CN101025407A - Analytical method for determining micro moisture in cyclopropyl amine by gas phase chromatography - Google Patents
Analytical method for determining micro moisture in cyclopropyl amine by gas phase chromatography Download PDFInfo
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- CN101025407A CN101025407A CN 200610007918 CN200610007918A CN101025407A CN 101025407 A CN101025407 A CN 101025407A CN 200610007918 CN200610007918 CN 200610007918 CN 200610007918 A CN200610007918 A CN 200610007918A CN 101025407 A CN101025407 A CN 101025407A
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- cyclopropylamine
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- propyl amine
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Abstract
The invention discloses a analyze method of measuring micro wet of cycle propyl amine, its chief process is that On a 5A molecular sieve suction treated with cycle propyl amine as the solvent, the 5A molecular sieve suction treated with anhydrous ethanol as internal standard substance, distilled water as the standard, water and ethanol made from different ratio to manufacture cycle propyl amine solution, in accordance with the measurement of the selected chromatogram conditions, it can reckon up the correction factor. When the invention measure sample, in a certain amount of cycle propyl amine, accurate enter a certain amount dehydrated alcohol internal standard substance by the dehydrated treatment, measure according to the selected chromatography conditions, by calculating it can obtain the analysis results of water in cycle propyl amine. The chromatographic analysis condition is: phi3*2000mm stainless steel packed column, inner filled GDX-201(80-100order); the column temperature is 100- 110deg.C; detecting temperature is 140-150deg.C; aerification temperature is 180-200deg.C; carrier gas: high pure hydrogen, flow rate is 25-30ml.min-1; former press of column is 0.02-0.03MPa; bridge current is 140-150mA; enter sample quantity is 1-3mul. The method is simple, applicable, rapid, accurate and can be used for product quality cycle propyl amine Detection.
Description
Technical field
The invention belongs to a kind of chromatogram analysis method, is the analytical approach with micro-moisture in the gas Chromatographic Determination cyclopropylamine product concretely.
Background technology
Cyclopropylamine is the fatty amine that contains three-membered ring, is a kind of important fine-chemical intermediate.Be widely used in fields such as medicine, agricultural chemicals, organic synthesis.In medicine, be mainly used in synthesizing new antibiotic Ciprofloxacin, Profloxacin, sparfloxacin, Enrofloxacin etc.; In pesticide industry, be used for chemical herbicides such as the synthetic ring third careless amine, cyprazine, ring third cyanogen Tianjin, propyl group methyl cyclopropylamine.Application prospect in this external organic synthesis is also very wide.Cyclopropylamine product requirement cyclopropylamine content is more than 99.0%, and moisture is below 0.1%.The content of micro-moisture is the important means of control product quality in the assay determination cyclopropylamine.The assay method of moisture is a lot of in the organism, and gravimetric method, karl Fischer method, vapor-phase chromatography are arranged, and for the analysis of micro-moisture in the organism, generally adopts karl Fischer method and vapor-phase chromatography.The karl Fischer method is with the minor amount of water quantitative reaction in karl Fischer reagent (solution that iodine, sulphuric dioxide, pyridine and methyl alcohol are formed) and the sample, comes micro-moisture in the working sample with the karl Fischer reagent of known water content then.This method complex operation, fixed to the advanced rower of karl Fischer reagent important affair, just carry out titrimetry then, and the difficult keeping of Ka Er reagent and poisonous, the time of assay determination sample is longer, and analysis result data repeatability is also not so good.And vapor-phase chromatography is easy, quick, accurate because of it, has obtained general application in the assay determination of organism micro-moisture.Domestic production producer adopts karl Fischer method and gas chromatography normalization method substantially to the assay determination of micro-moisture in the cyclopropylamine at present.The gas chromatography normalization method just can draw measurement result after requiring all components all to go out the peak, and it is longer to expend time in, and is unfavorable for the quick monitoring of product quality.The condition of normalization method is that analysis result was more accurate when content differed not very big between component simultaneously.Because cyclopropylamine and moisture differ greatly in the cyclopropylamine product, are difficult to accurately measure the content of micro-moisture in the cyclopropylamine with normalization method.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of chromatogram analysis method of measuring micro-moisture content in the cyclopropylamine.
