CN104237437A - Gas chromatography detection method of p-xylylene dichloride - Google Patents
Gas chromatography detection method of p-xylylene dichloride Download PDFInfo
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- CN104237437A CN104237437A CN201410487113.9A CN201410487113A CN104237437A CN 104237437 A CN104237437 A CN 104237437A CN 201410487113 A CN201410487113 A CN 201410487113A CN 104237437 A CN104237437 A CN 104237437A
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Abstract
The invention provides a gas chromatography detection method of p-xylylene dichloride. The method comprises the following steps: performing gas chromatographic analysis on a sample-to-be-detected solution to obtain a gas chromatogram of the sample-to-be-detected solution; calculating the purity of p-xylylene dichloride by an area normalization method through the integrating function of an N2,000 chromatographic working station, wherein the gas chromatography conditions are as follows: an Agilent DB-23 capillary chromatography column is 50 m*0.25 mm*0.50 mum in size, the temperature of a detection chamber is 235 DEG C, the temperature of a vaporizing chamber is 235 DEG C, and carrier gas is nitrogen. According to the method, an analytic result is accurate, the chromatogram is clearly analyzed, daily production schedule can be effectively guided, the production energy consumption is reduced, and the production cost is saved.
Description
Technical field:
The present invention relates to a kind of gas-chromatography detection method to benzyl dichloride.
Background technology:
Be used as organic synthesis intermediate to benzyl dichloride to have many uses, with benzyl dichloride being added to alkali synthesis terephthalyl alcohol; Terephthalaldehyde is synthesized with urotropine; With sodium methoxide Reactive Synthesis terephthaldehyde base dimethyl ether; With to benzyl dichloride for crosslinking chemical, synthesis polysulfone hollow fibre Nano filtering composite membrane; Kunming chemical institute synthesizes novel phenolic resin the earliest, and this resin is used for aviation electronics wiring board and smears, and also for high-abrasive material synthesis, may be used for manufacturing navigation motorboat material, domestic application amount is less.Domestic have certain use amount in synthesis on benzene benzyl ether, methothrin, Isosorbide-5-Nitrae-hexichol.Someone synthesis Luo Suoluo phenol sodium intermediate-on bromomethyl benzenpropanoic acid as initiation material, reaction process obviously reduces, and wastewater flow rate is also little.Also be widely used in dyestuff, sewage-treating agent synthesis in addition.
Owing to there is no national standard to the detection of benzyl dichloride, so have references to GB/T 6678-2003 chemical products sampling general provisions; GB/T 6680-2003 chemical products sampling general rule; After GB/T 9722-1988 chemical reagent vapor-phase chromatography general rule, our company has worked out the company standard be applicable to benzyl dichloride inspection.
Through long production practices and the analysis to chromatogram, find with DB-5 chromatographic column be difficult to material composition to carry out clear, analyze accurately, cause analysis result unstable, can not accurately instruct normal explained hereafter.So under the test in many ways of our company's person skilled and analyst, material composition clearly can be separated by discovery DB-23 chromatographic column on chromatogram, and reproducible.
Summary of the invention:
The object of the present invention is to provide a kind of gas-chromatography detection method to benzyl dichloride, the method not only analysis speed is fast, and detection sensitivity is high, and analysis result is accurate.
The invention provides a kind of gas-chromatography detection method to benzyl dichloride, comprise the steps:
(1) set instrument condition of work: post case temperature: 120-230 DEG C, temperature of vaporization chamber: 235 DEG C, sensing chamber's temperature: 235 DEG C, chromatogram rain glass sets: nitrogen: 0.08MPa, hydrogen: 0.04MPa, air: 0.12MPa; Flow rate of carrier gas: 35ml/min;
(2) sample introduction: use microsyringe sample introduction, starts to detect and records chromatogram;
(3) result characterizes: the integrating function utilizing N2000 chromatographic work station, usable floor area normalization method calculates the purity to benzyl dichloride.
The chromatographic column that described gas-chromatography detection method adopts is Agilent DB-23 capillary chromatographic column, and specification is: 50m × 0.25mm × 0.50 μm.
The detecting device that described gas-chromatography detection method adopts is flame ionization ditector.
Described post phase temperature adopts temperature programme, and programming rate is 15 DEG C/min.
