1、Designation: D1691 12D1691 17Standard Test Methods forZinc in Water1This standard is issued under the fixed designation D1691; 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 indic
2、ates 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 U.S. Department of Defense.1. Scope*1.1 These test methods cover the determination of zinc in water. Section 26 on
3、Quality Control pertains to these test methods.Two test methods are given as follows:Test Method ConcentrationRange SectionsAAtomic Absorption, Direct 0.05 to 2 mg/L 8 16BAtomic Absorption,Chelation-Extraction20 to 200 g/L 17 25Test Method ConcentrationRangeSectionsAAtomic Absorption, Direct 0.05 to
4、 2 mg/L 8 16BAtomic Absorption,Chelation-Extraction20 to 200 g/L 17 251.2 Either dissolved or total recoverable zinc may be determined.1.3 These test methods have been used successfully with reagent grade water. See the specific test method for applicability toother matrices. It is the users respons
5、ibility to assure the validity of these test methods in other matrices.1.4 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values statedgivenin each system are mathematical conversions and may not be exact equivalents; therefore, each system sh
6、all be used independentlyof the other.parentheses are mathematical conversion to inch-pound units that are provided for information only and are notconsidered standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityo
7、f the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazard statements, see Section 6 and Note 612.7.1, Note 1021.7, and23.10Note 16.1.6 Two former colorimetric test methods were discontin
8、ued. Refer to Appendix X1 for historical information.1.7 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby
9、the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D858 Test Methods for Manganese in WaterD1066 Practice for Sampling SteamD1068 Test Methods for Iron in WaterD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD16
10、87 Test Methods for Chromium in WaterD1688 Test Methods for Copper in Water1 These test methods are under the jurisdiction of ASTM Committee D19 on Water and are the direct responsibility of Subcommittee D19.05 on Inorganic Constituentsin Water.Current edition approved Sept. 1, 2012June 1, 2017. Pub
11、lished September 2012June 2017. Originally approved in 1959. Last previous edition approved in 20022012 asD1691 02D1691 12.(2007)E01. DOI: 10.1520/D1691-12.10.1520/D1691-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For An
12、nual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not b
13、e technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end o
14、f this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D1886 Test Methods for Nickel in WaterD1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission SpectroscopyD2777 Practice for Determinat
15、ion of Precision and Bias of Applicable 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 WaterD4841 Practice for Estimation of Holding Time for Wate
16、r Samples Containing Organic and Inorganic ConstituentsD5673 Test Method for Elements in Water by Inductively Coupled PlasmaMass SpectrometryD5810 Guide for Spiking into Aqueous SamplesD5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis3. Terminolog
17、y3.1 DefinitionsDefinitions: For definitions of terms used in these test methods, refer to Terminology D1129.3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.3.2 Definitions:3.2.1 continuing calibration blank, na solution containing no analytes (of interest) which is
18、used to verify blank response andfreedom from carryover.3.2.2 continuing calibration verification, na solution (or set of solutions) of known concentration used to verify freedom fromexcessive instrumental drift; the concentration is to cover the range of calibration curve.3.2.3 total recoverable zi
19、nc, nan arbitrarya descriptive analytical term relating to the recoverable form of zinc that isdeterminable by the digestion method that is included in the Procedure.this test standard.4. Significance and Use4.1 Zinc is an essential and beneficial element in body growth. Concentrations above 5 mg/L
