CN105158384A - Gas chromatography examination method of 4-ethoxy-2,3-difluorobenzene - Google Patents
Gas chromatography examination method of 4-ethoxy-2,3-difluorobenzene Download PDFInfo
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- CN105158384A CN105158384A CN201510404315.7A CN201510404315A CN105158384A CN 105158384 A CN105158384 A CN 105158384A CN 201510404315 A CN201510404315 A CN 201510404315A CN 105158384 A CN105158384 A CN 105158384A
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- ethoxy
- difluorobenzene
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- AVOGLGBKOFOSBN-UHFFFAOYSA-N 1-ethoxy-2,3-difluorobenzene Chemical compound CCOC1=CC=CC(F)=C1F AVOGLGBKOFOSBN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000010606 normalization Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 14
- 238000007689 inspection Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 238000002347 injection Methods 0.000 abstract description 2
- 239000007924 injection Substances 0.000 abstract description 2
- 230000010354 integration Effects 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 11
- 239000000203 mixture Substances 0.000 description 8
- 230000014759 maintenance of location Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000003822 preparative gas chromatography Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- VUCWHNVRSUUSKP-UHFFFAOYSA-N 1-ethoxy-2,3-difluoro-4-nitrobenzene Chemical compound C1(N(=O)=O)=C(F)C(F)=C(OCC)C=C1 VUCWHNVRSUUSKP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
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Abstract
The invention discloses a gas chromatography examination method of 4-ethoxy-2,3-difluorobenzene, and relates to the technical field of chemical analysis. The method comprises the following steps: setting the heating program of a column oven, the temperature of an injection port, the temperature of a detector, the flow of a chromatographic column and the gas flow of a chromatograph, introducing a sample, and calculating the purity of 4-ethoxy-2,3-difluorobenzene through an area normalization technique by using the integration function of an Agilent ChemStation chromatographic workstation. The temperature of the column oven adopts temperature programming, and two step temperature programming is adopted, so the analysis speed is fast, the analysis result is accurate, the production consumption is reduced, and the production cost is saved; and when an Agilent HP-5 capillary chromatographic column is used, the peak appearance time and the peak value of a material are stable, and the repeatability is good.
Description
Technical field:
The present invention relates to chemical analysis technology field, be specifically related to a kind of gas chromatography method of inspection of 4-ethoxy-2,3-difluorobenzene.
Background technology:
4-ethoxy-2,3-difluorobenzene is a kind of conventional industrial chemicals, makes the negative liquid crystal material of the display screen such as televisor, mobile phone for liquid crystal intermediates.Lcd technology is one of main display mode of flat display field, and it is widely used at various display terminal.Therefore along with the development of lcd technology, more and more urgent to the requirement of researching and developing novel liquid crystal material.The preparation method of domestic disclosed 4-ethoxy-2,3-difluorobenzene: be by 4-ethoxy-2,3-difluoro nitrobenzene, obtain through hydrogenation reduction, diazo-reaction, concentrated and distillation.
Because the detection of 4-ethoxy-2,3-difluorobenzene does not have national standard, so have references to GB/T6678-2003 chemical products sampling general provisions; GB/T6680-2003 chemical products sampling general rule; After GB/T9722-1988 chemical reagent vapor-phase chromatography general rule, our company has worked out the company standard of applicable 4-ethoxy-2,3-difluorobenzene inspection.
Through long production practices and the analysis to chromatogram, find with DB-1 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 HP-5 chromatographic column on chromatogram, and reproducible.
Summary of the invention:
Technical matters to be solved by this invention is to provide that a kind of analysis speed is fast, detection sensitivity is high and the gas chromatography method of inspection of analysis result 4-ethoxy-2,3-difluorobenzene accurately.
