Method for valuing purity standard substance of triphenyl phosphate

Abstract

The invention relates to the technical field of novel material chemical analysis, and discloses a triphenyl phosphate purity standard substance valuing method, which comprises the following steps: filtering, drying, dissolving and sterilizing a triphenyl phosphate sample; a triphenyl phosphate sample is comprehensively analyzed from different angles by comprehensively applying a GC-MS (Gas Chromatography-Mass Spectrometry) technology, an NMR (Nuclear Magnetic Resonance) technology, an infrared spectroscopy, a gas chromatography-flame ionization detector method, a Karl Fischer method and an inductively coupled plasma mass spectrometry, and finally, the purity value of the triphenyl phosphate purity standard substance is calculated by a mass balance method. The method provides a scientific and accurate technical means for quality control and standard formulation of the triphenyl phosphate product, has important practical application value for related industries in the fields of chemical engineering and material science, and is beneficial for improving the product quality and promoting industrial upgrading.

Description

Technical Field

[0001] This invention relates to the field of novel material chemical analysis technology, and in particular to a method for determining the purity of triphenyl phosphate standard material. Background Technology

[0002] In the current field of triphenyl phosphate purity detection, single detection techniques, such as gas chromatography (GC) or infrared spectroscopy (IR), are typically employed. While these methods have wide applications in specific areas, they also have significant limitations. For example, although gas chromatography can determine the content of the main component, it struggles to accurately identify impurities; while infrared spectroscopy can verify functional groups, it cannot perform further quantitative analysis. Furthermore, existing technologies lack detailed methods for systematic sample pretreatment, making samples susceptible to contamination, and moisture in the sample can interfere with the detection results, affecting the accuracy and repeatability of the assay.

[0003] Triphenyl phosphate, as an important chemical raw material, is widely used in plasticizers, flame retardants and other fields. Its purity has a crucial impact on the performance and quality of the products. At present, there is an urgent need in the market for a method to determine the purity of triphenyl phosphate that can integrate multiple detection technologies. This method should include component identification, chemical structure confirmation, functional group verification, determination of main component content, determination of moisture content and determination of inorganic metal content, so as to ensure the comprehensiveness and accuracy of purity determination.

[0004] Existing purity determination techniques lack detailed methods for systematic pretreatment of water-based samples. Samples are easily contaminated in the sampling environment, affecting the accuracy and repeatability of subsequent detections. Therefore, developing a method for determining the purity of triphenyl phosphate that integrates multiple detection techniques and optimizes sample pretreatment is of significant practical importance. Summary of the Invention

[0005] The purpose of this invention is to provide a method for determining the purity of triphenyl phosphate standard material in order to solve the problems in the prior art.

[0006] To achieve the above objectives, the present invention employs the following technical solution: a method for determining the purity of triphenyl phosphate standard material, comprising the following steps: Step S1: Collect the triphenyl phosphate sample for determination and pretreatment to obtain the sample solution and its weight; Step S2: Determine the sample components using GC-MS. Step S3: Confirm the chemical structure of the sample components using NMR technology; Step S4: Verify the functional groups of the main components of the sample using infrared spectroscopy; Step S5: Determine the content of the main components in the sample by gas chromatography-flame ionization detector method; Step S6: Determine the moisture content of the sample using the Karl Fischer method; Step S7: Determine the inorganic metal content of the sample by inductively coupled plasma mass spectrometry; Step S8: Based on the content of the main components, moisture content, inorganic metal content, and sample weight of the sample solution, calculate the purity value of the triphenyl phosphate purity standard material using the mass balance method.

[0007] The beneficial effects of the technical solution provided by this invention include at least the following: This invention comprehensively analyzes triphenyl phosphate samples from different perspectives by integrating multiple detection technologies. Specifically, GC-MS is used to accurately identify the main components and impurities in the samples, NMR is used to confirm the chemical structure of the samples, and infrared spectroscopy is used to verify the functional groups of the main components. Gas chromatography-flame ionization detector (GC-MS) is used to accurately determine the content of the main components, Karl Fischer titration is used to determine the moisture content of the samples, and inductively coupled plasma mass spectrometry (ICP-MS) is used to determine the inorganic metal content of the samples. This comprehensive application ensures the comprehensiveness and accuracy of the detection results, and can more accurately reflect the true purity of the triphenyl phosphate purity standard material, providing a solid data foundation for subsequent quality control and standard setting.

