CN102507561A - Rapid detection kit and detection method of forbidden azo dyes in dyed textiles - Google Patents
Rapid detection kit and detection method of forbidden azo dyes in dyed textiles Download PDFInfo
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- CN102507561A CN102507561A CN2011103502557A CN201110350255A CN102507561A CN 102507561 A CN102507561 A CN 102507561A CN 2011103502557 A CN2011103502557 A CN 2011103502557A CN 201110350255 A CN201110350255 A CN 201110350255A CN 102507561 A CN102507561 A CN 102507561A
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Abstract
The invention discloses a rapid detection kit of forbidden azo dyes in dyed textiles, which comprises: 1) an extracting reagent A: 10 mL of methyl ten-butyl ether; 2) an extracting reagent B: 5 mL of 0.1-1.0 mol/L hydrochloric acid solution; 3) a reagent 1: 0.05 mL of 50 g/L NaNO2 solution; 4) a reagent 2: 0.5 mL of 25 g/L NH4SO3NH2 solution; 5) a reagent 3: 1 mL of o-metoxyphenol ethanol aqueous solution with volume percentage concentration of 2%; 6) a reagent 4: 1 mL of 0.5 mol/L NaOH solution; 7) a reducing agent 1: 16 mL of 0.06 mol/L citrate buffering solution with pH of 6.0; and 8) a reducing agent 2: 3.0 mL of 200 mg/L sodium hydrosulfite solution. According to the invention, the pre-treatment is realized by liquid-liquid extraction of textile reduction solution and discoloring, and the aromatic amine is measured by coloration; the pre-treatment is simple and rapid enough to greatly simplify the original steps, and no instrument or equipment is necessary in the measurement so as to realize the quick screening detection of forbidden azo dyes in textiles.
Description
Technical field
The present invention relates to the rapid screening detection method of forbidding azo dyes in a kind of dyed textiles, belong to technical field of analytical chemistry.
Background technology
The forbidding azo dyes is to import and export one of project that textile must examine.As far back as 1994, German Government took the lead in having issued " food and daily necessities method " (second amendment), forbade producing the textile that produces the azo dye dyeing of carcinogenic aromatic amine with intake energy.On September 11st, 2002; European Community's Official Journal is formally issued the 2002/61/EC instruction; Regulation can be disengaged the azo dyes of the concentration of forbidding aromatic amine above 30 mg/kg; Must not be used for the textile or the leather and fur products that possibly directly contact for a long time with human body skin or oral cavity, like clothes, bedding, towel, wig, cap etc.The textile product state compulsory standard GB 18401 of China " national textile product basic security technical manual " also can decompose the basic security technical requirement that the aromatic amine dyestuff is listed textile product in.
Domestic and international existing testing methods of banned azo dyes pre-treatment generally adopts reduction, cross means such as post separates, concentrates, constant volume, measures large-scale precision instruments such as adopting gas chromatograph, gas chromatograph-mass spectrometer (GCMS) or liquid chromatograph and separates, measures.Though these class methods accurately, reliable, complex pretreatment, need to be equipped with that instrument is accurate, round of visits is long, survey fees are with high, and the technical professional arranged, condition is harsh.
Summary of the invention
To the problems referred to above, the purpose of this invention is to provide a kind of simple to operate, quick, need not extras, and forbidding azo dyes quick detection kit and detection method thereof in the highly sensitive dyed textiles.
Ultimate principle of the present invention is: azo dyes is reduced the general colourless or very slight color of aromatic amine that degraded forms, and the product after the aromatic amine diazotising can generate the azo-compound colour developing with azo reagent generation coupling reaction.Utilize this principle, after the azo dyes reduction that contains in the textile, adopt effective method to decolour reducing solution, and the extraction aromatic amine compound; Under suitable diazotising-coupling condition, make the aromatic amine compound of extraction change into coloured azo-compound colour developing again; Final basis has or not the depth of color and color to make quick, preliminary judgement to whether containing the forbidding azo dyes in the textile apace.
