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2、 98 (Reapproved 2002)e1An American National StandardStandard Test Method forTritium in Drinking Water1This standard is issued under the fixed designation D 4107; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revi
3、sion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1 NOTESections 1.4, 10.1.1, 10.1.2, and 12.3.1 were editorially updated in July 2002.1. Scope1.1 This test method covers the determinatio
4、n of tritium in drinking water (as T2O or HTO) by liquid scintillation counting of the tritium beta particle activity.1.2 This test method is used successfully with drinking water. It is the users responsibility to ensure the validity of this test method for waters of untested matrices.1.3 The triti
5、um concentrations, which can be measured by this test method utilizing currently available liquid scintillation instruments, range from less than 0.037 Bq/mL (1 pCi/mL) to555 Bq/mL (15 000 pCi/mL) for a 10-mL sample aliquot. Higher tritium concentrations can be measured by diluting or using smaller
6、sample aliquots, or both.1.4 The maximum contaminant level for tritium in drinking water as given by the National Interim Primary Drinking Water Regulations (NIPDWR) is 0.740 Bq/mL (20 pCi/mL). The NIPDWR lists a required detection limit for tritium in drinking water of 0.037 Bq/mL (1 pCi/mL), meani
7、ng that drinking water supplies, where required, should be monitored for tritium at a sensitivity of 0.037 Bq/mL (1 pCi/mL). In Appendix X1, Eq X1.3 is given for determining the necessary counting time to meet the required sensitivity for drinking water monitoring.1.5 This standard does not purport
8、to address all of the safety concerns, if any, associated with its use. It is the responsibility 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.2. Referenced Documents2.1 ASTM Standards:D 11
9、29 Terminology Relating to Water2D 1193 Specification for Reagent Water2D 2777 Practice for Determination of Precision and Bias ofApplicable Methods of Committee D19 on Water2D 3370 Practices for Sampling Water from Closed Con- duits21 This test method is under the jurisdiction of ASTM Committee D19
10、 on WaterD 3648 Practices for the Measurement of Radioactivity33. Terminology3.1 DefinitionsFor definitions of terms used in this test method, refer to Terminology D 1129. For terms not defined in this test method or in Terminology D 1129, reference may be made to other published glossaries.44. Summ
11、ary of Test Method4.1 In this test method, a 100-mL drinking water sample aliquot is treated with a small amount of sodium hydroxide and potassium permanganate, distilled, and a specified fraction of the distillate is collected for tritium analysis. The alkaline treatment is to prevent other radionu
12、clides, such as radioiodine and radiocarbon from distilling over with the tritium. Some drinking water supplies will contain trace quantities of organic compounds, especially surface water sources that contain fish and other life. The permanganate treatment is to oxidize trace organics in the sample
13、 aliquots which could distill over and cause quenching interferences. A middle fraction of the distil- late is collected for tritium analysis because the early and late fractions are more apt to contain interfering materials for the liquid scintillation counting process.4.2 As the sample distills, t
14、here is a gradient in the tritium concentration in the accumulating distillate; therefore, it is important to collect the same fraction of the distillate for all samples and standards for tritium analysis.4.3 The collected distillate fraction is thoroughly mixed anda portion (up to 10 mL) is mixed w
15、ith liquid scintillator solution, and after dark adapting, is counted in the liquid scintillation counting system for tritium beta particle activity.5. Significance and Use5.1 This test method was developed for measuring tritium in water to determine if the concentration exceeds the regulatory statu
16、tes of drinking water. This test method also is applicable for the determination of tritium concentration in water as required by technical specifications governing the operations ofand is the direct responsibility of Subcommittee D19.04 on Methods of Radiochemi- cal Analysis.Current edition approve
