CN107064349B - A kind of method of polyamide 66 constituent content in measurement blending product - Google Patents
A kind of method of polyamide 66 constituent content in measurement blending product Download PDFInfo
- Publication number
- CN107064349B CN107064349B CN201710221558.6A CN201710221558A CN107064349B CN 107064349 B CN107064349 B CN 107064349B CN 201710221558 A CN201710221558 A CN 201710221558A CN 107064349 B CN107064349 B CN 107064349B
- Authority
- CN
- China
- Prior art keywords
- polyamide
- sample
- solution
- mass
- standard
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920002302 Nylon 6,6 Polymers 0.000 title claims abstract description 101
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000002156 mixing Methods 0.000 title claims abstract description 23
- 239000000470 constituent Substances 0.000 title claims abstract description 13
- 238000005259 measurement Methods 0.000 title claims abstract description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000000523 sample Substances 0.000 claims abstract description 50
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 48
- 235000019253 formic acid Nutrition 0.000 claims abstract description 48
- BGTOWKSIORTVQH-UHFFFAOYSA-N cyclopentanone Chemical compound O=C1CCCC1 BGTOWKSIORTVQH-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 32
- 239000012488 sample solution Substances 0.000 claims abstract description 22
- 239000012086 standard solution Substances 0.000 claims abstract description 16
- 238000005143 pyrolysis gas chromatography mass spectroscopy Methods 0.000 claims abstract description 8
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 6
- 238000005336 cracking Methods 0.000 claims description 14
- 238000013467 fragmentation Methods 0.000 claims description 13
- 238000006062 fragmentation reaction Methods 0.000 claims description 13
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000004445 quantitative analysis Methods 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 4
- 238000004949 mass spectrometry Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 238000003795 desorption Methods 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 238000005201 scrubbing Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000000197 pyrolysis Methods 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 description 27
- 229920000742 Cotton Polymers 0.000 description 18
- 239000000126 substance Substances 0.000 description 11
- 239000004952 Polyamide Substances 0.000 description 9
- 238000011978 dissolution method Methods 0.000 description 9
- 229920002647 polyamide Polymers 0.000 description 9
- 150000001412 amines Chemical class 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 8
- 238000002386 leaching Methods 0.000 description 8
- 210000002268 wool Anatomy 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- 238000003776 cleavage reaction Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000005194 fractionation Methods 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000007017 scission Effects 0.000 description 5
- 229920000728 polyester Polymers 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 229920000297 Rayon Polymers 0.000 description 2
- 229920002334 Spandex Polymers 0.000 description 2
- 229920004933 Terylene® Polymers 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 210000004209 hair Anatomy 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000004759 spandex Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- 241000254173 Coleoptera Species 0.000 description 1
- 229920000433 Lyocell Polymers 0.000 description 1
- 239000012494 Quartz wool Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention relates to a kind of methods of polyamide 66 constituent content in measurement blending product, comprising: 1) takes pure polyamide 66 standard items to be added in formic acid solution, standard solution group is made；2) it takes sample to be tested to be added in formic acid solution, sample solution is made；3) standard solution group and sample solution are injected into specimen cup respectively, are analyzed with pyrolysis-gas chromatography-mass spectrometry method, obtain pyrogram and mass spectrogram；4) Characteristic chromatographic peak compared in standard solution and sample solution pyrogram carries out qualitative analysis；5) using the mass concentration of the polyamide 66 of standard solution group as abscissa, the peak area of corresponding characteristic pyrolysis products cyclopentanone is that ordinate makes standard curve；6) mass concentration of polyamide 66 in sample solution is obtained according to standard curve, and calculates the mass percentage of polyamide 66 in sample to be tested.This method operating process is simple, time saving and energy saving, high sensitivity, small to testing crew health and surrounding environment influence.
Description
Technical field
The present invention relates to analysis detection fields, and in particular to a kind of side for measuring polyamide 66 constituent content in blending product
Method.
Background technique
The blended of difference composition accounts for very big a part in textile industry and trade.The fast qualitative of blended component and
The accurate quantitative analysis of blending rate is all highly important for trader and consumer and spinstry person.At present
Microscopic method, infra-red sepectrometry, thermal analysis system and chemical dissolution method etc. are mainly used to the qualitative, quantitative of blend fibre product,
Middle chemical dissolution method is the blending rate quantitative approach that GB/T 2910 national standard series is generallyd use.Chemical dissolution method is
The method being measured using solubility property of the various fibers in different chemical reagent, but this method it is cumbersome it is time-consuming,
Accuracy and data reappearance are low, and chemical reagent pollutes ambient enviroment and may hazard test person's health.
