1、Designation: B982 12B982 14Standard Specification forSampling and Sample Preparation of Lead and Lead Alloysfor Optical Emission Spectrometric ORor ICP Analysis1This standard is issued under the fixed designation B982; the number immediately following the designation indicates the year oforiginal ad
2、option or, 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.1. Scope1.1 This specification covers the sampling of lead and lead alloys to obta
3、in a sample suitable for quantitative optical emissionspectrochemical analysis. Included are procedures for sample preparation, obtaining representative samples from molten metal,from fabricated, or cast products that can be melted, and from other forms that cannot be melted.1.2 The values stated in
4、 inch-pound units are to be regarded as standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information only and are not considered standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use.
5、It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 The following documents of the issue in effect on the date of material purchase form a part of th
6、is specification to the extentreferenced herein.2.2 ASTM Standards:2E29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE37 Test Methods for Chemical Analysis of Pig LeadE88 Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determinati
7、on of Chemical CompositionE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Significance and Use3.1 This specification, used in conjunction with an appropriate quantitative opt
8、ical emission spectrochemical method, is suitablefor use in manufacturing control, material or product acceptance, and development and research.4. Ordering Information4.1 Orders for refined lead under this specification shall include the following information:4.1.1 ASTM designation and year of issue
9、,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 standard forms or shapes requested by the pu
10、rchaser in the following grades:5.1.1 Low bismuth low silver pure lead,1 This specification is under the jurisdiction ofASTM Committee B02 on Nonferrous Metals andAlloys and is the direct responsibility of Subcommittee B02.02 on RefinedLead, Tin, Antimony, and Their Alloys.Current edition approved M
11、ay 1, 2012Oct. 1, 2014. Published August 2012April 2015. Originally approved in 2012. Last previous edition approved in 2012 as B982 12. DOI: 10.1520/B098212.10.1520/B098214.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For A
12、nnual Book of ASTM Standardsvolume information, refer to the standardsstandards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit
13、 may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr H
14、arbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.1.2 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 be produced by any smelting and refining process from ore or r
15、ecycledmaterials to meet the chemical requirements of this specification.6. Composition6.1 This specification shall apply to lead alloys that contain greater than 80 % Pb and meet the requirements of 5.2 for materialmanufacture.7. Sizes and Shapes7.1 Pigs shall weigh up to a nominal 110 lb (50 kg).7
16、.2 Blocks or hogs shall be square or oblong and weigh up to 2530 lb (1150 kg).8. Appearance8.1 The lead shall be reasonably free from surface corrosion, surface cavities, excessive condensation or water, and adheringforeign material.9. Lot9.1 All lead of the same type produced and cast at one time s
17、hall constitute a lot for chemical analysis. Each pig or block ofthe lot shall bear a single identifying number that can be related to the manufacturing lot.10. Sampling for Chemical Analysis10.1 The sample for chemical analysis shall be selected by one of the following methods:10.1.1 Test samples t
18、aken form the lot during casting applies to all materials.10.1.2 Test samples taken from the final solidified cast product, for all materials except 5.1.5, calcium alloys.10.2 Sampling for Lot AnalysisThe supplier may obtain samples from the lot of molten metal during casting.Asample shouldbe taken
19、at the beginning, middle and end of casting. All or part of these samples may be cast into shapes suitable for use inspectrographic analytical methods. The composite element average 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 s
