1、Designation: E 1277 02Standard 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 7, 11.2, and 13.1.2. Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Wa
6、ter2E29 Practice for Using Significant Digits in Test Data toDetermine Conformance With Specifications3E50 Practices for Apparatus, Reagents, and Safety Precau-tions for Chemical Analysis of Metals4E55 Practice for Sampling Wrought Nonferrous Metals forDetermination of Chemical Composition4E88 Pract
7、ice for Sampling Nonferrous Metals and Alloysin Cast Form for Determination of Chemical Composition4E 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals4E 876 Practice for Use of Statistics in the Evaluation ofSpectrometric Data5E 1601 Practice for Conducti
8、ng an Interlaboratory Study toEvaluate the Performance of an Analytical Method53. Summary of Test Method3.1 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 spectr
9、um are compared to the intensities atthe same wavelengths measured with calibration solutions.4. Significance and Use4.1 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 a
10、llthose 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.5. Apparatus5.1 Inductively-Coupled Argon Plasma (ICP) Atomic Emis-sion SpectrometerThe instru
11、ment is equipped with an argon-plasma source, a sample transport system for introducing thetest sample and calibration solutions into the plasma. Themonochromator or polychromator must be capable of isolating1This test method is under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for
12、 Metals, Ores, and Related Materials and is the directresponsibility of Subcommittee E01.05 on Zn, Sn, Pb, Be, and Other Metals.Current edition approved October 10, 2002. Published December 2002. Origi-nally approved in 1991. Last previous edition in 1996 as E 1277 96.2Annual Book of ASTM Standards,
13、 Vol 11.01.3Annual Book of ASTM Standards, Vol 14.02.4Annual Book of ASTM Standards, Vol 3.05.5Annual Book of ASTM Standards, Vol 03.06.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the required wavelengths shown in Table 1 for mea
14、surement oftheir intensities by a linear photometer. Multielement pro-grammed analysis including automatic data acquisition andcomputer-controlled calibration and analysis calculations maybe used if available, provided that, in addition to calculatedresults, the instrument records intensity readings
15、 each time atest sample or calibration solution is presented to the instru-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 separat
16、e determination of aluminum must be made usingcalibration solutions No. 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 10.1 in determiningthe instrument settings for the e
17、lements in this matrix. Follow themanufacturers instructions to set the 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
18、 instruments responseover the range of solution concentrations given, a third standard, equidis-tant between the two listed standards, must be measured to verify linearity.6. Reagents6.1 Purity of ReagentsUnless otherwise indicated, allreagents used in this test method shall conform to the “ReagentG
19、rade” Specifications of the American Chemical Society.6Other chemicals 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.6.2 Purity of WaterUnless otherwise indicated, referenc
20、esto water shall be understood to mean reagent water as definedby Type II of Specification D 1193.6.3 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 ge
21、ntly 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 willremain undissolved). Transfer the solution to
22、 a 100-mL volu-metric flask, dilute to volume, and mix. Store in a polyethylenebottle.6.4 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 boil
23、ing 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.6.5 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
24、 % min) for4hat85C and cool to room temperature in a desiccator. Dissolve3.913 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.6.6 Cerium, Standard Solution B (1
25、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.6.7 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.6.
