CN104155380A - Detection method for banned azo-dye in textile - Google Patents
Detection method for banned azo-dye in textile Download PDFInfo
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- CN104155380A CN104155380A CN201410403275.XA CN201410403275A CN104155380A CN 104155380 A CN104155380 A CN 104155380A CN 201410403275 A CN201410403275 A CN 201410403275A CN 104155380 A CN104155380 A CN 104155380A
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Abstract
The invention provides a detection method for banned azo-dye in a textile. The method comprises the following steps: (a) sampling and sample cutting, wherein glue and attachments on samples are cleaned as much as possible and different samples are respectively processed; (b) pretreatment and reductive decomposition of the samples; and (c) extraction and measurement of results. According to the invention, 5 mL of t-butyl methyl ether is added and the principles of liquid-liquid extraction are employed to extract amine substances in extract; a few amount of anhydrous sodium sulfate is added to remove moisture in an organic phase and to allow samples floating between two phases to settle down to the bottom, which is beneficial for absorption of the organic phase; and screening with such a method needs short time and low cost.
Description
Technical field
The present invention relates to forbid in a kind of textile the detection method of azo dyes, belong to chemical detection technique field.
Background technology
Azo dyes is quantitatively maximum a kind of dyestuff of kind in existing Dyestuff Market, gains the name by containing azo group 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, make the DNA recurring structure of human body cell and the variation of function through a series of activations, become the inducement of human lesion.GB/T17592-2011, mensuration, the GB/T 23344 of textile forbidding azo dyes, the mensuration of textile 4-aminoazabenzol, the method is for quantitative method, relatively produces shortcoming many, as high in cost, consuming time for a long time, can not batch operation etc.
Summary of the invention
The object of the present invention is to provide the detection method of forbidding azo dyes in a kind of textile, the method is cost-saved, reduces operation, is applicable to produce in enormous quantities.
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 textile, comprises the following steps:
(a) sampling and sample cutting
Remove as far as possible neatly glue, attachment above sample, and different samples processed respectively:
(a1) as requested or grab sample,, for complicated sample, sampling spot need have mark and photo;
(a2) for the fabric that is printed on multicolour pattern, should sample be subdivided into solid color as far as possible, unlike material on product, or the fabric of different colours should sample respectively;
(a3) containing the fabric sample of dacron: the sample of getting is cut into 20mm × 30mm size, mixes;
(a4) not containing the fabric sample of dacron: the sample of getting is cut into 5mm × 5mm size, mixes;
(b) sample pretreatment and reduction decomposition reaction
(b1) containing the textile of dacron
From compound sample, take 1.000g sample, tighten with colourless yarn, in the vaporium of extraction equipment, vertically place, condensing solvent can be flow through from sample; In extraction equipment, add 25mL Benzene Chloride extracting 30 min, make color sample to the greatest extent de-; Extract cool to room temperature, on vacuum rotary evaporator, 45 DEG C～60 DEG C expulsion solvents, obtain a small amount of residue, and residue is transferred in 50mL test tube with 2mL methyl alcohol; In above-mentioned test tube, add 15mL and be preheated to the citrate buffer solution of (70 ± 2 DEG C), cover tightly cap test tube and test tube is put into ultrasound bath pot insulation (30 ± 1) min of (70 ± 2 DEG C); Open test tube cap, add 3mL 200mg/mL hydrosulfurous acid sodium solution, airtight rear firmly jolting, is incubated (30 ± 1) min again in (70 ± 2 DEG C) water-bath at once; After taking out test tube, in 2min, test tube is cooled to rapidly to room temperature;
(b2) not containing the textile of dacron
From compound sample, take 1.0000g sample and be placed in 50mL test tube; The citrate buffer solution that interpolation 17mL is preheated to (70 ± 2 DEG C), in test tube, covers tightly cap test tube firmly jolting, makes all fabrics fully wetting, insulation (30 ± 1) min in the water-bath of (70 ± 2 DEG C); Open test tube cap, add 3mL reductive agent, airtight rear jolting at once, is incubated (30 ± 1) min again in (70 ± 2 DEG C) water-bath; After taking out test tube, in 2min, with frozen water mixing water-bath, test tube is cooled to rapidly to room temperature;
(c) extraction (sieve counting method)
(c1) in test tube, add 5mL t-butyl methyl ether inner mark solution to extract amine substance, cover tightly lid, be placed in 250rmp/min concussion 30min on mechnical oscillator;
(c2) take off test tube, add 0.1-1g anhydrous sodium sulfate to dewater, get supernatant liquid and analyze on gas chromatograph-mass spectrometer (GCMS).
