1、Designation: D 1886 03Standard Test Methods forNickel in Water1This standard is issued under the fixed designation D 1886; 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
2、 the 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 methods2, 3, 4cover the atomic absorptiondetermination of nickel in wate
3、r and wastewaters. Three testmethods are given as follows:ConcentrationRange SectionsTest Method AAtomic Absorption,Direct 0.1 to 10 mg/L 7-16Test Method BAtomic Absorption,Chelation-Extraction 10 to 1000 g/L 17-26Test Method CAtomic Absorption,Graphite Furnace 5 to 100 g/L 27-361.2 Test Methods A,
4、B, and C have been used successfullywith reagent grade water and natural waters. Evaluation of TestMethod C was also made in condensate from a medium Btucoal gasification process. It is the users responsibility toensure the validity of these test methods for other matrices.1.3 This standard does not
5、 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 the applica-bility of regulatory limitations prior to use. For specific hazardsstatements, see Note
6、 4, 11.7.1, 21.9, 23.7, and 23.10.1.4 Two former colorimetric test methods were discontin-ued. Refer to Appendix X1 for historical information.2. Referenced Documents2.1 ASTM Standards:D 858 Test Methods for Manganese in Water5D 1066 Practice for Sampling Steam5D 1068 Test Methods for Iron in Water5
7、D 1129 Terminology Relating to Water5D 1192 Specification for Equipment for Sampling Waterand Steam in Closed Conduits5D 1193 Specification for Reagent Water5D 1687 Test Methods for Chromium in Water5D 1688 Test Methods for Copper in Water5D 1691 Test Methods for Zinc in Water5D 2777 Practice for De
8、termination of Precision and Bias ofApplicable Methods of Committee D-19 on Water5D 3370 Practices for Sampling Water from Closed Con-duits5D 3557 Test Methods for Cadmium in Water5D 3558 Test Methods for Cobalt in WaterD 3559 Test Methods for Lead in Water5D 3919 Practice for Measuring Trace Elemen
9、ts in Water byGraphite Furnace Atomic Absorption Spectrophotometry5D 4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and Inorganic Constituents5D 5810 Guide for Spiking into Aqueous Samples5D 5847 Practice for Writing Quality Control Specificationsfor Standard Test M
10、ethods for Water Analysis63. Terminology3.1 Definitions:3.1.1 For definitions of terms used in these test methods,refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 total recoverable nickelan arbitrary analytical termrelating to the recoverable forms of nickel that
11、are determin-able by the digestion method that is included in these testmethods.4. Significance and Use4.1 Elemental constituents in potable water, receiving water,and wastewater need to be identified for support of effectivepollution control programs. Test Methods A, B, and C providethe techniques
12、necessary to make such measurements.4.2 Nickel is considered to be relatively nontoxic to manand a limit for nickel is not included in the EPA National1These test methods are under the jurisdiction of ASTM Committee D19 onWater and are the direct responsibility of Subcommittee D19.05 on InorganicCon
13、stituents in Water.Current edition approved June 10, 2003. Published July 2003. Originallyapproved in 1961. Last previous edition approved in 1998 as D1886 94 (1998).2Chilton, J. M., “Simultaneous Colorimetric Determination of Copper, Cobalt,and Nickel as Diethyldithiocarbamates,”Analytical Chemistr
14、y, Vol 25, 1953, pp.12741275.3Platte, J.A., and Marcy, V. M., “ANew Tool for the Water Chemist,” IndustrialWater Engineering, May 1965.4Brown, E., Skougstad, M. W., and Fishman, M. J., “Methods for Collection andAnalysis of Water Samples for Dissolved Minerals and Gases,” Techniques ofWater-Resource
15、s Investigations of the U.S. Geological Survey, Book 5, Chapter ,1970, p. 115.5Annual Book of ASTM Standards, Vol 11.01.6Annual Book of ASTM Standards, Vol 11.02.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West
16、Conshohocken, PA 19428-2959, United States.Interim Primary Drinking Water Regulations.7The toxicity ofnickel to aquatic life indicates tolerances that vary widely andthat are influenced by species, pH, synergistic effects, and otherfactors.4.3 Nickel is a silver-white metallic element seldom occur-r
