CN105067748B - Method used for determining melamine resin in textiles - Google Patents
Method used for determining melamine resin in textiles Download PDFInfo
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- CN105067748B CN105067748B CN201510483740.XA CN201510483740A CN105067748B CN 105067748 B CN105067748 B CN 105067748B CN 201510483740 A CN201510483740 A CN 201510483740A CN 105067748 B CN105067748 B CN 105067748B
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- 229920000877 Melamine resin Polymers 0.000 title claims abstract description 30
- 239000004640 Melamine resin Substances 0.000 title claims abstract description 20
- 239000004753 textile Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 17
- 150000002500 ions Chemical class 0.000 claims abstract description 26
- 238000004817 gas chromatography Methods 0.000 claims abstract description 18
- CASUWPDYGGAUQV-UHFFFAOYSA-M potassium;methanol;hydroxide Chemical compound [OH-].[K+].OC CASUWPDYGGAUQV-UHFFFAOYSA-M 0.000 claims abstract description 14
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical group NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 12
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 5
- 239000000835 fiber Substances 0.000 claims description 25
- 238000004227 thermal cracking Methods 0.000 claims description 22
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 16
- 238000004458 analytical method Methods 0.000 claims description 15
- 238000005336 cracking Methods 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- -1 Melamine methylol Chemical class 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- USDJGQLNFPZEON-UHFFFAOYSA-N [[4,6-bis(hydroxymethylamino)-1,3,5-triazin-2-yl]amino]methanol Chemical compound OCNC1=NC(NCO)=NC(NCO)=N1 USDJGQLNFPZEON-UHFFFAOYSA-N 0.000 claims description 7
- 239000000284 extract Substances 0.000 claims description 7
- 238000000197 pyrolysis Methods 0.000 claims description 7
- 229920002994 synthetic fiber Polymers 0.000 claims description 7
- 241001465754 Metazoa Species 0.000 claims description 6
- 238000001819 mass spectrum Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000012209 synthetic fiber Substances 0.000 claims description 6
- 229920000742 Cotton Polymers 0.000 claims description 4
- 235000013877 carbamide Nutrition 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000003431 cross linking reagent Substances 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 3
- 241000255789 Bombyx mori Species 0.000 claims description 3
- 229920006052 Chinlon® Polymers 0.000 claims description 3
- 241001597008 Nomeidae Species 0.000 claims description 3
- 241000283973 Oryctolagus cuniculus Species 0.000 claims description 3
- 241000283898 Ovis Species 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 229920000297 Rayon Polymers 0.000 claims description 3
- 229920002334 Spandex Polymers 0.000 claims description 3
- 229920004933 Terylene® Polymers 0.000 claims description 3
- 229920006221 acetate fiber Polymers 0.000 claims description 3
- HGINCPLSRVDWNT-UHFFFAOYSA-N acrylaldehyde Natural products C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 claims description 3
- 235000013399 edible fruits Nutrition 0.000 claims description 3
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- 239000004759 spandex Substances 0.000 claims description 3
- 238000006467 substitution reaction Methods 0.000 claims description 3
- YGCOKJWKWLYHTG-UHFFFAOYSA-N [[4,6-bis[bis(hydroxymethyl)amino]-1,3,5-triazin-2-yl]-(hydroxymethyl)amino]methanol Chemical compound OCN(CO)C1=NC(N(CO)CO)=NC(N(CO)CO)=N1 YGCOKJWKWLYHTG-UHFFFAOYSA-N 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 7
- 238000005143 pyrolysis gas chromatography mass spectroscopy Methods 0.000 abstract 1
- 238000009736 wetting Methods 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 11
- 239000000047 product Substances 0.000 description 10
- 239000004744 fabric Substances 0.000 description 7
- 239000000178 monomer Substances 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 2
- 229920003270 Cymel® Polymers 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N glycolonitrile Natural products N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000005829 trimerization reaction Methods 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 238000004078 waterproofing Methods 0.000 description 2
- CTRPRMNBTVRDFH-UHFFFAOYSA-N 2-n-methyl-1,3,5-triazine-2,4,6-triamine Chemical compound CNC1=NC(N)=NC(N)=N1 CTRPRMNBTVRDFH-UHFFFAOYSA-N 0.000 description 1
- 206010019133 Hangover Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000001736 capillary Anatomy 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000675 fabric finishing Substances 0.000 description 1
- 238000009962 finishing (textile) Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to the technical field of analytic chemistry, and more specifically relates to a method used for determining melamine resin in textiles. The method comprises following steps: samples are weighed, and are delivered into a sample boat, and a potassium hydroxide methanol solution is added for wetting the samples; the sample boat is delivered into a pyrolysis gas chromatography mass spectrometry instrument for determination; qualitative analysis of methyl substituted products in obtained pyrolytic products is carried out, qualitative characteristic ions m/z140, m/z154, m/z168, m/z196, and m/z210 are extracted based on that the characteristic products of melamine resin pryolysis are melamine derivatives substituted with 3 to 6 methyl groups, if all the characteristic ions can be observed, it can be determined that the samples contain melamine resin, if not all the characteristic ions can be observed, it can be determined that the samples contain no melamine resin. The method is capable of reducing polarity of melamine greatly, and improving peak patterns of melamine in gas chromatography; detection is convenient; and relatively low detection limit can be reached.