20、can cause a bitter astringent tasteand opalescence in alkaline waters. The zinc concentration of U.S. drinking waters varies between 0.06 and 7.0 mg/L with a meanof 1.33 mg/L. Zinc most commonly enters the domestic water supply from deterioration of galvanized iron and dezincification ofbrass. Zinc
21、in water also may result from industrial water pollution.34.2 ICP-MS or ICP-AES may also be appropriate but at a higher instrument cost. See Test Methods D5673 and D1976.5. Purity of Reagents5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all r
22、eagents shall conformto the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening
23、the accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming toSpecification D1193, Type I. Other reagent water types may be used, provided it is first ascertained that the water is of sufficientlyhigh purit
24、y to permit its use without adversely affecting the bias and precision of the test method. Type II water was specified atthe time of round-robin testing of this test method.6. Hazards6.1 Although zinc is nontoxic to man, these test methods require the use of certain other toxic and hazardous reagent
25、s andmaterials. Each should be used with care and exerting proper precautions.7. Sampling7.1 Collect the sample in accordance with PracticePractices D1066 and Practices D3370, as applicable.7.2 Samples shall be preserved with nitric acid (HNO3) (sp gr 1.42) to a pH of 2 or less immediately at the ti
26、me of collection,normally about 2 mL/L of HNO3. If only dissolved zinc is to be determined, the sample, shall be filtered through a 0.45-mmembrane filter before acidification. The holding time for samples may be calculated in accordance with Practice D4841.NOTE 1Alternatively, the pH may be adjusted
27、 in the laboratory if the sample is returned within 14 days. within 14 days of collection. However, acid3 “Standard Methods for the Examination of Water and Wastewater,” 16th edition, 1985, APHA, AWWA-WPCF.4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Wash
28、ington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D1691 1
29、72must be added at least 24 hours before analysis to dissolve any metals that adsorb to the container walls. This could reduce hazards of working with acidsin the field when appropriate.TEST METHOD AATOMIC ABSORPTION, DIRECT8. Scope8.1 This test method covers the determination of dissolved and total
30、 recoverable zinc in most waters and wastewaters.8.2 This test method is applicable in the range from 0.05 to 2.0 mg/L of zinc. The range may be extended to concentrationsgreater than 2.0 mg/L by dilution of the sample.8.3 This test method has been used successfully with reagent grade water, river w
31、ater, wastewater, ground water, tap water, lakewater, refinery effluent. The information on precision and bias may not apply to other waters.8. Scope8.1 This test method covers the determination of dissolved and total recoverable zinc in most waters and wastewaters.8.2 This test method is applicable
32、 in the range from 0.05 to 2.0 mg/L of zinc. The range may be extended to concentrationsgreater than 2.0 mg/L by dilution of the sample.8.3 This test method has been used successfully with reagent grade water, river water, wastewater, ground water, tap water, lakewater, refinery effluent. The inform
33、ation on precision and bias may not apply to other waters.9. Summary of Test Method9.1 Zinc is determined by atomic absorption spectrophotometry. Dissolved zinc is determined by aspirating a portion of thefiltered and preserved sample directly with no pretreatment. Total recoverable zinc is determin
34、ed by aspirating the samplefollowing hydrochloric-nitric acid digestion and filtration. The same digestion procedure is used to determine total recoverablecadmium (Test Methods D3557), chromium, (Test Methods D1687), cobalt (Test Methods D3558), copper (Test Methods D1688),iron (Test Methods D1068),
35、 lead (Test Methods D3559), manganese (Test Methods D858), and nickel (Test Methods D1886).10. Interferences10.1 Sodium, potassium, sulfate, and chloride (9000 mg/L each), calcium and magnesium (4000 mg/L each), nitrate (2000mg/L), and cadmium, lead, copper, nickel, cobalt, and chromium (10 mg/L eac
36、h) do not interfere.10.2 Background correction or a chelation-extraction procedure (see Test Method B) may be necessary to determine low levelsof zinc in some waters.NOTE 2Instrument manufacturers instructions for use of the specific correction technique should be followed.11. Apparatus11.1 Atomic A
