CN101706441A - Method of quantitative chemical analysis of content of active group bromo alkyl acyl chloride - Google Patents
Method of quantitative chemical analysis of content of active group bromo alkyl acyl chloride Download PDFInfo
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- CN101706441A CN101706441A CN200910228587A CN200910228587A CN101706441A CN 101706441 A CN101706441 A CN 101706441A CN 200910228587 A CN200910228587 A CN 200910228587A CN 200910228587 A CN200910228587 A CN 200910228587A CN 101706441 A CN101706441 A CN 101706441A
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- active group
- acyl chloride
- alkyl acyl
- bromo alkyl
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Abstract
The invention relates to a method of quantitative chemical analysis of the content of active group bromo alkyl acyl chloride, which comprises the following steps: reacting a primary standard substance with sample active group bromo alkyl acyl chloride, wherein the mol ratio of the primary standard substance is larger than the theoretical mol ratio; using sodium nitrite standard solution to conduct titration, thus leading the residual primary standard substance to be reacted completely; and calculating the quality content of active group bromo alkyl acyl chloride in the sample active group bromo alkyl acyl chloride according to the mol ratio of the primary standard substance, the quality of the sample active group bromo alkyl acyl chloride and the mol ratio of the sodium nitrite.
Description
Technical field
The invention belongs to chemical analysis field, relate to a kind of method of quantitative chemical analysis of content of active group bromo alkyl acyl chloride specifically.
Background technology
Active group bromo alkyl acyl chloride content analysis method, use is very extensive in producing dyestuff enterprise, it is very big that its analysis result whether accurate plays a part production quality control, used analytical approach can not satisfy the demand that high quality of products is produced in the enterprise at present, quantitative chemical analysis of content of active group bromo alkyl acyl chloride method of the present invention relevant record on the document at home and abroad, the excellence point of quantitative chemical analysis of content of active group bromo alkyl acyl chloride method of the present invention is that the result is accurate, can correctly instruct production.
Summary of the invention
The invention provides a kind of quantitative chemical analysis of content of active group bromo alkyl acyl chloride method, this method comprises the steps:
With primary standard substance and sample active group bromo alkyl acyl chloride reaction, wherein the molal quantity of primary standard substance is greater than the theoretical molar number of sample active group bromo alkyl acyl chloride, use the sodium nitrite standard solution titration again, make remaining primary standard substance react completely, according to the mass content of active group bromo alkyl acyl chloride in the molal quantity calculation sample active group bromo alkyl acyl chloride of the quality of the molal quantity of primary standard substance, sample active group bromo alkyl acyl chloride and sodium nitrite.
The molal quantity that the sample quality that the theoretical molar number is meant the sample active group bromo alkyl acyl chloride that contains impurity in the said method obtains divided by the molecular weight of active group bromo alkyl acyl chloride, this numerical value is not the actual molal quantity of active group bromo alkyl acyl chloride, and this theoretical molar number is greater than the actual molal quantity of active group bromo alkyl acyl chloride in the sample.
The formula of the mass content of active group bromo alkyl acyl chloride is as follows in calculating according to the molal quantity of the quality of the molal quantity of primary standard substance, sample active group bromo alkyl acyl chloride and sodium nitrite:
Primary standard substance among the present invention is meant and can reacts with active group bromo alkyl acyl chloride, generate amido link, be also referred to as peptide bond, can also generate the material of diazo-compounds with the sodium nitrite reaction, such material satisfies as the material of measuring active group bromo alkyl acyl chloride content.Preferably, primary standard substance is for having the compound of following structural formula (I):
R wherein
1Be H or alkyl, alkyl is preferably C
1-4Alkyl.
Preferably, primary standard substance is an aminobenzenesulfonic acid, and aminobenzenesulfonic acid can be a sulfanilic acid.
Active group bromo alkyl acyl chloride among the present invention is meant and contains acid chloride group, in compound, also there is simultaneously the substituting group bromine, make the chlorosity on the acid chloride group easily slough, compound with amino reaction generation amido link. preferably, active group bromo alkyl acyl chloride is for having the compound of following structural formula (II):
R wherein
2Be H or alkyl, alkyl is preferably C
1-4Alkyl.
