CN104897665A - One-step color-development screening method for banned azo-dye in dyeing textiles - Google Patents
One-step color-development screening method for banned azo-dye in dyeing textiles Download PDFInfo
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Abstract
The invention discloses a one-step color-development screening method for banned azo-dye in dyeing textiles. The one-step color-development screening method comprises the following steps: (1) reducing a sample; (2) color-development, to be specific, at the same position of filter paper, dripping a drop of a color-developing agent, and then dripping 1-2 drops of tert-butyl methyl ether extracting solution for color development, wherein the color-developing agent is an ethanol solution comprising paradimethylaminobenzaldehyde with the mass-volume ratio of 0.1-10% and hydrochloric acid with the volume ratio of 10-25%; (3) screening and determination, to be specific, judging results according to the fact that whether obvious color change occurs or not after dripping the sample solution on the color-developing agent, wherein if no obvious color change occurs after color development of the sample solution, the sample does not contain a substance to be detected or the concentration of the substance to be detected is lower than the detection limitation, and the result is negative; if obvious color change occurs after color development of the sample solution, the sample is likely to contain the banned azo-dye, the result is positive, and further confirmation is required to be carried out by a chromatographic apparatus. The one-step color-development screening method is simple and fast, the sample can be directly subjected to color-development to be determined after being reduced, and the whole color development process can be completed within 1 min.
Description
Technical field
The present invention relates to a step colour developing screening method of forbidding azo dyes in a kind of dyed textiles, belong to technical field of analytical chemistry.
Background technology
From first regulation about Consumer Product Safety in the world: the state compulsory standard GB 18401-2003 " National Textile basic security technical manual " of the 97/548/EC instruction that " food and daily necessities method " that German federal government promulgated on April 10th, 1992 was passed through in 1997 to European Union and China, it is safety specifications most important, the most basic in the trade of International Textile clothes that the forbidding azo dyes being accused of carcinogenic aromatic amine detects always, is also simultaneously the focuses of attention of global consumers in general when consuming.
Up to the present, the detection method of a series of maturation has been put into effect for the test of forbidding azo dyes in fabric clothing both at home and abroad.But there is following problem in these class methods:
(1) degree of dependence of existing detection method to instrument is high
At present, forbid the detection method of aromatic amine in the yarn fabric clothes of all corresponding formulation of European Union, Germany and China, mainly adopt the instrument analytical method of gas chromatography, compounds GC-MS, liquid chromatography or liquid-mass chromatography isochromatic spectrum.Method is ripe, accurate, highly sensitive.But because pretreatment process is complicated, testing process needs to be equipped with exact instrument, round of visits is longer, Expenses of laboratory examination is high, testing conditions is harsh, strong to the dependence of large-scale chromatographic apparatus, to reasons such as the technical merit of practitioner have higher requirements, these class methods are made also to be only limitted to part laboratory with good conditionsi in application.
(2) sample size detected is large
China is the big export country of fabric clothing, the detection case of forbidding azo dyes from textile in recent years, a large amount of detection demands to detection technique efficient, fast propose challenge.
(3) positive recall rate is low
Along with the Environmental Safety consciousness of China's weaving, printing and dyeing, apparel industry strengthens gradually, positive research and development and use environmental protection type dye, auxiliary agent etc., the quality of exported product and greatly improving in the competitive power of international market, the recall rate of the objectionable impuritiess such as forbidding azo dyes reduces gradually.In recent years, actual detect in the verification and measurement ratio of textile forbidding azo dyes less than 1%.
For the problems referred to above, in current fabric clothing, in forbidding azo dyes testing, also establish some quick screening methods simple, quick, with low cost not needing to rely on large-scale chromatographic apparatus.200910192737.7) and the article " based on forbidding azo dyes fast qualitative screening technique in the textile that diazotising-coupling colour development reacts " delivered at analytical chemistry such as " in dyed textiles forbidding azo dyes method for quick " (patent No.: ZL 201110350255.7) and Ye Xiwen utilize the principle rapid screening of colour developing to detect the method for forbidding azo dyes in textile to appear in the newspapers in recent years, as Chinese patent " a kind of rapid screening detection method detected for forbidding azo dyes in the textile " (patent No.:.These class methods are according to the architectural feature of aromatic amine, introduce diazotising-coupling colour development reaction mechanism, development process is utilized to replace traditional chromatographic apparatus analysis, establish forbidding azo dyes rapid screening detection method in dyed textiles, detection technique achieves important breakthrough, is measure forbidding azo dyes in textile at present to detect method the most fast and effectively.
