CN111157660B - Method for measuring content of tetrakis (hydroxymethyl) phosphonium chloride in textile or foam - Google Patents
Method for measuring content of tetrakis (hydroxymethyl) phosphonium chloride in textile or foam Download PDFInfo
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Abstract
The invention relates to a method for measuring the content of tetrakis (hydroxymethyl) phosphonium chloride in textiles or foam, which comprises the following steps: 1) sample pretreatment: crushing the textile sample or the foam sample to a size not more than 2 multiplied by 2mm, uniformly mixing the crushed textile sample or the foam sample, putting the mixture into a clean and dry self-sealing bag, and sealing and storing the bag for later use; 2) and (3) extracting a sample: ultrasonically extracting with 85% methanol-water or 8mmol/L sodium hydroxide solution, diluting with water, and mixing; 3) determining the concentration of tetrakis hydroxymethyl phosphonium chloride in the sample extraction solution by adopting an LC-MS method; 4) calculating the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample according to the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution; the method is quick and simple to determine, can accurately determine the content of the tetramethylolphosphonium chloride in the textile or the foam, has the lowest quantitative concentration of 500mg/kg, and solves the problem that the method for detecting the content of the tetramethylolphosphonium chloride in the flame retardant is unavailable.
Description
[ technical field ]
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for measuring the content of tetrakis (hydroxymethyl) phosphonium chloride in textiles or foam.
[ background art ]
The fire-retardant fireproof door is suitable for the requirements of safe production and life of the society, prevents fire, protects the lives and properties of people, and adopts a fire-retardant scientific technology. The flame retardant is an application of flame retardant technology in actual life, is a special chemical auxiliary agent for improving the combustion performance of combustible and combustible materials, and is widely applied to flame retardant processing of various materials. The material processed by the flame retardant can effectively prevent, delay or stop the propagation of flame when being attacked by an external fire source, thereby achieving the flame retardant effect. The traditional flame retardant represented by the halogen flame retardant has good flame retardant effect, and can be widely applied without influencing the physical and chemical properties of materials. However, the polymer added with the halogen flame retardant has large smoke quantity during combustion, is easy to emit toxic and harmful gases and is easy to cause secondary damage. With the increasing awareness of environmental protection and safety, the research on the flame retardant in the world is rapidly developing towards the non-halogenated novel flame retardant.
As a novel phosphate flame retardant, the condensed phosphate has high phosphorus content, high relative molecular weight, high thermal stability, basically no influence on the environment, good flame retardant effect, low toxicity, less smoke, low price and the like, and shows excellent application effect. The flame retardant can keep the original strength and flexibility of the fiber, can be used for military face, rain-proof cloth and work flame-retardant treatment, and has wide application fields. The phosphorus-containing flame retardant conforms to the development trend of the flame retardant, and is rapidly developed in recent years.
Although tetrakis (hydroxymethyl) phosphonium chloride is a novel flame retardant and is widely applied to products such as textiles and foam, the tetrakis (hydroxymethyl) phosphonium chloride is a novel flame retardant product, the safety data of the tetrakis (hydroxymethyl) phosphonium chloride is not complete, and a certain safety risk still exists when the tetrakis (hydroxymethyl) phosphonium chloride is added in a large amount in household products as the flame retardant. The requirement of limiting the amount of tetrakis (hydroxymethyl) phosphonium chloride and the content detection are more and more important abroad. At present, no method for detecting the content of tetrakis (hydroxymethyl) phosphonium chloride in textiles and foam at home and abroad exists. The tetrakis (hydroxymethyl) phosphonium chloride compound has larger polarity, good solubility in water and almost no solubility in most organic solvents such as toluene and acetone, and the conventional flame retardant detection method is obviously not suitable for detecting the tetrakis (hydroxymethyl) phosphonium chloride. Thus. If a method for detecting the content of the tetrakis (hydroxymethyl) phosphonium chloride in the textile and the foam can be established, the need is urgent.
[ summary of the invention ]
The invention aims to solve the defects and provide a method for measuring the content of the tetrakis (hydroxymethyl) phosphonium chloride in the textile or the foam, the measuring method is quick and simple, the content of the tetrakis (hydroxymethyl) phosphonium chloride in the textile or the foam can be accurately measured, and the problem that the method for measuring the content of the tetrakis (hydroxymethyl) phosphonium chloride in the flame retardant is not available is solved.
