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Lowering MDLs for Analysis of Drinking Water for USEPA Method 525.2 美国环保局方法525.2降低饮用水分析MDL
发布日期: 2007-11-01
这项研究的目的是观察是否可以通过选择特定的样本来提高分析的整体性能 仪器耗材,包括浪涌压力无分流注入,以降低 美国环境保护局(USEPA)方法525.2的检测限(MDL)。美国环境保护署 (美国环保局)方法525.2是一种通用方法,用于分析成品饮料中的有机化合物 水、水源水或任何处理阶段的饮用水。用固相法制备一升样品 提取,在乙酸乙酯中生成最终提取物。所有校准标准均采用乙酸乙酯制成,以避免 在与提取物不同的溶剂中进行校准时产生的任何不良影响。注射法 在1µL的进样量下,浪涌压力不可分离。质谱仪设置为EI全扫描 从45米到450米。对色谱柱进行编程,使其在25分钟内洗脱所有化合物。这个 校准曲线在以下浓度下运行:0.1,0.5,1,2,5和10µg/mL。重复 MDL以0.5微克/毫升的浓度运行。使用的仪器系统是DSQ II、痕量GC Ultra和AS 3000 自动取样器。 在对各种入口衬管和柱相进行初步评估后,首选衬管(5 mm无分流衬管)和 选择柱(TR 525 0.25 mm x 30 m,0.25µm)进行研究。班轮的选择是基于 产生最低的异狄氏体分解。选择的柱相在室温下表现出最好的线性 浓度低于0.50µg/mL,表明不可逆吸附最小。优选衬管和柱的研究 显示出极好的灵敏度,并且在每次运行中都很容易满足DFTPP的调整标准。校准曲线 通过平均相对标准偏差百分比和最小平方拟合满足线性拟合的所有QC标准 方法中列出了一些有问题的化合物。为了说明该系统的性能 本研究中测试的质量控制标准方法讨论如下:临界时间影响GC/MS性能; 符合校准曲线标准;和 MDL或仪器检测限(IDL)的测定。
The objective of this study was to see if the overall performance of the analysis could be improved by selecting specific consumables for the instrument and incorporating a surge pressure splitless injection to lower the Detection Limits (MDLs) for U.S. Environmental Protection Agency (USEPA) Method 525.2. U.S. Environmental Protection Agency (USEPA) Method 525.2 is a general purpose method for the analysis of organic compounds in finished drinking water, source water, or drinking water in any stage of treatment. A one liter sample is prepared by solid phase extraction, generating a final extract in ethyl acetate. All calibration standards are made in ethyl acetate to avoid any adverse effects caused by calibration in a different solvent from that of the extracts. The injection method was surge pressure splitless at an injection volume of 1 µL. The mass spectrometer was set up for EI full scan from m/z 45 to 450. The column was programmed to elute all compounds in less than 25 minutes. The calibration curve was run at the following concentrations: 0.1, 0.5, 1, 2, 5, and 10 µg/mL. The replicates for MDLs were run at 0.5 µg/mL. The instrument system used was the DSQ II, TRACE GC Ultra, and AS 3000 autosampler. After an initial evaluation of various inlet liners and column phases, the preferred liner (5 mm Splitless liner) and column (TR 525 0.25 mm x 30 meter, 0.25 µm) were selected for the study. The liner was selected based on producing the lowest endrin breakdown. The column phase was selected which showed the best linearity at levels below 0.50 µg/mL, indicating minimal irreversible adsorption. The study of the preferred liner and column showed excellent sensitivity and met the tuning criteria for DFTPP easily from run to run. The calibration curve met all of the QC criteria for a linear fit by average percent relative standard deviation and by least square fit for a few of the problem compounds listed in the method. In order to illustrate the performance of the system, the Quality Control criteria method tested in this study is discussed as follows: Critical Time affects GC/MS Performance; Meeting the Calibration Curve Criteria; and, Determination of MDLs or Instrument Detection Limits (IDLs).
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发布单位或类别: 美国-美国给水工程协会
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