CN107356683A

CN107356683A - A kind of method of acrylamide in Air of Workplace by Gas Chromatography

Info

Publication number: CN107356683A
Application number: CN201710361558.6A
Authority: CN
Inventors: 夏怀翔; 赵华芝; 严章飞; 孔玉萍; 张强; 方栋; 段志祥
Original assignee: Anhui Hongyuan Professional Health Technology Service Co Ltd
Current assignee: Anhui Hongyuan Professional Health Technology Service Co Ltd
Priority date: 2017-05-22
Filing date: 2017-05-22
Publication date: 2017-11-17

Abstract

The invention belongs to workplace air detection technique field, and in particular to a kind of method of acrylamide in Air of Workplace by Gas Chromatography, by taken air sample, bromination reaction obtains dibromo propionamide for detecting in reaction tube.The present invention has advantages below compared with prior art：Method by acrylamide by generating dibromo propionamide in the present invention, it is easy to detect, it is high using method acrylamide bromination rate in the present invention, it is favorably improved the degree of accuracy of experiment, in the relatively low acrylamide of concentration in determining workplace, reliability is high, meets national requirements, detection speed is fast, in terms of gathering 50L samples, concentration limit is 0.004mg/m3, strong interference immunity, the concentration mensuration available for acrylamide in workplace air.

Description

A kind of method of acrylamide in Air of Workplace by Gas Chromatography

Technical field

The invention belongs to workplace air detection technique field, and in particular to a kind of gas chromatography determines workplace The method of acrylamide in air.

Background technology

In occupational health detection work, the pollution condition of the harmful substance such as acrylic acid in accurate evaluation workplace air, For protection labourer health, occupational hazards generation, guarantee enterprise safety operation, the stabilization that promotes social harmony is avoided to have reality Meaning, acrylamide is a kind of noxious material, can be entered by skin, respiratory tract, alimentary canal internal, is raw material production using him Polyacrylamide be widely used in every field, supply falls short of demand, occupies in China's energy strategy, water conservation strategies very heavy The status wanted, but the improvement of acrylamide production technology reduces dust in air concentration, makes its harm to worker more hidden Covering property, while certain difficulty also is brought for the scientific research task research of acrylamide Site Detection part, at present in often use The packed column of polarity carries out chromatography of gases detection, and its precision and sensitivity do not adapt to low dense in existing acrylamide production The process characteristics such as degree, humidity operation, therefore should be to this further research.

The content of the invention

The purpose of the present invention is to be directed to the problem of existing, there is provided third in a kind of Air of Workplace by Gas Chromatography The method of acrylamide.

The present invention is achieved by the following technical solutions：Acryloyl in a kind of Air of Workplace by Gas Chromatography The method of amine, with the impinger equipped with 10mL water, with 500mL/min flow velocity in the workplace that sampled point gathers Air 20 minutes, by weight, take 10 parts of gained absorbing liquid to add in reaction tube, be 10% sulphur acid for adjusting pH with mass concentration To 1.5,1.6 parts of the KBr that mass concentration is 20% is added, after shaking up, with frequency 2400MHz, power 20W microwave radiation 5 Minute, then place 10 minutes in the dark, add 0.5mol/L 2 parts of sodium thiosulfate, inversion shaking of jumping a queue is multiple, removes more Remaining bromine, 2 parts of ethyl acetate is then added, extracts 2 minutes, 1 part of upper liquid is taken after being layered, is dehydrated with anhydrous sodium sulfate Afterwards, 0.001 part of sample introduction is taken, is determined under selected GC conditions.

As further improvement of these options, the ethyl acetate is limited by the grand glad edible alcohol of Zhejiang Province's Yuyao City Company provides, active constituent content >=99.9%.

As further improvement of these options, selected gas chromatograph equipment has electron capture detector (ECD), and carrier gas is Nitrogen, the purity of nitrogen is more than 99.999%.

As further improvement of these options, the chromatographic condition is：From long 2m, internal diameter 3mm stainless steel FFAP posts；Column temperature：200 DEG C, vaporizer and detection room temperature are 240 DEG C, flow rate of carrier gas 60mL/min, the μ L of sample size 2.

As further improvement of these options, take 0.1 μ g/mL acrylamide titers compound concentration for 0.01, 0.03rd, 0.05,0.07,0.09 μ g/mL, bromination and extraction process are identical with preceding method, 2 μ L extract sample introductions are taken, with propylene Amide content is mapped to peak area, draws standard curve.

As further improvement of these options, the peak height phase that the peak height that institute's test sample product obtain is obtained with standard sample Compare, obtain institute's test sample product and standard sample peak height difference, thus obtain being detected the acrylamide concentration in sample.

As further improvement of these options, the air sampling selects low discharge air sampler, model TWA-300。

As further improvement of these options, the gag material used of jumping a queue is silica gel.

The present invention has advantages below compared with prior art：Method by acrylamide by generating dibromo propionyl in the present invention Amine, it is easy to detect, it is high using method acrylamide bromination rate in the present invention, the degree of accuracy of experiment is favorably improved, in measure work When making the relatively low acrylamide of concentration in place, reliability is high, meets national requirements, detection speed is fast, to gather 50L samples Meter, concentration limit 0.004mg/m3, strong interference immunity, the concentration available for acrylamide in workplace air are surveyed It is fixed.

