ASTM B982-20

Standard Specification for Sampling and Sample Preparation of Lead and Lead Alloys for Optical Emission Spectrometric or ICP Analysis

ABSTRACT
This specification covers the sampling of lead and lead alloys to obtain a sample suitable for quantitative optical emission spectrochemical analysis. It includes 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. This specification, used in conjunction with an appropriate quantitative optical emission spectrochemical method, is suitable for use in manufacturing control, material or product acceptance, and development and research. It deals with ordering information, materials and manufacture, composition, sizes and shapes, appearance, lot, sampling for chemical analysis, apparatus, preparation of specimens, marking and special requirements, inspection, and rejection and rehearing.
SCOPE
1.1 This specification covers the sampling of lead and lead alloys to obtain a sample suitable for quantitative optical emission spectrochemical 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 inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions 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. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Sep-2020
• ICS: 77.120.60 - Lead, zinc, tin and their alloys
• Technical Committee: B02 - Nonferrous Metals and Alloys
• Drafting Committee: B02.02 - Refined Lead, Tin, Antimony, and Their Alloys

Relations

• Refers: ASTM E88-11(2017) - Standard Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition
• Effective Date: 01-Sep-2017
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011
• Refers: ASTM E88-11 - Standard Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition
• Effective Date: 01-May-2011
• Refers: ASTM E37-05(2011) - Standard Test Methods for Chemical Analysis of Pig Lead (Withdrawn 2020)
• Effective Date: 01-Feb-2011
• Refers: ASTM E177-10 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2010
• Refers: ASTM E691-08 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Oct-2008
• Refers: ASTM E29-08 - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 01-Oct-2008
• Refers: ASTM E177-08 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2008
• Refers: ASTM E29-06b - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 15-Nov-2006
• Refers: ASTM E177-06b - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 15-Nov-2006
• Refers: ASTM E177-06a - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2006
• Refers: ASTM E29-06a - Standard Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
• Effective Date: 15-Sep-2006

Overview

ASTM B982-20 is a standard specification developed by ASTM International that establishes the requirements and procedures for the sampling and sample preparation of lead and lead alloys for quantitative optical emission spectrometric or inductively coupled plasma (ICP) analysis. This standard ensures that samples taken from various forms of lead materials-including molten metal, fabricated or cast products, and forms that cannot be easily melted-are suitable for reliable chemical composition determination. Proper adherence to ASTM B982-20 guarantees representative sampling, accurate analysis, and consistency in quality assurance across manufacturing, product acceptance, and research environments.

Key Topics

• Sampling Procedures for Lead and Lead Alloys: Covers methods for obtaining samples from molten metal, fabricated or cast products, and hard-to-melt forms.
• Sample Preparation: Details cleaning, sawing, drilling, melting, machining, and solution preparation to ensure analytical accuracy for spectrochemical analysis.
• Apparatus and Equipment: Specifies requirements for ladles, sample molds, and lathes to avoid contamination and achieve homogenous samples.
• Lot Identification and Traceability: Defines how to assemble product lots, assign identification numbers, and ensure traceability for quality control.
• Marking and Documentation: Outlines the need for clear labelling of samples with lot numbers, types, and other identifiers.
• Precision and Reproducibility: Provides guidelines for achieving high repeatability within laboratories and comparability across different labs.
• Inspection, Rejection, and Rehearing: Sets processes for handling non-conforming material and dispute resolution.
• Safety and Regulatory Compliance: Emphasizes the user’s responsibility for implementing appropriate safety, health, and environmental measures.

Applications

ASTM B982-20 is instrumental in industries and laboratories that require precise chemical analysis of lead and lead alloys. Major use cases include:

• Manufacturing Control: Monitoring and verifying batch composition during lead or lead alloy production.
• Material or Product Acceptance: Ensuring that material shipments conform to compositional specifications before acceptance or further processing.
• Development and Research: Facilitating accurate material analysis required in alloy development, process optimization, or investigative studies.
• Quality Assurance: Supporting traceable documentation and representative testing in the supply chain of lead-based materials.
• Regulatory Testing: Assisting with compliance to industry regulations regarding composition and properties of lead products.