But still there is some defects and deficiency in said method.On the one hand: the sample pre-treatments of method, except the reduction of azo dyes, also needs to carry out t-butyl methyl ether and the liquid-liquid extraction of hydrochloric acid two step, to realize aromatic amine extraction and reactant liquor decolouring, step is still very loaded down with trivial details; On the other hand: whole process color is the diazonium coupled reaction process of aromatic amine and aldehydes matter, need use 4 kinds of reagent, multistep develops the color, and developing time needs about 15min.The method of whole pre-treatment is easy not enough, and quick not, the consuming time length of coloration method.
Summary of the invention
For the problems referred to above, the object of this invention is to provide a kind of faster, easier, and a step colour developing screening method of forbidding azo dyes in highly sensitive dyed textiles.
Reagent of the present invention only comprises a kind of developer, fills a prescription as follows: the paradime thylaminobenzaldehyde of mass volume ratio 0.1%-10% and volume ratio are the ethanolic solution of the hydrochloric acid of 10% ~ 25%.
Detection method step of the present invention is as follows:
(1) reduction of sample: textile samples with reference to EN 14362-1-2012 " textile some come from the assay method Part I of the aromatic amine of azo colouring agent: through or determine whether to employ the method for some azo colouring agent without extracting fiber " or the equivalent standard of technology contents carry out reduction pretreatment.Concrete steps are: take representative sample that 2.0g shreds in reaction bulb, add 16mL citrate buffer solution (0.06mol/L, and 3.0mL hydrogensulfite solution (200mg/mL pH=6), matching while using), reaction bulb is airtight, and firmly jolting, makes all samples be dipped in liquid, be placed in 70 ± 2 DEG C of water-baths and be incubated 30min, take out cool to room temperature in 2min.Add 0.5mL NaOH solution (40% aqueous solution), 7g sodium chloride, 5mL t-butyl methyl ether, firmly jolting, stratification (if solution milkiness is not stratified, can be centrifugal), gets upper strata t-butyl methyl ether extract chromogenic assay.
(2) develop the color: at the same position of filter paper, first drip a developer, then drip t-butyl methyl ether extract colour developing (sample extraction solution drops on developer) that 1-2 drips; If the t-butyl methyl ether extract layer of sample has color, then drip separately 1-2 at the blank position of filter paper and drip t-butyl methyl ether extract and contrast.
(3) screening judges: carry out judged result according to whether there is the change of obvious color after drip sample solution on developer.
Negative: the change of obvious color does not occur after sample solution colour developing, to represent in sample containing thing to be checked or its concentration lower than detectability.
Positive: the change of obvious color occurs after sample solution colour developing, then represent in sample and may contain forbidding azo dyes, need be confirmed further by chromatographic apparatus.
Wherein, described filter paper is filter paper at a slow speed.
The formula of described developer be preferably mass volume ratio be 1% paradime thylaminobenzaldehyde and volume ratio be the ethanolic solution of 25% hydrochloric acid.
Advantage of the present invention: the present invention adopts filter paper development process rapid screening aromatic amine, simply, fast, direct chromogenic assay after sample reduction, without the need to liquid-liquid extraction, without the need to concentrating, without the need to decolouring; Without the need to any instrument and equipment on measuring, only use a kind of developer, filter paper drips colour developing, naked eyes are seen and are looked into, and whole process color can complete in 1min.The present situation large for current textile forbidding azo dyes detection sample size, positive rate is low, this screening method is quick, accurate, low cost, really achieves the rapid screening of textile forbidding azo dyes.Due to without the need to equipment investment, cost is low, and technology is simple, is easy to grasp, makes it not only to can be used for the rapid screening of textile inspection mechanism but also can be used for the Self-control of manufacturing enterprise, be with a wide range of applications.
Accompanying drawing explanation
Fig. 1 has forbidding azo dyes operational flowchart in determination of color dyed textiles.
The operational flowchart of Fig. 2 the inventive method.
Embodiment
The present invention is further illustrated by specific embodiment below in conjunction with accompanying drawing.
The testing result of embodiment 1-29:29 actual cloth sample
First, developer formula: after 1g N, N-dimethyl-4-aminobenzaldehyde being added the dissolving of 75mL ethanol, add 25mL hydrochloric acid, use after mixing.
