ASTM D7572-15(2022)

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: D7572 − 15 (Reapproved 2022)
Standard Guide for
Recovery of Aqueous Cyanides by Extraction from Mine
Rock and Soil
This standard is issued under the fixed designation D7572; 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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This guide is applicable for the collection, extraction,
D1129 Terminology Relating to Water
and preservation of extracts from mine rock and soil samples
D1193 Specification for Reagent Water
for the analysis of cyanide in the extracts. Responsibilities of
D1293 Test Methods for pH of Water
field sampling personnel and the laboratory are indicated.
D2036 Test Methods for Cyanides in Water
1.2 The sampling, preservation, and extraction procedures
D3694 Practices for Preparation of Sample Containers and
described in this guide are recommended for the analysis of
for Preservation of Organic Constituents
total cyanide, available cyanide, weak acid dissociable
D3856 Guide for Management Systems in Laboratories
cyanide, and free cyanide by Test Methods D2036, D4282,
Engaged in Analysis of Water
D4374, D6888, D6994, D7237, and D7284. The information
D4282 Test Method for Determination of Free Cyanide in
supplied in this guide can also be applied to other analytical
Water and Wastewater by Microdiffusion
methods for cyanide, for example, US EPA Method 335.4.
D4374 Test Methods for Cyanides in Water—Automated
1.3 The procedure options methods appear in the following Methods for Total Cyanide, Weak Acid Dissociable
order:
Cyanide, and Thiocyanate (Withdrawn 2012)
D4840 Guide for Sample Chain-of-Custody Procedures
Procedure Option Sections
Option A 11 and 12
D4841 Practice for Estimation of Holding Time for Water
Laboratory Processing of Field
Samples Containing Organic and Inorganic Constituents
Preserved Samples
D5847 Practice for Writing Quality Control Specifications
Option B 13 and 14
Laboratory Processing of Moist
for Standard Test Methods for Water Analysis
Field Samples
D6696 Guide for Understanding Cyanide Species
1.4 The values stated in SI units are to be regarded as
D6888 Test Method for Available Cyanides with Ligand
standard. No other units of measurement are included in this
Displacement and Flow InjectionAnalysis (FIA) Utilizing
standard.
Gas Diffusion Separation and Amperometric Detection
D6994 Test Method for Determination of Metal Cyanide
1.5 This standard does not purport to address all of the
Complexes in Wastewater, Surface Water, Groundwater
safety concerns, if any, associated with its use. It is the
and Drinking Water Using Anion Exchange Chromatog-
responsibility of the user of this standard to establish appro-
raphy with UV Detection
priate safety, health, and environmental practices and deter-
D7237 Test Method for Free Cyanide and Aquatic Free
mine the applicability of regulatory limitations prior to use.
Cyanide with Flow InjectionAnalysis (FIA) Utilizing Gas
1.6 This international standard was developed in accor-
Diffusion Separation and Amperometric Detection
dance with internationally recognized principles on standard-
D7284 Test Method for Total Cyanide in Water by Micro
ization established in the Decision on Principles for the
Distillation followed by Flow InjectionAnalysis with Gas
Development of International Standards, Guides and Recom-
Diffusion Separation and Amperometric Detection
mendations issued by the World Trade Organization Technical
D7365 Practice for Sampling, Preservation and Mitigating
Barriers to Trade (TBT) Committee.
Interferences in Water Samples for Analysis of Cyanide
1 2
This guide is under the jurisdiction ofASTM Committee D19 on Water and is For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the direct responsibility of Subcommittee D19.06 on Methods for Analysis for contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Organic Substances in Water. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2022. Published May 2022. Originally the ASTM website.
approved in 2009. Last previous edition published 2015 as D7572 – 15. DOI: The last approved version of this historical standard is referenced on
10.1520/D7572-15R22. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7572 − 15 (2022)
D7511 Test Method for Total Cyanide by Segmented Flow in sample preservation, storage, and handling to avoid possible
InjectionAnalysis, In-Line Ultraviolet Digestion andAm- contamination of the extracts.
perometric Detection
5.5 This guide uses a comparative test method and is
2.2 U.S. EPA Methods:
intended for use as a routine method for monitoring mine rock
EPA OIA-1677 Available Cyanide in Water
and soils. It is assumed that all who use this guide will be
EPA Method 335.2 Cyanide, Total (Titrimetric; Spectropho-
trained analysts capable of performing it skillfully and safely.
tometric)
It is expected that work will be performed in a properly
EPA Method 335.4 Determination of Total Cyanide by
equipped laboratory applying appropriate quality control prac-
Semi-Automated Colorimetry
tices such as those described in Guide D3856.
5.6 This guide identifies proper methods for obtaining mine
3. Terminology
rock and soil samples for the specific purpose of measuring
3.1 Definitions—For definitions of terms used in this guide,
cyanide concentrations.
refer to Terminology D1129 and Guide D6696.