This standard is applicable to a wide range of products, such as lead used in batteries, construction, radiation shielding, and specialized industrial applications where sample integrity and analytical accuracy are critical.

Related Standards

Several referenced and supporting standards are integral to implementing ASTM B982-20:

• ASTM E88: Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition.
• ASTM E177: Practice for Use of the Terms Precision and Bias in ASTM Test Methods.
• ASTM E29: Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications.
• ASTM E691: Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method.
• Formerly referenced: ASTM E37, Test Methods for Chemical Analysis of Pig Lead (now withdrawn).

Consistent use of ASTM B982-20 in combination with these standards guarantees precise, repeatable, and traceable lead sampling processes, supporting advanced spectrochemical analysis and robust quality assurance in the lead metallurgy sector.

Keywords: ASTM B982-20, lead sampling, lead alloy sample preparation, optical emission spectrometric analysis, ICP analysis, spectrochemical analysis, quality control, nonferrous metals analysis, sample traceability, material acceptance, manufacturing control.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation:B982 −20
Standard Specification for
Sampling and Sample Preparation of Lead and Lead Alloys
for Optical Emission Spectrometric or ICPAnalysis
This standard is issued under the fixed designation B982; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope E37 Test Methods for Chemical Analysis of Pig Lead
(Withdrawn 2020)
1.1 This specification covers the sampling of lead and lead
E88 Practice for Sampling Nonferrous Metals and Alloys in
alloys to obtain a sample suitable for quantitative optical
Cast Form for Determination of Chemical Composition
emissionspectrochemicalanalysis.Includedareproceduresfor
E177 Practice for Use of the Terms Precision and Bias in
sample preparation, obtaining representative samples from
ASTM Test Methods
molten metal, from fabricated, or cast products that can be
E691 Practice for Conducting an Interlaboratory Study to
melted, and from other forms that cannot be melted.
Determine the Precision of a Test Method
1.2 The values stated in inch-pound units are to be regarded
3. Significance and Use
as standard. The values given in parentheses are mathematical
conversions to SI units that are provided for information only
3.1 This specification, used in conjunction with an appro-
and are not considered standard.
priate quantitative optical emission spectrochemical method, is
suitable for use in manufacturing control, material or product
1.3 This standard does not purport to address all of the
acceptance, and development and research.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Ordering Information
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4.1 Orders for refined lead under this specification shall
1.4 This international standard was developed in accor- include the following information:
dance with internationally recognized principles on standard-
4.1.1 ASTM designation and year of issue,
ization established in the Decision on Principles for the 4.1.2 Quantity (weight),
Development of International Standards, Guides and Recom- 4.1.3 Name of material (for example, pure lead),
mendations issued by the World Trade Organization Technical 4.1.4 Size and shape (see Section 7),
Barriers to Trade (TBT) Committee. 4.1.5 Grade, and
4.1.6 Certification or test report if specified (Section 13).
2. Referenced Documents
5. Materials and Manufacture
2.1 The following documents of the issue in effect on the
5.1 Lead shall be supplied in commercial standard forms or
date of material purchase form a part of this specification to the
shapes requested by the purchaser in the following grades:
extent referenced herein.
5.1.1 Low bismuth low silver pure lead,
2.2 ASTM Standards:
5.1.2 Refined pure lead,
E29 Practice for Using Significant Digits in Test Data to
5.1.3 Pure lead, and
