CN112255341A - Method for detecting benzene series in water by negative pressure headspace gas chromatography - Google Patents
Method for detecting benzene series in water by negative pressure headspace gas chromatography Download PDFInfo
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- CN112255341A CN112255341A CN202011092244.9A CN202011092244A CN112255341A CN 112255341 A CN112255341 A CN 112255341A CN 202011092244 A CN202011092244 A CN 202011092244A CN 112255341 A CN112255341 A CN 112255341A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
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Abstract
The invention discloses a method for detecting benzene series in water by negative pressure headspace gas chromatography. The method comprises the steps of pumping a certain volume of gas out of a headspace bottle, accurately adding a water sample with the same volume, balancing at a certain temperature, pumping a proper amount of gas, and analyzing by using a gas chromatograph. The method can effectively analyze the content of the benzene series in the water, can well increase the content of the target compound in a gas phase during gas-liquid balance by utilizing the negative pressure headspace, obviously improves the sensitivity of the target compound, can obtain a very low detection limit even if the target compound is balanced for 10min at room temperature, does not add sodium chloride in the pretreatment process, reduces the interference of impurities, improves the detection sensitivity, and can better meet the requirements of analysis and monitoring.
Description
Technical Field
The invention relates to a method for detecting benzene series in water, in particular to a method for rapidly detecting the benzene series in the water by negative pressure headspace gas chromatography.
Background
The benzene series is a widely used chemical solvent and organic intermediate, has strong volatility, is widely present in the environment and seriously harms human health. Benzene series is a toxic and harmful substance recognized internationally, has high toxicity and has mutagenic, carcinogenic and teratogenic hazards, wherein 6 kinds of benzene series, namely benzene, toluene, ethylbenzene, paraxylene, metaxylene and orthoxylene, are listed in the water environment priority control pollutant list of China. Therefore, the method has important significance for the research of the detection method of the benzene series content in the water environment.
At present, the detection method of the benzene series in water mainly comprises a gas chromatography and a gas chromatography mass spectrometry, the gas chromatography can well separate the benzene series, the FID detector can provide lower detection limit and stability, and the price is relatively low, so that the gas chromatography is widely applied. The difficulty and limitation of the current detection method for the benzene series in water lie in a pretreatment method, and how to extract the benzene series in water more quickly and conveniently is a problem which is concerned. The pretreatment methods include liquid-liquid extraction, headspace method, solid-phase microextraction, purging and trapping method, and the like. The liquid-liquid extraction method has long analysis time and low sensitivity, and adopts carbon disulfide as a solvent, so that the carbon disulfide has toxicity, and the extraction process is easy to cause pollution and loss; when the solid-phase microextraction technology is used for measuring the benzene series in water, the method has poor repeatability; while purging the capture equipment is expensive. The headspace method is the most widely applied determination method at present, is simple to operate and low in cost, and is an environment-friendly analysis method. However, in the existing headspace gas chromatography, when gas and liquid are balanced, the content of benzene series in the gas phase is low, and the lower detection limit is difficult to achieve, so that the trace benzene series in water cannot be detected.
Disclosure of Invention
Aiming at the defects of the existing headspace gas chromatography for determining the benzene series in water, the invention aims to provide a method for rapidly detecting the benzene series in water by using the negative pressure headspace gas chromatography, the method utilizes the negative pressure headspace technology, can increase the content of a substance to be detected in a gas phase of a target compound during gas-liquid equilibrium, obviously improves the sensitivity of the target compound, can obtain a very low detection limit even if the target compound is equilibrated for 10min at room temperature, does not add sodium chloride in a pretreatment process, reduces the interference of impurities, and has the advantages of simple operation, good stability and high accuracy.
In order to achieve the aim, the invention provides a method for rapidly detecting benzene series in water by using negative pressure headspace gas chromatography, which comprises the following steps: pumping a certain volume of gas from the headspace bottle, accurately adding a water sample with the same volume, balancing at a certain temperature, pumping a proper amount of gas, and analyzing by using a gas chromatograph.
Preferably, the draw volume is 5-60 ml.
