CN104459020A - Method for detecting content of 1-chloroformyl-3-mesyl-2-imidazolidone - Google Patents
Method for detecting content of 1-chloroformyl-3-mesyl-2-imidazolidone Download PDFInfo
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- CN104459020A CN104459020A CN201410778224.5A CN201410778224A CN104459020A CN 104459020 A CN104459020 A CN 104459020A CN 201410778224 A CN201410778224 A CN 201410778224A CN 104459020 A CN104459020 A CN 104459020A
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Abstract
The invention relates to a detection method and specifically relates to a method for detecting the content of 1-chloroformyl-3-mesyl-2-imidazolidone. The method comprises the following steps: firstly, preparing a sample solution and a blank sample solution, next, preparing a standard solution, and testing an electrode after cleaning and correction; dropwise adding AgNO3 to the sample solution, and when the potential of the electrode is 0, recording the volume of the AgNO3 added so far, namely the volume for a test sample to consume; dropwise adding AgNO3 to the blank sample solution, and when the potential of the electrode is 0, recording the volume of the AgNO3 added so far, namely the volume for the blank sample to consume; next, calculating the content of the 1-chloroformyl-3-mesyl-2-imidazolidone. The method for detecting the content of the 1-chloroformyl-3-mesyl-2-imidazolidone is simple to operate, high in accuracy, capable of reducing the errors of subjective color determination terminal points, and good in depth of parallelism; besides, the use of a color developing agent is reduced.
Description
Technical field
The present invention relates to a kind of detection method, be specifically related to a kind of 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content.
Background technology
1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone is the necessary important intermediate in synthesis mezlocillin.In recent years along with the quick growth in microbiotic market, the demand of 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone also rapidly increases thereupon.How its content of Accurate Determining also seems particularly important.
Current 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content is mainly back titration.Back titration principle: containing in the salpeter solution of halogen atom, adding a certain amount of excessive silver nitrate, take ferriammonium sulfate as indicator, with the silver nitrate that sulphur cyanamide standard solution back titration is excessive.The defect existed: the judgement of titration end-point judges terminal with color, there is malobservation, and namely the judgement of titration end-point varies with each individual, and cause result to occur deviation, the depth of parallelism is poor.
Summary of the invention
For the deficiencies in the prior art, the object of this invention is to provide a kind of 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content, simple to operate, accuracy is high, reduce the error that subjectivity color judges terminal, the depth of parallelism is good; Reduce the use of developer.
1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content of the present invention, comprises the following steps:
(1) take test sample, add 1mol/L alcohol KOH solution, then add the HNO of 6mol/L
3after obtain sample solution; By 1mol/L alcohol KOH solution, add the HNO of 6mol/L
3after obtain blank sample solution;
(2) standard solution preparation
Take 7.45g potassium chloride, add in 100mL volumetric flask and use distilled water constant volume, accurately measure this solution 1mL, use distilled water constant volume in 10mL, 100mL, 1000mL volumetric flask respectively, be numbered 1,2, No. 3 solution respectively; Then from No. 3 solution, accurately measure 1mL, use distilled water constant volume in 10mL, 100mL, 1000mL volumetric flask respectively, be numbered 4,5, No. 6 solution respectively, 1 ~ No. 6 solution is for subsequent use as standard solution;
(3) electrode clean
By chlorine ion electrode together with contrast electrode, cleaning electrode current potential in deionized water;
(4) electrode alignment
To go forward side by side line item at 1 ~ No. 6 solution testing electrode potential;
(5) potential measurement
By in the sample solution in electrode insertion step (1), drip AgNO
3, when electrode potential is 0, stop dripping, and record the AgNO now dripped
3volume, be for sample consume AgNO
3volume; By in the blank sample solution in electrode insertion step (1), drip AgNO
3, when electrode potential is 0, stop dripping, and record the AgNO now dripped
3volume, be that blank sample consumes AgNO
3volume;
(6) 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone cubage
Content=C (V
sample-V
empty) M/W × 100%
C is AgNO
3concentration, V
samplefor consuming AgNO for sample
3volume, V
emptyfor blank sample consumes AgNO
3volume, M is the relative molecular mass of chloroformyl thing, and W is the quality of test sample.
