ASTM E1335-2008 Standard Test Methods for Determination of Gold in Bullion by Fire Assay Cupellation Analysis《用火试金灰吹法分析测定金条中纯金的标准试验方法》.pdf
《ASTM E1335-2008 Standard Test Methods for Determination of Gold in Bullion by Fire Assay Cupellation Analysis《用火试金灰吹法分析测定金条中纯金的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM E1335-2008 Standard Test Methods for Determination of Gold in Bullion by Fire Assay Cupellation Analysis《用火试金灰吹法分析测定金条中纯金的标准试验方法》.pdf(6页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E 1335 08Standard Test Methods forDetermination of Gold in Bullion by Fire Assay CupellationAnalysis1This standard is issued under the fixed designation E 1335; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、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. Scope1.1 These test methods cover cupellation analysis of bullionhaving chemical compositions within the following limits:El
3、ement Concentration Range, %Gold 0.5 to 4.0 and 20.0 to 99.8Silver 1.0 to 99.5Total gold plus silver 75.0 to 100.01.2 These test methods appear in the following order:Sections20.0 % 99.0 % gold 10-170.5 % 4.0 % gold 18-2398.9 % 99.8 % gold 24-301.3 The values stated in SI units are to be regarded as
4、standard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the
5、applica-bility of regulatory limitations prior to use. For specific safetyhazards, see Section 8.2. Referenced Documents2.1 ASTM Standards:2B 562 Specification for Refined GoldE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated Material
6、sE 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals3E 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method3. Termi
7、nology3.1 DefinitionsFor definitions of terms used in these testmethods, refer to Terminology E 135.3.2 Definitions of Terms Specific to This Standard:3.2.1 anneala thermal treatment to change the propertiesor grain structure of the product.3.2.2 cupela small, shallow, porous cup, usually made ofbon
8、e ash or from magnesium oxide.3.2.3 cupellationan oxidizing fusion of lead, sample basemetals and gold, and silver in a cupel. The lead is oxidized tolitharge (PbO); other base metals which may be present, suchas copper and tin, are oxidized as well. The oxidized metals areabsorbed into the cupel, l
9、eaving a gold and silver dor bead onthe cupel surface.3.2.4 dor beada gold and silver alloy bead which resultsfrom cupellation.3.2.5 inquartationthe addition of silver to an assaysample to enable parting.3.2.6 partthe separation of silver from gold by selectivelydissolving the silver in acid, usuall
10、y nitric acid (HNO3).3.2.7 proofa synthetic standard having a compositionsimilar to the test sample.3.2.8 proof correctionanalyzing the proof concurrentlywith the test sample and using the results to correct the finalassay.4. Significance and Use4.1 These test methods are intended for the determinat
11、ion ofthe gold content of gold and silver bullion. It is assumed that allwho use these test methods are trained assayers capable ofperforming common fire assay procedures skillfully and safely.It is expected that work will be performed in a properlyequipped laboratory.1These test methods are under t
12、he jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.03 on Precious Metals.Current edition approved Nov. 1, 2008. Published December 2008. Originallyapproved in 1990. Last previous edition approved i
13、n 2004 as E 1335 04e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version o
14、f this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Interferences5.1 If the bullion contains any of the following elements inexcess of the concentrations shown, the accuracy and
15、precisionrequirements of these test methods may not be achieved.Element Maximum Level, %Arsenic 2.0Antimony 2.0Bismuth 2.0Iron 2.0Nickel 2.0Platinum group, total (Ir, Os, Pd, Pt, Rh, Ru) 0.01Selenium 2.0Tellurium 2.0Thallium 2.0Tungsten 0.5Zinc 5.06. Apparatus6.1 Assay FurnaceCapable of temperatures
16、 up to1100 C, accurate to 6 10 C, with draft controls and fumehood.6.2 Hammer.6.3 Hammering Block.6.4 Rolling Mill.6.5 Analytical Balance.6.5.1 For Test Methods A and B, capable of weighing to0.01 mg.6.5.2 For Test Method C, capable of weighing to 0.002 mg.6.6 Parting BasketPlatinum basket or porcel
17、ain goochcrucibles in stainless steel basket/vessel.6.6.1 Gooch Porcelain Crucible13 mL capacity, bottominside diameter (ID) 18 mn, top ID 29 mn.6.6.2 Stainless Steel Basket316 stainless steel.7. Reagents47.1 Copper Metal, 99.9 % purity, minimum; 0.0005 % gold,maximum.7.2 Gold Metal, 99.99 % purity,
18、 minimum.7.2.1 Gold metal, 99.999 % purity, minimum for TestMethod C only.7.3 Lead Foil, 99.99 % purity, minimum (0.001 % silver,maximum; 0.0005 % gold, maximum).7.4 Silver Metal, 99.9 % purity, minimum (0.0005 % gold,maximum).7.5 Nitric Acid, 0.0002 % chloride, maximum.7.6 CupelsMagnesium oxide or
19、bone ash.8. Hazards8.1 For precautions to be observed in the use of certainreagents and equipment in these test methods refer to PracticesE50.8.2 Use care when handling hot crucibles and operatingfurnaces to avoid personal injury by either burn or electricalshock.8.3 Lead and litharge (PbO) are toxi
20、c materials and arevolatile at low temperatures. Avoid inhalation, ingestion, orskin contact.9. Sampling9.1 Use shot or pin tube samples. Brush the samples toremove any adhering glass or flux.9.2 Prepare shot samples from molten metal poured intowater. Use only whole single pieces between 1 mm and 3
21、 mmin diameter.9.3 Pin tube samples are prepared from molten metal drawninto vacuum-evacuated glass tubes. Break the glass and inspectthe samples to ensure that they are not hollow and that they arefree from slag and inclusions.9.3.1 Roll the samples lengthwise on a clean rolling mill to0.127 mm, th
22、en clean them with alcohol.9.3.2 Cut the strip into horizontal slices to obtain the desiredsample weight.9.4 Drillings are not usually as representative of a melt aspin tube or shot samples. If bar drillings are to be analyzed,obtain them as directed in Specification B 562.TEST METHOD A10. Scope10.1
23、 This test method covers cupellation analysis of gold inbullion containing 20.0 % to 99.0 % gold and 1.0 % to 80.0 %silver.11. Summary of Test Method11.1 A preliminary assay is performed to estimate theapproximate gold content and approximate gold plus silvercontent. Other methods such as X-ray fluo
24、rescence (XRF),inductively coupled plasma emission (ICP), direct currentplasma emission (DCP), or atomic absorption spectroscopy(AAS) can also be used for a preliminary assay if they havebeen shown to have an accuracy of better than 6 1 % for goldand 6 2 % for silver. The sample is weighed and silve
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