17、d March 10, 1998. Published December 1998. Originally published as D 4107 91. Last previous edition D 4107 98.2 Annual Book of ASTM Standards, Vol 11.01.3 Annual Book of ASTM Standards, Vol 11.02.4 American National Glossary of Terms in Nuclear Science and Technology, available from American Nationa
18、l Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.1D 4107 98 (2002)e1nuclear power facilities. With suitable counting technique,sample size, and counting time a
19、 detection limit of less than 37Bq/L (1000 pCi/L) is attainable by liquid scintillation.6. Interferences6.1 A reduced counting efficiency may result from quench- ing in the sample scintillator mixture. Quenching is caused by impurities in the sample, which can inhibit the transfer of energy, or by c
20、olored materials, which may absorb some of the emitted light. Corrections for quenching can be made by the use of internal standards4 or by the ratio method.5 The approach described in this test method, distillation after alka- line permanganate treatment, eliminates quenching substances, as well as
21、 radionuclides which might be present in a volatile chemical form such as radioiodine and radiocarbon. A boiling chip must be used with each distillation to avoid bumping, which can amount to a carry over excursion.6.2 Scintillator stock solution or samples exposed to day- light must be dark-adapted
22、. Also, toluene or xylene base scintillators exposed to fluorescent lighting should be dark- adapted for a minimum of 6 h and dioxane base scintillators exposed to fluorescent lighting for 24 h. All fluors should he checked for excitation under lighting conditions being used, and if possible, they s
23、hould be exposed only to red light.7. Apparatus7.1 Liquid Scintillation Spectrometer, coincidence-type.7.2 Liquid Scintillation Vials, of low-potassium glass are recommended. Polyethylene vials may be used when dioxane scintillator solution is used.7.3 Distillation ApparatusFor aqueous distillation,
24、250-mL and 1000-mL round bottom borosilicate flasks, con- necting side arm adapter,6 condenser, graduated cylinder, boiling chips, and heating mantle.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
25、 reagents shall conform to the specifications of the Commit- tee on Analytical Reagents of the American Chemical Society, where such specifications are available.7 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without les
26、sening the accuracy of the determination.8.1.1 All chemicals should be of reagent-grade or equiva- lent whenever they are commercially available.8.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming to Specification D 1193, Type III.8
27、.3 Reagents of Distillation Treatment:5 Bush, E.T., “General Applicability of the Channels Radio Method of MeasuringLiquid Scintillation Counting Efficiencies,” Analytical Chemistry, 35:1024, 1963.6 Corning part no. 9060 has been found satisfactory for this purpose.7 Reagent Chemicals, American Chem
28、ical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory8.3.1 Sodium Hydroxide Pellets.8.3.2 Potassium Permanganate.8.4 Background Water, with tritium activity b
29、elow the minimum detectable activity (most deep well waters are low in tritium content).8.5 Scintillator Solutions:8.5.1 Dioxane Liquid Scintillator SolutionDissolve 4 g of scintillation-grade PPO (2,5-diphenyloxazole), 0.05 g of scintillation-grade POPOP 1,4-bis (5-phenyloxazolyl-2-yl)- benzene, an
30、d 120 g of naphthalene in 1 L of spectroquality,1,4-dioxane. Store the solution in a dark (amber) bottle. This solution can be used with glass or polyethylene vials.8.5.2 Solution G Scintillator SolutionDissolve 18 g of scintillation-grade PPO (2,5-diphenyloxazole) and 3.6 g of scintillation-grade B
31、IS-MSB p-bis (o-methylstyryl) benzene in 2 L of spectroquality p-xylene. Add 1 L of Triton N-1018 detergent to the p-xylene scintillator solution. Dissolve 50 g of SXS (sodium xylene sulfonate) in 100 mL of water and add this solution to the p-xylene scintillator-Triton solution. Mix thoroughly. Sto
32、re the solution in a dark (amber) bottle. This solution should be used with glass vials since the p-xylene solvent evaporates slowly through the wall of the polyethylene vials.8.5.3 Other commercially available scintillators can be used, such as the environmentally safe di-isopropyl napthalene based
