1、Designation: D7572 11aD7572 13Standard Guide forRecovery of Aqueous Cyanides by Extraction from MineRock and Soil After Remediation of Process Releases1This standard is issued under the fixed designation D7572; the number immediately following the designation indicates the year oforiginal adoption o
2、r, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This guide is applicable for the collection, extraction, and preservation of
3、extracts from mine rock and soil samples for theanalysis 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 practiceguide are recommended for the analysis oftotal cyanid
4、e, available cyanide, weak acid dissociable cyanide, and free cyanide by Test Methods D2036, D4282, D4374, D6888,D6994, D7237, and D7284. The information supplied in this practiceguide can also be applied to other analytical methods forcyanide, for example, US EPA Method 335.4.1.3 The procedure opti
5、ons methods appear in the following order:Procedure Option SectionsOption ALaboratory Processing of FieldPreserved Samples11 and 12Option BLaboratory Processing of MoistField Samples13 and 141.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included
6、in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.
7、2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD1293 Test Methods for pH of WaterD2036 Test Methods for Cyanides in WaterD3694 Practices for Preparation of Sample Containers and for Preservation of Organic ConstituentsD3856 Guide fo
8、r Management Systems in Laboratories Engaged in Analysis of WaterD4282 Test Method for Determination of Free Cyanide in Water and Wastewater by MicrodiffusionD4374 Test Methods for Cyanides in WaterAutomated Methods for Total Cyanide, Weak Acid Dissociable Cyanide, andThiocyanate (Withdrawn 2012)3D4
9、840 Guide for Sample Chain-of-Custody ProceduresD4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic ConstituentsD5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water AnalysisD6696 Guide for Understanding Cyanide Spe
10、cies1 This practiceguide is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis forOrganic Substances in Water.Current edition approved June 15, 2011June 1, 2013. Published July 2011July 2013. Originally approved in 20
11、09. Last previous edition published 20092011 as D757209.DOI: 10.1520/D7572-11A. 11a. DOI: 10.1520/D7572-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standa
12、rds Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version.
13、 Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section
14、appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D6888 Test Method forAvailable Cyanide with Ligand Displacement and Flow InjectionAnalysis (FIA) Utilizing Gas DiffusionSeparation and Amperometric Det
15、ectionD6994 Test Method for Determination of Metal Cyanide Complexes in Wastewater, Surface Water, Groundwater and DrinkingWater Using Anion Exchange Chromatography with UV DetectionD6696 Guide for Understanding Cyanide SpeciesD7237 Test Method for Free Cyanide with Flow InjectionAnalysis (FIA) Util
16、izing Gas Diffusion Separation andAmperometricDetectionD7284 Test Method for Total Cyanide in Water by Micro Distillation followed by Flow Injection Analysis with Gas DiffusionSeparation and Amperometric DetectionD7365 Practice for Sampling, Preservation and Mitigating Interferences in Water Samples
17、 for Analysis of CyanideD7511 Test Method for Total Cyanide by Segmented Flow Injection Analysis, In-Line Ultraviolet Digestion and AmperometricDetection2.2 U.S. EPA Methods:4EPA OIA-1677 Available Cyanide in WaterEPA Method 335.2 Cyanide, Total (Titrimetric; Spectrophotometric)EPA Method 335.4 Dete
18、rmination of Total Cyanide by Semi-Automated Colorimetry3. Terminology3.1 DefinitionsFor definitions of terms used in this practice,guide, refer to Terminology D1129 and Guide D6696.3.2 Definitions of Terms Specific to This Standard:3.2.1 mine rock, nore, waste rock or overburden excavated in order
19、to construct an ore-processing site, or recover metals orminerals during mining operations; or coarse processed ore such as heap-leach spoils.3.2.2 nominal size, nninin sampling, for a screen of the standard series, the opening that would pass 95 % of arepresentative sample.3.2.3 refrigeration, nsto