Fypro because with good elastic, wear-resisting, endurance and the performances such as corrosion-resistant due tos be usually used in cotton, fiber crops,
Other fiber blends such as silk, hair, terylene, spandex, viscose glue, are made various blending products.Polyamide 66 and polyamides currently on the market
Amine 6 is mainly used for spinning the polyamide of synthetic fibers, accounts for 98% or more of Fypro total amount.Standard GB/T/T
2910.7 define chemical dissolution method quantitative determination Fypro and other fibre blends, except the above statement the shortcomings that in addition to,
This method can only measure the total amount of polyamide component, but can not identify Nylon66 or daiamid-6 fiber.It is qualitative and
Quantitative analysis need to usually be completed using different method substeps.
Therefore, exploitation is established a kind of easy, quickly, polyamide 66 component and surely it in secured identification blended fabric
The detection technique method for measuring analysis is very necessary.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide polyamide 66 component in a kind of measurement blending product
The method of content, operating process is simple, time saving and energy saving, high sensitivity, dosage are few, to testing crew health and ambient enviroment
It influences small.
Technical solution provided by the present invention are as follows:
The method of polyamide 66 constituent content, includes the following steps: in a kind of measurement blending product
1) it the preparation of standard solution: takes pure polyamide 66 standard items to be added in formic acid solution, standard solution group is made；
2) it the preparation of sample solution: takes sample to be tested to be added in formic acid solution, sample solution is made；
3) standard solution group and sample solution: being injected into specimen cup by cracking analysis respectively, with pyrolysis gas chromatograph-matter
Spectrum combination method is analyzed, and pyrogram and mass spectrogram are obtained；
4) qualitative analysis: the Characteristic chromatographic peak compared in standard solution and sample solution pyrogram carries out qualitative point
Analysis；
5) standard curve making: using the mass concentration of the polyamide 66 of standard solution group as abscissa, corresponding feature is split
The peak area for solving product cyclopentanone is that ordinate makes standard curve；
6) quantitative analysis: the mass concentration of polyamide 66 in sample solution is obtained according to standard curve, and is calculated to test sample
The mass percentage of polyamide 66 in product.
In above-mentioned technical proposal, the cracking color that is generated under the conditions of cracking gas scrubbing due to polyamide 66 component
Spectrogram has its characteristic, can identify according to characteristic pyrolysis products cyclopentanone polyamide 66 component in blending product.Secondly,
Dissolve pretreated method using formic acid, eliminate the interference of other components, no matter percentage composition height can be to polyamides
The valid certainty of 66 component of amine.And polyamide 66 constituent content in blending product can be carried out according to the area of cyclopentanone characteristic peak
It is quantitative, i.e., using the mass concentration of the polyamide 66 of standard solution group as abscissa, cyclopentanone that corresponding polyamide 66 cracks out
It is that ordinate makes standard curve that feature, which splits peak area, and the quality for obtaining polyamide 66 in sample solution according to standard curve is dense
Degree, and the mass percentage of polyamide 66 in blended sample is calculated.Qualitative and quantitative analysis is using a kind of side of the present invention
Method can synchronously complete.
Preferably, the sample to be tested is Nylon66 and cotton, hair, silk, fiber crops, regenerated celulose fibre (such as viscose glue
Fiber, lyocell, Modal etc.) or other types chemical fibre (such as terylene, acrylic fibers, spandex) blending product.
Preferably, in the step 3) in pyrolysis-gas chromatography-mass spectrometry method, chromatographic condition are as follows: initial chromatographic column column
50~130 DEG C of temperature is warming up to 250~300 DEG C with the rate of 5~20 DEG C/min, keeps 5~10min；Injector temperature is 200
~300 DEG C, split ratio is 20~100:1；Mass Spectrometry Conditions: 15~650amu of mass number scanning range；Ion source temperature 230~
280 DEG C, 150~180 DEG C of quadrupole rod temperature, 250~300 DEG C of mass spectrometer interface temperature；Cracker condition: cracking furnace temperature 400~
850 DEG C, crack 200~300 DEG C of interface temperature.Under the conditions of the cracking gas scrubbing, polyamide 66 component in blending product
Characteristic pyrolysis products be mainly cyclopentanone and hexamethylene diamine and other amines, amides, olefines and nitriles substance, middle ring
Pentanone peak area accounts for about 40% or more, is relative intensity maximum peak.
