CN106990189A - A kind of detection method of textile forbidding azo dyes - Google Patents
A kind of detection method of textile forbidding azo dyes Download PDFInfo
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- CN106990189A CN106990189A CN201710436471.0A CN201710436471A CN106990189A CN 106990189 A CN106990189 A CN 106990189A CN 201710436471 A CN201710436471 A CN 201710436471A CN 106990189 A CN106990189 A CN 106990189A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
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Abstract
The invention discloses a kind of detection method of textile forbidding azo dyes, comprise the following steps：1）Preparation of samples；2）Reduction；3）Liquid-liquid extraction；4）Extract and measure result；The present invention substantially reduces detection time, the problem of testing process present in current examination criteria is long is solved, and testing cost is low, expends few, the testing cost that textile disables ice color is greatly reduced, the detection efficiency that textile disables ice color is improved.
Description
Technical field
The present invention relates to a kind of detection method of textile forbidding azo dyes, belong to textile azo dyes detection technique
Field.
Background technology
Azo dyes, is fabric clothing most widely used class synthetic dyestuffs in dyeing and printing process, for a variety of days
Dyeing and the stamp of right and synthetic fibers, are also used for the coloring of paint, plastics, rubber etc..Under specific condition, azo dyes energy
Decompose and produce the carcinogenic aromatic amine compound of kind more than 20, this compound can be absorbed by the body, make by a series of activations
The DNA recurring structures of human body cell and the change of function, cause human lesion and induce cancer.
The content of the invention
（One）The technical problem to be solved
To solve the above problems, the present invention, which proposes one kind, substantially reduces detection time, solve current examination criteria and deposited
Testing process it is long the problem of, and testing cost is low, expends few, greatly reduce the detection of textile disabling ice color into
This, improves the detection method of the textile forbidding azo dyes of the detection efficiency of textile disabling ice color.
（Two）Technical scheme
A kind of detection method of textile forbidding azo dyes of the present invention, it is characterised in that：Comprise the following steps：
1）Preparation of samples：Take 1~10 gram of textile fabric in reactor, prepare sample solution；
2）Reduction：Plus 15 in the reactor~30ml is preheated to 70~80 DEG C of citrate buffer solution, by reactor
Seal and 25~30min is kept at 60~70 DEG C, then add 3.0ml200mg/ml reductive cleavage agent hydrosulfurous acids
Sodium water solution, directly keeps 30~35min at 65~75 DEG C after firmly shaking, reactor is removed and cold in 2min
But to room temperature；Then, 0.2ml10%m/m sodium hydroxide solutions are added in reaction solution and are firmly shaken, transfer reaction is molten
Liquid fully absorbs 15min to siliceous earth column, while plus 10ml methyl tertiary butyl ether(MTBE)s firmly shaken into reactor, 15 minutes
Afterwards above methyl tertiary butyl ether(MTBE) and fibre migration to post, eluate is collected with 100ml standard gauge round-bottomed flask, instead
Answer in device plus 10ml methyl tertiary butyl ether(MTBE)s, and solution is transferred in post, be finally directly added into 60ml methyl tertiary butyl ether(MTBE)s
Into post, methyl tertiary butyl ether(MTBE) extract concentrated by rotary evaporation is quickly used into methyl tertiary butyl ether(MTBE) to about 1ml at no more than 50 DEG C
By residue constant volume to 2.0ml, sample concentration liquid is obtained；
3）The citrate buffer that 15mL will be added to be preheating to 65~70 DEG C in sample concentration liquid, is then placed in sample bottle sealing,
35min is kept at 65~70 DEG C, 2.0mL reductive cleavage agent hydrosulfurous acid sodium water solutions are then added in sample bottle, firmly
Sample bottle is shaken, directly 30min is kept at 65~70 DEG C, room temperature is subsequently cooled to, reductive cleavage liquid is obtained；
4）Liquid-liquid extraction：It is the deuterated of 6mg/L that 0.5mL sodium hydroxides, 7g sodium chloride, 5mL concentration are added in reductive cleavage liquid
Sample bottle, is then placed on horizontal oscillator tube and vibrates 15min by naphthalene standard liquid, obtains liquid-liquid extraction liquid；
5）Forbidding azo dyes are determined：A small amount of liquid-liquid extraction liquid is pipetted into auto injection bottle, GC/ is used by gas chromatograph
MSD methods carry out forbidding azo dyes measure
6）Gaschromatographic mass spectrometric analysis condition：Using helium as carrier gas, using gradient increased temperature pattern；With DB-35 capillary columns
For chromatographic column；Using EI as ion gun, ionization pattern is holotype；Flow velocity is 1ml/min, and split ratio is 15:1 ；With complete
Scan mode is data acquisition modes；
7）By step 2）The sample concentration liquid injection gas chromatography-mass spectrometry of gained, point of gas chromatography-mass spectrometry
Analysis condition is according to step 3）；
8）Quantification and qualification：It is carried out according to disabling azo-compound retention time on a column and mass spectrogram
Qualitative analysis, according to the peak area of disabling azo-compound on a column, and carries out quantitative analysis using internal standard method to it.
