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2、n American National StandardStandard Test Method forAntimony in Water1This standard is issued under the fixed designation D 3697; 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 in
3、dicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method2 covers the determination of dissolved and total recoverable antimony in water by atomic absorption spectroscopy.1.2 This test method is appl
4、icable in the range from 1 to 15g/L of antimony. The range may be extended by less scale expansion or by dilution of the sample.1.3 The precision and bias data were obtained on reagent water, tap water, salt water, and two untreated wastewaters. The information on precision and bias may not apply to
5、 other waters.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appro- priate safety and health practices and determine the applica- bility of regulatory limitations prior to u
6、se.2. Referenced Documents2.1 ASTM Standards:D 1129 Terminology Relating to Water3D 1193 Specification for Reagent Water3D 2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D-19 on Water3D 3370 Practices for Sampling Water from Closed Con- duits3D 4691 Prac
7、tice for Measuring Elements in Water by FlameAtomic Absorption Spectrophotometry3D 4841 Practice for Estimation of Holding Time for WaterSamples Containing Organic and Inorganic Constituents3D 5847 Practice for the Writing Quality Control Specifica- tions for Standard Test Methods for Water Analysis
8、43. Terminology3.1 Definitions: For definitions of terms used in this test method, refer to Terminology D 1129.1 This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in Water.Current edition approv
9、ed May 10, 2002. Published June 2002. Originally published as D 3697 78. Last previous edition D 3697 92 (1996).2 Platte, J. A., and Marcy, V. M., “A New Tool for the Water Chemist,” IndustrialWater Engineering, IWEGA, May 1965.3 Annual Book of ASTM Standards, Vol 11.01.4 Annual Book of ASTM Standar
10、ds, Vol 11.02.3.2 Definition of Term Specific to This Standard:3.2.1 total recoverable antimonyan arbitrary analytical term relating to forms of antimony that are determinable by the digestion method which is included in the procedure. Some organic compounds may not be completely recovered.3.2.2 lab
11、oratory control sample, na solution with a cer- tified concentration of the antimony.4. Summary of Test Method4.1 Organic antimony-containing compounds are decom- posed by adding sulfuric and nitric acids and repeatedly evaporating the sample to fumes of sulfur trioxide. The antimony so produced, to
12、gether with inorganic antimony originally present, is subsequently reacted with potassium iodide and stannous chloride, and finally with sodium borohy- dride to form stibine. The stibine is removed from solution by aeration and swept by a flow of nitrogen into a hydrogen flame where it is determined
13、 by atomic absorption at 217.6 nm.5. Significance and Use5.1 Because of the association with lead and arsenic in industry, it is often difficult to assess the toxicity of antimony and its compounds. In humans, complaints referable to the nervous system have been reported. In assessing human cases, h
14、owever, the possibility of lead or arsenic poisoning must always be borne in mind. Locally, antimony compounds are irritating to the skin and mucous membranes.6. Interference6.1Since the stibine is freed from the original sample matrix, interferences in the flame are minimized.6.2 Selenium and arsen
15、ic, which also form hydrides, do not interfere at concentrations of 100 g/L. Higher concentrations were not tested.7. Apparatus7.1 Atomic Absorption Spectrophotometer, for use at 217.6 nm with a scale expansion of approximately 3. A general guide for the use of flame atomic absorption applications i
16、s given in Practice D 4691.NOTE 1The manufacturers instructions should be followed for all instrumental parameters.7.1.1 Antimony Electrodeless Discharge Lamp.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.1D 3697 02FIG. 1 Stibine Va
