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Quantitative-Determination-of-Silver-Content-Using-Fire-Assay-New-proposal-AR25.pdf

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1、QUANTITATIVE DETERMINATION OF SILVER CONTENT USING FIRE ASSAY:NEW PROPOSAL FOR ISO TC174 Simone MarsanLBMA Assaying&Refining Conference17th March 20252ANALYTICAL METHODS FOR DETERMINING SILVER PURITY:A WIDE RANGE OF CHOICESpectrometric AnalysisMetallurgical AnalysisVolumetric AnalysisCupellation(Fir

2、e Assay)Inductively Coupled Plasma Mass Spectrometry(ICP-MS)Inductively Coupled Plasma Optical EmissionSpectrometry(ICP-OES)Spark-Optical Emission Spectrometry(Spark-OES/LA-Spark)X-Ray Fluorescence Spectrometry(WDXRF/EDXRF)Potentiometric TitrationTitration with indicator:Gay-Lussac,Mohr,Volhard,Faja

3、ns.3MethodSampleProsConsRangeCostCupellation method(fireassay)solidHistorical and well-established methodDestructive,affected by the presence of other metals400-999(proposed)Low(if Au by fire assay is in place)X-Ray FluorescenceSpectrometry(EDXRF)solidNon-destructive,quick,easy to useLimited sensiti

4、vity for light elements,expensive for equipmentIntended for jewellery products(800-958)Medium/HISpark-OESsolidHigh sensitivity,easy to useExpensive,requires sample preparation999HIfor trace determinationICP-OESliquidExtremely sensitive,trace detectionExpensive,complex to operate999 HIfor trace deter

5、minationVolumetric MethodsliquidGood precision,relatively simpleRequires specific reagents,less suitable for complex samples,affected by the presence of other metals100 to 999Quite low4ALTERNATIVES TO SILVER ASSAYING BY CUPELLATIONCan we still consider Silver assaying by cuppelation an up to date me

6、thod?Yes but repeatability&uncertainty must be evaluated very carefully!Overlapping area?MethodStandard05100 200 400 800 925 958 999(1000)Fire assayV ariousTitrationISO 11427:2024ED-X RFISO 23345:2021ICP-OESISO 15096:2020Spark-OESISO 18214:2024Ag5The determination of Ag content via fire assay is a t

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1. **ISO新提案**:ISO NP 25643提案将火试金法(Cupellation)标准化,用于400‰-999‰银含量测定,覆盖珠宝及贵金属产业链。 2. **方法对比**:火试金法成本低、历史久,但需评估重复性(如928‰时范围2.95‰);EDXRF、ICP-OES等非破坏性方法适用高纯度(>999‰)但成本高。 3. **干扰因素**:Au、Pt、Pd需量化,因其影响测量不确定度(如2022年含0.26‰ Au时,Ag测定范围2.28‰)。 4. **性能验证**: proficiency测试显示,无干扰时重复性良好(如803‰时范围1.16‰),含Pd或常见金属时需谨慎评估。 5. **标准进展**:提案处于委员会阶段(30),未来将评估<800‰范围的重复性。
**银含量测定方法?** **火试金法适用范围?** **ISO新标准进展?**
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