33、 scintillators. It is the responsibility of the user to verify the acceptability of a substitute scintillator.9. Sampling9.1 Collect the sample in accordance with Practices D 3370.9.2 Since tritium in drinking water is likely to be in the form of T2O or HTO, there is no need for special handling or
34、preservation.10. Calibration10.1 Determination of Recovery and Counting EffciencyFactors:10.1.1 Prepare in a 1-L volumetric flask, a tritium standardsolution containing approximately 17 disintegrations/s(dps)/mL using low level tritium background raw water (un- distilled) and standard tritium activi
35、ty. Label this solution as raw water tritium standard solution. Distill approximately 600 mL of water obtained from the same raw water source (RWS) as above (without tritium activity added).10.1.1.1 Use this distillate for background tritium determi- nations. Using the distillate and standard tritiu
36、m activity, prepare a tritium standard solution in a 500-mL volumetric flask to contain the same specific activity as the raw water tritium standard solution. Label this solution as distilled water tritium standard solution.10.1.2 Aqueous Alkaline Permanganate DistillationPlacea 100-mL aliquot of th
37、e raw water tritium standard solution ina 250-mL distillation flask. Add 0.5 g of sodium hydroxide, 0.1g of potassium permanganate, and a boiling chip. Proceed with the distillate according to the procedure described in 11.1,Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopei
38、a and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.8 Triton products are available from Rohm and Haas Company, IndependenceMall West, Philadelphia, PA 19105.2D 4107 98 (2002)e1discard 10 mL, and collect 50 mL of distillate for analysis. Mixthe 50-mL distillate fracti
39、on. Repeat the distillation with two more 100-mL aliquots for triplicate analyses.10.1.3 Prepare for counting three aliquots of the raw water tritium standard solution distillate (from 10.1.2), three aliquotswhere:RWS= raw water standard.12.3 Sample Tritium Activity, A:R 2 Bof the distilled water tr
40、itium standard solution, and threealiquots of the distilled raw water (for background). Mix 4 mLof water with 16 mL of the dioxane scintillator solution, or 10where:ABq/mL! 5 e 3 V 3 F(3)mL of water with 12 mL of Solution G scintillator solution ina liquid scintillator vial (glass vials should be us
41、ed for detergent-type scintillator solutions). Shake well, dark-adapt the vials overnight, and count in a liquid scintillation counter. Count each vial long enough to meet the required detection(0.037 Bq/mL) or longer (see Appendix X1 for calculating required counting time).11. ProcedureR = sample a
42、liquot gross count rate, cps,B = background aliquot count rate, cps,e = counting efficiency, as determined in Eq 1,V = volume of the sample aliquot, mL, andF = recovery factor, as determined in Eq 2.12.3.1 Error associated with the results of the analysis should be reported.12.4 The total propagated
43、 uncertainty associated with the measured concentration, A, can be calculated as follows:11.1 Add 0.5 g of sodium hydroxide and 0.1 g of potassiumpermanganate to a 100-mL aliquot of the sample in a 250-mL distillation flask. Add a boiling chip to the flask. Connect a side-arm adapter and a condenser
44、 to the outlet of the flask.dNNwhere:21 S de D21 S dV D21 S dF D2(4)Place a graduated cylinder at the outlet of the condenser. Heatthe sample to boiling to distill, collect the first 10 mL of distillate as a separate fraction and discard it.NOTE 1It is important that only the first 10-mL fraction be
45、 discarded or the same fraction for samples and standards alike since there is a gradient in the tritium concentration of the distillate. Collect the next 50 mL of distillate for tritium analysis. Thoroughly mix the 50-mL distillate fraction.11.2 Thoroughly mix 4 mL of the distillate with 16 mL of t
46、he dioxane scintillator or 10 mL of distillate with 12 mL of Solution G scintillator in a liquid scintillation vial. Three aliquots of each sample distillate should be analyzed for tritium.11.3 Prepare background standard tritium-water solutions for counting, using the same amount of water and the same scintillator as used in the preparation of samples. Use low tritium background distilled water for these preparations (dis- tillate of most deep wel