20、tandard pigs (Fig. 1), the sample for chemical analysis shall be taken in accordance with10.3.3.1, 10.3.3.2, or 10.3.3.3.10.3.1.1 If the pigs differ in shape 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
21、be followed in sampling such shapes. The method of sampling in 10.3 does notapply to alloys that exhibit segregation of alloy agents during casting. This means the calcium aluminum alloys are not to besampled according to this procedure. The preferred method of determining lot chemistry for calcium
22、aluminum lots is suppliersampling of quick frozen wafers during casting.10.3.2 Sampling Pig LeadA portion representative of the total shipment shall be selected at random for the final sample. Forlots containing at least 100 00 lb (45 400 kg) of pig lead, one pig shall be taken from every 20 000 lb
23、(9080 kg). For smaller lots,a total of five pigs shall be taken.10.3.3 Sample PreparationEach pig shall be cleaned thoroughly to rid the surface of dirt or adhering foreign material priorto sampling by one of the following methods: sawing, drilling, or melting.10.3.3.1 SawingThe pigs selected shall
24、be sawed completely through as illustrated in Fig. 1. The sawings from the pigs shallbe mixed thoroughly and quartered, and the samples for analysis taken from the mixed material. The sawings must be free ofextraneous material introduced from the saw blade. All sawings shall be treated with a strong
25、 magnet in order to remove ironintroduced by sawing.10.3.3.2 DrillingThe pigs shall be drilled at least halfway through from two opposite sides as illustrated in Fig. 2. A drill ofabout 12 in. (12.7 mm) in diameter shall be used. In drilling, the holes shall be spaced along a diagonal line from one
26、corner ofthe pig to the other. Holes may be made in a single pig or in each of several pigs placed as illustrated in Fig. 2. The drillings shallbe clipped into pieces not over 12 in. (12.7 mm) in length, mixed thoroughly, and treated with a strong magnet to remove ironintroduced by drilling.10.3.3.3
27、 MeltingWhole pigs, portions of pigs produced by sawing, drillings, or sawings shall be melted in a clean vessel. Themelting temperature must not exceed 685F (363C) to prevent excessive drossing. The lead must be stirred immediately prior tosampling. The molten lead shall be cast into shapes suitabl
28、e for use in spectrographic analysis, cast into thin sample bars not toexceed 38 in. (9.5 mm) thick for sawing, or granulated by pouring into distilled water and drying the material thoroughly. ForB982 142sample bars, saw cuts shall be made halfway across the bar from each side and staggered so that
29、 they are about 12 in. (12.7 mm)apart. The sawings so produced are treated in accordance with 10.3.3.1.10.3.4 Sample Size:10.3.4.1 For spectrographic analysis, three samples shall be prepared of a size and shape satisfactory for use by the laboratoryat which the analysis is to be made.10.3.4.2 For w
30、et chemical analysis, each prepared sample (sawings, drillings, or granules) shall weigh at least 600 g.310.3.5 Aspects of sampling and sample preparation not specifically covered in this specification shall be carried out inaccordance with Practice E88.11. Apparatus11.1 Ladle, of steel, designed to
31、 hold sufficient molten metal to completely fill the sample mold, with a handle of sufficientlength to reach into a furnace, trough, pot, or crucible.NOTE 1Pure lead metal (Special High Grade) is sampled using a ceramic or graphite ladle, as the solubility of iron in Special High Grade Lead issuffic
32、ient to cause a measurable contamination.11.2 Sample Molds, designed to produce homogeneous chillcast specimens having smooth surfaces, free from surface pocketsand pores. The specimens shall be representative (in the region to be excited) of the product metal. The samples shall have aspectrochemica
33、l response similar to the standards used in preparing the analytical curves. This is ensured by casting standards andspecimens in the same manner. Also, the specimens shall have a repeatability of measurement for major elements fromexcitation-to-excitation with a relative error of no more than 2 %.
