1、Designation: E34 11Standard Test Methods forChemical Analysis of Aluminum and Aluminum-Base Alloys1This standard is issued under the fixed designation E34; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision.
2、A number in parentheses indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 These test methods cover the chemical analysis ofalu
3、minum and aluminum-base alloys having compositionswithin the following limits:Beryllium, ppm 0.3 to 100Bismuth, % 0.02 to 1.0Boron, % 0.005 to 0.060Cadmium, % 0.001 to 0.50Chromium, % 0.01 to 1.0Copper, % 0.01 to 20.0Gallium, % 0.001 to 0.05Iron, % 0.01 to 3.0Lead, % 0.01 to 1.0Lithium, % 0.001 to 4
4、.0Magnesium, % 0.002 to 12.0Manganese, % 0.005 to 2.0Nickel, % 0.01 to 4.0Silicon, % 0.05 to 20.0Tin, % 0.03 to 1.0Titanium, % 0.002 to 0.30Vanadium, % 0.002 to 0.16Zinc, % 0.003 to 12.0Zirconium, % 0.01 to 0.301.2 The analytical procedures appear in the following sec-tions:Procedure SectionsBerylli
5、um:Beryllium by Argon Plasma Optical EmissionSpectroscopy283 to 292Beryllium by the Morin (Fluorometric) TestMethod1eBismuth:Bismuth by the Thiourea (Photometric) Method1aBismuth and Lead by the Atomic AbsorptionTest Method188 to 198Boron:Procedure SectionsBoron by the Carmine (Photometric) Test Met
6、hod1eCadmium:Cadmium by the Atomic Absorption Test Method 167 to 177Chromium:Chromium by the Diphenylcarbazide (Photometric)Test Method1eChromium by the Persulfate Oxidation (Titrimetric)Test Method1bChromium by the Atomic Absorption Test Method 199 to 209Copper:Copper and Lead by the Electrolytic (
7、Gravimetric)Test Method1cCopper and Zinc by the Atomic AbsorptionSpectometry Test Method210 to 220Copper by the Electrolytic (Gravimetric) Test Method 303 to 311Copper by the Neocuproine (Photometric)Test Method1aGallium:Gallium by the Ion Exchange-Atomic AbsorptionTest Method312 to 323Iron:Iron by
8、the 1,10-Phenanthroline (Photometric) Method 73 to 81Iron and Manganese by the Atomic AbsorptionSpectometry Method221 to 231Lead:Copper and Lead by the Electrolytic (Gravimetric)Test Method1cBismuth and Lead by the Atomic AbsorptionSpectrometry Test Method188 to 198Lithium:Lithium by the Atomic Abso
9、rption Test Method 324 to 334Magnesium:Magnesium by the Pyrophosphate (Gravimetric)Method1bMagnesium by the Ethylenediamine Tetraacetate(Titrimetric) Test Method1eMagnesium by the Atomic Absorption SpectrometryTest Method232 to 242Manganese:Iron and Manganese by the Atomic AbsorptionSpectrometry Tes
10、t Method221 to 231Manganese by the Periodate (Photometric)Test Method293 to 302Nickel:Nickel by the Dimethylglyoxime (Photometric)Test Method1aNickel by the Dimethylglyoxime (Gravimetric)Test Method1bNickel by the Atomic Absorption SpectrometryTest Method243 to 253Silicon:1These test methods are und
11、er the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.04 on Aluminum and Magnesium.Current edition approved July 1, 2011. Published August 2011. Originallypublished as E34 60 T. Last previous edit
12、ion E34 94 (Reapproved 2002).1aDiscontinued as of Feb. 25, 1983.1bDiscontinued as of May 29, 1981.1cDiscontinued as of Oct. 25, 1985.1dDiscontinued as of March 25, 1983. DOI: 10.1520/E0034-11.1eDiscontinued as of July 1, 2011. DOI: 10.1520/E0034-11.1Copyright ASTM International, 100 Barr Harbor Driv
13、e, PO Box C700, West Conshohocken, PA 19428-2959, United States.Silicon by the Molybdisilicic Acid (Photometric)Test Method1eSilicon by the Sodium Hydroxide-Perchloric Acid(Gravimetric) Method1eTin:Tin by the Iodate (Titrimetric) Test Method1eTitanium:Titanium by the Chromotropic Acid (Photometric)T
