1、Designation: E 34 94 (Reapproved 2002)Standard Test Methods forChemical Analysis of Aluminum and Aluminum-Base Alloys1This standard is issued under the fixed designation E 34; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the yea
2、r of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon (e) 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 ch
3、emical 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 0.05Iron, % 0.01 to 3.0Lead, % 0.01 to 1.0
4、Lithium, % 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 procedures appear in the following order:Sections
5、Beryllium by Argon Plasma Optical EmissionSpectroscopy 283 to 292Beryllium by the Morin (Fluorometric) Test Method 8-19Bismuth by the Thiourea (Photometric) Method1aBismuth and Lead by the Atomic Absorption TestMethod 188 to 198Boron by the Carmine (Photometric) Test Method 30 to 38Cadmium by the At
6、omic Absorption Test Method 167 to 177Chromium:Diphenylcarbazide (Photometric) Test Method 39 to 47Persulfate Oxidation (Titrimetric) Test Method1bChromium by the Atomic Absorption Test Method 199 to 209SectionsCopper and Lead by the Electrolytic (Gravimetric) TestMethod1cCopper and Zinc by the Atom
7、ic Absorption TestMethod 210 to 220Copper by the Electrolytic (Gravimetric) Test Method 303 to 311Copper by the Neocuproine (Photometric) Test Method1aGallium by the Ion Exchange-Atomic Absorption TestMethod 312 to 323Iron by the 1,10-Phenanthroline (Photometric) Method 73 to 81Iron and Manganese by
8、 the Atomic Absorption Method 221 to 231Lithium by the Atomic Absorption Test Method 324 to 334Magnesium:Pyrophosphate (Gravimetric) Method1bEthylenediamine Tetraacetate (Titrimetric) TestMethod 88 to 93Magnesium by the Atomic Absorption Test Method 232 to 242Manganese by the Periodate (Photometric)
9、 TestMethod 293 to 302Nickel:Dimethylglyoxime (Photometric) Test Method1aDimethylglyoxime (Gravimetric) Test Method1bNickel by the Atomic Absorption Test Method 243 to 253Silicon:Molybdisilicic Acid (Photometric) Test Method 118 to 127Sodium Hydroxide-Perchloric Acid (Gravimetric)Method 128 to 133Ti
10、n by the Iodate (Titrimetric) Test Method 134 to 140Titanium by the Chromotropic Acid (Photometric) TestMethod 141 to 150Titanium by the Diantipyrylmethane Photometric TestMethod 254 to 263Vanadium by an Extraction-Photometric Test Methodusing N-Benzoyl-N-Phenylhydroxylamine 264 to 273Zinc:Ammonium
11、Mercuric Thiocyanate or the ZincOxide (Gravimetric) Test Method1bEthylenediamine Tetraacetate (Titrimetric) TestMethod1dIon Exchange-EDTA Titrimetric Test Method 274 to 282Zirconium by the Arsenazo III (Photometric) Method 178 to 1871.3 The values stated in SI units are to be regarded as thestandard
12、.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 prior to use. Specific haza
13、rdstatements are given throughout these test methods.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 Jan. 15,
14、1994. Published March 1994. Originallypublished as E 34 60 T. Last previous edition E 34 88.1aDiscontinued as of Feb. 25, 1983.1bDiscontinued as of May 29, 1981.1cDiscontinued as of Oct. 25, 1985.1dDiscontinued as of March 25, 1983.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, W
15、est Conshohocken, PA 19428-2959, United States.2. Referenced Documents2.1 ASTM Standards:E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications2E50 Practices for Apparatus, Reagents, and Safety Precau-tions for Chemical Analysis of Metals3E55 Practice for
16、Sampling Wrought Nonferrous Metals andAlloys for Determination of Chemical Composition3E60 Practice for Photometric and SpectrophotometricMethods for Chemical Analysis of Metals3E88 Practice for Sampling Nonferrous Metals and Alloysin Cast Form for Determination of Chemical Composition3E 173 Practic
17、e for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals3E 716 Practices for Sampling Aluminum and AluminumAlloys for Spectrochemical Analysis4E 1024 Guide for Chemical Analysis of Metals and MetalBearing Ores by Flame Atomic Absorption Spectropho-tometry43. Significance an
18、d Use3.1 These test methods for the chemical analysis of metalsand alloys are primarily 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-f
19、ully and safely. It is expected that work will be performed ina properly equipped laboratory.4. Apparatus, Reagents, and Photometric Practice4.1 Apparatus and reagents required for each determinationare listed in separate sections preceding the procedure. Theapparatus, standard solutions, and certai