The solvent of described testing sample solution is acetone.
Described testing sample is to the volume ratio 1:2 of benzyl dichloride and acetone.
Described microsyringe is 10 μ L microsyringes.
The split ratio of described gas-chromatography detection method: 1/30.
Testing sample is dissolved in acetone solvent to benzyl dichloride, carry out gas chromatographic analysis, to obtain the gas chromatogram of testing sample to benzyl dichloride, by analysis software, adopt area normalization method determine the area of the characteristic peak of p-dichlorobenzene 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.
The invention has the beneficial effects as follows: the method analysis speed is fast, result accurate, and spectrum analysis is clear, can effectively instruct daily scheduling of production, reduce to produce consuming, save production cost; Use Agilent DB-23 capillary chromatographic column instead, specification is: 50m × 0.25mm × 0.50 μm, and the appearance time of material and peak steady are reproducible.
Accompanying drawing illustrates:
Fig. 1 Fig. 2 is respectively the gas chromatogram of commercial production to twice test of benzyl dichloride sample.
Embodiment:
To a gas-chromatography detection method for benzyl dichloride, the method comprises the following steps
1, reagent and instrument
Reagent: industrial to benzyl dichloride, acetone (AR level).
Instrument: the capillary gas chromatograph of tape program intensification function; The computer of N2000 chromatographic work station is housed; 10 μ L microsyringes; Agilent DB-23 capillary chromatographic column, specification is: 50m × 0.25mm × 0.50 μm; Flame ionization ditector.
2, detecting step
(1) instrument condition of work is set: post case temperature: 120-230 DEG C; Temperature of vaporization chamber: 235 DEG C; Sensing chamber's temperature: 235 DEG C; Chromatogram rain glass sets: nitrogen: 0.08MPa, hydrogen: 0.04MPa, air: 0.12MPa;
(2) sample introduction: use microsyringe sample introduction, starts to detect and records chromatogram;
(3) result characterizes: the integrating function utilizing N2000 chromatographic work station, usable floor area normalization method calculates the purity to benzyl dichloride.
The chromatographic column that described gas-chromatography detection method adopts is Agilent DB-23 capillary chromatographic column, and specification is: 50m × 0.25mm × 0.50 μm.
The detecting device that described gas-chromatography detection method adopts is flame ionization ditector.
Described post phase temperature adopts temperature programme, and programming rate is 15 DEG C/min.
The solvent of described testing sample solution is acetone.
Described testing sample is to the volume ratio 1:2 of benzyl dichloride and acetone.
Described microsyringe is 10 μ L microsyringes.
The split ratio of described gas-chromatography detection method: 1/30.
Testing sample is dissolved in acetone solvent to benzyl dichloride, carry out gas chromatographic analysis, to obtain the gas chromatogram of testing sample to benzyl dichloride, by analysis software, the area of the characteristic peak of p-dichlorobenzene in described gas chromatogram accounts for the number percent of the total area at all peaks after the solvent peak eliminated in this gas chromatogram to adopt area normalization method to determine.This number percent is the percentage composition of testing sample to benzyl dichloride, namely to the purity of benzyl dichloride.Various method known in the field can be adopted to the defining method of the characteristic peak of benzyl dichloride in described gas chromatogram.Such as, can under identical chromatographic conditions, analyze to the standard items of benzyl dichloride, thus under determining this condition, to retention time and the characteristic peak of benzyl dichloride, and by carrying out contrasting the characteristic peak obtained to benzyl dichloride in testing sample with the gas chromatogram of testing sample, and then determine its peak area.
Embodiment 1
Commercial production is to the gas chromatographic analysis of benzyl dichloride: get industrial to benzyl dichloride sample and acetone miscible according to the volume ratio of 1:2.With reference to the condition of operating conditions setting gas chromatography, post case temperature: 120-230 DEG C, post case temperature adopts temperature programme, and step is as follows: initial temperature 120 DEG C, keeps 2 minutes, is warming up to 230 DEG C with the speed of 15 DEG C/min, and 230 DEG C keep 20 minutes; Temperature of vaporization chamber: 235 DEG C; Sensing chamber's temperature: 235 DEG C; Chromatogram rain glass sets: nitrogen: 0.08MPa, hydrogen: 0.04MPa, air: 0.12MPa; Split ratio: 1/30; Set the condition of gas chromatography, after baseline stability, with 10 μ L microsyringes from injection port sample introduction, sample size is 0.4 μ L, temperature programme to be done institute in steps after, the chromatogram utilizing workstation to generate and the integrating function of workstation, usable floor area normalization method calculates the purity to benzyl dichloride; Replicate determination twice, the difference of twice parallel determinations must not be greater than 0.1%.