In order to achieve the purpose, the method for measuring the content of the tetrakis (hydroxymethyl) phosphonium chloride in the textile or the foam comprises the following steps: 1) sample pretreatment: crushing the textile sample or the foam sample to the size of no more than 2mm multiplied by 2mm, then uniformly mixing the crushed textile sample or the foam sample, putting the mixture into a clean and dry self-sealing bag, and sealing and storing the bag for later use; 2) and (3) extracting a sample: weighing the sample obtained in the step 1), performing ultrasonic extraction by using 85% methanol-water solution or 8mmol/L sodium hydroxide solution, diluting by using water, and uniformly mixing to obtain a sample extraction solution; 3) determining the concentration of tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution obtained in the step 2) by adopting a liquid chromatography-mass spectrometry LC-MS method; 4) calculating the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample according to the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution obtained in the step 3).
Further, in the step 1), shearing the textile sample by using scissors until the size of the textile sample does not exceed 2 multiplied by 2 mm; for the foam sample, the foam is crushed to a size not exceeding 2X 2mm by a crusher.
Further, in the step 2), when the content of tetrakis (hydroxymethyl) phosphonium chloride in the sample is less than 200mg/kg, 0.5g +/-0.01 g of the sample is weighed in an empty bottle, 25mL of methanol-water solution is added, the sample is sealed and subjected to ultrasonic extraction in a water bath at 60 ℃ for 60min, 0.5mL of extracting solution is obtained after cooling, the methanol-water solution is added to dilute the extracting solution to 1mL, and the extracting solution is filtered by a 0.2 mu mPTE filter membrane and then subjected to LC-MS analysis; when the content of tetrakis (hydroxymethyl) phosphonium chloride in the sample is more than 200mg/kg, 0.5g +/-0.01 g of the sample is weighed and placed in an empty bottle, 25mL of 8mmol/L sodium hydroxide solution is added, the bottle is sealed and then is subjected to ultrasonic extraction in a water bath at 60 ℃ for 60min, 500 mu L of extracting solution is taken after the solution is cooled to room temperature, 500 mu L of pure water is added, the solution is uniformly mixed, and the mixture is filtered through a 0.2 mu mPTEF filter membrane and then is subjected to LC-MS analysis.
Further, in step 3), the LC-MS measurement conditions are as follows:
1) the liquid chromatographic column adopts a ZIC-cHILIC column, and has a column length of 15cm, a column inner diameter of 2.1mm and a particle size of 3 μm;
2) the temperature of the liquid chromatographic column is set to be 30 ℃;
3) sample introduction amount: 10 mu L of the solution;
4) mobile phase: 10mmol/L ammonium acetate: acetonitrile 45: 55;
5) flow rate: 0.3 mL/min;
6) operating time: 20 min;
7) the mass spectral parameters are given in the following table:
further, in the step 4), comparing the retention time of the sample peak with that of the standard sample peak, comparing the sample peak full-scanning mass spectrogram with that of the standard substance full-scanning mass spectrogram, determining whether tetrakis (hydroxymethyl) phosphonium chloride is detected in the sample, and quantifying by adopting a solvent calibration curve external standard method.
Further, in the step 4), the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution is converted into the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample, and the content is quantified by an external standard method according to a solvent calibration curve, wherein the lowest quantitative concentration is 500 mg/kg.
Compared with the prior art, the invention provides the method for directly measuring the content of the tetrakis (hydroxymethyl) phosphonium chloride in the textile or the foam by using the liquid chromatography-mass spectrometer (LC-MS) after a sample is directly extracted by the organic solvent or the alkaline solution, the measuring method is not only quick and simple, but also can realize the accurate measurement of the content of the tetrakis (hydroxymethyl) phosphonium chloride in the textile or the foam, the lowest quantitative concentration is 500mg/kg, the problem that the method for detecting the content of the flame retardant tetrakis (hydroxymethyl) phosphonium chloride does not exist is solved, the requirement for monitoring the content of the tetrakis (hydroxymethyl) phosphonium chloride in the textile or the foam is completely met, and the method is worthy of popularization and application.
