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GC-MS method for detecting dimethyl sulphate content in industrial waste liquid

A technology of dimethyl sulfate and GC-MS, which is applied in the field of chemical analysis, can solve the problems of instability in contact with water, lack of UV-absorbing functional groups, low content of dimethyl sulfate, etc., and achieve the effect of accurate sensitivity

Inactive Publication Date: 2018-04-27
CHANGZHOU HEQUAN PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the relevant detection reports of dimethyl sulfate focus on air, environment, drugs, surfactants, soil and textiles, etc. The detection methods used include colorimetry, high performance liquid chromatography, gas chromatography, gas chromatography- Mass spectrometry, etc., but each method has certain defects in terms of specificity, sensitivity, method precision and repeatability, method operability and convenience, and cannot provide reliable quantitative analysis results. Establishment of Gas Chromatography-Pristine Detection Method for Dimethyl Sulfate in Industrial Waste Liquid
[0005] The content of dimethyl sulfate in industrial waste liquid is low, unstable in contact with water, and does not have UV-absorbing functional groups. It is extremely challenging to accurately and quantitatively determine the content of dimethyl sulfate in industrial waste liquid

Method used

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  • GC-MS method for detecting dimethyl sulphate content in industrial waste liquid
  • GC-MS method for detecting dimethyl sulphate content in industrial waste liquid
  • GC-MS method for detecting dimethyl sulphate content in industrial waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Instruments and Conditions:

[0033] Gas chromatography mass spectrometry: Agilent 7890B GC, 5977A MS detector

[0034] Chromatographic column: Agilent DB-5MS (30m×0.25mm ID×0.25μm)

[0035] Ion source: Electron ionization source

[0036] Carrier Gas: Helium

[0037] Solvent delay: 4.5min

[0038] Mode: Constant Current

[0039] Flow rate: 0.65ml / min

[0040] Split ratio: 10:1

[0041] Injection volume: 1μL

[0042] Extracted molecular weight: 95 and 96;

[0043] Injection port temperature: 200°C

[0044] The column temperature gradient is as follows:

[0045] Ramp

temperature

hold time

-

50℃

0min

10℃ / min

120℃

2min

30℃ / min

240℃

5min

[0046] Experimental steps:

[0047] Diluent: Acetonitrile.

[0048] Standard dimethyl sulfate solution: Accurately weigh about 50mg of dimethyl sulfate into a 10mL volumetric flask containing 2ml of diluent, add diluent to constant volume and shake well, accurately ...

Embodiment 2

[0052] Instruments and Conditions:

[0053] Gas chromatography mass spectrometry: Agilent 7890B GC, 5977A MS detector

[0054] Chromatographic column: Agilent DB-1 (30m×0.25mm ID×0.25μm)

[0055] Ion source: Electron ionization source

[0056] Carrier Gas: Helium

[0057] Solvent delay: 4.5min

[0058] Mode: Constant Current

[0059] Flow rate: 0.65ml / min

[0060] Split ratio: 10:1

[0061] Injection volume: 1μL

[0062] Extracted molecular weight: 95 and 96;

[0063] Injection port temperature: 200°C

[0064] The column temperature gradient is as follows:

[0065] Ramp

temperature

hold time

-

50℃

0min

10℃ / min

120℃

2min

30℃ / min

240℃

5min

[0066] Experimental steps:

[0067] Diluent: Acetonitrile.

[0068] Standard dimethyl sulfate solution: Accurately weigh about 50mg of dimethyl sulfate into a 10mL volumetric flask containing 2ml of diluent, add diluent to constant volume and shake well, accurately pi...

Embodiment 3

[0071] Example 3: Methodological Validation

[0072] 1. Exclusive experiment

[0073] Get dimethyl sulfate reference substance appropriate amount, according to the method for example 2, prepare standard dimethyl sulfate solution, and this solution adopts gas chromatography mass spectrometry to detect and analyze according to the method for example 2.

[0074] The experimental results show that at the retention time of dimethyl sulfate, there is no interference from the blank; the tailing factor of dimethyl sulfate is 0.93, and the peak shape is good; the separation between dimethyl sulfate and its adjacent peaks is 6.65, which is good. see details Figure 6 .

[0075] 2. Quantitation limit experiment

[0076] Get an appropriate amount of dimethyl sulfate reference substance, according to the method for example 2, prepare standard dimethyl sulfate solution, accurately pipette 5mL of the above-mentioned solution to a 10mL volumetric flask, add diluent to constant volume and s...

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Abstract

The invention discloses a GC-MS method for detecting dimethyl sulphate content in industrial waste liquid. The method comprises the following steps: 1) configuring a standard dimethyl sulphate solution, and configuring a sample solution; 2) employing an ion source as an electron ionization source, employing an Agilent DB-5MS chromatographic column or an Agilent DB-1 chromatographic column, takinghelium as a carrier gas, employing a constant current mode, employing a gradient heating mode for column temperature from 50 DEG C to 240 DEG C; 3) taking a standard dimethyl sulphate solution in thestep 1) and a sample solution for respective sampling, and recording a mass spectrum total ion chromatorgraphy; and 4) according to the concentration of the standard dimethyl sulphate solution, and integration areas of the standard dimethyl sulphate solution and the sample solution, calculating the concentration of dimethyl sulphate in the sample solution. The method employs a GC-MS analysis technology, a sample is subjected to bombardment through an EI ion source, existence of dimethyl sulphate is identified through characteristic ion fragments and then quantification is carried out, and themethod has the advantages of rapidity, accuracy and high sensitivity.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to a method for determining the content of dimethyl sulfate in industrial waste liquid. Background technique [0002] Dimethyl sulfate, the structure is as follows: [0003] [0004] At present, the relevant detection reports of dimethyl sulfate focus on air, environment, drugs, surfactants, soil and textiles, etc. The detection methods used include colorimetry, high performance liquid chromatography, gas chromatography, gas chromatography- Mass spectrometry, etc., but each method has certain defects in terms of specificity, sensitivity, method precision and repeatability, method operability and convenience, and cannot provide reliable quantitative analysis results. Establishment of gas chromatography-pristine detection method for dimethyl sulfate in industrial waste liquid. [0005] The content of dimethyl sulfate in industrial waste liquid is low, unstable in contact with wat...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 张楠朱小红褚乐之鲍华军蒋竞赵初芒
Owner CHANGZHOU HEQUAN PHARMA CO LTD
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