1、Designation: D3559 15Standard Test Methods forLead in Water1This standard is issued under the fixed designation D3559; 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 the
2、 year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 These test methods cover the determination of dissolvedand total recoverable lead i
3、n 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
4、 1000 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, fi
5、ltered 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 The values stated in SI units are to be rega
6、rded asstandard. The values given in parentheses are mathematicalconversions to inch-pound units that are provided for informa-tion only and are not considered standard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility o
7、f 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 Note 3, 11.3, 11.4, 11.8.1, 21.8, 21.9, 21.12,23.7, 23.10, 32.2.1, and 33.1.2. Referenced Documents2.1 ASTM S
8、tandards:3D858 Test Methods for Manganese in WaterD1066 Practice for Sampling SteamD1068 Test Methods for Iron in WaterD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD1687 Test Methods for Chromium in WaterD1688 Test Methods for Copper in WaterD1691 Test Methods for Zinc in
9、WaterD1886 Test Methods for Nickel in WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD3557 Test Methods for Cadmium in WaterD3558 Test Methods for Cobalt in WaterD3919 Practice for
10、Measuring Trace Elements in Water byGraphite Furnace Atomic Absorption SpectrophotometryD4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and Inorganic ConstituentsD5673 Test Method for Elements in Water by InductivelyCoupled PlasmaMass SpectrometryD5810 Guide for Spi
11、king into Aqueous SamplesD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE60 Practice for Analysis of Metals, Ores, and RelatedMaterials by SpectrophotometryE275 Practice for Describing and Measuring Performance ofUltraviolet and Visible Spectroph
12、otometers3. Terminology3.1 DefinitionsFor definition of terms used in these testmethods, refer to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 total recoverable lead, na descriptive term relatingto the lead forms recovered in the acid-digestion procedurespecified in the
13、se test methods.1These 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 June 1, 2015. Published October 2015. Originallyapproved in 1977. Last previous edition app
14、roved in 2008 as D3559 08. DOI:10.1520/D3559-15.2Platte, 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 andGases,” Techniques
15、 of Water-Resources Investigations of the U. S. GeologicalSurvey, Book 5, 1970, p. 115.3For 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 Document Summar
16、y page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14. Significance and Use4.1 The test for lead is necessary because it is a toxicant andbecause t
17、here is a limit specified for lead in potable water in theNational Interim Primary Drinking Water Regulations. Thistest 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.Unle
18、ss otherwise indicated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society.4Other gradesmay be used, provided it is first ascertained that the reagent isof sufficiently high purity to permit its use without less
19、eningthe accuracy of the determination.5.2 Unless otherwise indicated, references to water shall beunderstood to mean reagent water conforming to SpecificationD1193, Type I. Other reagent water types may be usedprovided it is first ascertained that the water is of sufficientlyhigh purity to permit i
20、ts 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 D1066and Practices D3370, as applicable.6.2 Samples shall be preserved with HN
21、O3(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.NOTE 1Alternatively, the pH may be adjusted in the laboratory if thesam
22、ple is returned within 14 days. However, acid must be added at least24 hours before analysis to dissolve any metals that adsorb to the containerwalls. This could reduce hazards of working with acids in the field whenappropriate.TEST METHOD AATOMICABSORPTION, DIRECT7. Scope7.1 This test method covers
23、 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.8. Summary of Test Meth
24、od8.1 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 digestion and filtration. Thes
25、ame digestion procedure may be used to determine totalrecoverable cadmium (Test Methods D3557), chromium (TestMethods D1687), cobalt (Test Methods D3558), copper (TestMethods D1688), iron (Test Methods D1068), manganese (TestMethods D858), nickel (Test Methods D1886), and zinc (TestMethods D1691).9.
26、 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 atomic state.9.2 High concentrations
27、 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 manufacturers instructions for use
28、 ofspecific correction technique shall be followed.10. Apparatus10.1 Atomic Absorption Spectrophotometer, for use at 283.3nm.NOTE 2The manufacturers instructions shall be followed for allinstrumental parameters. Wavelengths other than 283.3 nm may be used ifthey have been determined to be equally su
29、itable.10.2 Lead Light Source, hollow-cathode lamps orelectrodeless-discharge lamps have been found satisfactory.10.3 Pressure-Reducing ValvesThe supplies of fuel andoxidant shall be maintained at pressures somewhat higher thanthe controlled operating pressure of the instrument by suitablevalves.11.