[ description of the drawings ]
FIG. 1 is a TIC chromatogram obtained by measuring the content of tetrakis (hydroxymethyl) phosphonium chloride in a cotton sample by LC-MS in example 2 of the present invention.
[ detailed description of the invention ]
The invention provides a method for directly measuring the content of tetrakis (hydroxymethyl) phosphonium chloride in textiles and foam cotton by LC-MS (liquid chromatography-mass spectrometry) through extraction, aiming at the problem that the content of tetrakis (hydroxymethyl) phosphonium chloride which is a novel flame retardant is not added but is not detected. The principle is as follows: ultrasonically extracting tetrakis (hydroxymethyl) phosphonium chloride in a sample by using an organic solution or a sodium hydroxide aqueous solution, diluting and filtering, and then determining the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample by using LC-MS (liquid chromatography-mass spectrometry), wherein the specific determination steps are as follows:
1) sample pretreatment: shearing a textile sample by using scissors or crushing a foam sample by using a crusher to ensure that the size of the textile or the foam sample is not more than 2mm multiplied by 2mm, uniformly mixing the crushed samples, filling the mixture into a clean and dry self-sealing bag, and sealing and storing the bag for later use;
2) and (3) extracting a sample: when the content of tetrakis hydroxymethyl phosphonium chloride in the sample is less than 200mg/kg, weighing 0.5g +/-0.01 g of the sample in a 40mL capping headspace bottle, adding 25mL of methanol-water (85: 15) solution, sealing, performing ultrasonic extraction in a water bath at 60 ℃ for 60min, cooling, taking 0.5mL of extract, adding the methanol-water (85: 15) solution to dilute to 1mL, filtering by a 0.2 mu mPTEF filter membrane, and analyzing by LC-MS; when the content of tetrakis hydroxymethyl phosphonium chloride in the sample is more than 200mg/kg, weighing 0.5g +/-0.01 g of sample in a 40mL capping headspace bottle, adding 25mL of 8mmol/L sodium hydroxide solution, sealing, performing ultrasonic extraction in a water bath at 60 ℃ for 60min, cooling to room temperature, taking 500 mu L of extracting solution, adding 500 mu L of pure water, uniformly mixing, filtering through a 0.2 mu m TFE filter membrane, and analyzing by LC-MS;
3) determining the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution obtained in the step 2) by adopting LC-MS, wherein the determination conditions of a liquid chromatogram-mass spectrometer are as follows:
a) the liquid chromatographic column adopts a ZIC-cHILIC column, and has a column length of 15cm, a column inner diameter of 2.1mm and a particle size of 3 μm;
b) the temperature of the liquid chromatographic column is set to be 30 ℃;
c) sample introduction amount: 10 μ L
d) Mobile phase: 10mmol/L ammonium acetate: acetonitrile: 45: 55
e) Flow rate: 0.3mL/min
f) Operating time: 20min
g) The mass spectral parameters are given in the following table:
4) calculating the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample according to the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution obtained in the step 3); specifically, the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample is obtained by converting the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution, and the lowest quantitative concentration is 500mg/kg by adopting an external standard method for quantification according to a solvent calibration curve.
The invention is further illustrated below with reference to specific embodiments:
example 1: determination of content of tetrakis (hydroxymethyl) phosphonium chloride in filling cotton
1. Preparation of sample solution:
crushing the filling cotton by a crusher, wherein the size of a sample is not more than 2mm multiplied by 2 mm; uniformly mixing the crushed samples, filling the samples into clean and dry self-sealing bags, and sealing and storing the self-sealing bags for later use; weighing 0.5g of sample into a 40mL glass screw bottle, adding 25mL of methanol-water (85: 15) solution, sealing, performing ultrasonic extraction in a water bath at 60 ℃ for 60min, cooling, taking 0.5mL of extract, adding methanol-water (85: 15) solution to dilute to 1mL, filtering through a 0.2 mu mTFE filter membrane, and performing LC-MS analysis.
