CN103713062A - Method for fast detection of residual amount of restricted organic solvents in textile - Google Patents
Method for fast detection of residual amount of restricted organic solvents in textile Download PDFInfo
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Abstract
The invention provides a method for fast detection of residual amount of restricted organic solvents in a textile. An extraction agent is utilized for extraction, and an extraction solution is determined by using gas chromatography-mass spectrometry. Compared with the prior art, a conventional chemical analytical instrument of gas chromatography-mass spectrometry is adopted for detecting the content of a variety of harmful organic solvents in the textile, the pretreatment is fast and simple, detection limits are low, the accuracy is high, and the detection throughput is high, so that the method is very suitable for batch detection of restricted substances; and in addition, by adopting the detection method provided by the invention, the current blank in the method for detecting the content of the variety of the harmful organic solvents in a light and textile product is filled up, important technical support is provided for product quality control and safety monitoring, and the method can be used for detecting the residual amount of the organic solvents in textile products, leather products and various raw materials and further has good economic and social benefits.
Description
Technical field
The invention belongs to product quality detection field, be specifically related to limit the use of in a kind of textile the high flux method for quick of Determination of Residual Organic Solvents.
Background technology
Textile arranges and all unavoidably can use a large amount of organic solvents from raw material production and processing to finished product.Existing a series of laws and regulations forbid using the poisonous and hazardous organic solvent of part at textile in the world, be included in process of manufacture and ban use of, must not be residual on final products, or on final products, volatilizable organism must not surpass the different statements such as a certain Limited Doses.
The organic solvent that in textile, rules limit the use of at present mainly contains amide solvent, glycol ethers solvent and 1-METHYLPYRROLIDONE solvent.The 2003/36/EC of European Union instruction in 2003 is by following material: formamide, N-METHYLFORMAMIDE, N-methylacetamide, N, dinethylformamide, N, the materials such as N-dimethyl acetamide, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, glycol dimethyl ether, diethylene glycol dimethyl ether are listed in REACH instruction restricted substances list, are classified as the inventory of the 2nd class genotoxicity material.Europe chemicals management board (ECHA) listed amide solvent (totally 3 kinds), glycol ethers solvent (totally 5 kinds) and 1-METHYLPYRROLIDONE to show great attention to material SVHC inventory in successively from year Dec in Dec, 2010 to 2012, stipulated that such material need could be used through authorizing.International Textile ecological study with detect association's issue 2012 ecological textile Valuation Standard (Oeko-TexStandard100) by N, the Determination of Residual Organic Solvents such as N-dimethyl acetamide and 1-METHYLPYRROLIDONE are listed in sensing range, within 2013, increase again N newly, dinethylformamide, and the requirement that proposes to limit the quantity of is: 0.1%.
Therefore, need detection technique that timely foundation has an independent intellectual property right badly for measuring the multiple Determination of Residual Organic Solvents that limits the use of in textile, realize to textile produce and circulation in security control.
For the above-mentioned organic solvent that limits the use of, the existing detection method of part.The people such as Cheng Qun use DMF in the ultrasonic extraction textile of methylene chloride, and gas chromatograph-mass spectrometer (GCMS) detects, and detection limit can reach 0.5mg/kg.The people such as Xiang Zhongchao set up the detection method of dimethyl formamide and dimethyl acetamide in high effective liquid chromatography for measuring workshop air, for environment measuring and hygienical evaluation.The people such as Lian Qiuyan, by the ultrasonic extraction of methyl alcohol to the hexylene glycol monomethyl ether in textile and ethylene glycol monoethyl ether, adopt mass spectrometer to analyze mensuration, and method detects and is limited to 2.0mg/kg～3.5mg/kg.The people such as Kong Xiangwei adopt Headspace-Gas Chromatography Analysis to detect the residual quantity of DMA and 1-METHYLPYRROLIDONE in textile, and detectability is respectively 6.8mg/kg and 11.6mg/kg.The people such as Cheng little Yan have set up high performance liquid chromatography-series connection quadrupole rod measuring method of mass spectrum of 1-METHYLPYRROLIDONE in the gentle sample of water.