20、ring the sample between its freezing point and 6C.4. Summary of Guide4.1 Samples are collected in appropriate containers at the sampling site, refrigerated optionally field preserved, refrigerated, andtransported to the laboratory where they are weighed, optionally sub-sampled, the moisture is deter
21、mined or aqueous massestimated, and cyanides are extracted prior to analysis. Results of the analysis of the extract are applied to the original solid sampleto determine the apparent concentrationcontent of cyanides dissolved in water present in the solids as the result of the processrelease.on the
22、basis of dry weight.5. Significance and Use5.1 This practiceguide is intended as a means for obtaining an extract from mine rock and soil samples to measure cyanideconcentrations. content in the aqueous portion of the sample on a dry weight basis. Cyanide is analyzed in mine rock and soilextracts fo
23、r measurement of cyanide concentration; however, improper sample collection and extraction can result in significantpositive or negative bias.5.2 This practiceguide is designed to mobilize aqueous cyanides present in the solids, so that the resulting extract can be usedto assess leachate that could
24、potentially be produced from mine rock or soil.5.3 This practiceguide is not intended to simulate actual site leaching conditions.5.4 This practiceguide produces extracts that are amenable to the determination of trace cyanides. When trace cyanides arebeing determined, it is especially important tha
25、t precautions be taken in sample preservation, storage, and handling to avoidpossible contamination of the extracts.5.5 This practiceguide uses a comparative test method and is intended for use as a routine method for monitoring mine rockand soils. It is assumed that all who use this practiceguide w
26、ill 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 suchas those described in Guide D3856.5.6 This practiceguide identifies proper methods for obtaining mine
27、 rock and soil samples for the specific purpose of measuringcyanide concentrations.4 Available from United States Environmental Protection Agency (EPA), Ariel Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http:/www.epa.gov.D7572 1326. Interferences6.1 Many interferences are known for
28、 the analysis of cyanide and could effect the results of the analysis of extracts producedusing this practice.guide. Refer to Practice D7365 for proper handling of the extracts during sampling, mitigation of interferences,and preservation prior to cyanide analysis.6.2 Unless otherwise specified, sam
29、ples must be extracted as soon as possible after sampling and the extracts must be analyzedwithin 14 days; however, it is recommended to estimate the actual holding time for each new sample matrix as described in PracticeD4841. Certain sample matrices may require immediate analysis to avoid cyanide
30、degradation due to interferences.Aholding timestudy is required if there is evidence that cyanide degradation occurs from interferences which would cause the holding time tobe less than specified in this practiceguide or Practice D7365. Potential interferences for cyanide analytical methods are show
31、n inTable 1.7. Apparatus7.1 Agitation Equipment, of any type that rotates the extraction vessel in an end-over-end fashion at a rate of 30 6 2 r/min suchthat the axis of rotation is horizontal and it passes through the center of the bottle (see Fig. 1).7.2 Drying Pans or Dishes, for moisture content
32、 determinations, 500 g to 8 kg capacity.7.3 Drying OvenAny thermostatically controlled drying oven capable of maintaining a steady temperature of 62C in a rangeof 100 to 110C.7.4 Extraction Vessels, cylindrical, wide-mouth, of a composition suitable to the nature of the mine rock or soil and cyanide
33、analyses to be performed, constructed of materials that will not allow sorption of the constituents of interest, and sturdy enoughto withstand the impact of the falling sample fragments. The size of the container should be selected so that the sample, plusextraction fluid occupy approximately 5095 %
34、 of the container in order to provide good mixing without overfilling. Thecontainers must have water-tight closures of sufficient diameter to fill with the samples.7.5 Filtration Device, pressure or vacuum of a composition suitable to the nature of the analyses to be performed and equippedwith a pre