[0008] This invention describes in detail a sample pretreatment method, including steps such as filtration, drying, dissolving, sterilization, and preservation. These pretreatment steps can effectively remove impurities and moisture from the sample, prevent the sample from being contaminated during preservation and testing, provide a reliable basis for subsequent high-precision testing, and ensure the stability and reliability of the test results.

[0009] The method for determining the purity of triphenyl phosphate standard material provided by this invention offers a scientific and accurate technical means for the quality control and standard setting of triphenyl phosphate products. It has significant practical application value for related industries in the fields of chemical engineering and materials science. Through the method of this invention, related industries can more effectively control quality, enhance market competitiveness, and promote technological progress in the industry. Attached Figure Description

[0010] To more clearly illustrate the technical solutions and advantages in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0011] Figure 1 This is a flowchart of a method provided in an embodiment of the present invention. Detailed Implementation

[0012] To further illustrate the technical means and effects adopted by the present invention to achieve its intended purpose, the following, in conjunction with the accompanying drawings and preferred embodiments, details the specific implementation, structure, features, and effects of a method for determining the purity of triphenyl phosphate standard material according to the present invention. In the following description, different "one embodiment" or "another embodiment" do not necessarily refer to the same embodiment. Furthermore, specific features, structures, or characteristics in one or more embodiments can be combined in any suitable form.

[0013] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

[0014] The following examples are for illustrative purposes only and are not intended to limit the scope of the invention.

[0015] The following describes in detail, with reference to the accompanying drawings, a specific scheme for determining the purity standard substance of triphenyl phosphate provided by the present invention.

[0016] Please see Figure 1 The diagram illustrates a method flowchart for determining the purity of triphenyl phosphate standard material according to an embodiment of the present invention. The method includes the following steps: Step S1: Collect the triphenyl phosphate sample for determination and pretreatment to obtain the sample solution and its weight; Step S1 further includes the following sub-steps: S1-1, Collect the original sample from the triphenyl phosphate sample to be determined using a glass sampling bottle, and record the sampling time, sampling location, sampling batch and sample source; S1-2, the original sample is filtered through filter paper and then dried in a vacuum drying oven to obtain the dried original sample; S1-3, The methanol solvent is sterilized by ultraviolet light, and the dried original sample is dissolved in the sterilized methanol solvent to obtain a sample solution; S1-4, sterilize the glass container with high temperature and ultraviolet light, store the sample solution in the sterilized glass container and seal it; S1-5, Weigh the sample solution using an electronic balance to obtain the sample volume, store the sample solution in a refrigerator, and label it with the sample name, sample batch and storage date.

[0017] It should be noted that a vacuum drying oven is a device that reduces the air pressure inside the chamber by drawing a vacuum, thereby lowering the boiling point of water inside the chamber. This allows the moisture in the material to vaporize and escape at a lower temperature, thus achieving the drying of the material at a lower temperature.

[0018] Methanol ( It is an organic compound that is a colorless liquid with a pungent odor at room temperature and is one of the commonly used organic solvents.

[0019] Fusion sealing is a technique that involves heating materials such as glass to melt them and then sealing them. It is commonly used to seal containers. Fusion sealing of glass containers holding sample solutions can effectively isolate them from external air and impurities, prevent the samples from being contaminated during storage, ensure the stability and purity of the samples, and provide reliable conditions for subsequent value determination analysis.

[0020] An electronic balance is an instrument that uses the principle of electromagnetic force balance for weighing. It features high weighing accuracy, simple operation, and fast response. The accurate weighing amount is an important basis for subsequent calculation of the purity value of triphenyl phosphate standard material.