Secondly, detect containing 2-naphthylamines, parachloroanilinum, ortho-aminotoluene, 3 to the instrument collected, 3 '-dimethoxy benzidine, 5-nitro-o-toluidine, 2,4-diaminotoluene, 2,4-diamino anisoles and 4-aminoazabenzol etc. 8 kinds forbidding aromatic amine, content range is from 29 cloth samples of 5 mg/kg-557 mg/kg, measure according to step of the present invention, all develop the color, this method recall rate 100%, without false negative.Concrete steps are as follows:
(1) reduction of sample: take representative sample that 2.0g shreds in reaction bulb, add 16mL citrate buffer solution (0.06mol/L, and 3.0mL hydrogensulfite solution (200mg/mL pH=6), matching while using), reaction bulb is airtight, and firmly jolting, makes all samples be dipped in liquid, be placed in 70 ± 2 DEG C of water-baths and be incubated 30min, take out cool to room temperature in 2min.Add 0.5mL NaOH solution (40% aqueous solution), 7g sodium chloride, 5mL t-butyl methyl ether, firmly jolting, stratification (if solution milkiness is not stratified, can be centrifugal), gets upper strata t-butyl methyl ether extract chromogenic assay.
(2) develop the color: at the same position of filter paper at a slow speed, first drip a developer, then drip t-butyl methyl ether extract colour developing (sample extraction solution drops on developer) that 1-2 drips; If the t-butyl methyl ether extract layer of sample has color, then drip separately 1-2 at the blank position of filter paper and drip t-butyl methyl ether extract and contrast.
(3) screening judges: carry out judged result according to whether there is the change of obvious color after drip sample solution on developer.
Negative: the change of obvious color does not occur after sample solution colour developing, to represent in sample containing thing to be checked or its concentration lower than detectability.
Positive: the change of obvious color occurs after sample solution colour developing, then represent in sample and may contain forbidding azo dyes, need be confirmed further by chromatographic apparatus.
The concrete screening results of 29 actual cloth samples is as shown in table 1.
Table 1 the inventive method is to actual sample screening results
The detection limit of the inventive method:
For the detection limit of verification method, certain density aromatic amine standard solution is added citrate buffer solution and the rear chromogenic assay of hydrogensulfite solution reduction.After colour developing, naked eyes can be observed out comparatively significantly color and be changed to foundation, judge the method detection limit of this aromatic amine.
Concrete steps are: pipette 1mL 15mg/L and 1mL 30mg/L 24 kinds of carcinogenic aromatic amines and aniline standard solution respectively and add 16mL citrate buffer solution and 3.0mL hydrogensulfite solution, reaction bulb is airtight, firmly jolting, be placed in 70 ± 2 DEG C of water-baths and be incubated 30min, take out cool to room temperature in 2min.Add 0.5mL NaOH solution, 7g sodium chloride, 5mL t-butyl methyl ether, firmly jolting, stratification (if solution milkiness is not stratified, can be centrifugal).
Use filter paper at a slow speed, select the same position at filter paper, first drip a developer, then drip 1-2 and drip t-butyl methyl ether extract, colour developing.
The detection limit of method to 24 kinds of carcinogenic aromatic amines and aniline can reach 7.5mg/kg-15mg/kg.At present, it is 24 that European Union comprises the forbidding aromatic amine that German regulations specifies, detecting maximum limitation is on the textile 30mg/kg; Oeko-Tex standard 100 and China GB 18401 regulation forbidding aromatic amine are 24, and detecting maximum limitation is on the textile 20mg/kg.The detection limit of this method is lower than the Limited Doses that specifies of laws and regulations both at home and abroad at present.
Compared with existing testing methods of banned azo dyes in textiles, advantage of the present invention:
In textile, the detection of forbidding azo dyes is divided into two large steps usually.1st step is sample pre-treatments, and azo dyes is reduced to aromatic amine, and carries out purifying, concentrating.2nd step measures, and measures the aromatic amine content extracted.Compared with existing assay method, the technology of the present invention enormously simplify two large steps, achieves the rapid screening to forbidding azo dyes in dyed textiles.
