CN104459020B - 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content - Google Patents
1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content Download PDFInfo
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Abstract
The present invention relates to a kind of detection method, it is specifically related to a kind of 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content. First prepare sample solution and blank sample solution, then preparing standard solution, electrode is through cleaning and after correction, tests; Sample solution drips and adds AgNO3, when electropotential is 0, record now drips the AgNO added3Volume, be for sample consume AgNO3Volume; Blank sample solution drips and adds AgNO3, when electropotential is 0, record now drips the AgNO added3Volume, be that blank sample consumes AgNO3Volume; Then 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone content is calculated. The present invention is simple to operate, accuracy height, it is possible to reducing the error that subjectivity color judges terminal, parallelism is good; And decrease the use of developer.
Description
Technical field
The present invention relates to a kind of detection method, it is 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 fast growth in microbiotic market, the demand of 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone also rapidly increases thereupon. How accurately to measure its content and also seem 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 cyanogen amine standardized solution back titration is excessive. The defect existed: the judgement of titration end point judges terminal with color, there is observation error, and namely the judgement of titration end point varies with each individual, and causes result deviation occur, and parallelism is poor.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content, simple to operate, accuracy height, reduce the error that subjectivity color judges terminal, 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 trial-product, add 1mol/L alcohol KOH solution, then add the HNO of 6mol/L3After obtain sample solution; By 1mol/L alcohol KOH solution, add the HNO of 6mol/L3After obtain blank sample solution;
(2) standardized solution preparation
Take 7.45g Repone K, add in 100mL volumetric flask and surely hold with distilled water, accurately measure this solution 1mL, surely hold in 10mL, 100mL, 1000mL volumetric flask with distilled water respectively, be numbered 1,2, No. 3 solution respectively; Then accurately measuring 1mL from No. 3 solution, surely hold in 10mL, 100mL, 1000mL volumetric flask with distilled water respectively, be numbered 4,5, No. 6 solution respectively, 1��No. 6 solution is for subsequent use as standardized solution;
(3) electrode clean
By chlorine ion electrode together with reference electrode, cleaning electrode current potential in deionized water;
(4) electrode correction
At 1��No. 6 solution testing electropotential and carry out record;
(5) potential measurement
In sample solution in electrode inserting step (1), will drip and add AgNO3, when electropotential is 0, stopping is dripped and is added, and records and now drip the AgNO added3Volume, be for sample consume AgNO3Volume; In blank sample solution in electrode inserting step (1), will drip and add AgNO3, when electropotential is 0, stopping is dripped and is added, and records and now drip the AgNO added3Volume, be that blank sample consumes AgNO3Volume;
(6) 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone cubage
Content=C (VSample-VEmpty) M/W �� 100%
C is AgNO3Concentration, VSampleFor consuming AgNO for sample3Volume, VEmptyFor blank sample consumes AgNO3Volume, M is the relative molecular mass of chloroformyl thing, and W is the quality of trial-product.
Wherein:
Step (1) is: take trial-product 0.20g, adds 1mol/L alcohol KOH solution 100mL, and reflux 1 hour, puts to 25 DEG C, adds the HNO of 6mol/L3Sample solution is obtained after 10mL; By 1mol/L alcohol KOH solution 100mL, reflux 1 hour, puts to 25 DEG C, adds the HNO of 6mol/L3Blank sample solution is obtained after 10mL.
Step (3) be by chlorine ion electrode together with reference electrode, it may also be useful to magnetic stirring apparatus is cleaning electrode current potential in deionized water, during solution temperature 25 DEG C, clean current potential at-115��-105mV.
Step (5) is dripped the AgNO added3Concentration is 0.1mol/L.
The present invention has the following advantages:
(1) the present invention is simple to operate, accuracy height, it is possible to reduce the error that subjectivity color judges terminal,
(2) 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) taking trial-product 0.20g, add 1mol/L alcohol KOH solution 100mL, reflux 1 hour, puts to 25 DEG C, adds the HNO of 6mol/L3Sample solution is obtained after 10mL; By 1mol/L alcohol KOH solution 100mL, reflux 1 hour, puts to 25 DEG C, adds the HNO of 6mol/L3Blank sample solution is obtained after 10mL. Same batch sample configures three parts, is respectively sample 1, sample 2 and sample 3.
