1、Designation: E 1277 08Standard Test Method forChemical Analysis of Zinc-5 % Aluminum-Mischmetal Alloysby ICP Emission Spectrometry1This standard is issued under the fixed designation E 1277; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 t
3、he followinglimits:Element Concentration 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 Included are procedures for elements in
4、 the followingconcentration ranges:Element Concentration Range, %Aluminum 3.08.0Cadmium 0.00160.025Cerium 0.0050.10Iron 0.00150.10Lanthanum 0.0090.10Lead 0.0020.0261.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the
5、 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 in Section 8, 12.2, and 14.1.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent W
6、aterE29 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 andAlloys for Determi
7、nation of Chemical CompositionE88 Practice for Sampling Nonferrous Metals and Alloysin Cast Form for Determination of Chemical CompositionE 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemi
8、cal Analysis of Metals3E 876 Practice for Use of Statistics in the Evaluation ofSpectrometric Data3E 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method2.2 NIST Standard Reference Materials:4SRM 728 Zinc, Intermediate Purity3. Terminology3.1 For d
9、efinitions of terms used in this test method, refer toTerminology E 135.4. Summary of Test Method4.1 The sample is dissolved in mixed acids. The samplesolution is introduced into the plasma source of an ICPspectrometer and the intensities at selected wavelengths fromthe plasma emission spectrum are
10、compared to the intensities atthe same wavelengths measured with 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
11、 who use this test method will be trained analysts capableof performing common laboratory procedures skillfully andsafely. It is expected that work will be performed in a properlyequipped laboratory.1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals,
12、Ores and Related Materials and is the directresponsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, their Alloys andRelated Metals.Current edition approved March 1, 2008. Published May 2008. Originallyapproved in 1991. Last previous edition in 2002 as E 1277 02.2For referenced ASTM standard
13、s, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.4Available from National Institute of Standards and Technology (NIST), 100Burea
14、u Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Apparatus6.1 Inductively-Coupled Argon Plasma (ICP) Atomic Emis-sion SpectrometerThe instrument is equipped with an
15、argon-plasma source and a sample transport system for introducingthe test sample and calibration solutions into the plasma. Themonochromator or polychromator must be capable of isolatingthe required wavelengths shown in Table 1 for measurement oftheir intensities by a linear photometer. Multielement
16、 pro-grammed analysis including automatic data acquisition andcomputer-controlled calibration and determinations may beused if available, provided that, in addition to calculatedresults, the instrument records intensity readings each time atest sample or calibration solution is presented to the inst
17、ru-ment.NOTE 1All elements (including aluminum) are calibrated as linearfunctions of intensity. 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 must be made usingcalibration solutions No.
18、1, No. 2, and No. 4. The other elements can thenbe determined together in another run using only calibration solutions No.2 and No. 3. Use the calibration solutions prepared in 11.1 in determiningthe instrument settings for the elements in this matrix. Follow themanufacturers instructions to set the
19、 wavelengths and parameters toprovide as large a difference between the intensity readings for the highand low calibration concentrations as is consistent with stable instrumentreadings. If there is a question of linearity of the instruments responseover the range of solution concentrations given, a
20、 third standard, equidis-tant between the two listed standards, must be measured to verify linearity.7. Reagents7.1 Purity of ReagentsUnless otherwise indicated, allreagents used in this test method shall conform to the “ReagentGrade” Specifications of the American Chemical Society.5Other chemicals
21、may be used provided that it is first ascer-tained that the reagent used is of sufficiently high purity topermit its use without lessening the accuracy of the determi-nation.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type
22、II of Specification D 1193.7.3 Aluminum, Standard Solution (1 mL = 20.0 mg Al)Transfer 2.0000 g of aluminum (purity: 99.999 % min) to a250-mL beaker. Cover, add 50 mL of HCl (1 + 1) and a smallcrystal of mercuric nitrate. Heat gently to accelerate thereaction, but avoid temperatures high enough to c
23、ause 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 willremain undissolved). Transfer the solution to a 100-mL volu-metric flask, dilute to volume, and mix. Store in a poly
24、ethylenebottle.7.4 Cadmium, Standard Solution (1 mL = 1.00 mg Cd)Transfer 1.000 g of cadmium (purity: 99.95 % min) to a250-mL beaker. Cover and add 40 mL of HNO3(1 + 1) and 10mL of HCl. After dissolution is complete, heat to boiling toremove oxides of nitrogen. Cool, transfer to a 1-L volumetricflas
25、k, 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 asammonium hexanitrato cerate) (purity: 99.95 % min) for4hat85 C and cool to room temperature in a desiccator. Disso
