CN111855846A - Method for detecting banned azo dye in textile - Google Patents
Method for detecting banned azo dye in textile Download PDFInfo
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- CN111855846A CN111855846A CN202010645986.3A CN202010645986A CN111855846A CN 111855846 A CN111855846 A CN 111855846A CN 202010645986 A CN202010645986 A CN 202010645986A CN 111855846 A CN111855846 A CN 111855846A
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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
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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
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a method for detecting banned azo dyes in textiles, which comprises the following steps: (1) processing a sample; (2) reacting a sample; (3) reducing the sample; (4) extracting a sample reaction solution; (5) and (6) measuring results. The method conforms to the green requirement of the textile dye, adopts the detection method of the banned azo dye in the textile, greatly shortens the detection time, solves the problem of long test flow existing in the current detection standard, has low detection cost and low consumption, greatly reduces the detection cost of the banned azo fuel in the textile, improves the detection efficiency of the banned azo fuel in the textile, is widely applied to the test of the textile fabrics dyed by various dyes, and has the advantages of simple and rapid method, low cost and wide application field.
Description
Technical Field
The invention relates to the technical field of textile detection, in particular to a method for detecting banned azo dyes in textiles.
Background
Azo dyes are a class of synthetic dyes most widely used in textile apparel in printing and dyeing processes, for dyeing and printing a variety of natural and synthetic fibers, and also for coloring paints, plastics, rubbers, and the like. Under special conditions, azo dyes can decompose to generate more than 20 carcinogenic aromatic amine compounds, after the clothes or other consumer goods dyed by forbidden azo dyes are contacted with human skin for a long time, the clothes or other consumer goods can be mixed with components released in the metabolic process, and a reduction reaction is generated to form carcinogenic aromatic amine compounds, the compounds can be absorbed by human bodies, and DNA of human cells is subjected to structural and functional changes through a series of activation effects to become a cause of human pathological changes. GB/T17592-2011, most of measurement methods for banning azo dyes on textiles have more defects relative to production, such as high cost, long time consumption, incapability of batch operation and the like.
Disclosure of Invention
The invention aims to provide a method for detecting banned azo dyes in textiles so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method of detecting banned azo dyes in a textile, comprising the steps of:
step 1: weighing 1-3 g of sample, placing the sample into a reaction bottle, and adding 15-20 ml of citrate buffer solution and 3ml of sodium hydrosulfite solution;
step 2: sealing the reaction bottle, shaking forcibly, putting the reaction bottle into a water bath at 68-72 ℃ for heat preservation for 25-30 min, taking out the reaction bottle, and cooling to room temperature within 2 min;
and step 3: adding 8-10 ml of methyl tert-butyl ether into a reaction bottle, sealing the reaction bottle, and then placing the reaction bottle on an oscillating device to shake forcibly;
and 4, step 4: transferring the reaction solution in the reaction bottle to a diatomite extraction column, standing and absorbing for 15-20 min;
and 5: adding 10ml of methyl tert-butyl ether into a reaction bottle to elute the reaction solution in the reaction bottle, and pouring the eluted reaction solution onto a kieselguhr extraction column;
step 6: pouring 70ml of methyl tert-butyl ether into a diatomite extraction column, controlling the flow rate, and collecting all eluent into a 150ml standard-caliber flat-bottom flask;
And 7: performing rotary evaporation and concentration on the extracting solution in the flat-bottomed flask to nearly 1ml, and quickly metering the remainder to 2ml by using methyl tert-butyl ether to obtain a sample concentrated solution;
and 8: adding 15-20 mL of citrate buffer solution preheated to 68-72 ℃ into the sample concentrated solution, placing the sample concentrated solution into a sample bottle, sealing the sample bottle, keeping the temperature of 68-72 ℃ for 35min, adding 2mL of reduction cracking agent sodium dithionite aqueous solution, forcibly shaking the sample bottle, directly keeping the sample bottle at 68-72 ℃ for 30min, and then cooling to room temperature to obtain reduction cracking solution;
and step 9: adding 0.3mL of sodium hydroxide, 5g of sodium chloride and 4mL of deuterated naphthalene standard solution with the concentration of 10mg/L into the reduction lysate, and then placing a sample bottle on a horizontal oscillator to oscillate for 15min to obtain an extract liquor;
step 10: and (4) transferring a small amount of extract liquid into an automatic sample feeding bottle, and performing forbidden azo dye determination by a gas chromatograph by adopting a GC/MSD method.
