CN108387649A - Detection method that is a kind of while detecting a variety of pernicious gases in workplace - Google Patents

Detection method that is a kind of while detecting a variety of pernicious gases in workplace Download PDF

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Publication number
CN108387649A
CN108387649A CN201711173255.8A CN201711173255A CN108387649A CN 108387649 A CN108387649 A CN 108387649A CN 201711173255 A CN201711173255 A CN 201711173255A CN 108387649 A CN108387649 A CN 108387649A
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China
Prior art keywords
workplace
toluene
acetone
detecting
benzene
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CN201711173255.8A
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Chinese (zh)
Inventor
何文辉
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Guangdong Zhonghui Certification Co Ltd
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Guangdong Zhonghui Certification Co Ltd
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Priority to CN201711173255.8A priority Critical patent/CN108387649A/en
Publication of CN108387649A publication Critical patent/CN108387649A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The present invention relates to a kind of while detecting the detection methods of a variety of pernicious gases in workplace,This method uses the gas chromatography of flame ionization ditector FID,Detect benzene in workplace air simultaneously,Toluene,Acetone,Butanone,Ethyl acetate,The content of butyl acetate,With activated carbon tube collecting work place air,Cord blood is sealed after acquisition,Take the front and back section activated carbon in activated carbon tube,It is respectively put into parsing bottle,It is each that 1mL carbon disulfide is added,Shake 1min,Desorb 30min,Stripping liquid is for measuring using external standard method to benzene in workplace air,Toluene,Acetone,Butanone,Ethyl acetate,Butyl acetate carries out quantitative analysis,The present invention can measure benzene in workplace air simultaneously,Toluene,Acetone,Butanone,Ethyl acetate,Butyl acetate content,Further,Improve the detection efficiency of noxious material in detection workplace air,Save many manpower and materials,And this method has operation simpler,Accuracy is high,The high advantage of detection efficiency.

