Method for determining content of hydrogenated bisphenol A epoxy resin and application of hydrogenated bisphenol A epoxy resin

Abstract

The invention discloses a method for determining the content of hydrogenated bisphenol A epoxy resin and application of the hydrogenated bisphenol A epoxy resin, and the method comprises the following steps: determining a hydrogenated bisphenol A epoxy resin standard solution by adopting a thermal cracking-gas chromatography-mass spectrometer, and drawing a standard working curve, the gas chromatographic column is a capillary column chromatographic column of which the filler is (50%-phenyl)-methylpolysiloxane or a capillary column chromatographic column of which the filler is polyethylene glycol; testing the sample by adopting the same step as the step of determining the hydrogenated bisphenol A epoxy resin standard solution; and calculating the content of hydrogenated bisphenol A epoxy resin in the sample according to the obtained standard working curve. According to the method, hydrogenated bisphenol A epoxy resin can be cracked into hydrogenated bisphenol A, so that the hydrogenated bisphenol A epoxy resin in a sample (such as a sealant) can be quantitatively analyzed.

Description

Technical Field

[0001] The invention relates to the field of polymer detection and analysis, and in particular to a method for determining the content of hydrogenated bisphenol A epoxy resin and application thereof. Background Art

[0002] Hydrogenated bisphenol A epoxy resin is polymerized from hydrogenated bisphenol A. It is a new type of resin raw material with the advantages of non-toxicity, chemical stability, UV resistance, thermal stability and weather resistance. Therefore, it is widely used in various plastics, waterproof coatings, adhesives and other fields. Using hydrogenated epoxy resin as a material in caulking agent can improve the performance of the product, such as being more environmentally friendly and healthy and extending the service life. At present, many caulking agent manufacturers claim that the caulking agents they produce are added with hydrogenated bisphenol A epoxy resin, but because hydrogenated bisphenol A epoxy resin is a polymer, it cannot be directly measured. There is no direct method for detecting hydrogenated bisphenol A epoxy resin in China. Therefore, it is impossible to determine whether hydrogenated bisphenol A epoxy resin is added to the caulking agent and its content.

[0003] In summary, it is necessary to provide a method for directly determining the content of hydrogenated bisphenol A epoxy resin in a sample. Summary of the invention

[0004] In view of this, the present invention provides a method for determining the content of hydrogenated bisphenol A epoxy resin and its use. The method can crack the hydrogenated bisphenol A epoxy resin into hydrogenated bisphenol A, thereby quantitatively analyzing the hydrogenated bisphenol A epoxy resin in a sample (such as a seam beauty agent).

[0005] The present invention provides the following technical solutions:

[0006] A method for determining the content of hydrogenated bisphenol A epoxy resin in a sample comprises adopting a thermal cracking-gas chromatography-mass spectrometer to determine a hydrogenated bisphenol A epoxy resin standard solution and drawing a standard working curve, wherein the hydrogenated bisphenol A epoxy resin in the sample is determined by detecting hydrogenated bisphenol A, and wherein the gas chromatography column is a capillary column chromatographic column filled with (50%-phenyl)-methyl polysiloxane or a capillary column chromatographic column filled with polyethylene glycol; the sample is tested by adopting the same steps as those for determining the hydrogenated bisphenol A epoxy resin standard solution; and the content of hydrogenated bisphenol A epoxy resin in the sample is calculated according to the obtained standard working curve.

[0007] The present invention provides the following non-conventional alternatives:

[0008] The correlation coefficient of the obtained standard working curve was at least 0.995.

[0009] In the gas chromatography, the capillary chromatographic column has a length of 10-60m, an inner diameter of 0.18-0.53mm, and a film thickness of 0.18-0.53μm; wherein the gas chromatographic column is a capillary column chromatographic column whose filler is polyethylene glycol.

[0010] The gas chromatograph has an injection port temperature of 200-240°C, a flow rate of 0.8-1.5 mL / min, an injection mode of split injection, and a split ratio of (8-15):1. The temperature is programmed to rise from 90-110°C to 260-270°C at a heating rate of 5-15°C / min and maintained for 20-40 minutes.

[0011] The thermal cracking adopts a double-click mode, and the thermal cracking heating program is: starting from 50-70°C, heating to 100-130°C at a heating rate of 20-40°C / min, maintaining for 0.1-0.3min, and then heating to 480-520°C at a heating rate of 30-50°C / min, maintaining for 0.5-2min.

