CN106770724B - A method of phosphoguanidine content in measurement textile and packing material - Google Patents
A method of phosphoguanidine content in measurement textile and packing material Download PDFInfo
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Abstract
The present invention relates to a kind of methods of phosphoguanidine content in measurement textile and packing material, the following steps are included: 1) sample pretreatment: by textile or packing material sample, it is shredded with scissors or is crushed with pulverizer, sample size is no more than 2 × 2 × 2mm, it is fitted into the valve bag of clean dried, seals spare after mixing；2) extraction of sample: weighing appropriate amount of sample, using methanol-water solution ultrasonic extraction；3) liquid chromatography-mass spectrometry determination step 2 is used) concentration of phosphoguanidine in resulting sample extraction solution；4) in the sample extraction solution according to measured by step 3) phosphoguanidine concentration, calculate sample in phosphoguanidine content；Not only measuring method is quick, simple by the present invention, but also can be realized the Accurate Determining of phosphoguanidine content in textile and packing material, and minimum quantitative concentrations are 5mg/kg, are solved the problems, such as currently without detection fire retardant phosphoguanidine content method.
Description
[technical field]
The invention belongs to technical field of analytical chemistry, phosphoguanidine in specifically a kind of measurement textile and packing material
The method of content.
[background technique]
In order to adapt to the needs of social safety production and life, fire preventing occurs, and protects people life property safety, resistance
Combustion science and technology is come into being.Fire retardant is application of the flame-retarded technology in actual production and life, it is a kind of for improving
The special auxiliary chemicals of flammable combustible material combustibility, are widely used in the fire-retardant processing of various types of materials.By fire-retardant
Material after agent processing can effectively prevent, delay or terminate flame transmission when being attacked by extraneous fire source, thus
Have the function that fire-retardant.It is the conventional flame retardant of representative with its good flame retardation effect using halogenated flame retardant, does not influence material materialization
It can be used widely.But it is big to be added the polymer of the halogen flame smoke amount in burning, easily releases poisonous and harmful gas
Body be easy to cause secondary injury.With the continuous improvement that people's environmental protection and inherently safe are realized, the fire retardant of the world today
It studies and is grown rapidly towards non-halogen new flame retardant direction.
Phosphoguanidine (guani dine phosphate) is used as a kind of novel nitrogenated flame retardant, has good flame retardation effect, low
The few cigarette of poison, lower-price characteristic, and show excellent application effect.Phosphoguanidine is widely used as fire-retardant processing aid, can be single
It solely or is used in mixed way and is post-processed in fiber, it can also be used to which the inorganic agent of timber and paper has compatibility good, and it is excellent that hygroscopicity is small etc.
Good characteristic, it can also be used to polyactide compound it is fire-retardant.
The trend for being the nitrogenous flame ratardant of representative due to meeting fire retardant using phosphoguanidine, develops rapidly in recent years.Though
Right phosphoguanidine is shown one's talent as a kind of novel fire retardant, is widely used in the products such as textile and packing material, but by
Then a kind of novel flame retardant products, secure data is also incomplete, and as fire retardant, largely addition has in household items
Certain security risk.Foreign countries are also increasingly heavier to the limitation requirement and content detection of phosphoguanidine in fire retardant treated product
Depending on.
Currently, there is no the detection method of phosphoguanidine content in textile and packing material both at home and abroad.Phosphoguanidine have compared with
Big polarity, there is good dissolubility in water, almost insoluble in toluene, acetone and other organic solvent, conventional fire retardant inspection
Survey method is obviously not suitable for.Therefore, the detection method for establishing phosphoguanidine content in a textile and packing material is extremely urgent.
[summary of the invention]
Phosphoric acid in a kind of measurement textile and packing material is provided present invention aim to solve above-mentioned deficiency
The method of guanidine content, not only measuring method is quick, simple, but also can be realized phosphoguanidine content in textile and packing material
Accurate Determining is solved the problems, such as currently without detection fire retardant phosphoguanidine content method.
A kind of method for measuring phosphoguanidine content in textile and packing material is designed to achieve the above object, including following
Step:
1) sample pretreatment: by textile or packing material sample, being shredded with scissors or crushed with pulverizer, sample size
Size is no more than 2 × 2 × 2mm, is fitted into the valve bag of clean dried after mixing, seals spare；
2) extraction of sample: weighing appropriate amount of sample, using methanol-water solution ultrasonic extraction, mixes, spare；
3) liquid chromatography-mass spectrometry determination step 2 is used) concentration of phosphoguanidine in resulting sample extraction solution；
4) in the sample extraction solution according to measured by step 3) phosphoguanidine concentration, calculate phosphoguanidine in sample and contain
Amount.