2. Setting instrument parameters:
a) the liquid chromatographic column adopts a ZIC-cHILIC column, and has a column length of 15cm, a column inner diameter of 2.1mm and a particle size of 3 μm;
b) the temperature of the liquid chromatographic column is set to be 30 ℃;
c) sample introduction amount: 10 μ L
d) Mobile phase: 10mmol/L ammonium acetate: acetonitrile: 45: 55
e) Flow rate: 0.3mL/min
f) Operating time: 20min
g) The mass spectral parameters are given in the following table:
3. qualitative and quantitative
a) And (3) qualitative determination: and comparing the retention time of the sample peak with that of the standard sample peak, and comparing the sample peak full-scanning mass spectrogram with that of the standard substance full-scanning mass spectrogram to determine whether the tetrakis (hydroxymethyl) phosphonium chloride is detected in the sample.
b) Quantification: quantification was done using a solvent calibration curve external standard method.
4. And (3) calculating:
and calculating the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample according to the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution. No tetrakis hydroxymethyl phosphonium chloride is detected in the filling cotton sample.
Example 2: determination of Tetrahydroxymethyl Phosphorus chloride in Cotton cloth
1. Preparation of a sample:
shearing cotton cloth with scissors until the size of the sample is not more than 2mm × 2mm × 2mm, mixing, packaging into clean and dry self-sealing bag, and sealing; weighing 0.5g of sample into a 40mL glass screw bottle, adding 25mL of methanol-water (85: 15) solution, sealing, performing ultrasonic extraction in a water bath at 60 ℃ for 60min, cooling, taking 0.5mL of extract, adding methanol-water (85: 15) solution to dilute to 1mL, filtering through a 0.2 mu mTFE filter membrane, and performing LC-MS analysis.
2. Setting instrument parameters:
a) the liquid chromatographic column adopts a ZIC-cHILIC column, and has a column length of 15cm, a column inner diameter of 2.1mm and a particle size of 3 μm;
b) the temperature of the liquid chromatographic column is set to be 30 ℃;
c) sample introduction amount: 10 μ L
d) Mobile phase: 10mmol/L ammonium acetate: acetonitrile: 45: 55
e) Flow rate: 0.3mL/min
f) Operating time: 20min
g) The mass spectral parameters are given in the following table:
3. qualitative and quantitative
a) And (3) qualitative determination: and comparing the retention time of the sample peak with that of the standard sample peak, and comparing the sample peak full-scanning mass spectrogram with that of the standard substance full-scanning mass spectrogram to determine whether the tetrakis (hydroxymethyl) phosphonium chloride is detected in the sample.
b) And (3) quantification: quantification was done using a solvent calibration curve external standard method.
4. And (3) calculating:
and calculating the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample according to the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution. The concentration of tetrakis hydroxymethyl phosphonium chloride in the sample was found to be greater than 200 mg/kg.
5. Re-extraction and detection of the sample:
weighing 0.5g +/-0.01 g of sample, adding 25mL of 8mmol/L sodium hydroxide solution into a 40mL capped headspace bottle, sealing, performing ultrasonic extraction in a water bath at 60 ℃ for 60min, cooling to room temperature, taking 500 mu L of extract, adding 500 mu L of pure water, mixing uniformly, filtering through a 0.2 mu mTFE filter membrane, and performing LC-MS analysis. And (4) performing LC-MS detection and qualitative and quantitative analysis on the sample extraction solution according to the steps 2) to 4). And calculating the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample according to the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution.
The cotton cloth sample is detected to have the content of the tetrakis (hydroxymethyl) phosphonium chloride of 1102.32 mg/kg. As shown in figure 1, the chromatographic peak of 1.887min is the chromatographic peak of tetrakis (hydroxymethyl) phosphonium chloride in cotton cloth extract solution, which is a TIC chromatogram obtained by detecting the tetrakis (hydroxymethyl) phosphonium chloride content in a cotton cloth sample by LC-MS.
The present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents and are included in the scope of the present invention.
