CN104165952A - Method for detecting banned azo dyes in printing ink, coatings and paint - Google Patents
Method for detecting banned azo dyes in printing ink, coatings and paint Download PDFInfo
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- CN104165952A CN104165952A CN201410403270.7A CN201410403270A CN104165952A CN 104165952 A CN104165952 A CN 104165952A CN 201410403270 A CN201410403270 A CN 201410403270A CN 104165952 A CN104165952 A CN 104165952A
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Abstract
The invention provides a method for detecting banned azo dyes in printing ink, coatings and paint. The method comprises the following steps: performing reduction and decomposition on a sample in a sodium citrate buffer solution medium in the presence of sodium hydrosulfite to generate possible banned aromatic amine, then extracting aromatic amine from an extracting solution by a liquid-liquid extraction method, and detecting by GCMS with a mass selection detector. According to the method, methyl alcohol is used to extract disperse dyes in the sample, so that the disperse dyes in the sample can be extracted as much as possible, and other impurities in the sample are prevented from being extracted overmuch. A sodium hydroxide solution is added into a test tube so as to neutralize to obtain proper pH, and a generated amine substance is relative stable under the pH condition. Five milliliters of tert-butyl methyl ether is added to facilitate liquid-liquid extraction. A moderate amount of sodium sulfate is added so as to absorb water, accelerate layering and facilitate removing of part of impurities in an organic phase.
Description
Technical field
The present invention relates to a kind of detection method, refer to especially the detection method of forbidding azo dyes in a kind of ink, coating, paint.
Background technology
Azo dyes is kind maximum a kind of dyestuff quantitatively in existing Dyestuff Market, contains azo group and gain the name in dye molecule.Be widely used in dyeing and the stamp of multiple natural and synthon, also for painting, plastics, rubber etc. painted.These are with being prohibited after the clothes or other consumer goods and human body skin Long Term Contact of azo dye dyeing, can mix with the composition discharging in metabolic process, and produce reduction reaction, form carcinogenic aromatic amine compound, this compound can be absorbed by the body, through a series of activations, make the DNA recurring structure of human body cell and the variation of function, become the inducement of human lesion.Present forbidding Azo dye object is mainly for leather, textile, seldom has directly detecting with azo dyes for ink, paint, coating etc.
Summary of the invention
In view of this, the object of the invention is to propose a kind of can be directly for forbidding the detection method of azo dyes in the ink detecting with azo dyes of ink, paint, coating etc., coating, paint.
For solving the problems of the technologies described above, technology of the present invention by the following technical solutions:
A detection method of forbidding azo dyes in ink, coating, paint, comprises the following steps:
(1) extraction of disperse dyes
(1.1) by ink, paint drying and pulverize, standby as sample;
(1.2) take 1.0g sample in 50ml screw socket test tube with cover, and in test tube, add 25mL methyl alcohol, tighten test tube cap, be placed in 40 ℃ of water-bath ultrasound waves, ultrasonic extraction 60min;
(1.3) take out test tube and be cooled to room temperature, extracting liquid filtering, to 150ml round-bottomed flask, is then used to 5ml methyl alcohol drip washing test tube, leacheate is filtered in round-bottomed flask equally;
(1.4) filtrate is revolved and is steamed near dry with Rotary Evaporators under 50 ℃ of 300mbar conditions, with 2 * 1ml methyl alcohol, evaporate to dryness thing is transferred in clean tube;
(2) reductive cleavage
(2.1) in test tube, add 15mL to be preheated to the sodium citrate buffer of (70 ± 2) ℃, cover tightly test tube cap and test tube is placed in to (70 ± 2) ℃ water-bath insulation (30 ± 1) min;
(2.2) open test tube cap, add 3.0mL reductive agent, tighten test tube cap and firmly jolt, be then placed in (70 ± 2) ℃ water-bath insulation (30 ± 1) min;
(2.3) take out test tube, in 2min, test tube is cooled to room temperature;
(3) separation of amine
(3.1) in test tube, add the sodium hydroxide solution of 0.2mL 10%, tighten test tube cap and firmly jolt; In test tube, add again 5mL t-butyl methyl ether, tighten test tube cap, be placed on shaking table and jolt 30min under 250 turn/min;
(3.2) take off test tube, add anhydrous sodium sulfate in test tube, stratification, gets upper organic phase, crosses organic miillpore filter to 2mL gas chromatographic sample introduction bottle, for gc analysis.