Technical matters to be solved by this invention adopts following technical scheme to realize:
A kind of gas chromatography method of inspection of 4-ethoxy-2,3-difluorobenzene, comprises the steps:
(1) set instrument condition of work: column temperature rise program: 100 DEG C keep 1min, 10 DEG C/min heating rate, be warming up to 150 DEG C and keep 1min, then with 20 DEG C/min heating rate, be warming up to 280 DEG C and keep 5min; Injector temperature: 250 DEG C; Detector temperature: 280 DEG C; Column flow rate: 1.0ml/min; Chromatogram gas flow sets: hydrogen: 30ml/min, air: 300ml/min; Flow rate of carrier gas: 25ml/min;
(2) sample introduction: use microsyringe sample introduction, starts to detect and records chromatogram;
(3) result characterizes: the integrating function of Agilent ChemStation chromatographic work station, usable floor area normalization method calculates the purity of 4-ethoxy-2,3-difluorobenzene.
Described chromatographic column adopts Agilent HP-5 capillary chromatographic column, and specification is 30m × 0.32mm × 0.25 μm, and split ratio is 50/1.
Described detecting device is flame ionization ditector.
Described microsyringe is 10 μ L microsyringes.
Described sample size is 0.2 μ L.
Principle of work of the present invention:
Under identical chromatographic conditions, first to 4-ethoxy-2, the standard items of 3-difluorobenzene are analyzed, thus 4-ethoxy-2 under determining this condition, the retention time of 3-difluorobenzene and characteristic peak, then to testing sample 4-ethoxy-2,3-difluorobenzene, carry out gas chromatographic analysis, to obtain the gas chromatogram of testing sample 4-ethoxy-2,3-difluorobenzene, by analysis software, area normalization method is adopted to determine that the area of the characteristic peak of 4-ethoxy-2,3-difluorobenzene in described gas chromatogram accounts for the number percent of the total area at all peaks.This number percent is the percentage composition of testing sample 4-ethoxy-2,3-difluorobenzene, i.e. the purity of 4-ethoxy-2,3-difluorobenzene.
The invention has the beneficial effects as follows: the case temperature of post of the present invention adopts temperature programme, and adopts second order heating schedule, and analysis speed is fast, result is accurate, and spectrum analysis is clear, reduce to produce consuming, save production cost; Use Agilent HP-5 capillary chromatographic column instead, specification is: 30m × 0.32mm × 0.25 μm, and the appearance time of material and peak steady are reproducible.
Accompanying drawing illustrates:
Fig. 1-4 is the gas chromatogram of continuous 4 tests of the present invention.
Embodiment:
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with specific embodiment and diagram, setting forth the present invention further.
1, reagent and instrument
Reagent: industrial 4-ethoxy-2,3-difluorobenzene.
Instrument: Agilent 7820A gas chromatograph; The computer of ChemStation workstation is housed;
10 μ L microsyringes; Agilent HP-5 capillary chromatographic column, specification is: 30m × 0.32mm × 0.25 μm; Flame ionization ditector.
2, detecting step
(1) set instrument condition of work: column temperature rise program: 100 DEG C keep 1min, 10 DEG C/min heating rate, be warming up to 150 DEG C and keep 1min, then with 20 DEG C/min heating rate, be warming up to 280 DEG C and keep 5min; Injector temperature: 250 DEG C; Flame ionization ditector temperature: 280 DEG C; Column flow rate: 1.0ml/min; Chromatogram gas flow sets: hydrogen: 30ml/min, air: 300ml/min; Flow rate of carrier gas: 25ml/min;
(2) sample introduction: with microsyringe sample introduction 0.2 μ L, start to detect and record chromatogram;
(3) result characterizes: the integrating function of Agilent ChemStation chromatographic work station, usable floor area normalization method calculates the purity of 4-ethoxy-2,3-difluorobenzene.
Wherein, chromatographic column adopts Agilent HP-5 capillary chromatographic column, and specification is 30m × 0.32mm × 0.25 μm, and split ratio is 50/1.
