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Gas chromatography-mass spectrometry detection method for simultaneously detecting tetrachlorobenzene and pentachlorobenzene in chlorothalonil

A gas chromatography and mass spectrometry detection technology, which is applied in the field of gas chromatography-mass spectrometry detection methods for simultaneous detection of tetrachlorobenzene and pentachlorobenzene in chlorothalonil, can solve the problems such as no simultaneous detection of tetrachlorobenzene and pentachlorobenzene, and achieves the The effect of good linear correlation, good linear relationship and high sensitivity

Pending Publication Date: 2022-02-01
JIANGSU XINHE AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Based on the above studies, there is currently no method for the simultaneous detection of tetrachlorobenzene and pentachlorobenzene in chlorothalonil

Method used

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  • Gas chromatography-mass spectrometry detection method for simultaneously detecting tetrachlorobenzene and pentachlorobenzene in chlorothalonil
  • Gas chromatography-mass spectrometry detection method for simultaneously detecting tetrachlorobenzene and pentachlorobenzene in chlorothalonil
  • Gas chromatography-mass spectrometry detection method for simultaneously detecting tetrachlorobenzene and pentachlorobenzene in chlorothalonil

Examples

Experimental program
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preparation example Construction

[0107] Preparation of standard working solution: Accurately weigh 0.01g (accurate to 0.0001g) 1,2,3,5-tetrachlorobenzene standard sample, 1,2,4,5-tetrachlorobenzene standard sample, 1,2,3 , 4-tetrachlorobenzene standard sample and pentachlorobenzene standard sample were placed in four 100mL volumetric flasks respectively, and an appropriate amount of toluene was added for ultrasonic dissolution. Single-standard stock solution; use a pipette to take 2.5mL of each of the above-mentioned single-standard stock solutions in a 50mL volumetric flask, dilute to the mark with toluene, and shake well to make an intermediate dilution of 5.0μg / mL; Take out 2mL, 1mL, and 0.5mL of the above-mentioned mixed intermediate dilution, place them in three 100mL volumetric flasks, dilute to the mark with toluene, shake well, and prepare 0.1μg / mL (C1), 0.05μg / mL (C2), 0.025μg / mL (C3) series of standard working solutions, spare.

[0108] Preparation of the sample solution to be tested: Weigh 0.2g (a...

Embodiment 1

[0110] This embodiment provides a gas chromatography-mass spectrometry detection method for simultaneous detection of tetrachlorobenzene and pentachlorobenzene in chlorothalonil, wherein the gas chromatography conditions are set as follows: the temperature of the chromatographic column is programmed, and the temperature is kept at 70 ° C for 0.5 min. The temperature was raised to 125°C at ℃ / min and kept for 3 minutes, then raised at 40°C / min to the final column temperature of 300°C and kept for 2 minutes; the carrier gas was helium with a purity of ≥99.999%, and the flow rate was 1.0mL / min. The temperature of the injection port is 280°C; the injection volume is 1.0 μL; the injection method is pulse splitless injection, and the pulse pressure is 68kPa; the mass spectrometry conditions are set as follows: the ionization method is electron impact ionization (EI), the ionization energy is 70eV, GC-MSD The interface temperature is 300°C; the ion source temperature is 230°C; the quad...

Embodiment 2

[0116] This example provides a gas chromatography-mass spectrometry detection method for simultaneous detection of tetrachlorobenzene and pentachlorobenzene in chlorothalonil, in which, except that the initial temperature of the chromatographic column is kept at 60°C for 0.5min, other parameter settings, operations and implementation Example 1 is the same.

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Abstract

The invention provides a gas chromatography-mass spectrometry detection method for simultaneously detecting tetrachlorobenzene and pentachlorobenzene in chlorothalonil. The method comprises the steps that a standard working solution and a to-be-detected sample solution are prepared, the standard working solution contains tetrachlorobenzene and pentachlorobenzene standard samples, and tetrachlorobenzene comprises any one or a combination of at least two of 1, 2, 3, 5-tetrachlorobenzene, 1, 2, 4, 5-tetrachlorobenzene and 1, 2, 3, 4-tetrachlorobenzene; the to-be-detected sample solution contains a chlorothalonil sample; the standard working solution and the to-be-detected sample solution are separated and detected by adopting gas chromatography and mass spectrometry; and a standard curve is made according to a detection result, and the content of tetrachlorobenzene and pentachlorobenzene in the to-be-detected sample is calcualted. The method can be used to obtain stable detector response, can realize effective separation and detection of tetrachlorobenzene and pentachlorobenzene in chlorothalonil, and has high selectivity, sensitivity, repeatability and accuracy for detection of tetrachlorobenzene and pentachlorobenzene in chlorothalonil.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a gas chromatography-mass spectrometry detection method for simultaneously detecting tetrachlorobenzene and pentachlorobenzene in chlorothalonil, in particular to a simultaneous detection of chlorobenzene with good selectivity, high sensitivity and high accuracy. Gas chromatography-mass spectrometry detection of tetrachlorobenzene and pentachlorobenzene in bacteria serum. Background technique [0002] Chlorothalonil, whose chemical name is tetrachloroisophthalonitrile, is a broad-spectrum and protective fungicide with high efficiency and low toxicity. Prevention and treatment. Chlorothalonil technical will produce tetrachlorobenzene and pentachlorobenzene as impurities during the chlorination synthesis process. As chlorobenzene compounds, tetrachlorobenzene and pentachlorobenzene are one of the most common environmental pollutants in the world. They are highly toxic and pote...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/72G01N30/8679
Inventor 孙丽王冠辉谢雨杉丁娟王晴
Owner JIANGSU XINHE AGROCHEM
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