Further, the quality of described disabling azo standard substance is the mg of 11.2mg~12.5.
Further, described methyl tertiary butyl ether(MTBE) liquid is 60~100mL.
（Three）Beneficial effect
Compared with prior art, it has the advantages that the present invention：The present invention substantially reduces detection time, solves
The problem of testing process present in current examination criteria is long, and testing cost is low, expends few, greatly reduces textile disabling
The testing cost of ice color, improves the detection efficiency that textile disables ice color.
Embodiment
Embodiment 1
A kind of detection method of textile forbidding azo dyes, it is characterised in that：Comprise the following steps：
1）Preparation of samples：Take 1 gram of textile fabric in reactor, prepare sample solution；
2）Reduction：In the reactor plus 15ml is preheated to 70 DEG C of citrate buffer solution, by reactor seal and
25min is kept at 60 DEG C, 3.0ml200mg/ml reductive cleavage agent hydrosulfurous acid sodium water solutions is then added, firmly shakes
30min directly is kept at 65 DEG C afterwards, reactor is removed and room temperature is cooled in 2min；Then, in reaction solution
Middle addition 0.2ml10%m/m sodium hydroxide solutions are simultaneously firmly shaken, and transfer reaction solution is fully absorbed to siliceous earth column
15min, while plus 10ml methyl tertiary butyl ether(MTBE)s firmly shaken into reactor, methyl tertiary butyl ether(MTBE) and fibre after 15 minutes
Dimension is transferred to above post, is collected with 100ml standard gauge round-bottomed flask in eluate, reactor plus 10ml methyl- tert fourths
Base ether, and solution is transferred in post, finally it is added directly into 60ml methyl tertiary butyl ether(MTBE)s in post, no more than 50 DEG C
It is lower by methyl tertiary butyl ether(MTBE) extract concentrated by rotary evaporation to about 1ml, quickly residue constant volume is arrived with methyl tertiary butyl ether(MTBE)
2.0ml, obtains sample concentration liquid；
3）The citrate buffer that 15mL will be added to be preheating to 65 DEG C in sample concentration liquid, is then placed in sample bottle sealing, 65
35min is kept at DEG C, 2.0mL reductive cleavage agent hydrosulfurous acid sodium water solutions are then added in sample bottle, sample is firmly shaken
Bottle, directly keeps 30min at 65 DEG C, is subsequently cooled to room temperature, obtains reductive cleavage liquid；
4）Liquid-liquid extraction：It is the deuterated of 6mg/L that 0.5mL sodium hydroxides, 7g sodium chloride, 5mL concentration are added in reductive cleavage liquid
Sample bottle, is then placed on horizontal oscillator tube and vibrates 15min by naphthalene standard liquid, obtains liquid-liquid extraction liquid；
5）Forbidding azo dyes are determined：A small amount of liquid-liquid extraction liquid is pipetted into auto injection bottle, GC/ is used by gas chromatograph
MSD methods carry out forbidding azo dyes measure；
6）Gaschromatographic mass spectrometric analysis condition：Using helium as carrier gas, using gradient increased temperature pattern；Using DB-35 capillary columns as
Chromatographic column；Using EI as ion gun, ionization pattern is holotype；Flow velocity is 1ml/min, and split ratio is 15:1 ；To sweep entirely
Mode is retouched for data acquisition modes；
7）By step 2）The sample concentration liquid injection gas chromatography-mass spectrometry of gained, point of gas chromatography-mass spectrometry
Analysis condition is according to step 3）；
8）Quantification and qualification：It is determined according to disabling azo-compound retention time on a column and mass spectrogram
Property analysis, quantitative analysis is carried out to it according to disabling azo-compound peak area on a column, and using internal standard method；
Wherein, the quality of described disabling azo standard substance is 11.2mgmg；
Described methyl tertiary butyl ether(MTBE) liquid is 60mL.
