CN106770724A - A kind of method for determining phosphoguanidine content in textile and packing material - Google Patents
A kind of method for determining phosphoguanidine content in textile and packing material Download PDFInfo
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- CN106770724A CN106770724A CN201611070908.5A CN201611070908A CN106770724A CN 106770724 A CN106770724 A CN 106770724A CN 201611070908 A CN201611070908 A CN 201611070908A CN 106770724 A CN106770724 A CN 106770724A
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Abstract
The present invention relates to a kind of method for determining phosphoguanidine content in textile and packing material, comprise the following steps：1) sample pretreatment：By textile or packing material sample, 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 being well mixed, and seals standby；2) extraction of sample：Appropriate amount of sample is weighed, using methanol aqueous solution ultrasonic extraction；3) using liquid chromatography-mass spectrometry determination step 2) obtained by sample extraction solution in phosphoguanidine concentration；4) according to step 3) measured by sample extraction solution in phosphoguanidine concentration, calculate sample in phosphoguanidine content；Not only assay method is quick, simple for the present invention, and can realize the Accurate Determining of phosphoguanidine content in textile and packing material, and its minimum quantitative concentrations is 5mg/kg, is solved the problems, such as currently without detection fire retardant phosphoguanidine content method.
Description
[technical field]
It is specifically a kind of to determine phosphoguanidine in textile and packing material the invention belongs to technical field of analytical chemistry
The method of content.
[background technology]
The need in order to adapt to social safety production and life, fire preventing occurs, and protects people life property safety, resistance
Combustion science and technology is arisen at the historic moment.Fire retardant is application of the flame-retarded technology in actual production and life, and 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, when being attacked by extraneous burning things which may cause a fire disaster, can effectively prevent, delays or terminate flame transmission, so that
Reach fire-retardant effect.Conventional flame retardant with halogenated flame retardant as representative does not influence material materialization with its good flame retardation effect
Can be used widely.But, add the polymer of the halogen flame smoke amount in burning big, easily release poisonous and harmful gas
Body, easily causes secondary injury.With the continuous improvement that people's environmental protection and inherently safe are realized, the fire retardant of the world today
Study towards non-halogen BACN direction fast development.
Phosphoguanidine (guani dine phosphate) is low with good flame retardation effect as a kind of new nitrogenated flame retardant
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
Solely or it is used in mixed way in fiber post processing, it can also be used to which the inorganic agent of timber and paper, good with compatibility, it is excellent that hygroscopicity is small etc.
Good characteristic, it can also be used to polyactide compound it is fire-retardant.
Nitrogenous flame ratardant with phosphoguanidine as representative is developed rapidly in recent years due to meeting the trend of fire retardant.Though
Right phosphoguanidine is shown one's talent as a kind of new fire retardant, is widely used in the products such as textile and packing material, but by
Then a kind of new flame retardant products, secure data is also incomplete, and as fire retardant, a large amount of additions have in household articles
Certain security risk.External limitation requirement and content detection to phosphoguanidine in fire retardant treated product is also increasingly weighed
Depending on.
At present, the detection method of phosphoguanidine content in textile and packing material is there is no 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 not obviously applied to.Therefore, the detection method for setting up phosphoguanidine content in a textile and packing material is extremely urgent.
[content of the invention]
Phosphoric acid in a kind of measure textile and packing material is provided present invention aim to solve above-mentioned deficiency
The method of guanidine content, not only assay method is quick, simple, and can realize phosphoguanidine content in textile and packing material
Accurate Determining, solves the problems, such as currently without detection fire retardant phosphoguanidine content method.
A kind of method for determining phosphoguanidine content in textile and packing material is designed to achieve the above object, including it is following
Step：
1) sample pretreatment：By textile or packing material sample, 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 being well mixed, and seals standby；
2) extraction of sample：Appropriate amount of sample is weighed, using methanol-water solution ultrasonic extraction, is mixed, it is standby；
3) using LC/MS determination step 2) obtained by sample extraction solution in phosphoguanidine concentration；
4) according to step 3) measured by sample extraction solution in phosphoguanidine concentration, phosphoguanidine contains in calculating sample
Amount.
