CN105467034A - Gas chromatography detection method for benzotrichloride - Google Patents
Gas chromatography detection method for benzotrichloride Download PDFInfo
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- CN105467034A CN105467034A CN201510932525.3A CN201510932525A CN105467034A CN 105467034 A CN105467034 A CN 105467034A CN 201510932525 A CN201510932525 A CN 201510932525A CN 105467034 A CN105467034 A CN 105467034A
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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
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
The invention belongs to the technical of analysis, and particularly relates to a gas chromatography detection method for benzotrichloride. The detection method comprises the steps that 1, a sample to be detected is dissolved with a solvent; 2, working conditions of a gas chromatograph are set, wherein an Agilent DB-5 capillary column is adopted as a chromatographic column, the column box temperature is 150-240 DEG C, the sample inlet temperature is 280 DEG C, the temperature of a detector is 300 DEG C, the flow rate of carrier gas of the chromatographic column is 1 mL/min, the air flow speed is 300 mL/min, the hydrogen flow speed is 30 mL/min, and the split ratio is 100:1; 3, an automatic sampler is used for sampling, and a chromatogram starts to be detected and recorded; 4, an area normalization method is used for calculating out the content of benzotrichloride. The gas chromatography detection method has the advantages of being high in analysis speed, accurate in result, low in analysis cost, capable of effectively and rapidly guiding production arrangement, and capable of accurately measuring the content of a benzotrichloride product.
Description
Technical field
The invention belongs to analysis technical field, be specifically related to a kind of gas-chromatography detection method of benzotrichloride.
Background technology
Benzotrichloride is colourless transparent liquid, has specific stimulation smell, carries out free radical chlorination substitution reaction and obtains, be fuming in atmosphere primarily of toluene and chlorine under light or radical initiator cause, unstable, facile hydrolysis.Benzotrichloride fusing point is-5 DEG C, and boiling point is 220.8 DEG C.
Benzotrichloride is mainly used as the base stock of dyestuff, medicine intermediate and ultraviolet light absorber UV-9, UV-531, be a kind of important organic synthesis intermediate, can be used for manufacturing benzoic acid, benzoyl chloride, triphenhlmethane dye, anthraquinone dye and quinoline dye etc.
Benzotrichloride can produce the multiple by-product impurities such as a more chlorine replacement, dichloro replacement and phenyl ring replacement in process of production, and impurity boiling point is close, and polarity spectrum is little, for its analysis brings larger difficulty.At present, to the test stone that the detection of benzotrichloride is also ununified.
Summary of the invention
The object of this invention is to provide a kind of gas-chromatography detection method of benzotrichloride, have analysis speed fast, detection sensitivity is high, and analysis result is feature accurately.
The gas-chromatography detection method of benzotrichloride of the present invention, comprises the steps:
(1) testing sample is adopted dissolution with solvents;
(2) condition of work of gas chromatograph is set:
Chromatographic column: AgilentDB-5 capillary column;
Post case temperature: 150 ~ 240 DEG C;
Injector temperature: 280 DEG C;
Detector temperature: 300 DEG C;
Chromatographic column flow rate of carrier gas: 1mL/min;
Air velocity: 300mL/min;
Hydrogen flow rate: 30mL/min;
Split ratio: 100:1;
(3) use automatic sampler sample introduction, start to detect and record chromatogram;
(4) usable floor area normalization method calculates the content of benzotrichloride.
Wherein:
Described solvent is phenixin.
Described chromatogram column length is 30m, and bore is 0.32mm, and thickness is 0.25 μm.
Described detecting device is flame ionization ditector.
Described post case temperature adopts temperature programme, initial temperature 150 DEG C, keeps 1min, is warmed up to 240 DEG C with the programming rate of 10 DEG C/min, keeps 5min.
Described uses automatic sampler sample introduction, and sample size is 0.6 μ L.
Utilize the integrating function of AgilentOpenLAB workstation, usable floor area normalization method calculates the content of benzotrichloride.
Testing sample benzotrichloride is dissolved in carbon tetrachloride solvent, carry out gas chromatographic analysis, obtain the gas chromatogram of testing sample benzotrichloride, by analysis software, adopt area normalization method determine the area of the characteristic peak of benzotrichloride in described gas chromatogram account for the solvent peak eliminated in this gas chromatogram after the number percent of the total area at all peaks.
