1、Designation: E396 121E396 17Standard Test Methods forChemical Analysis of Cadmium1This standard is issued under the fixed designation E396; 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 pare
2、ntheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1 NOTEEditorial corrections were made throughout in August 2012.1. Scope1.1 These test methods cover the chemical analysis of cadmium having chemical composition
3、s with the following limits:Element Composition, max, %Antimony 0.001Arsenic 0.003Copper 0.015Lead 0.025Silver 0.010Thallium 0.003Tin 0.010Zinc 0.0351.2 The test methods appear in the following order:SectionsAntimony by the Rhodamine B Spectrophotometric Method0.0002 % to 0.0010 %62 72Arsenic by the
4、 Molybdenum Blue Spectrophotometric Method0.001 % to 0.005 %40 50Copper by the Neocuproine Spectrophotometric Method 0.002 % to0.030 %10 19Copper, Lead, Silver, and Zinc by the Atomic Absorption Spectrom-etry Method 0.004 % to 0.02 % Cu, 0.01 % to 0.05 % Pb, 0.004 %to 0.02 % Ag,and 0.01 % to 0.05 %
5、Zn51 61Lead by the Dithizone Spectrophotometric Method 0.001 % to0.05 %20 29Lead by the Dithizone Spectrophotometric Method 0.001 % to 0.05%20 29Thallium by the Rhodamine B Spectrophotometric Method0.0003 % to 0.005%30 39Thallium by the Rhodamine B Spectrophotometric Method0.0003 % to 0.005 %30 39Ti
6、n by the 8-Quinolinol Spectrophotometric Method 0.0025 % to0.0150 %73 821.3 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 safety, health, and healthenvironmen
7、tal practices and determine theapplicability of regulatory limitations prior to use. Specific precautionary information is given in Section 6, , , and .1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision
8、 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 Standards:2B440 Specification for Cadmium1 These test methods are under the jurisdiction ofASTM
9、Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and are the direct responsibilityof Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, Precious Metals, their Alloys, and Related Metals.Current edition approved Jan. 27, 2012Dec. 15, 2017. Published February 2012January 2017.
10、 Originally approved in 1970. Last previous edition approved in 20112012as E396 05E396 121(2011) DOI: 10.1520/E0396-12.10.1520/E0396-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume inf
11、ormation, 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 be technically possible to adequately
12、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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA
13、 19428-2959. United States1D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE55 Practice f
14、or Sampling Wrought Nonferrous Metals and Alloys for Determination of Chemical CompositionE60 Practice for Analysis of Metals, Ores, and Related Materials by SpectrophotometryE88 Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical CompositionE135 Terminology
15、 Relating to Analytical Chemistry for Metals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals (Withdrawn 1998)3E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method3. Termi
16、nology3.1 For definitions of terms used in this test method, refer to Terminology E135.4. Significance and Use4.1 These test methods for the chemical analysis of cadmium are primarily intended to test such material for compliance withcompositional specifications in Specification B440. It is assumed
17、that all who use these test methods will be trained analystscapable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properlyequipped laboratory.5. Apparatus, Reagents, and Spectrophotometric Practice5.1 Apparatus and reagents required
18、 for each determination are listed in separate sections preceding the procedure. Theapparatus, standard solutions, and reagents shall conform to the requirements prescribed in Practices E50. Spectrophotometers shallconform to the requirements prescribed in Practice E60.5.2 Spectrophotometric practic
19、e prescribed in these methods shall conform to Practice E60.5.3 Reagents5.3.1 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conformingto Type II of Specification D1193. Type III or Type IV may be used if they effect no measurable change in t
20、he blank or sample.5.3.2 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where suchspecifications are available.4 O
21、ther grades may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.6. Safety Hazards6.1 For precautions to be observed in the use of certain reagents in these test methods, refer to Practices
22、E50.7. Sampling7.1 Wrought products shall be sampled in accordance with Practice E55. Cast products shall be sampled in accordance withPractice E88. However, these test methods do not supersede any sampling requirements specified in a specific ASTM materialspecification.8. Rounding Calculated Values
23、8.1 Calculated values shall be rounded to the desired numberRounding of test results obtained using this test method shall beperformed in accordance with Practice E29of places as directed in Practice, Rounding Method, unless an alternative E29.roundingmethod is specified by the customer or applicabl
24、e material specification.9. Interlaboratory Studies9.1 These test methods have been evaluated in accordance with Practices E173, unless otherwise noted in the precision section.9.2 Practice E173 has been replaced by Practice E1601. The reproducibility index, R2, of Practice E173 corresponds to there
25、producibility index, R, of Practice E1601. The repeatability index, R1 , of Practice E173, corresponds to the repeatability index,r, of Practice E1601.COPPER BY THE NEOCUPROINE SPECTROPHOTOMETRIC METHOD10. Scope10.1 This test method covers the determination of copper content from 0.002 % to 0.030 %.
