CN101308121A - Sulfonic acid analog anion surfactants rapid checking method - Google Patents
Sulfonic acid analog anion surfactants rapid checking method Download PDFInfo
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- CN101308121A CN101308121A CNA2007100406176A CN200710040617A CN101308121A CN 101308121 A CN101308121 A CN 101308121A CN A2007100406176 A CNA2007100406176 A CN A2007100406176A CN 200710040617 A CN200710040617 A CN 200710040617A CN 101308121 A CN101308121 A CN 101308121A
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- potassium iodide
- sulfonic acid
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Abstract
The invention discloses a fast detection method for detecting anionic surface active agent of sulfuric acids, which comprises: a potassium iodide is mixed with a sulfuric acid negative ion surface active agent by a molar ratio of 1:1-10:1, then N and N-dimethyl formamide having the amount of 5 to 20ml/mol of potassium iodide are added into the mixture, the mixture is agitated to reach complete dissolution, then trifluoroacetic anhydride with the molar ratio one to ten times the amount of potassium iodide is added into the solution, the solution turns into red and is taken for implementing the conventional gas phase chromatography-mass spectrum detection and then data processing analysis when the color stops darkening, thereby obtaining the detecting result. The detection method has advantages of fast and simple reaction process and easy control of conditions, and makes up defects that the traditional detection method has false positive easily and can not ensure detection results and has high requirements on sample pre-processing, and the method is particularly suitable for qualitative and quantitative analysis of all components in complex compounds such as anionic surface active agent.
Description
Technical field
The present invention relates to a kind of detection method of surfactant, belong to the analytical chemistry field, relate to a kind of detection method of sulfonic acid analog anion surfactants particularly.
Background technology
Sulfonic acid analog anion surfactants is the compound of a class in chemical industry, medicine and other fields widespread use, and it has the characteristic of strong polarity, difficult volatilization.All play great effect in every respect, sulfonic acid analog anion surfactants has also brought very serious environmental problem in a large amount of productions and widely used while.After they enter water body, can make the water generates foam, phenomenons such as emulsification and particle suspension, the exchange of oxygen influences water body purification in oxygen in the exclusion of water and the air, causes water quality deterioration, contaminated environment.Therefore, the analysis of sulfonic acid analog anion surfactants and evaluation have very important meaning.
The method of traditional analysis sulfonic acid analog anion surfactants mainly contains gravimetric method, extraction, the precipitation method and colourimetry etc., and these methods are subjected to the restriction of sensitivity, selectivity etc., generally only is used for classification and differentiates.
Modern method for separating and analyzing such as vapor-phase chromatography, Capillary Electrophoresis and high performance liquid chromatography have been substituted the classical way that is confined to classify and differentiates, become the main means of alkyl benzene sulfonate surfactant compartment analysis.Vapor-phase chromatography has high separation efficiency and characteristics such as quantitatively accurate.But can not direct injected, derivatization in advance because sulfonic acid analog anion surfactants is difficult to volatilization.
The deriving method of traditional sulfonic acid analog anion surfactants mainly contains esterification process, silanization derivatization method, sulfonic acid halogen process, reducing process, one-tenth amine derivatization method and phosphoric acid pyrolysis, alkali fusion, additive methods such as direct pyrolysis.
The esterification of sulfonic compound is the most widely used derivatization reaction of a class.But for sulfonic acid, the step of preparation methylmesylate is more loaded down with trivial details, need be prepared into free sulfonic earlier.If adopt the ammonium salt pyrolysismethod, then the detection that the chromatographic peak that obtains of cracking amine can the p-sulfonic acid derivant causes difficulty.
Because the stability of sulfonic acid group, the derivatization reaction effect of its silanization is also bad, and the shortcoming of preparation trouble is still arranged.
The preparation of same sulfonamide is just more loaded down with trivial details, need obtain sulfonic acid halide earlier, just can make with the secondary amine reaction again.
Preparation sulfonic acid halide step comparatively speaking is a little convenient, but the aliphatic chain sulfonic acid halide very easily decomposes, and can't carry out the gas chromatography compartment analysis.
The reduction of sulfonic acid is difficulty comparatively, also very unripe so far passes through that single step reaction is reduced into sulfydryl by sulfonic acid and the derivative reaction that can carry out stratographic analysis.
Summary of the invention
Technical matters to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of method for quick of sulfonic acid analog anion surfactants is provided.