[0021] Step S2: Determine the sample components using GC-MS. Step S2 further includes the following sub-steps: S2-1, The sample solution is taken out from the sealed glass container by ultrasonic-assisted washing method, and the sample solution is diluted with methanol solvent to obtain the diluted sample solution; S2-2, a quartz capillary column with a length of 30 meters, an inner diameter of 0.25 mm, and a film thickness of 0.25 micrometers is selected as the mass spectrometry column of the GC-MS instrument, and 99.999% pure helium is selected as the carrier gas of the GC-MS instrument. The operating parameters of the GC-MS instrument are set, including the carrier gas flow rate, temperature control temperature, and duration. S2-3, inject the diluted sample solution into the inlet of the GC-MS instrument, run the GC-MS instrument, and obtain the mass spectrum of the sample solution, which includes molecular ion peaks, fragment ion peaks and isotope peaks; S2-4, compare the mass spectrum with the NIST standard mass spectrometry database to find compounds that match the mass spectrum, thereby obtaining sample components. The sample components include a main component and impurity components. The main component is triphenyl phosphate, and the impurity components include organic impurities, inorganic impurities, and polymer impurities.

[0022] It should be noted that, by definition, GC-MS (Gas Chromatography-Mass Spectrometry) is an analytical instrument that combines gas chromatography (GC) and mass spectrometry (MS). Gas chromatography is used to separate the components in a sample, while mass spectrometry is used to identify and quantify these components. Its working principle is as follows: Gas chromatography section: The sample is vaporized at high temperature and carried into the chromatographic column by a carrier gas (such as helium). The stationary phase in the chromatographic column separates the components in the sample according to the differences in boiling point and polarity of each component. Mass spectrometry section: The separated components enter the mass spectrometer and are ionized by a high-energy electron beam to generate molecular ions and fragment ions. The mass spectrometer automatically generates a mass spectrum by detecting the mass-to-charge ratio (m / z) of these ions.

[0023] An example of the operating parameters for a GC-MS coupled instrument is as follows: Carrier gas flow rate: 1.0 mL / min; Initial temperature: 50℃, hold for 2 minutes; Heating rate: 10℃ / min; Final temperature: 300℃, hold for 10 minutes.

[0024] The NIST (National Institute of Standards and Technology) Standard Mass Spectrometry Database is a database containing a large number of mass spectra of known compounds, used for mass spectrum comparison and compound identification.

[0025] Step S3: Confirm the chemical structure of the sample components using NMR technology; Step S3 further includes the following sub-steps: S3-1, The sample solution is taken out from the sealed glass container by ultrasonic-assisted washing method, and the sample solution is filtered through a filter membrane with a pore size of 0.22 micrometers to obtain the filtered sample solution; S3-2, select 400MHz frequency, with Broadband probe and A broadband probe NMR spectrometer, wherein the operating parameters of the NMR spectrometer are set, including pulse sequence, sampling time, and number of scans; S3-3, Load the filtered sample solution into an NMR tube, then place the NMR tube into the NMR spectrometer, start the NMR spectrometer, and obtain... NMR spectra and NMR spectrum; S3-4, using spectral analysis software to analyze the... NMR spectra and The chemical structures of the main components and impurities of the sample were obtained by NMR spectroscopy analysis.

[0026] It should be noted that ultrasonic-assisted elution is a method of extracting liquid materials from a container using the cavitation effect of ultrasound. The specific operation is as follows: Set the power and time of the ultrasonic cleaner (e.g., power 200W, time 10 minutes), open the sealed glass container by heat treatment, put it into the ultrasonic cleaner for ultrasonic treatment, transfer the solution to a centrifuge tube for centrifugation, and take the supernatant as the sample solution.

[0027] NMR (Nuclear Magnetic Resonance) spectroscopy is an instrument that uses the principle of nuclear magnetic resonance for structural analysis. It is primarily used to determine the structure of organic compounds. It works by placing the sample in a strong magnetic field and using radio frequency pulses to excite the nuclei (such as...) in the sample. 1 H, 13 (e.g., C) causes energy level transitions, and the relaxation process of the nucleus is detected to obtain NMR spectra.

[0028] An example of the operating parameters for an NMR spectrometer is as follows: Frequency: 400MHz; Pulse sequence: CPMG (Carr-Purcell-Meiboom-Gill) sequence; Sampling time: 1 second; Number of scans: 64.

[0029] Spectrum analysis software is computer software used to analyze and interpret NMR spectra. It helps researchers quickly and accurately identify signals in spectra and determine the structure of compounds. Its functions include: By comparing the spectrum with a database of known compounds, compounds in the sample can be quickly identified. The chemical shifts and coupling constants of atomic peaks in the spectrum are automatically identified, and the chemical structure of the compound is automatically deduced based on the chemical shifts and coupling constants.