Further, in the step 3) in pyrolysis-gas chromatography-mass spectrometry method: the preferred low-pole column of chromatographic column；Column temperature
It is preferred that 120 DEG C of initial temperature, the rate of preferably 20 DEG C/min is warming up to 260 DEG C, preferably remains 5min；Injector temperature is preferred
300 DEG C, split ratio 20:1；Mass Spectrometry Conditions: 230 DEG C of preferred ion source temperature, preferably 150 DEG C of quadrupole rod temperature, preferably mass spectrum
280 DEG C of interface temperature；Cracker condition: preferred 550 DEG C of furnace temperature of cracking preferably cracks 300 DEG C of interface temperature.
Preferably, the formula that the mass percentage of polyamide 66 in blending product is calculated in the step 6) is as follows:
Wherein, x is the mass percentage of polyamide 66 in sample to be tested, and m is the sampling quality of sample to be tested, and C is sample
The mass concentration of polyamide 66 in product solution；V is the volume of sample solution.
Preferably, the mass fraction of the formic acid solution is not less than 70%.Further preferably anhydrous formic acid.
Preferably, the processing of formic acid solution is removed in the step 3) before cracking analysis.
Preferably, the processing method of the removal formic acid solution includes: normal pressure drying, vacuum drying or online thermal desorption.
Preferably, pure polyamide 66 standard items are selected from pure Nylon66 in the step 1), pure polyamide 66 is sliced
Or pure polyamide 66 fabric.
Compared with the existing technology, the beneficial effects of the present invention are embodied in: measured using pyrolysis-gas chromatography-mass spectrometry method
The component of polyamide 66 and content simplicity are quick, sensitive reliable, high-efficient in blending product, and sample and reagent dosage are few, favorably
In experimental situation and human health.
Detailed description of the invention
Fig. 1 is the canonical plotting of Examples 1 to 6；
Fig. 2 is the cleavage map of polyamide 66 standard items formic acid solution；
Fig. 3 is the mass spectrogram of polyamide 66 standard items characteristic fragmentation peak cyclopentanone；
Fig. 4 is the cleavage map of the formic acid leaching liquor of 1 Nylon66 of embodiment and cotton fiber blended sample 1；
Fig. 5 is the cleavage map of the formic acid leaching liquor of 2 Nylon66 of embodiment and cotton fiber blended sample 2；
Fig. 6 is the cleavage map of the formic acid leaching liquor of 3 Nylon66 of embodiment and wool fibre blended sample 3；
Fig. 7 is the cleavage map of the formic acid leaching liquor of 4 Nylon66 of embodiment and polyester fiber blended sample 4；
Fig. 8 is the cracking of the formic acid leaching liquor of 5 Nylon66 of embodiment and cotton fiber and wool fibre blended sample 5
Figure.
Specific embodiment
The invention will be further described combined with specific embodiments below, but does not limit the protection scope of the patent application.
Embodiment 1
1. instrument and reagent
Gas chromatograph-mass spectrometer (GC-MS) model: Agilent 7890B-5977A (Agilent company, the U.S.)；Crack type
Number are as follows: PY-3030D double-click declines furnace cracker (Japanese Frontier Lab company)；Column model are as follows: HP-5ms quartz wool
Capillary column, 30m × 0.25mm × 0.25 μm (Agilent company, the U.S.).
Polyamide 66 standard items (slice), anhydrous formic acid (analysis is pure), Nylon66 and cotton fiber blended sample 1.
2. analyzing parameter
Chromatographic condition: injector temperature is 280 DEG C；Carrier gas is helium, flow 1.0mL/min, split ratio 20:1；Color
120 DEG C of column initial temperature of spectrum is warming up to 260 DEG C with 20 DEG C/min, keeps 5min.
Mass Spectrometry Conditions: 25~250amu of mass number scanning range；The source EI, ionizing energy 70eV, 230 DEG C of ion source temperature,
150 DEG C of quadrupole rod temperature, 280 DEG C of mass spectrometer interface temperature；Mensuration mode: SCAN, using Nist14 mass spectrum library searching.
