ASTM E1335-08
(Test Method)Standard Test Methods for Determination of Gold in Bullion by Fire Assay Cupellation Analysis
Standard Test Methods for Determination of Gold in Bullion by Fire Assay Cupellation Analysis
SIGNIFICANCE AND USE
These test methods are intended for the determination of the gold content of gold and silver bullion. It is assumed that all who use these test methods are trained assayers capable of performing common fire assay procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.
SCOPE
1.1 These test methods cover cupellation analysis of bullion having chemical compositions within the following limits:
Element Concentration Range, % Gold 0.5 to 4.0 and 20.0 to 99.8 Silver 1.0 to 99.5 Total gold plus silver75.0 to 100.0
1.2 These test methods appear in the following order:
Sections 20.0 % – 99.0 % gold10-17 0.5 % – 4.0 % gold18-23 98.9 % – 99.8 % gold24-30
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific safety hazards, see Section 8.
10.1 This test method covers cupellation analysis of gold in bullion containing 20.0 % to 99.0 % gold and 1.0 % to 80.0 % silver.
18.1 This test method covers the determination of gold in bullion estimated to contain from 0.5 % to 4.0 % gold and 75.0 % to 99.5 % silver.
24.1 This test method covers the cupellation analysis of gold in grade 99.5 refined gold.
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Designation: E1335 − 08
Standard Test Methods for
Determination of Gold in Bullion by Fire Assay Cupellation
1
Analysis
This standard is issued under the fixed designation E1335; 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 Scope Methods for Chemical Analysis of Metals (Withdrawn
3
1998)
1.1 These test methods cover cupellation analysis of bullion
E1601 Practice for Conducting an Interlaboratory Study to
having chemical compositions within the following limits:
Evaluate the Performance of an Analytical Method
Element Concentration Range, %
3. Terminology
Gold 0.5 to 4.0 and 20.0 to 99.8
Silver 1.0 to 99.5
3.1 Definitions—For definitions of terms used in these test
Total gold plus silver 75.0 to 100.0
methods, refer to Terminology E135.
1.2 These test methods appear in the following order:
3.2 Definitions of Terms Specific to This Standard:
Sections
3.2.1 anneal—a thermal treatment to change the properties
or grain structure of the product.
20.0% – 99.0% gold 10-17
0.5% – 4.0% gold 18-23
3.2.2 cupel—a small, shallow, porous cup, usually made of
98.9% – 99.8% gold 24-30
bone ash or from magnesium oxide.
1.3 The values stated in SI units are to be regarded as
3.2.3 cupellation—an oxidizing fusion of lead, sample base
standard. No other units of measurement are included in this
metals and gold, and silver in a cupel. The lead is oxidized to
standard.
litharge (PbO); other base metals which may be present, such
1.4 This standard does not purport to address all of the
ascopperandtin,areoxidizedaswell.Theoxidizedmetalsare
safety concerns, if any, associated with its use. It is the
absorbed into the cupel, leaving a gold and silver doré bead on
responsibility of the user of this standard to establish appro-
the cupel surface.
priate safety and health practices and determine the applica-
3.2.4 doré bead—a gold and silver alloy bead which results
bility of regulatory limitations prior to use. For specific safety
from cupellation.
hazards, see Section 8.
3.2.5 inquartation—theadditionofsilvertoanassaysample
2. Referenced Documents
to enable parting.
2
2.1 ASTM Standards:
3.2.6 part—the separation of silver from gold by selectively
B562 Specification for Refined Gold
dissolving the silver in acid, usually nitric acid (HNO ).
3
E50 Practices for Apparatus, Reagents, and Safety Consid-
3.2.7 proof—a synthetic standard having a composition
erations for Chemical Analysis of Metals, Ores, and
similar to the test sample.
Related Materials
3.2.8 proof correction—analyzing the proof concurrently
E135 Terminology Relating to Analytical Chemistry for
with the test sample and using the results to correct the final
Metals, Ores, and Related Materials
assay.
