Designation: E 1600 – 02

Standard Test Method for

Determination of Gold in Cyanide Solutions by Atomic
Absorption Spectrometry1
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 E 1060 Practice for Interlaboratory Testing of Spectro-

1.1 This test method covers the determination of gold in ore chemical Methods of Analysis5
processing cyanide solution in the range from 0.3 to 10.0 E 1601 Practice for Conducting an Interlaboratory Study to
µg/mL of gold by direct aspiration into an atomic absorption Evaluate the Performance of an Analytical Method6
spectrophotometer. 3. Terminology
1.1.1 This test method may also be applied to cyanide leach
solutions from metallurgical evaluation procedures. 3.1 Definitions—For definitions of terms used in this test
1.2 This standard does not purport to address all of the method, refer to Terminology E 135.
safety concerns, if any, associated with its use. It is the 4. Summary of Test Method
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 4.1 The sample solution is collected and preserved with
bility of regulatory limitations prior to use. Specific precau- sodium hydroxide, if necessary, by careful adjustment of pH.
tions are given in 8.3, 8.5, Section 9, and 10.4.1.1. The test solution is filtered and gold content is determined by
flame atomic absorption spectrophotometry.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
D 1193 Specification for Reagent Water2 5.1 In primary metallurgical processes for gold bearing ores,
D 1293 Test Methods for pH of Water2 gold is extracted with an alkaline cyanide solution. Metallur-
E 29 Practice for Using Significant Digits in Test Data to gical accounting, process control, and ore evaluation proce-
Determine Conformance with Specifications3 dures depend on accurate, precise, and prompt measurements
E 50 Practices for Apparatus, Reagents and Safety Precau- of the gold concentrations.
tions for Chemical Analysis of Metals4 5.2 This test method is a referee method for compliance
E 135 Terminology Relating to Analytical Chemistry for with compositional specifications for metal content. It is
Metals, Ores and Related Materials4 assumed that all who use this procedure will be trained analysts
E 173 Practice for Conducting Interlaboratory Studies of capable of performing common laboratory procedures skill-
Methods for Chemical Analysis of Metals5 fully and safely. It is expected that work will be performed in
E 663 Practice for Flame Atomic Absorption Analysis6 a properly equipped laboratory and that proper waste disposal
E 882 Guide for Accountability and Quality Control in the procedures will be followed. Follow appropriate quality con-
Chemical Analysis Laboratory6 trol practices such as those described in Guide E 882.
E 1024 Guide for Chemical Analysis of Metals and Metal 6. Interferences
Bearing Ores by Flame Atomic Absorption Spectropho-
tometry6 6.1 Elements normally found in ore processing cyanide
solutions do not interfere. Use of instrumental background
correction is required to compensate for nonspecific absorption
1
This test method is under the jurisdiction of ASTM Committee E01 on interferences in the flame.
Analytical Chemistry for Metal, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal- 7. Apparatus
lurgical Materials.
Current edition approved May 10, 2002. Published June 2002. Originally 7.1 Atomic Absorption Spectrophotometer, equipped with
published as E 1600 – 94. Last previous edition E 1600 – 96. background correction and capable of measuring gold at the
2
Annual Book of ASTM Standards, Vol 11.01. 242.8-nm wavelength using an air and acetylene flame over a
3
Annual Book of ASTM Standards, Vol 14.02.
4
Annual Book of ASTM Standards, Vol 03.05.
5
Discontinued 1998; Available from Global Engineering, 15 Inverness Way
East, Englewood, CO 80112.
6
Annual Book of ASTM Standards, Vol 03.06.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 E 1600
linear range from 0.3 to 10.0 µg/mL gold. 10. Procedure
10.1 Collect, store, and dispose of the sample in accordance
8. Reagents and Materials
with Practices E 50.
8.1 Purity of Reagents—Reagent grade chemicals shall be 10.2 Determine the pH of the solution immediately after
used in all tests. Unless otherwise indicated, it is intended that sampling in accordance with Test Method D 1293. If the pH of
all reagents conform to the specifications of the Committee on the sample is less than 10, adjust the pH with small additions
Analytical Reagents of the American Chemical Society were of solid sodium hydroxide, followed by mixing, until the pH is
such specifications are available.7 Other grades may be used, greater than 10.
provided it is first ascertained that the reagent is of sufficiently 10.3 Test Solutions—Filter two 50-mL portions of sample
high purity to permit its use without lessening the accuracy of solution through a coarse-porosity filter paper.
the determination. 10.4 Photometry:
8.2 Purity of Water—Unless otherwise indicated, references 10.4.1 Follow the instrument manufacturer’s instructions to
to water shall be understood to mean reagent water as defined adjust the instrument for gold at 242.8 nm. Warm up the
by Type I of Specification D 1193. instrument with background correction applied in accordance
8.3 Sodium Cyanide–Sodium Hydroxide Solution— with the manufacturer’s instructions. With the gold hollow
Dissolve 10 g of sodium hydroxide (NaOH) and 10 g of cathode lamp in position, energized and stabilized, adjust the
sodium cyanide (NaCN) in 1 L of water. (Warning—The wavelength to maximize the energy response of the 242.8-nm
preparation, storage, use, and disposal of NaCN solutions line. Light the burner, allow it to reach thermal equilibrium,
require special care and attention. Avoid any possibility of and adjust the instrument to zero while aspirating water.
inhalation, ingestion, or skin contact with the compound, its
10.4.1.1 The use of an air-acetylene, lean, blue flame and
solution, or its vapors. Work only in a well-ventilated hood.
caustic stabilized drain bottle is required. (Warning—Reaction
Refer to Practices E 50.)
of acid and cyanide solutions in the burner chamber drain
8.4 Gold Standard Solution A—Weigh 1.000 g of gold metal
bottle may release toxic hydrogen cyanide gas. Add an excess
(99.99 % min purity) and transfer to a 1-L beaker in a fume
of sodium hydroxide to the drain bottle to maintain the pH
hood. Add 200 mL of water, 80 mL of HCl, and 50 mL of
above 11.)
HNO3(1 + 1). Boil gently to expel NOx fumes, cool, transfer to
10.4.2 Precision of Measurements—Use Practice E 663 to
a 1-L volumetric flask, dilute to volume, and mix.
determine if the instrument precision is acceptable as follows:
8.4.1 A certified reference solution meeting these specifica-
10.4.2.1 Calibrate the instrument in accordance with the
tions may also be used.
manufacturer’s instructions in absorbance. Set the absorbance
8.5 Gold Calibration Solutions (0.5, 1.0, 2.0, 5.0, 10.0
to zero while aspirating the reference solution.
µg/mL)—In a fume hood, pipette 10 mL of gold standard
10.4.2.2 Aspirate the calibration solutions in order of in-
Solution A into a 1-L volumetric flask containing 100 mL of
creasing concentration, and select a calibration solution in the
sodium cyanide-sodium hydroxide solution. Dilute to volume
range from 0.2 to 0.4 absorbance.
and mix (10 µg/mL). (Warning—Reaction of acid or chlorine
and cyanide solutions releases toxic hydrogen cyanide or 10.4.2.3 Alternate readings on the selected calibration solu-
cyanogen chloride gases. Prepare in a fume hood.) tion and reference solution, and calculate the standard devia-
8.5.1 Pipette 5, 10, 20, and 50 mL of the 10 µg/mL gold tion of the readings on the selected calibration solution using
calibration solution into each of four 100-mL volumetric flasks, accepted statistical methods. Measure the standard deviation in
respectively. Add 10 mL of sodium cyanide-sodium hydroxide this way at increased measurement integration times until a
solution, dilute to volume, and mix. relatively constant value is achieved.
8.6 Reference Solution—Dilute 100 mL of sodium cyanide- 10.4.2.4 If the standard deviation under these conditions is
sodium hydroxide solution to 1 L with water. greater than 1 % of the average absorbance, determine the
cause of the variability (for example, deposits in the burner or
9. Hazards clogged capillary), and take corrective action.
9.1 For precautions to be observed in this method, refer to 10.4.2.5 If the minimum requirements are not met, do not
Practice E 50. use the instrument with this test method until the required
9.2 Hydrogen cyanide and alkali cyanide are very toxic stability is obtained.
substances. Use an efficient fume hood. Cyanide must be 10.4.2.6 Collect all instrumental measurements for the test
disposed of with care, avoiding contact with acid that releases method using the instrumental settings which gave the opti-
hydrogen cyanide gas. Oxidation of cyanide with chlorine or mum precision of measurement on the selected calibration
hypochlorite must be carried out at high pH (greater than 11) to solution.
prevent generation of toxic cyanogen chloride gas. 10.4.3 Linearity of Instrument Response—Use Practice
E 663 to determine if the instrument response is acceptable as
follows:
7
Reagent Chemical, American Chemical Society Specifications, American 10.4.3.1 Record absorbance measurements for each of the
Chemical Society, Washington, DC. For suggestions on the testing of reagents not calibration solutions and the reference solution, prior to deter-
listed by the American Chemical Society, see Analar Standards for Laboratory mining samples.
Chemicals, BDH Ltd., Poole Dorset, U. K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc., (USPC), Rockville, 10.4.3.2 Adequate instrument response is obtained if the
MD. difference between the 5-µg/mL calibration solution and the

