ASTM D7572-09
(Guide)Standard Guide for Recovery of Aqueous Cyanides by Extraction from Mine Rock and Soil After Remediation of Process Releases
Standard Guide for Recovery of Aqueous Cyanides by Extraction from Mine Rock and Soil After Remediation of Process Releases
SIGNIFICANCE AND USE
This practice is intended as a means for obtaining an extract from mine rock and soil samples to verify the effectiveness of cyanide release remediation. Cyanide is analyzed in mine rock and soil extracts after remediation of process spills, to demonstrate regulatory compliance; however, improper sample collection and extraction can result in significant positive or negative bias, potentially resulting in unnecessary permit violations or undetected cyanide releases into the environment.
This practice is designed to mobilize aqueous cyanides present in the solids, so that the resulting extract can be used to assess leachate that could potentially be produced from remediated mine rock or soil in the field.
This practice is not intended to simulate actual site leaching conditions.
This practice produces extracts that are amenable to the determination of minor (trace) constituents. When minor constituents are being determined, it is especially important that precautions be taken in sample preservation, storage and handling to avoid possible contamination of the extracts.
This practice uses a comparative test method and is intended for use as a routine method for monitoring remediated mine rock and soils after process releases and remediation. It is assumed that all who use this practice will be trained analysts capable of performing it skillfully and safely. It is expected that work will be performed in a properly equipped laboratory applying appropriate quality control practices such as those described in Guide D 3856.
SCOPE
1.1 This guide is applicable for the collection, extraction and preservation of extracts from mine rock and soil samples after remediation of cyanide process releases for the analysis of cyanide in the extracts. Responsibilities of field sampling personnel and the laboratory are indicated.
1.2 The sampling, preservation and extraction procedures described in this practice are recommended for the analysis of total cyanide, available cyanide, weak acid dissociable cyanide, and free cyanide by Test Methods D 2036, D 4282, D 4374, D 6888, D 6994, D 7237, and D 7284. The information supplied in this practice can also be applied to other analytical methods for cyanide, for example, US EPA Method 335.4.
1.3 The values stated in SI units are to be regarded as 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.
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Designation:D7572–09
Standard Guide for
Recovery of Aqueous Cyanides by Extraction from Mine
Rock and Soil After Remediation of Process Releases
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 D4282 Test Method for Determination of Free Cyanide in
Water and Wastewater by Microdiffusion
1.1 This guide is applicable for the collection, extraction
D4374 Test Methods for Cyanides in Water—Automated
and preservation of extracts from mine rock and soil samples
Methods for Total Cyanide, Weak Acid Dissociable Cya-
afterremediationofcyanideprocessreleasesfortheanalysisof
nide, and Thiocyanate
cyanide in the extracts. Responsibilities of field sampling
D4840 Guide for Sample Chain-of-Custody Procedures
personnel and the laboratory are indicated.
D5847 Practice for Writing Quality Control Specifications
1.2 The sampling, preservation and extraction procedures
for Standard Test Methods for Water Analysis
described in this practice are recommended for the analysis of
D4841 Practice for Estimation of Holding Time for Water
total cyanide, available cyanide, weak acid dissociable cya-
Samples Containing Organic and Inorganic Constituents
nide,andfreecyanidebyTestMethodsD2036,D4282,D4374,
D6888 Test Method for Available Cyanide with Ligand
D6888, D6994, D7237, and D7284. The information supplied
Displacement and Flow InjectionAnalysis (FIA) Utilizing
in this practice can also be applied to other analytical methods
Gas Diffusion Separation and Amperometric Detection
for cyanide, for example, US EPA Method 335.4.
D6994 Test Method for Determination of Metal Cyanide
1.3 The values stated in SI units are to be regarded as
Complexes in Wastewater, Surface Water, Groundwater
standard.
and Drinking Water UsingAnion Exchange Chromatogra-
1.4 This standard does not purport to address all of the
phy with UV Detection
safety concerns, if any, associated with its use. It is the
D6696 Guide for Understanding Cyanide Species
responsibility of the user of this standard to establish appro-
D7237 Test Method for Aquatic Free Cyanide with Flow
priate safety and health practices and determine the applica-
Injection Analysis (FIA) Utilizing Gas Diffusion Separa-
bility of regulatory limitations prior to use.