Preferably, in the step 1, the concentration of the sodium hydrosulfite solution is 200-250 mg/ml.
Preferably, in the step 3, the oscillation device is a mechanical oscillator, the oscillation speed of the mechanical oscillator is 220 to 240rmp/min, and the oscillation time is 25 to 30 min.
Preferably, in the step 7, the device for rotary evaporation and concentration of the extracting solution in the flat-bottomed flask is a vacuum rotary evaporator, and the concentration temperature of the vacuum rotary evaporator is 38-40 ℃.
Preferably, in step 10, the extract is filtered through a 0.22um organic microporous membrane and then the azo dye is measured by a gas chromatograph.
Compared with the prior art, the invention has the beneficial effects that:
the method conforms to the green requirement of the textile dye, adopts the detection method of the banned azo dye in the textile, greatly shortens the detection time, solves the problem of long test flow existing in the current detection standard, has low detection cost and low consumption, greatly reduces the detection cost of the banned azo fuel in the textile, improves the detection efficiency of the banned azo fuel in the textile, is widely applied to the test of the textile fabrics dyed by various dyes, and has the advantages of simple and rapid method, low cost and wide application field.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a technical scheme that: a method of detecting banned azo dyes in a textile, comprising the steps of:
step 1: weighing 1g of sample, placing the sample into a reaction bottle, adding 15ml of citrate buffer solution and 3ml of sodium hydrosulfite solution, wherein the concentration of the sodium hydrosulfite solution is 200 mg/ml;
step 2: sealing the reaction bottle, shaking vigorously, placing into 68 deg.C water bath, keeping the temperature for 25min, taking out the reaction bottle, and cooling to room temperature within 2 min;
and step 3: adding 8ml of methyl tert-butyl ether into a reaction bottle, sealing the reaction bottle, and then placing the reaction bottle on an oscillating device to shake forcibly, wherein the oscillating device is a mechanical oscillator, the oscillating speed of the mechanical oscillator is 220rmp/min, and the oscillating time is 25 min;
and 4, step 4: transferring the reaction solution in the reaction bottle to a diatomite extraction column, standing and absorbing for 15 min;
and 5: adding 10ml of methyl tert-butyl ether into a reaction bottle to elute the reaction solution in the reaction bottle, and pouring the eluted reaction solution onto a kieselguhr extraction column;
step 6: pouring 70ml of methyl tert-butyl ether into a diatomite extraction column, controlling the flow rate, and collecting all eluent into a 150ml standard-caliber flat-bottom flask;
And 7: performing rotary evaporation and concentration on the extracting solution in the flat-bottomed flask to nearly 1ml, quickly metering the volume of the remainder to 2ml by using methyl tert-butyl ether to obtain a sample concentrated solution, wherein the rotary evaporation and concentration device of the extracting solution in the flat-bottomed flask is a vacuum rotary evaporator, and the concentration temperature of the vacuum rotary evaporator is 38 ℃;
and 8: adding 15mL of citrate buffer solution preheated to 68 ℃ into the sample concentrated solution, placing the sample into a sample bottle, sealing, keeping the temperature of 68 ℃ for 35min, adding 2mL of reduction cracking agent sodium dithionite aqueous solution, shaking the sample bottle forcibly, keeping the temperature at 68 ℃ for 30min directly, and then cooling to room temperature to obtain reduction cracking solution;
and step 9: adding 0.3mL of sodium hydroxide, 5g of sodium chloride and 4mL of deuterated naphthalene standard solution with the concentration of 10mg/L into the reduction lysate, and then placing a sample bottle on a horizontal oscillator to oscillate for 15min to obtain an extract liquor;
step 10: transferring a small amount of extract liquid into an automatic sample injection bottle, filtering the extract liquid by using an organic microporous filter membrane of 0.22um, and then determining the forbidden azo dyes by adopting a GC/MSD method through a gas chromatograph.