2
 E 1600
10-µg/mL calibration solution is sufficient to permit estimation using the graphical method in accordance with Guide E 1024,
of 1⁄50 of the difference between them. by simple linear regression, or by an equivalent computer
10.4.3.3 Adequate linearity is confirmed if the slope of the method.
calibration curve between the 5 and 10-µg/mL calibration 11.3 Average the results of the duplicate test sample solu-
solutions is at least 90 % of the slope between the reference tions and round the results to the nearest 0.1 µg/mL in
solution and the 0.5-µg/mL calibration solution. accordance with Practice E 29.
10.4.4 High-Precision Method:
10.4.4.1 Calibrate the instrument in accordance with the 12. Precision and Bias
manufacturer’s instructions in absorbance or gold concentra- 12.1 Precision—An interlaboratory study was undertaken to
tion. test the precision of this test method in accordance with
10.4.4.2 Adjust the instrument to zero with the reference Practice E 173 on six solutions in eight laboratories. The
solution and measure the test sample solution to determine its results from the study are summarized in Table 1. Since as few
place in the order of increasing concentration of the calibration as three laboratories returned results for some of the materials,
solutions. Practice E 1060 was used to estimate the precision. The base
10.4.4.3 Aspirate the test solution and the closely bracketing data and statistics are documented.8
calibration solutions in order of increasing absorbance or NOTE 1—Solutions 1 through 6 were analyzed by more laboratories
concentration without intervening water aspirations. Repeat than Solutions 7 through 12.
three times and calculate the average absorbance or concentra- NOTE 2—The reproducability, R2 of Practice E 1060 corresponds to the
tion value for each of the three solutions. reproducability index, R, of Practice E 1601 and the repeatability, R1 of
10.4.5 Linear Curve Method: Practice E 1060 corresponds to the repeatability index, r, of Practice
10.4.5.1 Calibrate the instrument in accordance with the E 1601.
manufacturer’s instructions in absorbance or gold concentra- 12.1.1 Repeatability—The repeatability standard deviation
tion. (sw) ranged from 0.01 to 0.12 µg/mL gold over the range of the
10.4.5.2 Record the reference solution and calibration solu- materials tested. The R1 value in Table 1 for each of the
tion readings before and after each test sample solution, materials tested indicates the maximum difference expected
selecting a different calibration solution after each test solution. between results in a single laboratory at 95 % confidence.
10.4.5.3 Continue recording measurements until at least 12.1.2 Reproducibility—The reproducibility standard devia-
three readings have been recorded for all test sample solutions tion (ssr) ranged from 0.01 to 0.15 µg/mL gold over the range
and at least one reading has been recorded for each calibration of the materials tested. The R2 value in Table 1 for each of the
solution. Calculate the average reading for each of the solu- materials tested indicates the maximum difference expected
tions. between results in different laboratories at 95 % confidence.
12.2 Bias—No information on the bias of this test method is
11. Calculation known. Accepted reference materials were not included in the
11.1 High-Precision Method—The gold concentration of materials used in the interlaboratory study. Users of this test
the test solution is calculated in accordance with Guide E 1024 method are encouraged to employ accepted reference materi-
as follows: als, if available, and to judge the bias of the test method from
the difference between the accepted value for the gold concen-
At~Ch 2 C1!
Ct 5 (1) tration and the mean value from interlaboratory testing of the
~ Ah 2 A 1 !
reference material.
where:
Ct = concentration of gold in the test solution, µg/mL, 8
Ch = concentration of gold in the higher calibration solu- Supporting data are available from ASTM International Headquarters. Request
RR:E01-1013.
tion, µg/mL,
C1 = concentration of gold in the lower calibration solu-
TABLE 1 Gold in Cyanide Solutions—Statistical Information
tion, µg/mL,
At = average absorbance or concentration reading of the R1 (Practice R2 (Practice
Solutions Mean, Au, µg/mL E 1060), Au,µ E 1060), Au,
test solution, g/mL µg/mL
Ah = average absorbance or concentration reading of the
1, 4 2.19 0.10 0.18
higher calibration solution, and 2, 5 0.19 0.05 0.21
A1 = average absorbance or concentration of the lower 3, 6 0.96 0.02 0.05
calibration solution. 7, 10 4.87 0.17 0.22
8, 11 5.97 0.27 0.69
11.2 Linear Curve Method—Calculate the gold concentra- 9, 12 10.7 0.15 1.28
tion of each test sample solution in micrograms per millilitre

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 E 1600
13. Keywords
13.1 cyanide solutions; gold content

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