Determine Conformance with Specifications
5.1.4 Chemical copper lead.
5.1.5 Calcium alloys.
5.1.6 Antimony alloys.
This specification is under the jurisdiction of ASTM Committee B02 on
5.2 The grade of lead listed in 5.1.1 – 5.1.6 shall be
Nonferrous Metals and Alloys and is the direct responsibility of Subcommittee
produced by any smelting and refining process from ore or
B02.02 on Refined Lead, Tin, Antimony, and Their Alloys.
recycled materials to meet the chemical requirements of this
Current edition approved Oct. 1, 2020. Published October 2020. Originally
ɛ1
approved in 2012. Last previous edition approved in 2014 as B982 – 14 . DOI:
specification.
10.1520/B0982-20.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
B982−20
6. Composition
6.1 This specification shall apply to lead alloys that contain
greater than 80 % Pb and meet the requirements of 5.2 for
material manufacture.
7. Sizes and Shapes
7.1 Pigs shall weigh up to a nominal 110 lb (50 kg).
7.2 Blocks or hogs shall be square or oblong and weigh up
to 2530 lb (1150 kg).
8. Appearance
8.1 The lead shall be reasonably free from surface
corrosion, surface cavities, excessive condensation or water,
and adhering foreign material.
9. Lot
9.1 All lead of the same type produced and cast at one time
shallconstitutealotforchemicalanalysis.Eachpigorblockof
thelotshallbearasingleidentifyingnumberthatcanberelated
to the manufacturing lot.
10. Sampling for Chemical Analysis
10.1 The sample for chemical analysis shall be selected by
one of the following methods:
10.1.1 Test samples taken from 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 Analysis—The supplier may obtain
FIG. 1Method of Sampling Lead by Sawing
samples from the lot of molten metal during casting.Asample
shouldbetakenatthebeginning,middleandendofcasting.All
orpartofthesesamplesmaybecastintoshapessuitableforuse
10.3.3.1 Sawing—The pigs selected shall be sawed com-
in spectrographic analytical methods. The composite element
pletely through as illustrated in Fig. 1. The sawings from the
average for the three grab samples will represent the lot.
pigs shall be mixed thoroughly and quartered, and the samples
10.3 Sampling of Cast Product: for analysis taken from the mixed material. The sawings must
10.3.1 If the lead is in the form of standard pigs (Fig. 1), the be free of extraneous material introduced from the saw blade.
sample for chemical analysis shall be taken in accordance with All sawings shall be treated with a strong magnet in order to
10.3.3.1, 10.3.3.2,or 10.3.3.3. remove iron introduced by sawing.
10.3.1.1 If the pigs differ in shape from those shown in Fig. 10.3.3.2 Drilling—The pigs shall be drilled at least halfway
1 or the product is cast into blocks or hogs, the supplier and the
through from two opposite sides as illustrated in Fig. 2.Adrill
purchaser shall agree mutually as to the method to be followed of about ⁄2 in. (12.7 mm) in diameter shall be used. In drilling,
in sampling such shapes. The method of sampling in 10.3 does the holes shall be spaced along a diagonal line from one corner
not apply to alloys that exhibit segregation of alloy agents of the pig to the other. Holes may be made in a single pig or in
during casting. This means the calcium aluminum alloys are each of several pigs placed as illustrated in Fig. 2.The drillings
not to be sampled according to this procedure. The preferred shall be clipped into pieces not over ⁄2 in. (12.7 mm) in length,
method of determining lot chemistry for calcium aluminum mixed thoroughly, and treated with a strong magnet to remove
lots is supplier sampling of quick frozen wafers during casting. iron introduced by drilling.
10.3.2 Sampling Pig Lead—A portion representative of the 10.3.3.3 Melting—Whole pigs, portions of pigs produced by
total shipment shall be selected at random for the final sample. sawing, drillings, or sawings shall be melted in a clean vessel.
For lots containing at least 100 000 lb (45 400 kg) of pig lead, The melting temperature must not exceed 685°F (363°C) to