[0030] Step S4: Verify the functional groups of the main components of the sample using infrared spectroscopy; Step S4 further includes the following sub-steps: S4-1, The sample solution is removed from the sealed glass container using an ultrasonic-assisted elution method, and the sample solution is dropped onto... A sample slice was obtained on the salt plate; S4-2, Set the operating parameters of the Fourier transform infrared spectrometer, including the scanning range, resolution, and number of scans; S4-3, Place the sample slice into the sample cell of the Fourier transform infrared spectrometer, start the Fourier transform infrared spectrometer, and perform a spectral scan on the sample slice to obtain the infrared absorption spectrum of the sample. S4-4. By comparing the infrared absorption spectrum of the sample with the standard spectrum, the functional groups of the main components of the sample are verified. The functional groups include phosphorus oxygen bonds (P=O), benzene rings and phenoxy groups (OC6H5).

[0031] It should be noted that Fourier Transform Infrared Spectroscopy (FTIR) is an infrared spectroscopy analysis instrument based on the Fourier transform principle, used to measure the infrared absorption spectrum of molecules, thereby identifying the functional groups present in the molecules.

[0032] An example of the operating parameters for a Fourier transform infrared spectrometer is as follows: Scan range: 4000 Up to 400 ; Resolution: 4 ; Number of scans: 32.

[0033] The functional groups of the principal components of the sample include: Phosphorus-oxygen bond (P=O): usually at 1200 Up to 1000 There are characteristic absorption peaks between them; Benzene ring: at 1600 Up to 1400 There are multiple characteristic absorption peaks, corresponding to the skeletal vibrations of the benzene ring; Phenoxy group (OC6H5): at 1250 Up to 1000 There are characteristic absorption peaks between them, corresponding to CO stretching vibrations.

[0034] Step S5: Determine the content of the main components in the sample by gas chromatography-flame ionization detector method; Step S5 further includes the following sub-steps: S5-1, The sample solution is taken out from the sealed glass container by ultrasonic-assisted washing, filtered through a filter membrane with a pore size of 0.22 micrometers, and diluted with methanol solvent to obtain a diluted sample solution; S5-2 uses a quartz capillary column with a length of 30 meters, an inner diameter of 0.25 mm, and a film thickness of 0.25 micrometers as the column of the gas chromatograph, and uses 99.999% pure helium as the carrier gas of the gas chromatograph. The operating parameters of the gas chromatograph are set, including the carrier gas flow rate, temperature control temperature, and duration. S5-3, using 99.999% pure hydrogen and air as the carrier gas of the hydrogen flame ionization detector, and setting the carrier gas flow rate of the hydrogen flame ionization detector; S5-4, the sample solution is injected into the chromatographic column, the gas chromatograph is run to obtain the separated components, the separated components are passed into the hydrogen flame ionization detector to generate an electrical signal, and the peak area and peak height of the main component of the sample are obtained based on the electrical signal; S5-5, Obtain a triphenyl phosphate standard solution from the National Institute of Standards and Testing, and use the triphenyl phosphate standard solution as a sample solution to perform the operations of steps S5-1 to S5-4 to obtain the peak area and peak height of the standard solution. Plot a standard curve with the concentration of the standard solution as the abscissa and the peak area or peak height as the ordinate, and then calculate the standard curve equation by linear regression. S5-6, Substitute the peak area and peak height of the main component of the sample into the standard curve equation to calculate the concentration of the main component in the sample. Then, calculate the content of the main component in the sample based on the concentration of the main component and the sample weight, as shown in the following formula: It should be noted that an example of the operating parameters for a gas chromatograph is as follows: Carrier gas flow rate: 1.0 mL / min; Initial temperature: 50℃, hold for 2 minutes; Heating rate: 10℃ / min; Final temperature: 300℃, hold for 10 minutes.

[0035] An example of a carrier gas flow rate for a hydrogen flame ionization detector is as follows: Hydrogen flow rate: 30 mL / min; Airflow rate: 300 mL / min.

[0036] The National Center for Standardization is an official organization that provides standard reference materials and solutions that have undergone rigorous national-level calibration to calibrate and verify the accuracy of analytical instruments.