Description
[technical field]
The invention belongs to technical field of analytical chemistry, specifically a kind of side measuring melmac in textile
Method.
[background technology]
Melamine resin (mf) is the polymer with tripolycyanamide as Material synthesis, and this resin hardness is than ureaformaldehyde tree
Fat is high, nonflammable, water-fast, heat-resisting, ageing-resistant, resistance to electric arc, resistance to chemical attack, has good insulating properties, glossiness and machinery
Intensity, is widely used in timber, plastics, coating, papermaking, weaving, leather, the industry such as electric, medical.Melamine-formaldehyde resin
It is fabric finishing agent, the basis of the profit agent of leather tan, glazing agent and water repellent agent.
Tripolycyanamide is contained on market and has carbamide with the fabric-treating agent that tripolycyanamide is main material production
Condensation substance cross-linking agent, trimethylol melamine resin, hexamethylol melamine resin, trimethylol melamine resin
(tmm), polyhydroxy methyl etherified melamine resin (6md), waterproofing agent such as waterproofing agent aeg, 703, ftc, ftg, mdt etc. belong to many
Melamine methylol derivant type.
These contain the general polymer shape all being formed of fabric-treating agent of tripolycyanamide with tripolycyanamide and other chemicals
Formula exist, when carrying out fabric treating, fabric-treating agent can with fabric on chemical bonding reaction, so that fabric-treating agent grafting is existed
On fabric or temporarily adsorb on fabric fibre, to play certain Chemical Physics effect.But it is as the use of fabric, such as day
Act on according to, detergent, fabric-treating agent easily decomposes the monomer discharging tripolycyanamide, as fabric and contact human skin, three
Paracyanogen amine monomers easily stimulate skin, damage.Therefore, because there is health risk, measure in textile whether contain three
Cymel is very necessary.
At present, whether the method for testing containing melmac has much for identification, has the method measuring free monomer, but
It is that tripolycyanamide is typically existed with resin and polymer form on the textile, in the case of high-load, be only only possible to trip
Presence from monomer.Thermal cracking can be used for the discriminating of melmac, but in directly measuring, cracking trimerization out
Cyanamide monomer is big due to polarity, is difficult to detection in gas chromatogram, and it is poor to show as peak type, hangover seriously, and ion not feature,
Easily disturbed by textile pyrolysis product.
[content of the invention]
Present invention aim to solving above-mentioned deficiency and providing melmac in a kind of mensure textile
Method, greatly reduces the polarity of tripolycyanamide so as to the peak type in gas chromatogram, more preferably it is easier to detection, can reach
Relatively low detection limit.
Design a kind of method measuring melmac in textile for achieving the above object, comprise the following steps:
1) weigh sample, sample is put in example boat, add potassium hydroxide methanol solution to soak sample；
2) example boat is put into thermal cracking gas chromatography GC-MS to measure；
3) qualitative analyses: carry out qualitative analyses according to methyl substitution product in pyrolysis product, split based on melmac
The feature product of solution is 3-6 methyl substituted tripolycyanamide, extractions qualitative features ion is m/z140, m/z154, m/z168,
M/z196, m/z210, if all characteristic ions all exist in sample, are judged to contain melmac in sample, if sample
In product, characteristic ion is not complete, then be judged in sample not contain melmac；
4) quantitative analyses: if qualitative analysis of samples is containing melmac, take melamine solution, add hydroxide
Potassium methanol solution, puts into thermal cracking gas chromatography GC-MS and measures, and as quantitative criterion material, extracts characteristic ion m/
Z210 carries out quantitation according to external standard method, calculates the content of melmac in sample, content is in terms of melamine monomer.