Preferably, active group bromo alkyl acyl chloride is 2,3-two bromo propionyl chloros.
Concrete, the present invention also provides a kind of quantitative chemical analysis of content of active group bromo alkyl acyl chloride method, and the concrete steps of this method are:
Accurately take by weighing the primary standard substance of 1 mass parts, add distilled water, transfer pH=6-7 with 10% aqueous sodium carbonate or 10% sodium bicarbonate aqueous solution, material is dissolved fully, adjust temperature to 0-25 ℃, the sample that adds 1 mass parts, be placed on the stirrer, holding temperature insulation reaction 2-6 hour, is constantly transferred pH with 10% sodium carbonate liquor or 10% sodium bicarbonate aqueous solution at 0-25 ℃ in course of reaction, is reaction end when reaction keeps pH for neutral constant the time, after reaching home, add hydrochloric acid, cool to 0-5 ℃, with the excessive primary standard substance of sodium nitrite standard solution titration, titration to starch potassium iodide paper is little blueness, and keeps 3-5 minute, and nondiscolouring is a titration end-point.
The computing formula of the active group bromo alkyl acyl chloride content of said method is as follows:
In the said method, preferably adjust temperature to 10-25 ℃.
In the said method, preferred holding temperature is at 10-25 ℃, insulation reaction 3-5 hour.
More specifically, the present invention also provides a kind of quantitative chemical analysis of content of active group bromo alkyl acyl chloride method, and the concrete steps of this method are:
Accurately taking by weighing mass concentration is the primary standard substance G of A
1Restrain in iodine flask, add distilled water, transfer pH=6-7, material is dissolved fully, adjust temperature, take by weighing G again to 0-25 ℃ with 10% aqueous sodium carbonate or 10% sodium bicarbonate aqueous solution
2The gram sample adds in the above-mentioned solution, be placed on the stirrer, holding temperature is at 0-25 ℃, insulation reaction 2-6 hour, in course of reaction, constantly transfer pH with 10% sodium carbonate liquor or 10% sodium bicarbonate aqueous solution, is reaction end when reaction keeps pH for neutral constant the time, after terminal point arrives, add hydrochloric acid, at 0-5 ℃ is the excessive primary standard substance of sodium nitrite standard solution titration of N with concentration down, and titration to starch potassium iodide paper is little blueness, and keeps 3-5 minute, nondiscolouring is a titration end-point, has used sodium nitrite solution V.
The computing formula of the active group bromo alkyl acyl chloride content of said method is as follows:
In the top formula:
A: the quality percentage composition of primary standard substance;
G
1: the quality of primary standard substance (unit is g)
N: the concentration of sodium nitrite standard solution (unit is mol/L)
V: the volume (unit is ml) that consumes the sodium nitrite standard solution;
G
2: the quality (unit is g) of sample active group bromo alkyl acyl chloride
B: the molecular weight of primary standard substance (173.19)
C: the molecular weight (250.32) of active group bromo alkyl acyl chloride
The principle of quantitative chemical analysis of content of active group bromo alkyl acyl chloride method of the present invention is:
Active group bromo alkyl acyl chloride is a kind of compound of living very much; chlorine atom in its molecule is very active; utilize this characteristic; select to react with the chlorine in excessive primary standard substance and the active group bromo alkyl acyl chloride molecule; use the remaining primary standard substance of sodium nitrite standard solution titration again; can determine like this and primary standard substance reactive activity base bromo alkyl acyl chloride molal quantity, thus active group bromo alkyl acyl chloride real content in the sample that can determine.
In the said method, when primary standard substance is a sulfanilic acid, active group bromo alkyl acyl chloride is 2, and during 3-two bromo propionyl chloros, reaction equation of the present invention is:
Used raw material can be bought from the market and obtain in the method for the present invention.
The excellence point of quantitative chemical analysis of content of active group bromo alkyl acyl chloride method of the present invention is that the result is accurate, and is simple to operate, economical and practical, can correctly instruct production.