[0012] In the mass spectrometry detection, the transmission line temperature is: 23-270°C; the ion source temperature is: 280-320°C; the acquisition mode is: SCAN∼ and the solvent delay time is: 2-5min.

[0013] When the gas chromatography column is a capillary column whose filler is (50%-phenyl)-methylpolysiloxane, in the gas chromatogram, the retention time of hydrogenated bisphenol A is 15.79-15.99 min.

[0014] When the gas chromatography column is a capillary column whose filler is polyethylene glycol, in the gas chromatogram, the retention time of hydrogenated bisphenol A is 30.29-34.19 min.

[0015] The steps of using a pyrolysis-gas chromatography-mass spectrometer to measure a hydrogenated bisphenol A epoxy resin standard solution and draw a standard working curve include using an organic solvent to configure a hydrogenated bisphenol A epoxy resin standard substance into a series of hydrogenated bisphenol A epoxy resin standard solutions of concentration; using a pyrolysis-gas chromatography-mass spectrometer to test the obtained standard solution, and then drawing a standard working curve with the chromatographic peak area of ​​the hydrogenated bisphenol A epoxy resin as the ordinate and the concentration of the standard solution as the abscissa; wherein the organic solvent includes one or more of toluene, dichloromethane, chloroform, ether, ethyl acetate, methyl acetate, acetone, and n-propanol.

[0016] The present invention also provides the method as described above for determining the use of hydrogenated bisphenol A epoxy resin in a seam-beautifying agent.

[0017] According to the technical solution of the present invention, the method of the present invention adopts thermal cracking-gas chromatography-mass spectrometry to determine the content of hydrogenated bisphenol A epoxy resin in the sample; wherein the gas chromatography column is a capillary column chromatographic column filled with (50%-phenyl)-methyl polysiloxane or a capillary column chromatographic column filled with polyethylene glycol. Thus, the hydrogenated bisphenol A epoxy resin is cracked into hydrogenated bisphenol A for detection and analysis, and the specific capillary column chromatographic column used can distinguish the isomers of hydrogenated bisphenol A, and at the same time make the peak of hydrogenated bisphenol A symmetrical and sharp. Through the accurate standard working curve, the content of hydrogenated bisphenol A epoxy resin can be accurately quantitatively analyzed. In addition, the method does not need to perform cumbersome pre-treatment steps on the sample and consume a large amount of solvent, the detection process is simple, and the detection cost is low. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] For purposes of illustration and not limitation, the present invention will now be described in terms of preferred embodiments thereof, with particular reference to the accompanying drawings, in which:

[0019] Figure 1 is a chromatogram of hydrogenated epoxy resin pyrolysis products separated by a polyethylene glycol capillary chromatography column in this embodiment;

[0020] Figure 2 is a mass spectrum of the hydrogenated epoxy resin pyrolysis product in this embodiment;

[0021] Figure 3 is a chromatogram of hydrogenated epoxy resin pyrolysis products separated by a (50%-phenyl)-methylpolysiloxane chromatography column in the present embodiment;

[0022] Figure 4 is a chromatogram of the hydrogenated epoxy resin pyrolysis product separated by a (5%-phenyl)-methylpolysiloxane chromatography column in a comparative example; and

[0023] Figure 5 It is the chromatogram of the hydrogenated epoxy resin pyrolysis product separated by the 100% methyl polysiloxane chromatography column in the comparative example. DETAILED DESCRIPTION

[0024] For ease of understanding of the present invention, the present invention will be described more fully below with reference to examples. Preferred embodiments of the present invention are provided in the examples. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0025] Hydrogenated bisphenol A epoxy resin is a polymer that cannot be directly detected and its content in various samples determined. In the field of caulking agents, many businesses claim that the caulking agents they produce are added with hydrogenated bisphenol A epoxy resin. Since there is no effective method for detecting hydrogenated bisphenol A epoxy resin, the quality of caulking agents cannot be monitored, and consumers cannot be sure of the authenticity of the merchants' propaganda. The method for determining hydrogenated bisphenol A epoxy resin in a sample according to an embodiment of the present invention provides a feasible and accurate method for monitoring the content of hydrogenated bisphenol A epoxy resin in a sample, which adopts thermal pyrolysis-gas chromatography-mass spectrometry (PY-GC-MS) to first crack hydrogenated bisphenol A epoxy resin into hydrogenated bisphenol A, and then perform gas chromatography and mass spectrometry detection on the generated hydrogenated bisphenol A, so that hydrogenated bisphenol A epoxy resin can be determined and its content can be determined.