Technical matters of the present invention is solved by following scheme: the analytical approach of micro-moisture in a kind of gas Chromatographic Determination cyclopropylamine, it is characterized in that: with the cyclopropylamine through 5A molecular sieve suction processing is solvent, the absolute ethyl alcohol of handling through the suction of 5A molecular sieve is an internal standard compound, distilled water is reference material, make water and ethanol than different cyclopropylamine solution, determine the result according to selected chromatographic condition, go out correction factor according to data computation then
During each mensuration, get in a certain amount of cyclopropylamine sample, accurately adding a certain amount of absolute ethyl alcohol of handling through the suction of 5A molecular sieve is internal standard compound, measure by selected chromatographic condition, the data that draw through gas Chromatographic Determination by the cyclopropylamine sample that adds internal standard compound, calculate the analysis result that can draw moisture in the cyclopropylamine through following formula, the analysis result of moisture in the cyclopropylamine:
In the formula: As is the peak area of internal standard compound; A
RPeak area for tester; Cs is the concentration of internal standard compound; C
RConcentration for tester; Ax is the peak area of specimen; Cx is the concentration of specimen; f
nBe the single calibration factor;
Be the average correction factor.The condition that stratographic analysis is used is: Ф 3 * 2000mm stainless steel packed column, interior filling GDX-201 (80～100 order); 100～110 ℃ of column temperatures; Thermal conductivity detector (TCD); 140～150 ℃ of detected temperatures; 180～200 ℃ of gasification temperatures; Carrier gas: High Purity Hydrogen, flow velocity 25～30mlmin
-1Press 0.02～0.03Mpa before the post; Bridge electric current 140～150mA; Sample size 1～3 μ l.
Advantage of the present invention is: the present invention has overcome normalization method needs all components such as long period all to go out the shortcoming that the peak just can draw measurement result, complete as long as water peak and ethanol peak go out the peak in the mensuration process, needn't wait main content cyclopropylamine to go out the peak, can adopt internal standard method to carry out quantitative test, realize measuring the purpose of micro-moisture in the cyclopropylamine.And internal standard method also can to offset stability of instrument poor, the quantitative test error that reason such as sample size is not accurate enough is brought.This method is easy, suitable, quick, accurate, can be used for the detection of product quality in the cyclopropylamine production.
Embodiment
1 instrument, reagent, sample
Gas chromatograph, thermal conductivity detector (TCD), data processing work station; GDX-201 (80～100 order); Distilled water is made reference material; Absolute ethyl alcohol (AR) is made internal standard compound; The 5A molecular sieve; The cyclopropylamine sample.
2 chromatographic run conditions
Chromatographic column: Ф 3 * 2000mm stainless steel packed column, interior filling GDX-201 (80～100 order); 100 ℃ of column temperatures; 150 ℃ of detected temperatures; 200 ℃ of gasification temperatures; Carrier gas: High Purity Hydrogen, flow velocity 25～30mlmin
-1Press 0.02Mpa before the post; Bridge electric current 150mA; Sample size 2 μ l.
3 experimental techniques
The absolute ethyl alcohol of handling through the suction of 5A molecular sieve is an internal standard compound, distilled water is reference material, and the cyclopropylamine of handling through 5A molecular sieve suction is a solvent, makes moisture and ethanol ratio and be 1: 4～4: 1 cyclopropylamine solution, measure liquid as measuring correction factor, measure by selected chromatographic condition.
Get in a certain amount of cyclopropylamine sample, accurately adding a certain amount of absolute ethyl alcohol of handling through 5A molecular sieve suction is internal standard compound, shakes up, and measures by selected chromatographic condition.
4 measurement results are calculated
Measure the data that liquid draws through gas Chromatographic Determination by correction factor, calculate the correction factor that each measures liquid, calculate the mean value of correction factor then according to following formula.
Correction factor calculates:
By the data that the cyclopropylamine sample that adds internal standard compound draws through gas Chromatographic Determination, calculate the analysis result that can draw moisture in the cyclopropylamine through following formula.The analysis result of moisture in the cyclopropylamine:
In following formula: As is the peak area of internal standard compound; A
RPeak area for tester; Cs is the concentration of internal standard compound; C
RConcentration for tester; Ax is the peak area of specimen; Cx is the concentration of specimen; f
nBe the single calibration factor;
Be the average correction factor.
5 chromatographic peak peak sequences
The cyclopropylamine sample under selected chromatographic condition, through gas Chromatographic Determination draw chromatogram result.Peak sequence is water (1.06min), ethanol (3.24min), cyclopropylamine (5.18min), and visible separating effect on the GDX-201 post is better.Do the requirement that internal standard compound can satisfy internal standard method with ethanol.And before not going out the peak, cyclopropylamine can carry out quantitative test.
6 sample analysis results
3 samples of cyclopropylamine have been carried out 5 times respectively measured, analysis result sees Table 1.Result's relative standard deviation is 2.94～4.01%.