Preferably, step 2) in, sample is weighed in glass scre-cap bottle, it is 85 to add volume ratio：15 methanol-water is molten
Liquid, screws bottle cap after ultrasonic extraction 60min in 60 DEG C of water-baths, and the PTFE organic phase filter membranes that extract solution is through 0.45 μm are taken after cooling
Filter in boiling flask, done near in 70 DEG C of revolvings, then be 85 with volume ratio：15 methanol-water solution dissolved residue is simultaneously fixed
Hold, mix, so that liquid chromatograph-mass spectrometer is analyzed.
Preferably, step 3) in, the condition determination of liquid chromatograph-mass spectrometer is：
1) liquid-phase chromatographic column uses ZIC-cHILIC posts, and column length is 15cm, column internal diameter 2.1mm, 3 μm of particle diameter；
2) liquid chromatogram column temperature is set as 30 DEG C；
3) sample size is 10 μ L；
4) flow velocity is 0.3mL/min；
5) mobile phase：10mmol/L ammonium acetate solutions：Acetonitrile=45：55；
6) run time is 20min；
7) mass spectrometry parameters see the table below：
Preferably, step 3) in, compared with the retention time at standard items peak through sample peak, sample peak full scan mass spectrum
Whether figure compares with standard substance full scan mass spectrogram, to determine detect phosphoguanidine in sample.
Preferably, step 4) in, the content of phosphoguanidine in sample is obtained by the concentration conversion of phosphoguanidine in extraction solution,
According to solvent calibration curve, using quantified by external standard method, minimum quantitative concentrations are 5mg/kg.
The present invention is that one kind utilizes Solvent Extract methods, liquid chromatograph-mass spectrometer to determine textile compared with the existing technology
And in packing material phosphoguanidine method, not only assay method is quick, simple, and can realize textile and packing material
The Accurate Determining of phosphoguanidine content, its minimum quantitative concentrations are 5mg/kg, solve and contain currently without detection fire retardant phosphoguanidine
The problem of amount method, fully meets the requirement to phosphoguanidine content monitoring in textile and packing material, is worthy of popularization.
[brief description of the drawings]
Fig. 1 is using obtained by phosphoguanidine content in liquid chromatograph-mass spectrometer detection cotton swatch in the embodiment of the present invention 2
TIC chromatograms；
Fig. 2 is using going out peak position with phosphoguanidine 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 invention provides a kind of method for determining phosphoguanidine content in textile and packing material, its principle is：By sample
Phosphoguanidine in product extracts with methanol-water (85 ︰ 15) solution, then contained with phosphoguanidine in liquid chromatograph-mass spectrometer determination sample
Amount.Specifically include following steps：1) sample pretreatment：Sample is shredded with scissors, or is crushed with pulverizer, sample size size
2mm × 2mm × 2mm is must not exceed, after being well mixed, is fitted into the valve bag of clean dried, no sample should in the short time
Sealing preserve is standby；2) extraction of sample：0.3g samples are weighed in 40mL glass scre-caps bottle, 30mL methanol-waters (85 ︰ are added
15) solution, screws bottle cap after ultrasonic extraction 60min in 60 DEG C of water-baths, and 20mL extract solutions are taken after cooling to be had through 0.45 μm of PTFE
Machine phase membrane filtration is done in 70 DEG C of revolvings in 50mL boiling flasks near, and with methanol-water (85 ︰ 15), solution dissolved residue is simultaneously
1mL is settled to, is mixed, for liquid chromatograph-mass spectrometer analysis；3) using in LC/MS determination sample extraction solution
The concentration of phosphoguanidine；4) according to step 3) obtained by sample extraction solution in phosphoguanidine concentration, conversion obtain 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.
Further explained below is made to the present invention with reference to specific embodiment：
Embodiment 1：The measure of phosphoguanidine content in filling cotton
1. the preparation of sample solution：
Filling cotton is smashed with pulverizer, sample size size must not exceed 2mm × 2mm × 2mm, mixed, load clean
In dry valve bag, seal standby.0.3g samples are weighed in 40mL glass scre-caps bottle, 30mL methanol-waters (85 ︰ 15) is added
Solution, screws bottle cap and extracts 60min after 60 DEG C of water bath sonicators, and 20mL extract solutions are taken after cooling through 0.45 μm of PTFE organic phase
Membrane filtration is in 50mL boiling flasks.Solution is done in 70 DEG C of revolvings near in boiling flask, with methanol-water (85 ︰ 15) solution
Dissolved residue is simultaneously settled to 1mL, mixes, for LC-MS analysis.