Preferably, the headspace bottle has an equilibrium temperature of from room temperature to 70 ℃.
Preferably, the headspace bottle equilibration time is 10-30 min.
Preferably, said headspace bottle is characterized by an equilibrium temperature of from room temperature to 60 ℃.
Preferably, the temperature of the sample injection needle in the headspace part is 100-.
Preferably, the gas chromatography conditions are: sample introduction volume: 1.0ml, injection port temperature: 180 ℃, split ratio of 10: 1, the flow rate of a chromatographic column is 2.0ml/min, and the temperature programming of a column incubator is as follows: keeping the temperature at 60 deg.C for 10min at 0min, heating to 110 deg.C at 3 deg.C/min for 3min, heating to 180 deg.C at 6 deg.C/min, and keeping for 3 min; the detector is FID, and the detector temperature is 300 ℃. The gas chromatography column was selected to be HP-INNOWAX 30m 0.53mm 1.0. mu.m.
Preferably, the benzene series comprises: benzene, toluene, ethylbenzene, p-xylene, m-xylene, o-xylene, styrene and cumene.
Compared with the prior art, the method for rapidly detecting the benzene series in the water by using the negative pressure headspace gas chromatography has the following advantages:
1. compared with the conventional direct headspace gas chromatography, the method utilizes the negative pressure headspace technology, increases the content of the object compound to be detected in the gas phase during gas-liquid equilibrium, obviously increases the sensitivity of the object compound, and can reach a lower detection limit;
2. compared with the method of adding sodium chloride as a pretreatment means, the method does not add sodium chloride, reduces the interference of impurities, improves the detection sensitivity, and can better meet the requirements of analysis and monitoring;
3. compared with the current commonly used direct headspace gas chromatography, the method can finish analysis within 10 minutes at the fastest speed, and better meets the requirement of rapid analysis;
4. the method has the advantages of simple and rapid operation, low cost, high recovery rate, high accuracy and high precision.
Detailed Description
The invention is further illustrated, but not limited, by the following examples.
Example 1: standard curve and detection limit
Standard curves were prepared using 5 concentrations of benzene series standard solutions, 1.0. mu.g/L, 10.0. mu.g/L, 50.0. mu.g/L, 100. mu.g/L, and 500. mu.g/L. The blank water sample is added with standard to prepare 7 samples with the concentration of 0.5 mug/L for testing, the sampling volume is 10mL, the volume of the injection gas is 1.0mL, the standard deviation is calculated, then the detection limit is calculated according to MDL = t × S (t = 3.143), the 4-time detection limit is the lower limit of quantification, and the result is as follows:
example 2: accuracy and precision
Parallel tests were performed with 6 samples, and the results of method precision and recovery were as follows.
Example 3: detection of benzene series in drinking water
1. Sample pretreatment: accurately pumping 10ml of gas in the sealed headspace bottle, accurately adding 10ml of water sample, balancing for 10min at 60 ℃, and taking 1ml of gas on the liquid to enter gas chromatography for analysis;
2. configuration of the standard curve: diluting the benzene series standard substance step by step to prepare a standard curve with concentration gradient of 1.0 mug/L, 10.0 mug/L, 50.0 mug/L, 100 mug/L and 500 mug/L in sequence, and adding 10ml of the prepared standard curve into a negative pressure headspace bottle;
3. headspace instrument conditions: sample equilibrium temperature: 60 ℃, injection needle temperature: 110 ℃, transmission line temperature: 130 ℃, equilibration time: 10min, sample injection volume: 1.0 ml;
4. gas chromatography instrument conditions: sample inlet temperature: 180 ℃, split ratio of 10: 1, the flow rate of a chromatographic column is 2.0ml/min, the temperature of a column incubator is 60 ℃ when the temperature is programmed for 0min, the temperature is kept for 10min, the temperature is raised to 110 ℃ at the speed of 3 ℃/min and kept for 3min, the temperature is raised to 180 ℃ at the speed of 6 ℃/min and kept for 3 min; the detector is FID, and the temperature of the detector is 300 ℃;
5. and (3) sample determination: 10ml of sample was added to a negative pressure headspace bottle and measured under the above instrument conditions. The retention time of the benzene series standard substance is used for qualitative determination, and the external standard method is used for quantitative determination. The results show that the benzene series in the drinking water are all less than the detection limit.