Cracker condition: 550 DEG C of cracking temperature, pyrolysis time 30s, 300 DEG C of interface temperature are cracked.
3. standard curve
1.0g polyamide 66 standard items are accurately weighed, 100mL is dissolved and be settled to anhydrous formic acid, obtains 10.0mg/mL
Standard Stock solutions.The appropriate solution is pipetted respectively, is diluted with anhydrous formic acid and is prepared 0.5mg/mL, 1.0mg/mL, 2.0mg/
Then mL, 3.0mg/mL, 4.0mg/mL series standard solution are analyzed using above-mentioned 2 and take 2.0 μ L to carry out cracking color under Parameter Conditions
Spectrum-mass spectral analysis, using polyamide 66 mass concentration as abscissa, the cyclopentanone feature cracked out with polyamide 66 is split peak and (retained
Time is 3.28min) standard curve (see attached drawing Fig. 1) is drawn, linear regression obtains equation: A=1.854*107C+6.709*
105, coefficient R=0.9990.The pyrogram of polyamide 66 standard items formic acid solution is shown in attached drawing Fig. 2, polyamide 66 mark
The mass spectrogram of quasi- product characteristic fragmentation peak caprolactam is shown in attached drawing Fig. 3.
4. sample measures
10.0mg Nylon66 and cotton fiber blended sample 1 are accurately weighed, 10.0mL anhydrous formic acid, ultrasound leaching is added
30min is mentioned, takes the filtering of 2mL formic acid solution to get sample solution, then takes 2.0 μ L to inject specimen cup, with pyrolysis gas chromatograph-
Mass spectrometer is analyzed.
Attached drawing Fig. 4 is the formic acid solution pyrogram of Nylon66 and cotton fiber blended sample 1, wherein
3.30min chromatographic peak is the characteristic fragmentation peak (i.e. cyclopentanone) of Nylon66 component.According to characteristic fragmentation peak in chromatogram
Retention time (i.e. 3.30min) and assist mass spectrogram to Nylon66 carry out it is qualitative, further according to cyclopentanone chromatographic peak face
Product is obtained the concentration of polyamide 66 in formic acid solution using standard curve or regression equation, is then calculated in blended sample
The mass percentage of Nylon66 component is 41.2%.
As a comparison, chemical dissolution method as defined in GB/T 2910.7 measures polyamides in the blended sample according to national standards
The mass percentage of 66 fibre fractionation of amine is 40.0%.
Embodiment 2
1. instrument and reagent
In addition to Nylon66 and cotton fiber blended sample 2, the other the same as in Example 1.
2. analyzing parameter
With embodiment 1.
3. standard curve
With embodiment 1.
4. sample measures
5.0mg Nylon66 and cotton fiber blended sample 2 are accurately weighed, 10.0mL anhydrous formic acid, ultrasound leaching is added
60min is mentioned, takes the filtering of 2mL formic acid solution to get sample solution, then takes 2.0 μ L to inject specimen cup, with pyrolysis gas chromatograph-
Mass spectrometer is analyzed.
Attached drawing Fig. 5 is the formic acid solution pyrogram of Nylon66 and cotton fiber blended sample 2, wherein
3.30min chromatographic peak is the characteristic fragmentation peak (i.e. cyclopentanone) of Nylon66 component.According to characteristic fragmentation peak in chromatogram
Retention time (i.e. 3.30min) and assist mass spectrogram to Nylon66 carry out it is qualitative, further according to cyclopentanone chromatographic peak face
Product is obtained the concentration of polyamide 66 in formic acid solution using standard curve or regression equation, is then calculated in blended sample
The mass percentage of Nylon66 component is 84.7%.
As a comparison, chemical dissolution method as defined in GB/T 2910.7 measures polyamides in the blended sample according to national standards
The mass percentage of 66 fibre fractionation of amine is 85.7%.
Embodiment 3
1. instrument and reagent
In addition to 75% formic acid, Nylon66 and wool fibre blended sample 3, the other the same as in Example 1.
2. analyzing parameter
With embodiment 1.
3. standard curve
With embodiment 1.
4. sample measures
8.0mg Nylon66 and wool fibre blended sample 3 are accurately weighed, 75% formic acid 12.0mL, ultrasound leaching is added
45min is mentioned, takes the filtering of 2mL formic acid solution to get sample solution, 2.0 μ L is then taken to inject specimen cup, the thermal desorption at 140 DEG C
Except formic acid, analyzed with pyrolysis-gas chromatography-mass spectrometry instrument.
