1、Designation: D 3559 08Standard 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 () 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. Scope1.1 These test methods cover the determination of dissolvedand total recoverable lead in wa
3、ter 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 100
4、0 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, filter
5、ed 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 regarded
6、 asstandard. No other units of measurement are included in thisstandard.1.5 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 and health practices and determine t
7、he applica-bility of regulatory limitations prior to use. For specific hazardsstatements, see 10.4.1, Note 2, 11.2, 11.3, 21.7, 21.8, 21.11,23.7, 23.10, 32.2.1, and 33.1.2. Referenced Documents2.1 ASTM Standards:3D 858 Test Methods for Manganese in WaterD 1066 Practice for Sampling SteamD 1068 Test
8、Methods for Iron in WaterD 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 1687 Test Methods for Chromium in WaterD 1688 Test Methods for Copper in WaterD 1691 Test Methods for Zinc in WaterD 1886 Test Methods for Nickel in WaterD 2777 Practice for Determination of Precisio
9、n and Bias ofApplicable Test Methods of Committee D19 on WaterD 3370 Practices for Sampling Water from Closed ConduitsD 3557 Test Methods for Cadmium in WaterD 3558 Test Methods for Cobalt in WaterD 3919 Practice for Measuring Trace Elements in Water byGraphite Furnace Atomic Absorption Spectrophoto
10、metryD 4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and Inorganic ConstituentsD 5810 Guide for Spiking into Aqueous SamplesD 5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE 60 Practice for Analysis of Metals, O
11、res, and RelatedMaterials by Molecular Absorption SpectrometryE 275 Practice for Describing and Measuring Performanceof Ultraviolet, Visible, and Near-Infrared Spectrophotom-eters3. Terminology3.1 DefinitionsFor definition of terms used in these testmethods, refer to Terminology D 1129.1These test m
12、ethods 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 Oct. 1, 2008. Published October 2008. Originallyapproved in 1977. Last previous edition approved in 2003 as D 3559 03.2P
13、latte, 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,” Techniques ofWater-Resources Investigations of the U. S. G
14、eological Survey , 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 Summary page onthe ASTM website.1Copyright ASTM Intern
15、ational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2 total recoverable leadan arbitrary analytical 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 t
16、est for lead is necessary because it is a toxicant andbecause there 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 Reag
17、ents5.1 Reagent grade chemicals shall be used in all tests.Unless 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 reage
18、nt isof sufficiently high purity to permit its use without lesseningthe 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 asce
19、rtained that the water is of sufficientlyhigh purity to permit its 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 1066and Prac
20、tices D 3370, as applicable.6.2 Samples shall 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
21、METHOD AATOMIC ABSORPTION,DIRECT7. Scope7.1 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 gr
22、eater than 10 mg/L by dilution of thesample.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
23、 fol-lowing hydrochloric-nitric acid digestion 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 Met
24、hods D 858), nickel (Test Methods D 1886), and 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
25、 prevents conversion of thelead to the atomic 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-extractionproce
26、dure (Test Method B).9.2.1 The equipment manufacturers 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 o
27、ther than 283.3 nm may be used ifthey have been 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
28、substances, is the usualoxidant.10.4 Fuel:10.4.1 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 cont
29、aining aspecial proprietary solvent rather than 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 controll
30、ed operating pressure of the instrument by suitablevalves.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. Warning: WhenHCl is distilled
31、, an azeotropic mixture is formed (approximately 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)Commercially purchase or dissolve
32、 1.5999 g of lead nitrate (Pb4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, 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
33、 the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D3559082(NO3)2) in a mixture of 10 mL of HNO3(sp gr 1.42) and 100mLof water. Dilute to 1 Lwith water. Warning: Lead salts aretoxic. Handle with care and avoid personal contamination.11.3 L
34、ead 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. Warning: Leadsalts are toxic. Never pipette by mouth. Pipette with the end ofa suction device or employ other conventional means ofquantitative meas
35、urement.11.4 Nitric Acid (sp gr 1.42)Concentrated nitric acid(HNO3).NOTE 3If 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. Standardizatio
36、n12.1 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(11.3) with HNO3(1 + 499). Prepare the standards each timethe test is to be performed.12.2 When determining total recoverable
37、lead, add 0.5 mLof HNO3(sp gr 1.42) to each blank and standard solution andproceed 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
38、 dissolved lead, pro-ceed 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
39、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 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 sam
40、ples 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 5For samples having appreciable amounts of suspended matteror dissolved matter, the amount of reduction in volume is left to thediscretion of t
41、he analyst.13.4 Cool and filter the samples through a suitable filtersuch as 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
42、 or concentration 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 thi
43、s study. One operator performed the analysis in quadru-plicate, 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.15.4 This section on precision and bias confor
44、ms to PracticeD277777which was in place at the time of collaborativetesting. Under the allowances made in 1.4 of D 2777 06,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 analytica
45、l values obtainedusing these test methods are valid and accurate within theconfidence 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 four working standards containingconcentrations of lead that
46、 bracket the expected sample con-centration, prior to analysis of samples, to 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 ensu
47、re contamination was not a problemduring the batch analysis.16.2.2 Verify instrument 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
48、 If calibration cannot be verified, recalibrate theinstrument.16.3 Initial Demonstration of Laboratory Capability:5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D19-1030.TABLE 1 Determination of Bias, DirectAmountAdded,mg/LAmo
49、untFound,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 noD355908316.3.1 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.16.3.2 Analyze seven replica
