CN112557141A - Comparison method of textile formaldehyde detection standards - Google Patents

Abstract

The invention discloses a comparison method of textile formaldehyde detection standards, which is used for researching the influence of acetylacetone reagent preparation, textile detection sample preservation, sample shearing size, extraction temperature, time, oscillation frequency, color development temperature, time, cooling temperature, time and the like on textile formaldehyde content detection and optimal detection conditions. Compared with detection results of different fabrics, the fabrics with larger formaldehyde content are generally specially finished, the reasons of the fabrics are analyzed in detail, and the best detection scheme is determined by comparing the formaldehyde content measurement standards of the textiles at home and abroad, so that the detection accuracy is improved, and the dressing health of consumers is guaranteed. The fabric suitable for the market is better processed for the textile and clothing industry and textile detection centers, and the detection of the formaldehyde content of the textile can play an important guiding role, so that the green textile is better popularized.

Description

Comparison method of textile formaldehyde detection standards

Technical Field

The invention relates to a comparison method of textile formaldehyde detection standards, and belongs to the field of detection of functional textiles.

Background

Formaldehyde is widely used in textile production, is a colorless, irritant odor-sensitive, water-soluble organic substance, and has toxicity. Free formaldehyde is gradually released during the wearing or use of textiles containing formaldehyde. When the respiratory tract is contacted with formaldehyde or the skin touches formaldehyde, inflammation and the like may occur, and the eyes may be affected. It may also cause skin allergy, and even more particularly, induce cancer, etc., which presents a significant safety hazard to the human body. In recent years, people have higher living quality, and the consumer appearance is changed profoundly, so that the safety and the health of the textile are more emphasized besides the requirements of comfort and beauty of the textile. The formaldehyde content is an important textile safety detection project, and a plurality of standards are provided for the determination of the formaldehyde content at home and abroad, so that the safety and health of people are improved.

Based on the current situation, the determination method is reasonably selected, so that the determination of the textile formaldehyde has high efficiency. With the increasing requirements of people on the quality of life, textiles harmful to health are directly excluded from the purchasing range by consumers, so that the textiles containing high-concentration formaldehyde in the market are fewer and fewer. Therefore, the detection standard for effectively determining the content of the low-concentration formaldehyde meets the market demand in the detection standard of the content of the formaldehyde in the textile. But at the same time, the method has the advantages of easy operation, low cost and convenient use.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a comparison method of textile formaldehyde detection standards, so as to solve the technical problems.

In order to achieve the purpose, the invention adopts the technical scheme that: a comparison method of textile formaldehyde detection standards comprises the following steps;

the method comprises the following steps: preparing a correction solution, namely selecting 500ug/mL of formaldehyde stock solution to dilute the formaldehyde stock solution into more than 5 formaldehyde solutions with different concentrations; respectively making standard working curves according to different standards;

step two: preparing a color developing agent, namely adding a little of tertiary water into a 1000mL volumetric flask, weighing 150g of ammonium acetate, dissolving the ammonium acetate in the appropriate tertiary water, guiding the ammonium acetate solution into the volumetric flask by using a glass rod, then respectively transferring 3mL of glacial acetic acid and 2mL of acetic acid acetone into the volumetric flask by using a pipette, diluting the solution to a scale by using the tertiary water, and storing the solution in a brown reagent bottle;

step three: preparing a sample, wherein the sample needs to be sealed and stored before the preparation process of the sample, and the preparation of the sample adopts two preparation methods, namely a water extraction method and a steam absorption method;

an aqueous extraction method: weighing the sample with the mass of 1g under normal conditions, taking 2.5g if the formaldehyde content is too low, but distinguishing adult fabric and infant fabric, taking 1g adult fabric and 2.5g infant fabric, quickly shearing and putting the adult fabric and the infant fabric into a conical flask after sampling, and immediately closing a bottle cap;

steam absorption method: on one sample, the international standard and the American standard are the same in weighing, three samples are taken and 1g is taken respectively, and two samples are taken and 1g is taken respectively in the Chinese standard; if the formaldehyde content is too low, weighing 2.5g of the sample in China and international standards, and more accurately measuring the content;