one pig shall be taken from every 20 000 lb (9080 kg). For prevent excessive drossing. The lead must be stirred immedi-
smaller lots, a total of five pigs shall be taken. ately prior to sampling. The molten lead shall be cast into
10.3.3 SamplePreparation—Each pig shall be cleaned thor- shapes suitable for use in spectrographic analysis, cast into thin
oughly to rid the surface of dirt or adhering foreign material sample bars not to exceed ⁄8 in. (9.5 mm) thick for sawing, or
prior to sampling by one of the following methods: sawing, granulated by pouring into distilled water and drying the
drilling, or melting. material thoroughly. For sample bars, saw cuts shall be made
B982−20
11.2 Sample Molds, designed to produce homogeneous
chillcast specimens having smooth surfaces, free from surface
pockets and pores. The specimens shall be representative (in
the region to be excited) of the product metal. The samples
shall have a spectrochemical response similar to the standards
used in preparing the analytical curves. This is ensured by
casting standards and specimens in the same manner.Also, the
specimens shall have a repeatability of measurement for major
elements from excitation-to-excitation with a relative error of
no more than 2 %. 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
of the specimen. The mold dimensions are such as to produce
wafers approximately 2.5 in. (64 mm) in diameter by 0.5 in.
(13 mm) thickness. The mold excluding the handle must be
made of mild steel with a thickness in all dimensions of at least
0.5 in.This ensures 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 1.1 kg). Wafer specimens have been found to be
very homogeneous. If properly prepared, these specimens
provide very reliable results with only one burn. However, all
wafer specimens must be lathed according to 11.3 before
analysis or drilling.
11.2.2 Other Molds—Molds of different types, materials,
and dimensions may be used provided that the uniformity of
the specimens obtained is comparable to the uniformity of
specimensobtainedfromTypeAmolds.Further,thespecimens
shall have a spectrochemical response similar to the standards
used for preparing the analytical curves.
11.3 Lathe or Milling Machine—Lathe should be capable of
machining a smooth flat surface, 0.25 in. of material must be
removed from the surface.
FIG. 2Method of Sampling Lead by Drilling
12. Sampling
halfway across the bar from each side and staggered so that
12.1 Molten Metal—When molten metal is sampled, the
theyareabout ⁄2in.(12.7mm)apart.Thesawingssoproduced
temperature shall be well above the point at which any solid
are treated in accordance with 10.3.3.1.
phase can be present. Using a clean ladle, push any dross away
10.3.4 Sample Size:
from the sampling area. Then dip the ladle sideways into the
10.3.4.1 For spectrographic analysis, three samples shall be
clear area, well below the surface, and stir momentarily. Turn
prepared of a size and shape satisfactory for use by the
the ladle upright and quickly withdraw. Heating the ladle
laboratory at which the analysis is to be made.
preventsmetalfreezing,whileobtainingmetalwellbeneaththe
10.3.4.2 For wet chemical analysis, each prepared sample
surface minimizes the danger of inclusion of oxide. Unless the
(sawings, drillings, or granules) shall weigh at least 600 g.
mold is already hot, cast and discard a preliminary specimen.
10.3.5 Aspects of sampling and sample preparation not
12.2 Separate Sampling Ladles and Molds—Separate sam-
specifically covered in this specification shall be carried out in
pling molds and ladles are required where cross contamination
accordance with Practice E88.
can occur between alloys.
11. Apparatus
11.1 Ladle,ofsteel,designedtoholdsufficientmoltenmetal
to completely fill the sample mold, with a handle of sufficient
length to reach into a furnace, trough, pot, or crucible.
NOTE 1—Pure lead metal (Special High Grade) is sampled using a
ceramic or graphite ladle, as the solubility of iron in Special High Grade
Lead is suffici
...