[0026] In an embodiment of the present invention, a method for determining the content of hydrogenated bisphenol A epoxy resin in a sample comprises using a thermal cracking-gas chromatography-mass spectrometer to determine a hydrogenated bisphenol A epoxy resin standard solution and draw a standard working curve, wherein the hydrogenated bisphenol A epoxy resin in the sample is determined by detecting hydrogenated bisphenol A, and wherein the gas chromatography column is a capillary column chromatographic column filled with (50%-phenyl)-methylpolysiloxane or a capillary column chromatographic column filled with polyethylene glycol; the sample is tested using the same steps as those for determining the hydrogenated bisphenol A epoxy resin standard solution; and the content of hydrogenated bisphenol A epoxy resin in the sample is calculated based on the obtained standard working curve.

[0027] The hydrogenated bisphenol A epoxy resin of the embodiment of the present invention is any hydrogenated bisphenol A epoxy resin known in the art.

[0028] The steps of using a pyrolysis-gas chromatography-mass spectrometer to measure a hydrogenated bisphenol A epoxy resin standard solution and draw a standard working curve include using an organic solvent to configure a hydrogenated bisphenol A epoxy resin standard substance into a series of concentrations of hydrogenated bisphenol A epoxy resin standard solutions; using a pyrolysis-gas chromatography-mass spectrometer to test the obtained standard solution, and then drawing a standard working curve with the chromatographic peak area of ​​the hydrogenated bisphenol A epoxy resin as the ordinate and the concentration of the standard solution as the abscissa; wherein the organic solvent is a highly pure, analytically pure or chromatographically pure organic solvent, generally including one or more of toluene, dichloromethane, chloroform, ether, ethyl acetate, methyl acetate, acetone, and n-propanol, such as ethyl acetate or methyl acetate. The correlation coefficient of the obtained standard working curve can be at least 0.995, thereby configuring the standard solution with an organic solvent to measure a standard working curve with a high correlation coefficient, further improving the accuracy of determining the content of the hydrogenated bisphenol A epoxy resin.

[0029] Optionally, the step of testing the hydrogenated bisphenol A epoxy resin standard solution using a thermal cracking-gas chromatography-mass spectrometer and drawing a standard working curve includes preparing a series of concentrations of hydrogenated bisphenol A epoxy resin standard solutions, for example, using ethyl acetate (chromatographic grade) to dilute the hydrogenated bisphenol A epoxy resin standard substance to a set series of concentrations to obtain hydrogenated bisphenol A epoxy resin standard solutions, for example, standard solutions with concentrations of 400, 600, 800, 1000, and 2000 mg / L; placing the standard solutions of different concentrations in a thermal cracking vessel, testing them using a thermal cracking-gas chromatography-mass spectrometer, and then drawing a standard working curve with the chromatographic peak area of ​​the hydrogenated bisphenol A epoxy resin as the ordinate and the concentration of the standard solution as the abscissa.

[0030] In gas chromatography, the length of the capillary column is 10-60m, the inner diameter is 0.18-0.53mm, and the film thickness is 0.18-0.53μm, for example, the length is 30m, the inner diameter is 0.25mm, and the film thickness is 0.25μm. The capillary column chromatographic column filled with (50%-phenyl)-methylpolysiloxane refers to a capillary column whose filler composition is 50%-phenyl and 50% methylpolysiloxane, such as HP-17 (length 10m, inner diameter 0.53mm, film thickness 2.00μm) and DB-17 (length 30m, inner diameter 0.25mm, film thickness 0.25μm) purchased from Agilent Technologies. The capillary column chromatographic column filled with polyethylene glycol, for example, HP-INNOWax and DB-WAX purchased from Agilent Technologies.

[0031] In gas chromatography, the injection port temperature is 200-240°C, such as 210-230°C, 220°C; the flow rate is 0.8-1.5mL / min, such as 0.8-1.2mL / min, 1mL / min; the injection mode is split injection, the split ratio is (8-15):1, such as (8-11):1, 10:1; the program temperature is used: starting from 90-110°C, the temperature is increased to 260-270°C, such as 270°C, at a heating rate of 5-15°C / min, and maintained for 20-40min, such as 30min. Thus, the hydrogenated bisphenol A epoxy resin and other impurities in the sample can be effectively separated, thereby achieving accurate qualitative and quantitative analysis.