30、 Reagents and Materials11.1 Filter PaperPurchase suitable filter paper. Typicallythe filter papers have a pore size of 0.45-m membrane.Material such as fine-textured, acid-washed, ashless paper, orglass fiber paper are acceptable. The user must first ascertainthat the filter paper is of sufficient p
31、urity to use withoutadversely affecting the bias and precision of the test method.11.2 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (HCl).NOTE 3If the reagent blank concentration is greater than the methoddetection limit, distill the HCl or use a spectrograde acid. WarningWhen HCl i
32、s distilled, an azeotropic mixture is formed (approximately 6N HCl is formed). Therefore, whenever concentrated HCl is used in thepreparation of a reagent or in the procedure, use double the volumespecified if distilled HCl is used.11.3 Lead Solution, Stock (1 mL = 1 mg lead)Commercially purchase or
33、 dissolve 1.5999 g of lead nitrate (Pb(NO3)2) in a mixture of 10 mL of HNO3(sp gr 1.42) and 100mL of water. Dilute to 1 L with water. A purchased lead stocksolution of appropriate known purity is also acceptable.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society,
34、Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D3559
35、 152(WarningLead salts are toxic. Handle with care and avoidpersonal contamination.)11.4 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. (WarningLeadsalts are toxic. Never pipette by mouth. Pipet
36、te with the end ofa suction device or employ other conventional means ofquantitative measurement.)11.5 Nitric Acid (sp gr 1.42)Concentrated nitric acid(HNO3).NOTE 4If the reagent blank concentration is greater than the methoddetection limit, distill the HNO3or use a trace metal grade acid.11.6 Nitri
37、c Acid (1 + 499)Add 1 volume of HNO3(sp gr1.42) to 499 volumes of water.11.7 Oxidant:11.7.1 Air, which has been passed through a suitable filter toremove oil, water, and other foreign substances, is the usualoxidant.11.8 Fuel:11.8.1 AcetyleneStandard, commercially available acety-lene is the usual f
38、uel. Acetone, always present in acetylenecylinders, can affect analytical results. The cylinder should bereplaced at 345 kPa (50 psi).11.8.1.1 Warning“Purified” grade acetylene containing aspecial proprietary solvent rather than acetone should not beused with poly(vinyl chloride) tubing as weakening
39、 of thewalls can cause a potential hazardous situation.12. Standardization12.1 Prepare 100 mL each of a blank and at least fourstandard solutions to bracket the expected lead concentrationrange to be analyzed by diluting the lead standard solution(11.4) with HNO3(1 + 499) (11.6). Analyze at least fo
40、urworking standards containing concentrations of lead thatbracket the expected sample concentration, prior to analysis ofsamples, to calibrate the instrument. Prepare the standards eachtime the test is to be performed or as determined by PracticeD4841.12.2 When determining total recoverable lead, ad
41、d 0.5 mLof HNO3(sp gr 1.42) (11.5) to each blank and standard solutionand proceed as directed in 13.2 through 13.4. After thedigestion of the blank and standard solutions has been com-pleted in 13.4, return to 12.3 to complete the standardizationfor total recoverable determinations. When determining
42、 dis-solved lead, proceed with 12.3.12.3 Aspirate the blank and standards and 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 dire
43、ctly in concentration if thiscapability is provided with an instrument.13. Procedure13.1 Measure 100.0 mL of a well-mixed acidified sampleinto a 125-mL beaker or flask.NOTE 5If only dissolved lead is to be determined, start with 13.5.13.2 Add 5 mL of HCl (sp gr 1.19) (11.2) to each sample.13.3 Heat
44、the samples on a steam bath or hot plate in awell-ventilated hood until the volume has been reduced to 15to 20 mL, making certain that the samples do not boil.NOTE 6For samples having appreciable amounts of suspended matteror dissolved matter, the amount of reduction in volume is left to thediscreti
45、on of the analyst.NOTE 7Many laboratories have found block digestion systems auseful way to digest samples for trace metals analysis. Systems typicallyconsist of either a metal or graphite block with wells to hold digestiontubes. The block temperature controller must be able to maintain unifor-mity
46、of temperature across all positions of the block. For trace metalsanalysis, the digestion tubes should be constructed of polypropylene andhave a volume accuracy of at least 0.5 %. All lots of tubes should comewith a certificate of analysis to demonstrate suitability for their intendedpurpose.13.4 Co
47、ol and filter (11.1) the samples through a suitablefilter such as fine-textured, acid washed, ashless paper, into100-mL volumetric flasks. Wash the filter paper two or threetimes with water and adjust to volume.13.5 Aspirate each filtered and acidified sample and deter-mine its absorbance or concent
48、ration at 283.3 nm. AspirateHNO3(1 + 499) between samples.14. Calculation14.1 Calculate the concentration of lead in each sample, inmilligrams per litre, using the calibration curve established in12.4.15. Precision and Bias515.1 Fourteen operators from nine laboratories participatedin this study. On
49、e operator performed the analysis inquadruplicate, twelve in triplicate 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.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D19-1030. ContactASTM CustomerService at serviceastm.org.TABLE 1 Determination of Bias, DirectAmountAdded,mg/LAmountFound,mg/LST,mg/LS0,mg/LBias, %StatisticallySignificant(95 % Confi-dence Lev