37、bsorption Spectrophotometer , Spectrophotometer, for use at 213.9 nm.NOTE 3The manufacturers instructions should be followed for all instrumental parameters. Wavelengths other than 213.9 nm may be used if theyhave been determined to be equally suitable.11.1.1 Zinc Light SourceHollow-cathode lamps or
38、 electrodeless discharge lamps have been found satisfactory.11.2 OxidantSee 12.6.11.3 FuelSee 12.7.11.2 Pressure-Reducing ValvesThe supplies of fuel and oxidant shall be maintained at pressures somewhat higher than thecontrolled operating pressure of the instrument by suitable valves.12. Reagents an
39、d Materials12.1 Hydrochloric Acid (sp gr 1.19)Concentrated hydrochloric acid (HCl).NOTE 4If the reagent blank concentration is greater than the method detection limit, distill the HCl or use a spectrograde acid.WarningWhen HClis distilled an azeotropic mixture is obtained (approximately 6 N HCl). Th
40、erefore, whenever concentrated HCl is specified in the preparation of a reagentor in the procedure, use double the amount specified if a distilled acid is used.(WarningWhen HCl is distilled an azeotropic mixture is obtained (approximately 6 N HCl). Therefore, wheneverconcentrated HCl is specified in
41、 the preparation of a reagent or in the procedure, use double the amount specified if a distilled acidis used.)12.2 Nitric Acid (sp gr 1.42)Concentrated nitric acid (HNO3).NOTE 5If the reagent blank concentration is greater than the method detection limit, distill the HNO3 or use a trace metal grade
42、 acid.12.3 Nitric Acid (1 +499)Add 1 volume of HNO3 (sp gr 1.42) to 499 volumes of water.D1691 17312.4 Zinc Solution, Stock (1 mL = 1.0 mg Zn)Dissolve 1.245 g of zinc oxide (ZnO) in a mixture of 10 mL of HNO3 (sp gr1.42) and 10 mLof water. Dilute to 1 Lwith water.Apurchased zinc stock solution of ap
43、propriate known purity is also acceptable.12.5 Zinc Solution, Standard (1 mL = 0.1 mg Zn)Dilute 100.0 mL of the zinc stock solution and 1 mL of HNO3 (sp gr 1.42)to 1 L with water.12.6 Oxidant:12.6.1 Air, which has been passed through a suitable filter to remove oil, water, and other foreign substanc
44、es, is the usualoxidant.12.7 Fuel:12.7.1 AcetyleneStandard, commercially available acetylene is the usual fuel.Acetone, always present in acetylene cylinders,can affect analytical results.The cylinder should be replaced at 345 kPa (50 psi). (Warning“Purified” grade acetylene containinga special prop
45、rietary solvent rather than acetone should not be used with poly(vinyl chloride) tubing as weakening of the tubingwalls can cause a potentially hazardous situation.)NOTE 6Warning: “Purified” grade acetylene containing a special proprietary solvent rather than acetone should not be used with poly(vin
46、yl chloride)tubing as weakening of the tubing walls can cause a potentially hazardous situation.12.8 Filter PaperPurchase suitable filter paper. Typically the filter papers have a pore size of 0.45-m membrane. Materialsuch as fine-textured, acid-washed, ashless paper, or glass fiber paper are accept
47、able. The user must first ascertain that the filterpaper is of sufficient purity to use without adversely affecting the bias and precision of the test method.13. Standardization13.1 Prepare 100 mL each of a blank and at least four standard solutions to bracket the expected zinc concentration range o
48、fthe samples to be analyzed by diluting the standard zinc solution (12.5) with HNO3 (1 +499). Prepare the standards each time thetest is to be performed and select so as to give zero, middle, and maximum points for an analytical curve.curve or as determinedby Practice D4841.13.2 When determining tot
49、al recoverable zinc, add 0.5 mL of HNO3 (sp gr 1.42) to each blank and standard solution andproceed as directed in 14.214.3 14.414.5.After the digestion of the blank and standard solutions has been completed in 14.414.5,return to 13.3 to complete the standardization for total recoverable determinations. To determine dissolved zinc, proceed with 13.3.13.3 Aspirate the blank and standards, and record the absorbance or concentration of each at 213.9 nm.Aspirate HNO3 (1 +499)between each standard.13.4 Prepare Read directly in concent