Embodiment 2
A kind of detection method of textile forbidding azo dyes, it is characterised in that：Comprise the following steps：
1）Preparation of samples：Take 10 grams of textile fabrics in reactor, prepare sample solution；
2）Reduction：In the reactor plus 30ml is preheated to 80 DEG C of citrate buffer solution, by reactor seal and
30min is kept at 70 DEG C, 3.0ml200mg/ml reductive cleavage agent hydrosulfurous acid sodium water solutions is then added, firmly shakes
35min directly is kept at 75 DEG C afterwards, reactor is removed and room temperature is cooled in 2min；Then, in reaction solution
Middle addition 0.2ml10%m/m sodium hydroxide solutions are simultaneously firmly shaken, and transfer reaction solution is fully absorbed to siliceous earth column
15min, while plus 10ml methyl tertiary butyl ether(MTBE)s firmly shaken into reactor, methyl tertiary butyl ether(MTBE) and fibre after 15 minutes
Dimension is transferred to above post, is collected with 100ml standard gauge round-bottomed flask in eluate, reactor plus 10ml methyl- tert fourths
Base ether, and solution is transferred in post, finally it is added directly into 60ml methyl tertiary butyl ether(MTBE)s in post, no more than 50 DEG C
It is lower by methyl tertiary butyl ether(MTBE) extract concentrated by rotary evaporation to about 1ml, quickly residue constant volume is arrived with methyl tertiary butyl ether(MTBE)
2.0ml, obtains sample concentration liquid；
3）The citrate buffer that 15mL will be added to be preheating to 70 DEG C in sample concentration liquid, is then placed in sample bottle sealing, 70
35min is kept at DEG C, 2.0mL reductive cleavage agent hydrosulfurous acid sodium water solutions are then added in sample bottle, sample is firmly shaken
Bottle, directly keeps 30min at 70 DEG C, is subsequently cooled to room temperature, obtains reductive cleavage liquid；
4）Liquid-liquid extraction：It is the deuterated of 6mg/L that 0.5mL sodium hydroxides, 7g sodium chloride, 5mL concentration are added in reductive cleavage liquid
Sample bottle, is then placed on horizontal oscillator tube and vibrates 15min by naphthalene standard liquid, obtains liquid-liquid extraction liquid；
5）Forbidding azo dyes are determined：A small amount of liquid-liquid extraction liquid is pipetted into auto injection bottle, GC/ is used by gas chromatograph
MSD methods carry out forbidding azo dyes measure；
6）Gaschromatographic mass spectrometric analysis condition：Using helium as carrier gas, using gradient increased temperature pattern；Using DB-35 capillary columns as
Chromatographic column；Using EI as ion gun, ionization pattern is holotype；Flow velocity is 1ml/min, and split ratio is 15:1；With full scan side
Formula is data acquisition modes；
7）By step 2）The sample concentration liquid injection gas chromatography-mass spectrometry of gained, point of gas chromatography-mass spectrometry
Analysis condition is according to step 3）；
8）Quantification and qualification：It is determined according to disabling azo-compound retention time on a column and mass spectrogram
Property analysis, quantitative analysis is carried out to it according to disabling azo-compound peak area on a column, and using internal standard method；
Wherein, the quality of described disabling azo standard substance is 12.5 mg；
Described methyl tertiary butyl ether(MTBE) liquid is 100mL.
