ASTM D1886-14

Designation: D1886 − 14Standard Test Methods forNickel in Water1This standard is issued under the fixed designation D1886; 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 year of last reapproval. Asuperscript epsilon (´) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 These test methods2, 3, 4cover the atomic absorptiondetermination of nickel in water and wastewaters. Three testmethods are given as follows:ConcentrationRange SectionsTest Method A—Atomic Absorption,Direct 0.1 to 10 mg/L 7–16Test Method B—Atomic Absorption,Chelation-Extraction 10 to 1000 µg/L 17–26Test Method C—Atomic Absorption,Graphite Furnace 5 to 100 µg/L 27–361.2 Test Methods A, 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 user’s responsibility toensure the validity of these test methods for other matrices.1.3 The values stated in SI units are to be regarded asstandard. The values given in parentheses are mathematicalconversion to inch-pound units that are provided for informa-tion only and are not considered standard.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 practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardsstatements, see Note 5,11.8.1, 21.11, 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 Standards:5D858 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 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 WaterD3559 Test Methods for Lead in WaterD3919 Practice for 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 Plasma—Mass SpectrometryD5810 Guide for Spiking into Aqueous SamplesD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water Analysis3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in these test methods,refer to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 total recoverable nickel, n—a descriptive term relatingto the nickel forms recovered in the acid-digestion procedurespecified in these 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 Oct. 1, 2014. Published November 2014. Originallyapproved in 1961. Last previous edition approved in 2008 as D1886 – 08. DOI:10.1520/D1886-14.2Chilton, J. M., “Simultaneous Colorimetric Determination of Copper, Cobalt,and Nickel as Diethyldithiocarbamates,” Analytical Chemistry, Vol 25, 1953, pp.1274–1275.3Platte, 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-Resources Investigations of the U.S. Geological Survey, Book 5, 1970, p. 115.5For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at service@astm.org. For Annual Book of ASTMStandards volume information, refer to the standard’s Document Summary 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 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 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 NationalInterim Primary Drinking Water Regulations.6The 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-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 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 grades 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 Water—Unless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D1193, 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. Sampling6.1 Collect the sample in accordance with Practice D1066or Practices D3370, 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-µm membrane filterbefore acidification. The holding time for samples may becalculated in accordance with Practice D4841.NOTE 1—Alternatively, the pH may be adjusted in the laboratory if thesample 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 A—ATOMIC 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 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 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 cadmium (Test MethodsD3557), chromium (Test Methods D1687), cobalt (Test Meth-ods D3558), copper (Test Methods D1688), iron (Test MethodsD1068), lead (Test Methods D3559), manganese (Test Meth-ods D858), and zinc (Test Methods D1691).9. Interferences9.1 Sodium, potassium, sulfate, and chloride (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 2—Background 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 manufacturer’sinstructions for use of the specific correction technique should befollowed.10. Apparatus10.1 Atomic Absorption Spectrophotometer, for use at 232.0nm.NOTE 3—The manufacturer’s instructions should be followed for allinstrumental parameters. Wavelengths other than 232.0 nm may be used ifthey have been determined to be equally suitable.10.2 Nickel Hollow-Cathode Lamp—Multielement hollow-cathode lamps are available and also have been found satis-factory.10.3 Pressure-Reducing Valves—The supplies of fuel andoxidant shall be maintained at pressures somewhat higher thanthe controlled operating pressure of the instrument by suitablevalves.11. Reagents and Materials11.1 Filter Paper—Purchase suitable filter paper. Typicallythe filter papers have a pore size of 0.45-µm 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 purity to use withoutadversely affecting the bias and precision of the test method.6EPA 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.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 Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.D1886 − 14211.2 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-chloric acid (HCl).NOTE 4—If a high reagent blank is obtained, distill the HCl or use aspectrograde acid.NOTE 5—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.11.3 Nitric Acid (sp gr 1.42)—Concentrated nitric acid(HNO3).NOTE 6—If a high reagent blank is obtained, distill the HNO3or use aspectrograde acid.11.4 Nitric Acid (1 + 499)—Add 1 volume HNO3(sp gr1.42) to 499 volumes of water.11.5 Nickel Solution, Stock (1.0 mL = 1.0 mg Ni)—Commercially purchase or dissolve 4.953 g of nickelous nitrate[Ni(NO3)2·6H2O] in a mixture of 10 mL of HNO3(sp gr 1.42)and 100 mL of water. Dilute to 1 L with water. A purchasednickel stock solution of appropriate known purity is acceptable.11.6 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.11.7 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 Acetylene—Standard, commercially available acety-lene is the usual fuel. Acetone, always present in acetylenecylinders, can affect analytical results. The cylinder should bereplaced at 345 kPa (50 psig). (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 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 standard nickel solution withHNO3(1 + 499) as described in 11.6. Prepare the standards(100 mL) each time the test is to be performed or as determinedby Practice D4841.12.2 For total recoverable nickel add 0.5 mLof HNO3(sp gr1.42) and proceed as directed in 13.2 through 13.4. Fordissolved nickel proceed with 13.5.12.3 Analyze at least four working standards containingconcentrations of nickel that bracket the expected sampleconcentration, prior to analysis of samples, to calibrate theinstrument. Atomize the blank and standards and record theinstrument readings. Atomize HNO3(1 + 499) between eachstandard.12.4 Read directly in concentration if this capability isprovided with the instrument or prepare an analytical curve byplotting the absorbance versus the concentration for eachstandard on linear graph paper or use a computer.13. Procedure13.1 Measure 100.0 mL of a well-mixed acidified sampleinto a 125-mL beaker or flask.NOTE 7—If only dissolved nickel 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 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.NOTE 8—For samples with high levels of suspended matter or dissolvedsolids, the amount of reduction in volume is left to the discretion of theanalyst.NOTE 9—Many 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 of temperature (65°C to 85°C) across all positions of the block. Fortrace metals analysis, the digestion tubes should be constructed ofpolypropylene and have a volume accuracy of at least 0.5 %. All lots oftubes should come with a certificate of analysis to demonstrate suitabilityfor their intended purpose.13.4 Cool and filter the samples through a suitable filter(11.1), such as fine-textured, acid-washed, ashless paper, into100-mL volumetric flasks. Wash the filter paper two or threetimes with water 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, 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 laboratories 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 user’s responsibility to ensure the validity ofthis test method for waters of untested matrices.15.3 This section on precision and bias conforms to PracticeD2777 – 77 which was in place at the time of collaborativetesting. Under the allowances made in 1.4 of Practice8Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D19-1038. ContactASTM CustomerService at service@astm.org.TABLE 1 Precision and Concentration, Direct Aspiration(Test Method A)Reagent Water:Concentration (X¯), mg/