CN109164199A - 3,4- dimethylbenzaldehyde contents and impurity determination method - Google Patents
3,4- dimethylbenzaldehyde contents and impurity determination method Download PDFInfo
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- CN109164199A CN109164199A CN201811065900.9A CN201811065900A CN109164199A CN 109164199 A CN109164199 A CN 109164199A CN 201811065900 A CN201811065900 A CN 201811065900A CN 109164199 A CN109164199 A CN 109164199A
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- Prior art keywords
- dimethylbenzaldehyde
- aldehyde
- main peak
- impurity
- determination method
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
One kind 3,4- dimethylbenzaldehyde content and impurity determination method, belong to organic matter detection technique field, substantially it is measured using gas chromatography, it is characterized in that: the measuring method includes: to take 3,4- dimethylbenzaldehyde test sample sample introduction 0.5ul records chromatogram, calculates content according to area normalization method.Method of the invention quick and precisely, can carry out quantitative analysis to 3,4- dimethylbenzaldehyde and impurity.
Description
Technical field
The present invention relates to one kind 3,4- dimethylbenzaldehyde content and impurity determination methods, belong to organic object detecting method skill
Art field.
Background technique
3.4- dimethylbenzaldehyde is widely used in the synthesis of the fine chemicals such as medicine, pesticide, fragrance, beverage, food,
In particular for synthesizing new transparent nucleator for polypropylene 3,4- dimethylbenzylidensorbitol is that the non-toxic plastic of a new generation helps
Agent is widely used in packaging material for food.
" non-pressure process of 3,4- dimethylbenzaldehydes synthesizes and characterization " (Tang Xiaofei, Feng Baicheng, Zhao Lijun " applying chemical industry " the
The phase of volume 42 the 12nd, in December, 2013) a kind of dimethylbenzaldehyde characterizing method is provided, use nmr spectrum and mass spectrum
Chart levies target product.
" progress of synthesis of 3,4- dimethylbenzaldehyde " (Wu Yulong etc. " Guangdong chemical industry " the 6th phase P34-35 in 2005)
The synthetic method of 3,4- dimethylbenzaldehyde is reviewed.
It according to the knowledge of the applicant and retrieves, does not find the record of 3,4- dimethylbenzaldehyde content and impurity determination method.
Summary of the invention
The present invention provides one kind 3,4- dimethylbenzaldehyde content and impurity determination method, provides 3,4- dimethyl for the first time
Benzaldehyde quantitative analysis method.
The present invention it is specific the technical solution adopted is that:
One kind 3,4- dimethylbenzaldehyde content and impurity determination method, are substantially measured using gas chromatography,
It is characterized in that: the measuring method includes:
3,4- dimethylbenzaldehyde test sample sample introduction 0.5ul is taken, chromatogram is recorded, is contained according to area normalization method calculating
Amount,
Calculation formula:
Wherein, A3.4- aldehyde main peak --- -3.4- aldehyde main peak area；
The total peak area of ∑ A---- chromatogram.
Further, the determination condition of the measuring method is:
Chromatographic condition:
Chromatographic column: 30m × 0.32mm, 1.8um, stationary phase: -94% dimethyl polysiloxane of 6% cyanogen propyl phenyl；
Column temperature:, keeping 3min by 70 DEG C, rises to 220 DEG C with 10 DEG C/min, keeps 12min,
Injection port: 220 DEG C,
Detector: FID, 240 DEG C,
Sample volume: 0.5ul,
Split ratio: 30:1,
Flow velocity: 2ml/min,
Appearance time: ortho-xylene about 9.3min, 2.4- aldehyde about 15.4min, 3.4- aldehyde about 15.7min, main peak is about
18.5min。
Compared with prior art, the invention has the advantages that
1) present invention can quantitative determine 3,4- dimethylbenzaldehyde and impurity；
2) method of the invention is quick and precisely.
Specific embodiment
It is measured using gas chromatography, step includes:
3,4- dimethylbenzaldehyde test sample sample introduction 0.5ul is taken, chromatogram is recorded, is contained according to area normalization method calculating
Amount,
Calculation formula:
Wherein, A3.4- aldehyde main peak --- -3.4- aldehyde main peak area；
The total peak area of ∑ A---- chromatogram.