26、3 The last approved version of this historical standard is referenced on www.astm.org.4 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 the United States
27、 Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MDE396 17210. Scope10.1 This test method covers the determination of copper content from 0.002 % to 0.030 %.11. Summary of Test Method11.1 Copper is separated as cuprous copper from other metals by extractio
28、n of the copper-neocuproine complex withchloroform. Spectrophotometric absorbance measurement is made at approximately 455 nm.12. Concentration Range12.1 The recommended concentration range is from 0.01 mg to 0.15 mg of copper for each 25 mL of solution, using a 1-cmcell.NOTE 1This test method has b
29、een written for cells having a 1-cm light path. Cells having other dimensions may be used, provided suitableadjustments can be made in the amounts of sample and reagents used.13. Stability of Color13.1 The color develops within 5 min and the extracted complex is stable. However, because of the volat
30、ile nature of the solvent,it is advisable to take spectrophotometric readings promptly.14. Interferences14.1 The elements ordinarily present do not interfere if their contents are under the maximum limits shown in 1.1.15. Reagents15.1 Chloroform (CHCl3).15.2 Copper, Standard Solution (1 mL = 0.01 mg
31、 Cu)Dissolve 0.1000 g of copper (purity: 99.9 % min) in 10 mL of HNO3(1 + 1). Add 25 mL of water, heat to boiling, and boil gently for 2 min to eliminate oxides of nitrogen. Cool, transfer to a 100-mLvolumetric flask, dilute to volume, and mix. Transfer 5.00 mL to a 500-mL volumetric flask. Add 1 mL
32、 of HNO3 (1 + 1), diluteto volume, and mix.15.3 Hydroxylamine Hydrochloride Solution (100 g/L)Dissolve 5.0 g of hydroxylamine hydrochloride(NH2OH HCl)OHHCl) in 50 mL of water. Prepare fresh as needed.15.4 Metacresol Purple Indicator Solution (1 g/L)Dissolve 0.100 g of metacresol purple together with
33、 1 pellet of sodiumhydroxide (NaOH) NaOH in about 10 mL of water by warming. Dilute to 100 mL, and mix.15.5 Neocuproine Solution (1 g/L)Dissolve 0.10 g of neocuproine (2,9-dimethyl-1,10-phenanthroline hemihydrate) in 100 mLof either methanol or 95 % ethanol.15.6 Sodium Citrate Solution (300 g/L)Diss
34、olve 300 g of sodium citrate dihydrate in water, dilute to 1 L, and mix.15.7 Purity of WaterUnless otherwise indicated, reference to water shall be understood to mean reagent water as defined byType II of Specification D1193. Other Types may be used if they effect no measurable change in the referen
35、ce solution or sample.16. Preparation of Calibration Curve16.1 Calibration Solution:16.1.1 Using pipets, transfer (2, 5, 10, 15, and 20) mL of copper solution (1 mL = 0.01 mg Cu) to five 150-mL beakers, anddilute to about 40 mL.16.1.2 Add 2 drops of metacresol purple indicator solution, and then add
36、 HNO3 (1 + 1) dropwise to the red color change of theindicator. Proceed as directed in 16.3.16.2 Reference SolutionAdd 40 mL of water to a 150- mL beaker. Proceed as directed in 16.1.2.16.3 Color Development:16.3.1 Add 10 mL of NH2OH HCl OHHCl solution, and stir. Add 10 mL of sodium citrate solution
37、, and stir. Add NH4OHto the purple color of the indicator (pH about 8.5). Add 5.0 mL of neocuproine solution, stir, and allow to stand for 5 min.NOTE 2The precipitate that may form upon addition of sodium citrate solution will redissolve when the pH is raised to 8.5 with NH4OH.16.3.2 Transfer to a 1
38、25-mL separatory funnel marked at 80 mL, and dilute to the mark with water. Add 25.0 mL of CHCl3.Shake vigorously for 45 s, and allow the layers to separate. Draw off and discard about 1 mL of the CHCl3 layer to rinse the stemof the separatory funnel.16.4 Spectrophotometry:16.4.1 Multiple-Cell Spect