Kit of the present invention comprises:
1) extracts reagent A: methyl tertiary butyl ether, 10mL;
2) extract reagent B:0.1 mol/L-1.0mol/L hydrochloric acid solution, 5mL;
3) reagent 1:50g/L NaNO
2Solution, 0.05mL;
4) reagent 2:25g/L NH
4SO
3NH
2Solution, 0.5mL;
5) reagent 3: concentration expressed in percentage by volume is 2% o-methoxyphenol ethanol water, 1mL; Compound method: after getting the 2mL o-methoxyphenol and adding 20 mL dissolve with ethanol, add water and be settled to 100mL;
6) reagent 4:0.5mol/L NaOH solution, 1mL;
7) go back original reagent 1:0.06mol/L, pH=6.0 citrate buffer, 16mL; Compound method: take by weighing citric acid 12.526g and NaOH 6.320g, be dissolved in the 1000mL water;
8) go back original reagent 2:200mg/mL hydrosulfurous acid sodium solution, 3.0mL.
Detection method step of the present invention is following:
1) reduction of sample: the standard that textile samples is equal to reference to the GB/T 17592-2006 mensuration of azo dyes " textile forbidding " or technology contents is reduced pre-service.Concrete steps are: take by weighing representative sample that 1.0g shreds in reaction bulb, add also original reagent 1 and 3.0mL original reagent 2 also of 16mL, and reaction bulb is airtight; Firmly jolting; All samples are dipped in the liquid, place 70 ± 2 ℃ of water-baths insulation 30min after, take out cool to room temperature in 2min;
2) extraction and decolouring: reducing solution is changed in the bottle that 10mL extraction reagent A is housed, firmly jolting, standing demix is got upper strata liquid in the bottle that 5mL extraction reagent B is housed, the jolting of exerting oneself, standing demix takes off layer solution in empty reaction bulb C;
3) colour developing: in reaction bulb C, drip 0.05mL reagent 1, shake up the back and place 10min, drip 0.5mL reagent 2 again, ultrasonic or oscillating reactions 2min adds 1mL reagent 3, and 1mL reagent 4 shakes up;
4) screening is judged: if obvious change color takes place in sample solution colour developing back, can be judged to be positive sample, further confirm through chromatographic apparatus, otherwise negative, directly be judged to be qualified samples.
The present invention adopts the method for liquid-liquid extraction textile reducing solution and decolouring to carry out pre-treatment; Through the chromogenic assay aromatic amine, pre-treatment is simple, quick, has simplified in steps former greatly; Need not any instrument and equipment on the mensuration, realized that the rapid screening that textile forbidding azo dyes detects detects.Owing to need not the equipment input, cost is low, and technology is simple, is easy to grasp, and makes it the self check automatic control that not only can be used for the rapid screening of textile testing agency but also can be used for manufacturing enterprise, is with a wide range of applications.
Embodiment
Further specify the present invention through specific embodiment below.
1,10 actual sample testing results.
Instrument detecting is gone out to contain 10 cloth samples of aromatic amines such as 2-naphthylamines, biphenylamine, parachloroanilinum, measure according to rapid screening detection method of the present invention, the kit that adopts comprises: extract reagent A: methyl tertiary butyl ether, 10mL; Extract reagent B:0.3mol/L hydrochloric acid solution, 5mL; Reagent 1:50g/L NaNO
2Solution, 0.05mL; Reagent 2:25g/L NH
4SO
3NH
2Solution, 0.5mL; Reagent 3: concentration expressed in percentage by volume is 2% o-methoxyphenol ethanol water, 1mL; Reagent 4:0.5mol/L NaOH solution, 1mL; Original reagent 1:0.06mol/L also, pH=6.0 citrate buffer, 16mL; Original reagent 2:200mg/mL hydrosulfurous acid sodium solution also, 3.0mL.
Concrete detection method step is following:
1) reduction of sample: take by weighing representative sample that 1.0g shreds in reaction bulb; Add also original reagent 1 and 3.0mL original reagent 2 also of 16mL; Reaction bulb is airtight, and firmly jolting is dipped in the liquid all samples; After placing 70 ± 2 ℃ of water-bath insulation 30min, take out cool to room temperature in 2min;
2) extraction and decolouring: reducing solution is changed in the bottle that 10mL extraction reagent A is housed, firmly jolting, standing demix is got upper strata liquid in the bottle that 5mL extraction reagent B is housed, the jolting of exerting oneself, standing demix takes off layer solution in empty reaction bulb C;
3) colour developing: in reaction bulb C, drip 0.05mL reagent 1, shake up the back and place 10min, drip 0.5mL reagent 2 again, ultrasonic or oscillating reactions 2min adds 1mL reagent 3, and 1mL reagent 4 shakes up;
4) screening is judged: if obvious change color takes place in sample solution colour developing back, can be judged to be positive sample, further confirm through chromatographic apparatus, otherwise negative, directly be judged to be qualified samples.
