1、Designation: E1277 14Standard Test Method forAnalysis of Zinc-5 % Aluminum-Mischmetal Alloys by ICPEmission Spectrometry1This standard is issued under the fixed designation E1277; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the chemical analysis of zincalloys having chemical compositions within the following
3、limits:Element Composition Range, %Aluminum 3.08.0Antimony 0.002 maxCadmium 0.025 maxCerium 0.030.10Copper 0.10 maxIron 0.10 maxLanthanum 0.030.10Lead 0.026 maxMagnesium 0.05 maxSilicon 0.015 maxTin 0.002 maxTitanium 0.02 maxZirconium 0.02 max1.2 The values stated in SI units are to be regarded asst
4、andard. No other units of measurement are included in thisstandard.1.3 Included are procedures for elements in the followingcomposition ranges:Element Composition Range, %Aluminum 3.08.0Cadmium 0.00160.025Cerium 0.0050.10Iron 0.00150.10Lanthanum 0.0090.10Lead 0.0020.0261.4 This standard does not pur
5、port to address all of thesafety concerns, 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 safetyhazards statements are given
6、in Section 8, 11.2, and 13.1.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Me
7、tals, Ores, andRelated MaterialsE55 Practice for Sampling Wrought Nonferrous Metals andAlloys for Determination of Chemical CompositionE88 Practice for Sampling Nonferrous Metals and Alloys inCast Form for Determination of Chemical CompositionE135 Terminology Relating to Analytical Chemistry forMeta
8、ls, Ores, and Related MaterialsE173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals (Withdrawn1998)3E876 Practice for Use of Statistics in the Evaluation ofSpectrometric Data (Withdrawn 2003)3E1601 Practice for Conducting an Interlaboratory Study toEvaluate
9、the Performance of an Analytical Method2.2 NIST Standard Reference Materials:4SRM 728 Zinc, Intermediate Purity3. Terminology3.1 For definitions of terms used in this test method, refer toTerminology E135.4. Summary of Test Method4.1 The sample is dissolved in mixed acids. The samplesolution is intr
10、oduced into the plasma source of an ICPspectrometer and the intensities at selected wavelengths from1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and is the directresponsibility of Subcommittee E01.05 on Cu, Pb, Zn, C
11、d, Sn, Be, Precious Metals,their Alloys, and Related Metals.Current edition approved Nov. 1, 2014. Published January 2015. Originallyapproved in 1991. Last previous edition approved in 2008 as E1277 08. DOI:10.1520/E1277-14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcont
12、act ASTM Customer Service at serviceastm.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.4Available from National Institute of Standards and T
13、echnology (NIST), 100Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1the plasma emission spectrum are compared to the intensities atthe same wavelengths measured w
14、ith calibration solutions.5. Significance and Use5.1 This test method for the chemical analysis of metals andalloys is primarily intended to test such materials for compli-ance with compositional specifications. It is assumed that allthose who use this test method will be trained analysts capableof
15、performing common laboratory procedures skillfully andsafely. It is expected that work will be performed in a properlyequipped laboratory.6. Apparatus6.1 Inductively-Coupled Argon Plasma (ICP) Atomic Emis-sion SpectrometerThe instrument may be either sequential orsimultaneous, axial or radial, and s
16、hall be capable of isolatingthe required wavelengths shown in Table 1 for measurement oftheir intensities. Multielement programmed analysis includingautomatic data acquisition and computer-controlled calibrationand determinations may be used if available, provided that, inaddition to calculated resu
17、lts, the instrument records intensityreadings each time a test sample or calibration solution ispresented to the instrument.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of
18、 the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.5Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Purity of Wa
19、terUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type II of Specification D1193.7.3 Aluminum, Standard Solution (1 mL = 20.0 mg Al)Transfer 2.0000 g of aluminum (purity: 99.999 % minimum) toa 250-mL beaker. Cover, add 50 mL of HCl (1 + 1) and a
20、 smallcrystal of mercuric nitrate. Heat gently to accelerate thereaction, but avoid temperatures high enough to cause anoticeable volume loss. If the reaction slows, add moremercuric salt as needed. A number of hours may be required tocomplete the dissolution (only a small droplet of mercury willrem