Embodiment 3
A kind of detection method of textile forbidding azo dyes, it is characterised in that：Comprise the following steps：
1）Preparation of samples：Take 5 grams of textile fabrics in reactor, prepare sample solution；
2）Reduction：In the reactor plus 25ml is preheated to 75 DEG C of citrate buffer solution, by reactor seal and
28min is kept at 65 DEG C, 3.0ml200mg/ml reductive cleavage agent hydrosulfurous acid sodium water solutions is then added, firmly shakes
33min directly is kept at 70 DEG C afterwards, reactor is removed and room temperature is cooled in 2min；Then, in reaction solution
Middle addition 0.2ml10%m/m sodium hydroxide solutions are simultaneously firmly shaken, and transfer reaction solution is fully absorbed to siliceous earth column
15min, while plus 10ml methyl tertiary butyl ether(MTBE)s firmly shaken into reactor, methyl tertiary butyl ether(MTBE) and fibre after 15 minutes
Dimension is transferred to above post, is collected with 100ml standard gauge round-bottomed flask in eluate, reactor plus 10ml methyl- tert fourths
Base ether, and solution is transferred in post, finally it is added directly into 60ml methyl tertiary butyl ether(MTBE)s in post, no more than 50 DEG C
It is lower by methyl tertiary butyl ether(MTBE) extract concentrated by rotary evaporation to about 1ml, quickly residue constant volume is arrived with methyl tertiary butyl ether(MTBE)
2.0ml, obtains sample concentration liquid；
3）The citrate buffer that 15mL will be added to be preheating to 68 DEG C in sample concentration liquid, is then placed in sample bottle sealing, 68
35min is kept at DEG C, 2.0mL reductive cleavage agent hydrosulfurous acid sodium water solutions are then added in sample bottle, sample is firmly shaken
Bottle, directly keeps 30min at 68 DEG C, is subsequently cooled to room temperature, obtains reductive cleavage liquid；
4）Liquid-liquid extraction：It is the deuterated of 6mg/L that 0.5mL sodium hydroxides, 7g sodium chloride, 5mL concentration are added in reductive cleavage liquid
Sample bottle, is then placed on horizontal oscillator tube and vibrates 15min by naphthalene standard liquid, obtains liquid-liquid extraction liquid；
5）Forbidding azo dyes are determined：A small amount of liquid-liquid extraction liquid is pipetted into auto injection bottle, GC/ is used by gas chromatograph
MSD methods carry out forbidding azo dyes measure；
6）Gaschromatographic mass spectrometric analysis condition：Using helium as carrier gas, using gradient increased temperature pattern；Using DB-35 capillary columns as
Chromatographic column；Using EI as ion gun, ionization pattern is holotype；Flow velocity is 1ml/min, and split ratio is 15:1；With full scan side
Formula is data acquisition modes；
7）By step 2）The sample concentration liquid injection gas chromatography-mass spectrometry of gained, point of gas chromatography-mass spectrometry
Analysis condition is according to step 3）；
8）Quantification and qualification：It is carried out according to disabling azo-compound retention time on a column and mass spectrogram
Qualitative analysis, according to the peak area of disabling azo-compound on a column, and carries out quantitative analysis using internal standard method to it；
Wherein, the quality of described disabling azo standard substance is 11.3 mg；
Described methyl tertiary butyl ether(MTBE) liquid is 80mL.
The present invention substantially reduces detection time, solves the problem of testing process present in current examination criteria is long,
And testing cost is low, expend few, greatly reduce the testing cost that textile disables ice color, improve textile disabling even
The detection efficiency of nitrogen fuel.
The above-described embodiments are merely illustrative of preferred embodiments of the present invention, not to the structure of the present invention
Think and model point encloses and is defined.On the premise of design concept of the present invention is not departed from, skill of this area ordinary person to the present invention
The all variations and modifications that art scheme is made, all should be dropped into protection scope of the present invention, claimed technology of the invention
Hold, all recorded in detail in the claims.