[0037] Step S6: Determine the moisture content of the sample using the Karl Fischer method; Step S6 further includes the following sub-steps: S6-1, Karl Fischer reagent is prepared according to GB / T 606 standard, wherein the Karl Fischer reagent includes Karl Fischer titrant, Karl Fischer solvent and standard water solution; S6-2, the sample solution is taken out from the sealed glass container by ultrasonic-assisted washing method, 20mg of sample solution is dissolved in 1mL of Karl Fischer solvent to obtain the dissolved sample, and the dissolved sample is injected into the electrolytic cell of the Karl Fischer titrator using a microsyringe. S6-3, Start the Karl Fischer titrator. The Karl Fischer titrator will automatically add Karl Fischer titrant until the titration endpoint is reached. After the titration is completed, record the volume of Karl Fischer titrant consumed. S6-4. The moisture content in the sample is calculated based on the concentration of the Karl Fischer titrant and the volume of Karl Fischer titrant consumed.

[0038] It should be noted that GB / T 606 is a Chinese national standard that specifies the Karl Fischer method for moisture determination in chemical reagents. This standard describes in detail the principle, reagents, instruments, operating procedures, and calculation methods of the Karl Fischer method.

[0039] A Karl Fischer titrator is an instrument used to determine the moisture content in a sample. Based on the Karl Fischer reaction principle, it determines the moisture content in a sample by titration. The Karl Fischer titrant is added dropwise to the sample dissolved in Karl Fischer solvent until the moisture in the sample has completely reacted. The instrument automatically detects the titration endpoint. Karl Fischer titrants are reagents used for titration in the Karl Fischer process, and typically contain components such as iodine, sulfur dioxide, pyridine, or imidazole. Karl Fischer solvents are reagents used to dissolve samples in the Karl Fischer process. They typically contain components such as methanol, pyridine, or imidazole and are compatible with Karl Fischer titrants. Standard water solutions are reagents used in the Karl Fischer process to calibrate Karl Fischer titrators, ensuring the accuracy and reliability of the instrument.

[0040] The formula for calculating the moisture content of a sample using the concentration and volume of Karl Fischer titrant is as follows: In the formula, C is the concentration of Karl Fischer titrant (mol / L, known at the time of preparation), V is the volume of Karl Fischer titrant consumed (mL), M is the molar mass of water (18.015 g / mol, a constant), and m is the mass of the sample (g).

[0041] Step S7: Determine the inorganic metal content of the sample by inductively coupled plasma mass spectrometry; Step S7 further includes the following sub-steps: S7-1, Select an inductively coupled plasma mass spectrometer (ICP-MS), and prepare the reagents according to the ICP-MS instruction manual. The reagents include: concentration... of Solution, concentration of Solution, resistivity Deionized water and internal standard solution containing the metal element to be tested; S7-2, The sample solution is removed from the sealed glass container using an ultrasonic-assisted elution method, and then placed into a polytetrafluoroethylene digestion vessel. 5-10 mL of a concentrated solution is added. of Solution and 1-2 mL concentration of For the solution, set the operating parameters of the microwave digestion system, including temperature control temperature and duration; S7-3, the PTFE digestion vessel is placed in the microwave digestion system for digestion. After digestion, the PTFE digestion vessel is removed and cooled to room temperature. The solution in the PTFE digestion vessel is then transferred to a volumetric flask and analyzed using resistivity... The volume was adjusted to 50 mL with deionized water to obtain the digested sample solution. S7-4, the inductively coupled plasma mass spectrometer was calibrated using a commercially available internal standard solution containing the analyte metal element to obtain a calibration curve. The resistivity described above was then used. Deionized water was used as the blank solution for blank determination. The blank determination was repeated 3 times, and the average value of the 3 determinations was taken as the blank value. S7-5, Use an autosampler to inject the digested sample solution into the inductively coupled plasma mass spectrometer, start the inductively coupled plasma mass spectrometer, and the inductively coupled plasma mass spectrometer will automatically record the mass spectrometry signals of each inorganic metal element in the sample; S7-6: By comparing the mass spectrometry signals of each inorganic metal element in the sample with the calibration curve and blank value, the content of each inorganic metal element in the sample is calculated.

[0042] It should be noted that inductively coupled plasma mass spectrometry (ICP-MS) is a highly sensitive analytical instrument used to determine the content of multiple elements in a sample, especially trace and ultra-trace elements. It combines the high-temperature plasma source of inductively coupled plasma (ICP) with the high-sensitivity detector of mass spectrometry (MS).