2. instrument parameter is set：
1) liquid-phase chromatographic column uses ZIC-cHILIC posts, and specification is column length 15cm, column internal diameter 2.1mm, 3 μm of particle diameter；
2) liquid chromatogram column temperature is set as 30 DEG C；
3) sample size：10μL
4) flow velocity：0.3mL/min
5) mobile phase：10mmol/L acetic acid aqueous ammonium ︰ acetonitrile=45 ︰ 55
6) run time：20min
7) mass spectrometry parameters see the table below：
3. qualitative and quantitative
1) it is qualitative
Compared with the retention time at standard items peak through sample peak, sample peak full scan mass spectrogram and standard substance full scan
Whether mass spectrogram compares, and determines detect phosphoguanidine in sample.
2) it is quantitative
Using solvent standard 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.After testing, in the filling
Phosphoguanidine has not been detected in cotton sample product.
Embodiment 2：The measure of phosphoguanidine in cotton
1. the preparation of sample：
Cotton is shredded with scissors, sample size size must not exceed 2mm × 2mm × 2mm, mixed, load clean dried
Valve bag in, seal it is standby.0.3g samples are weighed in 40mL glass scre-caps bottle, adds 30mL methanol-waters (85 ︰ 15) molten
Liquid, screws bottle cap and extracts 60min after 60 DEG C of water bath sonicators, 20mL extract solutions is taken after cooling and is filtered through 0.45 μm of PTFE organic phase
Membrane filtration is in 50mL boiling flasks.Solution is dissolved in 70 DEG C of revolvings near dry with methanol-water (85 ︰ 15) solution in boiling flask
Residue is simultaneously settled to 1mL, mixes, for LC-MS analysis.
2. instrument parameter is set：
1) liquid-phase chromatographic column uses ZIC-cHILIC posts, and specification is column length 15cm, column internal diameter 2.1mm, 3 μm of particle diameter；
2) liquid chromatogram column temperature is set as 30 DEG C；
3) sample size：10μL
4) flow velocity：0.3mL/min
5) mobile phase：10mmol/L acetic acid aqueous ammonium ︰ acetonitrile=45 ︰ 55
6) run time：20min
7) mass spectrometry parameters see the table below：
3. qualitative and quantitative
1) it is qualitative
Compared with the retention time at standard items peak through sample peak, sample peak full scan mass spectrogram and standard substance full scan
Whether mass spectrogram compares, and determines detect phosphoguanidine in sample.
2) it is 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.
After testing, in the cotton swatch, the content of phosphoguanidine is 15.52mg/kg.As shown in Figures 1 and 2, to make
With phosphoguanidine content, the TIC chromatograms and mass spectrogram of gained in liquid chromatograph-mass spectrometer detection cotton swatch.
Embodiment 3：The measure of phosphoguanidine content in foam
1. the preparation of sample solution：
Foam is smashed with pulverizer, sample size size must not exceed 2mm × 2mm × 2mm, mixed, load clean dry
In dry valve bag, seal standby.0.3g samples are weighed in 40mL glass scre-caps bottle, adds 30mL methanol-waters (85 ︰ 15) molten
Liquid, screws bottle cap and extracts 60min after 60 DEG C of water bath sonicators, 20mL extract solutions is taken after cooling and is filtered through 0.45 μm of PTFE organic phase
Membrane filtration is in 50mL boiling flasks.Solution is done in 70 DEG C of revolvings near in boiling flask, molten with methanol-water (85 ︰ 15) solution
Solution residue is simultaneously settled to 1mL, mixes, for LC-MS analysis.