21、ain undissolved). Transfer the solution to a 100-mL volu-metric flask, dilute to volume, and mix. Store in a polyethylenebottle.7.4 Cadmium, Standard Solution (1 mL = 1.00 mg Cd)Transfer 1.000 g of cadmium (purity: 99.95 % minimum) to a250-mL beaker. Cover and add 40 mL of HNO3(1 + 1) and 10mL of HC
22、l. After dissolution is complete, heat to boiling toremove oxides of nitrogen. Cool, transfer to a 1-L volumetricflask, add 240 mL of HCl, dilute to volume, and mix. Store ina polyethylene bottle.7.5 Cerium, Standard Solution A (1 mL = 1.00 mg Ce)Dry ceric ammonium nitrate (NH4)2Ce(NO3)6, also known
23、 asammonium hexanitrato cerate) (purity: 99.95 % minimum) for4 h at 85 C and cool to room temperature in a desiccator.Dissolve 3.913 g of dry ceric ammonium nitrate in 100 mL ofHCl (1 + 9). Transfer to a 1-L volumetric flask, add 240 mL ofHCl and 20 mL of HNO3, dilute to volume, and mix. Store ina p
24、olyethylene bottle.7.6 Cerium, Standard Solution B (1 mL = 0.010 mg Ce)Using a pipet, transfer 1.00 mL of Cerium Standard Solution Ato a 100-mL volumetric flask. Dilute to volume with dilutionsolution and mix.7.7 Dilution SolutionHalf fill a 2-L volumetric flask withwater. Add 500 mL of HCl and 40 m
25、L of HNO3, swirl to mix,dilute to the mark, and mix.7.8 Iron, Standard Solution A (1 mL = 1.00 mg Fe)Transfer 1.000 g of iron (purity: 99.95 % minimum) to a250-mL beaker, cover, and add 100 mL of HCl (1 + 1). Boilgently to complete dissolution. Cool and transfer to a 1-Lvolumetric flask, add 200 mL
26、of HCl and 20 mL of HNO3,dilute to volume, and mix. Store in the polyethylene bottle.7.9 Iron, Standard Solution B (1 mL = 0.010 mg Fe)Usinga pipet, transfer 1.00 mL of Iron Standard Solution A to a100-mL volumetric flask. Dilute to volume with dilutionsolution and mix.7.10 Lanthanum, Standard Solut
27、ion A (1 mL = 0.010 mgLa)Ignite lanthanum oxide (La2O3) (purity: 99.9 % mini-mum) for1hat1000 C and cool to room temperature in adesiccator. Dissolve 1.173 g of dry lanthanum oxide in 100 mLof HCl (1 + 9) and transfer to a 1-L volumetric flask. Add 240mL of HCl and 20 mL of HNO3, dilute to volume, a
28、nd mix.Store in a polyethylene bottle.7.11 Lanthanum, Standard Solution B (1 mL = 0.010 mgLa)Using a pipet, transfer 1.00 mL of Lanthanum StandardSolutionAto a 100-mLvolumetric flask. Dilute to volume withdilution solution and mix.7.12 Lead, Standard Solution (1 mL = 1.00 mg Pb)Transfer 1.000 g of l
29、ead (purity: 99.9 % minimum) to a250-mL beaker, cover, and add 40 mL of HNO3(1 + 1). Boilgently to complete dissolution and to remove oxides of5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted
30、by the American Chemical Society, see the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.TABLE 1 Wavelengths and Instrument ConditionsAElementWavelength,nmTime, s No. Integ. BCor1 BCor2Aluminum 309.27 1.0 3 . .Cadmium 226.502 .5 3 226.446
31、226.558Cerium 418.66 .5 2 . .Iron 259.94 .5 2 . .Lanthanum 398.85 .5 2 398.754 398.906Lead 283.297 1.0 3 . 283.336AThe tabulated conditions were those found satisfactory on one instrument.Wavelengths are expressed in nanometres (nm). Time = seconds for eachintegration, No. Integ. = number of integra
32、tions averaged for each reading, andBCor1 and BCor2 are off-peak background correction wavelengths.E1277 142nitrogen. Cool, transfer to a 1-L volumetric flask, add 250 mLof HCl, dilute to volume, and mix. Store in a polyethylenebottle.7.13 Zinc Matrix Solution (50 mL = 3.75 g Zinc MatrixStandard)Tra
33、nsfer 18.75 g 6 0.10 g of Zinc Matrix Standardto a 250-mL plastic beaker. Cover and add about 50 mL ofwater. Add 62.5 mL of HCl and heat enough to maintain thereaction but not enough to evaporate the solution. When mostof the material has dissolved, add 5.0 mL of HNO3. When allsolids have dissolved,
34、 remove from the heat and allow to cool.Transfer to a 250-mL plastic volumetric flask, dilute to themark, and mix.7.14 Zinc Matrix StandardUse a zinc reference materialof known composition (SRM 728 has been found suitable)with respect to the elements listed in the scope of this testmethod.8. Hazards
35、8.1 For precautions to be observed in the use of certainreagents in this test method, refer to Practices E50.9. Sampling9.1 For procedures for sampling the material, refer toPractices E55 and E88.10. Calibration10.1 Prepare calibration and test sample solutions beforecalibration measurements are sta