There are following three problems in prior art at present: 1. issued relevant laws and regulations both at home and abroad and in textile, limited the use of some organic solvent, but also there is no at present corresponding detection method, as formamide, N-METHYLFORMAMIDE, N-methylacetamide, glycol dimethyl ether, ethylene glycol diethyl ether etc.; 2. existing method can not be measured the current multiple organic solvent that limits the use of simultaneously.Because the physicochemical property of various organic solvents is different, be difficult to carry out effective qualitative and quantitative analysis in same detection method.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, set up multiplely in a kind of textile to limit the use of simultaneously method for measuring of organic solvent, and the security performance that is applied to textile product detects.
The invention provides the method for quick that limits the use of Determination of Residual Organic Solvents in a kind of textile, utilize extractant to extract, extract is measured with gas chromatography-mass spectrum.
Further, in the textile that the present invention limits, limit the use of organic solvent and comprise formamide, N-METHYLFORMAMIDE, N-methylacetamide, N, dinethylformamide, DMA, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, glycol dimethyl ether, diethylene glycol dimethyl ether and 1-METHYLPYRROLIDONE.
Further, the concrete technical scheme of the present invention is as follows:
(1) configuration standard solution: as solvent, the standard items that limit the use of organic solvent are dissolved, thereby preparation becomes the standard operation solution of certain gradient with extractant;
(2) prepare testing sample solution:
A) testing sample is cut into 5cm * 5cm, then accurately takes testing sample 1g, and in testing sample, add the extractant of 10～30ml, then in extraction equipment, extract, filter and be extracted liquid;
B) by steps A) extract of gained, at bath temperature, be at 20～70 ℃, reduced pressure concentration after drying up, obtains concentrated residue again;
C) by step B) residue obtained use 1～10ml extractant fully dissolves, and the sample liquid of gained, with after 0.45 μ m membrane filtration, obtains testing sample solution;
(3) gas chromatography-mass spectrometry analysis condition is:
Chromatographic condition: middle polarity chromatographic column; Injector temperature, 230 ℃, Splitless injecting samples; Temperature programme, 60 ℃ of initial temperatures, keep 2min, with the speed of 20 ℃/min, are warming up to 260 ℃, keep 5min; Carrier gas is helium, and purity is 99.999%, 1mL/min constant current; Mass spectrum condition: transmission line temperature, 230 ℃; Ion gun adopts EI source; Ion source temperature is 250 ℃; The ionization energy is 70eV; Level Four bar temperature, 200 ℃; Sweep limit is 35～350amu;
(4) drawing standard curve
The mixed standard solution of preparing in (1), according to concentration, carry out successively from low to high gas chromatography-mass spectrum detection, parameter synchronization rapid (3), take and limit the use of material chromatographic peak area as horizontal ordinate, and limiting the use of material concentration is ordinate, drawing standard curve;
(5) measure
When reaching after mensuration requires, instrument indices detects, accurately sample solution 1 μ L injection gas chromatography-mass spectrum to be tested is detected, parameter synchronization rapid (3), reference standard curve, according to retention time and corresponding qualitative features ion, carry out qualitative, according to quota ion, carry out peak area quantification calculating, using signal/noise than S/N=3 as detection limit, S/N=10 is as quantitative limit.
Further, described extractant is selected from methyl alcohol, ethanol, acetone and acetonitrile; Methyl alcohol more preferably.
Further, described extraction equipment is selected from ultrasonic extraction instrument, soxhlet extraction instrument and microwave extracting apparatus; Ultrasonic extraction instrument more preferably.
Further, the extraction conditions in step (2) is in the ultrasound wave of 30～45kHz, at bath temperature, is ultrasonic extraction 10～60min at 20～70 ℃, filters and is extracted liquid.