20、n other reagents usedin more than one procedure are referred to by number and shallconform to the requirements prescribed in Practices E50,except that photometers shall conform to the requirementsprescribed in Practice E60.4.2 Photometric practice prescribed in these test methodsshall conform to Pra
21、ctice E60.5. Precautions5.1 For precautions to be observed in the use of certainreagents in these test methods, reference shall be made toPractices E50.6. Sampling6.1 Wrought products shall be sampled in accordance withPractice E55. Cast products shall be sampled in accordancewith Practice E88.6.2 C
22、hill cast disks produced for analysis by spectrochemi-cal methods (see Practices E 716) shall be considered castproducts. The principles of Practice E88shall apply.6.2.1 Prepare such disks for chemical analysis by drilling ormilling through the entire thickness of an unmachined disk(Note 1). Use a m
23、inimum of two positions approximatelyopposite each other and combine the drillings or millings.5NOTE 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
24、.6.2.2 The outer edges of the holes shall be approximately0.48 cm (316 in.) from the edge of the disk. Drills shall be notless than 0.95 cm (38 in.) in diameter and not larger than 1.27cm (12 in.) in diameter.46.2.3 Mill disks at similar points to a distance of 40 % of thesample diameter. Use a 0.95
25、-cm (38 in.) milling cutter.46.2.4 Sample book mold disks (Type A, Practices E 716)atapproximately the 9 oclock and the 3 oclock positions whenthe sprue is at the 12 oclock position. Center pour (Type B,Practices E 716) and vacuum cast disks may be sampledaround the entire circumference. Fig. 1 illu
26、strates the areassuitable for sampling Type A and Type B disks. Vacuum castdisks are sampled in the same manner as Type B disks.46.2.5 Drilling or milling techniques ideally should produceuniformly small chips. Break large continuous pieces into2Annual Book of ASTM Standards, Vol 14.02.3Annual Book
27、of ASTM Standards, Vol 03.05.4Annual Book of ASTM Standards, Vol 03.06.5Olson, H. A., and Macy, D. W., “Metallurgical Approach to EvaluatingChemical Sample Disks,” Light Metals, Vol 2, 1978, pp. 301311.NOTE 1Shaded areas are suitable for sampling.FIG. 1 Type A and Type B DisksE 34 94 (2002)2smaller
28、pieces 0.64 cm (14 in.) to 0.95 cm (38 in.) long. Drillingor milling techniques should minimize production of fine,dust-like material.47. Rounding Calculated Values7.1 Calculated values shall be rounded to the desired num-ber of places in accordance with the rounding method given in3.4 and 3.5 of Pr
29、actice E29.BERYLLIUM BY THE MORIN (FLUOROMETRIC)TEST METHOD8. Scope8.1 This test method covers the determination of berylliumin concentrations from 1 to 100 ppm.9. Summary of Test Method9.1 In an alkaline solution, beryllium and morin form acompound which produces a yellow-green fluorescence atappro
30、ximately 520 nm when excited by light at approximately430 nm.10. Concentration Range10.1 The recommended concentration range is from 0.05 to0.5 g of beryllium in 25 mL of solution.11. Stability of Fluorescence11.1 The fluorescence is stable for at least 1 h if the testsolutions are kept at constant
31、temperature.12. Interferences12.1 Silicon must be removed by dehydration or volatiliza-tion. Beryllium is separated from interfering ions by anacetylacetone extraction. Fluoride and pyrophosphate interferein the extraction.13. Apparatus13.1 Bottles, plastic, 500-mL capacity.13.2 Constant-Temperature
32、 Bath, 20 or 25C.13.3 Fluorescence-Measuring Instrument A suitable filterfluorometer or spectrofluorometer with primary excitation atapproximately 430 nm and a means of isolating and measuringthe secondary fluorescent emission at approximately 520 nm.14. Reagents14.1 Acetylacetone (2,4-pentanedione)
33、, practical.14.2 Aluminum Sulfate Solution (49 g/L)Dissolve 4.9 g ofaluminum sulfate (Al2(SO4)318H2O) in 70 mL of water, add1 mL of HClO4, transfer to a 100-mL volumetric flask, diluteto volume, and mix.14.3 Ammonium Nitrate Wash Solution (10 g/L)Dissolve5 g of ammonium nitrate (NH4NO3) in water and
34、 dilute to 500mL.14.4 Beryllium, Standard Solution A (1 mL = 100 g Be)Dissolve 1.964 g of beryllium sulfate (BeSO44H2O) in water,add 10 mL of HClO4, transfer to a 1-L volumetric flask, diluteto volume, and mix. Standardize as follows: transfer a 100-mLaliquot of this solution to a 250-mL beaker, add
35、 NH4OH (1+1)until a permanent turbidity forms, and then add 10 mL inexcess. Allow to stand for 2 to3horovernight. Filter using alow-ash, medium paper and wash well with NH4NO3washsolution. Transfer the precipitate and paper to a weighed,covered platinum crucible and char. Finally ignite to constantw
