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The applicability of a large-volume injection (LVI) system for quantitative analysis of permanent gases O-2 and N-2 using a gas chromatograph/barrier discharge ionization detector

机译:大体积进样(LVI)系统用于使用气相色谱仪/势垒放电电离检测器定量分析O-2和N-2永久性气体的适用性

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摘要

To develop accurate quantitation methods for two major permanent gases, N-2 and O-2, a series of calibration experiments were carried out using a gas chromatograph (GC)/barrier discharge ionization detector (BID) equipped with a large-volume injection (LVI) system. To this end, gaseous working standards (WSs) diluted with helium gas were prepared at ten different concentration levels representing three different concentration ranges (in ppm) in 1-L polyester aluminum (PEA) bags ((1) low, 209 similar to 2090 (O-2) and 791 similar to 7910 (N-2); (2) moderate, 2090 similar to 20,900 (O-2) and 7910 similar to 79,100 (N-2); and (3) high, 20,900 similar to 209,000 (O-2) and 79,100 similar to 791,000 (N-2)). Cross-calibration experiments for each individual WS were carried out using the loop injection system with four different capacities (0.01, 0.5, 1, and 10 mL). The calibration results were then evaluatedwith respect to key variables including loop capacity, concentration, and mass quantity. Accordingly, we observed the optimal performance of the BID in terms of sensitivity and linearity (R-2 > 0.98) when the WS of the moderate concentration range was analyzed with the small loop (0.01 and 0.5 mL). The method detection limit (MDL) values of the four loop sizes (between 0.01 and 10 mL) were 7 similar to 500 ng for O-2 (38.4 similar to 557 ppm) and 24 similar to 2230 ng for N-2 (195 similar to 2105 ppm).
机译:为了开发两种主要永久性气体N-2和O-2的准确定量方法,使用配备了大体积进样器的气相色谱(GC)/势垒放电电离检测器(BID)进行了一系列校准实验( LVI)系统。为此,在1-L聚酯铝(PEA)袋中制备了用十种不同浓度水平表示三种不同浓度范围(ppm)的用氦气稀释的气态工作标准液(WSs)((1)低,类似于2090年的209) (O-2)和791类似于7910(N-2);(2)中等,2090类似于20,900(O-2),7910类似于79,100(N-2);以及(3)高,类似于20,900 209,000(O-2)和79,100,类似于791,000(N-2))。使用具有四种不同容量(0.01、0.5、1和10 mL)的定量环进样系统,对每个单独的WS进行了交叉校准实验。然后针对关键变量评估校准结果,这些关键变量包括定量环容量,浓度和质量。因此,当使用小定量环(0.01和0.5 mL)分析中等浓度范围的WS时,我们观察到了BID在灵敏度和线性(R-2> 0.98)方面的最佳性能。四个定量环大小(在0.01和10 mL之间)的方法检测限(MDL)值对于O-2为7类似于500 ng(38.4与557 ppm类似),对于N-2为24类似于2230 ng(与195 ppm类似)至2105 ppm)。

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