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1 Ecological textile testing requirements
In recent years, with the strengthening of people's awareness of environmental protection, countries around the world are actively developing and producing products that are beneficial to human health and environmental protection. Ecological textiles are increasingly being watched and sought after by people. Eco-textiles not only require the textile itself to be non-toxic and harmless, but also have no irritating contact with the human body. At the same time, it requires that its production and processing processes such as printing and dyeing, finishing and other processes do not produce toxic and harmful substances, and dyes and dyeing auxiliaries should be safe and biodegradable. . Therefore, the international control of the content of harmful substances in textiles is becoming more and more strict. At present, eco-textile standards and domestic standards mainly include formaldehyde, color fastness to water, color fastness to perspiration, color fastness to rubbing, color fastness to saliva, decomposable aromatic amines, extractable heavy metals (锑, arsenic, lead). , cadmium, chromium, cobalt, copper, nickel, mercury), chlorophenol (tetrachlorophenol, pentachlorophenol), organic chlorine carrier, pH and other testing items. Among them, carcinogenic dyes, sensitizing dyes and insecticides are especially concerned.
At present, there are many technical problems in the detection of textiles. For example, in the detection technology of carcinogenic dyes, sensitizing dyes and insecticides in textiles, there is a common feature that the substances to be inspected are wrapped and deeply buried in fibers and fabrics. Pre-extraction treatment of these substances to be tested is more complicated and difficult, so special extraction means are needed! At the same time, with the continuous development of textiles, textiles are no longer one or two simple components of cotton, hemp or polyester. More and more blended and interwoven textiles have entered the market and become dominant, which further increases textiles. The difficulty of detecting pre-processing.
(l) Disabling azo dyes and allergic dyes
A variety of azo dyes are known to be carcinogenic dyes. It is strictly prohibited to use. Azo dyes can cause body vision, respiratory and skin irritation. In the international textile and apparel trade, allergic dyes are listed as banned by eco-textile standards. Sensitive disperse dyes are dyes that cause allergic effects on the skin and respiratory organs of human or animal bodies. They are widely used in textiles and leather products. Etching and printing processes.
(2) Insecticides
In the process of growing natural cotton plants such as cotton and hemp, pesticides should be used for pest control and weeding. Therefore, some pesticides are absorbed by crop fibers and remain on plants and garments, which will cause certain harm when worn. The standard stipulates that pesticide residues on fabric garments must not exceed 1 ppm. The residual amount on the infant's clothing must not exceed 0.5ppm. Â
2 Current pre-treatment methods and methods for eco-textiles
(1) Detection of banned azo dyes and sensitizing dyes
At present, the standard for the detection of azo dyes used in China is GB/T17592-2006 "Determination of banned azo dyes for textiles". The basic principle is to reduce the decomposition of textile samples to produce aromatic amines. After extraction and concentration, use gas chromatography. The instrument is measured and quantified by high pressure liquid chromatography, diode array detector or gas chromatography, mass spectrometry. According to the standard, the non-polyester sample was treated in the reactor for 1 h, then extracted by 15 min, concentrated and analyzed by gas chromatography. When testing polyester dyed samples, it requires nearly 1 hour more than the conventional method because of special pretreatment. In addition, if the composition of the sample is not known, the sample should be subjected to qualitative analysis of the fiber composition before testing. The detection procedure is complicated, the experiment time is long, and the efficiency is low.
(2) Detection of pesticides
At present, the pesticide testing standard adopted in China is GB/T18412 "Determination of textile pesticide residues", including the following parts: Part I: 77 pesticides; Part II: Organochlorine pesticides; Part III: Organophosphorus pesticides; Four parts: pyrethroid pesticides; the fifth part: organic nitrogen pesticides; the sixth part: stupid carboxylic acid pesticides; the seventh part: toxaphene. The detection principle is as follows: the sample is ultrasonically extracted and determined by gas chromatography or gas chromatography-mass spectrometry.
(3) A comparative analysis of the pre-treatment methods involved in the standard is as follows:
1) Solicitation (SE)
Soxhlet extraction is one of the classic pre-treatment methods commonly used to treat solid, semi-solid samples to achieve pre-separation of analytes from matrix materials. When multiple substances are simultaneously measured, different analytes can be extracted step by step by cable extraction. The extraction efficiency is high. The main disadvantage of this method is that it takes a long time (generally above 16h), the organic solvent consumption is large, the operation is complicated, and it is difficult to realize automation. At present, this method has rarely been used.
2) Ultrasonic extraction (UE)
Ultrasonic extraction is now a more common and effective extraction method, especially for solid and semi-solid samples. Ultrasonic extraction mainly uses the cavitation of ultrasonic waves to accelerate the extraction of the desired components, and the secondary effects of ultrasonic waves (such as mechanical vibration, emulsification, Diffusion, chemical effects, etc.) accelerate the diffusion release of the pre-extracted components, allowing them to be thoroughly mixed with the solvent. Compared with the conventional extraction method, ultrasonic extraction has the advantages of short extraction time, high yield, and no heating. Compared with cable extraction, the efficiency is greatly improved. However, ultrasonic extraction requires the use of a large amount of organic solvent (about 30 to 60 mL), which is not environmentally friendly compared to the more advanced pretreatment technology. In addition, ultrasonic extraction is often accompanied by a thermal effect, and there is a certain amount of loss for unstable and volatile decomposition materials.
With the improvement of testing requirements, the development of large-scale testing instruments. Trace detection has become more and more extensive, and the pretreatment technology of samples has been paid more and more attention by experts from all walks of life. The effect of sample pretreatment technology on the detection and analysis results has a large proportion, and there are analysis and identification: detection and analysis. Nearly 50% of the resulting error is due to sample preparation and processing, and less than 30% of the actual analysis. And most of the sample pre-processing takes up more than 70% of the entire analysis. Therefore, the sample pretreatment system is the basis and guarantee for the detection system to achieve fast and accurate purposes. Sample pretreatment technology is moving towards saving time and effort, reducing solvents, reducing environmental pollution, miniaturization, and automation.
