1、Designation: B982 141Standard Specification forSampling and Sample Preparation of Lead and Lead Alloysfor Optical Emission Spectrometric or ICP Analysis1This standard is issued under the fixed designation B982; the number immediately following the designation indicates the year oforiginal adoption o
2、r, in the case of revision, the 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.1NOTESection 13.4.2 was corrected editorially in January 2016.1. Scope1.1 This specificati
3、on covers the sampling of lead and leadalloys to obtain a sample suitable for quantitative opticalemission spectrochemical analysis. Included are procedures forsample preparation, obtaining representative samples frommolten metal, from fabricated, or cast products that can bemelted, and from other f
4、orms that cannot be melted.1.2 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.1.3 This standard does not purport to address all of thesa
5、fety 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.2. Referenced Documents2.1 The following documents of the issue in effect
6、 on thedate of material purchase form a part of this specification to theextent referenced herein.2.2 ASTM Standards:2E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE37 Test Methods for Chemical Analysis of Pig LeadE88 Practice for Sampling Nonferro
7、us Metals and Alloys inCast Form for Determination of Chemical CompositionE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Significance and Use3.1 This specification, used in co
8、njunction with an appro-priate quantitative optical emission spectrochemical method, issuitable for use in manufacturing control, material or productacceptance, and development and research.4. Ordering Information4.1 Orders for refined lead under this specification shallinclude the following informa
9、tion:4.1.1 ASTM designation and year of issue,4.1.2 Quantity (weight),4.1.3 Name of material (for example, pure lead),4.1.4 Size and shape (see Section 7),4.1.5 Grade, and4.1.6 Certification or test report if specified (Section 13).5. Materials and Manufacture5.1 Lead shall be supplied in commercial
10、 standard forms orshapes requested by the purchaser in the following grades:5.1.1 Low bismuth low silver pure lead,5.1.2 Refined pure lead,5.1.3 Pure lead, and5.1.4 Chemical copper lead.5.1.5 Calcium alloys.5.1.6 Antimony alloys.5.2 The grade of lead listed in 5.1.1 5.1.6 shall beproduced by any sme
11、lting and refining process from ore orrecycled materials to meet the chemical requirements of thisspecification.6. Composition6.1 This specification shall apply to lead alloys that containgreater than 80 % Pb and meet the requirements of 5.2 formaterial manufacture.7. Sizes and Shapes7.1 Pigs shall
12、weigh up to a nominal 110 lb (50 kg).1This specification is under the jurisdiction of ASTM Committee B02 onNonferrous Metals and Alloys and is the direct responsibility of SubcommitteeB02.02 on Refined Lead, Tin, Antimony, and Their Alloys.Current edition approved Oct. 1, 2014. Published April 2015.
13、 Originallyapproved in 2012. Last previous edition approved in 2012 as B982 12. DOI:10.1520/B098214E01.2For referenced ASTM standards, 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
14、 Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17.2 Blocks or hogs shall be square or oblong and weigh upto 2530 lb (1150 kg).8. Appearance8.1 The lead shall be reasonably free from surfacecor
15、rosion, surface cavities, excessive condensation or water,and adhering foreign material.9. Lot9.1 All lead of the same type produced and cast at one timeshall constitute a lot for chemical analysis. Each pig or block ofthe lot shall bear a single identifying number that can be relatedto the manufact
16、uring lot.10. Sampling for Chemical Analysis10.1 The sample for chemical analysis shall be selected byone of the following methods:10.1.1 Test samples taken form the lot during castingapplies to all materials.10.1.2 Test samples taken from the final solidified castproduct, for all materials except 5
17、.1.5, calcium alloys.10.2 Sampling for Lot AnalysisThe supplier may obtainsamples from the lot of molten metal during casting. A sampleshould be taken at the beginning, middle and end of casting.Allor part of these samples may be cast into shapes suitable for usein spectrographic analytical methods.