Extract before above-mentioned 10 samples colour developing is colourless, adds behind the developer extract and all shows various colors such as redness, orange red, yellow, and the recall rate of method is 100%, no false negative.
Concrete experimental result is as shown in table 1:
10 positive testing results of table 1
2, false positive probability
The aniline category matter that generates behind the reducing dyes (like aniline, p-phenylenediamine (PPD)) has identical chromogenic reaction under this experiment condition, method is had interference, false-positive result can occur.Running into this type of situation need further prove conclusively with chromatographic apparatus.Application this method does not contain the sample of forbidding azo dyes to 1001 instrument detecting and carries out the rapid screening detection, and wherein, 721 sample extracting solutions do not develop the color, and can directly be judged to be feminine gender, and false positive results appears in 280 sample extracting solutions colour developings.False-positive probability is 28%.
3, method detection limit
Be the detection limit of verification method, certain density aromatic amine standard solution is added citrate buffer solution and sodium hydrosulfite solution reduction after, extraction, chromogenic assay.After adding developer, naked eyes can observe out comparatively that obvious color is changed to foundation, judge the method detection limit of this aromatic amine.
Concrete steps are: pipette 23 kinds of aromatic amine standard solution of 1mL 15mg/L or 30mg/L and join 16mL also original reagent 1 and 3.0mL also in the mixed solution of original reagent 2; Reaction vessel is airtight; Firmly jolting; All samples are dipped in the liquid, place 70 ± 2 ℃ of water-baths insulation 30min after, take out cool to room temperature in 2min.Reducing solution is changed in the bottle that the extraction reagent A is housed, firmly jolting, standing demix is got upper strata liquid in the bottle that extracts reagent B is housed, the jolting of exerting oneself, standing demix takes off layer solution in empty reaction bulb C.In reaction bulb C, drip 0.05mL reagent 1, shake up the back and place 10min, drip 0.5mL again and drip reagent 2, ultrasonic reaction 2min adds 1mL reagent 3, and 1mL reagent 4 shakes up.Draw this method the detection limit of various aromatic amines seen table 2:
The detection limit of 23 kinds of aromatic amines of table 2
4, the scope of application
The detection of forbidding azo dyes in the textile product, the pre-treatment of sample has two kinds of methods, and a kind of is that directly reduction is handled, and another kind is to need extraction earlier, and then reduction is handled.Technology of the present invention is applicable to and can handles the textile product of measuring the forbidding azo dyes through direct reduction.
5, compare advantage of the present invention with existing method
The detection of forbidding azo dyes is divided into two big steps usually in the textile: the 1st step was a sample pre-treatments, and azo dyes is reduced to aromatic amine, and purified, concentrates; The 2nd step was to measure, and measured the aromatic amine content that extracts.Compare with existing assay method, technology of the present invention has been simplified two big steps greatly, has realized the rapid screening to forbidding azo dyes in the dyed textiles.
(1) with existing Instrument measuring method contrast, simplified determination step
Forbidding azo dyes examination criteria in the existing both at home and abroad relevant textile, employing be the method for instrument detecting.The 1st step sample pre-treatments generally adopts reduction, cross means such as post separates, concentrates, constant volume, and the 2nd pacing adopts surely that large-scale precision instruments such as gas chromatograph, gas chromatograph-mass spectrometer (GCMS) or liquid chromatograph separate, the mensuration aromatic amine.Though these class methods accurately, reliable, complex pretreatment needs to be equipped with exact instrument, round of visits is long, survey fees are with high, and needs to accomplish in the testing agency that is equipped with the professional and technical personnel, condition is harsh.Technology of the present invention need not any instrument and equipment, but pre-treatment step is reduced to also independent operation of reduction and two steps of extraction decolouring, simple to operate, reagent dosage is few, cost is low, general enterprise laboratory.