Further, if need first filter with 0.22um filtering head when in described step (c2), supernatant is muddy, when on the rear gas chromatograph-mass spectrometer (GCMS) of do not filter or filtration, test result is positive, in textile, forbid the detection of azo dyes from step (a) and (b), then use following methods instead and resurvey:
(d) extraction
First with the sample in glass bar extruding test tube, reactant liquor in test tube is all poured in zeyssatite extraction column, leave standstill and absorb 15min, then directly add 4 × 20mL ether and divide the sample in elution reaction device four times, need to mix ether and sample at every turn, then ether washing lotion is poured in extraction column, coutroi velocity, collects all eluants in 150mL flat bottom flask;
(e) concentrated
The above-mentioned flat bottom flask that fills ether extracted liquid is placed on vacuum rotary evaporator, under the vacuum tightness of (35 DEG C ± 2 DEG C) 10E5-10E2 Pa, is concentrated into nearly 1mL, then with the slow nitrogen stream of inert gas expulsion diethyl ether solution, it is concentrated near dry;
(f) interpretation of result
(f1) gas chromatograph-mass spectrometer (GCMS) analysis: accurately pipette and mark standard solution in the deuterated anthracene of 10mg/L of 1.0mL methyl alcohol preparation and be concentrated in nearly dry flat bottom flask to above-mentioned, mix, leave standstill, use 0.22um organic system filtering with microporous membrane to 2mL sample bottle to analyze for GC-MS.
(f2) HPLC/PDA analyzes: accurately pipette 1mL methyl alcohol and add above-mentioned being concentrated in nearly dry flat bottom flask, mix, leave standstill, use 0.22um organic system filtering with microporous membrane to 2mL sample bottle to analyze for HPLC/PDA.
Further, described step (f) if in can not complete instrumental analysis in 24 hours, sample need to be no more than one week lower than-18 DEG C of preservations.
The beneficial effect that the present invention compared with prior art has is:
1) in primary standard, add the amine substance in extracted with diethyl ether extract, and need to cross siliceous earth column, concentrated through selecting evaporimeter again, last constant volume, cost is very high, this sieve counting method utilizes t-butyl methyl ether, amine substance in liquid-liquid extraction principle extraction extract, do not need to select evaporation, directly filter examination with computer, only have and cannot filter or when test result is positive when sample extracting solution, just need to retest according to standard method step, cost-saving, reduce operation, be applicable to produce in enormous quantities;
2) add a little anhydrous sodium sulfate, can remove the moisture in organic phase, and be deposited to bottom by floating over two alternate samples, have to utilize and draw organic phase;
3) sieve number by the method, required time is short, expends few.
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.
Embodiment 1
A detection method of forbidding azo dyes in textile, comprises the following steps:
(a) sampling and sample cutting
Remove as far as possible neatly glue, attachment above sample, and different samples processed respectively:
(a1) as requested or grab sample,, for complicated sample, sampling spot need have mark and photo;
(a2) for the fabric that is printed on multicolour pattern, should sample be subdivided into solid color as far as possible, unlike material on product, or the fabric of different colours should sample respectively;
(a3) containing the fabric sample of dacron: the sample of getting is cut into 20mm × 30mm size, mixes;
(a4) not containing the fabric sample of dacron: the sample of getting is cut into 5mm × 5mm size, mixes;
(b) sample pretreatment and reduction decomposition reaction
(b1) containing the textile of dacron
From compound sample, take 1.000g sample, tighten with colourless yarn, in the vaporium of extraction equipment, vertically place, condensing solvent can be flow through from sample; In extraction equipment, add 25mL Benzene Chloride extracting 30 min, make color sample to the greatest extent de-; Extract cool to room temperature, on vacuum rotary evaporator, 45 DEG C～60 DEG C expulsion solvents, obtain a small amount of residue, and residue is transferred in 50mL test tube with 2mL methyl alcohol; In above-mentioned test tube, add 15mL and be preheated to the citrate buffer solution of (70 ± 2 DEG C), cover tightly cap test tube and test tube is put into ultrasound bath pot insulation (30 ± 1) min of (70 ± 2 DEG C); Open test tube cap, add 3mL hydrosulfurous acid sodium solution (200mg/ml), airtight rear firmly jolting, is incubated (30 ± 1) min again in (70 ± 2 DEG C) water-bath at once; After taking out test tube, in 2min, test tube is cooled to rapidly to room temperature;
(b2) not containing the textile of dacron
From compound sample, take 1.0000g sample and be placed in 50mL test tube; The citrate buffer solution that interpolation 17mL is preheated to (70 ± 2 DEG C), in test tube, covers tightly cap test tube firmly jolting, makes all fabrics fully wetting, insulation (30 ± 1) min in the water-bath of (70 ± 2 DEG C); Open test tube cap, add 3mL reductive agent, airtight rear jolting at once, is incubated (30 ± 1) min again in (70 ± 2 DEG C) water-bath; After taking out test tube, in 2min, with frozen water mixing water-bath, test tube is cooled to rapidly to room temperature;
(c) extraction (sieve counting method)
(c1) in test tube, add 5mL t-butyl methyl ether inner mark solution to extract amine substance, cover tightly lid, be placed in 250rmp/min concussion 30min on mechnical oscillator;
(c2) take off test tube, add 0.1-1g anhydrous sodium sulfate to dewater, get supernatant liquid and analyze on gas chromatograph-mass spectrometer (GCMS), obtain result.