35、-washed glass wool or equivalent filter. An assembly for pre-filtration or a centrifuge may be required if filtration isdifficult. Warning (WarningAvoid passing excessive amounts of air through the sample during filtration to prevent liberationof toxic hydrogen cyanide or cyanogen chloride gas. Avoi
36、d passing excessive amounts of air through the sample during filtrationto prevent liberation of toxic hydrogen cyanide or cyanogen chloride gas.)7.6 Laboratory Balance, capable of weighing to 1.0 g.7.7 pH Meter, with a readability of 0.01 units and an accuracy of at least 60.1 units at 25C.7.8 Riffl
37、e Splitter, SplitterA stationary sampler comprising an even number of equally-sized, adjacent chutes discharging inopposite directions. For use with this practice, there must be a minimum of twelve contained chutes (not bars) with an openingwidth of at least 3 times the nominal size.NOTE 1For riffle
38、 splitting finer materials ( 12.5 (12.5 mm) it is recommended not to exceed 312312 times nominal size as it is required that thefull width of the riffle be used since the accuracy of the split increases with the number of chutes. For free-flowing materials, the 3 times top size maybe reduced to 1121
39、12 times provided it is ascertained that there is no chute plugging for a particular materialmaterial.7.9 Rotary Sample Divider, DividerA rotating sampler fed from a single point comprising equally-sized or adjustableproportional collection pans. For use with this practice,guide, there must be a min
40、imum opening width of at least 3 times thenominal size.8. Reagents8.1 Purity of ReagentsReagent grade chemicals shall be used in this practice.guide. Unless otherwise indicated, it is intendedthat all reagents shall conform to the specifications of the Committee on Analytical Reagents of the America
41、n Chemical Society,where such specifications are available.5 Other grades may be used, provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to wa
42、ter shall be understood to mean reagent water that meets thepurity specifications of Type I or Type II water, presented in Specification D1193.8.3 Concentrated Sodium Hydroxide Solution (0.4 M)In a 1-L volumetric flask, dissolve 16 g NaOH in reagent water anddilute to volume.8.4 Dilute Sodium Hydrox
43、ide Solution Extraction Fluid (0.04 M)In a 1-L volumetric flask, add 100 mL of 0.4 M NaOH inreagent water and dilute to volume.5 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe America
44、n Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD. (http:/)D7572 1338.5 Sample BottlesSee Section 10.210.4.1 for further information abo
45、ut sample bottles.9. Hazards9.1 WarningBecause of the toxicity of cyanide, great care must be exercised in its handling. Acidification of cyanidesolutions produces toxic hydrocyanic acid (HCN). Adequate ventilation is necessary when handling cyanide solutions and a fumehood should be utilized whenev
46、er possible.WarningBecause of the toxicity of cyanide, great care must be exercised in itsTABLE 1 Examples of Potential Interferences if not Mitigated in Standard Cyanide MethodsNOTE 1Alkyl halides were identified as a potential interference for the distillation methods, however they are not normall
47、y found in soil and minerock.Method Description Measurement Interferences NumberTotalCyanideAutomatedUVColorimetric AldehydesColorFatty AcidsKetonesMercuryNitrateNitriteOxidantsSulfidesTurbiditySulfur CompoundsThiocyanateCFR Kelada-01D4374TotalCyanideManualDistillationMgCl2Amperometric AldehydesCarb
48、onatesKetonesNitriteNitrateOxidantsSulfideSulfur CompoundsThiocyanateD7284D2036, Test Method ATotalCyanideManualDistillationMgCl2Manual orAutomatedColorimetricAldehydesCarbonatesFatty AcidsNitrateNitriteOxidantsSugarsSulfideSulfur CompoundsThiocyanateColorTurbidityD2036 Test Method AStandard Methods
49、 4500-CN C/E,EPA Method 335.2EPA Method 335.2,EPA Method 335.4TotalCyanideManualDistillationMgCl2Manual orAutomatedColorimetricAldehydesCarbonatesFatty AcidsKetonesNitrateNitriteOxidantsSugarsSulfideSulfur CompoundsThiocyanateColorTurbidityD2036, Test Method AStandard Methods 4500-CN C/EEPA Method 335.2EPA Method 335.4TotalCyanideManualDistillationMgCl2ISE AldehydesCarbonatesFatty AcidsKetonesNitrateNitriteOxidantsSulfideSulfur CompoundsThiocyanateColorTurbidityD2036, Test Method AD7572 134handling. Acidification of cyanide solutions p