(2) with existing quick screening method contrast, simplified the pre-treatment process
Consult pertinent literature, utilize the principle rapid screening of colour developing to detect the existing report of the method for forbidding azo dyes in the textile, these class methods only are to decide step in the 2nd pacing to simplify, and the aromatic amine in the extract is through chromogenic assay, but not Instrument measuring.The 1st step sample pre-treatments then is equal to the standard that the existing GB/T 17592-2006 mensuration of azo dyes " textile forbidding " or technology contents are equal to fully.Textile need pass through reduction, cross post separates, concentrates and complex process such as dissolve with methanol constant volume; In contrast to this; Method of the present invention has not only been introduced the colour developing principle and has been measured aromatic amine, has simplified pre-treatment step especially, and will reduce, cross post and separate, concentrate and a series of complex process such as dissolving constant volume are reduced to: reduction and extraction decolouring two go on foot; The whole operation process does not rely on any instrument and equipment, has realized simply, purpose fast.
Claims (4)
1. forbid the azo dyes quick detection kit in a dyed textiles, it is characterized in that it comprises:
1) extracts reagent A: methyl tertiary butyl ether, 10mL;
2) extract reagent B:0.1mol/L-1.0mol/L hydrochloric acid solution, 5mL;
3) reagent 1:50g/L NaNO
2Solution, 0.05mL;
4) reagent 2:25g/L NH
4SO
3NH
2Solution, 0.5mL;
5) reagent 3: concentration expressed in percentage by volume is 2% o-methoxyphenol ethanol water, 1mL;
6) reagent 4:0.5mol/L NaOH solution, 1mL;
7) go back original reagent 1:0.06mol/L, pH=6.0 citrate buffer, 16mL;
8) go back original reagent 2:200mg/mL hydrosulfurous acid sodium solution, 3.0mL.
2. quick detection kit according to claim 1 is characterized in that the compound method of said reagent 3 is following: after getting the 2mL o-methoxyphenol and adding 20 mL dissolve with ethanol, add water and be settled to 100mL.
3. quick detection kit according to claim 1 is characterized in that said compound method of going back original reagent 1 is following: take by weighing citric acid 12.526g and NaOH 6.320g, be dissolved in the 1000mL water.
4. forbid the azo dyes method for quick in a dyed textiles, it is characterized in that comprising that step is following:
1) reduction of sample: take by weighing representative sample that 1.0g shreds in reaction bulb; Add also original reagent 1 and 3.0mL original reagent 2 also of 16mL; Reaction bulb is airtight, and firmly jolting is dipped in the liquid all samples; After placing 70 ± 2 ℃ of water-bath insulation 30min, take out cool to room temperature in 2min;
2) extraction and decolouring: reducing solution is changed in the bottle that 10mL extraction reagent A is housed, firmly jolting, standing demix is got upper strata liquid in the bottle that 5mL extraction reagent B is housed, the jolting of exerting oneself, standing demix takes off layer solution in empty reaction bulb C;
3) colour developing: in reaction bulb C, drip 0.05mL reagent 1, shake up the back and place 10min, drip 0.5mL reagent 2 again, ultrasonic or oscillating reactions 2min adds 1mL reagent 3, and 1mL reagent 4 shakes up;
4) screening is judged: if obvious change color takes place in sample solution colour developing back, can be judged to be positive sample, further confirm through chromatographic apparatus, otherwise negative, directly be judged to be qualified samples.