(2) standardized solution preparation
Take 7.45g Repone K, add in 100mL volumetric flask and surely hold with distilled water, accurately measure this solution 1mL, surely hold in 10mL, 100mL, 1000mL volumetric flask with distilled water respectively, be numbered 1,2, No. 3 solution respectively; Then accurately measuring 1mL from No. 3 solution, surely hold in 10mL, 100mL, 1000mL volumetric flask with distilled water respectively, be numbered 4,5, No. 6 solution respectively, 1��No. 6 solution is for subsequent use as standardized solution;
(3) electrode clean
Step (3) be by chlorine ion electrode together with reference electrode, it may also be useful to magnetic stirring apparatus is cleaning electrode current potential in deionized water, during solution temperature 25 DEG C, clean current potential at-110mV.
(4) electrode correction
At 1��No. 6 solution testing electropotential and carry out record;
(5) potential measurement
In sample solution in electrode inserting step (1), will drip and add 0.1mol/LAgNO3, when electropotential is 0, stopping is dripped and is added, and records and now drip the AgNO added3Volume, be for sample consume AgNO3Volume, V1Sample=10.721ml; V2Sample=10.723ml; V3Sample=10.720ml; In blank sample solution in electrode inserting step (1), will drip and add 0.1mol/LAgNO3, when electropotential is 0, stopping is dripped and is added, and records and now drip the AgNO added3Volume, be that blank sample consumes AgNO3Volume, V1Empty=2.011ml; V2Empty=2.014ml; V3Empty=2.012ml;
(6) 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone cubage
Content=C (VSample-VEmpty) M/W �� 100%
C is AgNO3Concentration, VSampleFor consuming AgNO for sample3Volume, VEmptyFor blank sample consumes AgNO3Volume, M is the relative molecular mass of chloroformyl thing, and W is the quality of trial-product.
C=0.1mol/L; M=226.63g/mol; W=0.20g; Bring V intoSample,VEmptyData, obtain:
Trial-product will be got and it will be divided into three parts, be respectively sample 1, sample 2 and sample 3. The step adopting embodiment to provide detects, and detected result is: sample 1 content=98.697%; Sample 2 content=98.686%; Sample 3 content=98.674%, mean value 98.685%;
The relative deviation of sample 1=(98.697%-98.685%)/98.685%*100%=0.121%,
The relative deviation of sample 2=(98.686%-98.685)/98.685%*100%=0.001%,
The relative deviation of sample 3=(98.674%-98.685%)/98.685%*100%=0.011%.
Claims (4)
1. a 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content, it is characterised in that: comprise the following steps:
(1) take trial-product, add 1mol/L alcohol KOH solution, then add the HNO of 6mol/L3After obtain sample solution; By 1mol/L alcohol KOH solution, add the HNO of 6mol/L3After obtain blank sample solution;
(2) standardized solution preparation
Take 7.45g Repone K, add in 100mL volumetric flask and surely hold with distilled water, accurately measure this solution 1mL, surely hold in 10mL, 100mL, 1000mL volumetric flask with distilled water respectively, be numbered 1,2, No. 3 solution respectively; Then accurately measuring 1mL from No. 3 solution, surely hold in 10mL, 100mL, 1000mL volumetric flask with distilled water respectively, be numbered 4,5, No. 6 solution respectively, 1��No. 6 solution is for subsequent use as standardized solution;
(3) electrode clean
By chlorine ion electrode together with reference electrode, cleaning electrode current potential in deionized water;
(4) electrode correction
At 1��No. 6 solution testing electropotential and carry out record;
(5) potential measurement
In sample solution in electrode inserting step (1), will drip and add AgNO3, when electropotential is 0, stopping is dripped and is added, and records and now drip the AgNO added3Volume, be for sample consume AgNO3Volume; In blank sample solution in electrode inserting step (1), will drip and add AgNO3, when electropotential is 0, stopping is dripped and is added, and records and now drip the AgNO added3Volume, be that blank sample consumes AgNO3Volume;
(6) 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone cubage
Content=C (VSample-VEmpty) M/W �� 100%
C is AgNO3Concentration, VSampleFor consuming AgNO for sample3Volume, VEmptyFor blank sample consumes AgNO3Volume, M is the relative molecular mass of chloroformyl thing, and W is the quality of trial-product.
2. 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content according to claim 1; it is characterized in that: step (1) is: take trial-product 0.20g, adds 1mol/L alcohol KOH solution 100mL, reflux 1 hour; put to 25 DEG C, add the HNO of 6mol/L3Sample solution is obtained after 10mL; By 1mol/L alcohol KOH solution 100mL, reflux 1 hour, puts to 25 DEG C, adds the HNO of 6mol/L3Blank 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 reference electrode; use magnetic stirring apparatus cleaning electrode current potential in deionized water; during solution temperature 25 DEG C, clean current potential at-115��-105mV.
4. 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone detection method of content according to claim 1, it is characterised in that: step (5) is dripped the AgNO added3Concentration is 0.1mol/L.
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