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高灵敏度和高选择性催化测定甲醛和乙醛。

Highly sensitive and selective catalytic determination of formaldehyde and acetaldehyde.

作者信息

Mohamed Ashraf A, Mubarak Ahmed T, Marestani Zakaria M H, Fawy Khaled F

机构信息

Department of Chemistry, Faculty of Science, King Khalid University, Abha 9033, Saudi Arabia.

出版信息

Talanta. 2008 Jan 15;74(4):578-85. doi: 10.1016/j.talanta.2007.06.020. Epub 2007 Jun 22.

Abstract

A highly sensitive, simple and selective kinetic method was developed for the determination of ultra-trace levels of formaldehyde and acetaldehyde based on their catalytic effect on the oxidation of N,N-diethyl-p-phenylenediamine (DPD) with hydrogen peroxide. The reaction was monitored spectrophotometrically by tracing the formation of the red-colored oxidized product of DPD at 510nm, within 30s of mixing the reagents. The optimum reaction conditions were: 20mmolL(-1) DPD, 250mmolL(-1) H(2)O(2), 150mmolL(-1) phosphate, 150mmolL(-1) citrate and pH 6.60+/-0.05 at 25 degrees C. Following the recommended procedure, formaldehyde and acetaldehyde could be determined with linear calibration graphs up to 0.50 and 1.4microg mL(-1) and detection limits, based on the 3S(b)-criterion, of 0.015 and 0.035microg mL(-1), respectively. In addition, analytical data for other 10 aldehydes were also presented. The high sensitivity and selectivity of the proposed method allowed its successful application to rain water, mainstream smoke (MSS) and disposed tips of smoked cigarettes (DTSC). A sample aliquot was directly analyzed for its total water-soluble aldehyde content. A second sample aliquot was heated at 80 degrees C for 10min to expel acetaldehyde and the aliquot was analyzed for its content of other water-soluble aldehydes (expressed as formaldehyde equivalent), and acetaldehyde was determined by difference. The analytical results were in excellent agreements with those obtained following the standard HPLC method based on pre-column derivatization with 2,4-dinitrophenylhydrazine. Moreover, published catalytic-spectrophotometric methods for the determination of aldehydes were reviewed.

摘要

基于甲醛和乙醛对N,N-二乙基对苯二胺(DPD)与过氧化氢氧化反应的催化作用,开发了一种高灵敏度、简单且选择性好的动力学方法,用于测定超痕量水平的甲醛和乙醛。通过在试剂混合后30秒内,在510nm处追踪DPD红色氧化产物的形成,用分光光度法监测反应。最佳反应条件为:20mmolL(-1) DPD、250mmolL(-1) H(2)O(2)、150mmolL(-1) 磷酸盐、150mmolL(-1) 柠檬酸盐,25℃时pH为6.60±0.05。按照推荐程序,甲醛和乙醛的线性校准曲线可达0.50和1.4μg mL(-1),基于3S(b)标准的检测限分别为0.015和0.035μg mL(-1)。此外,还给出了其他10种醛的分析数据。该方法的高灵敏度和选择性使其成功应用于雨水、主流烟气(MSS)和烟蒂(DTSC)。取一份样品等分试样直接分析其总水溶性醛含量。取另一份样品等分试样在80℃加热10分钟以驱除乙醛,然后分析该等分试样中其他水溶性醛(以甲醛当量表示)的含量,并通过差值确定乙醛含量。分析结果与基于2,4-二硝基苯肼柱前衍生化的标准HPLC方法得到的结果非常吻合。此外,还综述了已发表的用于测定醛的催化分光光度法。

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