(1) contrast with existing Instrument measuring method
Forbidding azo dyes examination criteria in domestic and international existing relevant textile, employing be the method that instrument detects.1st step sample pre-treatments generally adopts reduction, cross the means such as post is separated, concentrated, constant volume, and the 2nd pacing surely adopts the large-scale precision instruments such as gas chromatograph, gas chromatograph-mass spectrometer (GCMS) or liquid chromatograph to be separated, measures aromatic amine.These class methods are accurate, reliable, but complex pretreatment, need to be equipped with exact instrument, round of visits is longer, Expenses of laboratory examination is high, and need complete in the testing agency being equipped with professional and technical personnel, and condition is harsh.The technology of the present invention only need on filter paper chromogenic assay, rely on naked eyes explanation, without the need to any large-scale chromatographic apparatus equipment; Pre-treatment step only needs reduction one step, without the need to concentrated, purification; Whole experimental implementation is simple, reagent dosage is few, cost is low, the time is fast, and general enterprise laboratory also can independent operation.Specifically comparing as shown in table 2-table 4 in reagent cost, instrument cost, experiment are consuming time.Reagent cost needed for this method is 3% of existing instrument detection method; Required instrument cost is 0.6% of existing detection method; Detect 1 sample required time and be only 25% of existing detection method.
table 2 reagent cost contrasts
table 3 instrument cost contrasts
contrast consuming time tested by table 4
(2) contrast with existing quick screening method
Consult pertinent literature, the method utilizing the principle rapid screening of colour developing to detect forbidding azo dyes in textile has been reported, such as patent " a kind of rapid screening detection method detected for forbidding azo dyes in the textile " (patent No.: 200910192737.7); Patent " in dyed textiles forbidding azo dyes method for quick " (patent No.: ZL 201110350255.7).These class methods are according to the architectural feature of aromatic amine, introduce diazotising-coupling colour development reaction mechanism, traditional chromatographic apparatus analysis is replaced with development process, establish forbidding azo dyes rapid screening detection method in dyed textiles, dyed textiles forbidding azo dyes detection technique achieves important breakthrough, is measure forbidding azo dyes in textile at present to detect method the most fast and effectively.
But, in sample pre-treatments: the sample pre-treatments of these class methods, except the reduction of azo dyes, also needs to carry out t-butyl methyl ether and the liquid-liquid extraction of hydrochloric acid two step, to realize aromatic amine extraction and reactant liquor decolouring; Directly chromogenic assay can be carried out, without the need to other pre-treatment steps after the reduction of this method sample.In process color: existing patent and literature method, colour developing need use 4 kinds of reagent, and multistep develops the color, and developing time needs about 15min.The present invention's colour developing only needs a kind of developer, then the colour developing of filter paper previous step, and whole developing time can complete in 1min.As shown in Figure 1 and Figure 2.
Integrated comparative, method of the present invention is better than existing instrument and chromogenic assay method all greatly in sample pre-treatments and process color.Simple to operate, reagent dosage is few, speed is fast, cost is low.
Compared with existing similar development process, significant difference of the present invention:
Although having bibliographical information employing paradime thylaminobenzaldehyde is developer, colorimetric estimation urea, hydrazine, indoles, tryptophane, hydrazine etc., the present invention by comparison, has significant difference and more excellent effect.
1. filter paper color developing effect is obviously better than color comparison tube colour developing
Having been reported with paradime thylaminobenzaldehyde is the document that developer measures object, the color comparison tube colorimetric adopted without exception, the method for spectrophotometric determination.For contrast filter paper colour developing and color comparison tube develop the color significantly different, experiment adopts filter paper and plastic centrifuge tube colour developing respectively, wherein the step of filter paper colour developing is: use filter paper at a slow speed, select the same position at filter paper, first drip a developer, drip the aromatic amine standard solution of 2 30mg/L again, observe color developing effect (the inventive method).Centrifuge tube development step is: first drip a developer, then drip the aromatic amine standard solution of 2 30mg/L, mixing.
Experimental Comparison 12 aromatic amines two kinds of color developing effects: 7 aromatic amines, two kinds of equal naked eyes of colour developing mode such as the 4-aminobphenyl sensitive with chromogenic reagent, biphenylamine, 2-naphthylamines, 4-chloroaniline can distinguish that its color changes, and colour developing more insensitive 4-chloro-o-toluidine, 3,3 '-dimethoxy benzidine, 3,5 aromatic amines such as 3 '-dimethylbenzidine, filter paper development process can be observed visually obvious chromosphere and generate, and centrifuge tube color developing effect and blank are difficult to distinguish, cannot differentiate.The successful of filter paper colour developing is better than the colour developing in centrifuge tube.