Compared with prior art, the present invention has following beneficial effect: 1. this method adopts this conventional chemical analysis instrument of gas chromatography/mass spectrometry to detect the content of multiple harmful organic solvent in textile, pre-treatment is simple fast, detection limit is low, accuracy is high, detection flux is high, is highly suitable for limiting the use of in textile the batch detection of material.2. detection method of the present invention has been filled up the blank of multiple harmful organic solvent detection method of content in textiles and other light industrial goods at present, for production quality control and security monitoring provide important technical support, can, for detection of the organic solvent residual in textile product, leather and fur products and various raw material, there is good economic and social benefit.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
This method comprises formamide, N-METHYLFORMAMIDE, N-methylacetamide, N to limiting the use of organic solvent in textile, dinethylformamide, N, the materials such as N-dimethyl acetamide, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, glycol dimethyl ether, diethylene glycol dimethyl ether and 1-METHYLPYRROLIDONE carry out qualitative, quantitative mensuration, and concrete steps comprise:
(1) configuration standard solution: as solvent, the standard items that limit the use of organic solvent are dissolved, thereby preparation becomes the standard operation solution of certain gradient with methyl alcohol;
(2) prepare testing sample solution:
A) testing sample being cut into 5cm * 5cm, then accurately taking testing sample 1g, and in testing sample, add the extractant methyl alcohol of 20ml,, in the ultrasound wave of 45kHz, is then ultrasonic extraction 30min at 50 ℃ at bath temperature; Filtration is extracted liquid;
B) by steps A) extract of gained, at bath temperature, be at 50 ℃, reduced pressure concentration after drying up, obtains concentrated residue again;
C) by step B) residue obtainedly with 5ml methyl alcohol, fully dissolve, the sample liquid of gained, with after 0.45 μ m membrane filtration, obtains testing sample solution;
(3) gas chromatography-mass spectrometry analysis condition is:
Chromatographic condition: middle polarity chromatographic column; Injector temperature, 230 ℃, Splitless injecting samples; Temperature programme, 60 ℃ of initial temperatures, keep 2min, with the speed of 20 ℃/min, are warming up to 260 ℃, keep 5min; Carrier gas is helium, and purity is 99.999%, 1mL/min constant current; Mass spectrum condition: transmission line temperature, 230 ℃; Ion gun adopts EI source; Ion source temperature is 250 ℃; The ionization energy is 70eV; Level Four bar temperature, 200 ℃; Sweep limit is 35～350amu;
(4) drawing standard curve
The mixed standard solution of preparing in (1), according to concentration, carry out successively from low to high gas chromatography-mass spectrum detection, parameter synchronization rapid (3), take and limit the use of material chromatographic peak area as horizontal ordinate, and limiting the use of material concentration is ordinate, drawing standard curve;
(5) measure
When reaching after mensuration requires, instrument indices detects, accurately sample solution 1 μ L injection gas chromatography-mass spectrum to be tested is detected, parameter synchronization rapid (3), reference standard curve, according to retention time and corresponding qualitative features ion, carry out qualitative, according to quota ion, carry out peak area quantification calculating, using signal/noise than S/N=3 as detection limit, S/N=10 is as quantitative limit.
Adopt said method to measure the content that limits the use of organic solvent in testing sample in above-mentioned textile by qualitative, quantitative.