Embodiment 2
The present embodiment is tested according to embodiment 1, when in step (c2), supernatant is muddy, need first filter with 0.22um filtering head, when on the rear gas chromatograph-mass spectrometer (GCMS) of do not filter or filtration, test result is positive, the detection of forbidding azo dyes in textile is resurveyed according to following steps:
(a) sampling and sample cutting
Remove as far as possible neatly glue, attachment above sample, and different samples processed respectively:
(a1) as requested or grab sample,, for complicated sample, sampling spot need have mark and photo;
(a2) for the fabric that is printed on multicolour pattern, should sample be subdivided into solid color as far as possible, unlike material on product, or the fabric of different colours should sample respectively;
(a3) containing the fabric sample of dacron: the sample of getting is cut into 20mm × 30mm size, mixes;
(a4) not containing the fabric sample of dacron: the sample of getting is cut into 5mm × 5mm size, mixes;
(b) sample pretreatment and reduction decomposition reaction
(b1) containing the textile of dacron
From compound sample, take 1.000g sample, tighten with colourless yarn, in the vaporium of extraction equipment, vertically place, condensing solvent can be flow through from sample; In extraction equipment, add 25mL Benzene Chloride extracting 30 min, make color sample to the greatest extent de-; Extract cool to room temperature, on vacuum rotary evaporator, 45 DEG C～60 DEG C expulsion solvents, obtain a small amount of residue, and residue is transferred in 50mL test tube with 2mL methyl alcohol; In above-mentioned test tube, add 15mL and be preheated to the citrate buffer solution of (70 ± 2 DEG C), cover tightly cap test tube and test tube is put into ultrasound bath pot insulation (30 ± 1) min of (70 ± 2 DEG C); Open test tube cap, add 3mL 200mg/mL hydrosulfurous acid sodium solution, airtight rear firmly jolting, is incubated (30 ± 1) min again in (70 ± 2 DEG C) water-bath at once; After taking out test tube, in 2min, test tube is cooled to rapidly to room temperature;
(b2) not containing the textile of dacron
From compound sample, take 1.0000g sample and be placed in 50mL test tube; The citrate buffer solution that interpolation 17mL is preheated to (70 ± 2 DEG C), in test tube, covers tightly cap test tube firmly jolting, makes all fabrics fully wetting, insulation (30 ± 1) min in the water-bath of (70 ± 2 DEG C); Open test tube cap, add 3mL reductive agent, airtight rear jolting at once, is incubated (30 ± 1) min again in (70 ± 2 DEG C) water-bath; After taking out test tube, in 2min, with frozen water mixing water-bath, test tube is cooled to rapidly to room temperature;
(d) extraction
First with the sample in glass bar extruding test tube, reactant liquor in test tube is all poured in zeyssatite extraction column, leave standstill and absorb 15min, then directly add 4 × 20mL ether and divide the sample in elution reaction device four times, need to mix ether and sample at every turn, then ether washing lotion is poured in extraction column, coutroi velocity, collects all eluants in 150mL flat bottom flask;
(e) concentrated
The above-mentioned flat bottom flask that fills ether extracted liquid is placed on vacuum rotary evaporator, under the low vacuum of (35 DEG C ± 2 DEG C) 10E5-10E2 Pa, is concentrated into nearly 1mL, then with the slow nitrogen stream of inert gas expulsion diethyl ether solution, it is concentrated near dry;
(f) interpretation of result
(f1) gas chromatograph-mass spectrometer (GCMS) analysis: accurately pipette and mark standard solution in the deuterated anthracene of 10mg/L of 1.0mL methyl alcohol preparation and be concentrated in nearly dry flat bottom flask to above-mentioned, mix, leave standstill, with 0.22um organic system filtering with microporous membrane to 2mL sample bottle for GC-MS analyze, if can not complete instrumental analysis in 24 hours, sample need to be no more than one week lower than-18 DEG C of preservations.