34、Several types of molds have been found acceptable.11.2.1 Type A, Mass Chill Wafer Mold (Fig. 3)This mold produces one diagonally cast wafer without a sprues on the top ofthe specimen. The mold dimensions are such as to produce wafers approximately 2.5 in. (64 mm) in diameter by 0.5 in. (13 mm)thickn
35、ess. The mold excluding the handle must be made of mild steel with a thickness in all dimensions of at least 0.5 in. This3 Fox, G. J., “Determination of As, Sb, and Te in Lead and Lead Alloys Using Hydride Generation Atomic Absorption Spectrometry,” Atomic Spectroscopy, Vol 11, No.1, January 1990, p
36、. 13.FIG. 1 Method of Sampling Lead by SawingB982 143ensures that samples will cool quickly. The mold is made of steel or cast iron and weigh approximately 1.5 to 2. 5 lb (0.45 to 1.1kg). Wafer specimens have been found to be very homogeneous. If properly prepared, these specimens provide very relia
37、ble resultswith only one burn. However, all wafer specimens must be lathed according to 11.3 before analysis or drilling.11.2.2 Other MoldsMolds of different types, materials, and dimensions may be used provided that the uniformity of thespecimens obtained is comparable to the uniformity of specimen
38、s obtained from Type A molds. Further, the specimens shall havea spectrochemical response similar to the standards used for preparing the analytical curves.11.3 Lathe or Milling MachineLathe should be capable of machining a smooth flat surface, 0.25 in. of material must beremoved from the surface.12
39、. Sampling12.1 Molten MetalWhen molten metal is sampled, the temperature shall be well above the point at which any solid phase canbe present. Using a clean ladle, push any dross away from the sampling area. Then dip the ladle sideways into the clear area, wellFIG. 2 Method of Sampling Lead by Drill
40、ingFIG. 3 Wafer MoldB982 144below the surface, and stir momentarily. Turn the ladle upright and quickly withdraw. Heating the ladle prevents metal freezing,while obtaining metal well beneath the surface minimizes the danger of inclusion of oxide. Unless the mold is already hot, castand discard a pre
41、liminary specimen.12.2 Separate Sampling Ladles and MoldsSeparate sampling molds and ladles are required where cross contamination canoccur between alloys.12.3 Pouring of SamplesRemove any excess metal from the ladle, dip it into the molten metal as before, and fill the mold(Section 11). Avoid overf
42、illing the mold. Allow the metal to freeze without jarring. The sample should be visibly solid within 5s. The cast surfaces of the specimen, upon removal from the mold, shall be free from shrinkage, inclusions, cracks, or roughness.NOTE 2A change in the temperature profile of the mold, caused by a s
43、ignificant change in the sampling rate, may result in different Mass-Chill-Castcharacteristics and poor repeatability. Therefore, it is recommended that the sampling schedule be considered when an analysis program is beingdeveloped. Also, experience has shown that wafer specimens are much less sensi
44、tive than disk samples to temperature profile changes in the mold.13. Preparation of Specimens13.1 Mass-Chill-Cast Wafers from Type A MoldA minimum of 14 in. must be machined off of the sample, with a lathecompliant to 11.3.13.2 Mass-Chill-Cast Specimens from Other Acceptable MoldsSince a mold of di
45、fferent dimensions may result in a differentfreezing pattern, each type of mold shall be evaluated to determine the proper area and depth to machine the specimen to representthe true composition of the melt.13.3 Direct Excitation Without Casting a SpecimenIf the procedure outlined in Section 12 cann
46、ot be followed, onlyapproximate analyses can be made. The specimen shall be massive enough to prevent undue heating and shall have a flat surfacesuitable for excitation. Further, standards having a similar spectrochemical response shall be available. On sheet or platespecimens, machine off about 0.0
47、3 in. (0.8 mm) or one-fourth of the thickness, whichever is smaller. On thicker specimens,machine at least 0.05 in. (1.3 mm) below the original surface. Choose the location, depth, and number of areas to be analyzed toprovide a representative analysis of the product.13.4 Sample Preparation for ICP o
48、r AA Analysis:13.4.1 Taking the sample into solution:1.) In a 250 mL beaker make up a solution of; 3 g Tartaric acid, 25 mL 30 % H2O2. Bring to 100 mL level with distilled H2O.Heat solution until Tartaric is dissolved.2.) In a 250 mL beaker, put your weighed out sample (normally use 0.2 g), add 30 m
49、L HCL, 30 mL HNO3. Place beaker onheat at 300C for 5 min.3.) Let the sample boil for about 5 min. then add about 20 mL of the Tartaric solution. (Pay close attention when doing this asit tends to try and boil over.) Let boil again for about 5 min. and add about 10 mL distilled H2O. At 10 min. increments add 20mLTartaric and distilled H2O, as needed.About 30 min. into the process add about 5 mLeach of the HCLand HNO3. When clear,remove the sample and let cool to 90F. At this temperature dilute up to 200 mL with distilled water and run the sample on
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