tion and Amperometric Detection
2. Referenced Documents
D7284 Test Method for Total Cyanide in Water by Micro
Distillation followed by Flow InjectionAnalysis with Gas
2.1 ASTM Standards:
Diffusion Separation and Amperometric Detection
D75 Practice for Sampling Aggregates
D7365 Practice for Sampling, Preservation and Mitigating
D1129 Terminology Relating to Water
Interferences in Water Samples for Analysis of Cyanide
D1193 Specification for Reagent Water
D7511 Test Method for Total Cyanide by Segmented Flow
D1293 Test Methods for pH of Water
Injection Analysis, In-Line Ultraviolet Digestion and Am-
D2036 Test Methods for Cyanides in Water
perometric Detection
D3694 Practices for Preparation of Sample Containers and
E877 Practice for Sampling and Sample Preparation of Iron
for Preservation of Organic Constituents
Ores and Related Materials for Determination of Chemical
D3856 Guide for Good Laboratory Practices in Laborato-
Composition
ries Engaged in Sampling and Analysis of Water
2.2 U.S. EPA Methods:
EPA OIA-1677 Available Cyanide in Water
This practice is under the jurisdiction of ASTM Committee D19 on Water and
EPAMethod 335.2 Cyanide,Total (Titrimetric; Spectropho-
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
tometric)
Organic Substances in Water.
EPA Method 335.4 Determination of Total Cyanide by
Current edition approved Oct. 1, 2009. Published October 2009. DOI: 10.1520/
D7572-09.
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 Available from United States Environmental Protection Agency (EPA), Ariel
Standards volume information, refer to the standard’s Document Summary page on Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http://
the ASTM website. www.epa.gov.
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D7572–09
Semi-Automated Colorimetry 6.2 Unless otherwise specified, samples must be extracted
within 72 hours and the extracts must be analyzed within 14
3. Terminology
days; however, it is recommended to estimate the actual
3.1 Definitions: For definitions of terms used in this prac-
holding time for each new sample matrix as described in
tice, refer to Terminology D1129 and Guide D6696. Practice D4841. Certain sample matrices may require imme-
3.2 Definitions of Terms Specific to This Standard:
diate analysis to avoid cyanide degradation due to interfer-
3.2.1 refrigeration, n—storingthesamplebetweenitsfreez- ences.Aholding time study is required if there is evidence that
ing point and 6°C.
cyanide degradation occurs from interferences which would
3.2.2 mine rock, n—ore, waste rock or overburden exca- cause the holding time to be less than specified in this practice
vated in order to construct an ore-processing site, or recover
or Practice D7365. Potential interferences for cyanide analyti-
metals or minerals during mining operations; or coarse pro- cal methods are shown in Table 1.
cessed ore such as heap-leach spoils.
7. Apparatus
4. Summary of Guide
7.1 Agitation Equipment, of any type that rotates the extrac-
4.1 Samples are collected in appropriate containers at the
tion vessel in an end-over-end fashion at a rate of 30 6 2 r/min
remediation site, refrigerated and transported to the laboratory
such that the axis of rotation is horizontal and it passes through
where they are weighed, sub-sampled, the moisture is deter-
the center of the bottle (see Fig. 1).
mined and cyanides are extracted prior to analysis. Results of
7.2 Drying Pans or Dishes, for moisture content determina-
the analysis of the extract are applied to the original solid
tions, 500 g to 8 kg capacity.
sample to determine the apparent concentration of cyanides
7.3 Drying Oven—Any thermostatically controlled drying
dissolved in water present in the solids as the result of the
oven capable of maintaining a steady temperature of 62°C in
process release.
a range of 100 to 110°C.
7.4 Extraction Vessels, cylindrical, wide-mouth, of a com-
5. Significance and Use
position suitable to the nature of the mine rock or soil and
5.1 This practice is intended as a means for obtaining an
cyanide analyses to be performed, constructed of materials that
extract from mine rock and soil samples to verify the effec-
will not allow sorption of the constituents of interest, and
tivenessofcyanidereleaseremediation.Cyanideisanalyzedin
sturdy enough to withstand the impact of the falling sample
mine rock and soil extracts after remediation of process spills,
fragments. The size of the container should be selected so that
to demonstrate regulatory compliance; however, improper
the sample, plus extraction fluid occupy approximately
sample collection and extraction can result in significant
50–95 % of the container in order to provide good mixing
positive or negative bias, potentially resulting in unnecessary
without overfilling. The containers must have water-tight
permit violations or undetected cyanide releases into the
closures of sufficient diameter to fill with the samples.
environment.
7.5 Filtration Device, pressure or vacuum of a composition
5.2 This practice is designed to mobilize aqueous cyanides
suitable to the nature of the analyses to be performed and
present in the solids, so that the resulting extract can be used to
equipped with a pre-washed glass wool or equivalent filter.An
assess leachate that could potentially be produced from reme-
assembly for pre-filtration or a centrifuge may be required if
diated mine rock or soil in the field.
filtration is difficult. Warning—Avoid passing excessive
5.3 This practice is not intended to simulate actual site
amounts of air through the sample during filtration to prevent
leaching conditions.
liberation of toxic hydrogen cyanide or cyanogen chloride gas.
