Method for separating isomeride chlorobenzene and chlorotoluene by adopting gas chromatography-mass spectrometry

A technology of isomers and chlorinated toluene, applied in the field of chemical analysis and detection

Active Publication Date: 2020-10-20
南京海关工业产品检测中心 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the problem that it is difficult to simultaneously separate multiple isomers of chlorinated benzene and chlorinated toluene compounds in the prior art, the present invention provides a method for separating isomers of chlorinated benzene and chlorinated toluene by gas chromatography-mass spectrometry The method is based on the structural properties of the target compound to select a suitable organic solvent to quickly and efficiently extract chlorinated benzene and chlorinated toluene in dyeing and finishing auxiliaries, and use Agilent DB-23 (30m × 0.250mm × 0.25μm ) polar column to separate chlorinated benzene and chlorinated toluene, effectively separate the isomers, achieve the ideal separation effect, and solve the current problem that the isomers cannot be separated

Method used

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  • Method for separating isomeride chlorobenzene and chlorotoluene by adopting gas chromatography-mass spectrometry
  • Method for separating isomeride chlorobenzene and chlorotoluene by adopting gas chromatography-mass spectrometry
  • Method for separating isomeride chlorobenzene and chlorotoluene by adopting gas chromatography-mass spectrometry

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preparation example Construction

[0050] 3. Preparation of standard solution

[0051] Standard stock solution preparation: Accurately weigh each standard substance (accurate to 0.01 mg), and use n-hexane as solvent to accurately prepare approximately 1000 mg / L stock solution, and store at -18°C in the dark.

[0052] Preparation of standard working solution: use n-hexane to prepare a working solution of appropriate concentration.

[0053] 4. Sample pretreatment

[0054] Take a representative sample, weigh 0.5g (accurate to 0.01g), put it into the reactor, add 5mL saturated NaCl solution, vortex for 30s, then accurately add 5mL acetonitrile and saturated n-hexane for liquid-liquid extraction, shake for 20min , add a small amount of anhydrous sodium sulfate, take a sample through a 0.22 μm polytetrafluoroethylene filter membrane, (if necessary, first centrifuge and then pass through the membrane) gas chromatography-mass spectrometer for sample analysis.

[0055] 5. Instrument Analysis

[0056] Capillary column...

Embodiment 1

[0077] This embodiment is a qualitative analysis experiment aimed at 29 kinds of substances in Table 2.

[0078] This embodiment provides a method for separating isomers of chlorinated benzene and chlorinated toluene by gas chromatography-mass spectrometry, the method comprising the following steps:

[0079] 1) Preparation of standard solutions of 29 kinds of isomers of chlorinated benzene and chlorinated toluene, as in the aforementioned "three, preparation of standard solutions" part;

[0080] 2) Preparation of the sample solution to be tested: prepare a mixed solution containing 29 substances in Table 2 (the concentration of each substance is 5 mg / L);

[0081] 3) Use gas chromatography-mass spectrometry to detect the standard solution in step 1) and draw a standard working curve, wherein the capillary column adopts a DB-23 capillary column; the detection conditions are as described in the "V. Instrument Analysis" section;

[0082] 4) Qualitative and / or quantitative analysi...

Embodiment 2

[0085] Analyzed the linear range and minimum detection limit of chlorinated benzene and chlorinated toluene in the present embodiment (concrete test condition is the same as " five, instrument analysis " part), the linear range of chlorinated benzene and chlorinated toluene is 0.05-5mg / kg, the correlation coefficient can reach more than 0.995, and the detection limit is 0.5 mg / kg, as shown in Table 5.

[0086] Table 5 Linear range, correlation coefficient (r) and limit of quantification (LOQ) of 29 kinds of chlorinated benzene and chlorinated toluene

[0087]

[0088]

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Abstract

The invention discloses a method for separating isomeride chlorobenzene and chlorotoluene by adopting gas chromatography-mass spectrometry, and belongs to the field of chemical analysis and detection.According to the invention, chlorobenzene and chlorotoluene are separated by using the Agilent DB-23 (30 m * 0.250 mm * 0.25 [mu] m) polar column so as to effectively separate the isomeride, such that the ideal separation effect is achieved, and the problem that the isomeride is difficult to separate at present can be solved. The method provided by the invention effectively overcomes the problemof difficult sample extraction, realizes rapid and accurate qualitative and quantitative determination, is suitable for analysis of a large batch of samples, and meets the requirements of daily detection in laboratories.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis and detection, and more specifically relates to a method for separating isomers of chlorinated benzene and chlorinated toluene by gas chromatography-mass spectrometry. Background technique [0002] my country is the main producer and supplier of chlorinated benzene and chlorinated toluene in the world. The terminal derivatives of chlorinated benzene and chlorinated toluene are basically concentrated in the pesticide, pharmaceutical, dye and auxiliary industries, and are a kind of cheap and efficient textiles. Dyeing carrier, adding this kind of carrier in the normal pressure dyeing process of polyester fiber can improve the dyeing effect of polyester fiber. Therefore, this type of compound has a high probability of being present in textile dyeing and finishing auxiliaries. [0003] Chlorinated benzene and chlorinated toluene have strong biological toxicity, which can cause loss of liver ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02
CPCG01N30/02G01N30/06G01N2030/062
Inventor 周佳汤娟董绍伟丁友超钱凯曹立华
Owner 南京海关工业产品检测中心
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