1、Designation: D858 12D858 17Standard Test Methods forManganese in Water1This standard is issued under the fixed designation D858; 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 ind
2、icates 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 atomic absorption determination of dissolved
3、 and total recoverable manganese in water andcertain wastewaters. Section 34 on Quality Control pertains to these test methods. Three test methods are given as follows:Test Method Concentration Range SectionsAAtomic Absorption,Direct0.1 to 5 mg/L 7 to 15AAtomic Absorption,Direct0.1 to 5 mg/L 7 to 15
4、BAtomic Absorption,Chelation-Extraction10 to 500 g/L 16 to 24BAtomic Absorption,Chelation-Extraction10 to 500 g/L 16 to 24CAtomic Absorption,Graphite Furnace5 to 50 g/L 25 to 33CAtomic Absorption,Graphite Furnace5 to 50 g/L 25 to 331.2 Test MethodsA, B, and C were used successfully on reagent grade
5、and natural waters. Other matrices used in the study werebrine (Test Method B), effluent from a wood treatment plant, and condensate from a medium BTU coal gasification process (TestMethod C). It is the users responsibility to ensure the validity of a test method for waters of untested matrices.1.3
6、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 shall be used independentlyof the other.parentheses are mathematical conversi
7、on to inch-pound units that are provided for information only and are notconsidered standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health prac
8、tices and determine the applicability of regulatorylimitations prior to use. For specific hazard statements, see 11.7, 20.2, 20.9, and 22.1022.11.1.5 Former Test Method A (Colorimetric) was discontinued. For historical information, see Appendix X1.1.6 This international standard was developed in acc
9、ordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM
10、Standards:2D1066 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 Water1 These test methods are under the jurisdiction of ASTM Committee D19
11、on Water and are the direct responsibility of Subcommittee D19.05 on Inorganic Constituentsin Water.Current edition approved Sept. 1, 2012June 1, 2017. Published September 2012June 2017. Originally approved in 1945. Last previous edition approved in 20072012 asD858 07.D858 12. DOI: 10.1520/D0858-12.
12、10.1520/D0858-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual 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
13、 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 be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the
14、current versionof the standard as published by ASTM is to be considered the official document.*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 States1D1691 Test Methods for Zinc
15、 in WaterD1886 Test Methods for Nickel in WaterD1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission SpectroscopyD2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Cl
16、osed 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 by Graphite Furnace Atomic Absorption SpectrophotometryD4841 Practice for Estimation of Holding Time for Water Samples Co
17、ntaining 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. Terminology3.1 Definit
18、ions:3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.D858 1723.2 Definitions of Terms Specific to This Standard:3.2.1 continuing calibration blank, na solution containing no analytes (of interest) which is used to verify blank response andfreedom from carryover.3.2.2
19、 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 manganesemanganese, nan arbitrary analytical a descriptive term
20、 relating to the recoverable formsof manganese that are determinable by the digestion method that is included in the procedure.recovered in the acid digestionprocedure specified in this test standard.3.2 Definitions:3.2.1 For definitions of terms used in these test methods, refer to Terminology D112
21、9.4. 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 provide the techniques necessary to make such measurements.4.2 Although inhaled manganese dusts hav
22、e been reported to be toxic to humans, manganese normally is ingested as a tracenutrient in both food and water. Because it is considered to be relatively nontoxic to man, as well as aquatic life, a limit of 50 g/Lhas been established in the EPANational Secondary Drinking Water Regulations. This lim
23、it is based primarily on its ability to stainlaundry and produce objectionable tastes in beverages.4.3 Manganese does not occur naturally as a metal but is found in various salts and minerals, frequently in association with ironcompounds. Manganese is not mined in the United States except when manga
24、nese is contained in iron ores that are deliberatelyused to form ferro-manganese alloys. Manganese salts are used as fertilizer additives and are commonly found in surface andground waters.4.4 ICP-MS or ICP-AES may also be appropriate but at a higher instrument cost. See Test Methods D5673 and D1976
25、.5. Purity of Reagents5.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conformto the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such specifications areavailable. 3 Other grad
26、es may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming toSpecificatio
27、n D1193, Type I. Other reagent water types may be used, provided it is first ascertained that the water is of sufficientlyhigh purity to permit its use without lessening the bias and precision of the determination. Type II water was specified at the timeof round-robin testing of this test method.6.
28、Sampling6.1 Collect the sample in accordance with Practice D1066, or Practices D3370 as applicable.6.2 Samples shall be preserved with HNO3 (sp gr 1.42), normally about 2 mL/L, to a pH of 2 or less immediately at the timeof collection. If only dissolved manganese is to be determined, the sample shal
29、l be filtered through a 0.45-m (No. 325) membranefilter (11.8) before acidification. The holding time for samples may be calculated in accordance with Practice D4841.NOTE 1Alternatively, the pH may be adjusted in the laboratory if the sample is returned within 14 days. within 14 days of collection.