Description

Detection method that is a kind of while detecting a variety of pernicious gases in workplace
Technical field
The present invention relates to a kind of chemistry in detecting technical field, especially a kind of detect simultaneously a variety of in workplace has The detection method of evil gas.
Background technology
With the industrialized development of society, workplace air pollutes the health for having seriously affected workpeople, so It is particularly important to the detection of noxious material in workplace air, general organic toxic substance be mainly benzene, toluene, acetone, Butanone, ethyl acetate, butyl acetate etc..
The prior art is to organic toxic substance benzene, toluene, acetone, butanone, ethyl acetate, the acetic acid in workplace air The detection of butyl ester is all to be detected respectively, with different GC conditions, the different detector of different input modes into Row detection, be detected respectively it is cumbersome, expend the time it is long, efficiency is low;
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of detection method of pernicious gas in workplace, the detection Method can detect the noxious materials such as benzene in workplace air, toluene, acetone, butanone, ethyl acetate, butyl acetate simultaneously, carry The detection efficiency of noxious material in high workplace air.
The technical scheme is that:Detection method that is a kind of while detecting a variety of pernicious gases in workplace, the party Method uses the gas chromatography of flame ionization ditector FID, while detecting benzene in workplace air, toluene, acetone, fourth The content of ketone, ethyl acetate, butyl acetate, includes the following steps:
S1), with activated carbon tube collecting work place air, Cord blood is sealed after acquisition;
S2 the front and back section activated carbon in activated carbon tube), is taken, is respectively put into parsing bottle, it is each that 1mL carbon disulfide is added, it shakes 1min is shaken, desorbs 30min, stripping liquid is for measuring;
S3), take S2 in step) in stripping liquid, sample introduction is carried out by 1.0 μ L of sample size, under corresponding chromatographiccondition Carry out chromatography;
S4 standard curve), is prepared, according to chromatographic peak as a result, using external standard method to benzene, toluene, third in workplace air Ketone, butanone, ethyl acetate, butyl acetate carry out quantitative analysis.
Further, step S3) in chromatographiccondition be:
Gasify room temperature:230 DEG C,
Fid detector temperature:230 DEG C,
Chromatography column and programmed temperature:50-150 DEG C, 10 DEG C/min.
Column flow:1ml/min;
Hydrogen flowing quantity:40ml/min,
Air mass flow:400ml/min.
Preparing standard curve is specially:Benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate is taken to have card standard respectively In pure material 10.0mg to the 10mL volumetric flasks equipped with carbon disulfide, it is diluted to scale with carbon disulfide, is made into hybrid standard storage Standby liquid, pipettes 0,50,100,500,1000,2000 μ l of standard reserving solution in 10mL volumetric flasks, with carbon disulfide constant volume respectively To scale, be configured to benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate hybrid standard use liquid.
Further, chromatography uses capillary chromatographic column, and the column length of the capillary chromatographic column is 30m, interior diameter 0.25mm, film thickness are 0.25 μm.
Further, fid detector carrier gas is the nitrogen that purity is 99.999%.
Further, the standard curve regression equation in quantitative external standard method is drawn by the way of once fitting.
Beneficial effects of the present invention are:The present invention can measure simultaneously benzene in workplace air, toluene, acetone, butanone, Ethyl acetate, butyl acetate content further improve the detection efficiency of noxious material in detection workplace air, save very More manpower and materials, and this method has the advantages that operation is simpler, accuracy is high, detection efficiency is high.
Specific implementation mode
The specific implementation mode of the present invention is described further below:
Detection method that is a kind of while detecting a variety of pernicious gases in workplace, this method are examined using hydrogen flameionization The gas chromatography of device FID is surveyed, while detecting benzene in workplace air, toluene, acetone, butanone, ethyl acetate, acetic acid fourth The content of ester, includes the following steps:
S1), with activated carbon tube collecting work place air, Cord blood is sealed after acquisition;
S2 the front and back section activated carbon in activated carbon tube), is taken, is respectively put into parsing bottle, it is each that 1mL carbon disulfide is added, it shakes 1min is shaken, desorbs 30min, stripping liquid is for measuring;
S3), take S2 in step) in stripping liquid, sample introduction is carried out by 1.0 μ L of sample size, under following chromatographiccondition Carry out chromatography;
Island crystalline substance GC2010;
Chromatographic column DB-WAX;
Gasify room temperature:230℃;
Fid detector temperature:230℃;
Chromatography column and programmed temperature:50-150 DEG C, 10 DEG C/min;
Column flow:1ml/min;
Hydrogen flowing quantity:40ml/min;
Air mass flow:400ml/min;
S4 standard curve), is prepared, according to chromatographic peak as a result, using external standard method to benzene, toluene, third in workplace air Ketone, butanone, ethyl acetate, butyl acetate carry out quantitative analysis.
Chromatography uses capillary chromatographic column, and the column length of the capillary chromatographic column is 30m, and interior diameter is 0.25mm, film thickness are 0.25 μm.
Detector carrier gas is the nitrogen that purity is 99.999%.
Preparing standard curve is specially:Benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate is taken to have card standard respectively In pure material 10.0mg to the 10mL volumetric flasks equipped with carbon disulfide, it is diluted to scale with carbon disulfide, is made into hybrid standard storage Standby liquid, pipettes 0,50,100,500,1000,2000 μ l of standard reserving solution in 10mL volumetric flasks, with carbon disulfide constant volume respectively To scale, the hybrid standard of benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate is configured to using liquid, is grasped by above-mentioned chromatography It is measured as condition, is mapped to peak area A with mass concentration c (mg/L), calculate its regression equation, repeat aforesaid operations 3 times, It the results are shown in Table 1 and table 2;
1 each standard substance of table is repeated 3 times corresponding peak area
2 standard curve stability of table
Benzene, toluene, acetone, butanone, ethyl acetate, 5 μ g/mL standard solution of butyl acetate are pressed into above-mentioned operation condition of chromatogram It is measured, according to three times signal-to-noise ratio computation benzene, the detection limit of toluene, acetone, butanone, ethyl acetate, butyl acetate, measures knot Fruit is shown in Table 3;
3 detection limit of table
Standard deviation (method precision) is tested:Containing benzene, toluene, acetone, butanone, second from electrical apparatus factory's workplace air 6 acetoacetic ester, the place of butyl acetate while acquisition samples, number is Y1~Y6, is measured as stated above, according to chromatography The peak area of benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate in figure, according to its corresponding regression equation calculation sample The content of middle benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate, result of calculation are shown in Table 4.
4 standard deviation of table
Recovery testu (method accuracy test):3 intact original activated carbon tubes of sealing are chosen, it is accurate to move 50 μ l standard reserving solutions are taken to be added in activated carbon tube, sealing is stood overnight, and simulation has acquired the activated carbon tube of sample, by upper The method of stating is measured, according to the peak area of benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate in chromatogram, according to it The content of benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate, result of calculation are shown in corresponding regression equation calculation sample Table 5;
5 recovery testu result of table
The above embodiments and description only illustrate the principle of the present invention and most preferred embodiment, is not departing from this Under the premise of spirit and range, various changes and improvements may be made to the invention, these changes and improvements both fall within requirement and protect In the scope of the invention of shield.

