ASTM C1234-11 Standard Practice for Preparation of Oils and Oily Waste Samples by High-Pressure, High-Temperature Digestion for Trace Element Determinations

微量元素测定用高压高温消解制备油和含油废料样品的标准实施规程

基本信息

标准号
ASTM C1234-11
标准状态
历史
发布单位或类别
美国-美国材料与试验协会(US-ASTM);
发布日期
-
实施日期
-
废止日期
-
CCS分类
-
ICS分类
75.100 石油及相关技术 - 润滑剂、工业油及相关产品

研制信息

起草单位
- 展开▼
起草人
-
归口单位
D02.03

摘要

1.1 This practice covers a high-pressure, high-temperature digestion technique using the high-pressure asher (HPA) for preparation of oils and oily waste specimens for determination of up to 28 different elements by inductively coupled plasma-atomic emission plasma spectroscopy (ICP-AES), cold-vapor atomic absorption spectroscopy (CVAAS), and graphite furnace atomic absorption spectroscopy (GFAAS), inductively coupled plasma-mass spectrometry (ICPMS), and radiochemical methods. Oily and high-percentage organic waste streams from nuclear and non-nuclear manufacturing processes can be successfully prepared for trace element determinations by ICP-AES, CVAAS, and GFAAS. This practice is applicable to the determination of total trace elements in these mixed wastes. Specimens prepared by this practice can be used to characterize organic mixed waste streams received by hazardous waste treatment incinerators and for total element characterization of the waste streams.1.2 This practice is applicable only to organic waste streams that contain radioactivity levels that do not require special personnel or environmental protection from radioactivity or other acute hazards.1.3 A list of elements determined in oily waste streams is found in Table 1.1.4 This practice has been used successfully to completely digest a large variety of oils and oily mixed waste streams from nuclear processing facilities. While the practice has been used to report data on up to 28 trace elements, its success should not be expected for all analytes in every specimen. The overall nature of these oily wastes tends to be heterogeneous that can affect the results. Homogeneity of the prepared sample is critical to the precision and quality of the results.1.5 This practice is designed to be applicable to samples whose preparation practices are not defined, or not suitable, by other regulatory procedures or requirements, such as the U.S. Environmental Protection Agency (EPA) SW-846 and EPA-600/4-79-020 documents. This digestion practice is designed to provide a high level of accuracy and precision, but does not replace or override any regulatory requirements for sample preparation.1.6 This practice uses hazardous materials, operations, and equipment at high pressure (90–110 bars, 89–108 atm, or 1305–1595 lb/in.2) and high temperatures, up to 320°C, and therefore poses significant hazards if not operated properly.1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.7.1Exception—Pressure measurements are given in lb/in. units.1.8This 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.Specific