30、However, acidmust 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, DIRECT7. Scope7.1 This test method covers the determination of dissolve
31、d and total recoverable manganese and has been used successfully withreagent and natural water. It is the analysts responsibility to ensure the validity of the method in a particular matrix.7.2 This test method is applicable in the range from 0.1 to 5 mg/L of manganese. The range may be extended to
32、concentrationsgreater than 5 mg/L by dilution of the sample.3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals,
33、BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.D858 1737. Scope7.1 This test method covers the determination of dissolved and total recoverable manganese and has been used successfully withreagent and
34、 natural water. It is the analysts responsibility to ensure the validity of the method in a particular matrix.7.2 This test method is applicable in the range from 0.1 to 5 mg/L of manganese. The range may be extended to concentrationsgreater than 5 mg/L by dilution of the sample.8. Summary of Test M
35、ethod8.1 Manganese is determined by atomic absorption spectrophotometry. Dissolved manganese is determined by atomizing afiltered sample directly with no pretreatment. Total recoverable manganese in the sample is determined in a portion of the filtrateobtained after a hydrochloric-nitric acid digest
36、ion of the sample. The same digestion procedure is used to determine totalrecoverable cadmium (Test Methods D3557), chromium (Test Methods D1687), cobalt (Test Methods D3558), copper (TestMethods D1688), iron (Test Methods D1068), lead (Test Methods D3559), nickel (Test Methods D1886), and zinc (Tes
37、t MethodsD1691).9. Interferences9.1 Magnesium in concentrations greater than 100 mg/L may interfere.9.2 No interference from SiO2 in concentrations up to 100 mg/L has been observed.9.3 Background correction or chelation-extraction (see Test Method B) to remove interferences may be necessary to deter
38、minelow levels of manganese in some waters.NOTE 2Instrument manufacturers instructions for use of the specific correction technique should be followed.10. Apparatus10.1 Atomic Absorption Spectrophotometer, for use at 279.5 nm.NOTE 3The manufacturers instructions should be followed for all instrument
39、al parameters. A wavelength other than 279.5 nm may be used if it hasbeen determined to be equally suitable.10.1.1 Manganese Light SourceMultielement lamps, electrodeless discharge lamps, or hollow-cathode lamps have been foundsatisfactory.10.2 Pressure-Reducing ValvesThe supplies of fuel and oxidan
40、t shall be maintained at pressures somewhat higher than thecontrolled operating pressure of the instrument by suitable valves.11. Reagents and Materials11.1 Hydrochloric Acid (sp gr 1.19)Concentrated hydrochloric acid (HCl).NOTE 4If a high reagent blank is obtained, distill the HCl or use spectrogra
41、de acid. (WarningWhen HCl is distilled, an azeotropic mixture isobtained (approximately 6 NHCl.HCl.) Therefore, whenever concentrated HCl is specified in the preparation of a reagent or in the procedure, use doublethe amount specified if distilled acid is used.) Therefore, whenever concentrated HCl
42、is specified in the preparation of a reagent or in the procedure, usedouble the amount specified if distilled acid is used.)11.2 Manganese Solution, Stock (1.0 mL = 1.0 mg Mn)Dissolve 3.076 g of manganous sulfate monohydrate (MnSO4H2O)in a mixture of 10 mL of HNO3 (sp gr 1.42) and 100 mL of water. D
43、ilute to 1 L with water.Apurchased manganese stock solutionof appropriate known purity is also acceptable.11.3 Manganese Solution, Standard (1.0 mL = 0.1 mg Mn)Dilute 100.0 mL of manganese stock solution to 1 L with water.11.4 Nitric Acid (sp gr 1.42)Concentrated nitric acid (HNO3).NOTE 5If a high r
44、eagent blank is obtained, distill the HNO3 or use spectrograde acid.11.5 Nitric Acid (1 + 499)Add 1 volume of HNO3 (sp gr 1.42) to 499 volumes of water.11.6 Oxidant:11.6.1 Air, which has been passed through a suitable filter to remove oil, water, and other foreign substances, is the usualoxidant.11.
45、7 Fuel: Acetylenestandard, commercially available acetylene is the usual fuel. Acetone, always present in acetylenecylinders, can affect analytical results. The cylinder should be replaced at 345 kPa (50 psi). (Warning“Purified” grade acetylenecontaining a special proprietary solvent other than acet
46、one should not be used with poly(vinyl chloride) tubing as weakening ofthe tubing walls can cause a potentially hazardous situation.)11.8 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 p
47、aper, or glass fiber paper are acceptable. 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.D858 17412. Standardization12.1 Prepare 100 mLeach of a blank and at least four standard solutions to bra
48、cket the expected manganese concentration rangeof the samples to be analyzed by diluting the manganese standard solution with HNO3 (1 + 499). Prepare the standards each timethe test is to be performed, and select so as to give zero, middle, and maximum points for an analytical curve.NOTE 6It is reco
49、mmended that the blank (zero standard) be compared with reagent grade water to avoid the possibility of using a high blank.12.2 When determining total recoverable manganese add 0.5 mL of HNO3 (sp gr 1.42) and proceed as directed in 13.213.3.When determining dissolved manganese proceed with 13.513.6.12.3 Aspirate the blank and standards and record the instrument readings. Aspirate HNO3 (1 + 499) between each standard.12.4 Prepare Read directly in concentration if this capability is provided with the instrument or measure the absorban