18、 The composite elementaverage for the three grab samples will represent the lot.10.3 Sampling of Cast Product:10.3.1 If the lead is in the form of standard pigs (Fig. 1), thesample for chemical analysis shall be taken in accordance with10.3.3.1, 10.3.3.2,or10.3.3.3.10.3.1.1 If the pigs differ in sha
19、pe from those shown in Fig.1 or the product is cast into blocks or hogs, the supplier and thepurchaser shall agree mutually as to the method to be followedin sampling such shapes. The method of sampling in 10.3 doesnot apply to alloys that exhibit segregation of alloy agentsduring casting. This mean
20、s the calcium aluminum alloys arenot to be sampled according to this procedure. The preferredmethod of determining lot chemistry for calcium aluminumlots is supplier sampling of quick frozen wafers during casting.10.3.2 Sampling Pig LeadA portion representative of thetotal shipment shall be selected
21、 at random for the final sample.For lots containing at least 100 00 lb (45 400 kg) of pig lead,one pig shall be taken from every 20 000 lb (9080 kg). Forsmaller lots, a total of five pigs shall be taken.10.3.3 Sample PreparationEach pig shall be cleaned thor-oughly to rid the surface of dirt or adhe
22、ring foreign materialprior to sampling by one of the following methods: sawing,drilling, or melting.10.3.3.1 SawingThe pigs selected shall be sawed com-pletely through as illustrated in Fig. 1. The sawings from thepigs shall be mixed thoroughly and quartered, and the samplesfor analysis taken from t
23、he mixed material. The sawings mustbe free of extraneous material introduced from the saw blade.All sawings shall be treated with a strong magnet in order toremove iron introduced by sawing.10.3.3.2 DrillingThe pigs shall be drilled at least halfwaythrough from two opposite sides as illustrated in F
24、ig. 2. A drillof about12 in. (12.7 mm) in diameter shall be used. In drilling,the holes shall be spaced along a diagonal line from one cornerof the pig to the other. Holes may be made in a single pig or ineach of several pigs placed as illustrated in Fig. 2. The drillingsshall be clipped into pieces
25、 not over12 in. (12.7 mm) in length,mixed thoroughly, and treated with a strong magnet to removeiron introduced by drilling.10.3.3.3 MeltingWhole pigs, portions of pigs produced bysawing, drillings, or sawings shall be melted in a clean vessel.The melting temperature must not exceed 685F (363C) topr
26、event excessive drossing. The lead must be stirred immedi-ately prior to sampling. The molten lead shall be cast intoshapes suitable for use in spectrographic analysis, cast into thinsample bars not to exceed38 in. (9.5 mm) thick for sawing, orgranulated by pouring into distilled water and drying th
27、ematerial thoroughly. For sample bars, saw cuts shall be madehalfway across the bar from each side and staggered so thatthey are about12 in. (12.7 mm) apart. The sawings so producedare treated in accordance with 10.3.3.1.10.3.4 Sample Size:10.3.4.1 For spectrographic analysis, three samples shall be
28、prepared of a size and shape satisfactory for use by thelaboratory at which the analysis is to be made.FIG. 1 Method of Sampling Lead by SawingB982 141210.3.4.2 For wet chemical analysis, each prepared sample(sawings, drillings, or granules) shall weigh at least 600 g.310.3.5 Aspects of sampling and
29、 sample preparation notspecifically covered in this specification shall be carried out inaccordance with Practice E88.11. Apparatus11.1 Ladle, of steel, designed to hold sufficient molten metalto completely fill the sample mold, with a handle of sufficientlength to reach into a furnace, trough, pot,
30、 or crucible.NOTE 1Pure lead metal (Special High Grade) is sampled using aceramic or graphite ladle, as the solubility of iron in Special High GradeLead is sufficient to cause a measurable contamination.11.2 Sample Molds, designed to produce homogeneouschillcast specimens having smooth surfaces, fre
31、e from surfacepockets and pores. The specimens shall be representative (inthe region to be excited) of the product metal. The samplesshall have a spectrochemical response similar to the standardsused in preparing the analytical curves. This is ensured bycasting standards and specimens in the same ma
32、nner. Also, thespecimens shall have a repeatability of measurement for majorelements from excitation-to-excitation with a relative error ofno more than 2 %. Several types of molds have been foundacceptable.11.2.1 Type A, Mass Chill Wafer Mold (Fig. 3)This moldproduces one diagonally cast wafer witho
33、ut a sprues on the topof the specimen. The mold dimensions are such as to producewafers approximately 2.5 in. (64 mm) in diameter by 0.5 in.(13 mm) thickness. The mold excluding the handle must bemade of mild steel with a thickness in all dimensions of at least0.5 in. This ensures that samples will