14、est Method141 to 150Titanium by the Diantipyrylmethane PhotometricTest Method254 to 263Vanadium:Vanadium by an Extraction-Photometric Test Methodusing N-Benzoyl-N-Phenylhydroxylamine264 to 273Zinc:Zinc by the Ammonium Mercuric Thiocyanate or theZinc Oxide (Gravimetric) Test Method1bZinc by the Ethyl
15、enediamine Tetraacetate(Titrimetric) Test Method1dCopper and Zinc by the Atomic AbsorptionSpectrometry Test Method210 to 220Zinc by the Ion Exchange-EDTA TitrimetricTest Method274 to 282Zirconium:Zirconium by the Arsenazo III (Photometric) Method 178 to 1871.3 The values stated in SI units are to be
16、 regarded as thestandard.1.4 This standard does not purport to address all of thesafety problems, 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 pri
17、or to use. Specific hazardstatements are given throughout these test methods.2. Referenced Documents2.1 ASTM Standards:2E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications3E50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical An
18、alysis of Metals, Ores, andRelated Materials3E55 Practice for Sampling Wrought Nonferrous Metals andAlloys for Determination of Chemical Composition3E60 Practice for Analysis of Metals, Ores, and RelatedMaterials by Spectrophotometry3E88 Practice for Sampling Nonferrous Metals and Alloys inCast Form
19、 for Determination of Chemical CompositionE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals3 4E716 Practices for Sampling and Sample Preparation ofAluminum and Aluminu
20、m Alloys for Determination ofChemical Composition by Spectrochemical Analysis4E1024 Guide for Chemical Analysis of Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry5E1479 Practice for Describing and Specifying Inductively-Coupled Plasma Atomic Emission SpectrometersE1601 Pra
21、ctice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method3. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology E135.4. Significance and Use4.1 These test methods for the chemical analysis of metalsand alloys are pri
22、marily intended to test such materials forcompliance with compositional specifications. It is assumedthat all who use these test methods will be trained analystscapable of performing common laboratory procedures skill-fully and safely. It is expected that work will be performed ina properly equipped
23、 laboratory.5. Apparatus, Reagents, and Photometric Practice5.1 Apparatus and reagents required for each determinationare listed in separate sections preceding the procedure.5.2 Photometric practice prescribed in these test methodsshall conform to Practice E60.5.3 Calculated values shall be rounded
24、to the desired num-ber of places in accordance with the rounding method ofPractice E29.2Annual Book of ASTM Standards, Vol 14.02.3Annual Book of ASTM Standards, Vol 03.05.4Annual Book of ASTM Standards, Vol 03.06.5Withdrawn. The last approved version of this historical standard is referencedon www.a
25、stm.org.NOTE 1Shaded areas are suitable for sampling.FIG. 1 Type A and Type B DisksE341126. Precautions6.1 For precautions to be observed in the use of certainreagents in these test methods, reference shall be made toPractices E50.7. Sampling7.1 Wrought products shall be sampled in accordance withPr
26、actice E55. Cast products shall be sampled in accordancewith Practice E88.7.2 Chill cast disks produced for analysis by spectrochemi-cal methods (see Practices E716) shall be sampled by drillingor milling through the entire thickness. Drill bits or millingcutters should be carbide to avoid iron cont
