CN109470802A - A method of melamine phosphate content in measurement textile or foam - Google Patents
A method of melamine phosphate content in measurement textile or foam Download PDFInfo
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- CN109470802A CN109470802A CN201910023215.8A CN201910023215A CN109470802A CN 109470802 A CN109470802 A CN 109470802A CN 201910023215 A CN201910023215 A CN 201910023215A CN 109470802 A CN109470802 A CN 109470802A
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- 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
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
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Abstract
The present invention provides a kind of methods of melamine phosphate content in measurement textile or foam, the following steps are included: 1) sample pretreatment: textile samples are shredded with scissors, or foam sample is crushed with pulverizer, so that textile or foam sample size are no more than 2mm × 2mm × 2mm, smashed sample is uniformly mixed again, it is fitted into the valve bag of clean dried, is sealed, it is spare；2) extraction of sample: weighing appropriate amount of sample, with the aqueous hydrochloric acid solution ultrasonic extraction of 1mol/L；3) using the concentration of melamine phosphate in High Performance Liquid Chromatography/Mass Spectrometry LC-MS method measurement sample extraction solution；4) according to the concentration of MP in sample extraction solution, the content of melamine phosphate in sample is calculated；The present invention not only measuring method quickly, it is simple, but also can be realized textile, in foam melamine phosphate content Accurate Determining, solve the problems, such as not detect fire retardant melamine phosphate content method.
Description
[technical field]
The invention belongs to technical field of analytical chemistry, phosphoric acid melamine in specifically a kind of measurement textile or foam
The method of amine (hereinafter referred to as MP) content.
[background technique]
Fire retardant is that consumption figure is only second to plasticizer and occupies in the processing aid of the second major class in plastic additive, it is
It is a kind of for improving the special auxiliary chemicals of flammable combustible material combustibility, be widely used in the fire-retardant processing of various types of materials
In.Fire retardant is broadly divided into halogen system, phosphorus system, nitrogen system, phosphorus nitrogen system inorganic fire retardants.Material after fire retardant is processed, by
To when the attack of extraneous fire source, flame transmission can be effectively prevented, delays or terminate, to have the function that fire-retardant.
Inorganic fire retardants due to can fire-retardant, suppression cigarette, it is inexpensive the features such as, occupy biggish specific gravity in fire retardant, but add
Amount needs greatly, to be affected to the mechanical performance of fire proofing, be restricted using field.Using halogenated flame retardant as the biography of representative
Fire retardant unite with its good flame retardation effect, does not influence material physical and chemical performance and is used widely, still, the poly- of halogen flame is added
It is big to close object smoke amount in burning, easily releasing toxic and harmful gas, be easy to cause secondary injury, there are carcinogenic dangers, in recent years
By the pressure from environmental protection etc., many European Union member countries start to limit and do not use bromide fire retardant halogen flame, and
Try hard to promote the non-halogen process of fire retardant.In order to adapt to the needs of social safety production and life, fire preventing occurs, protection
People's lives and properties, fire-retardant science and technology are come into being.
A kind of novel phosphor nitrogen flame retardant that melamine phosphate exactly came into being in recent years has low cigarette, low toxicity, phase
Capacitive is good, coking coking when being heated and heat-insulated, oxygen barrier feature, therefore can be effectively fire-retardant and prevent from dripping, and prevents flame
It propagates and stretches.
As halogen-free flame retardants is developed rapidly in recent years, MP shows one's talent as one such new flame retardant,
Also largely it is used in fireproof coating (especially expanding fire-proof paint), timber, textile, foam and paper always over the years
Wait the fire-retardant of products.But due to being a kind of novel flame retardant products, almost there are no foundation for secure data, for being used for a long time
Daily necessity containing this fire retardant, if can be harmful to human body, environment, there is great harm, various countries are also constantly
In research and accumulation data.And foreign countries also increasingly pay attention to the limitation requirement and content detection of melamine phosphate.
Although there is no the detection of its content in textile, foam both at home and abroad currently, MP has been widely used
Method.Therefore, how to establish a textile, in foam MP content detection method, will be extremely urgent.
[summary of the invention]
MP content in a kind of measurement textile or foam is provided present invention aim to solve above-mentioned deficiency
Method, not only measuring method quickly, it is simple, but also can be realized textile, in foam MP content Accurate Determining, solve not
There is the problem of detection fire-retartant agent MP content method.
