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现行 ASTM D4059-00(2018)
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Standard Test Method for Analysis of Polychlorinated Biphenyls in Insulating Liquids by Gas Chromatography 用气相色谱法分析绝缘液体中多氯联苯的标准试验方法
发布日期: 2018-12-01
1.1 本试验方法描述了通过气相色谱法定量测定电绝缘液体中多氯联苯(PCB)的浓度。它也适用于测定被称为askarels的混合物中的PCB,用作电绝缘液体。 1.2 PCB混合物称为Aroclors 2. 在含有美国制造的askarels的PCB配方中使用。本试验方法可用于测定被单独Aroclors或Aroclors混合物污染的绝缘液体中的多氯联苯。该技术可能不适用于测定其他污染源的多氯联苯。 1.3 本试验方法的精度和偏差仅适用于电绝缘矿物油和硅酮中的PCB浓度。 尚未证明该试验方法适用于所有绝缘液。一些绝缘液体,如卤代烃,会干扰多氯联苯的检测,如果不进行预处理,则无法进行测试。 1.4 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。 1.5 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、健康和环境实践,并确定监管限制的适用性。 1.6 本国际标准是根据世界贸易组织技术性贸易壁垒(TBT)委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认标准化原则制定的。 ====意义和用途====== 5.1 美国政府法规要求通过特定程序处理和处置含有PCB的电气设备和电气绝缘液。用于特定设备或绝缘液量的程序由液体的PCB含量决定。该分析技术的结果可用于选择适当的处理和处置程序。 5.2 该技术中的量化需要将未知样本的色谱图与在相同条件下获得的标准Aroclor试样的色谱图进行逐峰比较。应独立知道标准色谱图中产生每个峰的PCB数量。 5.3 所述技术基于使用特定色谱柱填充材料和操作条件获得的Aroclors 1242、1254和1260的标准色谱图数据。 4. 相关色谱图复制于 图1 , 图2 和 图3 5. ,对于等温填充柱和图。X4.1至X4.3)。每个峰通过其相对于标准品的保留时间来确定。与每个峰相关的印刷电路板的类型和数量已通过质谱测定,并在中给出 表1 , 表2 和 表3 . 4. 其他色谱操作条件,尤其是其他柱填料,可能会产生不同的分离。 如果标准品的色谱图与图中所示的色谱图存在显著差异,则不应使用表中给出的数据。此类标准色谱图中的峰应独立识别和量化。 (A) 相对于的保留时间 p , p '-DDE = 100.从溶剂首次出现时开始测量。 (B) 六个结果的标准差占结果平均值的百分比( 碳化硅 变异系数)。 (C) 来自GC-MS数据。包含不同氯数异构体混合物的峰用括号括起来。 (A) 相对于的保留时间 p , p '-DDE = 100.从溶剂首次出现时开始测量。 (B) 六个结果的标准偏差占结果平均值的百分比( 碳化硅 变异系数)。 (C) 来自GC-MS数据。包含异构体混合物的峰用括号括起来。 (A) 相对于的保留时间 p , p '-DDE = 100.从溶剂首次出现时开始测量。量化为一个峰的重叠峰用括号括起来。 (B) 六个结果的标准差作为结果的平均值( 碳化硅 变异系数)。 (C) 来自GC-MS数据。包含不同氯数异构体混合物的峰用括号括起来。 D 在峰104的中心测定成分。 E 在峰232的中心测定成分。 5.4 具有相同数量氯取代基的PCB的不同异构体可能会引起EC检测器的显著不同响应。含有等量PCB但异构体比例不同的PCB混合物可以产生完全不同的色谱图。 只有当标准PCB混合物和未知试样中发现的PCB混合物密切相关时,该技术才有效。Aroclors 1242、1254和1260是足够的标准,因为它们是电绝缘油中最常见的PCB污染物。
1.1 This test method describes a quantitative determination of the concentration of polychlorinated biphenyls (PCBs) in electrical insulating liquids by gas chromatography. It also applies to the determination of PCB present in mixtures known as askarels, used as electrical insulating liquids. 1.2 The PCB mixtures known as Aroclors 2 were used in the formulation of the PCB-containing askarels manufactured in the United States. This test method may be applied to the determination of PCBs in insulating liquids contaminated by either individual Aroclors or mixtures of Aroclors. This technique may not be applicable to the determination of PCBs from other sources of contamination. 1.3 The precision and bias of this test method have been established only for PCB concentrations in electrical insulating mineral oils and silicones. The use of this test method has not been demonstrated for all insulating fluids. Some insulating liquids, such as halogenated hydrocarbons, interfere with the detection of PCBs and cannot be tested without pretreatment. 1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included 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 responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 5.1 United States governmental regulations mandate that electrical apparatus and electrical insulating fluids containing PCB be handled and disposed of through specific procedures. The procedure to be used for a particular apparatus or quantity of insulating fluid is determined by the PCB content of the fluid. The results of this analytical technique can be useful in selecting the appropriate handling and disposal procedure. 5.2 Quantification in this technique requires a peak-by-peak comparison of the chromatogram of an unknown specimen with that of standard Aroclor test specimens obtained under identical conditions. The amount of PCB producing each peak in the standard chromatogram shall be known independently. 5.3 The technique described is based on data for standard chromatograms of Aroclors 1242, 1254, and 1260 obtained using specific chromatographic column packing materials and operating conditions. 4 Relevant chromatograms are reproduced in Fig. 1 , Fig. 2 , and Fig. 3 5 , for isothermal packed columns and in Figs. X4.1 through X4.3) for temperature programmed mega-bore capillary columns. Each peak is identified by its retention time relative to that of a standard. The types and amounts of PCB associated with each peak have been determined by mass spectroscopy and are given in Table 1 , Table 2 , and Table 3 . 4 Other chromatographic operating conditions, and in particular, other column packing materials, may give different separations. The data given in the tables should not be used if chromatograms of the standards differ significantly from those shown in the figures. The peaks in such standard chromatograms shall be independently identified and quantified. 5.4 Different isomers of PCB with the same number of chlorine substituents can cause substantially different responses from EC detectors. Mixtures of PCB containing the same amount of PCB, but with a different ratio of isomers, can give quite different chromatograms. This technique is effective only when the standard PCB mixtures and those found in the unknown test specimen are closely related. Aroclors 1242, 1254, and 1260 are adequate standards because they have been found to be the most common PCB contaminant in electrical insulating oils.
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归口单位: D27.03
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