26、8 Iron, Standard Solution A (1 mL = 1.00 mg Fe)Transfer 1.000 g of iron (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
27、in the polyethylene bottle.6.9 Iron, Standard Solution B (1 mL = 0.010 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.6.10 Lanthanum, Standard Solution A (1 mL = 0.010 mgLa)Ignite lanthanum oxide (La2O3) (
28、purity: 99.9 % min) for1 h at 1000C and cool to room temperature in a 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.6.11 Lanthanum, Standa
29、rd 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.6.12 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 4
30、0 mL of HNO3(1 + 1). Boil gently tocomplete dissolution and to remove oxides of nitrogen. Cool,transfer to a 1-L volumetric flask, add 250 mL of HCl, dilute tovolume, and mix. Store in a polyethylene bottle.6.13 Zinc Matrix Solution (50 mL = 3.75 g Zinc MatrixStandard)Transfer 18.75 g 6 0.10 g of Zi
31、nc 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 all6Reagent Chemicals, American Chemical Society Spec
32、ifications, 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 the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Conv
33、ention, Inc. (USPC), Rockville,MD.TABLE 1 Wavelengths and Instrument ConditionsAElement Wavelength Time, s No. Integ. BCor1 BCor2Al 3092.7 1.0 3 . .Cd 2265.02 .5 3 2264.46 2265.58Ce 4186.6 .5 2 . .Fe 2599.4 .5 2 . .La 3988.5 .5 2 3987.54 3989.06Pb 2832.97 1.0 3 . 2833.36AThe tabulated conditions wer
34、e those found satisfactory on one instrument.Wavelengths are expressed in angstroms. Time = seconds for each integration,No. Integ. = number of integrations averaged for each reading, and BCor1 andBCor2 are off-peak background correction wavelengths.E1277022solids have dissolved, remove from the hea
35、t and allow to cool.Transfer to a 250-mL plastic volumetric flask, dilute to themark, and mix.6.14 Zinc Matrix StandardUse a zinc reference material7of known composition with respect to the elements listed in thescope of this test method.7. Hazards7.1 For precautions to be observed in the use of cer
36、tainreagents in this test method, refer to Practices E50.8. Sampling8.1 For procedures for sampling the material, refer toPractices E55andE88.9. Interlaboratory Studies and Rounding of CalculatedValues9.1 Only four laboratories were available to test thismethod, therefore, the interlaboratory test d
37、oes not complywith the protocol for Practice E 173. However, the statisticswere calculated according to Practice E 173.9.2 Calculated values shall be rounded to the desired num-ber of places as directed in 3.4 to 3.6 of Practice E29.9.3 E 173 has been replaced by Practice E 1601. The repro-ducibilit
38、y Index R, corresponds to the Reproducibility Index R2of Practice E 1601. Likewise the Repeatability Index R1ofE 173 corresponds to the Repeatability Index r of PracticeE 1601.10. Calibration10.1 Prepare calibration and test sample solutions beforecalibration measurements are started.10.2 Calibratio
39、n 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 MatrixSolution into each o
40、f 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:10.3 Test Sample SolutionTransfer a 3.8 to 4.2-g portionof the test sample weighed to the nearest 0
41、.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 mL of HNO3,let the solution cool for about 20 min, trans
42、fer 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 calculate and store the equations needed to convertinstrument readings from test samples directly into concentra
43、-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 5. If one of the parameters isa “lower limit” (used to establish a printed “less than” value),set it to 0 for each element. Enter the concentra
44、tions of theelements to be found in each calibration solution. Table 4 givesthe concentration table for solutions based upon NBS SRM7287as Zinc Matrix Standard. If a different Zinc MatrixStandard is used, Table 4 must be revised to reflect the differentcomposition of that material. Using the calibra
45、tion solutions,follow the manufacturers procedure to perform the instrumentcalibration at the wavelengths specified in Table 1. Withoutundue delay, proceed in accordance with 11.2.10.5 Nonautomatic ModeNo separate calibration run isrequired if intensity readings only are recorded. Set up theinstrume
46、nt to measure intensities at the wavelengths specifiedin Table 1 according to the manufacturers instructions andproceed to 11.3.11. Procedure11.1 Measurement SequencesTo reduce the distortion ofdata if instrument drift occurs while measurements are taken,solutions are presented to the instrument in
47、a specified orderand only a single reading (or, if desired, the average of severalintegrations) is recorded each time a solution is presented to theinstrument. Repeat the following sequence of solution presen-tations four times to obtain the required four replicate readings:calibration solution No.
48、1, calibration solution No. 2, testsample solution, calibration solution No. 3, and calibrationsolution No. 4. More than one test sample solution may bepresented to the instrument between calibration solutions No. 2and No. 3. Many instruments do not require a rinse betweeneach solution presentation,
49、 but it is advisable to rinse thesystem periodically. A rinse with dilution solution after eachcompleted sequence is the minimum recommended frequency.11.2 Automatic ModeCalibrate the instrument in accor-dance with 10.4. Without undue delay, proceed to analyze thesolutions as directed in 11.1.(WarningAttempting to shortenthe measurement time by substituting four readings taken7SRM 728, Intermediate Purity Zinc, available from The Office of StandardReference Materials, National Institute of Standards and Technology, Gaithersburg,MD 20899, has been f
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