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|---|---|---|---|
| CN 201110350255 CN102507561B (en) | 2011-11-08 | 2011-11-08 | Rapid detection kit and detection method of forbidden azo dyes in dyed textiles |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110350255 CN102507561B (en) | 2011-11-08 | 2011-11-08 | Rapid detection kit and detection method of forbidden azo dyes in dyed textiles |
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| CN102507561A true CN102507561A (en) | 2012-06-20 |
| CN102507561B CN102507561B (en) | 2013-03-27 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102798677A (en) * | 2012-08-27 | 2012-11-28 | 江苏出入境检验检疫局工业产品检测中心 | Method for quickly screening and detecting azo dyes forbidden in textile materials, leathers and dyes using gas chromatography mass spectrometry |
| CN103033579A (en) * | 2012-12-27 | 2013-04-10 | 通标标准技术服务(上海)有限公司 | Rapid determination method for content of banned azo dye |
| CN103091314A (en) * | 2013-01-16 | 2013-05-08 | 深圳市计量质量检测研究院 | Rapid detection method for water-soluble azo dyes in foods |
| CN104897665A (en) * | 2015-06-10 | 2015-09-09 | 山东出入境检验检疫局检验检疫技术中心 | One-step color-development screening method for banned azo-dye in dyeing textiles |
| CN105277552A (en) * | 2015-11-18 | 2016-01-27 | 福州大学 | Device for online detection of azo coloring agents and using method of device |
| CN105588832A (en) * | 2015-12-10 | 2016-05-18 | 厦门华厦学院 | Device and method for rapidly detecting basic orange, acid orange and basic tender yellow |
| CN105987901A (en) * | 2015-01-27 | 2016-10-05 | 江苏省微生物研究所有限责任公司 | Quick detection kit for forbidden azo dye in foods and detection method of same |
| CN106153780A (en) * | 2016-07-29 | 2016-11-23 | 杭州吉华江东化工有限公司 | A kind of detect the method for organochlorine residue in azo dye product |
| CN106442275A (en) * | 2016-09-18 | 2017-02-22 | 中国人民武装警察部队总医院 | Method and kit for qualitatively detecting chyle |
| CN106596232A (en) * | 2016-12-13 | 2017-04-26 | 广州大学 | Silver staining kit for detecting DNA in polyacrylamide gel and application of silver staining kit |
| CN108181278A (en) * | 2017-12-28 | 2018-06-19 | 上海烟草集团有限责任公司 | The assay method for the aromatic amine that azo dyes releases in a kind of paper material |
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| CN109557069B (en) * | 2018-05-30 | 2021-06-25 | 厦门市普识纳米科技有限公司 | Raman detection method for forbidden azo dyes |
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| CN102798677B (en) * | 2012-08-27 | 2014-01-29 | 江苏出入境检验检疫局工业产品检测中心 | Method for quickly screening and detecting azo dyes forbidden in textile materials, leathers and dyes using gas chromatography mass spectrometry |
| CN102798677A (en) * | 2012-08-27 | 2012-11-28 | 江苏出入境检验检疫局工业产品检测中心 | Method for quickly screening and detecting azo dyes forbidden in textile materials, leathers and dyes using gas chromatography mass spectrometry |
| CN103033579A (en) * | 2012-12-27 | 2013-04-10 | 通标标准技术服务(上海)有限公司 | Rapid determination method for content of banned azo dye |
| CN103091314A (en) * | 2013-01-16 | 2013-05-08 | 深圳市计量质量检测研究院 | Rapid detection method for water-soluble azo dyes in foods |
| CN105987901A (en) * | 2015-01-27 | 2016-10-05 | 江苏省微生物研究所有限责任公司 | Quick detection kit for forbidden azo dye in foods and detection method of same |
| CN104897665A (en) * | 2015-06-10 | 2015-09-09 | 山东出入境检验检疫局检验检疫技术中心 | One-step color-development screening method for banned azo-dye in dyeing textiles |
| CN105277552B (en) * | 2015-11-18 | 2018-10-30 | 福州大学 | A kind of device and its application method for azo colouring agent on-line checking |
| CN105277552A (en) * | 2015-11-18 | 2016-01-27 | 福州大学 | Device for online detection of azo coloring agents and using method of device |
| CN105588832A (en) * | 2015-12-10 | 2016-05-18 | 厦门华厦学院 | Device and method for rapidly detecting basic orange, acid orange and basic tender yellow |
| CN106153780A (en) * | 2016-07-29 | 2016-11-23 | 杭州吉华江东化工有限公司 | A kind of detect the method for organochlorine residue in azo dye product |
| CN106442275A (en) * | 2016-09-18 | 2017-02-22 | 中国人民武装警察部队总医院 | Method and kit for qualitatively detecting chyle |
| CN106596232A (en) * | 2016-12-13 | 2017-04-26 | 广州大学 | Silver staining kit for detecting DNA in polyacrylamide gel and application of silver staining kit |
| CN106596232B (en) * | 2016-12-13 | 2019-04-30 | 广州大学 | The silver staining kit of DNA and its application in a kind of detection polyacrylamide gel |
| CN108181278A (en) * | 2017-12-28 | 2018-06-19 | 上海烟草集团有限责任公司 | The assay method for the aromatic amine that azo dyes releases in a kind of paper material |
| CN113125428A (en) * | 2021-04-16 | 2021-07-16 | 青岛海关技术中心 | Method for rapidly screening phthalate in plastics and textiles |
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