Develop the color in centrifuge tube, the coloring matter that developer and object generate dissolves in organic solvent, and concentration reduces, display of light color, cannot distinguish by naked eyes after the aromatic amine colour developing causing developing portions weak; Filter paper development process, after organic solvent volatilization, the only surplus coloring matter generated, serve certain inspissation, color depth is dark.Meanwhile, chromogenic reagent solution itself is in yellow, and thus blank solution (1 developer+2 t-butyl methyl ether), also presents certain light yellow in centrifuge tube, but drop in filter paper is then shown as colourless.Visible, adopt filter paper method colour developing effectively can remove blank color, certain inspissation is played in the volatilization being simultaneously beneficial to organic solvent, is convenient to distinguishing of color and compares.This color just making traditional color comparison tube colourimetry distinguish, utilizes filter paper development process clearly to distinguish, realizes the colour developing screening of 25 kinds of amine substances.
2. filter paper chromogenic reagent consumption is few
In the detection pretreatment process of textile forbidding azo dyes, the extraction of 5mL t-butyl methyl ether is adopted after sample reduction, but due to reasons such as the absorptions with the miscible of aqueous phase and cloth, the t-butyl methyl ether used can be extracted after extraction and be only 2-3mL, according to spectrophotometry, only cuvette just at least needs the solution of 4mL, and according to the volume ratio of sample and developer 2:1, sample size is inadequate; The present invention only needs 1-2 to drip sample solution, and sample volume consumption is few, and remaining sample can provide later stage GC-MS qualitative, quantitative to confirm simultaneously and use.
3. simple and efficient
In spectrophotometry process, need to use spectrophotometer, the instrument and equipments such as color comparison tube, and color comparison tube only can be used for the colorimetric of a sample; This law only needs filter paper, dropper, distinguishes with naked eyes, and a filter paper can carry out the colour developing screening of multiple sample simultaneously, and simple and efficient, reagent consumables cost reduces greatly.
Claims (4)
1. a step colour developing examination method of forbidding azo dyes in dyed textiles, is characterized in that comprising the steps:
(1) sample reduction: take representative sample that 2.0g shreds in reaction bulb, add 16mL0.06mol/L, the hydrogensulfite solution that the citrate buffer solution of pH=6 and 3.0mL200mg/mL now join, reaction bulb is airtight, firmly jolting, make all samples be dipped in liquid, be placed in 70 ± 2 DEG C of water-baths and be incubated 30min, take out cool to room temperature in 2min; Add 0.5mL 40%NaOH solution, 7g sodium chloride, 5mL t-butyl methyl ether, firmly jolting, stratification, gets upper strata t-butyl methyl ether extract;
(2) develop the color: at the same position of filter paper, first drip a developer, then drip the t-butyl methyl ether extract colour developing that 1-2 drips; Described developer is the paradime thylaminobenzaldehyde of mass volume ratio 0.1% ~ 10% and the ethanolic solution of volume ratio 10% ~ 25% hydrochloric acid;
(3) screening judges: carry out judged result according to whether there is the change of obvious color after drip sample solution on developer: if there is not the change of obvious color after sample solution colour developing, to represent in sample containing thing to be checked or its concentration lower than detectability, result be feminine gender; If there is the change of obvious color after sample solution colour developing, then represent in sample and may contain forbidding azo dyes, result is positive, need be confirmed further by chromatographic apparatus.
2. a step colour developing examination method according to claim 1, is characterized in that described filter paper is for filter paper at a slow speed.
3. a step colour developing examination method according to claim 1, it is characterized in that the formula of described developer be preferably mass volume ratio be 1% paradime thylaminobenzaldehyde and volume ratio be the ethanolic solution of 25% hydrochloric acid.
4. a step colour developing examination method according to claim 1, is characterized in that the t-butyl methyl ether extract layer when sample has color, need drip separately 1-2 drip t-butyl methyl ether extract and contrast at the blank position of filter paper.
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| CN105891316A (en) * | 2016-04-26 | 2016-08-24 | 山东出入境检验检疫局检验检疫技术中心 | Method for simultaneously screening and analyzing forbidden and restricted dye in textiles |
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| CN111721881A (en) * | 2020-07-07 | 2020-09-29 | 东莞诺威检测认证有限公司 | Trifluoroacetylation GC-MS (gas chromatography-mass spectrometry) detection method for banned azo dyes of textiles |
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