27、amination.NOTE 1The use of a machined disk may result in the exclusion of anelement-rich portion of the sample. This practice should be avoidedwherever possible, especially for analyses affecting product acceptance.7.2.1 If samples are produced by drilling, use a minimum oftwo positions approximatel
28、y opposite each other and combinethe drillings.7.2.2 The outer edges of the holes shall be approximately0.48 cm (316 in.) from the edge of the disk. Drill bits shall benot less than 0.95 cm (38 in.) in diameter and not larger than1.27 cm (12 in.) in diameter.67.2.3 If samples are produced by milling
29、, mill disks atsimilar points to a distance of 40 % of the sample diameter orother methods that provide a representative sample such asquarter of half milling. A 0.95-cm (38 in.) milling cutter hasbeen shown to provide acceptable chips.67.2.4 Center pour (Type B, Practices E716) and vacuum castdisks
30、 may be sampled around the entire circumference. Fig. 1illustrates the areas suitable for sampling Type B disks.Vacuum cast disks are sampled in the same manner as Type Bdisks.67.2.5 Drilling or milling techniques ideally should produceuniformly small chips. Break large continuous pieces intosmaller
31、 pieces 0.64 cm (14 in.) to 0.95 cm (38 in.) long. Drillingor milling techniques should minimize production of fine,dust-like material.6BERYLLIUM BY THE MORIN (FLUOROMETRIC)TEST METHOD(This test method, which consisted of Sections 8 through 19of this standard, was discontinued in 2008.)BISMUTH BY TH
32、E THIOUREA(PHOTOMETRIC) TEST METHOD(This test method, which consisted of Sections 20 through 29of this standard, was discontinued in 1983.)BORON BY THE CARMINE (PHOTOMETRIC)TEST METHOD(This test method, which consisted of Sections 30 through 38of this standard, was discontinued in 2008.)CHROMIUM BY
33、THE DIPHENYLCARBAZIDE(PHOTOMETRIC) TEST METHOD(This test method, which consisted of Sections 39 through 47of this standard, was discontinued in 2008.)CHROMIUM BY THE PERSULFATE OXIDATION(TITRIMETRIC) TEST METHOD(This test method, which consisted of Sections 48 through 53of this standard, was discont
34、inued in 1981.)COPPER BY THE NEOCUPROINE(PHOTOMETRIC) TEST METHOD(This test method, which consisted of Sections 54 through 63of this standard, was discontinued in 1983.)COPPER AND LEAD BY THE ELECTROLYTIC(GRAVIMETRIC) TEST METHOD(This test method, which consisted of Sections 64 through 72of this sta
35、ndard, was discontinued in 1985.)IRON BY THE 1,10-PHENANTHROLINE(PHOTOMETRIC) TEST METHOD(This test method, which consisted of Sections 73 through 81of this standard, was discontinued in 2008.)MAGNESIUM BY THE PYROPHOSPHATE(GRAVIMETRIC) TEST METHOD(This test method, which consisted of Sections 82 th
36、rough 87of this standard, was discontinued in 1981.)MAGNESIUM BY THE ETHYLENEDIAMINETETRAACETATE (TITRIMETRIC) TEST METHOD(This test method, which consisted of Sections 88 through 93of this standard, was discontinued in 2008.)MANGANESE BY THE PERIODATE(PHOTOMETRIC) TEST METHOD(This test method, whic
37、h consisted of Sections 94 through102 of this standard, was replaced in 1984 by Sections 293through 302.)NICKEL BY THE DIMETHYLGLYOXIME(PHOTOMETRIC) TEST METHOD(This test method, which consisted of Sections 103 through111 of this standard, was discontinued in 1983.)NICKEL BY THE DIMETHYLGLYOXIME(GRA
38、VIMETRIC) TEST METHOD(This test method, which consisted of Sections 112 through117 of this standard, was discontinued in 1981.)SILICON BY THE MOLYBDISILICIC ACID(PHOTOMETRIC) TEST METHOD(This test method, which consisted of Sections 118 through127 of this standard, was discontinued in 2008.)6Olson,