[0043] A polytetrafluoroethylene (PTFE) digestion vessel is a container used for sample digestion. It is characterized by high temperature resistance, corrosion resistance, and non-contamination of samples. In this patent, it is used for microwave digestion of samples to ensure that the samples are completely dissolved under high temperature and high pressure.

[0044] A microwave digestion system is a device that uses microwave heating to digest samples. It can decompose organic matter in samples and release inorganic metal elements in a short time.

[0045] An example of the operating parameters for a microwave digestion system is as follows: Temperature control: 180℃; Duration: 30 minutes.

[0046] Internal standard solution is a standard solution containing a known concentration of the metal element to be measured. It is used to calibrate ICP-MS instruments and improve the accuracy and precision of measurements. The metal elements to be measured typically include: Lithium (Li): Used for calibration in the low mass number region; Yttrium (Y): Used for calibration in the medium mass number region; Indium (In): Used for calibration of high quality number regions.

[0047] Step S8: Calculate the purity value of the triphenyl phosphate purity standard material using the mass balance method based on the content of the main components, moisture content, inorganic metal content, and sample weight of the sample solution. Step S8 further includes the following sub-steps: S8-1, data processing and normalization of the main component content, moisture content, inorganic metal content and sample weight of the sample solution; S8-2, calculate the purity value of the main component of the sample, i.e., the purity value of the triphenyl phosphate purity standard, using the mass balance method, as follows: In the formula, The purity value of the triphenyl phosphate purity standard substance is given. The content of the main components in the sample. This refers to the sample volume of the sample solution. This refers to the moisture content of the sample. This represents the inorganic metal content of the sample.

[0048] It should be noted that normalization refers to converting data from different sources to the same scale for comparison and calculation. In this patent, the main purpose of normalization is to ensure that all data are on the same benchmark, which facilitates subsequent purity calculation. Specifically, it ensures that the units of all data are consistent, and the units of sample weight, principal component content, moisture content and inorganic metal content are unified as mg.

[0049] The above-described embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this application, and should all be included within the protection scope of this application.

Claims

1. A method for determining the purity of triphenyl phosphate standard material, characterized in that, The method includes: Step S1: Collect the triphenyl phosphate sample for determination and pretreatment to obtain the sample solution and its weight; Step S2: Determine the sample components using GC-MS. Step S3: Confirm the chemical structure of the sample components using NMR technology; Step S4: Verify the functional groups of the main components of the sample using infrared spectroscopy; Step S5: Determine the content of the main components in the sample by gas chromatography-flame ionization detector method; Step S6: Determine the moisture content of the sample using the Karl Fischer method; Step S7: Determine the inorganic metal content of the sample by inductively coupled plasma mass spectrometry; Step S8: Based on the content of the main components, moisture content, inorganic metal content, and sample weight of the sample solution, calculate the purity value of the triphenyl phosphate purity standard material using the mass balance method.

2. The method for determining the purity standard value of triphenyl phosphate according to claim 1, characterized in that: Step S1 further includes the following sub-steps: S1-1, Collect the original sample from the triphenyl phosphate sample to be determined using a glass sampling bottle, and record the sampling time, sampling location, sampling batch and sample source; S1-2, the original sample is filtered through filter paper and then dried in a vacuum drying oven to obtain the dried original sample; S1-3, The methanol solvent is sterilized by ultraviolet light, and the dried original sample is dissolved in the sterilized methanol solvent to obtain a sample solution; S1-4, sterilize the glass container with high temperature and ultraviolet light, store the sample solution in the sterilized glass container and seal it; S1-5, Weigh the sample solution using an electronic balance to obtain the sample volume, store the sample solution in a refrigerator, and label it with the sample name, sample batch and storage date.