Embodiment

Embodiment 1

A kind of method of acrylamide in Air of Workplace by Gas Chromatography, absorbed with the impact type equipped with 10mL water Pipe, with air 20 minute of the 500mL/min flow velocity in the workplace that sampled point gather, by weight, take gained absorption 10 parts of liquid is added in reaction tube, is 10% sulphur acid for adjusting pH to 1.5 with mass concentration, adds the KBr that mass concentration is 20% 1.6 parts, after shaking up, with frequency 2400MHz, power 20W microwave radiation 5 minutes, then place 10 minutes, add in the dark 2 parts of 0.5mol/L sodium thiosulfate, inversion shaking of jumping a queue is multiple, removes unnecessary bromine, then adds 2 parts of ethyl acetate, Extraction 2 minutes, 1 part of upper liquid is taken after being layered, after being dehydrated with anhydrous sodium sulfate, takes 0.001 part of sample introduction, in selected gas phase color Determined under spectral condition.

Wherein, the ethyl acetate is provided by Yuyao City Long Xin edible alcohols Co., Ltd of Zhejiang Province, active constituent content ≥99.9%。

Wherein, selected gas chromatograph equipment has electron capture detector (ECD), and carrier gas is nitrogen, and the purity of nitrogen exists More than 99.999%, gas chromatograph equipment choosing Agilent 6890GC；The air sampling selects low discharge air sampler, Model TWA-300；The gag material used of jumping a queue is silica gel；

The chromatographic condition is：From long 2m, internal diameter 3mm stainless steel FFAP posts；Column temperature：200 DEG C, vaporizer and detection room temperature Degree is 240 DEG C, flow rate of carrier gas 60mL/min, the μ L of sample size 2.

Titer is prepared, and it is 0.01,0.03,0.05,0.07,0.09 to take 0.1 μ g/mL acrylamide titers compound concentration μ g/mL, bromination and extraction process are identical with preceding method, take 2 μ L extract sample introductions, and peak area is made with acrylamide content Figure, draw standard curve.

Wherein, the peak height that institute's test sample product obtain is compared with the peak height that standard sample obtains, obtains institute's test sample product and mark The quasi- high difference of sample peak, thus obtains being detected the acrylamide concentration in sample.

The acrylamide bromination rate of different content is detected, every group of detection averages to obtain measurement result such as 3 times Under：

Table 1

It is higher that bromination rate in the present invention is can be seen that by data in table 1.

FFAP and DEGS posts are compared, compared from peak value mouldability, FFAP posts are preferable, therefore need to use FFAP posts.

6 detections are carried out according to method in the present invention to the acrylamide that concentration is 0.01mg/L, 0.05mg/L, obtain phase It is as follows to standard deviation：

Table 2

It is relatively low that its relative standard deviation rate is can be seen that by data in table 2, meets corresponding examination criteria, when scene occurs third When olefin(e) acid, acetone, acrylamide coexist, in above-mentioned detection, acrylic acid and acetone not appearance, to Determination of acrylamide without dry Disturb, the concentration mensuration available for acrylamide in workplace air.

Claims

1. a kind of method of acrylamide in Air of Workplace by Gas Chromatography, it is characterised in that use and 10mL water is housed Impinger, with air 20 minute of the 500mL/min flow velocity in the workplace that sampled point gathers, by weight Meter, take 10 parts of gained absorbing liquid to add in reaction tube, be 10% sulphur acid for adjusting pH to 1.5 with mass concentration, adding mass concentration is 1.6 parts of 20% KBr, after shaking up, with frequency 2400MHz, power 20W microwave radiation 5 minutes, 10 are then placed in the dark Minute, 0.5mol/L 2 parts of sodium thiosulfate is added, inversion shaking of jumping a queue is multiple, removes unnecessary bromine, then adds 2 parts Ethyl acetate, extract 2 minutes, 1 part of upper liquid is taken after being layered, after being dehydrated with anhydrous sodium sulfate, 0.001 part of sample introduction is taken, is selecting Determined under fixed GC conditions.

2. the method for acrylamide, its feature exist in a kind of Air of Workplace by Gas Chromatography as claimed in claim 1 In the ethyl acetate is provided by Yuyao City Long Xin edible alcohols Co., Ltd of Zhejiang Province, active constituent content >=99.9%.

3. the method for acrylamide, its feature exist in a kind of Air of Workplace by Gas Chromatography as claimed in claim 1 In selected gas chromatograph equipment has electron capture detector (ECD), and carrier gas is nitrogen, and the purity of nitrogen is more than 99.999%.

4. the method for acrylamide, its feature exist in a kind of Air of Workplace by Gas Chromatography as claimed in claim 3 In the chromatographic condition is：From long 2m, internal diameter 3mm stainless steel FFAP posts；Column temperature：200 DEG C, vaporizer and detection room temperature Degree is 240 DEG C, flow rate of carrier gas 60mL/min, the μ L of sample size 2.

5. the method for acrylamide, its feature exist in a kind of Air of Workplace by Gas Chromatography as claimed in claim 1 In it is 0.01,0.03,0.05,0.07,0.09 μ g/mL, bromination and extraction to take 0.1 μ g/mL acrylamide titers compound concentration Process is identical with preceding method, takes 2 μ L extract sample introductions, with acrylamide content to peak area mapping, drafting standard curve.

6. the method for acrylamide, its feature exist in a kind of Air of Workplace by Gas Chromatography as claimed in claim 1 In the peak height that institute's test sample product obtain is compared with the peak height that standard sample obtains, obtains institute's test sample product and standard sample peak height Difference, thus obtain being detected the acrylamide concentration in sample.

7. the method for acrylamide, its feature exist in a kind of Air of Workplace by Gas Chromatography as claimed in claim 1 In the air sampling selects low discharge air sampler, model TWA-300.

8. the method for acrylamide, its feature exist in a kind of Air of Workplace by Gas Chromatography as claimed in claim 1 In the gag material used of jumping a queue is silica gel.