17、por Analyzer7.2 Recorder or Digital Readout Any multirange variable speed recorder or digital readout accessory, or both, that is compatible with the atomic absorption spectrophotometer is suitable.7.3 Stibine Vapor Analyzer, assembled as shown in Fig. 1.NOTE 2A static system, such as one using a ba
18、lloon, has been found to be satisfactory. See McFarren, E. F., “New, Simplified Method for Metal Analysis,” Journal of American Water Works Assoc., JAWWA, Vol64, 1972, p. 28.8. Reagents and Materials8.1 Purity of Reagents Reagent grade chemicals shall be used in all tests. Unless otherwise indicated
19、, it is intended that all reagents shall conform to the specifications for the Com- mittee on Analytical Reagents of the American Chemical Society, where such specifications are available.5 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to
20、permit its use without lessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming to Specification D 1193, Type I, II, or III water. Type I is preferred and more commonly used. Other reagent wate
21、r types may be used provided it is first ascertained that the water is of sufficiently high purity to permit its use without adversely affecting the precision and bias of the test method. Type II water was specified at the time of round robin testing of these test methods.NOTE 3The user must ensure
22、the type of reagent water chosen is sufficiently free of interferences. The water should be analyzed using the test method.8.3 Antimony Solution, Stock (1.00 mL = 100 g Sb) Dissolve 274.3 mg of antimony potassium tartrate, KSbOC4H4O61/2H2O, in water and dilute to 1000 mL with water.8.4 Antimony Solu
23、tion, Intermediate (1.00 mL = 10 g Sb) Dilute 50.0 mL of antimony stock solution to 500.0 mL with water.8.5 Antimony Solution, Standard (1.0 mL = 0.10 g Sb) Dilute 5.0 mL of antimony intermediate solution to 500.0 mL with water. Prepare fresh before each use. This standard is used to prepare working
24、 standards at the time of analysis.5 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
25、 U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.8.6 Hydrochloric Acid (sp gr 1.19) Concentrated hydro-chloric acid (HCl).8.7 Nitric Acid (sp gr 1.42) Concentrated nitric acid(HNO3).8.8 Nitric Acid (1 + 1) Add 250 mL of conce
26、ntrated nitricacid (sp gr 1.42) to 250 mL of water.8.9 Potassium Iodide Solution (15 g/100 mL) Dissolve 15g of potassium iodide (KI) in 100 mL of water. This solution is stable when stored in an amber bottle or in the dark.8.10 Sodium Borohydride Solution (4 g/100 mL) Dissolve4 g of sodium borohydri
27、de (NaBH4) and 2 g of sodium hydroxide (NaOH) in 100 mL water. Prepare weekly.8.11 Stannous Chloride Solution (4.6 g/100 mL of concen- trated HCl)Dissolve5g of stannous chloride (SnCl2H2O) in100 mL of concentrated HCl (sp gr 1.19). This solution is stable if a few small pieces of mossy tin are added
28、 to prevent oxidation.8.12 Sulfuric Acid (1+ 1) Cautiously, and with constant stirring and cooling, add 250 mL of concentrated sulfuric acid(H2SO4, sp gr 1.84) to 250 mL of water.8.13 Hydrogen, commercially available. Set pressure onburner control box to 8 psig (55 KPa) and adjust flowmeter to appro
29、ximately 6 L/min.8.14 Nitrogen, commercially available. Set pressure on burner control box to 30 psig (206.8 KPa) and adjust flowmeter for maximum sensitivity by volatilizing standards. A flow of approximately 9 L/min has been found satisfactory. This will vary depending on the burner used.9. Sampli
30、ng9.1Collect the sample in accordance with Practices D 3370. The holding time for the samples may be calculated in accordance with Practice D 4841.9.2 Immediately preserve samples with HNO3 (sp gr 1.42) to a pH of 2 or less at the time of collection; normally about 2 mL/L is required. If only dissol
31、ved antimony is to be deter- mined, filter the sample through a (No. 325) 0.45-m mem- brane filter before acidification.10. Standardization10.1 Clean all glassware before use by rinsing first withHNO3 (1 + 1) and then with water.10.2 Prepare, in 200 to 300-mL wide-mouth glass contain-ers, a blank an
32、d sufficient standards that contain from 0.0 to 1.5g of antimony by diluting 0.0 to 15.0-mL portions of the antimony standard solution to 100 mL with water.10.3 Proceed as directed in 11.3 to 11.8.10.4 Prepare an analytical curve by plotting recorder scale readings versus micrograms of antimony on l
