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Gas chromatography analysis: Method validation and measurement uncertainty evaluation for volume fraction measurements of gases in simulated reformate gas stream

机译:气相色谱分析:模拟重整产品气流中气体体积分数测量的方法验证和测量不确定度评估

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摘要

It is important to understand each analytical system and its limitations when performing any chromatographic measurements. In the present paper, a methodology for method validation and measurement uncertainty evaluation for the measurement of volume fractions of selected gases (CO2, CO, CH4, H2) in simulated reformate gas streams by using gas chromatography was developed. A detailed procedure for in-house method validation based on a simple experimental design and consistent statistics is presented. The analytical protocol allowed us to quantify gases in volume fractions from 2.00 to 100.0 mL/(100 mL) with satisfactory recoveries. We proved that the method was selective for the measurement of gases in simulated reformate gas stream. In addition, a step-by-step illustration of modelling approach for measurement uncertainty evaluation of each component is also provided. Uncertainty arising from repeatability and trueness is relatively low, while the contribution from reproducibility is of higher level for all the analytes tested. The main reason for this is changes in atmospheric pressure that affect gas chromatographic measurements. Solution of this problem could be more frequent calibration of apparatus, yielding to higher costs and more time-consuming process, or by measuring the atmospheric pressure and using it to correct the response of the gas chromatograph for resulting variations in sample size. The obtained results confirm that it is imperative to fully characterize the analytical system before proceeding with an analysis.
机译:执行任何色谱测量时,了解每个分析系统及其局限性很重要。本文开发了一种方法验证和测量不确定度评估的方法,该方法用于通过气相色谱法测量模拟重整气中选定气体(CO2,CO,CH4,H2)的体积分数。提出了基于简单实验设计和一致统计数据的内部方法验证的详细过程。该分析规程使我们能够定量分析体积分数为2.00至100.0 mL /(100 mL)的气体,并具有令人满意的回收率。我们证明该方法对模拟重整产品气流中的气体测量具有选择性。此外,还提供了用于对每个组件进行测量不确定性评估的建模方法的分步说明。由重复性和真实性引起的不确定性相对较低,而对于所有测试的分析物,由再现性引起的不确定性较高。造成这种情况的主要原因是大气压力的变化会影响气相色谱测量。解决该问题的方法可能是更频繁地校准设备,导致更高的成本和更耗时的过程,或者通过测量大气压并将其用于校正气相色谱仪的响应以导致样品大小变化。获得的结果证实,在进行分析之前,必须全面表征分析系统。

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