Claims (6)

1. detection method that is a kind of while detecting a variety of pernicious gases in workplace, it is characterised in that:This method is using hydrogen fire The gas chromatography of flame ionization detector FID, while detecting benzene in workplace air, toluene, acetone, butanone, acetic acid second The content of ester, butyl acetate, includes the following steps:
S1), with activated carbon tube collecting work place air, seal Cord blood after acquisition;
S2), take front and back section activated carbon in activated carbon tube, be respectively put into parsing bottle, it is each that 1mL carbon disulfide, shaking is added 1min desorbs 30min, and stripping liquid is for measuring;
S3), take S2 in step)In stripping liquid, carry out sample introduction by 1 .0 μ L of sample size, carried out under corresponding chromatographiccondition Chromatography;
S4), prepare standard curve, according to chromatographic peak as a result, using external standard method to benzene, toluene, acetone, fourth in workplace air Ketone, ethyl acetate, butyl acetate carry out quantitative analysis.
2. detection method that is according to claim 1 a kind of while detecting a variety of pernicious gases in workplace, feature It is:Step S3)In chromatographiccondition be:
Gasify room temperature:230℃;
Fid detector temperature:230℃;
Chromatography column and programmed temperature:50-150 DEG C, 10 DEG C/min;
Column flow:1 ml/min;
Hydrogen flowing quantity:40ml/min;
Air mass flow:400ml/min.
3. detection method that is according to claim 1 a kind of while detecting a variety of pernicious gases in workplace, feature It is, preparing standard curve is specially:Benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate is taken to have the pure object of card standard respectively In matter 10.0mg to the 10mL volumetric flasks equipped with carbon disulfide, it is diluted to scale with carbon disulfide, is made into hybrid standard storing solution, 0,50,100,500,1000,2000 μ l of standard reserving solution are pipetted respectively in 10mL volumetric flasks, and quarter is settled to carbon disulfide Degree, be configured to benzene, toluene, acetone, butanone, ethyl acetate, butyl acetate hybrid standard use liquid.
4. detection method that is according to claim 1 a kind of while detecting a variety of pernicious gases in workplace, feature It is:Chromatography uses capillary chromatographic column, and the column length of the capillary chromatographic column is 30m, and interior diameter is 0.25mm, film thickness are 0.25 μm.
5. detection method that is according to claim 2 a kind of while detecting a variety of pernicious gases in workplace, feature It is:Fid detector carrier gas is the nitrogen that purity is 99 .999%.
6. detection method that is according to claim 2 a kind of while detecting a variety of pernicious gases in workplace, feature It is:Standard curve regression equation in quantitative external standard method is drawn by the way of once fitting.
CN201711173255.8A 2017-11-21 2017-11-21 Detection method that is a kind of while detecting a variety of pernicious gases in workplace Pending CN108387649A (en)

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CN201711173255.8A CN108387649A (en) 2017-11-21 2017-11-21 Detection method that is a kind of while detecting a variety of pernicious gases in workplace

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111855895A (en) * 2019-04-29 2020-10-30 上海岳源环境科技有限公司 Indoor air quality detection method
CN111983080A (en) * 2020-08-18 2020-11-24 浙江中昱环境工程股份有限公司 Method for measuring toxic substances in environment
CN115389664A (en) * 2022-08-25 2022-11-25 宝钢化工湛江有限公司 Method for measuring content of triphenyl in coke oven gas by gas chromatography

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111855895A (en) * 2019-04-29 2020-10-30 上海岳源环境科技有限公司 Indoor air quality detection method
CN111983080A (en) * 2020-08-18 2020-11-24 浙江中昱环境工程股份有限公司 Method for measuring toxic substances in environment
CN115389664A (en) * 2022-08-25 2022-11-25 宝钢化工湛江有限公司 Method for measuring content of triphenyl in coke oven gas by gas chromatography

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