36、rted.10.2 Calibration SolutionsAll calibration solutions con-tain the same composition of zinc as the test sample solutions.The aluminum content of calibration solutions No. 2 and No. 3shall be equal to the midpoint of the calibrated aluminumrange. Using a pipet, transfer 50.0 mL of the Zinc MatrixS
37、olution into each of four 100-mL plastic volumetric flasksmarked Cal No. 1 through Cal No. 4. Add the volumes ofstandard solutions specified in Table 2 (also see Table 3), diluteto volume with dilution solution, and mix.NOTE 1All elements (including aluminum) are calibrated as linearfunctions of int
38、ensity. If the instrument cannot be set to measurealuminum and ignore other elements in calibration solutions No. 1 and No.4, then a separate determination of aluminum shallbe made usingcalibration solutions No. 1, No. 2, and No. 4. The other elements can thenbe determined together in another run us
39、ing only calibration solutions No.2 and No. 3. Use the calibration solutions prepared in 10.1 in determiningthe instrument settings for the elements in this matrix. Follow themanufacturers instructions to set the wavelengths and parameters toprovide as large a difference between the intensity readin
40、gs for the highand low calibration compositions as is consistent with stable instrumentreadings. If there is a question of linearity of the instruments responseover the range of solution compositions given, a third standard, equidistantbetween the two listed standards, shallbe measured to verify lin
41、earity.10.3 Test Sample SolutionTransfer a 3.8-g to 4.2-g portionof the test sample weighed to the nearest 0.02 g to a 250-mLpolytetrafluoroethylene beaker. Add about 30 mL of water,cover, and cautiously add 25 mL of HCl in increments. Heatgently to maintain the reaction, if necessary, but do not bo
42、il.When most of the material has dissolved, add 2.0 mL of HNO3,let the solution cool for about 20 min, transfer to a 100-mLplastic volumetric flask, dilute to volume, and mix.10.4 Automatic Calibration Mode(If the instrument doesnot have the capability to take data from calibration solutionsand calc
43、ulate and store the equations needed to convertinstrument readings from test samples directly into composi-tion values automatically, or if that capability is not to be used,proceed in accordance with 10.5.) Set up the instrumentparameters as directed in Section 6. If one of the parameters isa “lowe
44、r limit” (used to establish a printed “less than” value),set it to 0 for each element. Enter the compositions of theelements to be found in each calibration solution. Table 4 givesthe composition table for solutions based upon SRM 728 asZinc Matrix Standard. If a different Zinc Matrix Standard isuse
45、d, Table 4 shall be revised to reflect the different composi-tion of that material. Using the calibration solutions, follow themanufacturers procedure to perform the instrument calibrationat the wavelengths specified in Table 1. Without undue delay,proceed in accordance with 11.2.10.5 Nonautomatic M
46、odeNo separate calibration run isrequired if intensity readings only are recorded. Set up theinstrument to measure intensities at the wavelengths specifiedin Table 1 according to the manufacturers instructions andproceed to 11.3.TABLE 2 Standard Solution Volumes Added, mLA,BElement No. 1 No. 2 No. 3
47、 No. 4Aluminum 6.00 11.0 11.0B16.0Cadmium . . 1.00 .Cerium . 2.00(B) 4.00(A) .Iron . 1.00(B) 4.00(A) .Lanthanum . 2.00(B) 4.00(A) .Lead . . 1.00 .AUse standard solution A or B as indicated in parentheses.BAdded to match solution No. 2, not for calibration purposes.TABLE 3 Solution Compositions Added
48、 mg/LAElement No. 1 No. 2 No. 3 No. 4Aluminum 1200 2200 . 3200Cadmium . . 10.0 .Cerium . 0.2 40.0 .Iron . 0.1 40.0 .Lanthanum . 0.2 40.0 .Lead . . 10.0 .ATable 4 is derived from this table by adding the trace element contributions fromthe zinc matrix solution to the compositions shown in this table
49、 and converting theresulting sum to weight percent.TABLE 4 Composition Table for Calibration SolutionsA,BElement No. 1 No. 2 No. 3 No. 4Aluminum 3.00 5.50 . 8.00Cadmium . .00011 .0251 .Cerium . .00050 .1000 .Iron . .00052 .1003 .Lanthanum . .00050 .1000 .Lead . .00104 .0260 .AThe values in this table assume SRM 728 as zinc matrix, a sample weight of 4.00g, and results reported in %.BTo calculate the composition table for a different zinc matrix material, add theparts per million contributed from 3.75 g of that material in a volume of 100 mL tothe
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