5.4 This practice produces extracts that are amenable to the
7.6 Laboratory Balance, capable of weighing to 1.0 g.
determination of minor (trace) constituents. When minor con-
7.7 pH Meter, with a readability of 0.01 units and an
stituents are being determined, it is especially important that
accuracy of at least 60.1 units at 25°C.
precautions be taken in sample preservation, storage and
handling to avoid possible contamination of the extracts. 8. Reagents
5.5 This practice uses a comparative test method and is
8.1 Purity of Reagents—Reagent grade chemicals shall be
intendedforuseasaroutinemethodformonitoringremediated
used in this practice. Unless otherwise indicated, it is intended
mine rock and soils after process releases and remediation. It is
that all reagents shall conform to the specifications of the
assumed that all who use this practice will be trained analysts
Committee on Analytical Reagents of the American Chemical
capableofperformingitskillfullyandsafely.Itisexpectedthat
Society, where such specifications are available. Other grades
work will be performed in a properly equipped laboratory
may be used, provided it is first ascertained that the reagent is
applying appropriate quality control practices such as those
of sufficiently high purity to permit its use without lessening
described in Guide D3856.
the accuracy of the determination.
6. Interferences
6.1 Many interferences are known for the analysis of
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
cyanide and could effect the results of the analysis of extracts
listed by the American Chemical Society, see Annual Standards for Laboratory
produced using this practice. Refer to Practice D7365 for
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
proper handling of the extracts during sampling, mitigation of
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
interferences and preservation prior to cyanide analysis. MD.
D7572–09
TABLE 1 Examples of Potential Interferences if not Mitigated in Standard Cyanide Methods
Method Description Measurement Interferences Number
Total Automated Colorimetric Aldehydes CFR Kelada-01
Cyanide UV Color D4374
Fatty Acids
Mercury
Nitrate
Nitrite
Oxidants
Sulfides
Turbidity
Sulfur Compounds
Thiocyanate
Total Manual Amperometric Aldehydes D7284
Cyanide Distillation Carbonates D2036 Test Method A
MgCl 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,
Nitrate EPA Method 335.4
Nitrite
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Color
Turbidity
Total Manual ISE Aldehydes D2036 Test Method A
Cyanide Distillation Carbonates
MgCl Fatty Acids
Nitrate
Nitrite
Oxidants
Sulfide
Sulfur Compounds
Thiocyanate
Color
Turbidity
Total Manual Titrimetric Aldehydes D2036 Test Method A
Cyanide Distillation Carbonates
MgCl Fatty Acids
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
Available Flow Injection Amperometric Carbonates D6888, EPA OIA-1677
Cyanide Ligand Exchange Oxidants
Sulfide
D7572–09
TABLE 1 Continued
Method Description Measurement Interferences Number
Cyanide Alkaline Manual Aldehydes D2036 Test Method B
Amenable to Chlorination and Colorimetric Carbonates
Chlorination Manual Fatty Acids
Distillations 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
Nitrate
Nitrite
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Turbidity
Weak Acid Automated Automated Aldehydes D4374
Dissociable Method Colorimetric Color
Cyanide Fatty Acids
Mercury
Nitrate
Nitrite
Oxidants
Sulfides
Turbidity
Weak Acid Buffered ISE Aldehydes D2036 Test Method C
Dissociable Distillation Carbonates
Cyanide Fatty Acids
Nitrate
Nitrite
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Turbidity
Weak Acid Buffered Titrimetric Aldehydes D2036 Test Method C
Dissociable Distillation Carbonates
Cyanide Fatty Acids
Nitrate
Nitrite
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Turbidity
Weak Acid Manual Aldehydes D2036 Test Method B
Dissociable Colorimetric Carbonates
Cyanide Fatty Acids
Nitrite
Nitrate
Oxidants
Sugars
Sulfide
Sulfur Compounds
Thiocyanate
Volatile Compounds
D7572–09
TABLE 1 Continued
Method Description Measurement Interferences Number
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
Oxidants
Sulfide
Sulfur Compounds
FIG. 1 Extractors
D7572–09
8.2 Purity of Water—Unless otherwise indicated, references 10.4.1 Sample and extract containers shall be made of
to water shall be understood to mean reagent water that meets materials that will not contaminate the sample, vapor barrier
the purity specifications of Type I or Type II water, presented bags and bottles need to be cleaned thoroughly to remove all
in D1193. extraneous surface contamination prior to use, if necessary.
8.3 Concentrated Sodium Hydroxide Solution (0.4 M)—In a Chemically resistant rigid plastic containers, such as those
1-Lvolumetric flask, dissolve 16 g NaOH in reagent water and made of high density polyethelene (HDPE) are suitable.
dilute to volume. Samples should be collected and stored in opaque containers
8.4 Dilute Sodium Hydroxide Solution Extraction Fluid and sealed in vapor barrier bags to minimize exposure to
(0.04 M)—In a 1-L volumetric flask, add 100 mL of 0.4 M ultraviolet radiation and loss of moisture and hydrogen cya-
NaOH in reagent water and di
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