step four: in the process of extraction, the extraction liquid is extracted,

an aqueous extraction method: putting the sample into a conical flask, adding 100mL of tertiary water, tightly covering the bottle cap, shaking the conical flask to ensure that the sample is completely immersed, putting the conical flask into a water bath oscillator at the temperature of 40 +/-5 ℃ to oscillate for 60 +/-5 min, taking out the conical flask, and filtering the conical flask into another conical flask by using a filter for analysis;

steam absorption method: adding 50mL of water into a wide-mouth bottle, tying the sample with a double-strand thread, hanging the thread end on a hook at the top of a bottle cap without directly contacting with the extract liquor, tightly covering the cap, carefully placing the wide-mouth bottle in an oven at 49 +/-2 ℃ for 1200 +/-15 min, taking out the test bottle, cooling for 30 +/-5 min, taking out the sample, tightly covering the cap again, and shaking up. Filter into erlenmeyer flasks with filter for analysis.

Step five: the color development process is carried out in the presence of a color developing agent,

an aqueous extraction method: taking 5mL of tertiary water and 5mL of a Narse reagent as blank reagents in each standard, transferring 5mL of filtered extract and 5mL of the Narse reagent into a test tube, covering a test tube cover, developing color in a water bath oscillator at 40 ℃ in a dark place for 30min, taking out, and cooling in a dark place for 30min at normal temperature;

steam absorption method: transferring 5mL of extract liquid and 5mL of a Nashi reagent into a test tube, using 5mL of distilled water and 5mL of the Nashi reagent as blank reagents, uniformly mixing, placing the test tube into a water bath with the temperature of 58 +/-1 ℃ for keeping the temperature for 6min, taking out the test tube for cooling, placing the test tube into a water bath with the temperature of 40 +/-2 ℃ for developing the color for 30 +/-5 min according to other standard criteria, taking out the test tube, and cooling the test tube in a dark place for 30 +/-5 min at normal temperature;

step six: in the detection process, the wavelength of a spectrophotometer in the standard water extraction method is 415nm, while the wavelength of other standard methods is 412nm, and the absorbance of the sample color development solution is measured by taking a blank reagent as a reference.

Further, the storage time of the solution obtained in the second step is 12 hours, and the effective period is 6 weeks.

The invention has the beneficial effects that: by comparing the formaldehyde content measurement standards of the textiles at home and abroad, the optimal detection scheme is determined, and the detection accuracy is improved, so that the dressing health of consumers is guaranteed. The fabric suitable for the market is better processed for the textile and clothing industry and textile detection centers, and the detection of the formaldehyde content of the textile can play an important guiding role, so that the green textile is better popularized.

Drawings

FIG. 1 is a schematic diagram showing the relationship between the formaldehyde content and the storage time of the fabric exposed to air according to the present invention;

FIG. 2 is a schematic representation of the effect of sample shear size on formaldehyde content of a fabric according to the present invention;

FIG. 3 is a graph showing the effect of extraction time on formaldehyde content measured according to the present invention;

FIG. 4 is a schematic diagram showing the effect of the extraction temperature on the amount of formaldehyde measured according to the present invention;

FIG. 5 is a schematic diagram showing the effect of the extraction oscillation frequency on the determination of the amount of formaldehyde in the present invention;

FIG. 6 is a graph showing the effect of the development time on the amount of formaldehyde measured in the present invention;

FIG. 7 is a schematic diagram showing the effect of the developing temperature on the measurement result of the formaldehyde content of the sample according to the present invention;

FIG. 8 is a graph showing the relationship between cooling time and formaldehyde content measurement according to the present invention;

FIG. 9 is a schematic diagram of formaldehyde content determination according to various standard methods of the present invention;

FIG. 10 is a schematic diagram showing the results of multiple detections of the same sample according to the present invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein in the specification of the present invention are for the purpose of describing particular embodiments only and are not intended to limit the present invention.

The method comprises the following specific steps:

(1) preparation of a correction solution:

diluting with 1500ug/mL formaldehyde stock solution to obtain more than 5 formaldehyde solutions with different concentrations. And respectively making standard working curves according to different standards. In the Japanese standards, the absorbance is measured at 415nm by a spectrophotometer, and the absorbance is measured at 412nm for all other standards. The data were then plotted as a standard working curve with the y = b + ax equation.