Moisture analysis result (%) in the table 1. cyclopropylamine sample
| Sample number into spectrum | Analysis result | Mean value | Relative standard deviation | ||||
| 1 | 0.0912 | 0.0883 | 0.0856 | 0.0920 | 0.0878 | 0.0890 | 2.94 |
| 2 | 0.0984 | 0.0952 | 0.0976 | 0.0921 | 0.1026 | 0.0972 | 4.01 |
| 3 | 0.0998 | 0.1003 | 0.0966 | 0.1058 | 0.0965 | 0.0998 | 3.79 |
The experiment of 7 recovery
Accurately add the distilled water of different amounts respectively in the cyclopropylamine sample, carry out stratographic analysis then, calculate the recovery that adds distilled water by the gained measurement result, measurement result is as shown in table 2.The recovery is 97.60～103.3%.
Table 2. determination of recovery rates result (%)
| Sample number into spectrum | Moisture in the sample | Add the water yield in the sample | Record water inventory | The recovery |
| 1 | 0.089Q | 0.0500 | 0.1378 | 97.60 |
| 2 | 0.0972 | 0.1000 | 0.2005 | 103.3 |
| 3 | 0.0998 | 0.0500 | 0.1492 | 98.87 |
Claims (1)
1, the analytical approach of micro-moisture in a kind of gas Chromatographic Determination cyclopropylamine, it is characterized in that: with the cyclopropylamine through 5A molecular sieve suction processing is solvent, the absolute ethyl alcohol of handling through the suction of 5A molecular sieve is an internal standard compound, distilled water is reference material, make water and ethanol than different cyclopropylamine solution, determine the result according to selected chromatographic condition, calculate correction factor.During each mensuration, get in a certain amount of cyclopropylamine sample, accurately add a certain amount of absolute ethyl alcohol internal standard compound of handling through the suction of 5A molecular sieve, measure by selected chromatographic condition, the data that draw through gas Chromatographic Determination by the cyclopropylamine sample that adds internal standard compound, can draw the analysis result of moisture in the cyclopropylamine as calculated, the condition that stratographic analysis is used is: Φ 3 * 2000mm stainless steel packed column, interior filling GDX-201 (80～100 order); 100～110 ℃ of column temperatures; Thermal conductivity detector (TCD); 140～150 ℃ of detected temperatures; 180～200 ℃ of gasification temperatures; Carrier gas: High Purity Hydrogen, flow velocity 25～30mlmin
-1Press 0.02～0.03Mpa before the post; Bridge electric current 140～150mA; Sample size 1～3 μ l.
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| CN 200610007918 CN101025407A (en) | 2006-02-23 | 2006-02-23 | Analytical method for determining micro moisture in cyclopropyl amine by gas phase chromatography |
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| CN 200610007918 CN101025407A (en) | 2006-02-23 | 2006-02-23 | Analytical method for determining micro moisture in cyclopropyl amine by gas phase chromatography |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102087253A (en) * | 2010-12-31 | 2011-06-08 | 广东中烟工业有限责任公司 | Method for determining content of free water in tobaccos |
| CN107179377A (en) * | 2017-05-23 | 2017-09-19 | 深圳职业技术学院 | The assay method of micro-moisture in organic solvent sample |
| CN108760905A (en) * | 2018-04-10 | 2018-11-06 | 广西壮族自治区柳州食品药品检验所 | A kind of method of moisture in measurement antibiotic |
| CN111921503A (en) * | 2020-07-16 | 2020-11-13 | 中国神华煤制油化工有限公司 | Application of divinylbenzene-trichloroethylene copolymer in determining water content of pentanal and method for determining water content of pentanal |
-
2006
- 2006-02-23 CN CN 200610007918 patent/CN101025407A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102087253A (en) * | 2010-12-31 | 2011-06-08 | 广东中烟工业有限责任公司 | Method for determining content of free water in tobaccos |
| CN102087253B (en) * | 2010-12-31 | 2013-06-12 | 广东中烟工业有限责任公司 | Method for determining content of free water in tobaccos |
| CN107179377A (en) * | 2017-05-23 | 2017-09-19 | 深圳职业技术学院 | The assay method of micro-moisture in organic solvent sample |
| CN108760905A (en) * | 2018-04-10 | 2018-11-06 | 广西壮族自治区柳州食品药品检验所 | A kind of method of moisture in measurement antibiotic |
| CN111921503A (en) * | 2020-07-16 | 2020-11-13 | 中国神华煤制油化工有限公司 | Application of divinylbenzene-trichloroethylene copolymer in determining water content of pentanal and method for determining water content of pentanal |
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