Because active group bromo alkyl acyl chloride is a kind of reactive dye active group, so method of the present invention particularly to reactive dye for wool active group content determine to have remarkable result, quantitative chemical analysis of content of active group bromo alkyl acyl chloride method of the present invention has important effect to producing reactive dye for wool.
Embodiment
In order to understand the present invention, further specify the present invention with embodiment below, but do not limit the present invention.
Embodiment 1:
Accurately taking by weighing mass concentration and be 99.9% sulfanilic acid 1.2390 restrains in iodine flask, add distilled water, with 10% sodium bicarbonate aqueous solution pH=6-7, material is dissolved fully, adjust temperature to 10 ± 2 ℃, take by weighing 0.9100 gram 2 again, 3-two bromo propionyl chloro samples add in the above-mentioned appearance liquid, be placed on the stirrer, holding temperature is at 0-5 ℃, and insulation reaction 2 hours is constantly transferred pH with 10% sodium bicarbonate aqueous solution in course of reaction, when keeping pH to be neutral constant, reaction adds hydrochloric acid, reducing the temperature to 0-5 ℃, is the excessive sulfanilic acid of sodium nitrite standard solution titration of 0.1086mol/L with concentration, and titration to starch potassium iodide paper is little blueness, and kept 3-5 minute, nondiscolouring is a titration end-point, uses sodium nitrite solution 33.67ml altogether, calculates according to above-mentioned formula, obtain target measurement material 2, the mass percentage content of 3-two bromo propionyl chloro samples is 94.82%.
Embodiment 2:
Accurately taking by weighing mass concentration and be 99.9% sulfanilic acid 1.4110 restrains in iodine flask, add distilled water, with 10% aqueous sodium carbonate pH=6-7, material is dissolved fully, adjust temperature to 18 ± 2 ℃, take by weighing 1.0200 grams 2 again, 3-two bromo propionyl chloro samples add in the above-mentioned solution, just on stirrer, holding temperature is at 10-15 ℃, and insulation reaction 5 hours is constantly transferred pH with 10% sodium carbonate liquor in course of reaction, when keeping pH to be neutral constant, reaction adds hydrochloric acid, reducing the temperature to 0-5 ℃, is the excessive sulfanilic acid of sodium nitrite standard solution titration of 0.1086mol/L with concentration, and titration to starch potassium iodide paper is little blueness, and kept 3-5 minute, nondiscolouring is a titration end-point, uses sodium nitrite solution 39.01ml altogether, calculates according to above-mentioned formula, obtain target measurement material 2, the mass percentage content of 3-two bromo propionyl chloro samples is 94.52%.
Method of the present invention is described by specific embodiment.Those skilled in the art can use for reference links such as content appropriate change raw material of the present invention, process conditions and realize corresponding other purpose, its relevant change does not all break away from content of the present invention, all similar replacements and change will become apparent to those skilled in the art that and all be regarded as comprising within the scope of the present invention.
Claims (9)
1. quantitative chemical analysis of content of active group bromo alkyl acyl chloride method, this method comprises the steps:
With primary standard substance and sample active group bromo alkyl acyl chloride reaction, wherein the molal quantity of primary standard substance is greater than the theoretical molar number of sample active group bromo alkyl acyl chloride, use the sodium nitrite standard solution titration again, make remaining primary standard substance react completely, according to the mass content of active group bromo alkyl acyl chloride in the molal quantity calculation sample active group bromo alkyl acyl chloride of the quality of the molal quantity of primary standard substance, sample active group bromo alkyl acyl chloride and sodium nitrite;
The molal quantity that obtains divided by the molecular weight of active group bromo alkyl acyl chloride of the theoretical molar number sample quality that is meant the sample active group bromo alkyl acyl chloride that contains impurity wherein;
The formula of the mass content of active group bromo alkyl acyl chloride is as follows in calculating according to the molal quantity of the quality of the molal quantity of primary standard substance, sample active group bromo alkyl acyl chloride and sodium nitrite:
Primary standard substance be meant can with the active group bromo alkyl acyl chloride generation amido link that reacts, can also generate the material of diazo-compounds with the sodium nitrite reaction;
Active group bromo alkyl acyl chloride is meant and contains acid chloride group, also has the substituting group bromine simultaneously in compound, makes that the chlorosity on the acid chloride group is easily sloughed, with the compound of amino reaction generation amido link.