E173 Practice for Conducting Interlaboratory Studies of
4. Significance and Use
1
These test methods are under the jurisdiction of ASTM Committee E01 on 4.1 Thesetestmethodsareintendedforthedeterminationof
Analytical Chemistry for Metals, Ores, and Related Materials and are the direct
thegoldcontentofgoldandsilverbullion.Itisassumedthatall
responsibility of Subcommittee E01.05 on Cu, Pb, Zn, Cd, Sn, Be, Precious Metals,
who use these test methods are trained assayers capable of
their Alloys, and Related Metals.
performing common fire assay procedures skillfully and safely.
Current edition approved Nov. 1, 2008. Published December 2008. Originally
ε1
approved in 1990. Last previous edition approved in 2004 as E1335 – 04 . DOI: It is expected that work will be performed in a properly
10.1520/E1335-08.
equipped laboratory.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
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, PA19428-2959. United States
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E1335 − 08
5. Interferences 8.2 Use care when handling hot crucibles and operating
furnaces to avoid personal injury by either burn or electrical
5.1 If the bullion contains any of the following elements in
shock.
excess of the concentrations shown, the accuracy and precision
requirements of these test methods may not be achieved. 8.3 Lead and litharge (PbO) are toxic materials and are
volatile at low temperatures. Avoid inhalation, ingestion, or
Element Maximum Level, %
skin contact.
Arsenic 2.0
Antimony 2.0
9. Sampling
Bismuth 2.0
Iron 2.0 9.1 Use shot or pi
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:E1335–04 Designation:E1335–08
Standard Test Methods for
Determination of Gold in Bullion by Fire Assay Cupellation
1
Analysis
This standard is issued under the fixed designation E 1335; 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
´ NOTE—Editorial changes were made throughout the text in February 2006.
1. Scope
1.1 These test methods cover cupellation analysis of bullion having chemical compositions within the following limits:
Element Concentration Range, %
Gold 0.5 to 4.0 and 20.0 to 99.0
Gold 0.5 to 4.0 and 20.0 to 99.8
Silver 1.0 to 99.5
Total gold plus silver 75.0 to 100.0
1.2 These test methods appear in the following order:
Sections
20.0–99.0% gold 10-16 20.0% – 99.0% gold
0.5–4.0% gold 17-21 0.5% – 4.0% gold
98.9–99.8% gold 22-2898.9% – 99.8% gold
1.3
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific safety hazards, see Section 8.
2. Referenced Documents
2
2.1 ASTM Standards:
B 562 Specification for Refined Gold
E29Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E 50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related
Materials
E 135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E 173 Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals
E882Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
3
E 1601Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E1763Guide for Interpretation and Use of Results from Interlaboratory Testing of Chemical Analysis Methods Practice for
Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
3. Terminology
3.1Definitions:
3.1.1annealing
1
These test methods are under the jurisdiction ofASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the direct responsibility
of Subcommittee E01.03 on Precious Metals.
Current edition approved Oct.Nov. 1, 2004.2008. Published November 2004.December 2008. Originally approved in 1990. Last previous edition approved in 20032004
e1
as E 1335 – 034 .
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Withdrawn. 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, PA19428-2959, United States.
1
---------------------- Page: 1 ----------------------
E1335–08
3.1 Definitions—For definitions of terms used in these test methods, refer to Terminology E 135.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 anneal—a thermal treatment to change the properties or grain structure of the product.
3.1.2
3.2.2 cupel—a small, shallow, porous cup, usually made of bone ash or from magnesitum oxide.
3.1.33.2.3 cupellation—an oxidizing fusion of lead, sample base metals and gold, and silver in a cupel. The lead is oxidized
to litharge (PbO); other base metals which may be present, such as copper and tin, are oxidized as well. The oxidized metals are
absorbed into the cupel, leaving a gold and silver doré bead on the cupel surface.
3.1.4
3.2.4 doré bead—a gold and silver alloy bead which results from cupellation.
3.1.5
3.2.5 inquartation—the addition of silver to an assay sample to facilitate parting.
3.1.6parting—separating silver from gold by selectively dissolving the silver in acid, usually nitric acid.
3.1.7—the addition of silver to an assay sample to enable parting.
3.2.6 part—the separation of silver from gold by selectively dissolving the silver in acid, usually nitric acid (HNO ).
3
3.2.7 proof—a synthetic standard having a composition similar
...
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