Preferably, weighing sample in glass scre-cap bottle in step 2), it is molten that the methanol-water that volume ratio is 85:15 is added
Liquid screws after bottle cap the ultrasonic extraction 60min in 60 DEG C of water-baths, takes extracting solution through 0.45 μm of PTFE organic phase filter membrane after cooling
It filters in boiling flask, is steamed near dry in 70 DEG C of rotations, then with the volume ratio methanol-water solution dissolved residue that is 85:15 and fixed
Hold, mix, for liquid chromatograph-mass spectrometer analysis.
Preferably, in step 3), the determination condition of liquid chromatograph-mass spectrometer are as follows:
1) liquid-phase chromatographic column use ZIC-cHILIC column, column length 15cm, column internal diameter 2.1mm, 3 μm of partial size；
2) liquid chromatogram column temperature is set as 30 DEG C；
3) sample volume is 10 μ L；
4) flow velocity is 0.3mL/min；
5) mobile phase: 10mmol/L ammonium acetate solution: acetonitrile=45:55；
6) runing time is 20min；
7) mass spectrometry parameters see the table below:
Preferably, compare through sample peak with the retention time at standard items peak in step 3), sample peak full scan mass spectrum
Figure compares with standard substance full scan mass spectrogram, to determine in sample whether detect phosphoguanidine.
Preferably, the content of phosphoguanidine in sample is obtained by the concentration conversion of phosphoguanidine in extraction solution in step 4),
According to solvent calibration curve, using quantified by external standard method, minimum quantitative concentrations are 5mg/kg.
The present invention is a kind of using organic solvent extraction, liquid chromatograph-mass spectrometer measures textile compared with the existing technology
And in packing material phosphoguanidine method, not only measuring method quickly, it is simple, but also can be realized in textile and packing material
The Accurate Determining of phosphoguanidine content, minimum quantitative concentrations are 5mg/kg, solve and contain currently without detection fire retardant phosphoguanidine
The problem of amount method, fully meets the requirement monitored to phosphoguanidine content in textile and packing material, is worthy of popularization.
[Detailed description of the invention]
Fig. 1 is resulting using phosphoguanidine content in liquid chromatograph-mass spectrometer detection cotton swatch in the embodiment of the present invention 2
TIC chromatogram；
Fig. 2 is to go out peak position with phosphoguanidine using in liquid chromatograph-mass spectrometer detection cotton swatch in the embodiment of the present invention 2
The mass spectrogram of identical chromatographic peak.
[specific embodiment]
The present invention provides a kind of method of phosphoguanidine content in measurement textile and packing material, principles are as follows: by sample
Phosphoguanidine in product is extracted with methanol-water (85 ︰ 15) solution, then is contained with phosphoguanidine in liquid chromatograph-mass spectrometer measurement sample
Amount.Specifically includes the following steps: 1) sample pretreatment: sample is shredded with scissors, or is crushed with pulverizer, sample size
It must not exceed 2mm × 2mm × 2mm, after mixing, be fitted into the valve bag of clean dried, unused sample is answered in the short time
It is sealed spare；2) extraction of sample: weighing 0.3g sample in 40mL glass scre-cap bottle, and 30mL methanol-water (85 ︰ are added
15) solution screws after bottle cap the ultrasonic extraction 60min in 60 DEG C of water-baths, takes 20mL extracting solution to have through 0.45 μm of PTFE after cooling
Machine phase membrane filtration is steamed near dry in 50mL boiling flask in 70 DEG C of rotations, and with methanol-water (85 ︰ 15), solution dissolved residue is simultaneously
It is settled to 1mL, is mixed, is analyzed for liquid chromatograph-mass spectrometer；3) using in liquid chromatography-mass spectrometry measurement sample extraction solution
The concentration of phosphoguanidine；4) according to the concentration of phosphoguanidine in the resulting sample extraction solution of step 3), conversion obtains phosphoric acid in sample
The content of guanidine, according to solvent calibration curve, using quantified by external standard method, minimum quantitative concentrations are 5mg/kg.