Example 2:
the invention provides a technical scheme that: a method of detecting banned azo dyes in a textile, comprising the steps of:
Step 1: weighing 2g of sample, placing the sample into a reaction bottle, adding 18ml of citrate buffer solution and 3ml of sodium hydrosulfite solution, wherein the concentration of the sodium hydrosulfite solution is 230 mg/ml;
step 2: sealing the reaction bottle, shaking with force, placing in 70 deg.C water bath, keeping the temperature for 30min, taking out the reaction bottle, and cooling to room temperature within 2 min;
and step 3: adding 9ml of methyl tert-butyl ether into a reaction bottle, sealing the reaction bottle, and then placing the reaction bottle on an oscillating device to shake forcibly, wherein the oscillating device is a mechanical oscillator, the oscillating speed of the mechanical oscillator is 230rmp/min, and the oscillating time is 30 min;
and 4, step 4: transferring the reaction solution in the reaction bottle to a diatomite extraction column, standing and absorbing for 15 min;
and 5: adding 10ml of methyl tert-butyl ether into a reaction bottle to elute the reaction solution in the reaction bottle, and pouring the eluted reaction solution onto a kieselguhr extraction column;
step 6: pouring 70ml of methyl tert-butyl ether into a diatomite extraction column, controlling the flow rate, and collecting all eluent into a 150ml standard-caliber flat-bottom flask;
and 7: performing rotary evaporation and concentration on the extracting solution in the flat-bottomed flask to nearly 1ml, quickly metering the volume of the remainder to 2ml by using methyl tert-butyl ether to obtain a sample concentrated solution, wherein the rotary evaporation and concentration device of the extracting solution in the flat-bottomed flask is a vacuum rotary evaporator, and the concentration temperature of the vacuum rotary evaporator is 39 ℃;
And 8: adding 20mL of citrate buffer solution preheated to 70 ℃ into the sample concentrated solution, placing the sample into a sample bottle, sealing, keeping the temperature of 70 ℃ for 35min, adding 2mL of reduction cracking agent sodium dithionite aqueous solution, shaking the sample bottle forcibly, keeping the temperature at 70 ℃ for 30min directly, and then cooling to room temperature to obtain reduction cracking solution;
and step 9: adding 0.3mL of sodium hydroxide, 5g of sodium chloride and 4mL of deuterated naphthalene standard solution with the concentration of 10mg/L into the reduction lysate, and then placing a sample bottle on a horizontal oscillator to oscillate for 15min to obtain an extract liquor;
step 10: transferring a small amount of extract liquid into an automatic sample injection bottle, filtering the extract liquid by using an organic microporous filter membrane of 0.22um, and then determining the forbidden azo dyes by adopting a GC/MSD method through a gas chromatograph.
