CN103994995A - Determination method for o-phthalaldehyde - Google Patents
Determination method for o-phthalaldehyde Download PDFInfo
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- CN103994995A CN103994995A CN201410229073.8A CN201410229073A CN103994995A CN 103994995 A CN103994995 A CN 103994995A CN 201410229073 A CN201410229073 A CN 201410229073A CN 103994995 A CN103994995 A CN 103994995A
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Abstract
The invention provides a determination method for o-phthalaldehyde. The determination method comprises the following steps: reacting an excess hydroxylamine hydrochloride solution and a triethanolamine solution with o-phthalaldehyde; and titrating a reacted solution by 0.1mol/L sulfuric acid standard solution while heating. Therefore, a titrating solution is sufficiently titrated and reacted, and the accuracy of determination on the content of o-phthalaldehyde in disinfection liquid is greatly improved. The determination method has the advantages of simplicity in operation and high precision.
Description
Technical field
The present invention relates to a kind of assay method of thimerosal effective constituent, be specifically related to a kind of assay method of o-phthalaldehyde(OPA).
Background technology
O-phthalaldehyde(OPA), is called for short OPA, faint yellow acicular crystal.Its fusing point 56-57 ℃, flash-point is greater than 110 ℃, and water-soluble and alcohol, ether etc., be slightly soluble in sherwood oil.It is medicine intermediate, is up-to-date external application highly effective and safe antibiosis and sterilization agent, uses the sterilization of apparatus as the endoscopy of hospital, can be used for synthetic new platelet aggregation inhibitor indoles ripple fragrant, is also chemical field analytical reagent.
At present in thimerosal production industry, to the assay of o-phthalaldehyde(OPA), mostly adopt the assay method of glutaraldehyde to detect, this assay method adopts the sulfuric acid standard solution of 0.25 mol/L to carry out titration, but in thimerosal, O-phthalic aldehyde is lower than the content of the glutaraldehyde in glutaraldehyde class thimerosal, adopt the sulfuric acid standard solution titration of 0.25 mol/L, cause blank consumption with product consumption to differ very little, cause error very large, through long-term practice operation, find the titration method of existing o-phthalaldehyde(OPA), result is very inaccurate, error is larger, had a strong impact on the quality control of o-phthalaldehyde(OPA) thimerosal.
Summary of the invention
The invention provides a kind of assay method of o-phthalaldehyde(OPA), the inaccurate problem of testing result existing to solve prior art.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of assay method of o-phthalaldehyde(OPA), first use excessive oxammonium hydrochloride solution and triethanolamine solution and O-phthalic aldehyde reaction, then adopt the sulfuric acid standard solution of 0.1 mol/L to carry out titration to reacting rear solution, heating edge titration in limit in titration process, concrete steps are as follows:
1) analytical solution preparation: prepare neutral hydrochloric acid hydroxylamine solution, the triethanolamine solution of preparation 6.5% mass content, prepares and demarcate the sulfuric acid standard solution of 0.1 mol/L;
2) reaction: use a certain amount of o-phthalaldehyde(OPA) thimerosal of pipette, extract, draw with respect to the excessive triethanolamine solution of o-phthalaldehyde(OPA) thimerosal and oxammonium hydrochloride solution, then these three solution are mixed to sealed reaction 1 hour;
3) titration: first use blank titration, consume sulfuric acid vs V1, will react the titration of 1 hour testing sample use sulfuric acid vs, be titrated to when blueness has a some variable color a little and heat and seethe with excitement, slowly titration, when solution colour and blank color approach but do not reach, ebuillition of heated, is titrated to identical with blank color while hot again, cooling rear color is constant, consume vs V2, calculate the content of o-phthalaldehyde(OPA), computing formula is shown below:
X＝C×(V1-V2)×0.3125÷10×100％
In formula, X is O-phthalic aldehyde, %;
V1 is blank vs, the ml of consuming;
V2 is that sample consumes vs, ml;
C is vs concentration, mol/L.
In above-mentioned steps (2), the uptake of o-phthalaldehyde(OPA) thimerosal is 8 milliliters-12 milliliters, and the uptake of triethanolamine solution is 15 milliliters-25 milliliters, and the uptake of oxammonium hydrochloride solution is 20 milliliters-30 milliliters.
The inventive method is used excessive oxammonium hydrochloride solution and triethanolamine solution and O-phthalic aldehyde reaction, then adopt the sulfuric acid standard solution of 0.1 mol/L to carry out titration to reacting rear solution, heating edge titration in limit in titration process, guaranteed the abundant drop reaction of vs, greatly improved the accuracy of thimerosal o-phthalaldehyde(OPA) assay, had advantages of simple to operate high with precision.