34、cool quickly. The mold ismade of steel or cast iron and weigh approximately 1.5 to 2. 5lb (0.45 to 1.1 kg). Wafer specimens have been found to bevery homogeneous. If properly prepared, these specimensprovide very reliable results with only one burn. However, allwafer specimens must be lathed accordi
35、ng to 11.3 beforeanalysis or drilling.11.2.2 Other MoldsMolds of different types, materials,and dimensions may be used provided that the uniformity ofthe specimens obtained is comparable to the uniformity ofspecimens obtained from TypeAmolds. Further, the specimensshall have a spectrochemical respon
36、se similar to the standardsused for preparing the analytical curves.11.3 Lathe or Milling MachineLathe should be capable ofmachining a smooth flat surface, 0.25 in. of material must beremoved from the surface.12. Sampling12.1 Molten MetalWhen molten metal is sampled, thetemperature shall be well abo
37、ve the point at which any solidphase can be present. Using a clean ladle, push any dross awayfrom the sampling area. Then dip the ladle sideways into theclear area, well below the surface, and stir momentarily. Turnthe ladle upright and quickly withdraw. Heating the ladleprevents metal freezing, whi
38、le obtaining metal well beneath thesurface minimizes the danger of inclusion of oxide. Unless themold is already hot, cast and discard a preliminary specimen.12.2 Separate Sampling Ladles and MoldsSeparate sam-pling molds and ladles are required where cross contaminationcan occur between alloys.12.3
39、 Pouring of SamplesRemove any excess metal fromthe ladle, dip it into the molten metal as before, and fill themold (Section 11). Avoid overfilling the mold. Allow the metalto freeze without jarring. The sample should be visibly solidwithin 5 s. The cast surfaces of the specimen, upon removalfrom the
40、 mold, shall be free from shrinkage, inclusions, cracks,or roughness.3Fox, G. J., “Determination of As, Sb, and Te in Lead and Lead Alloys UsingHydride Generation Atomic Absorption Spectrometry,” Atomic Spectroscopy,Vol11, No. 1, January 1990, p. 13.FIG. 2 Method of Sampling Lead by DrillingFIG. 3 W
41、afer MoldB982 1413NOTE 2A change in the temperature profile of the mold, caused by asignificant change in the sampling rate, may result in different Mass-Chill-Cast characteristics and poor repeatability. Therefore, it is recommendedthat the sampling schedule be considered when an analysis program i
42、sbeing developed. Also, experience has shown that wafer specimens aremuch less sensitive than disk samples to temperature profile changes in themold.13. Preparation of Specimens13.1 Mass-Chill-Cast Wafers from Type A MoldA mini-mum of14 in. must be machined off of the sample, with a lathecompliant t
43、o 11.3.13.2 Mass-Chill-Cast Specimens from Other AcceptableMoldsSince a mold of different dimensions may result in adifferent freezing pattern, each type of mold shall be evaluatedto determine the proper area and depth to machine thespecimen to represent the true composition of the melt.13.3 Direct
44、Excitation Without Casting a SpecimenIf theprocedure outlined in Section 12 cannot be followed, onlyapproximate analyses can be made. The specimen shall bemassive enough to prevent undue heating and shall have a flatsurface suitable for excitation. Further, standards having asimilar spectrochemical
45、response shall be available. On sheetor plate specimens, machine off about 0.03 in. (0.8 mm) orone-fourth of the thickness, whichever is smaller. On thickerspecimens, machine at least 0.05 in. (1.3 mm) below theoriginal surface. Choose the location, depth, and number ofareas to be analyzed to provid
46、e a representative analysis of theproduct.13.4 Sample Preparation for ICP or AA Analysis:13.4.1 Taking the sample into solution:1.) In a 250 mL beaker make up a solution of; 3 g Tartaricacid, 25 mL 30 % H2O2. Bring to 100 mL level with distilledH2O. Heat solution until Tartaric is dissolved.2.) In a
47、 250 mL beaker, put your weighed out sample(normally use 0.2 g), add 30 mL HCL, 30 mL HNO3. Placebeaker on heat at 300C for 5 min.3.) Let the sample boil for about 5 min. then add about 20mL of the Tartaric solution. (Pay close attention when doingthis as it tends to try and boil over.) Let boil aga
48、in for about 5min. and add about 10 mL distilled H2O. At 10 min. incre-ments add 20 mL Tartaric and distilled H2O, as needed. About30 min. into the process add about 5 mL each of the HCL andHNO3. When clear, remove the sample and let cool to 90F. Atthis temperature dilute up to 200 mL with distilled
49、 water andrun the sample on the ICP or AA.13.4.2 Matrix MatchingIt is recommended that a knownprimary lead sample is run through the sample preparation andis run on an ICP or AA to verify that the method is correct andto rule out spectral interference and matrix effects. Thesesamples can be obtained through Brammer, NIST or ASTM.14. Marking and Special Requirements14.1 A brand, by which the supplier can be identified, shallbe cast or marked legibly upon each pig, block, or hog. Inaddition, other markings shall identify the material by type andlot
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