Determination of Hydrogen Cyanide by Gas Chromatography With Post-Column Reaction and Flame Ionization Detection

IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL
Ronda Gras, Jim Luong, Robert A. Shellie
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引用次数: 0

Abstract

A straightforward and practical 15-min gas chromatographic method utilizing flame ionization detection has been developed to measure hydrogen cyanide in various matrices. This new approach features a catalyzed two-stage post-column reaction that significantly enhances the detection and quantification of hydrogen cyanide. Selecting the right separation column is crucial for accurate analysis. Initial tests with porous layer open tubular columns resulted in significant peak tailing, rendering them unsuitable for trace-level analysis. Modified polyethylene glycol stationary phases also exhibited strong peak tailing in addition to producing artifact peaks. In contrast, a polydimethylsiloxane-based column with a very low phase ratio (β = 10) demonstrated excellent analytical performance, including peak symmetry and inertness. The analytical approach achieved a minimum detection limit of 50 parts per billion (ppb, v/v) without preconcentration and a linear range from 0.05 to 200 parts per million (ppm, v/v). At a concentration level of 20 ppm (v/v), the RSD at the 95% confidence level was less than 1% (n = 10), and at a concentration level of 1 ppm (v/v), the RSD at the 95% confidence level was less than 3% (n = 10) under the established conditions. The method's effectiveness has been validated through real-life applications, including analyzing hydrogen cyanide in fruit seeds and the headspace of untreated water samples.

气相色谱-柱后反应-火焰电离法测定氰化氢
开发了一种直接实用的15分钟气相色谱法,利用火焰电离检测来测量各种基质中的氰化氢。这种新方法的特点是催化两阶段柱后反应,显著提高了氰化氢的检测和定量。选择合适的分离柱是准确分析的关键。用多孔层开管柱进行的初步试验产生了显著的峰值尾砂,使其不适合痕量水平分析。改性聚乙二醇固定相除产生伪峰外,还表现出较强的峰尾现象。相比之下,低相比(β = 10)的聚二甲基硅氧烷基色谱柱表现出优异的分析性能,包括峰对称性和惰性。该分析方法在没有预浓缩的情况下达到了50十亿分之一(ppb, v/v)的最低检测限,线性范围为0.05至200百万分之一(ppm, v/v)。在浓度为20 ppm (v/v)时,95%置信水平上的RSD小于1% (n = 10),在浓度为1 ppm (v/v)时,95%置信水平上的RSD小于3% (n = 10)。该方法的有效性已通过实际应用得到验证,包括分析水果种子中的氰化氢和未经处理的水样的顶空。
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来源期刊
Journal of separation science
Journal of separation science 化学-分析化学
CiteScore
6.30
自引率
16.10%
发文量
408
审稿时长
1.8 months
期刊介绍: The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.
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