1、Designation: D 3559 03Standard Test Methods forLead in Water1This standard is issued under the fixed designation D 3559; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates t
2、he year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 These test methods cover the determination of dissolvedand total recoverable lead in
3、water and waste water byatomic-absorption spectrophotometry2and differential pulseanodic stripping voltammetry. Four test methods are includedas follows:ConcentrationRange SectionsTest Method AAtomic Absorption, Direct 1.0 to 10 mg/L 7 to 15Test Method BAtomic Absorption,Chelation-Extraction100 to 1
4、000 g/L 16 to 24Test Method CDifferential Pulse AnodicStripping Voltammetry1to100g/L 25to35Test Method DAtomic Absorption,Graphite Furnace5to100g/L 36to441.2 Test Method B can be used to determine lead in brines.Test Method D has been used successfully with reagent water,lake water, well water, filt
5、ered tap water, condensate from amedium Btu coal gasification process, waste treatment planteffluent, and a production plant process water.1.3 It is the users responsibility to ensure the validity ofthese test methods for waters of untested matrices.1.4 This standard does not purport to address all
6、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. For specific hazardsstatements, see 10.4.1, Note 2, 11.2, 11.3,
7、21.7, 21.8, 21.11,23.7, 23.10, 32.2.1, and 33.1.2. Referenced Documents2.1 ASTM Standards:D 858 Test Methods for Manganese in Water3D 1066 Practice for Sampling Steam3D 1068 Test Methods for Iron in Water3D 1129 Terminology Relating to Water3D 1192 Specification for Equipment for Sampling Waterand S
8、team in Closed Conduits3D 1193 Specification for Reagent Water3D 1687 Test Methods for Chromium in Water3D 1688 Test Methods for Copper in Water3D 1691 Test Methods for Zinc in Water3D 1886 Test Methods for Nickel in Water3D 2777 Practice for Determination of Precision and Bias ofApplicable Methods
9、of Committee D-19 on Water3D 3370 Practices for Sampling Water from Closed Con-duits3D 3557 Test Methods for Cadmium in Water3D 3558 Test Methods for Cobalt in Water3D 3919 Practice for Measuring Trace Elements in Water byGraphite Furnace Atomic Absorption Spectrophotometry3D 4841 Practice for Estim
10、ation of Holding Time for WaterSamples Containing Organic and Inorganic Constituents3D 5810 Guide for Spiking into Aqueous Samples3D 5847 Practice for the Writing Quality Control Specifica-tions for Standard Test Methods for Water Analysis3E 60 Practice for Photometric and SpectrophotometricMethods
11、for Chemical Analysis of Metals4E 275 Practice for Describing and Measuring Performanceof Ultraviolet, Visible, and Near Infrared Spectrophotom-eters53. Terminology3.1 DefinitionsFor definition of terms used in these testmethods, refer to Terminology D 1129.3.2 total recoverable leadan arbitrary ana
12、lytical termrelating to the recoverable forms of lead that are determined bythe digestion method which are included in the procedure.4. Significance and Use4.1 The test for lead is necessary because it is a toxicant andbecause there is a limit specified for lead in potable water in theNational Inter
13、im Primary Drinking Water Regulations. This1These test methods are under the jurisdiction of ASTM Committee D19 onWater and are the direct responsibility of Subcommittee D19.05 on InorganicConstituents in Water.Current edition approved Jan. 10, 2003. Published January 2003. Originallyapproved in 197
14、7. Last previous edition approved in 1996 as D 3559 96.2Platte, J.A., and Marcy, V. M., “ANew Tool for the Water Chemist,” IndustrialWater Engineering, May 1965.Brown, E., Skougstad, M. W., and Fishman, M. J., “Methods for Collection andAnalysis of Water Samples for Dissolved Minerals and Gases,” Te
15、chniques ofWater-Resources Investigations of the U. S. Geological Survey, Book 5, Chapter ,1970, p. 115.3Annual Book of ASTM Standards, Vol 11.01.4Annual Book of ASTM Standards, Vol 03.05.5Annual Book of ASTM Standards, Vol 03.06.1*A Summary of Changes section appears at the end of this standard.Cop
16、yright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.test serves to determine whether the lead content of potablewater is above or below the acceptable limit.5. Purity of Reagents5.1 Reagent grade chemicals shall be used in all tests.Unless o
17、therwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society.6Other gradesmay be used, provided it is first ascertained that the reagent isof sufficiently high purity to permit its use without lessenin
18、gthe accuracy of the determination.5.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to SpecificationD 1193, Type I. Other reagent water types may be usedprovided it is first ascertained that the water is of sufficientlyhigh purity to permit its
19、use without adversely affecting thebias and precision of the test method. Type II water wasspecified at the time of round-robin testing of this test method.6. Sampling6.1 Collect the samples in accordance with Practice D 1066,Specification D 1192, and Practices D 3370, as applicable.6.2 Samples shal
20、l be preserved with HNO3(sp gr 1.42) to apH of 2 or less immediately at the time of collection, normallyabout 2 mL/L of HNO3. If only dissolved lead is to bedetermined, the sample shall be filtered through a 0.45-mmembrane filter before acidification.TEST METHOD AATOMIC ABSORPTION,DIRECT7. Scope7.1
21、This test method covers the determination of dissolvedand total recoverable lead in most waters and wastewaters.7.2 The test method is applicable in the range from 1.0 to 10mg/Lof lead. The upper limits of detectability can be increasedto concentrations greater than 10 mg/L by dilution of thesample.