Embodiment 2
This method comprises formamide, N-METHYLFORMAMIDE, N-methylacetamide, N to limiting the use of organic solvent in textile, dinethylformamide, N, the materials such as N-dimethyl acetamide, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, glycol dimethyl ether, diethylene glycol dimethyl ether and 1-METHYLPYRROLIDONE carry out qualitative, quantitative mensuration, and concrete steps comprise:
(1) configuration standard solution: as solvent, the standard items that limit the use of organic solvent are dissolved, thereby preparation becomes the standard operation solution of certain gradient with acetonitrile;
(2) prepare testing sample solution:
A) testing sample being cut into 5cm * 5cm, then accurately taking testing sample 1g, and in testing sample, add the extractant acetonitrile of 30ml,, in the ultrasound wave at 30kHz, is then ultrasonic extraction 10min at 70 ℃ at bath temperature, filters and is extracted liquid;
B) by steps A) extract of gained, at bath temperature, be at 70 ℃, reduced pressure concentration after drying up, obtains concentrated residue again;
C) by step B) residue obtainedly with 10ml extractant, fully dissolve, the sample liquid of gained, with after 0.45 μ m membrane filtration, obtains testing sample solution;
(3) gas chromatography-mass spectrometry analysis condition is:
Chromatographic condition: middle polarity chromatographic column; Injector temperature, 230 ℃, Splitless injecting samples; Temperature programme, 60 ℃ of initial temperatures, keep 2min, with the speed of 20 ℃/min, are warming up to 260 ℃, keep 5min; Carrier gas is helium, and purity is 99.999%, 1mL/min constant current; Mass spectrum condition: transmission line temperature, 230 ℃; Ion gun adopts EI source; Ion source temperature is 250 ℃; The ionization energy is 70eV; Level Four bar temperature, 200 ℃; Sweep limit is 35～350amu;
(4) drawing standard curve
The mixed standard solution of preparing in (1), according to concentration, carry out successively from low to high gas chromatography-mass spectrum detection, parameter synchronization rapid (3), take and limit the use of material chromatographic peak area as horizontal ordinate, and limiting the use of material concentration is ordinate, drawing standard curve;
(5) measure
When reaching after mensuration requires, instrument indices detects, accurately sample solution 1 μ L injection gas chromatography-mass spectrum to be tested is detected, parameter synchronization rapid (3), reference standard curve, according to retention time and corresponding qualitative features ion, carry out qualitative, according to quota ion, carry out peak area quantification calculating, using signal/noise than S/N=3 as detection limit, S/N=10 is as quantitative limit.
Adopt said method to measure the content that limits the use of organic solvent in testing sample in above-mentioned textile by qualitative, quantitative.
It will be recognized by those skilled in the art, do not departing under the prerequisite of protection scope of the present invention, can carry out various modifications, variation and combination to above-mentioned embodiment, and think that this modification, variation and combination are within the scope of originality thought.
Claims (8)
1. in textile, limit the use of a method for quick for Determination of Residual Organic Solvents, utilize extractant to extract, extract is measured with gas chromatography-mass spectrum.
2. method for quick according to claim 1, it is characterized in that in described textile, limiting the use of organic solvent comprises formamide, N-METHYLFORMAMIDE, N-methylacetamide, N, dinethylformamide, DMA, ethylene glycol monomethyl ether, ethylene glycol ethyl ether, glycol dimethyl ether, diethylene glycol dimethyl ether and 1-METHYLPYRROLIDONE.
3. according to the method for quick described in any one in claim 1-2, it is characterized in that concrete steps comprise:
(1) configuration standard solution: be solvent with extractant, the standard items that limit the use of organic solvent are dissolved, thereby preparation become the standard operation solution of certain gradient;
(2) prepare testing sample solution:
A) testing sample is cut into 5cm * 5cm, then accurately takes testing sample 1g, and in testing sample, add the extractant of 10～30ml, then in extraction equipment, extract, filter and be extracted liquid;
B) by steps A) extract of gained, at bath temperature, be at 20～70 ℃, reduced pressure concentration after drying up, obtains concentrated residue again;
C) by step B) residue obtained use 1～10ml extractant fully dissolves, and the sample liquid of gained, with after 0.45 μ m membrane filtration, obtains testing sample solution;
(3) gas chromatography-mass spectrometry analysis condition is:
Chromatographic condition: middle polarity chromatographic column; Injector temperature, 230 ℃, Splitless injecting samples; Temperature programme, 60 ℃ of initial temperatures, keep 2min, with the speed of 20 ℃/min, are warming up to 260 ℃, keep 5min; Carrier gas is helium, and purity is 99.999%, 1mL/min constant current; Mass spectrum condition: transmission line temperature, 230 ℃; Ion gun adopts EI source; Ion source temperature is 250 ℃; The ionization energy is 70eV; Level Four bar temperature, 200 ℃; Sweep limit is 35～350amu;
(4) drawing standard curve
The mixed standard solution of preparing in (1), according to concentration, carry out successively from low to high gas chromatography-mass spectrum detection, parameter synchronization rapid (3), take and limit the use of material chromatographic peak area as horizontal ordinate, and limiting the use of material concentration is ordinate, drawing standard curve;
(5) measure
When reaching after mensuration requires, instrument indices detects, accurately sample solution 1 μ L injection gas chromatography-mass spectrum to be tested is detected, parameter synchronization rapid (3), reference standard curve, according to retention time and corresponding qualitative features ion, carry out qualitative, according to quota ion, carry out peak area quantification calculating, using signal/noise than S/N=3 as detection limit, S/N=10 is as quantitative limit.