(2) Preparation of color-developing agent

The formulation and storage of the acetone acetate reagent is an important part of the development process. The method for reducing errors generated by the preparation of the composition is as follows: adding a little of tertiary water into a 1000mL volumetric flask, weighing 150g of ammonium acetate, dissolving the ammonium acetate in the appropriate tertiary water, guiding the ammonium acetate solution into the volumetric flask by using a glass rod, respectively transferring 3mL of glacial acetic acid and 2mL of acetic acid acetone into the volumetric flask by using a pipette, and then diluting the solution to a scale by using the tertiary water. Stored in brown reagent bottles. (Nassner reagent is available after 12 hours of storage and the expiration date is 6 weeks).

(3) Preparation of the samples

The sample treatment of each standard needs sealed preservation before testing, and the test also needs rapid operation.

An aqueous extraction method: on one sample, the Chinese standard takes two samples while the International standard takes three samples. And the two standards normally weigh the sample mass at 1g, and if the formaldehyde content is too low, 2.5 g. The Japanese standard requires only one sample. However, the fabric for adults and the fabric for infants need to be distinguished, wherein the fabric for adults is 1g, and the fabric for infants is 2.5 g. After sampling, the mixture is quickly cut into pieces and put into a conical flask, and then the bottle cap is immediately closed.

Steam absorption method: on one sample, the international standard and the American standard are the same in weighing, three samples are taken and each sample is 1g, and the Chinese standard is taken and each sample is 1g in two samples. If the formaldehyde content is too low, 2.5g of the sample is weighed in China and international standards, and the content can be measured more accurately.

(4) Extraction process

An aqueous extraction method: putting the sample into a conical flask, adding 100mL of tertiary water, tightly covering the bottle cap, shaking the conical flask to ensure that the sample is completely immersed, putting the conical flask into a water bath oscillator at the temperature of 40 +/-5 ℃ and oscillating for 60 +/-5 min, and taking out. Filter into another erlenmeyer flask with filter for analysis.

Steam absorption method: 50mL of water was added to the jar, the sample was tied with a double thread, the thread end was hung on a hook at the top of the bottle cap and was not in direct contact with the extract, and the cap was closed tightly. Carefully placing in an oven (1200 +/-15) at the temperature of (49 +/-2) DEG for min, taking out the test bottle, cooling for (30 +/-5) min, taking out the sample, tightly covering the cover, and shaking up. Filter into erlenmeyer flasks with filter for analysis.

(5) Color development process

An aqueous extraction method: for each standard, 5mL of tertiary water and 5mL of Narse reagent were used as blank reagents. Remove 5mL of filtered extract and 5mL of Nashi reagent into the tube and cover the tube. Color development was performed for 30min in a water bath shaker at 40 ℃ in the dark. Taking out, and cooling in dark at normal temperature for 30 min.

Steam absorption method: for each standard developing solution, 5mL of extraction solution and 5mL of Nardosta reagent are transferred into a test tube, and then 5mL of distilled water and 5mL of Nardosta reagent are used as blank reagents. The American standard is that after being mixed evenly, the test tube is put into a water bath with the temperature of 58 +/-1 ℃ and is kept constant for 6min, and then the test tube is taken out and cooled. Other standard method comprises placing the tube in water bath at 40 + -2 deg.C for developing color (30 + -5) min, taking out, and cooling in dark at room temperature for 30 + -5 min.

(6) Measuring

In the detection process, the wavelength of a spectrophotometer in the Japanese standard water extraction method is 415nm, while in other standard methods, the wavelength is 412nm, and the absorbance of the sample color development solution is measured by taking a blank reagent as a reference.

Experimental test results are compared with fig. 1 to 10.

The technical principle of the invention is as follows: the preparation of an acetylacetone reagent, the storage of a textile detection sample, the shearing size of a sample, the influence of extraction temperature, time, oscillation frequency, color development temperature, time, cooling temperature, time and the like on the detection of the formaldehyde content of the textile and the optimal detection condition are explored. Comparing the detection results of different fabrics, the fabric with larger formaldehyde content is generally specially finished, and the reason is analyzed in detail to find out a solution.