6. Interferences
3.2 Definitions of Terms Specific to This Standard:
6.1 Many interferences are known for the analysis of
3.2.1 mine rock, n—ore, waste rock or overburden exca-
vated in order to construct an ore-processing site, or recover cyanide and could effect the results of the analysis of extracts
produced using this guide. Refer to Practice D7365 for proper
metals or minerals during mining operations; or coarse pro-
cessed ore such as heap-leach spoils. handling of the extracts during sampling, mitigation of
interferences, and preservation prior to cyanide analysis.
3.2.2 nominal size, n—in sampling, for a screen of the
standard series, the opening that would pass 95 % of a
6.2 Unless otherwise specified, samples must be extracted
representative sample.
as soon as possible after sampling and the extracts must be
analyzed within 14 days; however, it is recommended to
3.2.3 refrigeration, n—storing the sample between its freez-
estimate the actual holding time for each new sample matrix as
ing point and 6 °C.
described in Practice D4841. Certain sample matrices may
requireimmediateanalysistoavoidcyanidedegradationdueto
4. Summary of Guide
interferences. A holding time study is required if there is
4.1 Samples are collected in appropriate containers at the
evidence that cyanide degradation occurs from interferences
sampling site, optionally field preserved, refrigerated, and
which would cause the holding time to be less than specified in
transported to the laboratory where they are weighed, option-
this guide or Practice D7365. Potential interferences for
ally sub-sampled, the moisture is determined or aqueous mass
cyanide analytical methods are shown in Table 1.
estimated, and cyanides are extracted prior to analysis. Results
of the analysis of the extract are applied to the original solid
7. Apparatus
sample to determine the apparent content of cyanides on the
7.1 Agitation Equipment, of any type that rotates the extrac-
basis of dry weight.
tion vessel in an end-over-end fashion at a rate of 30 6 2 r/min
such that the axis of rotation is horizontal and it passes through
5. Significance and Use
the center of the bottle (see Fig. 1).
5.1 This guide is intended as a means for obtaining an
7.2 Drying Pans or Dishes, for moisture content
extract from mine rock and soil samples to measure cyanide
determinations, 500 g to 8 kg capacity.
content in the aqueous portion of the sample on a dry weight
basis. Cyanide is analyzed in mine rock and soil extracts for
7.3 Drying Oven—Any thermostatically controlled drying
measurement of cyanide concentration; however, improper oven capable of maintaining a steady temperature of 62°Cin
sample collection and extraction can result in significant
a range of 100 °C to 110 °C.
positive or negative bias.
7.4 Extraction Vessels, cylindrical, wide-mouth, of a com-
5.2 This guide is designed to mobilize aqueous cyanides
position suitable to the nature of the mine rock or soil and
present in the solids, so that the resulting extract can be used to cyanide analyses to be performed, constructed of materials that
assess leachate that could potentially be produced from mine
will not allow sorption of the constituents of interest, and
rock or soil.
sturdy enough to withstand the impact of the falling sample
fragments. The size of the container should be selected so that
5.3 This guide is not intended to simulate actual site
the sample, plus extraction fluid occupy approximately
leaching conditions.
50–95 % of the container in order to provide good mixing
5.4 This guide produces extracts that are amenable to the
without overfilling. The containers must have water-tight
determinationoftracecyanides.Whentracecyanidesarebeing
closures of sufficient diameter to fill with the samples.
determined, it is especially important that precautions be taken
7.5 Filtration Device, pressure or vacuum of a composition
suitable to the nature of the analyses to be performed and
equipped with a pre-washed glass wool or equivalent filter.An
Available from United States Environmental Protection Agency (EPA), Ariel
assembly for pre-filtration or a centrifuge may be required if
Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http://
www.epa.gov. filtration is difficult. (Warning—Avoid passing excessive
D7572 − 15 (2022)
TABLE 1 Examples of Potential Interferences if not Mitigated in Standard Cyanide Methods
NOTE 1—Alkyl halides were identified as a potential interference for the distillation methods, however they are not normally found in soil and mine
rock.
