ASTM E1600-96
(Test Method)Standard Test Method for Determination of Gold in Cyanide Solutions by Atomic Absorption Spectrometry
Standard Test Method for Determination of Gold in Cyanide Solutions by Atomic Absorption Spectrometry
SCOPE
1.1 This test method covers the determination of gold in ore processing cyanide solution in the range from 0.3 to 10.0 μg/mL of gold by direct aspiration into an atomic absorption spectrophotometer.
1.1.1 This test method may also be applied to cyanide leach solutions from metallurgical evaluation procedures.
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. Specific precautions are given in 8.3, 8.5, Section 9, and 10.4.1.1.
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Designation: E 1600 – 96
Standard Test Method for
Determination of Gold in Cyanide Solutions by Atomic
Absorption Spectrometry
This standard is issued under the fixed designation E 1600; 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.
1. Scope sodium hydroxide, if necessary, by careful adjustment of pH.
The test solution is filtered and gold content is determined by
1.1 This test method covers the determination of gold in ore
flame atomic absorption spectrophotometry.
processing cyanide solution in the range from 0.3 to 10.0
μg/mL of gold by direct aspiration into an atomic absorption
4. Significance and Use
spectrophotometer.
4.1 In primary metallurgical processes for gold bearing ores,
1.1.1 This test method may also be applied to cyanide leach
gold is extracted with an alkaline cyanide solution. Metallur-
solutions from metallurgical evaluation procedures.
gical accounting, process control, and ore evaluation proce-
1.2 This standard does not purport to address all of the
dures depend on accurate, precise, and prompt measurements
safety concerns, if any, associated with its use. It is the
of the gold concentrations.
responsibility of the user of this standard to establish appro-
4.2 This test method is a referee method for compliance
priate safety and health practices and determine the applica-
with compositional specifications for metal content. It is
bility of regulatory limitations prior to use. Specific precau-
assumed that all who use this procedure will be trained analysts
tions are given in Section 8 and in specific warning notes
capable of performing common laboratory procedures skill-
throughout.
fully and safely. It is expected that work will be performed in
2. Referenced Documents a properly equipped laboratory and that proper waste disposal
procedures will be followed. Follow appropriate quality con-
2.1 ASTM Standards:
trol practices such as those described in Guide E 882.
D 1293 Test Methods for pH of Water
E 29 Practice for Using Significant Digits in Test Data to
5. Interferences
Determine Conformance with Specifications
5.1 Elements normally found in ore processing cyanide
E 50 Practices for Apparatus, Reagents and Safety Precau-
4 solutions do not interfere. Use of instrumental background
tions for Chemical Analysis of Metals
correction is required to compensate for nonspecific absorption
E 173 Practice for Conducting Interlaboratory Studies of
4 interferences in the flame.
Methods for Chemical Analysis of Metals
E 663 Practice for Flame Atomic Absorption Analysis
6. Apparatus
E 882 Guide for Accountability and Quality Control in the
5 6.1 Atomic Absorption Spectrophotometer, equipped with
Chemical Analysis Laboratory
background correction and capable of measuring gold at the
E 1024 Guide for Chemical Analysis of Metals and Metal
242.8-nm wavelength using an air and acetylene flame over a
Bearing Ores by Flame Atomic Absorption Spectropho-
linear range from 0.3 to 10.0 μg/mL gold.
tometry
E 1060 Practice for Interlaboratory Testing of Spectro-
7. Reagents
chemical Methods of Analysis
7.1 Sodium Cyanide–Sodium Hydroxide Solution—
Dissolve 10 g of sodium hydroxide (NaOH) and 10 g of
3. Summary of Test Method
sodium cyanide (NaCN) in 1 L of water.
3.1 The sample solution is collected and preserved with
NOTE 1—Warning: The preparation, storage, use, and disposal of
NaCN solutions require special care and attention. Avoid any possibility of
This test method is under the jurisdiction of ASTM Committee E-1 on
inhalation, ingestion, or skin contact with the compound, its solution, or its
Analytical Chemistry for Metal, Ores, and Related Materials and is the direct
vapors. Work only in a well-ventilated hood. Refer to Practices E 50.
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
7.2 Gold Standard Solution A—Weigh 1.000 g of gold metal
Current edition approved April 10, 1996. Published June 1996. Originally
(99.99 % min purity) and transfer to a 1-L beaker in a fume
published as E 1600 – 94. Last previous edition E 1600 – 94.
Annual Book of ASTM Standards, Vol 11.01. hood. Add 200 mL of water, 80 mL of HCl, and 50 mL of
Annual Book of ASTM Standards, Vol 14.02.
HNO (1 + 1). Boil gently to expel NO fumes, cool, transfer to
3 x
Annual Book of ASTM Standards, Vol 03.05.
a 1-L volumetric flask, dilute to volume, and mix.
Annual Book of ASTM Standards, Vol 03.06.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 1600
7.2.1 A certified reference solution meeting these specifica- 9.4.2.3 Alternate readings on the selected calibration solu-
tions may also be used. tion and reference solution, and calculate the standard devia-
7.3 Gold Calibration Solutions (0.5, 1.0, 2.0, 5.0, 10.0 tion of the readings on the selected calibration solution using
μg/mL)—In a fume hood, pipette 10 mL of gold standard accepted statistical methods. Measure the standard deviation in
Solution A into a 1-L volumetric flask containing 100 mL of this way at increased measurement integration times until a
sodium cyanide-sodium hydroxide solution. Dilute to volume relatively constant value is achieved.
and mix (10 μg/mL). 9.4.2.4 If the standard deviation under these conditions is
greater than 1 % of the average absorbance, determine the
NOTE 2—Warning: Reaction of acid or chlorine and cyanide solutions
cause of the variability (for example, deposits in the burner or
releases toxic hydrogen cyanide or cyanogen chloride gases. Prepare in a
clogged capillary), and take corrective action.
fume hood.
9.4.2.5 If the minimum requirements are not met, do not use
7.3.1 Pipette 5, 10, 20, and 50 mL of the 10 μg/mL gold
the instrument with this test method until the required stability
calibration solution into each of four 100-mL volumetric flasks,
is obtained.
respectively. Add 10 mL of sodium cyanide-sodium hydroxide
9.4.2.6 Collect all instrumental measurements for the test
solution, dilute to volume, and mix.
method using the instrumental settings which gave the opti-
7.4 Reference Solution—Dilute 100 mL of sodium cyanide-
mum precision of measurement on the selected calibration
sodium hydroxide solution to 1 L with water.
solution.
9.4.3 Linearity of Instrument Response—Use Practice
8. Hazards
E 663 to determine if the instrument response is acceptable as
8.1 Hydrogen cyanide and alkali cyanide are very toxic
follows:
substances. Use an efficient fume hood. Cyanide must be
9.4.3.1 Record absorbance measurements for each of the
disposed of with care, avoiding contact with acid that releases
calibration solutions and the reference solution, prior to deter-
hydrogen cyanide gas. Oxidation of cyanide with chlorine or
mining samples.
hypochlorite must be carried out at high pH (greater than 11) to
9.4.3.2 Adequate instrument response is obtained if the
prevent generation of toxic cyanogen chloride gas.
difference between the 5-μg/mL calibration solution and the
10-μg/mL calibration solution is sufficient to permit estimation
9. Procedure
of ⁄50 of the difference between them.
9.1 Collect, store, and
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