While the preferred embodiments of the present invention have been illustrated, various changes and modifications may be made by one skilled in the art without departing from the scope of the invention.
Claims (8)
1. A method for detecting benzene series in water by negative pressure headspace gas chromatography is characterized by comprising the following steps: pumping a certain volume of gas from the headspace bottle, accurately adding a water sample with the same volume, balancing at a certain temperature, pumping a proper amount of gas, and analyzing by using a gas chromatograph.
2. The method of claim 1, wherein: the extraction volume is 5-60 ml.
3. The method of claim 1, wherein: the headspace bottle equilibrium temperature was from room temperature to 70 ℃.
4. The method of claim 1, wherein: the headspace bottle equilibration time is 10-30 min.
5. The method of claim 1, wherein: the temperature of the sample injection needle in the headspace part is 100-110 ℃, and the temperature of the transmission line is 100-130 ℃.
6. The method of claim 1, wherein: gas chromatography conditions: sample introduction volume: 1.0ml, injection port temperature: 180 ℃, split ratio of 10: 1, the flow rate of a chromatographic column is 2.0ml/min, and the temperature programming of a column incubator is as follows: keeping the temperature at 60 deg.C for 10min at 0min, heating to 110 deg.C at 3 deg.C/min for 3min, heating to 180 deg.C at 6 deg.C/min, and keeping for 3 min; the detector is FID, and the detector temperature is 300 ℃.
7. The method of claim 6, wherein: the gas chromatography column was selected to be HP-INNOWAX 30m 0.53mm 1.0. mu.m.
8. The method of claim 1, wherein: the benzene series includes benzene, toluene, ethylbenzene, p-xylene, m-xylene, o-xylene, styrene and cumene.
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| CN202011092244.9A CN112255341A (en) | 2020-10-13 | 2020-10-13 | Method for detecting benzene series in water by negative pressure headspace gas chromatography |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115047114A (en) * | 2022-07-13 | 2022-09-13 | 自然资源部第三海洋研究所 | Method for detecting low-trace concentration benzene series monomer carbon stable isotope composition in water body |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3925496A (en) * | 1974-01-21 | 1975-12-09 | Atlantic Richfield Co | Production of styrene |
| CN105467030A (en) * | 2015-11-23 | 2016-04-06 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for detecting benzene series in dairy product |
-
2020
- 2020-10-13 CN CN202011092244.9A patent/CN112255341A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3925496A (en) * | 1974-01-21 | 1975-12-09 | Atlantic Richfield Co | Production of styrene |
| CN105467030A (en) * | 2015-11-23 | 2016-04-06 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for detecting benzene series in dairy product |
Non-Patent Citations (6)
| Title |
|---|
| 付翠轻 等: "自动顶空-气相色谱法测定水中甲醇的方法优化", 《中国环境监测》 * |
| 张晓琳 等: "水体中挥发性有机物超声雾化提取法的在线监测", 《环境化学》 * |
| 梁坚: "顶空-气相色谱法测定水中苯系物、乙腈和丙烯腈", 《理化检验(化学分册)》 * |
| 罗毅 等: "《地表水环境质量监测实用分析方法》", 31 December 2009, 中国环境科学出版社 * |
| 陈静 等: "毛细管顶空气相色谱法测定水源水中的氯丁二烯方法研究", 《重庆市预防医学会2010年论文集》 * |
| 魏复盛 等: "《水和废水监测分析方法指南 下册》", 31 March 1997, 中国环境科学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115047114A (en) * | 2022-07-13 | 2022-09-13 | 自然资源部第三海洋研究所 | Method for detecting low-trace concentration benzene series monomer carbon stable isotope composition in water body |
| CN115047114B (en) * | 2022-07-13 | 2024-06-04 | 自然资源部第三海洋研究所 | Method for detecting stable isotope composition of benzene series monomer carbon with low trace concentration in water body |
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