2. instrument parameter is set：
1) liquid-phase chromatographic column uses ZIC-cHILIC posts, and specification is column length 15cm, column internal diameter 2.1mm, 3 μm of particle diameter；
2) liquid chromatogram column temperature is set as 30 DEG C；
3) sample size：10μL
4) flow velocity：0.3mL/min
5) mobile phase：10mmol/L acetic acid aqueous ammonium ︰ acetonitrile=45 ︰ 55
6) run time：20min
7) mass spectrometry parameters see the table below：
3. qualitative and quantitative
1) it is qualitative
Compared with the retention time at standard items peak through sample peak, sample peak full scan mass spectrogram and standard substance full scan
Whether mass spectrogram compares, and determines detect phosphoguanidine in sample.
2) it is quantitative
Using solvent standard 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.After testing, the foam sample
Phosphoguanidine has not been detected in product.
The present invention is not limited by above-mentioned implementation method, other any without departing from Spirit Essence of the invention and principle
Lower made change, modification, replacement, combination, simplification, should be equivalent substitute mode, be included in protection model of the invention
Within enclosing.
Claims (5)
1. a kind of method for determining phosphoguanidine content in textile and packing material, it is characterised in that comprise the following steps：
1) sample pretreatment：By textile or packing material sample, shredded with scissors or crushed with pulverizer, sample size size
No more than 2 × 2 × 2mm, it is fitted into the valve bag of clean dried after being well mixed, seals standby；
2) extraction of sample：Appropriate amount of sample is weighed, using methanol-water solution ultrasonic extraction, is mixed, it is standby；
3) using LC/MS determination step 2) obtained by sample extraction solution in phosphoguanidine concentration；
4) according to step 3) measured by sample extraction solution in phosphoguanidine concentration, calculate sample in phosphoguanidine content.
2. the method for claim 1, it is characterised in that：Step 2) in, sample is weighed in glass scre-cap bottle, add body
Product is than being 85：15 methanol-water solution, screws bottle cap after ultrasonic extraction 60min in 60 DEG C of water-baths, and extract solution warp is taken after cooling
0.45 μm of PTFE organic phase filter membranes are filtered in boiling flask, are done near in 70 DEG C of revolvings, then are 85 with volume ratio：15 first
Alcohol-water solution dissolved residue and constant volume, mix, so that liquid chromatograph-mass spectrometer is analyzed.
3. the method for claim 1, it is characterised in that step 3) in, the condition determination of liquid chromatograph-mass spectrometer is：
1) liquid-phase chromatographic column uses ZIC-cHILIC posts, and column length is 15cm, column internal diameter 2.1mm, 3 μm of particle diameter；
2) liquid chromatogram column temperature is set as 30 DEG C；
3) sample size is 10 μ L；
4) flow velocity is 0.3mL/min；
5) mobile phase：10mmol/L ammonium acetate solutions：Acetonitrile=45：55；
6) run time is 20min；
7) mass spectrometry parameters see the table below：
4. the method for claim 1, it is characterised in that：Step 3) in, through sample peak and the retention time at standard items peak
Compare, sample peak full scan mass spectrogram compares with standard substance full scan mass spectrogram, to determine whether detect phosphorus in sample
Sour guanidine.
5. the method for claim 1, it is characterised in that：Step 4) in, 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109470802A (en) * | 2019-01-10 | 2019-03-15 | 通标标准技术服务(上海)有限公司 | A method of melamine phosphate content in measurement textile or foam |
| CN111157660A (en) * | 2020-02-28 | 2020-05-15 | 通标标准技术服务(上海)有限公司 | Method for measuring content of tetrahydroxy phosphorus chloride in textile or foam |
| CN112782316A (en) * | 2021-01-29 | 2021-05-11 | 京博农化科技有限公司 | Aminoformamidine hydrochloride content analysis method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109470802A (en) * | 2019-01-10 | 2019-03-15 | 通标标准技术服务(上海)有限公司 | A method of melamine phosphate content in measurement textile or foam |
| CN111157660A (en) * | 2020-02-28 | 2020-05-15 | 通标标准技术服务(上海)有限公司 | Method for measuring content of tetrahydroxy phosphorus chloride in textile or foam |
| 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 |
| CN112782316A (en) * | 2021-01-29 | 2021-05-11 | 京博农化科技有限公司 | Aminoformamidine hydrochloride content analysis method |
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