Method Description Measurement Interferences Number
Total Automated Colorimetric Aldehydes CFR Kelada-01
Cyanide UV Color D4374
Fatty Acids
Ketones
Mercury
Nitrate
Nitrite
Oxidants
Sulfides
Turbidity
Sulfur Compounds
Thiocyanate
Total Manual Amperometric Aldehydes D7284
Cyanide Distillation Carbonates D2036, Test Method A
MgCl Ketones
Nitrite
Nitrate
Oxidants
Sulfide
Sulfur Compounds
Thiocyanate
Total Manual Manual or Aldehydes D2036, Test Method A
Cyanide Distillation Automated Carbonates Standard Methods 4500-CN C/E
MgCl Colorimetric Fatty Acids EPA Method 335.2
Ketones EPA Method 335.4
Nitrate
Nitrite
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Color
Turbidity
Total Manual ISE Aldehydes D2036, Test Method A
Cyanide Distillation Carbonates
MgCl Fatty Acids
Ketones
Nitrate
Nitrite
Oxidants
Sulfide
Sulfur Compounds
Thiocyanate
Color
Turbidity
Total Manual Titrimetric Aldehydes D2036, Test Method A
Cyanide Distillation Carbonates
MgCl Fatty Acids
Ketones
Nitrate
Nitrite
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Turbidity
Total Micro Amperometric Carbonates D7284
Cyanide distillation Oxidants
Sulfide
Total UV/FIA Amperometric Carbonates D7511
Cyanide Oxidants
Sulfide
D7572 − 15 (2022)
TABLE 1 Continued
Method Description Measurement Interferences Number
Available Flow Injection Amperometric Carbonates D6888
Cyanide Ligand Exchange Oxidants EPA OIA-1677
Sulfide
Cyanide Alkaline Manual Aldehydes D2036, Test Method B
Amenable to Chlorination and Colorimetric Carbonates
Chlorination Manual Fatty Acids
Distillations Ketones
Nitrate
Nitrite
Oxidants
Sulfide
Sulfur Compounds
Thiocyanate
Color
Turbidity
Unknowns that cause negative
results
Weak Acid Buffered Manual Aldehydes D2036, Test Method C
Dissociable Distillation Colorimetric Carbonates
Cyanide Fatty Acids
Ketones
Nitrate
Nitrite
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Turbidity
Weak Acid Automated Automated Aldehydes D4374
Dissociable Method Colorimetric Color
Cyanide Fatty Acids
Ketones
Mercury
Nitrate
Nitrite
Oxidants
Sulfides
Turbidity
Weak Acid Buffered ISE Aldehydes D2036, Test Method C
Dissociable Distillation Carbonates
Cyanide Fatty Acids
Ketones
Nitrate
Nitrite
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Turbidity
Weak Acid Buffered Titrimetric Aldehydes D2036, Test Method C
Dissociable Distillation Carbonates
Cyanide Fatty Acids
Ketones
Nitrate
Nitrite
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Turbidity
amounts of air through the sample during filtration to prevent 7.6 Laboratory Balance, capable of weighing to 1.0 g.
liberationoftoxichydrogencyanideorcyanogenchloridegas.)
D7572 − 15 (2022)
TABLE 1 Continued
Method Description Measurement Interferences Number
Weak Acid Manual Aldehydes D2036, Test Method B
Dissociable Colorimetric Carbonates
Cyanide Fatty Acids
Ketones
Nitrite
Nitrate
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Volatile Compounds
Metal Ion UV Carbonate D6994
Cyanide Chromatography Dissolved Solids
Complexes Metal Anions
Metal Cations
Oxidants
Photodecomposition
Free Cyanide Flow Injection Amperometric Carbonate D7237
Oxidants
Sulfide
Free Cyanide Microdiffusion Colorimetric Aldehydes D4282
Ketones
Oxidants
Sulfide
Sulfur Compounds
7.7 pH Meter, with a readability of 0.01 units and an may be used, provided it is first ascertained that the reagent is
accuracy of at least 60.1 units at 25 °C. of sufficiently high purity to permit its use without lessening
the accuracy of the determination.
7.8 Riffle Splitter—Astationary sampler comprising an even
number of equally-sized, adjacent chutes discharging in oppo-
8.2 Purity of Water—Unless otherwise indicated, references
site directions. For use with this practice, there must be a
to water shall be understood to mean reagent water that meets
minimum of twelve contained chutes (not bars) with an
the purity specifications of Type I or Type II water, presented
opening width of at least 3 times the nominal size.
in Specification D1193.
NOTE1—Forrifflesplittingfinermaterials(<3mm)the3timesnominal
8.3 Concentrated Sodium Hydroxide Solution (0.4 M)—In a
size should be increased to the point where the plugging of chutes is
1 Lvolumetric flask, dissolve 16 g NaOH in reagent water and
eliminated. For riffle splitting coarser materials (>12.5 mm) it is recom-
dilute to volume.
mended not to exceed 3 ⁄2 times nominal size as it is required that the full
width of the riffle be used since the accuracy of the split increases with the
8.4 Dilute Sodium Hydroxide Solution Extraction Fluid
number of chutes. For free-flowing materials, the 3 times top size may be
(0.04 M)—In a 1 L volumetric flask, add 100 mL of 0.4 M
reduced to 1 ⁄2 times provided it is ascertained that there is no chute
NaOH in reagent water and dilute to volume.
plugging for a particular material.
8.5 Sample Bottles—See Section 10.4.1 for further informa-
7.9 Rotary Sample Divider—A rotating sampler fed from a
single point comprising equally-sized or adjustable propor- tion about sample bottles.
tional collection pans. For use with this guide, there must be a
minimum opening width of at least 3 times the nominal size. 9. Hazards
9.1 Warning—Because of the toxicity of cyanide, great
8. Reagents
care must be exercised in its handling.Acidification of cyanide
8.1 Purity of Reagents—Reagent grade chemicals shall be
solutions produces toxic hydrocyanic acid (HCN). Adequate
used in this guide. Unless otherwise indicated, it is intended
ventilation is necessary when handling cyanide solutions and a
that all reagents shall conform to the specifications of the
fume hood should be utilized whenever possible.
Committee on Analytical Reagents of the American Chemical
9.2 Warning—Many of the reagents used in these test
Society, where such specifications are available. Other grades
methods are highly toxic. These reagents and their solutions
and extracted solids must be disposed of properly.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
10. Sam
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