26、lve3.913 g of dry ceric ammonium nitrate in 100 mL of HCl(1 + 9). Transfer to a 1-L volumetric flask, add 240 mL of HCland 20 mL of HNO3, dilute to volume, and mix. Store in apolyethylene bottle.7.6 Cerium, Standard Solution B (1 mL = 0.010 mg Ce)Using a pipet, transfer 1.00 mL of Cerium Standard So
27、lution 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 mL 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 iro
28、n (purity: 99.95 % min) to a 250-mLbeaker, cover, and add 100 mL of HCl (1 + 1). Boil gently tocomplete dissolution. Cool and transfer to a 1-L volumetricflask, add 200 mL of HCl and 20 mL of HNO3, dilute tovolume, and mix. Store in the polyethylene bottle.7.9 Iron, Standard Solution B (1 mL = 0.010
29、 mg Fe)Using a pipet, transfer 1.00 mL of Iron Standard Solution A toa 100-mL volumetric flask. Dilute to volume with dilutionsolution and mix.7.10 Lanthanum, Standard Solution A (1 mL = 0.010 mgLa)Ignite lanthanum oxide (La2O3) (purity: 99.9 % min) for1 h at 1000 C and cool to room temperature in a
30、 desiccator.Dissolve 1.173 g of dry lanthanum oxide in 100 mL of HCl(1 + 9) and transfer to a 1-L volumetric flask. Add 240 mL ofHCl and 20 mL of HNO3, dilute to volume, and mix. Store ina polyethylene bottle.7.11 Lanthanum, Standard Solution B (1 mL = 0.010 mgLa)Using a pipet, transfer 1.00 mL of L
31、anthanum 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 lead (purity: 99.9 % min) to a 250-mLbeaker, cover, and add 40 mL of HNO3(1 + 1). Boil gently tocomplete dissolution and to remove
32、 oxides of nitrogen. Cool,5Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and th
33、e United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical 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 3 226.446 226.558Cerium 418.66 .5 2 . .Iron 259.94
34、 .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 each inte-gration, No. Integ. = number of integrations averaged for each reading, and B
35、Cor1and BCor2 are off-peak background correction wavelengths.E1277082transfer to a 1-L volumetric flask, add 250 mL of HCl, dilute tovolume, and mix. Store in a polyethylene bottle.7.13 Zinc Matrix Solution (50 mL = 3.75 g Zinc MatrixStandard)Transfer 18.75 g 6 0.10 g of Zinc Matrix Standardto a 250
36、-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, remove from the heat and allow to cool.Transfer to a
37、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. Hazards8.1 For precautions to be observed in the use of certa
38、inreagents in this test method, refer to Practices E50.9. Sampling9.1 For procedures for sampling the material, refer toPractices E55and E88.10. Interlaboratory Studies and Rounding of CalculatedValues10.1 Only four laboratories were available to test thismethod, therefore, the interlaboratory test
39、does not complywith the protocol for Practice E 173. However, the statisticswere calculated according to Practice E 173.10.2 Calculated values shall be rounded to the desirednumber of places as directed in 6.4 to 6.6 of Practice E29.10.3 Practice E 173 has been replaced by Practice E 1601.The Reprod
40、ucibility Index R2corresponds to the Reproduc-ibility Index R of Practice E 1601. Likewise, the RepeatabilityIndex R1of Practice E 173 corresponds to the RepeatabilityIndex r of Practice E 1601.11. Calibration11.1 Prepare calibration and test sample solutions beforecalibration measurements are start
41、ed.11.2 Calibration SolutionsAll calibration solutions con-tain the same concentration of zinc as the test sample solutions.The aluminum content of calibration solutions No. 2 and No. 3must be equal to the midpoint of the calibrated aluminumrange. Using a pipet, transfer 50.0 mL of the Zinc MatrixSo
42、lution 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.11.3 Test Sample SolutionTransfer a 3.8 to 4.2-g portionof the test sample weighe
43、d 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 boil.When most of the material has dissolved, add 2.0 mLof HNO3,let the solution cool for ab
44、out 20 min, transfer to a 100-mLplastic volumetric flask, dilute to volume, and mix.11.4 Automatic Calibration Mode(If the instrument doesnot have the capability to take data from calibration solutionsand calculate and store the equations needed to convertinstrument readings from test samples direct
45、ly into concentra-tion values automatically, or if that capability is not to be used,proceed in accordance with 11.5.) Set up the instrumentparameters as directed in Section 6. If one of the parameters isa “lower limit” (used to establish a printed “less than” value),set it to 0 for each element. En
46、ter the concentrations of theelements to be found in each calibration solution. Table 4 givesthe concentration table for solutions based upon SRM 728 asZinc Matrix Standard. If a different Zinc Matrix Standard isused, Table 4 must be revised to reflect the different composi-tion of that material. Us
47、ing the calibration solutions, follow themanufacturers procedure to perform the instrument calibrationat the wavelengths specified in Table 1. Without undue delay,proceed in accordance with 12.2.11.5 Nonautomatic ModeNo separate calibration run isrequired if intensity readings only are recorded. Set
48、 up theinstrument to measure intensities at the wavelengths specifiedin Table 1 according to the manufacturers instructions andproceed to 12.3.12. Procedure12.1 Measurement SequencesTo reduce the distortion ofdata if instrument drift occurs while measurements are taken,TABLE 2 Standard Solution Volu
49、mes Added, mLA,BElement No. 1 No. 2 No. 3 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 Concentrations Added, 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
