CN104237410A - Detection method of substituted benzene in environmental water - Google Patents
Detection method of substituted benzene in environmental water Download PDFInfo
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- CN104237410A CN104237410A CN201410477063.6A CN201410477063A CN104237410A CN 104237410 A CN104237410 A CN 104237410A CN 201410477063 A CN201410477063 A CN 201410477063A CN 104237410 A CN104237410 A CN 104237410A
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Abstract
The invention relates to a detection method of substituted benzene in environmental water, and belongs to the field of detection methods of environmental samples. The detection method of substituted benzene in environmental water comprises the steps as follows: (1), fourteen types of diethyl ether stock solutions of substituted benzene are prepared by chromatographic standard samples and diluted to obtain a standard concentration series; (2), a water sample is taken, pH of the water sample is regulated to be neutral, the water sample flows through an enriching column which is eluted by diethyl ether, and an eluent is subjected to dehydration and concentration to a constant volume by diethyl ether for chromatographic analysis; and (3), a double-column qualitative method is adopted, relative retention time of a standard sample and an actual sample is measured respectively, compounds corresponding to chromatographic peaks of the actual water sample are determined according to the relative retention time, and peak height quantitation is performed with an external standard method. According to the detection method, the operation is simple and convenient, the recovery rate is high, and the method for analyzing substituted benzene by double capillary columns qualitatively and quantitatively has the advantages of simplicity, convenience, flexibility, accuracy and wide linear range and is suitable for monitoring analysis of trace substituted benzene in water.
Description
Technical field
The present invention relates to the detection method of substituted benzene in a kind of environment water, belong to environmental analysis method field.
Background technology
Substituted benzene is poisonous and harmful substance, and acute poisoning mainly acts on human central nervous system, and slow poisoning mainly acts on hematopoietic tissue and nervous system, is confirmed to be carcinogenic substance recently, and in water, the content of substituted benzene is the important content of environmental monitoring.But because substituted benzene substance classes is too many, and content is low again, general monitoring method is difficult to disposable detection completely or detect accurately, and at present, in water, the detection of substituted benzene content is the large difficult point of one in water quality detection.
Therefore the detection method studying substituted benzene in the water body that a kind of accuracy is high, repeatability is high, easy and simple to handle, detection limit is low is necessary.
Summary of the invention
The present invention aims to provide the detection method of substituted benzene in the water body that a kind of accuracy is high, repeatability is high, easy and simple to handle, detection limit is low.
The detection method of substituted benzene in environment water of the present invention, comprises the following steps:
(1) prepare the ether stock solution of 14 kinds of substituted benzenes with chromatogram standard specimen, concentration 1000ng/ml, 50ng/ml, 5ng/ml, Standard Reserving Solution diluted, joins to obtain a normal concentration series: 0.1,1,5,10,100,200ng/ml.
(2) water sampling 10 liters, adjust pH to neutral, with the flow velocity of about 30 ml/min, flow through enriching column, drain in enriching column after residual moisture with decompression water pump, divide five wash-out enriching columns with 45 milliliters of ether, eluent is through anhydrous sodium sulfate dehydration, K-D concentrator is concentrated into and is less than 1 milliliter, with ether constant volume to 1 milliliter, for stratographic analysis.
(3) dual column identification is adopted, under certain chromatographic condition, with this two capillaries post that polarity is different, the relative retention time of bioassay standard sample and actual sample respectively, the compound corresponding according to each chromatographic peak of relative retention time determination actual water sample, adopts external standard method peak height quantitative.
Preferably, enriching column of the present invention is the glass column of internal diameter 1.5 centimetres, length 20 centimetres, in-built pregnant solution GDX-102 carrier, 5 grams, the 60-80 order handled well through acetone, methyl alcohol, the glass wool that lower plug is processed on a small quantity.
Preferred, chromatographic condition of the present invention is post 1 is nonpolar Shimadzu CBP1 post, 50m × 0.33mm, quartz capillary column, detector temperature 220 DEG C, injector temperature 220 DEG C, air 660 ml/min, hydrogen 28 ml/min, split ratio 32:1, column temperature initial temperature 60 DEG C, keep two minutes, be raised to 72 DEG C with 3 DEG C/minute of speed, then be raised to 122 DEG C with 5 DEG C/minute of speed; Post 2 is semipolar Shimadzu CBP10 post, 50m × 0.33mm quartz capillary column, detector temperature 220 DEG C, injector temperature 22O DEG C, air 48O ml/min, hydrogen 28 ml/min, split ratio 38:1, column temperature initial temperature 9O DEG C, keeps three minutes, is raised to 19O DEG C with 4 DEG C/minute of speed.