Under identical chromatographic conditions, first to 4-ethoxy-2, the standard items of 3-difluorobenzene are analyzed, thus 4-ethoxy-2 under determining this condition, the retention time of 3-difluorobenzene and characteristic peak, then to testing sample 4-ethoxy-2,3-difluorobenzene, carry out gas chromatographic analysis, to obtain the gas chromatogram of testing sample 4-ethoxy-2,3-difluorobenzene, by ChemStation analysis software, area normalization method is adopted to determine that the area of the characteristic peak of 4-ethoxy-2,3-difluorobenzene in described gas chromatogram accounts for the number percent of the total area at all peaks.This number percent is the percentage composition of testing sample 4-ethoxy-2,3-difluorobenzene, i.e. the purity of 4-ethoxy-2,3-difluorobenzene.
Embodiment 1
The gas chromatographic analysis of commercial production 4-ethoxy-2,3-difluorobenzene: get industrial 4-ethoxy-2,3-difluorobenzene sample.With reference to the condition of operating conditions setting gas chromatography, column temperature rise program: 100 DEG C keep 1min, 10 DEG C/min heating rate, is warming up to 150 DEG C and keeps 1min, then with 20 DEG C/min heating rate, is warming up to 280 DEG C and keeps 5min; Injector temperature: 250 DEG C; Detector temperature: 280 DEG C; Column flow rate: 1.0ml/min; Chromatogram gas flow sets: hydrogen: 30ml/min, air: 300ml/min; Flow rate of carrier gas: 25ml/min; Split ratio: 50/1; Set the condition of gas chromatography, after baseline stability, with 10 μ L microsyringes from injection port sample introduction, sample size is 0.2 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 of 4-ethoxy-2,3-difluorobenzene; Replicate determination 4 times, the difference of any twice parallel determinations must not be greater than 0.1%, and the relative standard deviation (RSD) of 4 results must not be greater than 1.0%.
With vapor-phase chromatography replicate determination 4 industrial 4-ethoxys-2,3-difluorobenzene, obtain 4-ethoxy-2, the gas chromatogram of 3-difluorobenzene, see accompanying drawing 1-4, by ChemStation analysis software, the area of the characteristic peak of area normalization method determination testing sample 4-ethoxy-2,3-difluorobenzene is adopted to account for the number percent of the total area at all peaks.Replicate determination 4 times, analysis result after measuring for 4 times is successively in Table 1-4, first time, measurement result was as table 1:4-ethoxy-2, the retention time of 3-difluorobenzene is 4.328min, 4-ethoxy-2, the peak area percentage composition of 3-difluorobenzene reaches 99.46917%, second time measurement result is as table 2:4-ethoxy-2, the retention time of 3-difluorobenzene is 4.326min, 4-ethoxy-2, 3-difluorobenzene peak area percentage composition reaches 99.47782%, third time, measurement result was as table 3:4-ethoxy-2, the retention time of 3-difluorobenzene is 4.323min, 4-ethoxy-2, 3-difluorobenzene peak area percentage composition reaches 99.48070%, 4th measurement result is as table 4:4-ethoxy-2, the retention time of 3-difluorobenzene is 4.318min, 4-ethoxy-2, 3-difluorobenzene peak area percentage composition reaches 99.48719%.
The analysis result of table 1 first time mensuration 4-ethoxy-2,3-difluorobenzene gas chromatography
Table 2 second time measures the analysis result of 4-ethoxy-2,3-difluorobenzene gas chromatography
The analysis result of table 3 third time mensuration 4-ethoxy-2,3-difluorobenzene gas chromatography
Table 4 measures the analysis result of 4-ethoxy-2,3-difluorobenzene gas chromatography for the 4th time
Get in workstation the purity that the number percent adopting the area of the characteristic peak of area normalization method determination testing sample 4-ethoxy-2,3-difluorobenzene to account for the total area at all peaks does 4-ethoxy-2,3-difluorobenzene.4-ethoxy-2,3-difluorobenzene four measured values are compared as table 5.Measured value is: the area of the characteristic peak of 4-ethoxy-2,3-difluorobenzene accounts for the number percent of the total area at all peaks, is used for representing the purity of testing sample 4-ethoxy-2,3-difluorobenzene.