The invention has the beneficial effects that: by comparing the formaldehyde content measurement standards of the textiles at home and abroad, the optimal detection scheme is determined, and the detection accuracy is improved, so that the dressing health of consumers is guaranteed. The fabric suitable for the market is better processed for the textile and clothing industry and textile detection centers, and the detection of the formaldehyde content of the textile can play an important guiding role, so that the green textile is better popularized.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (2)

1. A comparison method of textile formaldehyde detection standards is characterized by comprising the following steps;

the method comprises the following steps: preparing a correction solution, namely selecting 500ug/mL of formaldehyde stock solution to dilute the formaldehyde stock solution into more than 5 formaldehyde solutions with different concentrations; respectively making standard working curves according to different standards;

step two: preparing a color developing agent, namely adding a little of tertiary water into a 1000mL volumetric flask, weighing 150g of ammonium acetate, dissolving the ammonium acetate in the appropriate tertiary water, guiding the ammonium acetate solution into the volumetric flask by using a glass rod, then respectively transferring 3mL of glacial acetic acid and 2mL of acetic acid acetone into the volumetric flask by using a pipette, diluting the solution to a scale by using the tertiary water, and storing the solution in a brown reagent bottle;

step three: preparing a sample, wherein the sample needs to be sealed and stored before the preparation process of the sample, and the preparation of the sample adopts two preparation methods, namely a water extraction method and a steam absorption method;

an aqueous extraction method: weighing the sample with the mass of 1g under normal conditions, taking 2.5g if the formaldehyde content is too low, but distinguishing adult fabric and infant fabric, taking 1g adult fabric and 2.5g infant fabric, quickly shearing and putting the adult fabric and the infant fabric into a conical flask after sampling, and immediately closing a bottle cap;

steam absorption method: on one sample, the international standard and the American standard are the same in weighing, three samples are taken and 1g is taken respectively, and two samples are taken and 1g is taken respectively in the Chinese standard; if the formaldehyde content is too low, weighing 2.5g of the sample in China and international standards, and more accurately measuring the content;

step four: in the process of extraction, the extraction liquid is extracted,

an aqueous extraction method: putting the sample into a conical flask, adding 100mL of tertiary water, tightly covering the bottle cap, shaking the conical flask to ensure that the sample is completely immersed, putting the conical flask into a water bath oscillator at the temperature of 40 +/-5 ℃ to oscillate for 60 +/-5 min, taking out the conical flask, and filtering the conical flask into another conical flask by using a filter for analysis;

steam absorption method: adding 50mL of water into a wide-mouth bottle, tying the sample with a double-strand thread, hanging the thread end on a hook at the top of a bottle cap without directly contacting with the extract liquor, tightly covering the cap, carefully placing the wide-mouth bottle in a 49 +/-2 ℃ oven for 1200 +/-15 min, taking out the test bottle, cooling for 30 +/-5 min, taking out the sample, tightly covering the cap again, and shaking uniformly;

filtering with a filter into a conical flask for analysis;

step five: the color development process is carried out in the presence of a color developing agent,

an aqueous extraction method: taking 5mL of tertiary water and 5mL of a Narse reagent as blank reagents in each standard, transferring 5mL of filtered extract and 5mL of the Narse reagent into a test tube, covering a test tube cover, developing color in a water bath oscillator at 40 ℃ in a dark place for 30min, taking out, and cooling in a dark place for 30min at normal temperature;

steam absorption method: transferring 5mL of extract liquid and 5mL of a Nashi reagent into a test tube, using 5mL of distilled water and 5mL of the Nashi reagent as blank reagents, uniformly mixing, placing the test tube into a water bath with the temperature of 58 +/-1 ℃ for keeping the temperature for 6min, taking out the test tube for cooling, placing the test tube into a water bath with the temperature of 40 +/-2 ℃ for developing the color for 30 +/-5 min according to other standard criteria, taking out the test tube, and cooling the test tube in a dark place for 30 +/-5 min at normal temperature;

step six: in the detection process, the wavelength of a spectrophotometer in the standard water extraction method is 415nm, while the wavelength of other standard methods is 412nm, and the absorbance of the sample color development solution is measured by taking a blank reagent as a reference.

2. The method for comparing formaldehyde detection standards of textiles according to claim 1, wherein the storage time of the solution obtained in the second step is 12 hours and the expiration date is 6 weeks.

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