The detection method of sulfonic acid analog anion surfactants proposed by the invention comprises the steps:
(1) be that 1: 1～10: 1 potassium iodide and sulfonic acid analog anion surfactants mix with mol ratio;
(2) in said mixture, add N, the dinethylformamide of 5～20ml/mol potassium iodide amount, be stirred to dissolving fully;
(3) add the trifluoro-acetic anhydride that 1～10 times of mole of potassium iodide is made a gesture of measuring, solution becomes redness.After color is no longer deepened, can carry out the sample introduction analysis;
(4) get above-mentioned solution and carry out conventional gas chromatography-mass spectrum detection, carry out Data Management Analysis again, can obtain testing result.
In the present invention, the reduction that has proposed use potassium iodide/N, the dinethylformamide/trifluoro-acetic anhydride method of system of deriving, this invention has good novelty, overcome the shortcoming of traditional deriving method.Course of reaction is quick, simple, condition is controlled easily.The present invention has simultaneously adopted the analysis and detection technology of gas chromatography-mass spectrography, high score with capillary chromatography from characteristics such as mass spectral accurate evaluation, false positive appears in traditional detection method easily that remedied present use, can not prove conclusively and, be particularly suitable for qualitative, the quantitative test of each component in this class complex mixture of anionic surfactant the demanding deficiency of sample pre-treatments.
Generally speaking, the detection method of the sulfonic acid analog anion surfactants that the present invention proposes is not only convenient fast, condition is easily controlled, and product is stable, has good gas chromatography-mass spectrum behavior, can solve the difficult problem that the sulfonic acid analog anion surfactants analysis of effective component is identified well.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment one
Take by weighing commercially available trade mark profound, white cat by name, three kinds of each 5g of washing powder that contain sulfonic acid analog anion surfactants of Jiamei, all add the 0.2g potassium iodide respectively successively, 10mLN, dinethylformamide, vibration is to dissolving fully.Drip 0.7mL (about 5m mol) trifluoro-acetic anhydride again, solution becomes peony immediately, and the generation of adularescent smog, and reaction is violent, separates out iodine.After treating that its color is no longer deepened, the solution of this moment promptly carries out the chromaticness analysis.
The testing conditions that gas chromatography-mass spectrum detects is as follows:
Detecting instrument: Finnigan Voyager gas chromatograph-mass spectrometer (GCMS)
Chromatographic column: DB-5 (30m * 0.25mm, 0.25 μ m)
Column temperature: 90 ℃ (keeping 2min)～200 ℃ (keeping 10min)
Programming rate: 15 ℃/min
Vaporizer temperature: 250 ℃
Carrier gas (flow): He (1.0mL/min)
Sample size: 1 μ l
Split ratio: 20: 1
Mass detector: EI source, electron energy 70EV, 200 ℃ of acquisition time 25min of source temperature
Retrieval spectrum storehouse: NIST storehouse
Quality of scanning scope: 50～650amu
Sweep velocity: 0.5 second/time
Testing result
After each chromatographic peak ownership, use the computing machine integration.Can obtain the detailed composition of alkyl benzene sulphonate sodium sample in three kinds of washing powder samples, the alkyl benzene sulphonate sodium content of variant carbochain is listed in the table below:
Above-mentioned example shows, potassium iodide/N that the present invention proposes, dinethylformamide/trifluoro-acetic anhydride reduction redundant organism bind and close the gas chromatography-mass spectrum detection technique, be a kind of reliable and practical detection method, main effective constituent-aromatic sulphonic acid compounds that can the p-sulfonic acid analog anion surfactants separates efficiently and identifies.
Embodiment two
The present invention is applied in the middle of the detection of the sulfonic acid analog anion surfactants in the environmental water sample.Get the 1L washes, with 7 17 type strong-base anion-exchange resins (being quaternary ammonium type styrene-divinylbenzene strong basic type anion-exchange resin) with the anionic surfactant in the water advance enrichment and wash-out.Eluent is dried up with nitrogen, add the 0.2g potassium iodide successively, 10mLN, dinethylformamide, vibration is to dissolving fully.Drip 0.7mL (about 5m mol) trifluoro-acetic anhydride again, solution becomes peony immediately, and the generation of adularescent smog, and reaction is violent, separates out iodine.After treating that its color is no longer deepened, the solution of this moment promptly carries out the chromaticness analysis.Experimental result shows that potassium iodide and N, dinethylformamide and the trifluoro-acetic anhydride system of deriving is effective, in conjunction with the gas chromatography-mass spectrum detection technique, we can say the aromatic sulphonic acid compounds is separated efficiently with the aliphatic sulfonic compounds and identifies that the reduction system of therefore originally deriving should have good using value and prospect.