Beneficial effect of the present invention is as follows:
The present invention utilizes gas chromatographic analysis can obtain the content of benzotrichloride in testing sample, has analysis speed fast, and result is accurate, and analysis cost is low, can the feature that arranges of Instructing manufacture fast and effectively.
Adopt AgilentDB-5 capillary column product compositions clearly can be separated, reproducible.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 detects the gas chromatogram obtained for the first time;
Fig. 2 is that the embodiment of the present invention 1 detects the gas chromatogram obtained for the second time.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
1, reagent and instrument
Reagent: industrial benzotrichloride, phenixin (chromatographic grade).
Instrument: Agilent7820A gas chromatograph (band automatic sampler), AgilentOpenLAB workstation, AgilentDB-5 capillary column, specification is 30m × 0.32mm × 0.25 μm; Flame ionization ditector.
2, detecting step
The gas-chromatography detection method of described benzotrichloride, comprises the steps:
(1) get industrial benzotrichloride sample and phenixin miscible according to the volume ratio of 1:1;
(2) condition of work of gas chromatograph is set:
Chromatographic column: AgilentDB-5 capillary column;
Post case temperature: 150 ~ 240 DEG C;
Injector temperature: 280 DEG C;
Detector temperature: 300 DEG C;
Chromatographic column flow rate of carrier gas: 1mL/min;
Air velocity: 300mL/min;
Hydrogen flow rate: 30mL/min;
Split ratio: 100:1;
(3) after baseline is steady, use automatic sampler sample introduction, start to detect and record chromatogram;
(4) utilize the integrating function of AgilentOpenLAB workstation, usable floor area normalization method calculates the content of benzotrichloride, replicate determination twice, and the difference of twice parallel determinations must not be greater than 0.1%.
Described post case temperature adopts temperature programme, initial temperature 150 DEG C, keeps 1min, is warmed up to 240 DEG C with the programming rate of 10 DEG C/min, keeps 5min.
Described uses automatic sampler sample introduction, and sample size is 0.6 μ L.
In gas chromatogram, the number percent of the area of the characteristic peak of benzotrichloride total area at all peaks after accounting for the solvent peak eliminated in this gas chromatogram, is the degree of testing sample benzotrichloride.
In described gas chromatogram, the defining method of the characteristic peak of benzotrichloride can adopt under identical chromatographic condition, the standard items of benzotrichloride are analyzed, thus under determining this condition, the retention time of benzotrichloride and characteristic peak, and by contrasting with the gas chromatogram of testing sample, obtain the characteristic peak of benzotrichloride in testing sample, and then determine its peak area.
By vapor-phase chromatography, twice replicate determination is carried out to industrial benzotrichloride, obtain the gas chromatogram of benzotrichloride, see Fig. 1 and Fig. 2, by workstation, the number percent of the total area at all peaks after adopting the area of area normalization method determination testing sample benzotrichloride characteristic peak to account for the solvent peak eliminated in this gas chromatogram.Analysis result after twice mensuration is in table 1 and table 2, first time, measurement result was as table 1: the retention time of benzotrichloride is 3.567, the peak area percentage composition of benzotrichloride reaches 99.6360%, second time measurement result is as table 2: the retention time of benzotrichloride is 3.560, and the peak area percentage composition of benzotrichloride reaches 99.6368%.
The analysis result table that table 1 first time measures
The analysis result table that table 2 second time measures
| Peak is numbered | Retention time | Peak area | Degree |
| 1 | 2.873 | 205358 | 0.0571 |
| 2 | 3.560 | 358297065 | 99.6368 |
| 3 | 3.767 | 269252 | 0.0749 |
| 4 | 4.530 | 476500 | 0.1300 |
| 5 | 4.947 | 202309 | 0.0563 |
| 6 | 9.117 | 81296 | 0.0226 |
| 7 | 11.600 | 80198 | 0.0223 |
| Amount to | 359602978 | 100 |
Adopt area normalization method to calculate the content of benzotrichloride, twice measured value of benzotrichloride compares as table 3.