Attached drawing Fig. 6 is the formic acid solution pyrogram of Nylon66 and wool fibre blended sample 3, wherein
3.28min chromatographic peak is the characteristic fragmentation peak (i.e. cyclopentanone) of Nylon66 component.According to characteristic fragmentation peak in chromatogram
Retention time (i.e. 3.28min) and assist mass spectrogram to Nylon66 carry out it is qualitative, further according to cyclopentanone chromatographic peak face
Product is obtained the concentration of polyamide 66 in formic acid solution using standard curve or regression equation, is then calculated in blended sample
The mass percentage of Nylon66 component is 69.7%.
As a comparison, chemical dissolution method as defined in GB/T 2910.7 measures polyamides in the blended sample according to national standards
The mass percentage of 66 fibre fractionation of amine is 70.3%.
Embodiment 4
1. instrument and reagent
In addition to Nylon66 and polyester fiber blended sample 4, the other the same as in Example 1.
2. analyzing parameter
With embodiment 1.
3. standard curve
With embodiment 1.
4. sample measures
Nylon66 and polyester fiber blended sample 10.0mg are accurately weighed, anhydrous formic acid 10.0mL, ultrasound is added
30min is extracted, takes the filtering of 2mL formic acid solution to get sample solution, 2.0 μ L is then taken to inject specimen cup, the vacuum at 110 DEG C
Heating removes formic acid, is analyzed with pyrolysis-gas chromatography-mass spectrometry instrument.
Attached drawing Fig. 7 is the formic acid solution pyrogram of Nylon66 and polyester fiber blended sample, wherein
3.29min chromatographic peak is the characteristic fragmentation peak (i.e. cyclopentanone) of Nylon66 component.According to characteristic fragmentation peak in chromatogram
Retention time (i.e. 3.29min) and assist mass spectrogram to Nylon66 carry out it is qualitative, further according to cyclopentanone chromatographic peak face
Product is obtained the concentration of polyamide 66 in formic acid solution using standard curve or regression equation, is then calculated in blended sample
The mass percentage of Nylon66 component is 34.2%.
As a comparison, chemical dissolution method as defined in GB/T 2910.7 measures polyamides in the blended sample according to national standards
The mass percentage of 66 fibre fractionation of amine is 33.7%.
Embodiment 5
1. instrument and reagent
In addition to 80% formic acid, Nylon66 and cotton fiber and wool fibre blended sample 5, the other the same as in Example 1.
2. analyzing parameter
With embodiment 1.
3. standard curve
With embodiment 1.
4. sample measures
Nylon66 and cotton fiber and wool fibre blended sample 20.0mg are accurately weighed, 10.0mL is added without water beetle
Acid, ultrasound extraction 50min, takes the filtering of 2mL formic acid solution to get sample solution, then takes 2.0 μ L to inject specimen cup, at 135 DEG C
Lower heating removes formic acid, is analyzed using pyrolysis-gas chromatography-mass spectrometry instrument.
Attached drawing Fig. 8 is the formic acid solution pyrogram of Nylon66 and cotton fiber and wool fibre blended sample,
Middle 3.28min chromatographic peak is the characteristic fragmentation peak (i.e. cyclopentanone) of Nylon66 component.According to characteristic fragmentation in chromatogram
The retention time (i.e. 3.28min) at peak simultaneously assists mass spectrogram qualitative to Nylon66 progress, further according to cyclopentanone chromatographic peak
Area is obtained the concentration of polyamide 66 in formic acid solution using standard curve or regression equation, blended sample is then calculated
The mass percentage of middle Nylon66 component is 20.1%.
As a comparison, chemical dissolution method as defined in GB/T 2910.7 measures polyamides in the blended sample according to national standards
The mass percentage of 66 fibre fractionation of amine is 19.5%.