warning statements are given in Sections 10.TABLE 1 List of Elements and Applicable Lower Concentration RangesElementLower ReportableLimit,Aμg/gAnalysis MethodAluminum3.3ICP-AESAntimony8.3ICP-AES or GFAASArsenic8.3ICP-AES or GFAASBarium0.17ICP-AESBeryllium0.05ICP-AESBoron0.67ICP-AESCadmium0.50ICP-AES or GFAASCalcium0.67ICP-AESChromium1.7ICP-AESCobalt0.83ICP-AESCopper0.67ICP-AESIron0.67ICP-AESLead8.3ICP-AES or GFAASLithium0.67ICP-AESMagnesium0.08ICP-AESManganese0.17ICP-AESMercury0.03CVAASNickel1.7ICP-AESPotassium100ICP-AESSelenium8.3ICP-AES or GFAASSilver1.0ICP-AESSodium3.3ICP-AESStrontium0.07ICP-AESThallium1.7GFAASTitanium0.50ICP-AESVanadium0.83ICP-AESZinc0.17ICP-AESZirconium0.83ICP-AESALower reportable limits are based on a 0.3-g sample diluted to a final volume of 50 mL. These limits should only be used as a guide. Actual values are instrument and sample dependent. ====== Significance And Use ======This practice is useful for preparation of difficult-to-digest, primarily oils and oily wastes, specimens for trace element determinations of up to 28 elements by atomic absorption or plasma emission techniques. Specimen preparation by high-pressure ashing is primarily applicable to specimens whose preparation by EPA SW-846 protocols is either not applicable or not defined. This sample preparation practice is applicable for the trace element characterization of mixed oily wastes for use by waste treatment facilities such as incinerators or waste stabilization facilities. 1.1本规程涵盖了使用高压灰化炉(HPA)制备油和含油废物样品的高压高温消解技术,用于通过电感耦合等离子体原子发射光谱法(ICP-AES)、冷蒸汽原子吸收光谱法(CVAAS)测定多达28种不同元素,石墨炉原子吸收光谱法(GFAAS)、电感耦合等离子体质谱法(ICPMS)和放射化学方法。核和非核制造过程中产生的含油和高百分比有机废物流可成功制备,用于ICP-AES、CVAAS和GFAAS测定微量元素。本规程适用于这些混合废物中总微量元素的测定。通过本规程制备的样本可用于表征危险废物处理焚烧炉接收的有机混合废物流,并用于表征废物流的总元素特征。1.2本规程仅适用于放射性水平不需要特殊人员或环境保护以防止放射性或其他急性危害的有机废物流。1.3表1列出了含油废物流中测定的元素。1.4本规程已成功用于完全消化核处理设施中的各种油和含油混合废物流。虽然该实践已用于报告多达28种微量元素的数据,但不应期望其成功用于每个样本中的所有分析物。这些含油废物的整体性质往往是不均匀的,这可能会影响结果。制备样品的均匀性对结果的精度和质量至关重要。1.5本规程旨在适用于其他监管程序或要求(如美国环境保护局(EPA)SW-846和EPA-600/4-79-020文件)未定义或不适用制备规程的样品。本消解实践旨在提供高水平的准确度和精密度,但不会取代或超越任何样品制备的监管要求。1.6本规程使用高压(90–110巴,89巴–108 atm或1305–1595磅/英寸。2.)高温高达320°C、 因此,如果操作不当,会造成重大危险。1.7以国际单位制表示的数值应视为标准值。本标准不包括其他计量单位。1.7.1例外—压力测量值以磅/英寸为单位。单位。1.8本标准并非旨在解决与其使用相关的所有安全问题(如有)。本标准的用户有责任在使用前制定适当的安全和健康实践,并确定监管限制的适用性。第10节给出了具体的警告声明。表1元素清单和适用的较低浓度范围要素较低的可报告限度A.μ克/克分析方法铝3.3ICP-AES锑8.3ICP-AES或GFAAS砷8.3ICP-AES或GFAAS钡0.17ICP-AES铍0.05国际比较项目-AES公司硼0.67ICP-AES镉0.50ICP-AES或GFAAS钙0.67ICP-AES铬1.7ICP-AES钴0.83ICP-AES铜0.67ICP-AES铁0.67ICP-AES领导8.3ICP-AES或GFAAS锂0.67ICP-AES镁0.08ICP-AES锰0.17ICP-AES水星0.03CVAAS镍1.7ICP-AES钾100ICP-AES硒8.3ICP-AES或GFAAS银1ICP-AES钠3.3ICP-AES锶0.07ICP-AES铊1.7石墨炉原子吸收光谱法钛0.50ICP-AES钒0.83ICP-AES锌0.17ICP-AES锆0.83ICP-AESA.较低的报告限值基于稀释至最终体积为50 mL的0.3 g样品。这些限值仅供参考。实际值取决于仪器和样品。====意义和用途======本规程适用于通过原子吸收或等离子体发射技术制备难消化(主要是油和含油废物)的样品,以测定多达28种元素。通过高压制备试样-压力灰化主要适用于EPA SW-846协议制备不适用或未定义的样本。本样品制备规程适用于废物处理设施(如焚烧炉或废物稳定设施)使用的混合含油废物的微量元素表征。 展开▼

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