Further, in described step (1.1), bake out temperature is 105 ℃.
Further, described step (1.3) if in filtrate do not clarify, again filter, until filtrate is clarification.
Further, the hydrosulfurous acid sodium solution that in described step (2.2), reductive agent is 200g/L.
Further, in described step (3.2), the filter opening footpath of organic miillpore filter is 0.22um.
The present invention where necessary, selects one or more methods to confirm isomeride, by the fiery gas chromatography/mass spectrometry of high performance liquid chromatography-Diode array detector (HPLC/PDA), is used in conjunction instrument analysis.
Normative reference: GB/T17592-2011, the mensuration of textile forbidding azo dyes;
GB/T 23344, the mensuration of textile 4-aminoazabenzol.
The beneficial effect that the present invention compared with prior art has is:
1) the present invention extracts the disperse dyes in sample with methyl alcohol, can extract as far as possible the disperse dyes in sample, can avoid again too much being extracted of other impurity in sample.
2) in test tube, add 0.2mL 10% sodium hydroxide solution, can in and PH, the amine substance of generation is more stable under this PH condition; Add 5mL t-butyl methyl ether, be beneficial to liquid-liquid extraction and extract, t-butyl methyl ether demand is few, can be cost-saving greatly, reduce operation.
3) the present invention adds appropriate countless sodium sulphate, can absorb water, and accelerates layering, and is conducive to remove the partial impurities in organic phase.
Embodiment
For allowing the more clear and intuitive understanding the present invention of those skilled in the art, below the present invention is further illustrated.
A detection method of forbidding azo dyes in ink, coating, paint, comprises the following steps:
(1) extraction of disperse dyes
(1.1) by drying and pulverize under ink, 105 ℃ of conditions of paint, standby as sample;
(1.2) take 1.0g sample in 50ml screw socket test tube with cover, and in test tube, add 25mL methyl alcohol, tighten test tube cap, be placed in 40 ℃ of water-bath ultrasound waves, ultrasonic extraction 60min;
(1.3) take out test tube and be cooled to room temperature, extracting liquid filtering, to 150ml round-bottomed flask, is then used to 5ml methyl alcohol drip washing test tube, leacheate is filtered in round-bottomed flask equally, if filtrate is not clarified, again filters, until filtrate is clarification;
(1.4) filtrate is revolved and is steamed near dry with Rotary Evaporators under 50 ℃ of 300mbar conditions, with 2 * 1ml methyl alcohol, evaporate to dryness thing is transferred in clean tube;
(2) reductive cleavage
(2.1) in test tube, add 15mL to be preheated to the sodium citrate buffer of 70 ℃, cover tightly test tube cap and test tube is placed in to 70 ℃ of water-baths is incubated 30min;
(2.2) open test tube cap, add the hydrosulfurous acid sodium solution of 3.0mL200g/L as reductive agent, tighten test tube cap and firmly jolt, be then placed in 70 ℃ of water-baths and be incubated 30min;
(2.3) take out test tube, in 2min, test tube is cooled to room temperature;
(3) separation of amine
(3.1) in test tube, add the sodium hydroxide solution of 0.2mL 10%, tighten test tube cap and firmly jolt; In test tube, add again 5mL t-butyl methyl ether, tighten test tube cap, be placed on shaking table and jolt 30min under 250 turn/min;
(3.2) take off test tube, add anhydrous sodium sulfate in test tube, stratification, gets upper organic phase, crosses the organic miillpore filter of 0.22um to 2mL gas chromatographic sample introduction bottle, for gc analysis.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. in ink, coating, paint, forbid a detection method for azo dyes, it is characterized in that, comprise the following steps:
(1) extraction of disperse dyes
(1.1) by ink, paint drying and pulverize, standby as sample;
(1.2) take 1.0g sample in 50ml screw socket test tube with cover, and in test tube, add 25mL methyl alcohol, tighten test tube cap, be placed in 40 ℃ of water-bath ultrasound waves, ultrasonic extraction 60min;