(f2) HPLC/PDA analyzes: accurately pipette 1mL methyl alcohol and add above-mentioned being concentrated in nearly dry flat bottom flask, mix, leave standstill, with 0.22um organic system filtering with microporous membrane to 2mL sample bottle for HPLC/PDA analyze, if can not complete instrumental analysis in 24 hours, sample need to be no more than one week lower than-18 DEG C of preservations.
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 amendment of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. a detection method of forbidding azo dyes in textile, is characterized in that comprising the following steps:
(a) sampling and sample cutting
Remove as far as possible neatly glue, attachment above sample, and different samples processed respectively:
(a1) as requested or grab sample,, for complicated sample, sampling spot need have mark and photo;
(a2) for the fabric that is printed on multicolour pattern, should sample be subdivided into solid color as far as possible, unlike material on product, or the fabric of different colours should sample respectively;
(a3) containing the fabric sample of dacron: the sample of getting is cut into 20mm × 30mm size, mixes;
(a4) not containing the fabric sample of dacron: the sample of getting is cut into 5mm × 5mm size, mixes;
(b) sample pretreatment and reduction decomposition reaction
(b1) containing the textile of dacron
From compound sample, take 1.000g sample, tighten with colourless yarn, in the vaporium of extraction equipment, vertically place, condensing solvent can be flow through from sample; In extraction equipment, add 25mL Benzene Chloride extracting 30 min, make color sample to the greatest extent de-; Extract cool to room temperature, on vacuum rotary evaporator, 45 DEG C～60 DEG C expulsion solvents, obtain a small amount of residue, and residue is transferred in 50mL test tube with 2mL methyl alcohol; In above-mentioned test tube, add 15mL and be preheated to the citrate buffer solution of (70 ± 2 DEG C), cover tightly cap test tube and test tube is put into ultrasound bath pot insulation (30 ± 1) min of (70 ± 2 DEG C); Open test tube cap, add the hydrosulfurous acid sodium solution of 3mL 200mg/ml, airtight rear firmly jolting, is incubated (30 ± 1) min again in (70 ± 2 DEG C) water-bath at once; After taking out test tube, in 2min, test tube is cooled to rapidly to room temperature;
(b2) not containing the textile of dacron
From compound sample, take 1.0000g sample and be placed in 50mL test tube; The citrate buffer solution that interpolation 17mL is preheated to (70 ± 2 DEG C), in test tube, covers tightly cap test tube firmly jolting, makes all fabrics fully wetting, insulation (30 ± 1) min in the water-bath of (70 ± 2 DEG C); Open test tube cap, add 3mL reductive agent, airtight rear jolting at once, is incubated (30 ± 1) min again in (70 ± 2 DEG C) water-bath; After taking out test tube, in 2min, with frozen water mixing water-bath, test tube is cooled to rapidly to room temperature;
(c) extraction (sieve counting method)
(c1) in test tube, add 5mL t-butyl methyl ether inner mark solution to extract amine substance, cover tightly lid, be placed in 250rmp/min concussion 30min on mechnical oscillator;
(c2) take off test tube, add 0.1-1g anhydrous sodium sulfate to dewater, get supernatant liquid and analyze on gas chromatograph-mass spectrometer (GCMS).