Claims (7)
1. a kind of method of polyamide 66 constituent content in measurement blending product, which comprises the steps of:
1) it the preparation of standard solution: takes pure polyamide 66 standard items to be added in formic acid solution, standard solution group is made；
2) it the preparation of sample solution: takes sample to be tested to be added in formic acid solution, sample solution is made；
3) cracking analysis: standard solution group and sample solution are injected into specimen cup respectively, joined with cracking gas scrubbing
Usage is analyzed, and pyrogram and mass spectrogram are obtained；
In the step 3) in pyrolysis-gas chromatography-mass spectrometry method, chromatographic condition are as follows: initial 50~130 DEG C of column temperature of chromatographic column,
250~300 DEG C are warming up to the rate of 5~20 DEG C/min, keeps 5~10min；Injector temperature is 200~300 DEG C, is shunted
Than for 20~100:1；
Mass Spectrometry Conditions: 15~650amu of mass number scanning range；230~280 DEG C of ion source temperature, quadrupole rod temperature 150~180
DEG C, 250~300 DEG C of mass spectrometer interface temperature；
Cracker condition: 400~850 DEG C of furnace temperature of cracking cracks 200~300 DEG C of interface temperature；
4) qualitative analysis: the Characteristic chromatographic peak compared in standard solution and sample solution pyrogram carries out qualitative analysis；
5) standard curve making: using the mass concentration of the polyamide 66 of standard solution group as abscissa, corresponding characteristic fragmentation is produced
The peak area of object cyclopentanone is that ordinate makes standard curve；
6) quantitative analysis: the mass concentration of polyamide 66 in sample solution is obtained according to standard curve, and is calculated in sample to be tested
The mass percentage of polyamide 66.
2. the method for polyamide 66 constituent content in measurement blending product according to claim 1, which is characterized in that described
The formula that the mass percentage of polyamide 66 in blending product is calculated in step 6) is as follows:
Wherein, x is the mass percentage of polyamide 66 in sample to be tested, and m is the sampling quality of sample to be tested, and C is that sample is molten
The mass concentration of polyamide 66 in liquid, V are the volume of sample solution.
3. the method for polyamide 66 constituent content in measurement blending product according to claim 1, which is characterized in that described
The mass fraction of formic acid solution is not less than 70%.
4. the method for polyamide 66 constituent content in measurement blending product according to claim 1, which is characterized in that described
The processing of formic acid solution is removed in step 3) before cracking analysis.
5. the method for polyamide 66 constituent content in measurement blending product according to claim 4, which is characterized in that described
The processing method of removal formic acid solution includes: normal pressure drying, vacuum drying or online thermal desorption.
6. the method for polyamide 66 constituent content in measurement blending product according to claim 1, which is characterized in that described
Pure polyamide 66 standard items are selected from pure Nylon66 in step 1).
7. the method for polyamide 66 constituent content in measurement blending product according to claim 1, which is characterized in that described
Pure polyamide 66 standard items are selected from pure polyamide 66 slice or pure polyamide 66 fabric in step 1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710221558.6A CN107064349B (en) | 2017-04-06 | 2017-04-06 | A kind of method of polyamide 66 constituent content in measurement blending product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710221558.6A CN107064349B (en) | 2017-04-06 | 2017-04-06 | A kind of method of polyamide 66 constituent content in measurement blending product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107064349A CN107064349A (en) | 2017-08-18 |
| CN107064349B true CN107064349B (en) | 2019-08-30 |
Family
ID=59602942
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710221558.6A Active CN107064349B (en) | 2017-04-06 | 2017-04-06 | A kind of method of polyamide 66 constituent content in measurement blending product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107064349B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117233272A (en) * | 2020-04-10 | 2023-12-15 | 宁波海关技术中心 | Method for quantitative analysis of full-range proportion of PA66/PA6 blend |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091415A (en) * | 2012-12-30 | 2013-05-08 | 浙江工业大学 | Method for determining blending components and content in bi-component blending fabric containing dacron |