Step 1) in, in potassium hydroxide methanol solution, the concentration of potassium hydroxide is 1%-20%.
Step 2) in, the condition determination of thermal cracking gas chromatography GC-MS is: (1) gas chromatographic column adopts low pole
Hp-5ms post；(2) mass spectrum collection is carried out using selection full scan mode simultaneously；(3) the cracking tube temperature of thermal cracking is 600
Degree.
The parameter of thermal cracking gas chromatography GC-MS is: the column length of (1) gas chromatographic column is 30 meters, and column internal diameter is
0.25 millimeter, thickness is 0.25 micron；(2) gas chromatographic sample introduction mouth temperature is set as 300 DEG C, and temperature programming is 35 DEG C of initial temperature,
It is warmed up to 280 DEG C by 10 DEG C per minute, retain 5 minutes；(3) cracking instrument and gas chromatogram interface temperature are 280 DEG C, pyrolysis time
For 0.2 minute.
Described melmac is carbamide condensation substance cross-linking agent, trimethylol melamine resin, six hydroxyls
Methyl melamine resin, trimethylol melamine resin, polyhydroxy methyl etherified melamine resin or many methylols trimerization
Cyanamide derivant.
Described sample is textile, and described textile includes Plant fiber, animal fiber and synthetic fibers, and described plant is fine
Dimension includes Cotton Gossypii, fiber crops, fruit fiber, and described animal fiber includes Pilus Caprae seu Oviss, the rabbit hair, silkworm silk, and it is fine that described synthetic fibers include polyester
Dimension, viscose fiber, acetate fiber, chinlon, terylene, acrylon, spandex, polyvinyl, polypropylene, polyvinyl chloride fibre.
The present invention passes through to add potassium hydroxide methanol solution in the sample, and puts it into thermal cracking gas chromatography mass spectrum connection
Carried out with instrument reacting cracking so as to crack tripolycyanamide out and methanol reaction, generate methylated tripolycyanamide, thus greatly
Reduce greatly the polarity of tripolycyanamide so as to the peak type in gas chromatogram, more preferably it is easier to detection, can reach relatively low inspection
Rising limit.
[brief description]
Fig. 1 is the mensure total ion current figure of melmac in embodiment 1；
Fig. 2 is that the mensure of melmac in embodiment 1 extracts characteristic ion figure.
[specific embodiment]
Of the present invention is a kind of method measuring melmac in textile, comprises the following steps:
1) weigh sample, sample is shredded into little particle and puts in example boat, add potassium hydroxide methanol solution to soak sample
Product, in this potassium hydroxide methanol solution, the concentration of potassium hydroxide is 1%-20%；
2) example boat is put into thermal cracking gas chromatography GC-MS to measure；
3) qualitative analyses: carry out qualitative analyses according to methyl substitution product in pyrolysis product, split based on melmac
The feature product of solution is 3-6 methyl substituted tripolycyanamide, extractions qualitative features ion is m/z140, m/z154, m/z168,
M/z196, m/z210, if all characteristic ions all exist in sample, are judged to contain melmac in sample, if sample
In product, characteristic ion is not complete, then be judged in sample not contain melmac；
4) quantitative analyses: if qualitative analysis of samples is containing melmac, take melamine solution, add hydroxide
Potassium methanol solution, puts into thermal cracking gas chromatography GC-MS and measures, and as quantitative criterion material, extracts characteristic ion m/
Z210 carries out quantitation according to external standard method, calculates the content of melmac in sample, content in terms of melamine monomer, the party
Method detection is limited to 1%.
Step 1) in, sample is textile, and textile includes Plant fiber, animal fiber and synthetic fibers, Plant fiber
Including Cotton Gossypii, fiber crops, fruit fiber, animal fiber includes Pilus Caprae seu Oviss, the rabbit hair, silkworm silk, and synthetic fibers include polyester fiber, viscose fibre
Dimension, acetate fiber, chinlon, terylene, acrylon, spandex, polyvinyl, polypropylene, polyvinyl chloride fibre.