2. according to the detection method of forbidding azo dyes in the textile described in claim 1, it is characterized in that: if need first filter with 0.22um filtering head when in described step (c2), supernatant is muddy, when on the rear gas chromatograph-mass spectrometer (GCMS) of do not filter or filtration, test result is positive, in textile, forbid the detection of azo dyes from step (a) and (b), then use following methods instead and resurvey:
(d) extraction
First with the sample in glass bar extruding test tube, reactant liquor in test tube is all poured in zeyssatite extraction column, leave standstill and absorb 15min, then directly add 4 × 20mL ether and divide the sample in elution reaction device four times, need to mix ether and sample at every turn, then ether washing lotion is poured in extraction column, coutroi velocity, collects all eluants in 150mL flat bottom flask;
(e) concentrated
The above-mentioned flat bottom flask that fills ether extracted liquid is placed on vacuum rotary evaporator, under (35 DEG C ± 2 DEG C) low vacuum, is concentrated into nearly 1mL, then with the slow nitrogen stream of inert gas expulsion diethyl ether solution, it is concentrated near dry;
(f) interpretation of result
(f1) gas chromatograph-mass spectrometer (GCMS) analysis: accurately pipette and mark standard solution in the deuterated anthracene of 10mg/L of 1.0mL methyl alcohol preparation and be concentrated in nearly dry flat bottom flask to above-mentioned, mix, leave standstill, use 0.22um organic system filtering with microporous membrane to 2mL sample bottle to analyze for GC-MS.
3.(f2) HPLC/PDA analyzes: accurately pipette 1mL methyl alcohol and add above-mentioned being concentrated in nearly dry flat bottom flask, mix, leave standstill, use 0.22um organic system filtering with microporous membrane to 2mL sample bottle to analyze for HPLC/PDA.
4. according to the detection method of forbidding azo dyes in the textile described in claim 2, it is characterized in that: described step (f) if in can not complete instrumental analysis in 24 hours, sample need to be no more than one week lower than-18 DEG C of preservations.
5. according to the detection method of forbidding azo dyes in the textile described in claim 3, it is characterized in that: the low vacuum of described step (3) is (10E5-10E2) Pa.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458966A (en) * | 2014-12-23 | 2015-03-25 | 南京市产品质量监督检验院 | Detection method for forbidden azo dyes of textiles |
| CN105181876A (en) * | 2015-10-21 | 2015-12-23 | 国家烟草质量监督检验中心 | Method of measuring residual amount of 4-aminoazobenzene in paper for cigarettes |
| CN105319305A (en) * | 2014-12-30 | 2016-02-10 | 厦门中迅德检测技术有限公司 | Pretreatment method for conducting banned azo-dye measurement on textile |
| 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 |
| CN107860736A (en) * | 2017-10-22 | 2018-03-30 | 宁晋县质量技术监督检验所 | A kind of method for detecting 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 |
| CN111855846A (en) * | 2020-07-07 | 2020-10-30 | 江苏亚维检测技术服务有限公司 | Method for detecting banned azo dye in textile |
| CN112684054A (en) * | 2020-12-29 | 2021-04-20 | 必维申优质量技术服务江苏有限公司 | Novel method for determining azo dyes in textiles |
| CN114152693A (en) * | 2021-11-29 | 2022-03-08 | 苏州健雄职业技术学院 | Qualitative detection method for decomposable aromatic amine dye for textile clothes |
| CN114544814A (en) * | 2022-02-25 | 2022-05-27 | 南京海关工业产品检测中心 | Method for measuring forbidden azo dyes in disposable dyeing mask |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458966A (en) * | 2014-12-23 | 2015-03-25 | 南京市产品质量监督检验院 | Detection method for forbidden azo dyes of textiles |
| CN105319305A (en) * | 2014-12-30 | 2016-02-10 | 厦门中迅德检测技术有限公司 | Pretreatment method for conducting banned azo-dye measurement on textile |
| CN105181876A (en) * | 2015-10-21 | 2015-12-23 | 国家烟草质量监督检验中心 | Method of measuring residual amount of 4-aminoazobenzene in paper for cigarettes |
| 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 |
| CN107860736A (en) * | 2017-10-22 | 2018-03-30 | 宁晋县质量技术监督检验所 | A kind of method for detecting 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 |
| CN111855846A (en) * | 2020-07-07 | 2020-10-30 | 江苏亚维检测技术服务有限公司 | Method for detecting banned azo dye in textile |
| CN112684054A (en) * | 2020-12-29 | 2021-04-20 | 必维申优质量技术服务江苏有限公司 | Novel method for determining azo dyes in textiles |
| CN114152693A (en) * | 2021-11-29 | 2022-03-08 | 苏州健雄职业技术学院 | Qualitative detection method for decomposable aromatic amine dye for textile clothes |
| CN114544814A (en) * | 2022-02-25 | 2022-05-27 | 南京海关工业产品检测中心 | Method for measuring forbidden azo dyes in disposable dyeing mask |
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Application publication date: 20141119 |