Wherein:
Step (1) is: take test sample 0.20g, adds 1mol/L alcohol KOH solution 100mL, adds hot reflux 1 hour, puts to 25 DEG C, add the HNO of 6mol/L
3sample solution is obtained after 10mL; By 1mol/L alcohol KOH solution 100mL, add hot reflux 1 hour, put to 25 DEG C, add the HNO of 6mol/L
3blank sample solution is obtained after 10mL.
Step (3) is by chlorine ion electrode together with contrast electrode, uses magnetic stirring apparatus cleaning electrode current potential in deionized water, and during solution temperature 25 DEG C, cleaning current potential is at-115 ~-105mV.
The AgNO dripped in step (5)
3concentration is 0.1mol/L.
The present invention has the following advantages:
(1) the present invention is simple to operate, accuracy is high, can reduce the error that subjectivity color judges terminal,
(2) depth of parallelism of the present invention good (same sample, relative deviation≤0.15%); And decrease the use of developer.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment
A kind of 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content:
(1) take test sample 0.20g, add 1mol/L alcohol KOH solution 100mL, add hot reflux 1 hour, put to 25 DEG C, add the HNO of 6mol/L
3sample solution is obtained after 10mL; By 1mol/L alcohol KOH solution 100mL, add hot reflux 1 hour, put to 25 DEG C, add the HNO of 6mol/L
3blank sample solution is obtained after 10mL.Same batch sample configures three parts, is respectively sample 1, sample 2 and sample 3.
(2) standard solution preparation
Take 7.45g potassium chloride, add in 100mL volumetric flask and use distilled water constant volume, accurately measure this solution 1mL, use distilled water constant volume in 10mL, 100mL, 1000mL volumetric flask respectively, be numbered 1,2, No. 3 solution respectively; Then from No. 3 solution, accurately measure 1mL, use distilled water constant volume in 10mL, 100mL, 1000mL volumetric flask respectively, be numbered 4,5, No. 6 solution respectively, 1 ~ No. 6 solution is for subsequent use as standard solution;
(3) electrode clean
Step (3) is by chlorine ion electrode together with contrast electrode, uses magnetic stirring apparatus cleaning electrode current potential in deionized water, and during solution temperature 25 DEG C, cleaning current potential is at-110mV.
(4) electrode alignment
To go forward side by side line item at 1 ~ No. 6 solution testing electrode potential;
(5) potential measurement
By in the sample solution in electrode insertion step (1), drip 0.1mol/L AgNO
3, when electrode potential is 0, stop dripping, and record the AgNO now dripped
3volume, be for sample consume AgNO
3volume, V1
sample=10.721ml; V2
sample=10.723ml; V3
sample=10.720ml; By in the blank sample solution in electrode insertion step (1), drip 0.1mol/L AgNO
3, when electrode potential is 0, stop dripping, and record the AgNO now dripped
3volume, be that blank sample consumes AgNO
3volume, V1
empty=2.011ml; V2
empty=2.014ml; V3
empty=2.012ml;
(6) 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone cubage
Content=C (V
sample-V
empty) M/W × 100%
C is AgNO
3concentration, V
samplefor consuming AgNO for sample
3volume, V
emptyfor blank sample consumes AgNO
3volume, M is the relative molecular mass of chloroformyl thing, and W is the quality of test sample.
C=0.1mol/L; M=226.63g/mol; W=0.20g; Bring V into
sample,v
emptydata, obtain:
Test sample will be got and be divided into three parts, be respectively sample 1, sample 2 and sample 3.The step adopting embodiment to provide detects, and testing result is: sample 1 content=98.697%; Sample 2 content=98.686%; Sample 3 content=98.674%, mean value 98.685%;
Relative deviation=(the 98.697%-98.685%)/98.685%*100%=0.121% of sample 1,
Relative deviation=(the 98.686%-98.685)/98.685%*100%=0.001% of sample 2,
Relative deviation=(the 98.674%-98.685%)/98.685%*100%=0.011% of sample 3.