39、H. A., and Macy, D. W., “Metallurgical Approach to EvaluatingChemical Sample Disks,” Light Metals, Vol 2, 1978, pp. 301311.E34113SILICON BY THE SODIUM HYDROXIDE-PERCHLORIC ACID (GRAVIMETRIC)TEST METHOD(This test method, which consisted of Sections 128 through133 of this standard, was discontinued in
40、 2008.)TIN BY THE IODATE (TITRIMETRIC)TEST METHOD(This test method, which consisted of Sections 134 through140 of this standard, was discontinued in 2008.)TITANIUM BY THE CHROMOTROPIC ACID(PHOTOMETRIC) TEST METHOD141. Scope141.1 This test method covers the determination of titaniumin concentrations
41、from 0.002 to 0.3 %.142. Summary of Test Method142.1 The sample is dissolved in a sodium hydroxidesolution and acidified with nitric and sulfuric acids. Iron isreduced with ascorbic acid. The yellow complex of titaniumwith chromotropic acid is formed at a pH between 3.1 and 3.2.Photometric measureme
42、nt is made at approximately 470 nm.143. Concentration Range143.1 The recommended concentration range is from 0.002to 0.10 mg of titanium per 50 mLof solution, using a 2-cm cell.NOTE 2This test method has been written for cells having a 2-cmlight path. Cells having other dimensions may be used, provi
43、ded suitableadjustments can be made in the amounts of sample and reagents used.144. Stability of Color144.1 The color develops within 5 min and is stable for 40min.145. Interferences145.1 Chromium, if present, interferes because of the back-ground color of the solution. Provision is made to correct
44、forthis interference.146. Reagents146.1 Ascorbic Acid Solution (40 g/L)Dissolve1gofascorbic acid in 25 mL of water. Do not use a solution that hasstood more than 1 h.146.2 Chromotrophic Acid Solution (Disodium Salt) (20g/L)Dissolve2gofchromotropic acid (4,5-dihydroxy-2,7-naphthalenedisulfonic acid,
45、disodium salt) in 70 mL of watercontaining 0.75 mL of acetic acid. Add 0.2 g of sodiummetadisulfite (Na2S2O5) and stir until completely dissolved.Filter through a fine paper into a 100-mL volumetric flask.Wash with water, dilute to volume, and mix. Select a lot ofreagent that meets the following cri
46、teria: The solution must belight, clear yellow and have an absorbance reading of 0.3 orless when measured at 470 nm in a 2-cm cell, using distilledwater as the reference. Do not use a solution that has stoodmore than 3 weeks.146.3 Potassium Permanganate Solution (1 g/L)Dissolve0.1 g of potassium per
47、manganate (KMnO4) in water and diluteto 100 mL.146.4 Reagent MixtureTransfer 300 mL of water to a 1-Lvolumetric flask, add in order 250 mL of NaOH Solution A,250 mL of H2SO4(1+4), and 18 mL of HNO3and mix. Cool,dilute to volume, and mix. (The pH should be about 0.50.)146.5 Sodium Hydroxide Solution
48、A (200 g/L)Dissolve200 g of sodium hydroxide (NaOH) in about 500 mL of water,dilute to about 900 mL, and cool. Transfer to a 1-L volumetricflask, dilute to volume, and mix. Immediately transfer to aplastic bottle.146.6 Sodium Hydroxide Solution B (80 g/L)Dissolve 80g of sodium hydroxide (NaOH) in ab
49、out 200 mL of water,dilute to about 900 mL, and cool. Transfer to a 1-L volumetricflask, dilute to volume, and mix. Immediately transfer to aplastic bottle.146.7 Sodium Metadisulfite (Na2S2O5).146.8 Sodium Monochloroacetic Acid Buffer SolutionDissolve 189 g of monochloroacetic acid in 150 mL of water.Dissolve 40 g of sodium hydroxide (NaOH) in about 100 mLof water, and cool. Add the NaOH solution to the monochlo-roacetic acid solution, mix thoroughly, and cool. If turbid, filterthrough a fine paper and wash the filter with water. Transfer toa 500-mL volumetric flas