The present invention is made combined with specific embodiments below further explained below:
Embodiment 1: the measurement of phosphoguanidine content in filling cotton
1. the preparation of sample solution:
Filling cotton is smashed with pulverizer, sample size must not exceed 2mm × 2mm × 2mm, mix, and be packed into clean
In dry valve bag, seal spare.0.3g sample is weighed in 40mL glass scre-cap bottle, is added 30mL methanol-water (85 ︰ 15)
Solution screws and extracts 60min in 60 DEG C of water bath sonicators after bottle cap, takes 20mL extracting solution through 0.45 μm of PTFE organic phase after cooling
Membrane filtration is in 50mL boiling flask.Solution is steamed near dry in 70 DEG C of rotations in boiling flask, with methanol-water (85 ︰ 15) solution
Dissolved residue is simultaneously settled to 1mL, mixes, for LC-MS analysis.
2. setting instrument parameter:
1) liquid-phase chromatographic column use ZIC-cHILIC column, specification be column length 15cm, column internal diameter 2.1mm, 3 μm of partial size；
2) liquid chromatogram column temperature is set as 30 DEG C；
3) sample volume: 10 μ L
4) flow velocity: 0.3mL/min
5) mobile phase: 10mmol/L acetic acid aqueous ammonium ︰ acetonitrile=45 ︰ 55
6) runing time: 20min
7) mass spectrometry parameters see the table below:
3. qualitative and quantitative
1) qualitative
It compares through sample peak with the retention time at standard items peak, sample peak full scan mass spectrogram and standard substance full scan
Mass spectrogram compares, and determines in sample whether detect phosphoguanidine.
2) quantitative
Using solvent standard calibration curve quantified by external standard method.
4. calculating
According to the concentration of phosphoguanidine in sample extraction solution, the content of phosphoguanidine in sample is calculated.Through detecting, in the filling
Phosphoguanidine has been not detected in cotton sample product.
Embodiment 2: the measurement of phosphoguanidine in cotton
1. the preparation of sample:
Cotton is shredded with scissors, sample size must not exceed 2mm × 2mm × 2mm, mix, and be packed into clean dried
Valve bag in, seal it is spare.0.3g sample is weighed in 40mL glass scre-cap bottle, it is molten that 30mL methanol-water (85 ︰ 15) is added
Liquid screws and extracts 60min in 60 DEG C of water bath sonicators after bottle cap, takes 20mL extracting solution to filter through 0.45 μm of PTFE organic phase after cooling
Membrane filtration is in 50mL boiling flask.Solution is steamed near dry in 70 DEG C of rotations in boiling flask, is dissolved with methanol-water (85 ︰ 15) solution
Residue is simultaneously settled to 1mL, mixes, for LC-MS analysis.
2. setting instrument parameter:
1) liquid-phase chromatographic column use ZIC-cHILIC column, specification be column length 15cm, column internal diameter 2.1mm, 3 μm of partial size；
2) liquid chromatogram column temperature is set as 30 DEG C；
3) sample volume: 10 μ L
4) flow velocity: 0.3mL/min
5) mobile phase: 10mmol/L acetic acid aqueous ammonium ︰ acetonitrile=45 ︰ 55
6) runing time: 20min
7) mass spectrometry parameters see the table below:
3. qualitative and quantitative
1) qualitative
It compares through sample peak with the retention time at standard items peak, sample peak full scan mass spectrogram and standard substance full scan
Mass spectrogram compares, and determines in sample whether detect phosphoguanidine.
2) quantitative
Using solvent calibration curve quantified by external standard method
4 calculate
According to the concentration of phosphoguanidine in sample extraction solution, the content of phosphoguanidine in sample is calculated.
Through detecting, in the cotton swatch, the content of phosphoguanidine is 15.52mg/kg.As shown in Figure 1 and Figure 2, to make
With phosphoguanidine content, resulting TIC chromatogram and mass spectrogram in liquid chromatograph-mass spectrometer detection cotton swatch.
Embodiment 3: the measurement of phosphoguanidine content in foam
1. the preparation of sample solution:
Foam is smashed with pulverizer, sample size must not exceed 2mm × 2mm × 2mm, mix, and be packed into clean dry
In dry valve bag, seal spare.0.3g sample is weighed in 40mL glass scre-cap bottle, it is molten that 30mL methanol-water (85 ︰ 15) is added
Liquid screws and extracts 60min in 60 DEG C of water bath sonicators after bottle cap, takes 20mL extracting solution to filter through 0.45 μm of PTFE organic phase after cooling
Film filters in 50mL boiling flask.Solution is steamed near dry in 70 DEG C of rotations in boiling flask, molten with methanol-water (85 ︰ 15) solution
Solution residue is simultaneously settled to 1mL, mixes, for LC-MS analysis.