Step 2) in, the condition determination of thermal cracking gas chromatography GC-MS is: (1) gas chromatographic column adopts low pole
Hp-5ms post；(2) mass spectrum collection is carried out using selection full scan mode simultaneously；(3) the cracking tube temperature of thermal cracking is 600
Degree；The parameter of thermal cracking gas chromatography GC-MS is: the column length of (1) gas chromatographic column is 30 meters, and column internal diameter is 0.25 milli
Rice, thickness is 0.25 micron；(2) gas chromatographic sample introduction mouth temperature is set as 300 DEG C, and temperature programming is 35 DEG C of initial temperature, by every point
10 DEG C of clock is warmed up to 280 DEG C, retains 5 minutes；(3) cracking instrument and gas chromatogram interface temperature are 280 DEG C, and pyrolysis time is 0.2
Minute.
Wherein, melmac be carbamide condensation substance cross-linking agent, trimethylol melamine resin, six
Melamine methylol resin, trimethylol melamine resin, polyhydroxy methyl etherified melamine resin or many methylols three
Paracyanogen amine derivative.
The invention belongs to the mensure measuring melmac in textile in analytical chemistry field, its principle is: claim
Take sample, add potassium hydroxide methanol solution, put into the analysis of thermal cracking gas chromatography GC-MS, extract cleavage reaction product
Characteristic ion carry out qualitative and quantitative analysis.With reference to specific embodiment, the present invention is made further explained below:
Embodiment 1: the mensure of melmac in green polyester capillariess cloth
1) accurately weigh 1.0mg sample in example boat, add 50 μ l 5% potassium hydroxide methanol solution to soak sample, put
Enter the analysis of thermal cracking gas chromatography GC-MS.
2) thermal cracking-gas chromatograph mass spectrometry instrument parameter is:
(1) gas chromatographic column adopts the hp-5ms post of low pole, and specification is 30 meters of column length, and column internal diameter is 0.25 millimeter, film
Thickness is 0.25 micron；
(2) gas chromatographic sample introduction mouth temperature is set as 300 DEG C, and temperature programming is 35 DEG C of initial temperature, heats up by 10 DEG C per minute
To 280 DEG C, retain 5 minutes；
(3) mass spectrum collection is carried out using selection full scan mode；
(4) the cracking tube temperature of thermal cracking instrument: 600 DEG C, crack instrument and gas chromatogram interface temperature is 280 DEG C, cracking
Time is 0.2 minute.
3) result
(1) qualitative analyses: extraction qualitative features ion is m/z 140, m/z 154, m/z 168, m/z 196, m/z
210, in this sample, characteristic ion all exists, therefore is judged in sample contain melmac；
(2) quantitative analyses: take 1000ug/ml melamine solution 20 μ l, add potassium hydroxide methanol solution, put into hot tearing
Gas chromatography GC-MS measures, and as quantitative criterion material, extracts characteristic ion m/z 210 and carries out determining according to external standard method
Amount, calculates the content of melmac in sample, and content is 2.0% (in terms of melamine monomer).
As shown in Figures 1 and 2, accompanying drawing 1 is the mensure total ion current figure of melmac in embodiment 1, wherein,
The peak of 21-23 minute is the peak of melmac cleavage reaction product methylated melamine；Accompanying drawing 2 is three in embodiment 1
The mensure of cymel extracts characteristic ion figure.
Embodiment 2: the mensure of melmac in white cotton
1) accurately weigh 1.0mg sample in example boat, add 50 μ l 5% potassium hydroxide methanol solution to soak sample, put
Enter the analysis of thermal cracking gas chromatography GC-MS.
2) thermal cracking-gas chromatograph mass spectrometry instrument parameter:
(1) gas chromatographic column adopts the hp-5ms post of low pole, and specification is 30 meters of column length, and column internal diameter is 0.25 millimeter, film
Thickness is 0.25 micron；
(2) gas chromatographic sample introduction mouth temperature is set as 300 DEG C, and temperature programming is 35 DEG C of initial temperature, heats up by 10 DEG C per minute
To 280 DEG C, retain 5 minutes；
(3) mass spectrum collection is carried out using selection full scan mode；
(4) the cracking tube temperature of thermal cracking instrument: 600 DEG C, crack instrument and gas chromatogram interface temperature is 280 DEG C, cracking
Time is 0.2 minute.
3) result
Qualitative analyses: extraction qualitative features ion is m/z 140, m/z 154, m/z 168, m/z 196, m/z 210, this
In sample, characteristic ion does not all exist, therefore is judged in sample not contain melmac.
The present invention is not limited by above-mentioned embodiment, other any spirit without departing from the present invention and principle
Lower made change, modification, replacement, combination, simplification, all should be equivalent substitute mode, are included in the protection model of the present invention
Within enclosing.