Table 3 twice measured value comparison sheet
| Title | Detected value for the first time | Second time detected value | Mean value |
| Commercial production benzotrichloride | 99.6360 | 99.6368 | 99.6364 |
Conclusion:
Adopt retention time and the peak steady of each component of detection method of the present invention, reproducible, key component benzotrichloride is separated thoroughly, and degree of separation reaches more than 1.5, and content reaches more than 99.6%.
Claims (6)
1. a gas-chromatography detection method for benzotrichloride, is characterized in that: comprise the steps:
(1) testing sample is adopted dissolution with solvents;
(2) condition of work of gas chromatograph is set:
Chromatographic column: AgilentDB-5 capillary column;
Post case temperature: 150 ~ 240 DEG C;
Injector temperature: 280 DEG C;
Detector temperature: 300 DEG C;
Chromatographic column flow rate of carrier gas: 1mL/min;
Air velocity: 300mL/min;
Hydrogen flow rate: 30mL/min;
Split ratio: 100:1;
(3) use automatic sampler sample introduction, start to detect and record chromatogram;
(4) usable floor area normalization method calculates the content of benzotrichloride.
2. the gas-chromatography detection method of benzotrichloride according to claim 1, is characterized in that: described solvent is phenixin.
3. the gas-chromatography detection method of benzotrichloride according to claim 1, is characterized in that: described chromatogram column length is 30m, and bore is 0.32mm, and thickness is 0.25 μm.
4. the gas-chromatography detection method of benzotrichloride according to claim 1, is characterized in that: described detecting device is flame ionization ditector.
5. the gas-chromatography detection method of benzotrichloride according to claim 1, is characterized in that: described post case temperature adopts temperature programme, initial temperature 150 DEG C, keeps 1min, is warmed up to 240 DEG C with the programming rate of 10 DEG C/min, keeps 5min.
6. the gas-chromatography detection method of benzotrichloride according to claim 1, is characterized in that: described uses automatic sampler sample introduction, and sample size is 0.6 μ L.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106706806A (en) * | 2016-11-18 | 2017-05-24 | 韩超 | Ultrasonic extraction-gas chromatograph-mass spectrometer detection method for chlorotoluene organic pollutants in textiles |
| CN106770813A (en) * | 2016-11-18 | 2017-05-31 | 韩超 | The method that GC-MS determines chloromethane benzene-like compounds in leather simultaneously |
| CN108918706A (en) * | 2018-06-29 | 2018-11-30 | 江苏亿科检测技术服务有限公司 | The detection method of 2,4- bis- chloro- 1- (dichloromethyl) benzene in a kind of textile |
| CN111024830A (en) * | 2018-10-09 | 2020-04-17 | 江苏德旺化工工业有限公司 | Method for detecting organochlorine carrier in dye |
| CN111929369A (en) * | 2019-05-13 | 2020-11-13 | 定远县云森科技有限公司 | Method for measuring sulfur content in high-pressure sulfurized isobutylene by gas chromatography |
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| CN102866223A (en) * | 2012-09-14 | 2013-01-09 | 浙江出入境检验检疫局检验检疫技术中心 | Method for determining benzene and methylbenzene residue in nail polish by utilizing headspace-gas-chromatography mass spectrometry |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106706806A (en) * | 2016-11-18 | 2017-05-24 | 韩超 | Ultrasonic extraction-gas chromatograph-mass spectrometer detection method for chlorotoluene organic pollutants in textiles |
| CN106770813A (en) * | 2016-11-18 | 2017-05-31 | 韩超 | The method that GC-MS determines chloromethane benzene-like compounds in leather simultaneously |
| CN108918706A (en) * | 2018-06-29 | 2018-11-30 | 江苏亿科检测技术服务有限公司 | The detection method of 2,4- bis- chloro- 1- (dichloromethyl) benzene in a kind of textile |
| CN108918706B (en) * | 2018-06-29 | 2021-06-04 | 亿科检测认证有限公司 | Method for detecting 2, 4-dichloro-1- (dichloromethyl) benzene in textile |
| CN111024830A (en) * | 2018-10-09 | 2020-04-17 | 江苏德旺化工工业有限公司 | Method for detecting organochlorine carrier in dye |
| CN111929369A (en) * | 2019-05-13 | 2020-11-13 | 定远县云森科技有限公司 | Method for measuring sulfur content in high-pressure sulfurized isobutylene by gas chromatography |
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Application publication date: 20160406 |