flowmeter, and clock.6.8 Adsorption Tube having the critical dimensions shownin Fig. 1.6.9 Thermostat, capable
17、of maintaining the CCl4-laden airstream and sample tube at a temperature of 25 6 1C.7. Hazards7.1 Carbon tetrachloride vapor is toxic and should not beinhaled. It is advisable to handle carbon tetrachloride and thetest equipment described in this test method in a well-designedchemical fume-hood. The
18、 most recent regulations issued by theOccupational Safety and Health Administration and publishedin the Federal Register should be followed with regards toallowable human exposure. The most recently obtained Mate-rial Safety Data Sheet (MSDS) obtained from the supplier ormanufacturer of the carbon t
19、etrachloride should be available asa guide, as well. Acceptable concentrations of carbon tetrachlo-ride for stack release also should conform to the regulations ofthe United States Environmental Protection Agency, alsoavailable in the Federal Register.8. Sampling8.1 Guidance in sampling granular act
20、ivated carbon is givenin Practice E 300.9. Calibration9.1 Calibration of thermometers, flowmeters, and balancesshall be maintained by standard laboratory methods. Theconcentration of CCl4in the gas stream is determined asdescribed in 11.2.10. Procedure10.1 Dry the sample using the procedure describe
21、d in TestMethod D 2867.10.2 Weigh the dry sample tube to nearest the 10 mg andrecord the weight.10.3 Fill the sample tube to the 100-mm mark 61 mm,using the vibratory feeder described in Test Method D 2854.Isolate the sample by closing the sample tube stopcocks.10.4 Weigh the filled sample tube and
22、record the weight.10.5 Place the filled sample tube vertically in the testassembly (Fig. 1).10.6 Turn the three-way stopcock to vent the CCl4-laden airstream, bypassing the sample.10.7 Open the sample tube stopcocks. Flow the clean, dryair through the CCl4generator until the CCl4concentrationstabili
23、zes at 250 6 10 mg/L at 25 6 1C at a total gas-flow-rateof 1670 6 15 mL/min, corresponding to a superficial velocityof 10 m/min through the sample tube.NOTE 1These items for the apparatus are critical: the dimensions of the sample tube; the location of the flowmeter downstream of the CCl4saturator;a
24、nd the location of the stopcocks. Reheat coil must be adequate to bring the gas temperature to within 1C of the water bath temperature (that is, bedtemperature).NOTE 2Additional sampling tubes may be connected in parallel to allow several samples to be run simultaneously, provided flow through each
25、sampleis maintained within the limits set in 6.7.NOTE 3The pressure at the sample inlet must be maintained at 105 6 3 kPa.FIG. 1 Carbon Tetrachloride Activity Test ApparatusD 3467 04210.8 At the end of the equilibration period, open thesample-tube stopcocks, turn the three-way stopcock to pass theCC
26、l4-laden air through the sample; note the time. Air flow mustbe vertically downward through the carbon sample.10.9 Maintain the gas flow at a rate of 1670 mL/min throughthe sample for 30 min. At the end of that time, turn thethree-way stopcock to vent the gas flow (but maintain the gasflow through t
27、he stopcock). Close the sample tube stopcocks.Remove the sample tube from the test assembly, wipe theexterior dry, and weigh to the nearest 10 mg; record the weight.10.10 Replace the sample tube in the assembly, turn thestopcocks to resume the gas flow through the sample for anadditional 10 min.10.1
28、1 At the end of 10 min, repeat the weighing procedureof 6.9.10.12 Repeat 10.10 and 10.11 until the difference betweentwo successive weighings is less than 10 mg.11. Calculation11.1 ActivityDetermine the CCl4activity using Eq 1:A 5 100 D 2 C!/C 2 B ! (1)where:A = carbon tetrachloride activity, as a p
29、ercent of carbonweight,B = initial weight of dry sample tube, without carbon, g,C = initial weight of filled sample tube, g, andD = final weight of filled sample tube, g.11.2 CCl4Concentration The concentration is normallydetermined by the first measurement of weight gain, using Eq2:S 5 106Dt2 C !/
30、Qt (2)where:S = concentration of CCl4, mg/L,Dt= weight of filled sample tube after t min exposure, g,C = initial weight of filled sample tube, gQ = measured gas flow rate, mL/min, andt = measured exposure period, min (normally 10 min).If the carbon sample shows no weight gain between 10 and20 min ex
31、posure, the sample may have been saturated in lessthan 10 min, and the calculation given in Eq 2 will underestimate the actual concentration. A repeat test run at a timeperiod too short to saturate the carbon will yield a moreaccurate measure of concentration.12. Report12.1 Report the name of the ca
32、rbon supplier, the gradedesignation and nominal particle size range, the carbon tetra-chloride activity, the name of the agency and technicianmaking the test, and the identification number and date of thetest.13. Precision and Bias13.1 In a recent round-robin experiment involving threelaboratories a
33、nd four different carbons, the analysis of the datausing Practice E 691 is shown in Table 2. From this data, theoverall relative standard deviation of this test method is1.22.6 %.14. Keywords14.1 activated carbon; carbon tetrachlorideTABLE 1 CCl4Saturation Capacity (Activity) of Granular Activated C
34、arbonsGranule Diameter (Avg)mmBed Diameter mm Number of Runs Average Activity % Standard Deviation % Relative Std. Dev. %0.55 10.3 19 68.1 61.8 2.60.72 10.3 20 66.2 61.1 1.71.02 23.2 17 61.7 60.7 1.21.30 23.2 20 59.0 61.1 1.9D 3467 043ASTM International takes no position respecting the validity of a
35、ny 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, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to re
36、vision 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 revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. You
37、r 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 shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copy
38、righted 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 obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.or
39、g (e-mail); or through the ASTM website(www.astm.org).TABLE 2 Results of Round Robin Test According to PracticeE 691SampleNo.mathitxj(Sr)j(SL)j(Vr)j(VL)j(SR)j(SR)j%1 104.76 1.32 1.41 1.26 1.34 1.93 1.842 80.89 1.78 1.07 2.20 1.32 2.07 2.563 68.17 0.83 0 1.22 0 0.83 1.224 67.03 0.79 0.80 1.17 1.19 1.12 1.67D 3467 044