The comparison of table 54-ethoxy-2,3-difluorobenzene four measured values
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 4-ethoxy-2,3-difluorobenzene, and purity reaches 99.5%.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and instructions just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (5)
1. the gas chromatography method of inspection of 4-ethoxy-2, a 3-difluorobenzene, is characterized in that, comprise the steps:
(1) set instrument condition of work: column temperature rise program: 100 DEG C keep 1min, 10 DEG C/min heating rate, be warming up to 150 DEG C and keep 1min, then with 20 DEG C/min heating rate, be warming up to 280 DEG C and keep 5min; Injector temperature: 250 DEG C; Detector temperature: 280 DEG C; Column flow rate: 1.0ml/min; Chromatogram gas flow sets: hydrogen: 30ml/min, air: 300ml/min; Flow rate of carrier gas: 25ml/min;
(2) sample introduction: use microsyringe sample introduction, starts to detect and records chromatogram;
(3) result characterizes: the integrating function of Agilent ChemStation chromatographic work station, usable floor area normalization method calculates the purity of 4-ethoxy-2,3-difluorobenzene.
2. the gas chromatography method of inspection of 4-ethoxy-2,3-difluorobenzene according to claim 1, is characterized in that: described chromatographic column adopts Agilent HP-5 capillary chromatographic column, and specification is 30m × 0.32mm × 0.25 μm, and split ratio is 50/1.
3. the gas chromatography method of inspection of 4-ethoxy-2,3-difluorobenzene according to claim 1, is characterized in that: described detecting device is flame ionization ditector.
4. the gas chromatography method of inspection of 4-ethoxy-2,3-difluorobenzene according to claim 1, is characterized in that: described microsyringe is 10 μ L microsyringes.
5. the gas chromatography method of inspection of 4-ethoxy-2,3-difluorobenzene according to claim 1, is characterized in that: described sample size is 0.2 μ L.
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| CN201510404315.7A CN105158384B (en) | 2015-07-09 | 2015-07-09 | A kind of gas chromatogram method of inspection of 4-ethyoxyl-2,3-difluorobenzene |
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| CN201510404315.7A CN105158384B (en) | 2015-07-09 | 2015-07-09 | A kind of gas chromatogram method of inspection of 4-ethyoxyl-2,3-difluorobenzene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105842354A (en) * | 2016-03-18 | 2016-08-10 | 蚌埠市产品质量监督检测中心 | 3,4,5-trifluorobromobenzene gas chromatography detection method |
| 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 |
-
2015
- 2015-07-09 CN CN201510404315.7A patent/CN105158384B/en active Active
Non-Patent Citations (3)
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| 尚洪勇 等: "多氟二苯乙炔类负性液晶化合物的合成", 《液晶与显示》 * |
| 王平 等: "1-溴-4-乙氧基-2, 3-二氟苯的合成", 《应用化工》 * |
| 高丰琴 等: "4-乙氧基-2，3-二氟苯乙酸的合成及副产物研究", 《精细化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105842354A (en) * | 2016-03-18 | 2016-08-10 | 蚌埠市产品质量监督检测中心 | 3,4,5-trifluorobromobenzene gas chromatography detection method |
| 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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Denomination of invention: Gas chromatography examination method of 4-ethoxy-2,3-difluorobenzene Effective date of registration: 20170728 Granted publication date: 20161026 Pledgee: Bengbu financing guarantee Group Co., Ltd. Pledgor: China Synchem Technology Co., Ltd. Registration number: 2017340000130 |
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Denomination of invention: Gas chromatography examination method of 4-ethoxy-2,3-difluorobenzene Effective date of registration: 20191008 Granted publication date: 20161026 Pledgee: CITIC Bank Limited by Share Ltd Bengbu branch Pledgor: China Synchem Technology Co., Ltd. Registration number: Y2019340000102 |
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