Industrial to benzyl dichloride with vapor-phase chromatography replicate determination twice, obtain the gas chromatogram to benzyl dichloride, see accompanying drawing 1 and accompanying drawing 2, by analysis software, the area of the characteristic peak of area normalization method determination testing sample p-dichlorobenzene is adopted to account for the number percent of the total area at all peaks after the solvent peak eliminated in this gas chromatogram.Replicate determination twice, analysis result after twice mensuration is successively in table 1 and table 2, first time, measurement result was as table 1: be 5.515min to the retention time of benzyl dichloride, 99.3077% is reached to the peak area percentage composition of benzyl dichloride, second time measurement result is as table 2: be 5.552min to the retention time of benzyl dichloride, reach 99.3006% to the peak area percentage composition of benzyl dichloride.
Table 1 is analysis result first time measuring to benzyl dichloride gas chromatography:
| Peak number | Retention time (min) | Peak height | Peak area | Content (%) |
| 1 | 4.173 | 65.263 | 221.811 | 0.0409 |
| 2 | 4.357 | 31.895 | 77.626 | 0.0143 |
| 3 | 4.748 | 73.276 | 246.363 | 0.0454 |
| 4 | 4.923 | 269.105 | 1989.653 | 0.3666 |
| 5 | 5.365 | 44.625 | 115.000 | 0.0212 |
| 6 | 5.515 | 125679.672 | 539007.813 | 99.3077 |
| 7 | 6.448 | 457.947 | 1036.150 | 0.1909 |
| 8 | 6.607 | 30.800 | 71.100 | 0.0131 |
| Amount to | ? | 126652.584 | 542765.514 | 100.0000 |
Table 2 is the analysis result that second time measures to benzyl dichloride gas chromatography:
| Peak number | Retention time (min) | Peak height | Peak area | Content (% |
| 1 | 4.185 | 406.592 | 487.990 | 0.0662 |
| 2 | 4.373 | 136.243 | 315.250 | 0.0428 |
| 3 | 4.640 | 140.163 | 330.700 | 0.0449 |
| 4 | 4.93 | 327.478 | 2297.500 | 0.3119 |
| 5 | 5.385 | 31.784 | 56.750 | 0.0077 |
| 6 | 5.552 | 157922.844 | 731557.438 | 99.3006 |
| 7 | 6.467 | 760.360 | 1502.400 | 0.2039 |
| 8 | 6.623 | 78.609 | 161.700 | 0.0219 |
| Amount to | ? | 159804.074 | 736709.728 | 100.0000 |
Get in workstation the number percent that adopts the area of the characteristic peak of area normalization method determination testing sample p-dichlorobenzene to account for the total area at all peaks after the solvent peak eliminated in this gas chromatogram as to benzyl dichloride purity.To the comparison of benzyl dichloride twice measured value as table 3.Measured value is: the area of the characteristic peak of p-dichlorobenzene accounts for the number percent of the total area at all peaks after the solvent peak eliminated in this gas chromatogram, is used for representing that testing sample is to the purity of benzyl dichloride.
Table 3 is the comparison to benzyl dichloride twice measured value
Our company adopts appearance time and the peak steady of material after present chromatogram analysis method and chromatographic column, reproducible, and key component is separated thoroughly benzyl dichloride, and purity reaches more than 99.3%.
Claims (8)
1., to a gas-chromatography detection method for benzyl dichloride, it is characterized in that comprising the steps:
(1) instrument condition of work is set: post case temperature: 120-230 DEG C, temperature of vaporization chamber: 235 DEG C; Sensing chamber's temperature: 235 DEG C; Chromatogram rain glass sets: nitrogen: 0.08MPa, hydrogen: 0.04MPa, air: 0.12MPa; Flow rate of carrier gas: 35ml/min;
(2) sample introduction: use microsyringe sample introduction, starts to detect and records chromatogram;
(3) result characterizes: the integrating function utilizing N2000 chromatographic work station, usable floor area normalization method calculates the purity to benzyl dichloride.