17、ing in nature in the elemental form. Nickel salts are solubleand can occur as a leachate from nickel-bearing ores. Nickelsalts are used in metal-plating and may be discharged tosurface or ground waters.5. Purity of Reagents5.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indic
18、ated, it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society where suchspecifications are available.8Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit
19、 its use without lessening the accuracy ofthe determination.5.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D 1193, Type I. Other reagent water types maybe used, provided it is first ascertained that the water is
20、ofsufficiently high purity to permit its use without lessening thebias and precision of the determination. Type II water wasspecified at the time of the round-robin testing of this testmethod.6. Sampling6.1 Collect the sample in accordance with Practice D 1066,Specification D 1192, or Practices D 33
21、70, 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. If only dissolved nickel is to be determined, thesample shall be filtered through a 0.45-m membrane filterbefore acidification. The holding time for
22、 samples may becalculated in accordance with Practice D 4841.TEST METHOD AATOMIC ABSORPTION, DIRECT7. Scope7.1 This test method covers the determination of dissolvedand total recoverable nickel and has been used successfullywith reagent water, tap water, river water, lake water, groundwater, a refin
23、ery effluent, and a wastewater.7.2 This test method is applicable in the range from 0.1 to10 mg/L of nickel. The range may be extended upward bydilution of the sample.8. Summary of Test Method8.1 Nickel is determined by atomic absorption spectropho-tometry. Dissolved nickel is determined by aspirati
24、ng thefiltered sample directly with no pretreatment. Total recoverablenickel is determined by aspirating the sample followinghydrochloric-nitric acid digestion and filtration. The samedigestion procedure is used for cadmium (Test MethodsD 3557), chromium (Test Methods D 1687), cobalt (Test Meth-ods
25、D 3558), copper (Test Methods D 1688), iron (Test Meth-ods D 1068), lead (Test Methods D 3559), manganese (TestMethods D 858), and zinc (Test Methods D 1691).9. Interferences9.1 Sodium, potassium, sulfate, and chloride (9000 mg/Leach), calcium, magnesium and iron (4000 mg/L each), nitrate(2000 mg/L)
26、, and cadmium, lead, copper, zinc, cobalt, andchromium (10 mg/L each) do not interfere.NOTE 1Background correction by techniques such as a continuumsource, nonabsorbing lines, or chelation-extraction, may be necessary forlow levels of nickel for some types of water. Instrument manufacturersinstructi
27、ons for use of the specific correction technique should befollowed.10. Apparatus10.1 Atomic Absorption Spectrophotometer, for use at 232.0nm.NOTE 2The manufacturers instructions should be followed for allinstrumental parameters. Wavelengths other than 232.0 nm may be used ifthey have been determined
28、 to be equally suitable.10.2 Nickel Hollow-Cathode LampMultielement hollow-cathode lamps are available and also have been found satis-factory.10.3 Pressure-Reducing ValvesThe supplies of fuel andoxidant shall be maintained at pressures somewhat higher thanthe controlled operating pressure of the ins
29、trument by suitablevalves.11. Reagents and Materials11.1 Hydrochloric Acid (sp gr 1.19)Concentrated hydro-chloric acid (HCl).NOTE 3If a high reagent blank is obtained, distill the HCl or use aspectrograde acid.NOTE 4When HCl is distilled, an azeotropic mixture is formed (;6NHCl). Therefore, whenever
30、 concentrated HCl is used in the preparation ofreagents or in the procedure, use twice the volume of the distilled HCl.11.2 Nitric Acid (sp gr 1.42)Concentrated nitric acid(HNO3).NOTE 5If a high reagent blank is obtained, distill the HNO3or use aspectrograde acid.11.3 Nitric Acid (1 + 499)Add 1 volu
31、me HNO3(sp gr1.42) to 499 volumes of water.11.4 Nickel Solution, Stock (1.0 mL = 1.0 mg Ni)Dissolve4.953 g of nickelous nitrate Ni(NO3)26H2O in a mixture of10 mL of HNO3(sp gr 1.42) and 100 mL of water. Dilute to 1L with water.11.5 Nickel Solution, Standard (1 mL = 0.1 mg Ni)Dilute100.0 mL of the st
32、ock nickel solution and 1 mL of HNO3to 1L with water.7EPA Publication No. EPA-570/9-76-003 was originally published in 1976, andamended in 1980. Contact the Environmental Protection Agency, 401 “M” ST.,S.W., Washington, DC 20406 for availability.8Reagent Chemicals, American Chemical Society Specific
