1、Designation: D 1886 08Standard 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 () 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 methods2, 3, 4cover the atomic absorptiondetermination of nickel in water
3、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, B,
4、 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 The values stated in SI
5、units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 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 p
6、ractices and determine the applica-bility of regulatory limitations prior to use. For specific hazardsstatements, see Note 4, 11.7.1, 21.9, 23.7, and 23.10.1.5 Two former colorimetric test methods were discontin-ued. Refer to Appendix X1 for historical information.2. Referenced Documents2.1 ASTM Sta
7、ndards:5D 858 Test Methods for Manganese in WaterD 1066 Practice for Sampling SteamD 1068 Test 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 Zi
8、nc in WaterD 2777 Practice for Determination of Precision 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 3559 Test Methods for Lead in WaterD 3919 Pra
9、ctice for Measuring Trace Elements in Water byGraphite Furnace Atomic Absorption SpectrophotometryD 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 Spec
10、ificationsfor Standard Test Methods for Water Analysis3. Terminology3.1 Definitions: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 Oct. 1, 2008. Published
11、 October 2008. Originallyapproved in 1961. Last previous edition approved in 2003 as D 1886 03.2Chilton, J. M., “Simultaneous Colorimetric Determination of Copper, Cobalt,and Nickel as Diethyldithiocarbamates,” Analytical Chemistry, Vol 25, 1953, pp.12741275.3Platte, J.A., and Marcy, V. M., “ANew To
12、ol 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-Resources Investigations of the U.S. Geological Survey, Book 5, 1970, p. 115.5
13、For 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 International, 100 Barr Harbor Drive, PO Box C
14、700, West Conshohocken, PA 19428-2959, United States.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 are
15、 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 nec
16、essary 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 NationalInterim Primary Drinking Water Regulations.6The toxicity ofnickel to aquatic life indicates tolerances that vary widely andthat are influenced by specie
17、s, pH, synergistic effects, and otherfactors.4.3 Nickel is a silver-white metallic element seldom occur-ring 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
18、waters.5. Purity of Reagents5.1 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 where suchspecifications are available.7Other gra
19、des may be used, pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit 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 Specificatio
20、n D 1193, Type I. Other reagent water types maybe used, provided it is first ascertained that the water is 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
21、. Sampling6.1 Collect the sample in accordance with Practice D 1066or Practices 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. If only dissolved nickel is to be determined, thesample shall be
22、 filtered through a 0.45-m membrane filterbefore acidification. The holding time for 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 succ
23、essfullywith reagent water, tap water, river water, lake water, groundwater, a refinery 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
24、 by atomic absorption spectropho-tometry. Dissolved nickel is determined by aspirating 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
25、cadmium (Test MethodsD 3557), chromium (Test Methods D 1687), cobalt (Test Meth-ods 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 chlori
26、de (9000 mg/Leach), calcium, magnesium and iron (4000 mg/L each), nitrate(2000 mg/L), 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 necessar
27、y forlow levels of nickel for some types of water. Instrument manufacturersinstructions 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
28、 parameters. Wavelengths other than 232.0 nm may be used ifthey have been determined 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 main
29、tained at pressures somewhat higher thanthe controlled operating pressure of the instrument 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 4
30、When HCl is distilled, an azeotropic mixture is formed (;6NHCl). Therefore, whenever concentrated HCl is used in the preparation ofreagents or in the procedure, use twice the volume of the distilled HCl.6EPA Publication No. EPA-570/9-76-003 was originally published in 1976, andamended in 1980. Conta
31、ct the Environmental Protection Agency, 401 “M” ST.,S.W., Washington, DC 20406 for availability.7Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual St
32、andards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D188608211.2 Nitric Acid (sp gr 1.42)Concentrated nitric acid(HNO3).NOTE 5If a high reagent blank is obtained, distill th
33、e HNO3or use aspectrograde acid.11.3 Nitric Acid (1 + 499)Add 1 volume HNO3(sp gr1.42) to 499 volumes of water.11.4 Nickel Solution, Stock (1.0 mL = 1.0 mg Ni)Commercially purchase or dissolve 4.953 g of nickelous nitrateNi(NO3)26H2O in a mixture of 10 mL of HNO3(sp gr 1.42)and 100 mL of water. Dilu
34、te to 1 L with water.11.5 Nickel Solution, Standard (1 mL = 0.1 mg Ni)Dilute100.0 mL of the stock nickel solution and 1 mL of HNO3to 1L with water.11.6 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:
35、11.7.1 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). Warning: “Purified” gradeacetylene containing a special proprietary solvent rather thanace
36、tone should not be used with poly(vinyl chloride) tubing asweakening of the walls can cause a potentially hazardoussituation.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 sta
37、ndard nickel solution withHNO3(1 + 499) as described in 11.5. Prepare the standards(100 mL) each time the test 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
38、 and standards and record the instru-ment readings. Atomize HNO3(1 + 499) between each stan-dard.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 wit
39、h the instrument.13. Procedure13.1 Measure 100.0 mL of a well-mixed acidified sampleinto a 125-mL beaker or 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
40、 fume hood until the volume has been reducedto 15 to 20 mL, making certain that the samples do not boil.NOTE 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 suit
41、able filter,such as fine-textured, acid-washed, ashless paper, into 100-mLvolumetric flasks. Wash the filter 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 sa
42、mples.14. Calculation14.1 Calculate the concentration of nickel in each sample, inmilligrams per litre, using 12.4.15. Precision and Bias815.1 The precision of this test method was tested by elevenlaboratories in reagent water, natural waters, a refinery effluentand in a wastewater. Five laboratorie
43、s reported data for twooperators. The precision of this test method is shown in Table1; the bias is shown in 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 whi
44、ch was in place at the time of collaborativetesting. Under the allowances made in 1.4 of PracticeD 2777 06, these precision and bias data do meet existingrequirements of interlaboratory studies of Committee D19 testmethods.16. Quality Control16.1 In order to be certain that analytical values obtaine
45、dusing these test methods are valid and accurate within theconfidence limits of the test, the following QC procedures mustbe followed when analyzing nickel.16.2 Calibration and Calibration Verification16.2.1 Analyze at least four working standards containingconcentrations of nickel that bracket the
46、expected sampleconcentration, 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 ensure contaminatio
47、n 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 If calibration
48、cannot be verified, recalibrate theinstrument.8Supporting 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.
49、502 0.102 0.383SO0.261 0.045 0.324Natural Water:Concentration (X), mg/L 7.74 0.84 3.87ST0.629 0.108 0.401SO0.420 0.067 0.192D188608316.3 Initial Demonstration of Laboratory Capability16.3.1 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, and so forth, a precisionand bias study must be performed to demonstrate laboratorycapability.16.3.2 Analyze seven replicates of a standard solutionprepared from an Independent Reference Material containing