39、rophotometerMeasure the cell correction using absorption cells with a 1-cm light path and a lightband centered at approximately 455 nm (nm. Note 3). Using the test cell, take the spectrophotometric absorbance readings of thecalibration solutions.E396 173NOTE 3Avoid transfer of water to the absorptio
40、n cell in the following manner. Insert a loose plug of sterilized absorbent cotton into the stem of eachseparatory funnel. Just prior to filling the absorption cell with the solution in the separatory funnel, discard about 1 mL of the CHCl3 layer through thecotton plug and immediately transfer a sui
41、table portion of the CHCl3 layer into the dry absorption cell.16.4.1.1 Avoid transfer of water to the absorption cell in the following manner: Insert a loose plug of sterilized absorbent cottoninto the stem of each separatory funnel. Just prior to filling the absorption cell with the solution in the
42、 separatory funnel, discardabout 1 mL of the CHCl3 layer through the cotton plug and immediately transfer a suitable portion of the CHCl3 layer into thedry absorption cell.16.4.2 Single-Cell SpectrophotometerTransfer a suitable portion of the reference solution to an absorption cell with a 1-cmlight
43、 path and adjust the spectrophotometer to the initial setting, using a light band centered at approximately 455 nm (Note 1).While maintaining this adjustment, take the spectrophotometric absorbance readings of the calibration solutions.16.5 Calibration CurvePlot the net spectrophotometric absorbance
44、 readings of the calibration solutions against milligrams ofcopper per 25 mL of solution.17. Procedure17.1 Test SolutionTransfer a 0.5-g sample, weighed to the nearest 1 mg, to a 150-mL beaker. Add 5 mL of HNO3 (1 + 1).When dissolution is complete, add 20 mL of water and boil gently to eliminate oxi
45、des of nitrogen. Cool, dilute to about 40 mL,and add 2 drops of metacresol purple indicator solution. Proceed as directed in 17.3.17.2 Reference SolutionCarry a reagent blank through the entire procedure using the same amount of all reagents with thesample omitted, for use as the reference solution.
46、17.3 Color DevelopmentProceed as directed in 16.3.17.4 SpectrophotometryProceed as directed in 16.4.18. Calculation18.1 Convert the net spectrophotometric absorbance reading of the test solution to milligrams of copper by means of thecalibration curve. Calculate the percentage of copper as follows:C
47、opper,%5A/B 310! (1)where:A = copper found in the 25 mL of final test solution, mg, andB = sample represented in 25 mL of final test solution, g.19. Precision and Bias19.1 PrecisionEight laboratories cooperated in testing this test method and obtained the data summarized in Table 1.19.2 AccuracyBias
48、No certified reference materials suitable for testing this test method were available when theinterlaboratory testing program was conducted. The user of this test method is encouraged to employ accepted reference materials,if available, to determine the accuracy of this test method as applied in a s
49、pecific laboratory.19.3 E173 has been replaced by Practice E1601. The reproducibility Index R2 corresponds to the Reproducibility Index R ofPractice E1601. Likewise the Repeatability Index R1 corresponds to the Repeatability Index r of Practice E1601.LEAD BY THE DITHIZONE SPECTROPHOTOMETRIC METHOD20. Scope20.1 This test method covers the determination of lead in content from 0.001 % to 0.05 %.20. Scope20.1 This test method covers the determination of lead in content from 0.001 % to 0.05 %.21. Summary of Test