Claims (4)
1. a 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content, is characterized in that: comprise the following steps:
(1) take test sample, add 1mol/L alcohol KOH solution, then add the HNO of 6mol/L
3after obtain sample solution; By 1mol/L alcohol KOH solution, add the HNO of 6mol/L
3after obtain blank sample solution;
(2) standard solution preparation
Take 7.45g potassium chloride, add in 100mL volumetric flask and use distilled water constant volume, accurately measure this solution 1mL, use distilled water constant volume in 10mL, 100mL, 1000mL volumetric flask respectively, be numbered 1,2, No. 3 solution respectively; Then from No. 3 solution, accurately measure 1mL, use distilled water constant volume in 10mL, 100mL, 1000mL volumetric flask respectively, be numbered 4,5, No. 6 solution respectively, 1 ~ No. 6 solution is for subsequent use as standard solution;
(3) electrode clean
By chlorine ion electrode together with contrast electrode, cleaning electrode current potential in deionized water;
(4) electrode alignment
To go forward side by side line item at 1 ~ No. 6 solution testing electrode potential;
(5) potential measurement
By in the sample solution in electrode insertion step (1), drip AgNO
3, when electrode potential is 0, stop dripping, and record the AgNO now dripped
3volume, be for sample consume AgNO
3volume; By in the blank sample solution in electrode insertion step (1), drip AgNO
3, when electrode potential is 0, stop dripping, and record the AgNO now dripped
3volume, be that blank sample consumes AgNO
3volume;
(6) 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone cubage
Content=C (V
sample-V
empty) M/W × 100%
C is AgNO
3concentration, V
samplefor consuming AgNO for sample
3volume, V
emptyfor blank sample consumes AgNO
3volume, M is the relative molecular mass of chloroformyl thing, and W is the quality of test sample.
2. 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content according to claim 1; it is characterized in that: step (1) is: take test sample 0.20g, add 1mol/L alcohol KOH solution 100mL, add hot reflux 1 hour; put to 25 DEG C, add the HNO of 6mol/L
3sample solution is obtained after 10mL; By 1mol/L alcohol KOH solution 100mL, add hot reflux 1 hour, put to 25 DEG C, add the HNO of 6mol/L
3blank sample solution is obtained after 10mL.
3. 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content according to claim 1; it is characterized in that: step (3) for by chlorine ion electrode together with contrast electrode; use magnetic stirring apparatus cleaning electrode current potential in deionized water; during solution temperature 25 DEG C, cleaning current potential is at-115 ~-105mV.
4. 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content according to claim 1, is characterized in that: the AgNO dripped in step (5)
3concentration is 0.1mol/L.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108240984A (en) * | 2016-12-23 | 2018-07-03 | 九江天赐高新材料有限公司 | A kind of method with the double chlorine sulfimide purity of chemical determination |
| CN112903856A (en) * | 2021-01-22 | 2021-06-04 | 青岛农业大学 | Pretreatment method for detecting trace chloroformyl compound in water sample and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108240984A (en) * | 2016-12-23 | 2018-07-03 | 九江天赐高新材料有限公司 | A kind of method with the double chlorine sulfimide purity of chemical determination |
| CN112903856A (en) * | 2021-01-22 | 2021-06-04 | 青岛农业大学 | Pretreatment method for detecting trace chloroformyl compound in water sample and application thereof |
| CN112903856B (en) * | 2021-01-22 | 2023-02-17 | 青岛农业大学 | Pretreatment method for detecting trace chloroformyl compound in water sample and application thereof |
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| CN104459020B (en) | 2016-06-01 |
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Denomination of invention: Method for determination of 1-chloroformyl-3-methylsulfonyl-2-imidazolidinone Effective date of registration: 20211216 Granted publication date: 20160601 Pledgee: Commercial Bank of China Yiyuan branch of Limited by Share Ltd. Pledgor: SHANDONG XINQUAN PHARMACEUTICAL Co.,Ltd. Registration number: Y2021980015204 |
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Date of cancellation: 20220721 Granted publication date: 20160601 Pledgee: Commercial Bank of China Yiyuan branch of Limited by Share Ltd. Pledgor: SHANDONG XINQUAN PHARMACEUTICAL Co.,Ltd. Registration number: Y2021980015204 |