Claims (4)
1, the method for quick of sulfonic acid analog anion surfactants comprises the steps:
(1) be that 1: 1～10: 1 potassium iodide and sulfonic acid analog anion surfactants mix with mol ratio;
(2) in said mixture, add N, the dinethylformamide of 5～20ml/mol potassium iodide amount, be stirred to dissolving fully;
(3) add the trifluoro-acetic anhydride that 1～10 times of mole of potassium iodide is made a gesture of measuring, solution becomes redness.After color is no longer deepened, can carry out the sample introduction analysis;
(4) get above-mentioned solution and carry out conventional gas chromatography-mass spectrum detection.
2, the method for quick of sulfonic acid analog anion surfactants as claimed in claim 1 comprises the steps:
(1) be that 2: 1～8: 1 potassium iodide and sulfonic acid analog anion surfactants mix with mol ratio;
(2) in said mixture, add N, the dinethylformamide of 8～16ml/mol potassium iodide amount, be stirred to dissolving fully;
(3) add the trifluoro-acetic anhydride that 3～8 times of moles of potassium iodide are made a gesture of measuring, solution becomes redness.After color is no longer deepened, can carry out the sample introduction analysis;
(4) get above-mentioned solution and carry out conventional gas chromatography-mass spectrum detection.
3, the method for quick of sulfonic acid analog anion surfactants as claimed in claim 1 comprises the steps:
(1) be that 2: 1～6: 1 potassium iodide and sulfonic acid analog anion surfactants mix with mol ratio;
(2) in said mixture, add N, the dinethylformamide of 8～10ml/mol potassium iodide amount, be stirred to dissolving fully;
(3) add the trifluoro-acetic anhydride that 3～6 times of moles of potassium iodide are made a gesture of measuring, solution becomes redness.After color is no longer deepened, can carry out the sample introduction analysis;
(4) get above-mentioned solution and carry out conventional gas chromatography-mass spectrum detection.
4, the method for quick of sulfonic acid analog anion surfactants as claimed in claim 1 comprises the steps:
(1) be that 2: 1～8: 1 potassium iodide and sulfonic acid analog anion surfactants mix with mol ratio;
(2) in said mixture, add N, the dinethylformamide of 8～16ml/mol potassium iodide amount, be stirred to dissolving fully;
(3) add the trifluoro-acetic anhydride that 3～8 times of moles of potassium iodide are made a gesture of measuring, solution becomes redness.After color is no longer deepened, can carry out the sample introduction analysis;
(4) get above-mentioned solution and carry out conventional gas chromatography-mass spectrum detection.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102455319A (en) * | 2010-10-29 | 2012-05-16 | 中国科学院大连化学物理研究所 | Method for monitoring propofol narcotic in on-line manner |
| CN103543116A (en) * | 2013-09-24 | 2014-01-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Detection of sodium dodecyl benzene sulfonate in water by derivative spectrophotometry |
| CN106442771A (en) * | 2016-09-05 | 2017-02-22 | 上海上药第生化药业有限公司 | Detection method for determining sodium tetradecyl sulfate and related substances thereof |
| CN108562674A (en) * | 2018-07-26 | 2018-09-21 | 淄博职业学院 | The method that derivatization HPLC-UV methods measure methanesulfonates |
| CN114062352A (en) * | 2020-08-04 | 2022-02-18 | 中国石油天然气股份有限公司 | Method for identifying warm mixing agent containing amine surfactant in asphalt |
-
2007
- 2007-05-14 CN CNA2007100406176A patent/CN101308121A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102455319A (en) * | 2010-10-29 | 2012-05-16 | 中国科学院大连化学物理研究所 | Method for monitoring propofol narcotic in on-line manner |
| CN103543116A (en) * | 2013-09-24 | 2014-01-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Detection of sodium dodecyl benzene sulfonate in water by derivative spectrophotometry |
| CN106442771A (en) * | 2016-09-05 | 2017-02-22 | 上海上药第生化药业有限公司 | Detection method for determining sodium tetradecyl sulfate and related substances thereof |
| CN106442771B (en) * | 2016-09-05 | 2019-03-29 | 上海上药第一生化药业有限公司 | A kind of measurement sodium tetradecyl sulfate and its detection method in relation to substance |
| CN108562674A (en) * | 2018-07-26 | 2018-09-21 | 淄博职业学院 | The method that derivatization HPLC-UV methods measure methanesulfonates |
| CN108562674B (en) * | 2018-07-26 | 2021-06-15 | 淄博职业学院 | Method for measuring mesylate by derivatization HPLC-UV method |
| CN114062352A (en) * | 2020-08-04 | 2022-02-18 | 中国石油天然气股份有限公司 | Method for identifying warm mixing agent containing amine surfactant in asphalt |
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Open date: 20081119 |