Embodiment
A kind of assay method of o-phthalaldehyde(OPA), first use excessive oxammonium hydrochloride solution and triethanolamine solution and O-phthalic aldehyde reaction, then adopt the sulfuric acid standard solution of 0.1 mol/L to carry out titration to reacting rear solution, heating edge titration in limit in titration process, concrete steps are as follows:
1) analytical solution preparation: prepare neutral hydrochloric acid hydroxylamine solution, the triethanolamine solution of preparation 6.5% mass content, prepares and demarcate the sulfuric acid standard solution of 0.1 mol/L;
2) reaction: use 25 milliliters of triethanolamine solutions of pipette, extract, 20 milliliters of oxammonium hydrochloride solution and 10 milliliters of o-phthalaldehyde(OPA) thimerosals, these three solution are mixed to sealed reaction 1 hour;
3) titration: first use blank titration, consume sulfuric acid vs V1, will react the titration of 1 hour testing sample use sulfuric acid vs, be titrated to when blueness has a some variable color a little and heat and seethe with excitement, slowly titration, when solution colour and blank color approach but do not reach, ebuillition of heated, is titrated to identical with blank color while hot again, cooling rear color is constant, consume vs V2, calculate the content of o-phthalaldehyde(OPA), computing formula is shown below:
X＝C×(V1-V2)×0.3125÷10×100％
In formula, X is O-phthalic aldehyde, %;
V1 is blank vs, the ml of consuming;
V2 is that sample consumes vs, ml;
C is vs concentration, mol/L.
Claims (2)
1. the assay method of an o-phthalaldehyde(OPA), it is characterized in that first using excessive oxammonium hydrochloride solution and triethanolamine solution and O-phthalic aldehyde reaction, then adopt the sulfuric acid standard solution of 0.1 mol/L to carry out titration to reacting rear solution, heating edge titration in limit in titration process, concrete steps are as follows:
1) analytical solution preparation: prepare neutral hydrochloric acid hydroxylamine solution, the triethanolamine solution of preparation 6.5% mass content, prepares and demarcate the sulfuric acid standard solution of 0.1 mol/L;
2) reaction: use a certain amount of o-phthalaldehyde(OPA) thimerosal of pipette, extract, draw with respect to the excessive triethanolamine solution of o-phthalaldehyde(OPA) thimerosal and oxammonium hydrochloride solution, then these three solution are mixed to sealed reaction 1 hour;
3) titration: first use blank titration, consume sulfuric acid vs V1, will react the titration of 1 hour testing sample use sulfuric acid vs, be titrated to when blueness has a some variable color a little and heat and seethe with excitement, slowly titration, when solution colour and blank color approach but do not reach, ebuillition of heated, is titrated to identical with blank color while hot again, cooling rear color is constant, consume vs V2, calculate the content of o-phthalaldehyde(OPA), computing formula is shown below:
X＝C×(V1-V2)×0.3125÷10×100％
In formula, X is O-phthalic aldehyde, %;
V1 is blank vs, the ml of consuming;
V2 is that sample consumes vs, ml;
C is vs concentration, mol/L.
2. the assay method of o-phthalaldehyde(OPA) according to claim 1, the uptake that it is characterized in that o-phthalaldehyde(OPA) thimerosal in step (2) is 8 milliliters-12 milliliters, the uptake of triethanolamine solution is 15 milliliters-25 milliliters, and the uptake of oxammonium hydrochloride solution is 20 milliliters-30 milliliters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410229073.8A CN103994995A (en) | 2014-05-21 | 2014-05-21 | Determination method for o-phthalaldehyde |
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| CN201410229073.8A CN103994995A (en) | 2014-05-21 | 2014-05-21 | Determination method for o-phthalaldehyde |
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| CN103994995A true CN103994995A (en) | 2014-08-20 |
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| CN201410229073.8A Pending CN103994995A (en) | 2014-05-21 | 2014-05-21 | Determination method for o-phthalaldehyde |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105548166A (en) * | 2015-12-30 | 2016-05-04 | 广州市医德生物科技有限责任公司 | OPA (o-phthalaldehyde) disinfector concentration range detection test paper |
| CN106970078A (en) * | 2017-05-15 | 2017-07-21 | 北京长江脉医药科技有限责任公司 | A kind of test paper and its preparation and detection method for detecting OPA |
| CN107024473A (en) * | 2017-05-15 | 2017-08-08 | 北京长江脉医药科技有限责任公司 | A kind of O-phthalaldehyde disinfectant concentration quick detection test paper and preparation method and application |
-
2014
- 2014-05-21 CN CN201410229073.8A patent/CN103994995A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 上海市消毒品协会: "《医院消毒技术规范》", 31 August 2008, 中国标准出版社 * |
| 林立旺等: "复方邻苯二甲醛的研制及消毒性能观察", 《中国消毒学杂志》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105548166A (en) * | 2015-12-30 | 2016-05-04 | 广州市医德生物科技有限责任公司 | OPA (o-phthalaldehyde) disinfector concentration range detection test paper |
| CN106970078A (en) * | 2017-05-15 | 2017-07-21 | 北京长江脉医药科技有限责任公司 | A kind of test paper and its preparation and detection method for detecting OPA |
| CN107024473A (en) * | 2017-05-15 | 2017-08-08 | 北京长江脉医药科技有限责任公司 | A kind of O-phthalaldehyde disinfectant concentration quick detection test paper and preparation method and application |
| CN107024473B (en) * | 2017-05-15 | 2019-06-25 | 北京长江脉医药科技有限责任公司 | A kind of O-phthalaldehyde disinfectant concentration quick detection test paper and the preparation method and application thereof |
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