3 unique features of the fast solvent extraction instrument (APLE-1000/2000/3000)
Rapid Organic Solvent Extraction is a new sample preparation technology that combines the temperature and pressure with an organic solvent to quickly and efficiently extract various analytes from the substrate. Especially in the trace material detection technology for solid samples, APLE has its remarkable advantages compared to other extraction methods. (1) Fast, only 10-20 minutes to complete; (2) small solvent dosage, 10-40ML solvent dosage; (3) high extraction efficiency, and several solvent extraction options; (4) safety, automation High degree. Therefore, APLE has been widely used in residue detection in the fields of environment, medicine, food and the like. It was selected by the US Environmental Protection Agency (EPA) as the recommended pre-treatment standard method.
The APLE-1000/2000/3000 fast solvent extraction instrument is an advanced instrument with a wide range of applications and high extraction efficiency. It has a lot of innovations in technology.
(1) The advanced infusion pump “three-stage variable pressure pressurizationâ€: the infusion pump selects the pump speed of different sizes according to the volume of the extraction tank, and gradually reduces the speed of the addition according to the increase of the pressure in the extraction tank. Therefore, the pressure overshoot during the pressurization process is effectively avoided, which is very powerful for improving the long-term stability and safety of the instrument.
(2) Adopting pressure control center: The new “pressure control unit†adopts balanced pressure control and mechanical overpressure protection system to ensure safe and reliable operation of the instrument.
(3) Independently developed high pressure resistant extraction tank: easy to use, tightening and sealing, long sealing life (≥500 times), negligible use cost.
(4) Heating protection body: The new “360° full-circle heating furnace†design is adopted, and the extraction pool is heated more evenly, which can accelerate the balance between the electric heating furnace and the sample pool.
(5) The APLE-1000/2000/3000 fast solvent extraction instrument with innovative technology has the following properties: the temperature range is from room temperature to 200 ° C, and the pressure range is from atmospheric pressure to 20 MPa. Among them, the volume of the APLE-2000 extraction tank includes 11, 22, 33mL, which can continuously extract 24 samples; the volume of the APLE-3000 extraction tank includes 1, 5, 10, 22, 34, 66, 100mL, which can be continuously extracted. 12 samples. The development of the single-channel rapid solvent extractor APLE-1000 with 150mL extraction tank is mainly to solve the problem that some laboratory samples are not many, but the sample processing volume may be large, or the content of target compounds in some samples is very high. Low, each extraction requires a large sample size and other issues. Its low cost and simple structure provide users with fast and efficient extraction of individual samples.
4APLE application examples in eco-textile testing
(1) Ma Qiang, Bai Hua et al., using pre-treatment method of accelerated solvent extraction, detecting nonylphenol in different types of textile samples, using anhydrous ethanol as extraction solvent, static circulation extraction at 10.3MPa and 120°C After 2 times, the extract was purified by Supelclean Envi-Carb graphitized carbon black solid phase extraction column, and then qualitatively and quantitatively analyzed by chromatography-mass spectrometry. The limit of quantification of nonylphenol was 10 μg/kg. The average recoveries of nonylphenol ranged from 91.5% to 97.8% and the relative standard deviations ranged from 4.2% to 7.0% in the range of three addition levels of 10-100 μg/kg. . In this test, the pretreatment conditions of the sample were extracted with absolute ethanol (extraction time 30 min), shaking extraction (extraction time 30 min), Soxhlet extraction (extraction time 12 h) and accelerated solvent. The results of extraction (30min) showed that the extraction method of accelerated solvent extraction was superior to other extraction methods, and it had the advantages of less solvent, rapid, and full automation. Therefore, accelerated solvent extraction was chosen as the sample extraction method.
(2) Li Lin, Xue Xiuling and others established a high performance liquid chromatography/diode array detector (HPLC/DAD) method for the determination of chlorophenol in leather and textiles. The method uses accelerated solvent extraction to extract different types of leather and textile samples, using n-hexane as extractant, and statically extracting 3 times at 10.34MPa and 120 °C. The extract is concentrated by nitrogen blower and dissolved in n-hexane. And constant volume; using C18 column, acetonitrile / 0.5% acetic acid solution as mobile phase, DAD wavelength of 214nm for high performance liquid chromatography separation and analysis. The results showed that the concentration of tetrachlorophenol and pentachlorophenol in the range of 0.1-20 mg/L had a good linear relationship (r>0.9999); the average recovery ranged from 96.0% to 101.5%. The relative standard deviation is 0.50%~5.5% (n=7); the detection limit of the method is 0.02mg/kg, which is in compliance with the EU Directive 0.05mg/kg limit. And compared with the national standard GB/T18414.2-2006 "Determination of chlorophenol in textiles Part 2: Gas chromatography", it can be seen that the method extracts solvent and usage amount, extraction time, detection limit and Recycling rates and other aspects are superior to existing testing standards. The establishment of this method provides an efficient, simple and rapid new method for the determination of chlorophenol in leather and textiles.
In addition, rapid organic solvent extraction has been widely used in the detection of soil organic pesticides, volatile substances and food organic pesticides, fats, and organotins. In the textile testing, pesticides are also included (including 77 pesticides, organochlorine pesticides, organophosphorus pesticides, organic nitrogen pesticides, pyrethroid pesticides, phenoxycarboxylic acid pesticides), organotin compounds, pentachlorophenol, and four. Detection of chlorophenol, etc. It is believed that the application of APLE in textile testing will be more and more extensive.
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