22、8. Summary of Test Method8.1 Lead is determined by atomic absorption spectropho-tometry. Dissolved lead is determined by aspirating the filteredand preserved sample directly with no pretreatment. Totalrecoverable lead is determined by aspirating the sample fol-lowing hydrochloric-nitric acid digesti
23、on and filtration. Thesame digestion procedure may be used to determine totalrecoverable cadmium (Test Methods D 3557), chromium (TestMethods D 1687), cobalt (Test Methods D 3558), copper (TestMethods D 1688), iron (Test Methods D 1068), manganese(Test Methods D 858), nickel (Test Methods D 1886), a
24、nd zinc(Test Methods D 1691).9. Interferences9.1 Other metals usually do not interfere in the determina-tion of lead by increasing or decreasing the amount of absorbedradiation. The most common interference is caused by achemical reaction in the flame that prevents conversion of thelead to the atomi
25、c state.9.2 High concentrations of calcium, such as those connectedwith the coal industry, will give lead concentrations higher thanwhich actually exist. This can be corrected by using a back-ground correction technique, or by the chelation-extractionprocedure (Test Method B).9.2.1 The equipment man
26、ufacturers instructions for use ofspecific correction technique shall be followed.10. Apparatus10.1 Atomic Absorption Spectrophotometer, for use at 283.3nm.NOTE 1The manufacturers instructions shall be followed for allinstrumental parameters. Wavelengths other than 283.3 nm may be used ifthey have b
27、een determined to be equally suitable.10.2 Lead Light Source, hollow-cathode lamps orelectrodeless-discharge lamps have been found satisfactory.10.3 Oxidant:10.3.1 Air, which has been passed through a suitable filter toremove oil, water, and other foreign substances, is the usualoxidant.10.4 Fuel:10
28、.4.1 AcetyleneStandard, commercially available acety-lene is the usual fuel. Acetone, always present in acetylenecylinders, can affect analytical results. The cylinder should bereplaced at 50 psig (345 kPa).10.4.1.1 Warning“Purified” grade acetylene containing aspecial proprietary solvent rather tha
29、n acetone should not beused with poly(vinyl chloride) tubing as weakening of thewalls can cause a potential hazardous situation.10.5 Pressure-Reducing ValvesThe supplies of fuel andoxidant shall be maintained at pressures somewhat higher thanthe controlled operating pressure of the instrument by sui
30、tablevalves.11. Reagents11.1 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (HCl).NOTE 2If the reagent blank concentration is greater than the methoddetection limit, distill the HCl or use a spectrograde acid. CautionWhenHCl is distilled, an azeotropic mixture is formed (approximately
31、 6 N HClis formed). Therefore, whenever concentrated HCl is used in the prepa-ration of a reagent or in the procedure, use double the volume specified ifdistilled HCl is used.11.2 Lead Solution, Stock (1 mL = 1 mg lead)Dissolve1.5999 g of lead nitrate (Pb (NO3)2) in a mixture of 10 mL ofHNO3(sp gr 1
32、.42) and 100 mL of water. Dilute to 1 L withwater. WarningLead salts are toxic. Handle with care andavoid personal contamination.11.3 Lead Solution, Standard (1 mL = 0.1 mg lead)Dilute100.0 mL of stock lead solution to 1 L with HNO3(1 + 499).Store all solutions in polyethylene bottles. WarningLead6R
33、eagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
34、and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.D3559032salts are toxic. Never pipet by mouth. Pipet with the end of asuction device or employ other conventional means of quanti-tative measurement.11.4 Nitric Acid (sp gr 1.42)Concentrated nitric acid(HNO3).NOTE 3If
35、the reagent blank concentration is greater than the methoddetection limit, distill the HNO3or use a trace metal grade acid.11.5 Nitric Acid (1 + 499)Add 1 volume of HNO3(sp gr1.42) to 499 volumes of water.12. Standardization12.1 Prepare 100 mL each of a blank and at least fourstandard solutions to b
36、racket the expected lead concentrationrange to be analyzed by diluting the lead standard solution(11.3) with HNO3(1 + 499). Prepare the standards each timethe test is to be performed.12.2 When determining total recoverable lead, add 0.5 mLof HNO3(sp gr 1.42) to each blank and standard solution andpr