A kind of method for measuring MP content in textile or foam is designed to achieve the above object, comprising the following steps: 1)
Sample pretreatment: textile samples are shredded with scissors, or foam sample is crushed with pulverizer, so that textile or foam sample
Product size is no more than 2mm × 2mm × 2mm, then smashed sample is uniformly mixed, and is packed into the valve bag of clean dried
In, it is sealed, it is spare；2) extraction of sample: weighing appropriate amount of sample, with the aqueous hydrochloric acid solution ultrasonic extraction of 1mol/L；3) it adopts
With High Performance Liquid Chromatography/Mass Spectrometry LC-MS method determination step 2) concentration of MP in resulting sample extraction solution；4) according to step 3)
The concentration of MP in resulting sample extraction solution calculates the content of MP in sample.
Further, in step 2), 0.5g sample is weighed in 40mL glass scre-cap bottle, the hydrochloric acid that 1mol/L is added is water-soluble
25~30mL of liquid, screws bottle cap, extracts 60min in 60 DEG C of water bath sonicators and accurately pipettes extraction solution 0.1mL after cooling,
It is diluted with water to 1mL, is mixed, the extracting solution after dilution is analyzed after pin type membrane filtration for LC-MS.
Further, in step 4), the content of MP in sample is obtained by the concentration conversion of MP in extraction solution, according to solvent
Calibration curve, using quantified by external standard method, minimum quantitative concentrations are 500mg/kg.
It further,, can if High Performance Liquid Chromatography/Mass Spectrometry (hereinafter referred to as LC-MS) testing result is the positive in step 3)
Result is confirmed using other instruments (such as liquid chromatography-tandem mass spectrometry instrument LC-MSMS).
Further, the determination condition of the LC-MS are as follows:
The present invention compared with the existing technology, has the advantages that
(1) present invention is a kind of sample after acid flux material extracts, and MP in textile or foam is directly measured with LC-MS and is contained
The method of amount；
(2) not only measuring method is quick, easy to operate by the present invention, but also can be realized textile, MP content in foam
Accurate Determining, minimum quantitative concentrations are 500mg/kg；
(3) present invention solves the problems, such as not detect fire-retartant agent MP content method, fully meets in textile, foam
The requirement of MP content monitoring.
[Detailed description of the invention]
Fig. 1 is in the embodiment of the present invention 2 using TIC chromatogram obtained by MP content in LC-MS detection cotton swatch.
[specific embodiment]
Although the present invention adds for new flame retardant MP but do not establish this problem of detection method of content, one is provided
The extracted method for directly measuring MP content in textile or foam with LC-MS of kind.The principle of the present invention are as follows: by the MP in sample
It is extracted with 1mol/L aqueous hydrochloric acid solution, then measures the content of MP in sample with LC-MS.Its determination step is as follows:
1) sample pretreatment: textile samples are shredded with scissors, or foam sample is crushed with pulverizer, so that weaving
Product or foam sample size are no more than 2mm × 2mm × 2mm, then smashed sample is uniformly mixed, and are packed into clean dried
Valve bag in, be sealed, it is spare.
2) extraction of sample: weighing appropriate amount of sample, with the aqueous hydrochloric acid solution ultrasonic extraction of 1mol/L.Specifically: it weighs
0.5g sample is added 25~30mL of aqueous hydrochloric acid solution of 1mol/L, screws bottle cap in 40mL glass scre-cap bottle, in 60 DEG C of water-baths
Ultrasonic extraction 60min accurately pipettes extraction solution 0.1mL, is diluted with water to 1mL after cooling, mixes, mentioning after dilution
It takes liquid after pin type membrane filtration, is analyzed for LC-MS.
3) LC-MS method determination step 2 is used) concentration of MP in resulting sample extraction solution；If LC-MS testing result is
Other instruments (such as liquid chromatography-tandem mass spectrometry instrument LC-MSMS) can be used to confirm result for the positive.
4) according to the concentration of MP in the resulting sample extraction solution of step 3), the content of MP in sample is calculated；Specifically, by
The concentration conversion for extracting MP in solution obtains the content of MP in sample, minimum using quantified by external standard method according to solvent calibration curve
Quantitative concentrations are 500mg/kg.