Claims (4)
1. A method for measuring the content of tetrakis (hydroxymethyl) phosphonium chloride in textiles or foam is characterized by comprising the following steps:
1) sample pretreatment: the textile sample or the foam sample is crushed to the size not more than 2mm multiplied by 2mm, and then the crushed textile sample or the foam sample is uniformly mixed, put into a clean and dry self-sealing bag and sealed for storage for standby;
2) and (3) extracting a sample: weighing the sample obtained in the step 1), performing ultrasonic extraction by using 85% methanol-water solution or 8mmol/L sodium hydroxide solution, diluting with water, and mixing uniformly to obtain a sample extraction solution;
3) measuring the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution obtained in the step 2) by adopting a liquid chromatography-mass spectrometry (LC-MS) method;
4) calculating the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample according to the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution obtained in the step 3);
in the step 2), when the content of tetrakis hydroxymethyl phosphonium chloride in the sample is less than 200mg/kg, 0.5g +/-0.01 g of the sample is weighed in an empty bottle, 25mL of methanol-water solution is added, the sample is sealed and is subjected to ultrasonic extraction in a water bath at 60 ℃ for 60min, 0.5mL of extracting solution is taken after cooling, the methanol-water solution is added to dilute the extracting solution to 1mL, and the extracting solution is filtered by a 0.2 mu mPTEF filter membrane and is subjected to LC-MS analysis; when the content of tetrakis hydroxymethyl phosphonium chloride in the sample is more than 200mg/kg, weighing 0.5g +/-0.01 g of the sample in an empty bottle, adding 25mL of 8mmol/L sodium hydroxide solution, sealing, carrying out ultrasonic extraction in a water bath at 60 ℃ for 60min, cooling to room temperature, taking 500 mu L of extracting solution, adding 500 mu L of pure water, mixing uniformly, filtering through a 0.2 mu mPTFE filter membrane, and analyzing by LC-MS;
in the step 3), the LC-MS determination conditions are as follows:
1) the liquid chromatographic column adopts a ZIC-cHILIC column, and has a column length of 15cm, a column inner diameter of 2.1mm and a particle size of 3 μm;
2) the temperature of the liquid chromatographic column is set to be 30 ℃;
3) sample introduction amount: 10 mu L of the solution;
4) mobile phase: 10mmol/L ammonium acetate: acetonitrile 45: 55;
5) flow rate: 0.3 mL/min;
6) operating time: 20 min;
7) the mass spectral parameters are given in the following table:
2. the method of claim 1 for determining the level of tetrakis hydroxymethyl phosphonium chloride in a textile or foam, wherein: in the step 1), shearing a textile sample by using scissors until the size of the textile sample is not more than 2mm multiplied by 2 mm; for the foam sample, the foam sample is crushed to a size not exceeding 2mm × 2mm × 2mm by a crusher.
3. The method of claim 1 for determining the level of tetrakis hydroxymethyl phosphonium chloride in a textile or foam, wherein: in the step 4), comparing the retention time of the sample peak with that of the standard sample peak, comparing the sample peak full-scanning mass spectrogram with that of the standard substance full-scanning mass spectrogram, determining whether tetrakis (hydroxymethyl) phosphonium chloride is detected in the sample, and quantifying by adopting a solvent calibration curve external standard method.
4. The method of claim 1 for determining the level of tetrakis hydroxymethyl phosphonium chloride in a textile or foam, wherein: in the step 4), the concentration of the tetrakis (hydroxymethyl) phosphonium chloride in the sample extraction solution is converted into the content of the tetrakis (hydroxymethyl) phosphonium chloride in the sample, and the lowest quantitative concentration is 500mg/kg by adopting an external standard method according to a solvent calibration curve.
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| CN106018615A (en) * | 2016-06-28 | 2016-10-12 | 中纺标检验认证有限公司 | Detection method for unallowable or restricted fire retardant in textile |
| CN106770724A (en) * | 2016-11-29 | 2017-05-31 | 通标标准技术服务(上海)有限公司 | A kind of method for determining phosphoguanidine content in textile and packing material |
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| CN106018615A (en) * | 2016-06-28 | 2016-10-12 | 中纺标检验认证有限公司 | Detection method for unallowable or restricted fire retardant in textile |
| CN106770724A (en) * | 2016-11-29 | 2017-05-31 | 通标标准技术服务(上海)有限公司 | A kind of method for determining phosphoguanidine content in textile and packing material |
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