4. according to the detection method described in claim 3, it is characterized in that, described extractant is selected from a kind of in methyl alcohol, ethanol, acetone or acetonitrile.
5. according to the detection method described in claim 4, it is characterized in that, described extractant is methyl alcohol.
6. detection method according to claim 3, is characterized in that, described extraction equipment is selected from ultrasonic extraction instrument, soxhlet extraction instrument or microwave extracting apparatus.
7. detection method according to claim 6, is characterized in that, described extraction equipment is ultrasonic extraction instrument.
8. detection method according to claim 3, is characterized in that, the extraction conditions in step (2) is in the ultrasound wave of 30～45kHz, at bath temperature, is ultrasonic extraction 10～60min at 20～70 ℃, filters and is extracted liquid.
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| CN109142609A (en) * | 2018-10-25 | 2019-01-04 | 深圳出入境检验检疫局工业品检测技术中心 | A kind of method of glycol ether and its acetate residual quantity in measurement dyeing and finishing auxiliaries |
| CN109490456A (en) * | 2018-11-21 | 2019-03-19 | 山东省产品质量检验研究院 | The detection method of formamide content in a kind of foamed plastic pad |
| CN109490455A (en) * | 2018-11-21 | 2019-03-19 | 山东省产品质量检验研究院 | The detection method of formamide burst size and rate of release in Yoga mat |
| CN109490455B (en) * | 2018-11-21 | 2021-02-02 | 山东省产品质量检验研究院 | Method for detecting formamide release amount and release rate in yoga mat |
| CN111781287A (en) * | 2020-07-21 | 2020-10-16 | 宁波卫生职业技术学院 | Method for detecting residual solvent in medical non-woven fabric product |
| CN114487248A (en) * | 2020-10-27 | 2022-05-13 | 天津市职业大学 | Method for measuring total volatile organic compounds in disposable mask |
| CN114441653A (en) * | 2020-10-30 | 2022-05-06 | 谱尼测试集团深圳有限公司 | Gas chromatography-mass spectrometry detection method for measuring content of tetraethylene glycol dimethyl ether |
| CN113092621A (en) * | 2021-04-07 | 2021-07-09 | 华东理工大学 | Method for detecting formamide content in product |
| CN113092621B (en) * | 2021-04-07 | 2022-04-01 | 华东理工大学 | Method for detecting formamide content in product |
| CN114200062A (en) * | 2021-12-14 | 2022-03-18 | 福建省纤维检验中心 | Method for detecting tetraethylene glycol dimethyl ether in leather |
| CN114414708A (en) * | 2021-12-16 | 2022-04-29 | 深圳天祥质量技术服务有限公司 | Method for detecting tetraethylene glycol dimethyl ether |
| CN114414708B (en) * | 2021-12-16 | 2024-01-23 | 深圳天祥质量技术服务有限公司 | Method for detecting tetraethylene glycol dimethyl ether |
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