The present invention is made combined with specific embodiments below further explained below:
Embodiment 1: the measurement of MP 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.0.5g sample is weighed in 40mL glass scre-cap bottle, 1mol/L aqueous hydrochloric acid solution is added
30mL screws bottle cap, extracts 60min in 60 DEG C of water bath sonicators.After cooling, the 0.1mL extraction solution is accurately pipetted, it is dilute with water
1mL is released, is mixed.The extracting solution after dilution is filtered in LC sample introduction bottle through 0.22 μm of PTFE water phase filter membrane, for LC-MS
Analysis other instruments (such as LC-MSMS) can be used to confirm result if testing result is the positive.
2. setting LC-MS instrument parameter:
3. qualitative and quantitative
(1) qualitative: the retention time and feature of MP in the compound and standard solution detected in comparative sample extracting solution
Ion is qualitative.
(2) quantitative: according to the characteristic ion peak area of MP, using calibration curve quantified by external standard method.
4. calculating: according to the concentration of MP in sample extraction solution, calculating the content of MP in sample.Through detecting, in the filling
MP has been not detected in cotton sample product.
Embodiment 2: the measurement of MP 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.0.5g sample is weighed in 40mL glass scre-cap bottle, 1mol/L aqueous hydrochloric acid solution 30mL is added,
It screws lid and extracts 60min in 60 DEG C of water bath sonicators, take 0.1mL extracting solution to be diluted with water to 1mL after cooling, mix.Through 0.22 μ
The PTFE water phase filter membrane of m filters the extracting solution after dilution in LC sample introduction bottle, for LC-MS analysis.
2. setting instrument parameter:
The determination condition of LC-MS:
3. qualitative and quantitative
(1) qualitative: the retention time and feature of MP in the compound and standard solution detected in comparative sample extracting solution
Ion is qualitative.
(2) quantitative: according to the characteristic ion peak area of MP, using calibration curve quantified by external standard method.
4. calculating: according to the concentration of MP in sample extraction solution, calculating the content of MP in sample.
Through detecting, in the cotton swatch, the content of MP is 500mg/kg.
As shown in Fig. 1, MP content in cotton swatch, resulting TIC chromatogram are detected using LC-MS for the embodiment 2.
In figure, the chromatographic peak of 1.329min is the chromatographic peak that cotton extracts MP in solution.
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 (5)
1. a kind of method of melamine phosphate content in measurement textile or foam, which comprises the following steps:
1) sample pretreatment: textile samples are shredded with scissors, or foam sample is crushed with pulverizer so that textile or
Foam sample size is no more than 2mm × 2mm × 2mm, then smashed sample is uniformly mixed, and is packed into clean dried oneself
In envelope, it is sealed, it is spare；
2) extraction of sample: weighing appropriate amount of sample, with the aqueous hydrochloric acid solution ultrasonic extraction of 1mol/L；
3) High Performance Liquid Chromatography/Mass Spectrometry LC-MS method determination step 2 is used) concentration of MP in resulting sample extraction solution；
4) according to the concentration of melamine phosphate in the resulting sample extraction solution of step 3), melamine phosphate in sample is calculated
Content.
2. the method as described in claim 1, it is characterised in that: in step 2), weigh 0.5g sample in 40mL glass scre-cap bottle
In, 25~30mL of aqueous hydrochloric acid solution of 1mol/L is added, screws bottle cap, extracts 60min in 60 DEG C of water bath sonicators, after cooling,
Extraction solution 0.1mL is accurately pipetted, 1mL is diluted with water to, is mixed, the extracting solution after dilution supplies after pin type membrane filtration
LC-MS analysis.
3. the method as described in claim 1, it is characterised in that: in step 4), by extraction solution melamine phosphate it is dense
Degree conversion obtains the content of melamine phosphate in sample, minimum quantitative dense using quantified by external standard method according to solvent calibration curve
Degree is 500mg/kg.
4. the method as described in claim 1, it is characterised in that: in step 3), if LC-MS testing result is the positive, use liquid
Phase chromatography-tandem mass spectrometer LC-MSMS confirms result.
5. method as claimed in claim 4, which is characterized in that the determination condition of the LC-MS are as follows:
。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115792024A (en) * | 2022-12-09 | 2023-03-14 | 通标标准技术服务(上海)有限公司 | Method for measuring content of flame retardant FRC-2 in textiles and foam |
| CN117686620A (en) * | 2024-02-01 | 2024-03-12 | 深圳天祥质量技术服务有限公司 | Method for measuring melamine in textile and polymer material |
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Cited By (3)
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