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. Because
it 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 version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: B982 − 14 B982 − 20
Standard Specification for
Sampling and Sample Preparation of Lead and Lead Alloys
for Optical Emission Spectrometric or ICP Analysis
This standard is issued under the fixed designation B982; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Section 13.4.2 was corrected editorially in January 2016.
1. Scope
1.1 This specification covers the sampling of lead and lead alloys to obtain a sample suitable for quantitative optical emission
spectrochemical 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 inch-pound units are to be regarded as standard. The values given in parentheses are mathematical
conversions 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. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 The following documents of the issue in effect on the date of material purchase form a part of this specification to the extent
referenced herein.
2.2 ASTM Standards:
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E37 Test Methods for Chemical Analysis of Pig Lead (Withdrawn 2020)
E88 Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
This specification is under the jurisdiction of ASTM Committee B02 on Nonferrous Metals and Alloys and is the direct responsibility of Subcommittee B02.02 on Refined
Lead, Tin, Antimony, and Their Alloys.
Current edition approved Oct. 1, 2014Oct. 1, 2020. Published April 2015October 2020. Originally approved in 2012. Last previous edition approved in 20122014 as
ɛ1
B982B982 – 14 – 12. DOI: 10.1520/B0982–14E01. DOI: 10.1520/B0982-20.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
B982 − 20
3. Significance and Use
3.1 This specification, used in conjunction with an appropriate quantitative optical emission spectrochemical method, is suitable
for use in manufacturing control, material or product acceptance, and development and research.
4. Ordering Information
4.1 Orders for refined lead under this specification shall include the following information:
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, and
4.1.6 Certification or test report if specified (Section 13).
5. Materials and Manufacture
5.1 Lead shall be supplied in commercial standard forms or shapes 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, and
5.1.4 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 recycled materials
to meet the chemical requirements of this specification.
6. Composition
6.1 This specification shall apply to lead alloys that contain greater than 80 % Pb and meet the requirements of 5.2 for material
manufacture.
7. Sizes and Shapes
7.1 Pigs shall weigh up to a nominal 110 lb (50 kg).
7.2 Blocks or hogs shall be square or oblong and weigh up to 2530 lb (1150 kg).
8. Appearance
8.1 The lead shall be reasonably free from surface corrosion, surface cavities, excessive condensation or water, and adhering
foreign material.
B982 − 20
9. Lot
9.1 All lead of the same type produced and cast at one time shall constitute a lot for chemical analysis. Each pig or block of the
lot shall bear a single identifying number that can be related to the manufacturing lot.
10. Sampling for Chemical Analysis
10.1 The sample for chemical analysis shall be selected by one of the following methods:
10.1.1 Test samples taken formfrom 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 Analysis—The supplier may obtain samples from the lot of molten metal during casting. A sample should
be taken at the beginning, middle and end of casting. All or part of these samples may be cast into shapes suitable for use in
spectrographic 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 standard pigs (Fig. 1), the sample for chemical analysis shall be taken in accordance with
10.3.3.1, 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 the
purchaser shall agree mutually as to the method to be followed in sampling such shapes. The method of sampling in 10.3 does not
FIG. 1 Method of Sampling Lead by Sawing
B982 − 20
apply to alloys that exhibit segregation of alloy agents during casting. This means the calcium aluminum alloys are not to be
sampled according to this procedure. The preferred method of determining lot chemistry for calcium aluminum lots is supplier
sampling of quick frozen wafers during casting.
10.3.2 Sampling Pig Lead—A portion representative of the total shipment shall be selected at random for the final sample. For lots
containing at least 100 00000 lb (45 400 kg) of pig lead, one pig shall be taken from every 20 000 lb (9080 kg). For smaller lots,
a total of five pigs shall be taken.