33、inear graph paper or calculate a standard curve. Alternatively, read directly in concentration if a concentration readout is provided with the instrument.11. Procedure11.1 Clean all glassware before use by rinsing first withHNO3 (1 + 1) and then with water.11.2 Pipet a volume of well-mixed acidified
34、 sample con-taining less than 1.5 g of antimony (100-mL max) into a 2002D 3697 02NumberTrueTABLE 1 Recovery and Precision DataMeanStatedMethodTestSolutionofLabsValue,g/LValue,g/LST,g/LSo,g/LBias,%Range,g/LR 2Precision RegressionEquationsHydride/ FlameRGW43.03.150.920.70+ 5.01150.80ST = 0.451 + 0.104
35、 xAAS7.012.06.4211.160.881.710.781.548.3 y7.00.89So = 0.255 + 0.109 xWOC43.07.012.02.746.0010.730.661.221.730.660.951.438.714.3 y10.6 y0.981.00ST = 0.346 + 0.132 xSo = 0.386 + 0.0967 xto 300-mL wide-mouth glass container, and dilute to 100 mLwith water (see Fig. 1).NOTE 4If only dissolved antimony i
36、s to be determined, use a filtered and acidified sample (9.2).11.3 To each container, add 7 mL of H2SO4 (1 + 1) and 5 mL of concentrated HNO3. Add a small boiling chip and carefully evaporate to fumes of SO3. Maintain an excess of HNO3 until all organic matter is destroyed. This prevents darkening o
37、f the solution and possible reduction and loss of antimony. Cool, add 25 mL of water, and again evaporate to fumes of SO3 to expel oxides to nitrogen.11.4Cool, and adjust the volume of each container to approximately 100 mL with water.11.5 To each container, add successively, with thorough mixing af
38、ter each addition, 8 mL of concentrated HCl, 1 mL of KI solution, and 0.5 mL of SnCl2 solution. Allow about 15 min for reaction.11.6 Attach one container at a time to the rubber stopper containing the gas dispersion tube.11.7 Fill the medicine dropper or syringe with 1 mL ofNaBH4 solution and insert
39、 into the hole in the rubber stopper.11.8 Add the NaBH4 solution to the sample solution. Afterthe recorder reading (scale reading) has reached a maximumand has returned to the baseline, remove the container. Rinse the gas dispersion tube in water before proceeding to the next sample. Treat each succ
40、eeding sample, blank, and standard ina like manner.12. Calculation12.1 Determine the weight or concentration of antimony in each sample by referring to 10.4. If the weight is determined from the analytical curve, calculate the concentration of antimony in the sample in micrograms per litre, as follo
41、ws:Antimony, g/L 5 1000 3 W/Vwhere:V= volume of sample, mL, andW= weight of antimony in sample, g.13. Precision and Bias13.1 The single operator and overall precision of this test method for four laboratories, which included a total of six operators analyzing each sample on three different days, wit
42、hin its designated range varies with the quantity being tested.13.2Recoveries of known amounts of antimony (fromantimony potassium tartrate) in a series of prepared standard for the same laboratories and operators are given in Table 1.13.3 The precision and bias data were obtained on reagent water,
43、tap water, salt water, and two untreated wastewaters. The information on precision and bias may not apply to other waters.13.4 Precision and bias for this test method conforms to Practice D 2777-77, which was in place at the time of collaborative testing. Under the allowances made in 1.4 of D2777-98
44、, these precision and bias data do meet existing requirements for interlaboratory studies of Committee D19 test methods.14. Quality Control (QC)14.1 The following quality control information is recom- mended for the determination of antimony in water.14.2 The instrument shall be calibrated using a m
45、inimum of four calibration standards and a calibration blank. The calibra- tion correlation coefficient shall be equal to or greater than0.990. In addition to the initial calibration blank, a calibration blank should be analyzed at the end of the batch run to ensure contamination was not a problem during the batch analysis.14.3 An instrument check standard shall be analyzed at a minimum frequency of 10 % throughout the batch analysis. The value of the instrument check standard shall fall between80 % and 120 % of