3. The method for determining the purity standard value of triphenyl phosphate according to claim 1, characterized in that: Step S2 further includes the following sub-steps: S2-1, The sample solution is taken out from the sealed glass container by ultrasonic-assisted washing method, and the sample solution is diluted with methanol solvent to obtain the diluted sample solution; S2-2, a quartz capillary column with a length of 30 meters, an inner diameter of 0.25 mm, and a film thickness of 0.25 micrometers was selected as the mass spectrometry column for the GC-MS instrument. 99.999% pure helium was selected as the carrier gas for the GC-MS instrument. The operating parameters of the GC-MS instrument were set, including the carrier gas flow rate, temperature control temperature, and duration. The operating parameters of the GC-MS instrument are as follows: Carrier gas flow rate: 1.0 mL / min; Initial temperature: 50℃, hold for 2 minutes; Heating rate: 10℃ / min; Final temperature: 300℃, hold for 10 minutes; S2-3, inject the diluted sample solution into the inlet of the GC-MS instrument, run the GC-MS instrument, and obtain the mass spectrum of the sample solution, which includes molecular ion peaks, fragment ion peaks and isotope peaks; S2-4, compare the mass spectrum with the NIST standard mass spectrometry database to find compounds that match the mass spectrum, thereby obtaining sample components. The sample components include a main component and impurity components. The main component is triphenyl phosphate, and the impurity components include organic impurities, inorganic impurities, and polymer impurities.

4. The method for determining the purity standard value of triphenyl phosphate according to claim 1, characterized in that: Step S3 further includes the following sub-steps: S3-1, The sample solution is taken out from the sealed glass container by ultrasonic-assisted washing method, and the sample solution is filtered through a filter membrane with a pore size of 0.22 micrometers to obtain the filtered sample solution; S3-2, select 400MHz frequency, with Broadband probe and A broadband probe NMR spectrometer, wherein the operating parameters of the NMR spectrometer are set, including pulse sequence, sampling time, and number of scans; the operating parameters of the NMR spectrometer are as follows: Frequency: 400MHz; Pulse sequence: CPMG sequence; Sampling time: 1 second; Number of scans: 64; S3-3, Load the filtered sample solution into an NMR tube, then place the NMR tube into the NMR spectrometer, start the NMR spectrometer, and obtain... NMR spectra and NMR spectrum; S3-4, using spectral analysis software to analyze the... NMR spectra and The chemical structures of the main components and impurities of the sample were obtained by NMR spectroscopy analysis.

5. The method for determining the purity standard value of triphenyl phosphate according to claim 1, characterized in that: Step S4 further includes the following sub-steps: S4-1, The sample solution is removed from the sealed glass container using an ultrasonic-assisted elution method, and the sample solution is dropped onto... A sample slice was obtained on the salt plate; S4-2, Set the operating parameters of the Fourier transform infrared spectrometer, including the scanning range, resolution, and number of scans; the operating parameters of the Fourier transform infrared spectrometer are as follows: Scan range: 4000 Up to 400 ; Resolution: 4 ; Number of scans: 32; S4-3, Place the sample slice into the sample cell of the Fourier transform infrared spectrometer, start the Fourier transform infrared spectrometer, and perform a spectral scan on the sample slice to obtain the infrared absorption spectrum of the sample. S4-4. By comparing the infrared absorption spectrum of the sample with the standard spectrum, the functional groups of the main components of the sample are verified. The functional groups include phosphorus-oxygen bonds, benzene rings, and phenoxy groups.

6. The method for determining the purity standard value of triphenyl phosphate according to claim 1, characterized in that: Step S5 further includes the following sub-steps: S5-1, The sample solution is taken out from the sealed glass container by ultrasonic-assisted washing, filtered through a filter membrane with a pore size of 0.22 micrometers, and diluted with methanol solvent to obtain a diluted sample solution; S5-2 uses a 30-meter-long quartz capillary column with an inner diameter of 0.25 mm and a film thickness of 0.25 micrometers as the column of a gas chromatograph, and 99.999% pure helium as the carrier gas. The operating parameters of the gas chromatograph are set, including the carrier gas flow rate, temperature control temperature, and duration. The operating parameters of the gas chromatograph are as follows: Carrier gas flow rate: 1.0 mL / min; Initial temperature: 50℃, hold for 2 minutes; Heating rate: 10℃ / min; Final temperature: 300℃, hold for 10 minutes; S5-3, using 99.999% pure hydrogen and air as the carrier gas for the hydrogen flame ionization detector, the carrier gas flow rate of the hydrogen flame ionization detector is set; the carrier gas flow rate of the hydrogen flame ionization detector is: Hydrogen flow rate: 30 mL / min; Airflow rate: 300 mL / min; S5-4, the sample solution is injected into the chromatographic column, the gas chromatograph is run to obtain the separated components, the separated components are passed into the hydrogen flame ionization detector to generate an electrical signal, and the peak area and peak height of the main component of the sample are obtained based on the electrical signal; S5-5, Obtain a triphenyl phosphate standard solution from the National Institute of Standards and Testing, and use the triphenyl phosphate standard solution as a sample solution to perform the operations of steps S5-1 to S5-4 to obtain the peak area and peak height of the standard solution. Plot a standard curve with the concentration of the standard solution as the abscissa and the peak area or peak height as the ordinate, and then calculate the standard curve equation by linear regression. S5-6, substitute the peak area and peak height of the main component of the sample into the standard curve equation to calculate the concentration of the main component in the sample, and then calculate the content of the main component of the sample based on the concentration of the main component and the sample weight.