Preferred further, 14 kinds of substituted benzene compounds of the present invention are toluene, chlorobenzene, ethylbenzene, m-dimethylbenzene, p-dimethylbenzene, ortho-xylene, isopropyl benzene, bromobenzene, n-proplbenzene, 1,2,4-trimethylbenzene, nitrobenzene, N, accelerine, ortho-methylnitrobenzene, 1,2,3-trichloro-benzenes.
Detection method of the present invention, GDX-102 macroreticular resin is used to carry out Sync enrichment to alkyl benzene micro-in water, nitrobenzene, halogeno-benzene class, water sample after the enrichment capillary column that two polarity is different carries out gas chromatography dual column identification, quantified by external standard method.Described detection method is 92%-98% to the recovery of standard addition of 14 kinds of substituted benzenes, and relative standard deviation is below 5%, and lowest detectable limit reaches 3.25ng, and the dual-capillary column quilitative method of employing is easy and simple to handle, reliable results.
Detection method of the present invention, by GDX-1O2 macroreticular resin Sync enrichment underwater trace alkyl benzene, nitrobenzene and halogeno-benzene class, easy and simple to handle, the recovery is high, the dual-capillary column qualitative and quantitative analysis substituted benzene method set up, there is easy, sensitive, accurate, that the range of linearity is wide advantage, be suitable for the monitoring analysis of underwater trace substituted benzene.
Embodiment
Embodiment one:
(1) 14 kinds of substituted benzenes (toluene, chlorobenzene, ethylbenzene, m-dimethylbenzene, p-dimethylbenzene, ortho-xylene, isopropyl benzene, bromobenzene, n-proplbenzene, 1 is prepared with chromatogram standard specimen, 2,4-trimethylbenzene, nitrobenzene, N, accelerine, ortho-methylnitrobenzene, 1,2,3-trichloro-benzenes) ether stock solution, concentration 1000ng/ml, 50ng/ml, 5ng/ml, Standard Reserving Solution is diluted, joins to obtain a normal concentration series: 0.1,1,5,10,100,200ng/ml.
(2) water sampling 10 liters, adjust pH to neutral, with the flow velocity of about 30 ml/min, (enriching column is the glass column of internal diameter 1.5 centimetres, length 20 centimetres to flow through enriching column, in-built pregnant solution GDX-102 carrier, 5 grams, the 60-80 order handled well through acetone, methyl alcohol, the glass wool that lower plug is processed on a small quantity), to drain in enriching column after residual moisture with decompression water pump, five wash-out enriching columns are divided with 45 milliliters of ether, eluent is through anhydrous sodium sulfate dehydration, K-D concentrator is concentrated into and is less than 1 milliliter, with ether constant volume to 1 milliliter, for stratographic analysis.
(3) dual column identification is adopted, under certain chromatographic condition, (chromatographic condition is post 1 is nonpolar Shimadzu CBP1 post, 50m × 0.33mm, quartz capillary column, detector temperature 220 DEG C, injector temperature 220 DEG C, air 660 ml/min, hydrogen 28 ml/min, split ratio 32:1, column temperature initial temperature 60 DEG C, keep two minutes, be raised to 72 DEG C with 3 DEG C/minute of speed, then be raised to 122 DEG C with 5 DEG C/minute of speed; Post 2 is semipolar Shimadzu CBP10 post, 50m × 0.33mm quartz capillary column, detector temperature 220 DEG C, injector temperature 22O DEG C, air 48O ml/min, hydrogen 28 ml/min, split ratio 38:1, column temperature initial temperature 9O DEG C, keeps three minutes, is raised to 19O DEG C with 4 DEG C/minute of speed), with this two capillaries post that polarity is different, the relative retention time of bioassay standard sample and actual sample respectively, the compound corresponding according to each chromatographic peak of relative retention time determination actual water sample, adopts external standard method peak height quantitative.