33、ations, 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 Pharmacopeiaand National Formulary, U.S. Pharmaceutical Conventi
34、on, Inc. (USPC), Rockville,MD.D 1886 03211.6 Oxidant:11.6.1 Air, which has been passed through a suitable filter toremove oil, water, and other foreign substances is the usualoxidant.11.7 Fuel:11.7.1 AcetyleneStandard, commercially available acety-lene is the usual fuel. Acetone, always present in a
35、cetylenecylinders, can affect analytical results. The cylinder should bereplaced at 50 psig (345 kPa). (Warning“Purified” gradeacetylene containing a special proprietary solvent rather thanacetone should not be used with poly(vinyl chloride) tubing asweakening of the walls can cause a potentially ha
36、zardoussituation.)12. Standardization12.1 Prepare a blank and at least four standard solutions tobracket the expected nickel concentration range of the samplesto be analyzed by diluting the standard nickel solution withHNO3(1 + 499) as described in 11.5. Prepare the standards(100 mL) each time the t
37、est is to be performed.12.2 For total recoverable nickel add 0.5 mL of HNO3(sp gr1.42) and proceed as directed in 13.2 through 13.4. Fordissolved nickel proceed with 13.5.12.3 Atomize the blank and standards and record the instru-ment readings. Atomize HNO3(1 + 499) between each stan-dard.12.4 Prepa
38、re 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 the instrument.13. Procedure13.1 Measure 100.0 mL of a well-mixed acidified sampleinto a 125-mL beaker or
39、 flask.NOTE 6If only dissolved nickel 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 hotplate in awell-ventilated fume hood until the volume has been reducedto 15 to 20 mL, making certain that the samples do not boil.NOT
40、E 7For samples with high levels of suspended matter or dissolvedsolids, the amount of reduction in volume is left to the discretion of theanalyst.13.4 Cool and filter the samples through a suitable filter,such as fine-textured, acid-washed, ashless paper, into 100-mLvolumetric flasks. Wash the filte
41、r paper two or three times withwater and bring filtrate to volume.13.5 Atomize each filtered and acidified sample and deter-mine its absorbance or concentration. Atomize HNO3(1 + 499)between samples.14. Calculation14.1 Calculate the concentration of nickel in each sample, inmilligrams per litre, usi
42、ng 12.4.15. Precision and Bias915.1 The precision of this test method was tested by elevenlaboratories in reagent water, natural waters, a refinery effluentand in a wastewater. Five laboratories reported data for twooperators. The precision of this test method is shown in Table1; the bias is shown i
43、n Table 2.15.2 It is the users responsibility to ensure the validity ofthis test method for waters of untested matrices.15.3 This section on precision and bias conforms to PracticeD 2777 77 which was in place at the time of collaborativetesting. Under the allowances made in 1.4 of D 2777 98,these pr
44、ecision 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 theconfidence limits of the test, the following QC procedur
45、es mustbe followed when analyzing nickel.16.2 Calibration and Calibration Verification16.2.1 Analyze at least three working standards containingconcentrations of nickel that bracket the expected sampleconcentration, prior to analysis of samples, to calibrate theinstrument. The calibration correlatio
46、n 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 instrument calibration after standardization byanalyzin
47、g 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 Demonstration of Laboratory Capability16.3.1 If a labor
48、atory has not performed the test before, or ifthere has been a major change in the measurement system, forexample, new analyst, new instrument, and so forth, a precisionand bias study must be performed to demonstrate laboratorycapability.16.3.2 Analyze seven replicates of a standard solutionprepared
49、 from an Independent Reference Material containing amidrange concentration of nickel. The matrix and chemistry ofthe solution should be equivalent to the solution used in thecollaborative study. Each replicate must be taken through the9Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D191038.TABLE 1 Precision and Concentration, Direct Aspiration(Test Method A)Reagent Water:Concentration (X), mg/L 7.74 0.84 3.93ST0.502 0.102 0.383SO0.261 0.045 0.324Natural Water:Concentration (X
