ASTM E1446-92(1997)e1
(Test Method)Standard Test Method for Chemical Analysis of Refined Gold by Direct Current Plasma Emission Spectrometry
Standard Test Method for Chemical Analysis of Refined Gold by Direct Current Plasma Emission Spectrometry
SCOPE
1.1 This test method covers the analysis of refined gold for the following elements having the following chemical composition limits:
1.2 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 precautionary statements, see Section 6.
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e1
Designation: E 1446 – 92 (1997)
Standard Test Method for
Chemical Analysis of Refined Gold by Direct Current
Plasma Emission Spectrometry
This standard is issued under the fixed designation E 1446; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—E 1446 was reapproved with a title change in April 1997.
1. Scope 3. Summary of Test Method
1.1 This test method covers the analysis of refined gold for 3.1 The sample is dissolved with acids. Calibration solu-
the following elements having the following chemical compo- tions are prepared from pure reagents to match the sample
sition limits: matrix. Analysis is performed with the d-c argon plasma
optical emission spectrometer. Element concentrations are
Element Concentration Range, ppm
Copper 17 to 300
measured by comparing emission intensities from the sample
Iron 6 to 150
with those of the calibration solutions. Copper is measured at
Lead 17 to 100
327.3 nm or 324.7 nm; iron at 259.9 nm; lead at 405.7 nm;
Palladium 7 to 350
Silver 17 to 500
palladium at 340.4 nm; and silver at 328.0 nm or 338.3 nm.
1.2 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 Thistestmethodfortheanalysisoffinegoldisprimarily
responsibility of the user of this standard to establish appro-
intended to test such material for compliance with composi-
priate safety and health practices and determine the applica-
tional specifications. It is assumed that all who use this test
bility of regulatory limitations prior to use. For specific
methodwillbetrainedanalystscapableofperformingcommon
precautionary statements, see Section 8.
laboratory procedures skillfully and safely. It is expected that
2. Referenced Documents
work will be performed in a properly equipped laboratory.
2.1 ASTM Standards:
5. Interferences
B 562 Specification for Refined Gold
5.1 Spectral line interferences and spectrochemical back-
E 29 Practice for Using Significant Digits in Test Data to
ground effects are overcome by preparing a matrix-matched
Determine Conformance with Specifications
calibration standard series to approximate the prepared sample.
E 50 Practices for Apparatus, Reagents, and Safety Precau-
5.2 The analyte wavelengths mentioned herein have been
tions for Chemical Analysis of Metals
previously evaluated for spectral line interferences and found
E 173 Practice for Conducting Interlaboratory Studies of
to be the optimum emission wavelengths for refined gold
Methods for Chemical Analysis of Metals
sample testing.Alternative wavelengths, if shown to be free of
E 691 Practice for Conducting An Interlaboratory Study to
interferences, may also be used.
Determine the Precision of a Test Method
E 882 Guide for Accountability and Quality Control in the
6. Apparatus
Chemical Analysis Laboratory
6.1 D-C Argon Plasma Optical Emission Spectrometer—
E 1097 Guide for Direct Current Plasma Emission Spec-
The instrument must be equipped with a sample nebulization
trometry Analysis
system compatible with mineral acids and with test solutions
containing 4 % total solids. Follow the manufacturer’s instruc-
tions for installation and operation.
This test method is under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
7. Reagents and Materials
responsibility of Subcommittee E01.03 on Precious Metals.
Current edition approved Jan. 15, 1992. Published June 1992.
7.1 Argon—Purity: 99.998 % minimum.
Annual Book of ASTM Standards, Vol 02.04.
7.2 Copper Standard Solution (1 mL 5 1.0 mg Cu)—
Annual Book of ASTM Standards, Vol 14.02.
Transfer 1.000 g of copper metal (purity: 99.9 % minimum) to
Annual Book of ASTM Standards, Vol 03.05.
Annual Book of ASTM Standards, Vol 03.06. a 400-mL beaker. Add 60 mL of HNO (1+1) in 10-mL
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E 1446
TABLE 1 Master Analyte Solution
increments and heat gently on a hot plate. When dissolution is
complete, cool, then transfer to a 1-L volumetric flask. Dilute Master Analyte Solution Final
Element Standard Solution, mL
Concentration, µg/mL
to volume with HNO (1+99) and mix. This solution is stable
Copper 6 60
for at least six months.
Iron 2 20
7.3 Iron Standard Solution (1 mL 5 1.0 mg Fe)—Transfer
Lead 2 20
1.000 g of iron metal (purity: 99.9 % minimum) to a 400-mL
Palladium 6 60
Silver 10 100
beaker.Add 50 mLof HCl plus HNO (4+1) and heat gently on
a hot plate. When dissolution is complete, cool and then
transfer to a 1-L volumetric flask. Dilute to volume with HCL
previously cleaned by boiling with HCl (1+1) for 10 min and
(1+99) and mix. This solution is stable for six months.
rinsing with water. Add 15 mL of HCl plus HNO (4+1) and
7.4 Lead Standard Solution (1 mL 5 1.0 mg Pb)—Transfer
heat gently until dissolved. If the gold does not completely
1.000 g of lead metal (purity: 99.9 % minimum) to a 400-mL
dissolve,add10mLofHClplusHNO (4+1)andheatgentlyto
beaker.Add 50 mLof HNO (1+4) and heat gently on hot plate 3
complete dissolution. Cool, then transfer by pipet 10 mL of
to dissolve and then cool. Transfer the lead solution to a 1-L
master analyte solution and dilute to volume with HCl (1+2),
volumetric flask, dilute to volume with water, and mix. This
and mix. This solution is equivalent to 300 ppm copper, 100
solution is stable for six months.
ppm iron, 100 ppm lead, 300 ppm palladium, and 500 ppm
7.5 Matrix Gold—Gold purity must be a minimum
silver in the matrix gold.
99.9999 % based on total metallic impurities.
10.1.3 Medium Calibration Solution—Weigh 2.000 6
7.6 Palladium Standard Solution (1 mL 5 1.0 mg Pd)—
0.003 g of matrix gold and transfer to a 50-mL volumetric
Transfer 1.000 g of palladium metal (purity: 99.9 % minimum)
flask, previously cleaned by boiling with HCl (1+1) for 10 min
to a 400-mL beaker. Add 50 mL of HCl plus HNO (4+1) and
and rinsing with water. Add 15 mL of HCl plus HNO (4+1)
heat gently on a hot plate. When dissolution is complete, cool,
and heat gently until dissolved. If the gold does not dissolve
then transfer to a 1-L volumetric flask and dilute to volume
completely,add10mLofHClplusHNO (4+1)andheatgently
with HCl (1+99) and mix. This solution is stable for six
to complete dissolution. Cool, then transfer by pipet 5 mL of
months.
the master analyte solution and dilute to volume with HCl
7.7 Silver Standard Solution (1 mL 5 1.0 mg Ag)—
(1+2), and mix. This solution is equivalent to 150 ppm copper;
Transfer 1.000 g of silver metal (purity: 99.9 % minimum) to
50 ppm iron; 50 ppm lead; 150 ppm palladium; and 250 ppm
a400-mLbeaker.Add60mLofHNO (1+1)andheatgentlyon
silver in the matrix gold.
a hot plate.When dissolution is complete, cool, then transfer to
10.1.4 Low Calibration Solution—Weigh 2.000 6 0.003
...
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