(1.3) take out test tube and be cooled to room temperature, extracting liquid filtering, to 150ml round-bottomed flask, is then used to 5ml methyl alcohol drip washing test tube, leacheate is filtered in round-bottomed flask equally;
(1.4) filtrate is revolved and is steamed near dry with Rotary Evaporators under 50 ℃ of 300mbar conditions, with 2 * 1ml methyl alcohol, evaporate to dryness thing is transferred in clean tube;
(2) reductive cleavage
(2.1) in test tube, add 15mL to be preheated to the sodium citrate buffer of (70 ± 2) ℃, cover tightly test tube cap and test tube is placed in to (70 ± 2) ℃ water-bath insulation (30 ± 1) min;
(2.2) open test tube cap, add 3.0mL reductive agent, tighten test tube cap and firmly jolt, be then placed in (70 ± 2) ℃ water-bath insulation (30 ± 1) min;
(2.3) take out test tube, in 2min, test tube is cooled to room temperature;
(3) separation of amine
(3.1) in test tube, add the sodium hydroxide solution of 0.2mL 10%, tighten test tube cap and firmly jolt; In test tube, add again 5mL t-butyl methyl ether, tighten test tube cap, be placed on shaking table and jolt 30min under 250 turn/min;
(3.2) take off test tube, add anhydrous sodium sulfate in test tube, stratification, gets upper organic phase, crosses organic miillpore filter to 2mL gas chromatographic sample introduction bottle, for gc analysis.
2. in ink according to claim 1, coating, paint, forbid the detection method of azo dyes, it is characterized in that: in described step (1.1), bake out temperature is 105 ℃.
3. in ink according to claim 2, coating, paint, forbid the detection method of azo dyes, it is characterized in that: described step (1.3) if in filtrate do not clarify, again filter, until filtrate is clarification.
4. in ink according to claim 3, coating, paint, forbid the detection method of azo dyes, it is characterized in that: the hydrosulfurous acid sodium solution that in described step (2.2), reductive agent is 200g/L.
5. in ink according to claim 4, coating, paint, forbid the detection method of azo dyes, it is characterized in that: in described step (3.2), the filter opening footpath of organic miillpore filter is 0.22um.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410403270.7A CN104165952A (en) | 2014-08-15 | 2014-08-15 | Method for detecting banned azo dyes in printing ink, coatings and paint |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410403270.7A CN104165952A (en) | 2014-08-15 | 2014-08-15 | Method for detecting banned azo dyes in printing ink, coatings and paint |
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| CN201410403270.7A Pending CN104165952A (en) | 2014-08-15 | 2014-08-15 | Method for detecting banned azo dyes in printing ink, coatings and paint |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105486794A (en) * | 2015-12-25 | 2016-04-13 | 广州广电计量检测股份有限公司 | Method for detecting banned dye in printing ink |
| CN106990189A (en) * | 2017-06-12 | 2017-07-28 | 浙江唯质检测技术服务有限公司 | A kind of detection method of textile forbidding azo dyes |
| CN109541080A (en) * | 2019-01-16 | 2019-03-29 | 深圳天祥质量技术服务有限公司 | The detection method of azo dyes in water |
| CN110389189A (en) * | 2019-07-19 | 2019-10-29 | 日染检(南通)纺织品检测中心有限公司 | A kind of Determination of Banned Azo Dyes in Leather detection method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105486794A (en) * | 2015-12-25 | 2016-04-13 | 广州广电计量检测股份有限公司 | Method for detecting banned dye in printing ink |
| CN106990189A (en) * | 2017-06-12 | 2017-07-28 | 浙江唯质检测技术服务有限公司 | A kind of detection method of textile forbidding azo dyes |
| CN109541080A (en) * | 2019-01-16 | 2019-03-29 | 深圳天祥质量技术服务有限公司 | The detection method of azo dyes in water |
| CN110389189A (en) * | 2019-07-19 | 2019-10-29 | 日染检(南通)纺织品检测中心有限公司 | A kind of Determination of Banned Azo Dyes in Leather detection method |
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Application publication date: 20141126 |