Example 3:
the invention provides a technical scheme that: a method of detecting banned azo dyes in a textile, comprising the steps of:
step 1: weighing 3g of sample, placing the sample into a reaction bottle, and adding 20ml of citrate buffer solution and 3ml of sodium hydrosulfite solution, wherein the concentration of the sodium hydrosulfite solution is 250 mg/ml;
step 2: sealing the reaction bottle, shaking vigorously, placing in 72 deg.C water bath, keeping the temperature for 30min, taking out the reaction bottle, and cooling to room temperature within 2 min;
And step 3: adding 10ml of methyl tert-butyl ether into a reaction bottle, sealing the reaction bottle, and then placing the reaction bottle on an oscillating device to shake forcibly, wherein the oscillating device is a mechanical oscillator, the oscillating speed of the mechanical oscillator is 240rmp/min, and the oscillating time is 30 min;
and 4, step 4: transferring the reaction solution in the reaction bottle to a diatomite extraction column, standing and absorbing for 20 min;
and 5: adding 10ml of methyl tert-butyl ether into a reaction bottle to elute the reaction solution in the reaction bottle, and pouring the eluted reaction solution onto a kieselguhr extraction column;
step 6: pouring 70ml of methyl tert-butyl ether into a diatomite extraction column, controlling the flow rate, and collecting all eluent into a 150ml standard-caliber flat-bottom flask;
and 7: performing rotary evaporation and concentration on the extracting solution in the flat-bottomed flask to nearly 1ml, quickly metering the volume of the remainder to 2ml by using methyl tert-butyl ether to obtain a sample concentrated solution, wherein the rotary evaporation and concentration device of the extracting solution in the flat-bottomed flask is a vacuum rotary evaporator, and the concentration temperature of the vacuum rotary evaporator is 40 ℃;
and 8: adding 20mL of citrate buffer solution preheated to 72 ℃ into the sample concentrated solution, placing the sample into a sample bottle for sealing, keeping the temperature of 72 ℃ for 35min, adding 2mL of reduction cracking agent sodium dithionite aqueous solution, shaking the sample bottle forcibly, keeping the temperature of 72 ℃ for 30min directly, and then cooling to room temperature to obtain reduction cracking solution;
And step 9: adding 0.3mL of sodium hydroxide, 5g of sodium chloride and 4mL of deuterated naphthalene standard solution with the concentration of 10mg/L into the reduction lysate, and then placing a sample bottle on a horizontal oscillator to oscillate for 15min to obtain an extract liquor;
step 10: transferring a small amount of extract liquid into an automatic sample injection bottle, filtering the extract liquid by using an organic microporous filter membrane of 0.22um, and then determining the forbidden azo dyes by adopting a GC/MSD method through a gas chromatograph.
In summary, the embodiment greatly reduces the detection cost of the banned azo fuel of the textile, and improves the detection efficiency of the banned azo fuel of the textile.
Application method
A method of detecting banned azo dyes in a textile, comprising the steps of:
step 1: weighing 1-3 g of sample, placing the sample into a reaction bottle, and adding 15-20 ml of citrate buffer solution and 3ml of sodium hydrosulfite solution;
step 2: sealing the reaction bottle, shaking forcibly, putting the reaction bottle into a water bath at 68-72 ℃ for heat preservation for 25-30 min, taking out the reaction bottle, and cooling to room temperature within 2 min;
and step 3: adding 8-10 ml of methyl tert-butyl ether into a reaction bottle, sealing the reaction bottle, and then placing the reaction bottle on an oscillating device to shake forcibly;
and 4, step 4: transferring the reaction solution in the reaction bottle to a diatomite extraction column, standing and absorbing for 15-20 min;
And 5: adding 10ml of methyl tert-butyl ether into a reaction bottle to elute the reaction solution in the reaction bottle, and pouring the eluted reaction solution onto a kieselguhr extraction column;
step 6: pouring 70ml of methyl tert-butyl ether into a diatomite extraction column, controlling the flow rate, and collecting all eluent into a 150ml standard-caliber flat-bottom flask;
and 7: performing rotary evaporation and concentration on the extracting solution in the flat-bottomed flask to nearly 1ml, and quickly metering the remainder to 2ml by using methyl tert-butyl ether to obtain a sample concentrated solution;
and 8: adding 15-20 mL of citrate buffer solution preheated to 68-72 ℃ into the sample concentrated solution, placing the sample concentrated solution into a sample bottle, sealing the sample bottle, keeping the temperature of 68-72 ℃ for 35min, adding 2mL of reduction cracking agent sodium dithionite aqueous solution, forcibly shaking the sample bottle, directly keeping the sample bottle at 68-72 ℃ for 30min, and then cooling to room temperature to obtain reduction cracking solution;