2. setting instrument parameter:
1) liquid-phase chromatographic column use ZIC-cHILIC column, specification be column length 15cm, column internal diameter 2.1mm, 3 μm of partial size；
2) liquid chromatogram column temperature is set as 30 DEG C；
3) sample volume: 10 μ L
4) flow velocity: 0.3mL/min
5) mobile phase: 10mmol/L acetic acid aqueous ammonium ︰ acetonitrile=45 ︰ 55
6) runing time: 20min
7) mass spectrometry parameters see the table below:
3. qualitative and quantitative
1) qualitative
It compares through sample peak with the retention time at standard items peak, sample peak full scan mass spectrogram and standard substance full scan
Mass spectrogram compares, and determines in sample whether detect phosphoguanidine.
2) quantitative
Using solvent standard calibration curve quantified by external standard method.
4. calculating
According to the concentration of phosphoguanidine in sample extraction solution, the content of phosphoguanidine in sample is calculated.Through detecting, the foam sample
Phosphoguanidine has been not detected in product.
The present invention is simultaneously not limited to the embodiments described above, other any without departing from spiritual essence and principle of the invention
Changes, modifications, substitutions, combinations, simplifications made by lower, should be equivalent substitute mode, are included in protection model of the invention
Within enclosing.
Claims (4)
1. a kind of method of phosphoguanidine content in measurement textile and its packing material, which comprises the following steps:
1) sample pretreatment: by textile or packing material sample, being shredded with scissors or crushed with pulverizer, sample size
It no more than 2 × 2 × 2mm, is fitted into the valve bag of clean dried, seals spare after mixing；
2) extraction of sample: weighing appropriate amount of sample, using methanol-water solution ultrasonic extraction, mixes, spare；
3) liquid chromatography-mass spectrometry determination step 2 is used) concentration of phosphoguanidine in resulting sample extraction solution；
In step 3), the determination condition of liquid chromatograph-mass spectrometer are as follows:
1. liquid-phase chromatographic column use ZIC-cHILIC column, column length 15cm, column internal diameter 2.1mm, 3 μm of partial size；
2. liquid chromatogram column temperature is set as 30 DEG C；
3. sample volume is 10 μ L；
4. flow velocity is 0.3mL/min；
5. mobile phase: 10mmol/L ammonium acetate solution: acetonitrile=45:55；
6. runing time is 20min；
7. mass spectrometry parameters see the table below:
4) in the sample extraction solution according to measured by step 3) phosphoguanidine concentration, calculate sample in phosphoguanidine content.
2. the method as described in claim 1, it is characterised in that: in step 2), weigh sample in glass scre-cap bottle, body is added
Product screws after bottle cap the ultrasonic extraction 60min in 60 DEG C of water-baths, takes extracting solution to pass through after cooling than the methanol-water solution for being 85:15
0.45 μm of PTFE organic phase filter membrane filters in boiling flask, is steamed near dry in 70 DEG C of rotations, then the first for being 85:15 with volume ratio
Alcohol-water solution dissolved residue and constant volume mix, for liquid chromatograph-mass spectrometer analysis.
3. the method as described in claim 1, it is characterised in that: in step 3), the retention time through sample peak and standard items peak
It compares, sample peak full scan mass spectrogram compares with standard substance full scan mass spectrogram, to determine in sample whether detect phosphorus
Sour guanidine.
4. the method as described in claim 1, it is characterised in that: in step 4), by the concentration conversion of phosphoguanidine in extraction solution
The content of phosphoguanidine in sample is obtained, according to solvent calibration curve, using quantified by external standard method, minimum quantitative concentrations are 5mg/kg.
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| CN111157660B (en) * | 2020-02-28 | 2022-06-21 | 通标标准技术服务(上海)有限公司 | Method for measuring content of tetrakis (hydroxymethyl) phosphonium chloride in textile or foam |
| CN112782316B (en) * | 2021-01-29 | 2023-06-30 | 山东京博农化科技股份有限公司 | Method for analyzing content of amitraz hydrochloride |
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| CN102628843B (en) * | 2012-03-14 | 2014-09-17 | 浙江出入境检验检疫局检验检疫技术中心 | Gas chromatography for detection of phosphate fire-retardant plasticizer in textile |
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