Claims (5)
1. a kind of method measuring melmac in textile is it is characterised in that comprise the following steps:
1) weigh sample, sample is put in example boat, add potassium hydroxide methanol solution to soak sample；
2) example boat is put into thermal cracking gas chromatography GC-MS to measure；
3) qualitative analyses: carry out qualitative analyses according to methyl substitution product in pyrolysis product, based on melmac cracking
Feature product is 3-6 methyl substituted tripolycyanamide, and extracting qualitative features ion is m/z140, m/z154, m/z168, m/
Z196, m/z210, if all characteristic ions all exist in sample, are judged to contain melmac in sample, if sample
Middle characteristic ion is not complete, then be judged in sample not contain melmac；
4) quantitative analyses: if qualitative analysis of samples is containing melmac, take melamine solution, add potassium hydroxide first
Alcoholic solution, puts into thermal cracking gas chromatography GC-MS and measures, and as quantitative criterion material, extracts characteristic ion m/z210 and presses
Carry out quantitation according to external standard method, calculate the content of melmac in sample, content is in terms of melamine monomer；
Wherein, the parameter of thermal cracking gas chromatography GC-MS is:
(1) column length of gas chromatographic column is 30 meters, and column internal diameter is 0.25 millimeter, and thickness is 0.25 micron；
(2) gas chromatographic sample introduction mouth temperature is set as 300 DEG C, and temperature programming is 35 DEG C of initial temperature, is warmed up to 280 by 10 DEG C per minute
DEG C, retain 5 minutes；
(3) cracking instrument and gas chromatogram interface temperature are 280 DEG C, and pyrolysis time is 0.2 minute.
2. the method for claim 1 it is characterised in that: step 1) in, potassium hydroxide in potassium hydroxide methanol solution
Concentration is 1%-20%.
3. method as claimed in claim 2 is it is characterised in that step 2) in, the survey of thermal cracking gas chromatography GC-MS
Fixed condition is:
(1) gas chromatographic column adopts the hp-5ms post of low pole；
(2) mass spectrum collection is carried out using selection full scan mode simultaneously；
(3) the cracking tube temperature of thermal cracking is 600 degree.
4. method as claimed in claim 3 it is characterised in that: described melmac be carbamide condensation substance
Cross-linking agent, trimethylol melamine resin, hexamethylol melamine resin, polyhydroxy methyl etherified melamine resin or many
Melamine methylol derivant.
5. method as claimed in claim 4 it is characterised in that: described sample is textile, and it is fine that described textile includes plant
Dimension, animal fiber and synthetic fibers, described Plant fiber includes Cotton Gossypii, fiber crops, fruit fiber, described animal fiber include Pilus Caprae seu Oviss,
The rabbit hair, silkworm silk, described synthetic fibers include polyester fiber, viscose fiber, acetate fiber, chinlon, terylene, acrylon, spandex, dimension
Synthetic fibre, polypropylene, polyvinyl chloride fibre.
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| CN105651898A (en) * | 2016-03-29 | 2016-06-08 | 阿特斯(中国)投资有限公司 | Method for testing cross-linking agent content in EVA (ethylene vinyl acetate copolymer) film |
| CN107085047B (en) * | 2017-04-07 | 2019-10-29 | 浙江工业大学 | The analysis method of polyacrylic acid and its esters polymer in a kind of detection textile |
| CN109270175A (en) * | 2018-08-17 | 2019-01-25 | 安徽佳通乘用子午线轮胎有限公司 | Resin analyzes and identifies method in a kind of vulcanized rubber |
| CN112858537B (en) * | 2021-04-14 | 2023-09-05 | 上海市质量监督检验技术研究院 | Quick detection method for permethrin in anti-mosquito fabric |
| CN114460200B (en) * | 2022-02-09 | 2023-08-08 | 上海市质量监督检验技术研究院 | Method for identifying weight gain of silk floss methacrylamide grafted polymer |
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|---|---|---|---|---|
| US7267845B2 (en) * | 2000-12-22 | 2007-09-11 | Basf Corporation | Coating systems containing modified crosslinkers |
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| Pyrolysis and THM reactions of melamine and its resins;Manuela Leidl et al.;《J.Anal.Appl.Pyrolysis》;20041225;第74卷;第200页"Abstract"，第200页右栏末段至第202页右栏首段，表1，第203页第4节 * |
| 气相色谱质谱联用法检测牛奶中三聚氰胺的探讨;周德刚 等;《饲料研究》;20091231;第9卷;467-474页 * |
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