ASTM E34 - 11e1 Standard Test Methods for Chemical Analysis of Aluminum and Aluminum-Base Alloys (Withdrawn 2017).pdf

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1、Designation: E34 111Standard 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、Anumber in parentheses indicates the year of last reapproval.Asuperscriptepsilon () 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.1NOTEEditorial changes were made throughout in August 2012.1.

3、Scope1.1 These test methods cover the chemical analysis ofaluminum 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.

4、05Iron, % 0.01 to 3.0Lead, % 0.01 to 1.0Lithium, % 0.001 to 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 procedure

5、s appear in the following sec-tions:Procedure SectionsBeryllium: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:

6、Procedure SectionsBoron by the Carmine (Photometric) Test Method1eCadmium: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

7、Method 199 to 209Copper:Copper and Lead by the Electrolytic (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

8、 Exchange-Atomic AbsorptionTest Method312 to 323Iron:Iron by 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 Method1 cBismuth and Lead by the Atomic AbsorptionSpectr

9、ometry Test Method188 to 198Lithium:Lithium by the Atomic Absorption Test Method 324 to 334Magnesium:Magnesium by the Pyrophosphate (Gravimetric)Method1 bMagnesium by the Ethylenediamine Tetraacetate(Titrimetric) Test Method1 eMagnesium by the Atomic Absorption SpectrometryTest Method232 to 242Manga

10、nese:Iron and Manganese by the Atomic AbsorptionSpectrometry Test 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 Spec

11、trometryTest Method243 to 253Silicon:1These test methods are under 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

12、August 2011. Originallypublished as E34 60 T. Last previous edition E34 94 (Reapproved 2002). DOI:10.1520/E0034-11E01.1aDiscontinued as of Feb. 25, 1983.1bDiscontinued as of May 29, 1981.1cDiscontinued as of Oct. 25, 1985.1dDiscontinued as of March 25, 1983.1eDiscontinued as of July 1, 2011.Copyrigh

13、t ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesNOTICE: This standard has either been superseded and replaced by a new version or withdrawn.Contact ASTM International (www.astm.org) for the latest information1Silicon by the Molybdisilicic Acid

14、 (Photometric)Test Method1 eSilicon by the Sodium Hydroxide-Perchloric Acid(Gravimetric) Method1 eTin:Tin by the Iodate (Titrimetric) Test Method1 eTitanium:Titanium by the Chromotropic Acid (Photometric)Test Method141 to 150Titanium by the Diantipyrylmethane PhotometricTest Method254 to 263Vanadium

15、: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 Ethylenediamine Tetraacetate(Titrimetric) Test Method1dCopper and Zinc by the Atomic AbsorptionSpect

16、rometry 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 regarded as thestandard.1.4 This standard does not purport to address all of thesafety problem

17、s, 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 prior to use. Specific hazardstatements are given throughout these test methods.2. Referenced Docu

18、ments2.1 ASTM Standards:2E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE55 Practice for Sampling Wrought Nonferrous Metals

19、andAlloys for Determination of Chemical CompositionE60 Practice for Analysis of Metals, Ores, and RelatedMaterials by SpectrophotometryE88 Practice for Sampling Nonferrous Metals and Alloys inCast Form for Determination of Chemical CompositionE135 Terminology Relating to Analytical Chemistry forMeta

20、ls, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals (Withdrawn1998)3E716 Practices for Sampling and Sample Preparation ofAluminum and Aluminum Alloys for Determination ofChemical Composition by Spectrochemical AnalysisE1024 Gu

21、ide for Chemical Analysis of Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry (Withdrawn 2004)3E1479 Practice for Describing and Specifying Inductively-Coupled Plasma Atomic Emission SpectrometersE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performa

22、nce 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 primarily intended to test such materials forcompliance with composition

23、al 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 laboratory.5. Apparatus, Reagents, and Photometric Practice5.1 Appar

24、atus 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 E60.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at ser

25、viceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.NOTE 1Shaded areas are suitable for sampling.FIG. 1 Type A and Type B DisksE3411125.3

26、 Calculated values shall be rounded to the desired num-ber of places in accordance with the rounding method ofPractice E29.6. 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 sha

27、ll be sampled in accordance withPractice 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 sh

28、ould be carbide to avoid iron contamination.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 mi

29、nimum oftwo positions approximately 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.47.2.3

30、If samples are produced by milling, 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.47.2.4 Center pour (Type B, Pr

31、actices E716) and vacuum castdisks 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.47.2.5 Drilling or milling techniques ideally should produceuniformly small chips. Break l

32、arge continuous pieces intosmaller pieces 0.64 cm (14 in.) to 0.95 cm (38 in.) long. Drillingor milling techniques should minimize production of fine,dust-like material.4BERYLLIUM BY THE MORIN (FLUOROMETRIC)TEST METHOD(This test method, which consisted of Sections 8 through 19of this standard, was d

33、iscontinued in 2008.)BISMUTH BY THE 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) TESTMETHOD(This test method, which consisted of Sections 30 through 38of this standard, was

34、discontinued in 2008.)CHROMIUM BY 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 throu

35、gh 53of this standard, was discontinued 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

36、 Sections 64 through 72of this standard, 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,

37、 which consisted of Sections 82 through 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)

38、TEST METHOD(This test method, which 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.)

39、NICKEL BY THE DIMETHYLGLYOXIME(GRAVIMETRIC) 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,

40、was discontinued in 2008.)4Olson, H. A., and Macy, D. W., “Metallurgical Approach to EvaluatingChemical Sample Disks,” Light Metals, Vol 2, 1978, pp. 301311.E341113SILICON BY THE SODIUM HYDROXIDE-PERCHLORIC ACID (GRAVIMETRIC) TESTMETHOD(This test method, which consisted of Sections 128 through133 of

41、 this standard, was discontinued in 2008.)TIN BY THE IODATE (TITRIMETRIC) TESTMETHOD(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 determin

42、ation of titaniumin concentrations 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 betw

43、een 3.1 and 3.2.Photometric measurement 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-cm lightpath. Cells havin

44、g other dimensions may be used, provided 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 so

45、lution. Provision is made to correct 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-dihyd

46、roxy-2,7-naphthalenedisulfonic acid, 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 o

47、freagent that meets the following criteria: 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

48、(1 g/L)Dissolve0.1 g of potassium permanganate (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

49、.50.)146.5 Sodium Hydroxide Solution 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 about 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 Monochl