磷酸-乙酸体系中乙酸含量的气相色谱分析方法

doi:10.19964/j.issn.1006-4990.2022-0440

Abstract

Abstract:

A method using gas chromatography with propionic acid as an internal standard was proposed to solve the problems of low accuracy and cumbersome operation in the analysis of acetic acid content in the phosphoric acid and acetic acid mixed system.The accuracy and applicability of this method were verified through recovery experiments，precision experiments，comparison tests with literature methods，and experiments on the interference of phosphoric acid concentration.The experimental results showed that the recoveries of blank standard of acetic acid was 97.67%~104.55%，and the recoveries of sample standard of acetic acid was 97.72%~104.35%，and the precision of multiple test results was 1.26%.Compared with the literature methods，this method had high accuracy.In addition，for phosphoric acid concentrations at the range of 0~70%，the analytical results of acetic acid were not affected by the phosphoric acid content.Therefore，this chromatographic analysis method could accurately，rapidly，and easily determine the content of acetic acid in the phosphoric acid and acetic acid mixed system.This method was of great importance for the analysis of acetic acid content in related industries.

Key words: phosphoric acid, acetic acid, propionic acid, gas chromatography, internal standard method

CLC Number:

TQ115

LI Jiaqiang, LI Jun, JIN Yang, CHEN Ming. A gas chromatographic analysis method for acetic acid content in phosphoric acid and acetic acid mixed system[J]. Inorganic Chemicals Industry, 2023, 55(5): 115-120.

Figures/Tables 9

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序号	加标量/ （mg·L^-1）	测量值/ （mg·L^-1）	加标回收率/%
1	415.00	405.34	97.67
2	689.00	687.27	99.75
3	1 083.00	1 081.93	99.90
4	1 260.00	1 317.33	104.55
5	1 519.00	1 574.18	103.63

序号	样品加入量/ （mg·L^-1）	加标量/ （mg·L^-1）	加标试样测定值/（mg·L^-1）	样品加标回收率/%
1	253.82	273.00	520.59	97.72
2	264.41	427.00	683.37	98.12
3	264.82	582.00	872.10	104.35
4	256.96	1 049.00	1 338.36	103.09
5	255.79	1 290.00	1 577.43	102.45

序号	乙酸质量分数/%		误差/ %	相对偏差/ %
序号	色谱法	间接法	误差/ %	相对偏差/ %
1	6.01	5.97	0.04	0.67
2	4.73	4.71	0.02	0.42
3	4.00	3.92	0.08	2.04
4	3.17	3.08	0.09	2.92
5	2.29	2.22	0.07	3.15

m（磷酸）/ m（乙酸）	乙酸质量分数/%	m（磷酸）/ m（乙酸）	乙酸质量分数/%
0	0.94	400	0.87
100	0.93	500	0.88
200	0.88	600	0.86
300	0.89

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A gas chromatographic analysis method for acetic acid content in phosphoric acid and acetic acid mixed system

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