Further, the determination condition of the measuring method is:
Chromatographic condition:
Chromatographic column: 30m × 0.32mm, 1.8um, stationary phase: -94% dimethyl polysiloxane of 6% cyanogen propyl phenyl；
Column temperature:, keeping 3min by 70 DEG C, rises to 220 DEG C with 10 DEG C/min, keeps 12min,
Injection port: 220 DEG C,
Detector: FID, 240 DEG C,
Sample volume: 0.5ul,
Split ratio: 30:1,
Flow velocity: 2ml/min,
Appearance time: ortho-xylene about 9.3min, 2.4- aldehyde about 15.4min, 3.4- aldehyde about 15.7min, main peak is about
18.5min。
Claims (2)
1. one kind 3,4- dimethylbenzaldehyde content and impurity determination method, are substantially measured using gas chromatography,
Be characterized in: the measuring method includes:
3,4- dimethylbenzaldehyde test sample sample introduction 0.5ul is taken, chromatogram is recorded, calculates content according to area normalization method,
Calculation formula:
Wherein, A3.4- aldehyde main peak --- -3.4- aldehyde main peak area；
The total peak area of ∑ A---- chromatogram.
2. 3,4- dimethylbenzaldehyde content according to claim 1 and impurity determination method, characterized in that the measurement
The determination condition of method is:
Chromatographic condition:
Chromatographic column: 30m × 0.32mm, 1.8um, stationary phase: -94% dimethyl polysiloxane of 6% cyanogen propyl phenyl；
Column temperature:, keeping 3min by 70 DEG C, rises to 220 DEG C with 10 DEG C/min, keeps 12min,
Injection port: 220 DEG C,
Detector: FID, 240 DEG C,
Sample volume: 0.5ul,
Split ratio: 30:1,
Flow velocity: 2ml/min,
Appearance time: ortho-xylene about 9.3min, 2.4- aldehyde about 15.4min, 3.4- aldehyde about 15.7min, main peak about 18.5min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811065900.9A CN109164199A (en) | 2018-09-13 | 2018-09-13 | 3,4- dimethylbenzaldehyde contents and impurity determination method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811065900.9A CN109164199A (en) | 2018-09-13 | 2018-09-13 | 3,4- dimethylbenzaldehyde contents and impurity determination method |
Publications (1)
| Publication Number | Publication Date |
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| CN109164199A true CN109164199A (en) | 2019-01-08 |
Family
ID=64894939
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811065900.9A Pending CN109164199A (en) | 2018-09-13 | 2018-09-13 | 3,4- dimethylbenzaldehyde contents and impurity determination method |
Country Status (1)
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5324702A (en) * | 1991-11-22 | 1994-06-28 | Amoco Corporation | Catalytic oxidation and oxidative dehydrogenation using metal-compound-loaded, deboronated hams-1b crystalline borosilicate molecular sieve compositions |
| US6156910A (en) * | 1997-12-26 | 2000-12-05 | Daicel Chemical Industries, Ltd. | ε-Caprolactone, process for producing the same, polycaprolactone obtained therefrom, and process for producing the polycaprolactone |
| CN1865211A (en) * | 2006-06-23 | 2006-11-22 | 江苏工业学院 | High purity 3,4-dimethyl benzaldehyde preparation method |
| CN101980997A (en) * | 2008-04-22 | 2011-02-23 | 三菱瓦斯化学株式会社 | Process for production of high-purity trimellitic acid |
| CN104020246A (en) * | 2014-06-24 | 2014-09-03 | 上海大学 | Method for simultaneously detecting plurality of volatile trace carbonyl compounds in atmosphere |
| CN106795326A (en) * | 2016-09-05 | 2017-05-31 | 呈和科技股份有限公司 | A kind of transparent nucleater composition comprising the acetal of sorbierite three and monoacetal |
-
2018
- 2018-09-13 CN CN201811065900.9A patent/CN109164199A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5324702A (en) * | 1991-11-22 | 1994-06-28 | Amoco Corporation | Catalytic oxidation and oxidative dehydrogenation using metal-compound-loaded, deboronated hams-1b crystalline borosilicate molecular sieve compositions |
| US6156910A (en) * | 1997-12-26 | 2000-12-05 | Daicel Chemical Industries, Ltd. | ε-Caprolactone, process for producing the same, polycaprolactone obtained therefrom, and process for producing the polycaprolactone |
| CN1865211A (en) * | 2006-06-23 | 2006-11-22 | 江苏工业学院 | High purity 3,4-dimethyl benzaldehyde preparation method |
| CN101980997A (en) * | 2008-04-22 | 2011-02-23 | 三菱瓦斯化学株式会社 | Process for production of high-purity trimellitic acid |
| CN104020246A (en) * | 2014-06-24 | 2014-09-03 | 上海大学 | Method for simultaneously detecting plurality of volatile trace carbonyl compounds in atmosphere |
| CN106795326A (en) * | 2016-09-05 | 2017-05-31 | 呈和科技股份有限公司 | A kind of transparent nucleater composition comprising the acetal of sorbierite three and monoacetal |
Non-Patent Citations (2)
| Title |
|---|
| 吴雨龙等: "CO羰基化合成3,4-二甲基苯甲醛的反应机理研究", 《广东化工》 * |
| 陈丹等: "色谱组合法分析对二甲苯氧化产物", 《石油化工》 * |
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Application publication date: 20190108 |