10.3.3 Sample Preparation—Each pig shall be cleaned thoroughly to rid the surface of dirt or adhering foreign material prior to
sampling by one of the following methods: sawing, drilling, or melting.
10.3.3.1 Sawing—The pigs selected shall be sawed completely through as illustrated in Fig. 1. The sawings from the pigs shall
be mixed thoroughly and quartered, and the samples for analysis taken from the mixed material. The sawings must be free of
extraneous material introduced from the saw blade. All sawings shall be treated with a strong magnet in order to remove iron
introduced by sawing.
10.3.3.2 Drilling—The pigs shall be drilled at least halfway through from two opposite sides as illustrated in Fig. 2. A drill of about
⁄2 in. (12.7 mm) in diameter shall be used. In drilling, the holes shall be spaced along a diagonal line from one corner of the 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 shall be
clipped into pieces not over ⁄2 in. (12.7 mm) in length, mixed thoroughly, and treated with a strong magnet to remove iron
introduced by drilling.
10.3.3.3 Melting—Whole pigs, portions of pigs produced by sawing, drillings, or sawings shall be melted in a clean vessel. The
FIG. 2 Method of Sampling Lead by Drilling
B982 − 20
melting temperature must not exceed 685°F (363°C) to prevent excessive drossing. The lead must be stirred immediately prior to
sampling. The molten lead shall be cast into shapes suitable for use in spectrographic analysis, cast into thin sample bars not to
exceed ⁄8 in. (9.5 mm) thick for sawing, or granulated by pouring into distilled water and drying the material thoroughly. For
sample bars, saw cuts shall be made halfway across the bar from each side and staggered so that they are about ⁄2 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 laboratory at
which the analysis is to be made.
10.3.4.2 For wet chemical analysis, each prepared sample (sawings, drillings, or granules) shall weigh at least 600 g.
10.3.5 Aspects of sampling and sample preparation not specifically covered in this specification shall be carried out in accordance
with Practice E88.
11. Apparatus
11.1 Ladle, of steel, designed to hold sufficient molten metal to completely fill the sample mold, with a handle of sufficient length
to reach into a furnace, trough, pot, or crucible.
NOTE 1—Pure lead metal (Special High Grade) is sampled using a ceramic or graphite ladle, as the solubility of iron in Special High Grade Lead is
sufficient to cause a measurable contamination.
11.2 Sample Molds, designed to produce homogeneous chillcast specimens having smooth surfaces, free from surface pockets and
pores. The specimens shall be representative (in the region to be excited) of the product metal. The samples shall have a
spectrochemical response similar to the standards used in preparing the analytical curves. This is ensured by casting standards and
specimens in the same manner. Also, the specimens shall have a repeatability of measurement for major elements from
excitation-to-excitation with a relative error of no more than 2 %. 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 of the
specimen. The mold dimensions are such as to produce wafers approximately 2.5 in. (64 mm) in diameter by 0.5 in. (13 mm)
thickness. The mold excluding the handle must be made of mild steel with a thickness in all dimensions of at least 0.5 in. This
ensures that samples will cool quickly. The mold is made of steel or cast iron and weigh approximately 1.5 to 2. 5 2.5 lb (0.45
to 1.1 kg). Wafer specimens have been found to be very homogeneous. If properly prepared, these specimens provide very reliable
results with only one burn. However, all wafer specimens must be lathed according to 11.3 before analysis or drilling.
11.2.2 Other Molds—Molds of different types, materials, and dimensions may be used provided that the uniformity of the
specimens obtained is comparable to the uniformity of specimens obtained from Type A molds. Further, the specimens shall have
a spectrochemical response similar to the standards used for preparing the analytical curves.
11.3 Lathe or Milling Machine—Lathe should be capable of machining a smooth flat surface, 0.25 in. of material must be removed
from the surface.
FIG. 3 Wafer Mold
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. 13.
B982 − 20
12. Sampling
12.1 Molten Metal—When molten metal is sampled, the temperature shall be well above the point at which any solid phase can
be present. Using a clean ladle, push any dross away from the sampling area. Then dip the ladle sideways into the clear area, well
below 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, cast
and discard a preliminary specimen.
12.2 Separate Sampling Ladles and Molds—Separate sam
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