36、eight at 1000C and weigh as beryllium oxide (BeO).14.5 Beryllium, Standard Solution B (1 mL = 0.10 g Be)Transfer a 10-mL aliquot of Beryllium Solution A to a 100-mLvolumetric flask. Add 1 mL of HClO4, dilute to volume, andmix. Transfer a 10-mL aliquot of this solution to a 1-Lvolumetric flask. Add 1
37、0 mL of HClO4, dilute to volume, andmix.14.6 Chloroform (CHCl3).14.7 Diethylenetriaminepentaacetic Acid (DTPA), Recrys-tallized (Note 2)Add 100 g of DTPA to 800 mL of boilingwater and heat to boiling. Add 8 to 10 g of high-qualitydecolorizing carbon and mix thoroughly. Filter with suctionthrough a h
38、ardened retentive paper. Transfer the clear filtrate toa 1-L beaker and stir vigorously to induce crystallizationthroughout the solution. Cool thoroughly in a water bath. Filterwith suction using a hardened paper and remove as much wateras possible. Dry the salts at 110C.NOTE 2It is essential that t
39、he DTPA salts be recrystallized sincecommercial DTPA contains impurities that absorb ultraviolet and visiblelight. These impurities produce bright blue fluorescence under ultravioletlight, and react under certain conditions to produce a bright yellowfluorescence.14.8 Disodium Ethylenediaminetetraace
40、tate (EDTA) Solu-tion (100 g/L)Dissolve 100 g of EDTA in water and dilute to1L.14.9 EDTA Wash SolutionAdd5mLofH2SO4and 10 mLof the EDTA solution to 300 mL of water. Add 2 drops ofphenol red indicator solution and NH4OH until the solutionturns red. Cool and dilute to 500 mL.14.10 Morin Solution (0.07
41、5 g/L)Dissolve 0.0075 g ofanhydrous morin (3,5,7,28,48-penta-hydroxyflavone), reagentgrade, in 40 mL of ethanol. Transfer to a 100-mL volumetricflask with water, dilute to volume, and mix.14.11 Phenol Red Indicator Solution (1 g/L)Dissolve 0.1g of phenol red in 50 mL of methanol and dilute to 100 mL
42、with water.14.12 Piperidine Buffer SolutionDissolve 15 g of therecrystallized DTPA in 200 mL of water. Add 75 mL ofredistilled piperidine and cool. Add 20 g of anhydrous sodiumsulfite (Na2SO3) and dilute to 500 mL. Store in a plastic bottle.This solution slowly decomposes and should be discarded aft
43、er6 months.14.13 Potassium Iodide-Starch Paper.14.14 Quinine Sulfate Solution (0.1 g/L)Dissolve 0.1 g ofquinine sulfate in 300 mL of water. Add 10 mL of HClO4anddilute to 1 L.14.15 Sodium Hydroxide-Sodium Perchlorate-DTPA-Triethanolamine (TEA) SolutionDissolve 60 g of sodiumhydroxide (NaOH) and 320
44、g of anhydrous sodium perchlorate(NaClO4) in 250 mL of water. Filter through a double 7-cmglass-fiber filter. Add 10 mL of TEA solution (20 volume %) to13.0 g of the recrystallized DTPA and dissolve in 50 mL ofwater and about 20 mL of the NaOH-NaClO4solution. WhenE 34 94 (2002)3dissolution is comple
45、te, add the remainder of the NaOH-NaClO4solution and dilute to 500 mL. Store in a plastic bottle.Acidify a small portion of the solution and test for oxidizingagents with the potassium iodide-starch paper. If the presenceof an oxidizing agent is indicated, add sodium sulfite (Na2SO3)in small portion
46、s until the oxidizing agent is destroyed.14.16 Sodium Hydroxide Solution (40 g/L)Dissolve 20 gof NaOH in water and dilute to 500 mL. Store in a plasticbottle.15. Hazards15.1 Beryllium and its compounds are extremely toxic andcare must be exercised in the handling of these compounds.Hot perchloric ac
47、id and organic compounds present the possi-bility of an explosion if not handled carefully.16. Preparation of Calibration Curve16.1 Calibration SolutionsTransfer 0.5, 1.0, 3.0, 5.0, 7.0,and 9.0 mL of Beryllium Solution B (1 mL = 0.10 g Be) to six25-mL volumetric flasks. Proceed as directed in 16.3.1
48、6.2 Reference SolutionTransfer 5 mL of water to a25-mL volumetric flask and proceed as directed in 16.3.16.3 Fluorescence Development:16.3.1 Add 1 mL of Al2(SO4)3solution, 3 mL of NaOH-NaClO4-DTPA-TEA solution, and 3 drops of quinine sulfatesolution.16.3.2 Add HClO4dropwise until the solution fluore
49、scesunder an ultraviolet light, then add 1 drop in excess. Swirl thecontents of the flask so that any beryllium that may have beendeposited as the hydroxide on the wall of the flask is redis-solved.16.3.3 Add NaOH solution dropwise until the fluorescenceis destroyed and then add 2 drops in excess. Rinse down theneck of the flask with water.16.3.4 Add 5 mL of piperidine buffer solution and mix.16.3.5 Add 1.00 mLof morin solution, dilute to volume, andmix. Place the flask in the constant-temperature bath for 20min.16.4 Fluorometry:16.4.1 Followin
