1、Designation: D3467 04 (Reapproved 2014)Standard Test Method forCarbon Tetrachloride Activity of Activated Carbon1This standard is issued under the fixed designation D3467; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、 last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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.
3、 Therefore, use of this test method is discouraged.Instead, the use of Test Method D5742 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 ac
4、ti-vation level 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 The values
5、stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport 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
6、 and health practices and determine the applica-bility of regulatory limitations prior to use. Specific hazardsstatements are given in Section 7.2. Referenced Documents2.1 ASTM Standards:3D2652 Terminology Relating to Activated CarbonD2854 Test Method for Apparent Density of ActivatedCarbonD2867 Tes
7、t Methods for Moisture in Activated CarbonD5742 Test Method for Determination of Butane Activity ofActivated CarbonE300 Practice for Sampling Industrial ChemicalsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 DefinitionsTerms relatin
8、g to this test method aredefined in Terminology D2652.4. Summary of Test Method4.1 Activity is determined by flowing CCl4-laden 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
9、CCl4adsorbed. Theapparatus required for the test consists essentially of means tocontrol the supply air pressure, to remove oil 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 fl
10、ow rate of the gas (air +CCl4) mixture through the sample.5. Significance and Use5.1 Activity as measured by this test method 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
11、, hence a useful meansof quality control for gas-phase activated carbons. This activitynumber does not necessarily provide an absolute or relativemeasure of the effectiveness of the tested carbon on otheradsorbates, or at other conditions of operation.6. Apparatus and Materials6.1 Carbon Tetrachlori
12、de, reagent grade.6.2 Supply of Clean, Dry, Oil-Free AirThe air must bepassed through a HEPA filter and a bed of activated carboncontaining 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 AS
13、TM Committee D28 onActivated Carbon and is the direct responsibility of Subcommittee D28.04 on GasPhase Evaluation Tests.Current edition approved July 1, 2014. Published September 2014. Originallyapproved in 1976. Last previous edition approved in 2009 as D3467 04 (2009).DOI: 10.1520/D3467-04R14.2Th
14、e data for this correlation is available from ASTM International Headquar-ters. Request RR: D281000.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Do
15、cument Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.3 Balance, capable of weighing to within 610 mg.6.4 Pressure Regulator.6.5 CCl4Gas-Generating Device, capable of maintaining aCCl4concentration o
16、f 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 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
17、.7 Regulating Valve, needle valve, flowmeter, and clock.6.8 Adsorption Tube having the critical dimensions shownin Fig. 1.6.9 Thermostat, capable 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 beinh
18、aled. It is advisable to handle carbon tetrachloride and thetest equipment described in this test method in a well-designedchemical fume-hood. The most recent regulations issued by theOccupational Safety and Health Administration and publishedin the Federal Register should be followed with regards t
19、oallowable human exposure. The most recently obtained Mate-rial Safety Data Sheet (MSDS) obtained from the supplier ormanufacturer of the carbon tetrachloride should be available asa guide, as well.Acceptable concentrations of carbon tetrachlo-ride for stack release also should conform to the regula
20、tions ofthe United States Environmental Protection Agency, alsoavailable in the Federal Register.8. Sampling8.1 Guidance in sampling granular activated carbon is givenin Practice E300.9. Calibration9.1 Calibration of thermometers, flowmeters, and balancesshall be maintained by standard laboratory me
21、thods. Theconcentration of CCl4in the gas stream is determined asdescribed in 11.2.10. Procedure10.1 Dry the sample using the procedure described in TestMethod D2867.10.2 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
22、vibratory feeder described in Test Method D2854.Isolate the sample by closing the sample tube stopcocks.10.4 Weigh the filled sample tube and 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,
23、 bypassing the sample.NOTE 1These items for the apparatus are critical: the dimensions of the sample tube; the location of the flowmeter downstream of the CCl4saturator;and the location of the stopcocks. Reheat coil must be adequate to bring the gas temperature to within 1C of the water bath tempera
24、ture (that is, bedtemperature).NOTE 2Additional sampling tubes may be connected in parallel to allow several samples to be run simultaneously, provided flow through each 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 C
25、arbon Tetrachloride Activity Test ApparatusD3467 04 (2014)210.7 Open the sample tube stopcocks. Flow the clean, dryair through the CCl4generator until the CCl4concentrationstabilizes 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
26、 m/min through the sample tube.10.8 At the end of the equilibration period, open thesample-tube stopcocks, turn the three-way stopcock to pass theCCl4-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 167
27、0 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 the 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
28、 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.10.11 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 tha
29、n 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 percent of carbonweight,B = initial weight of dry sample tube, without carbon, g,C = initial weight of filled sample tube, g, andD = final weight of fille
30、d sample tube, g.11.2 CCl4Concentration The concentration is normallydetermined by the first measurement of weight gain, using Eq2:S 5 106Dt2 C !/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 = measur
31、ed 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 exposure, the sample may have been saturated in lessthan 10 min, and the calculation given in Eq 2 will underestimate the actual concentration. A repeat tes
32、t 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 carbon supplier, the gradedesignation and nominal particle size range, the carbon tetra-chloride activity, the name of the agency and technicianmaking the t
33、est, and the identification number and date of thetest.13. Precision and Bias13.1 In a recent round-robin experiment involving threelaboratories and four different carbons, the analysis of the datausing Practice E691 is shown in Table 2. From this data, theoverall relative standard deviation of this
34、 test method is1.22.6 %.14. Keywords14.1 activated carbon; carbon tetrachlorideTABLE 1 CCl4Saturation Capacity (Activity) of Granular Activated CarbonsGranule Diameter (Avg)mmBed Diameter mm Number of Runs Average Activity % Standard Deviation % Relative Std. Dev. %0.55 10.3 19 68.1 1.8 2.60.72 10.3
35、 20 66.2 1.1 1.71.02 23.2 17 61.7 0.7 1.21.30 23.2 20 59.0 1.1 1.9TABLE 2 Results of Round Robin Test According to PracticeE691SampleNo.xj(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.
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