Poster Dianne L, Schantz Michele M, Leigh Stefan D, Wise Stephen A
National Institute of Standards and Technology, Gaithersburg, MD 20899-0001, USA.
J Res Natl Inst Stand Technol. 2004 Apr 1;109(2):245-66. doi: 10.6028/jres.109.016. Print 2004 Mar-Apr.
Six Standard Reference Materials (SRMs®) have been prepared by the National Institute of Standards and Technology (NIST) for the determination of PCBs as different Aroclor mixtures in methanol. Six additional SRMs of the same Aroclors in transformer oil have also been prepared. Specifically, solutions of Aroclors 1016, 1232, 1242, 1254, and 1260 have been gravimetrically prepared (individually) in methanol and transformer oil, mixed, and transferred to amber glass ampoules in approximately 1.2 mL aliquots. Gas chromatography with electron capture detection (GC-ECD) has been used to verify the gravimetric data for each solution and transformer oil SRM. Liquid chromatography was used for the isolation of the Aroclors from the transformer oil SRMs prior to GC-ECD analysis. Separate calibration solutions and oils were prepared with Aroclor levels similar to those in each methanol solution and transformer oil SRM and were processed alongside the samples. The GC-ECD response of each Aroclor was monitored relative to internal standards that were added to the complex mixtures for quantification. The gravimetric concentrations of Aroclors 1242 and 1254 in methanol were also examined by the same method of analysis (GC-ECD) using several different sources of Aroclors and two different capillary GC columns: a 5 % phenyl methylpolysiloxane phase and a relatively non-polar phase. The preparation of the materials, the gas chromatographic results, and the certified concentration values for each Aroclor SRM are described in this paper.
美国国家标准与技术研究院(NIST)制备了六种标准参考物质(SRMs®),用于测定甲醇中不同艾氏剂混合物形式的多氯联苯。还制备了六种同样艾氏剂含量的变压器油标准参考物质。具体而言,已通过重量法(分别)在甲醇和变压器油中制备了艾氏剂1016、1232、1242、1254和1260的溶液,混合后以约1.2 mL的等分试样转移至琥珀色玻璃安瓿中。已使用带有电子捕获检测的气相色谱法(GC-ECD)来验证每种溶液和变压器油标准参考物质的重量数据。在进行GC-ECD分析之前,使用液相色谱法从变压器油标准参考物质中分离出艾氏剂。制备了与每种甲醇溶液和变压器油标准参考物质中艾氏剂含量相似的单独校准溶液和油,并与样品一起进行处理。相对于添加到复杂混合物中用于定量的内标,监测每种艾氏剂的GC-ECD响应。还使用几种不同来源的艾氏剂和两根不同的毛细管GC柱:5%苯基甲基聚硅氧烷固定相和相对非极性固定相,通过相同的分析方法(GC-ECD)检查了甲醇中艾氏剂1242和1254的重量浓度。本文描述了这些物质的制备、气相色谱结果以及每种艾氏剂标准参考物质的认证浓度值。