2. a kind of gas-chromatography detection method to benzyl dichloride according to claim 1, is characterized in that: the chromatographic column that described gas-chromatography detection method adopts is Agilent DB-23 capillary chromatographic column, and specification is: 50m × 0.25mm × 0.50 μm.
3. a kind of gas-chromatography detection method to benzyl dichloride according to claim 1, is characterized in that: the detecting device that described gas-chromatography detection method adopts is flame ionization ditector.
4. a kind of gas-chromatography detection method to benzyl dichloride according to claim 1, is characterized in that: post phase temperature adopts temperature programme, and programming rate is 15 DEG C/min.
5. a kind of gas-chromatography detection method to benzyl dichloride according to claim 1, is characterized in that: the solvent of described testing sample solution is acetone.
6. a kind of gas-chromatography detection method to benzyl dichloride according to claim 1, is characterized in that: the volume ratio of described testing sample to benzyl dichloride and acetone is 1:2.
7. a kind of gas-chromatography detection method to benzyl dichloride according to claim 1, is characterized in that: described microsyringe is 10 μ L microsyringes.
8. a kind of gas-chromatography detection method to benzyl dichloride according to claim 1, is characterized in that: the split ratio of described gas-chromatography detection method: 1/30.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112345662A (en) * | 2020-10-22 | 2021-02-09 | 潜江新亿宏有机化工有限公司 | Purity detection method of m-methylbenzyl chloride |
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| US5552508A (en) * | 1992-07-01 | 1996-09-03 | University Of Michigan, The Board Of Regents | Difunctional bitricyclodecatriene monomers |
| US6270843B1 (en) * | 2000-03-27 | 2001-08-07 | Air Products And Chemicals, Inc. | Process for generating useful electrophiles from common anions and their application in electrophilic reactions with organic substrates |
| CN103288604A (en) * | 2013-05-27 | 2013-09-11 | 潜江新亿宏有机化工有限公司 | Novel process of 1,4-bis(methoxymethyl)-benzene preparation method |
| US20130317159A1 (en) * | 2012-05-22 | 2013-11-28 | Chevron Phillips Chemical Company Lp | Reinforced Poly(Arylene Sulfide) Compositions |
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2014
- 2014-09-22 CN CN201410487113.9A patent/CN104237437A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5552508A (en) * | 1992-07-01 | 1996-09-03 | University Of Michigan, The Board Of Regents | Difunctional bitricyclodecatriene monomers |
| US6270843B1 (en) * | 2000-03-27 | 2001-08-07 | Air Products And Chemicals, Inc. | Process for generating useful electrophiles from common anions and their application in electrophilic reactions with organic substrates |
| US20130317159A1 (en) * | 2012-05-22 | 2013-11-28 | Chevron Phillips Chemical Company Lp | Reinforced Poly(Arylene Sulfide) Compositions |
| CN103288604A (en) * | 2013-05-27 | 2013-09-11 | 潜江新亿宏有机化工有限公司 | Novel process of 1,4-bis(methoxymethyl)-benzene preparation method |
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| J.BERMEJO ET AL.: "CAPILLARY GAS CHROMATOGRAPHY OF CHLORO DERIVATIVES OF CHLORO DERIVATIVES OF 1,4-DIMETHYLBENZENE", 《JOURNAL OF CHROMATOGRAPHY》 * |
| J.BERMEJO ET AL.: "GAS CHROMATOGRAPHY OF DEUTERATED AND PROTIATED CHLORO DERIVATIVES OF 1,4-DIMETHYLBENZENE", 《JOURNAL OF CHROMATOGRAPHY》 * |
| 熊佳丽 等: "对二氯苄-聚乙烯咪唑型聚合离子液体的制备及对煤焦油中苯酚的吸附性能", 《高等学校化学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112345662A (en) * | 2020-10-22 | 2021-02-09 | 潜江新亿宏有机化工有限公司 | Purity detection method of m-methylbenzyl chloride |
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