37、oceed as directed in 13.2 through 13.4.After the digestion ofthe blank and standard solutions has been completed in 13.4,return to 12.3 to complete the standardization for total recov-erable determinations. When determining dissolved lead, pro-ceed with 12.3.12.3 Aspirate the blank and standards and
38、 record the instru-ment readings. Aspirate HNO3(1 + 499) between standards.12.4 Prepare an analytical curve by plotting the absorbanceversus the concentration for each standard on linear graphpaper. Alternatively, read directly in concentration if thiscapability is provided with an instrument.13. Pr
39、ocedure13.1 Measure 100.0 mL of a well-mixed acidified sampleinto a 125-mL beaker or flask.NOTE 4If only dissolved lead is to be determined, start with 13.5.13.2 Add 5 mL of HCl (sp gr 1.19) to each sample.13.3 Heat the samples on a steam bath or hot plate in awell-ventilated hood until the volume h
40、as been reduced to 15to 20 mL, making certain that the samples do not boil.NOTE 5For samples having appreciable amounts of suspended matteror dissolved matter, the amount of reduction in volume is left to thediscretion of the analyst.13.4 Cool and filter the samples through a suitable filtersuch as
41、fine-textured, acid washed, ashless paper, into 100-mLvolumetric flasks. Wash the filter paper two or three times withwater and adjust to volume.13.5 Aspirate each filtered and acidified sample and deter-mine its absorbance or concentration at 283.3 nm. AspirateHNO3(1 + 499) between samples.14. Calc
42、ulation14.1 Calculate the concentration of lead in each sample, inmilligrams per litre, using the calibration curve established in12.4.15. Precision and Bias715.1 Fourteen operators from nine laboratories participatedin this study. One operator performed the analysis in quadru-plicate, twelve in tri
43、plicate and one in duplicate at eachconcentration level.15.2 The bias of this test method for lead is listed in Table1.15.3 These data may not apply to waters of other matrices.15.4 This section on precision and bias conforms to PracticeD277777which was in place at the time of collaborativetesting.
44、Under the allowances made in 1.4 of D 2777 98,these precision and bias data do meet existing requirements ofinterlaboratory studies of Committee D19 test methods.16. Quality Control16.1 In order to be certain that analytical values obtainedusing these test methods are valid and accurate within theco
45、nfidence limits of the test, the following QC procedures mustbe followed when analyzing lead.16.2 Calibration and Calibration Verification:16.2.1 Analyze at least three working standards containingconcentrations of lead that bracket the expected sample con-centration, prior to analysis of samples, t
46、o calibrate theinstrument. The calibration correlation coefficient shall beequal to or greater than 0.990. In addition to the initialcalibration blank, a calibration blank shall be analyzed at theend of the batch run to ensure contamination was not a problemduring the batch analysis.16.2.2 Verify in
47、strument calibration after standardization byanalyzing a standard at the concentration of one of thecalibration standards. The concentration of a mid-range stan-dard should fall within 615 % of the known concentration.16.2.3 If calibration cannot be verified, recalibrate theinstrument.16.3 Initial D
48、emonstration of Laboratory Capability:16.3.1 If a laboratory has not performed the test before, or ifthere has been a major change in the measurement system, forexample, new analyst, new instrument, etc., a precision andbias study must be performed to demonstrate laboratorycapability.7Supporting dat
49、a are available from ASTM Headquarters. Request RR:D19-1030.TABLE 1 Determination of Bias, DirectAmountAdded,mg/LAmountFound,mg/LST,mg/LS0,mg/LBias, %StatisticallySignificant(95 % Confi-dence Level)Reagent Water, Type II1 1.01 0.08 0.04 +1.00 no6 6.01 0.28 0.14 +0.17 no8 8.02 0.34 0.14 +0.25 noSelected Water Matrices1 1.00 0.00 0.06 0.00 no6 6.11 0.25 0.16 +1.83 yes8 7.99 0.36 0.23 0.13 noD355903316.3.2 Analyze seven replicates of a standard solutionprepared from an Independent Reference Material containing amid-range concentration of lead. The matrix