and step 9: adding 0.3mL of sodium hydroxide, 5g of sodium chloride and 4mL of deuterated naphthalene standard solution with the concentration of 10mg/L into the reduction lysate, and then placing a sample bottle on a horizontal oscillator to oscillate for 15min to obtain an extract liquor;
step 10: and (4) transferring a small amount of extract liquid into an automatic sample feeding bottle, and performing forbidden azo dye determination by a gas chromatograph by adopting a GC/MSD method.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for detecting banned azo dyes in textiles, comprising the steps of:
step 1: weighing 1-3 g of sample, placing the sample into a reaction bottle, and adding 15-20 ml of citrate buffer solution and 3ml of sodium hydrosulfite solution;
step 2: sealing the reaction bottle, shaking forcibly, putting the reaction bottle into a water bath at 68-72 ℃ for heat preservation for 25-30 min, taking out the reaction bottle, and cooling to room temperature within 2 min;
and step 3: adding 8-10 ml of methyl tert-butyl ether into a reaction bottle, sealing the reaction bottle, and then placing the reaction bottle on an oscillating device to shake forcibly;
and 4, step 4: transferring the reaction solution in the reaction bottle to a diatomite extraction column, standing and absorbing for 15-20 min;
and 5: adding 10ml of methyl tert-butyl ether into a reaction bottle to elute the reaction solution in the reaction bottle, and pouring the eluted reaction solution onto a kieselguhr extraction column;
Step 6: pouring 70ml of methyl tert-butyl ether into a diatomite extraction column, controlling the flow rate, and collecting all eluent into a 150ml standard-caliber flat-bottom flask;
and 7: performing rotary evaporation and concentration on the extracting solution in the flat-bottomed flask to nearly 1ml, and quickly metering the remainder to 2ml by using methyl tert-butyl ether to obtain a sample concentrated solution;
and 8: adding 15-20 mL of citrate buffer solution preheated to 68-72 ℃ into the sample concentrated solution, placing the sample concentrated solution into a sample bottle, sealing the sample bottle, keeping the temperature of 68-72 ℃ for 35min, adding 2mL of reduction cracking agent sodium dithionite aqueous solution, forcibly shaking the sample bottle, directly keeping the sample bottle at 68-72 ℃ for 30min, and then cooling to room temperature to obtain reduction cracking solution;
and step 9: adding 0.3mL of sodium hydroxide, 5g of sodium chloride and 4mL of deuterated naphthalene standard solution with the concentration of 10mg/L into the reduction lysate, and then placing a sample bottle on a horizontal oscillator to oscillate for 15min to obtain an extract liquor;
step 10: and (4) transferring a small amount of extract liquid into an automatic sample feeding bottle, and performing forbidden azo dye determination by a gas chromatograph by adopting a GC/MSD method.
2. A method of detecting banned azo dye in a textile according to claim 1, wherein: in the step 1, the concentration of the sodium hydrosulfite solution is 200-250 mg/ml.
3. A method of detecting banned azo dye in a textile according to claim 1, wherein: in the step 3, the oscillation device is a mechanical oscillator, the oscillation speed of the mechanical oscillator is 220 to 240rmp/min, and the oscillation time is 25 to 30 min.
4. A method of detecting banned azo dye in a textile according to claim 1, wherein: in the step 7, a device for rotary evaporation and concentration of the extracting solution in the flat-bottomed flask is a vacuum rotary evaporator, and the concentration temperature of the vacuum rotary evaporator is 38-40 ℃.
5. A method of detecting banned azo dye in a textile according to claim 1, wherein: in step 10, the extract is filtered through a 0.22um organic microporous membrane and then azo dye is measured by a gas chromatograph.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010645986.3A CN111855846A (en) | 2020-07-07 | 2020-07-07 | Method for detecting banned azo dye in textile |
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| CN202010645986.3A CN111855846A (en) | 2020-07-07 | 2020-07-07 | Method for detecting banned azo dye in textile |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN118706556A (en) * | 2024-08-23 | 2024-09-27 | 成都产品质量检验研究院有限责任公司 | Azo dye detection pretreatment device in leather for full-automatic furniture product and application method thereof |
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Application publication date: 20201030 |