-
2017
- 2017-04-06 CN CN201710221558.6A patent/CN107064349B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091415A (en) * | 2012-12-30 | 2013-05-08 | 浙江工业大学 | Method for determining blending components and content in bi-component blending fabric containing dacron |
Non-Patent Citations (6)
| Title |
|---|
| IDENTIFICATION OF SELECTED FIBERS BY PYROLYSIS-GAS CHROMATOGRAPHY-MASS SPECTROMETRY;Rosa Linda Riel-Bagalawis;《TECHNICAL REPORT》;20040419;第1-33页 |
| 石英砂固体分散剂制样的裂解气相色谱法测定涤/毛纤维混纺比列;胡晓燕 等;《分析化学》;20140228;第42卷(第2期);第288-292页 |
| 红外光谱和热裂解气相色谱质谱联用技术鉴别芳香族聚酯纤维;刘文莉 等;《中国纤维》;20100331;第59-61页 |
| 聚乙烯尼龙共混物的PGC-MS和FT-IR联用鉴别;王忠友 等;《分析测试学报》;20040331;第23卷(第2期);第92-94页 |
| 聚酰胺的裂解色谱分析;刘尔嘉 等;《北京化纤工学院学报》;19851231(第2期);第64-73页 |
| 裂解气相色谱法对纯纤和混纤的定性研究;尹桂珍 等;《大众标准化》;20011231(第3期);第31-32页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107064349A (en) | 2017-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101393183B (en) | Method for measuring pesticide residue of six kinds of dinitroaniline in tobacco and tobacco products | |
| CN104316634B (en) | The measuring method of volatile organic acids in a kind of cigarette mainstream flue gas | |
| CN107085046A (en) | The authentication method of polyamide 6 or polyamide 66 in a kind of blending product | |
| CN101943686B (en) | Method for detecting polydimethylsiloxane | |
| CN106706794B (en) | A kind of method of main tongue fur faint scent characteristic chicken flavor substance in quantitative analysis ramuscule cigarette mainstream flue gas | |
| CN102128906A (en) | Method for detecting volatile organic compound in cigarette filter | |
| CN107102073B (en) | A kind of method of polyamide 6 constituent content in measurement blending product | |
| CN105572241B (en) | The method for determining amphetamine in blood and urine, ketamine, pethidine and methadone | |
| CN109406690B (en) | Method for detecting related substances in chloral hydrate | |
| CN105974007A (en) | Method for detecting phthalic acid ester in soil | |
| CN101603952B (en) | Method for determining content of formaldehyde in water-based adhesive for cigarettes | |
| CN107561182A (en) | Volatility and the detection method of semi-volatile organic compounds in cigarette mainstream flue gas | |
| CN108387663B (en) | Method for detecting content of phthalic anhydride in toy by using gas chromatography-mass spectrometry | |
| CN108169385A (en) | A kind of method using six kinds of glucides in ultra performance liquid chromatography concatenation QDa simultaneously quick detection health liquor | |
| CN107064349B (en) | A kind of method of polyamide 66 constituent content in measurement blending product | |
| CN105319296A (en) | Measuring method for methyl alcohol content | |
| CN101393180B (en) | Method for measuring beta-naphthol content in additive agent for cigarette | |
| CN102507773B (en) | Method for selectively determining residual vinyl acetate in white latex for cigarette through static headspace gas and chromatography mass spectrometry | |
| CN105606435A (en) | Pretreatment method for measuring content of mercury in soil and detection method using same | |
| CN109507354B (en) | Method for determining content of K powder in human hair by flash evaporation-gas chromatography-mass spectrometry | |
| CN102519955B (en) | Measuring method for gun shooting time | |
| CN103115881A (en) | Method for evaluating and reducing uncertainty value of potassium in iron ore | |
| CN108956835B (en) | Fingerprint detection method of oral medicine for clearing heat from throat | |
| CN113759037B (en) | Characteristic spectrum of formula granules of semen lepidii and/or semen lepidii as well as construction method and identification method thereof | |
| CN102106888A (en) | Quality control method for extraction process of Chinese medicine ainsliaea fragrans champ |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20211209 Address after: 314503 Wutong Street development avenue, 1488, Zhejiang, Jiaxing, Tongxiang, 1 and 1, South and 3 floors South and 4 floor south, Patentee after: Zhejiang University of science and technology Tongxiang Research Institute Co.,Ltd. Address before: 310018 No. 2 street, Baiyang street, Hangzhou economic and Technological Development Zone, Zhejiang 928 Patentee before: ZHEJIANG SCI-TECH University |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20220915 Address after: Room 601, 6th Floor, No. 1488, Development Avenue, Wutong Street, Tongxiang City, Jiaxing City, Zhejiang Province, 314500 Patentee after: Zhejiang Li (Zhejiang) Testing Technology Co.,Ltd. Address before: 314503 Wutong Street development avenue, 1488, Zhejiang, Jiaxing, Tongxiang, 1 and 1, South and 3 floors South and 4 floor south, Patentee before: Zhejiang University of science and technology Tongxiang Research Institute Co.,Ltd. |