Claims (3)
1. a kind of detection method of textile forbidding azo dyes, it is characterised in that：Comprise the following steps：
1）Preparation of samples：Take 1~10 gram of textile fabric in reactor, prepare sample solution；
2）Reduction：Plus 15 in the reactor~30ml is preheated to 70~80 DEG C of citrate buffer solution, and reactor is close
Seal and 25~30min is kept at 60~70 DEG C, then add 3.0ml200mg/ml reductive cleavage agent sodium dithionites
The aqueous solution, directly keeps 30~35min at 65~75 DEG C after firmly shaking, reactor is removed and cooled down in 2min
To room temperature；Then, 0.2ml10%m/m sodium hydroxide solutions are added in reaction solution and are firmly shaken, transfer reaction solution
To siliceous earth column, fully absorb 15min, while plus 10ml methyl tertiary butyl ether(MTBE)s firmly shaken into reactor, after 15 minutes
Above methyl tertiary butyl ether(MTBE) and fibre migration to post, eluate, reaction are collected with 100ml standard gauge round-bottomed flask
Add 10ml methyl tertiary butyl ether(MTBE)s in device, and solution is transferred in post, be finally added directly into 60ml methyl tertiary butyl ether(MTBE)s
, quickly will with methyl tertiary butyl ether(MTBE) by methyl tertiary butyl ether(MTBE) extract concentrated by rotary evaporation to about 1ml at no more than 50 DEG C in post
Residue constant volume obtains sample concentration liquid to 2.0ml；
3）The citrate buffer that 15mL will be added to be preheating to 65~70 DEG C in sample concentration liquid, is then placed in sample bottle sealing,
35min is kept at 65~70 DEG C, 2.0mL reductive cleavage agent hydrosulfurous acid sodium water solutions are then added in sample bottle, firmly
Sample bottle is shaken, directly 30min is kept at 65~70 DEG C, room temperature is subsequently cooled to, reductive cleavage liquid is obtained；
4）Liquid-liquid extraction：It is the deuterated of 6mg/L that 0.5mL sodium hydroxides, 7g sodium chloride, 5mL concentration are added in reductive cleavage liquid
Sample bottle, is then placed on horizontal oscillator tube and vibrates 15min by naphthalene standard liquid, obtains liquid-liquid extraction liquid；
5）Forbidding azo dyes are determined：A small amount of liquid-liquid extraction liquid is pipetted into auto injection bottle, GC/ is used by gas chromatograph
MSD methods carry out forbidding azo dyes measure；
6）Gaschromatographic mass spectrometric analysis condition：Using helium as carrier gas, using gradient increased temperature pattern；Using DB-35 capillary columns as
Chromatographic column；Using EI as ion gun, ionization pattern is holotype；Flow velocity is 1ml/min, and split ratio is 15:1；In full scan mode
For data acquisition modes；
7）By step 2）The sample concentration liquid injection gas chromatography-mass spectrometry of gained, point of gas chromatography-mass spectrometry
Analysis condition is according to step 3）；
8）Quantification and qualification：It is determined according to disabling azo-compound retention time on a column and mass spectrogram
Property analysis, quantitative analysis is carried out to it according to disabling azo-compound peak area on a column, and using internal standard method.
2. a kind of detection method of textile forbidding azo dyes according to claim 1, it is characterised in that：Described taboo
Quality with azo standard substance is the mg of 11.2mg~12.5.
3. a kind of testing methods of banned azo dyes in textiles according to claim 1, it is characterised in that：Described methyl
Tertbutyl ether liquid is 60~100mL.
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| CN201710436471.0A CN106990189A (en) | 2017-06-12 | 2017-06-12 | A kind of detection method of textile forbidding azo dyes |
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| CN201710436471.0A CN106990189A (en) | 2017-06-12 | 2017-06-12 | A kind of detection method of textile forbidding azo dyes |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108896669A (en) * | 2018-05-23 | 2018-11-27 | 江苏省纺织产品质量监督检验研究院 | Textile azo rapid detection method |
| CN108918741A (en) * | 2018-10-11 | 2018-11-30 | 重庆市计量质量检测研究院 | Disable the automation pre-treating method of harmful aromatic amine dyestuff detection |
| 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 |
| 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 |
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| 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 |
| CN104155380A (en) * | 2014-08-15 | 2014-11-19 | 广州衡创测试技术服务有限公司 | Detection method for banned azo-dye in textile |
| CN104165952A (en) * | 2014-08-15 | 2014-11-26 | 广州衡创测试技术服务有限公司 | Method for detecting banned azo dyes in printing ink, coatings and paint |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN104155380A (en) * | 2014-08-15 | 2014-11-19 | 广州衡创测试技术服务有限公司 | Detection method for banned azo-dye in textile |
| CN104165952A (en) * | 2014-08-15 | 2014-11-26 | 广州衡创测试技术服务有限公司 | Method for detecting banned azo dyes in printing ink, coatings and paint |
| 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108896669A (en) * | 2018-05-23 | 2018-11-27 | 江苏省纺织产品质量监督检验研究院 | Textile azo rapid detection method |
| CN108918741A (en) * | 2018-10-11 | 2018-11-30 | 重庆市计量质量检测研究院 | Disable the automation pre-treating method of harmful aromatic amine dyestuff detection |
| CN108918741B (en) * | 2018-10-11 | 2021-07-09 | 重庆市计量质量检测研究院 | Automatic pretreatment method for forbidden detection of harmful aromatic amine dye |
| 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 |
| 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 |
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