Embodiment two: the mensuration of actual water sample
Use detection method of the present invention, carry out substituted benzene material to some water body and detect, testing result as shown in Table-1.
Table-l testing result (ng/ml).
。
Claims (4)
1. the detection method of substituted benzene in environment water, comprises the following steps:
(1) prepare the ether stock solution of 14 kinds of substituted benzenes with chromatogram standard specimen, concentration 1000ng/ml, 50ng/ml, 5ng/ml, Standard Reserving Solution diluted, joins to obtain a normal concentration series: 0.1,1,5,10,100,200ng/ml;
(2) water sampling 10 liters, adjust pH to neutral, with the flow velocity of about 30 ml/min, flow through enriching column, drain in enriching column after residual moisture with decompression water pump, divide five wash-out enriching columns with 45 milliliters of ether, eluent is through anhydrous sodium sulfate dehydration, K-D concentrator is concentrated into and is less than 1 milliliter, with ether constant volume to 1 milliliter, for stratographic analysis;
(3) dual column identification is adopted, under certain chromatographic condition, with this two capillaries post that polarity is different, the relative retention time of bioassay standard sample and actual sample respectively, the compound corresponding according to each chromatographic peak of relative retention time determination actual water sample, adopts external standard method peak height quantitative.
2. the detection method of substituted benzene in environment water as claimed in claim 1, it is characterized in that described enriching column is the glass column of internal diameter 1.5 centimetres, length 20 centimetres, in-built pregnant solution GDX-102 carrier, 5 grams, the 60-80 order handled well through acetone, methyl alcohol, the glass wool that lower plug is processed on a small quantity.
3. the detection method of substituted benzene in environment water as claimed in claim 1, it is characterized in that described chromatographic condition be post 1 is nonpolar Shimadzu CBP1 post, 50m × 0.33mm, quartz capillary column, detector temperature 220 DEG C, injector temperature 220 DEG C, air 660 ml/min, hydrogen 28 ml/min, split ratio 32:1, column temperature initial temperature 60 DEG C, keep two minutes, be raised to 72 DEG C with 3 DEG C/minute of speed, then be raised to 122 DEG C with 5 DEG C/minute of speed; Post 2 is semipolar Shimadzu CBP10 post, 50m × 0.33mm quartz capillary column, detector temperature 220 DEG C, injector temperature 22O DEG C, air 48O ml/min, hydrogen 28 ml/min, split ratio 38:1, column temperature initial temperature 9O DEG C, keeps three minutes, is raised to 19O DEG C with 4 DEG C/minute of speed.
4. the detection method of substituted benzene in environment water as claimed in claim 1, it is characterized in that 14 kinds of described substituted benzene compounds are toluene, chlorobenzene, ethylbenzene, m-dimethylbenzene, p-dimethylbenzene, ortho-xylene, isopropyl benzene, bromobenzene, n-proplbenzene, 1,2,4-trimethylbenzene, nitrobenzene, N, accelerine, ortho-methylnitrobenzene, 1,2,3-trichloro-benzenes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849385A (en) * | 2015-05-14 | 2015-08-19 | 惠州市食品药品检验所 | Gas chromatographic mass spectrometry determination method for chlorobenzene compounds |
| CN106324110A (en) * | 2015-06-23 | 2017-01-11 | 大连瑞贤达塑胶有限公司 | Method for testing isopropyl benzene in plastic package material |
| CN110579557A (en) * | 2019-09-19 | 2019-12-17 | 北京科技大学 | HPLC analysis detection method for simultaneously detecting 12 monocyclic aromatic hydrocarbons in water |
-
2014
- 2014-09-18 CN CN201410477063.6A patent/CN104237410A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849385A (en) * | 2015-05-14 | 2015-08-19 | 惠州市食品药品检验所 | Gas chromatographic mass spectrometry determination method for chlorobenzene compounds |
| CN106324110A (en) * | 2015-06-23 | 2017-01-11 | 大连瑞贤达塑胶有限公司 | Method for testing isopropyl benzene in plastic package material |
| CN110579557A (en) * | 2019-09-19 | 2019-12-17 | 北京科技大学 | HPLC analysis detection method for simultaneously detecting 12 monocyclic aromatic hydrocarbons in water |
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