2. method according to claim 1, wherein primary standard substance is for having the compound of following structural formula (I):
R wherein
1Be H or alkyl, alkyl is preferably C
1-4Alkyl.
3. method according to claim 1 and 2, wherein primary standard substance is an aminobenzenesulfonic acid.
4. method according to claim 3, wherein aminobenzenesulfonic acid is a sulfanilic acid.
5. according to each described method of claim 1-4, wherein active group bromo alkyl acyl chloride is the compound with following structural formula (II):
R wherein
2Be H or alkyl, alkyl is preferably C
1-4Alkyl.
6. method according to claim 5, wherein active group bromo alkyl acyl chloride is 2,3-two bromo propionyl chloros.
7. method according to claim 1, this method comprise the steps into:
Accurately take by weighing the primary standard substance of 1 mass parts, add distilled water, transfer pH=6-7 with 10% aqueous sodium carbonate or 10% sodium bicarbonate aqueous solution, material is dissolved fully, adjust temperature to 0-25 ℃, the sample that adds 1 mass parts, be placed on the stirrer, holding temperature is at 0-25 ℃, insulation reaction 2-6 hour, in course of reaction, constantly transfer pH with 10% sodium carbonate liquor or 10% sodium bicarbonate aqueous solution, is reaction end when reaction keeps pH for neutral constant the time, after reaching home, adds hydrochloric acid, cool to 0-5 ℃, with the excessive primary standard substance of sodium nitrite standard solution titration, titration to starch potassium iodide paper is little blueness, and keeps 3-5 minute, nondiscolouring is a titration end-point
The computing formula of active group bromo alkyl acyl chloride content is as follows:
8. method according to claim 7 is wherein adjusted temperature to 10-25 ℃.
9. method according to claim 7, wherein holding temperature is at 10-25 ℃, insulation reaction 3-5 hour.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101726490B (en) * | 2009-11-16 | 2011-09-21 | 天津德凯化工股份有限公司 | Quantitative chemical analysis method of content of active group bromo-alkyl acyl chloride |
| CN102645513A (en) * | 2012-05-02 | 2012-08-22 | 成都苑东药业有限公司 | Method for determining sodion content in diphosphonic acid monosodium salt compound |
| CN117092274A (en) * | 2023-07-14 | 2023-11-21 | 国药集团致君（深圳）坪山制药有限公司 | Method for determining sevelamer carbonate content |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215425B (en) * | 2008-01-22 | 2011-05-25 | 天津德凯化工股份有限公司 | Red reactive dyestuffs and preparation method thereof |
| CN101726490B (en) * | 2009-11-16 | 2011-09-21 | 天津德凯化工股份有限公司 | Quantitative chemical analysis method of content of active group bromo-alkyl acyl chloride |
| CN101726488B (en) * | 2009-11-16 | 2011-10-05 | 天津德凯化工股份有限公司 | Method for quantitatively chemically analyzing content of 2,3-dibromopropionyl chloride |
| CN101726489B (en) * | 2009-11-16 | 2011-09-21 | 天津德凯化工股份有限公司 | Quantitative chemical analysis method of 2,3-dibromo-propionyl chloride content |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101726490B (en) * | 2009-11-16 | 2011-09-21 | 天津德凯化工股份有限公司 | Quantitative chemical analysis method of content of active group bromo-alkyl acyl chloride |
| CN102645513A (en) * | 2012-05-02 | 2012-08-22 | 成都苑东药业有限公司 | Method for determining sodion content in diphosphonic acid monosodium salt compound |
| CN102645513B (en) * | 2012-05-02 | 2014-07-16 | 成都苑东药业有限公司 | Method for determining sodion content in diphosphonic acid monosodium salt compound |
| CN117092274A (en) * | 2023-07-14 | 2023-11-21 | 国药集团致君（深圳）坪山制药有限公司 | Method for determining sevelamer carbonate content |
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