7. The method for determining the purity standard value of triphenyl phosphate according to claim 1, characterized in that: Step S6 further includes the following sub-steps: S6-1, Karl Fischer reagent is prepared according to GB / T 606 standard, wherein the Karl Fischer reagent includes Karl Fischer titrant, Karl Fischer solvent and standard water solution; S6-2, the sample solution is taken out from the sealed glass container by ultrasonic-assisted washing method, 20mg of sample solution is dissolved in 1mL of Karl Fischer solvent to obtain the dissolved sample, and the dissolved sample is injected into the electrolytic cell of the Karl Fischer titrator using a microsyringe. S6-3, Start the Karl Fischer titrator. The Karl Fischer titrator will automatically add Karl Fischer titrant until the titration endpoint is reached. After the titration is completed, record the volume of Karl Fischer titrant consumed. S6-4. The moisture content in the sample is calculated based on the concentration of the Karl Fischer titrant and the volume of Karl Fischer titrant consumed.

8. The method for determining the purity of triphenyl phosphate standard material according to claim 1, characterized in that: Step S7 further includes the following sub-steps: S7-1, Select an inductively coupled plasma mass spectrometer (ICP-MS), and prepare the reagents according to the ICP-MS instruction manual. The reagents include: concentration... of Solution, concentration of Solution, resistivity Deionized water and internal standard solution containing the metal element to be tested; S7-2, The sample solution is removed from the sealed glass container using an ultrasonic-assisted elution method, and then placed into a polytetrafluoroethylene digestion vessel. 5-10 mL of a concentrated solution is added. of Solution and 1-2 mL concentration of The solution was prepared, and the operating parameters of the microwave digestion system were set, including temperature control and duration. The operating parameters of the microwave digestion system are as follows: Temperature control: 180℃; Duration: 30 minutes; S7-3, the PTFE digestion vessel is placed in the microwave digestion system for digestion. After digestion, the PTFE digestion vessel is removed and cooled to room temperature. The solution in the PTFE digestion vessel is then transferred to a volumetric flask and analyzed using resistivity... The volume was adjusted to 50 mL with deionized water to obtain the digested sample solution. S7-4, the inductively coupled plasma mass spectrometer was calibrated using a commercially available internal standard solution containing the analyte metal element to obtain a calibration curve. The resistivity described above was then used. Deionized water was used as the blank solution for blank determination. The blank determination was repeated 3 times, and the average value of the 3 determinations was taken as the blank value. S7-5, Use an autosampler to inject the digested sample solution into the inductively coupled plasma mass spectrometer, start the inductively coupled plasma mass spectrometer, and the inductively coupled plasma mass spectrometer will automatically record the mass spectrometry signals of each inorganic metal element in the sample; S7-6: By comparing the mass spectrometry signals of each inorganic metal element in the sample with the calibration curve and blank value, the content of each inorganic metal element in the sample is calculated.

9. The method for determining the purity of triphenyl phosphate standard material according to claim 1, characterized in that: Step S8 further includes the following sub-steps: S8-1, data processing and normalization of the main component content, moisture content, inorganic metal content and sample weight of the sample solution; S8-2, calculate the purity value of the main component of the sample, i.e., the purity value of the triphenyl phosphate purity standard, using the mass balance method, as follows: In the formula, The purity value of the triphenyl phosphate purity standard substance. The content of the principal components in the sample. This refers to the sample volume of the sample solution. This refers to the moisture content of the sample. This represents the inorganic metal content of the sample.

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