[0032] When the gas chromatographic column is a capillary column filled with (50%-phenyl)-methylpolysiloxane, the retention time of hydrogenated bisphenol A in the gas chromatogram is 15.79-15.99 min, such as 15.791 min, 15.889 min, and 15.982 min. When the gas chromatographic column is a capillary column filled with polyethylene glycol, the retention time of hydrogenated bisphenol A in the gas chromatogram is 30.29-34.19 min, such as 30.299 min, 32.116 min, and 34.185 min.

[0033] The thermal cracking adopts the double-click mode, and the thermal cracking temperature program is: starting from 50-70℃, heating up to 100-130℃ at a heating rate of 20-40℃ / min, maintaining for 0.1-0.3min, and then heating up to 480-520℃ at a heating rate of 30-50℃ / min, maintaining for 0.5-2min. The double-click mode can be used to volatilize the solvent ethyl acetate for dissolving the sample during the thermal cracking process, and then the temperature is increased to crack the hydrogenated bisphenol A epoxy resin.

[0034] In mass spectrometry detection, the transmission line temperature is: 23-270°C; the ion source temperature is: 280-320°C; the acquisition mode is: SCAN∼ the solvent delay time is: 2-5min; the SCAN mode is: 29-600amu; the SIM mode is: quantitative ion (M / Z): 123; the qualitative ion (M / Z): 67, 81, 141.

[0035] The steps of testing the sample by adopting the same steps as those for determining the hydrogenated bisphenol A epoxy resin standard solution and calculating the content of the hydrogenated bisphenol A epoxy resin in the sample according to the obtained standard working curve include fully dissolving the sample with the same organic solvent as that used in the standard solution, such as ethyl acetate, to obtain a sample solution; after optionally filtering the prepared sample solution with hydrophobic polytetrafluoroethylene (PTFE), testing the sample solution by adopting the same steps as those for determining the hydrogenated bisphenol A epoxy resin standard solution, and calculating the content of the hydrogenated bisphenol A epoxy resin in the sample according to the obtained standard working curve.

[0036] Optionally, the sample is tested using the same steps as those for determining the hydrogenated bisphenol A epoxy resin standard solution, and the step of calculating the content of hydrogenated bisphenol A epoxy resin in the sample according to the obtained standard working curve includes fully dissolving the sample with the above-mentioned organic solvent, such as ethyl acetate, to obtain a sample solution; after filtering the prepared sample solution with hydrophobic PTFE, 10-30 μL of the sample solution is aspirated with, for example, a pipette, and the same steps as those for determining the hydrogenated bisphenol A epoxy resin standard solution are used for testing, and the retention time and the qualitative ion are used for qualitative determination, and the quantitative ion peak area is measured for quantitative determination.

[0037] Hydrogenated bisphenol A epoxy resin content:

[0038] X—the content of hydrogenated bisphenol A epoxy resin in the sample, in %;

[0039] C—Concentration of hydrogenated bisphenol A epoxy resin read on the standard curve, in milligrams per liter (mg / L);

[0040] V—fixed volume, 10mL;

[0041] F—dilution factor, 1;

[0042] m—sample mass, in grams (g);

[0043] 10000—Conversion factor.

[0044] In an embodiment of the present invention, the above method for determining hydrogenated bisphenol A epoxy resin in a sample can be used to determine hydrogenated bisphenol A epoxy resin in a seam-beautifying agent and to determine its content in the seam-beautifying agent.

[0045] Those skilled in the art should understand that the method of the embodiment of the present invention is applicable to any field requiring qualitative and quantitative analysis of hydrogenated bisphenol A epoxy resin, such as outdoor coatings, indoor coatings, adhesives, etc.

[0046] The present invention is described below by specific examples. The examples described below are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention. If no specific techniques or conditions are specified in the examples, the techniques or conditions described in the literature in this area or the product instructions are used. If the manufacturer of the reagents or instruments is not specified, they are all conventional products that can be obtained commercially.

[0047] Seam beautifier

[0048] The epoxy resin (model CYD-128, purchased from Baling Petrochemical), hydrogenated bisphenol A epoxy resin (model XYH001, purchased from Hubei Xinyuhong Biomedical Technology Co., Ltd.), and curing agent (model R-3609H, purchased from Rich Chemical) were fully mixed at a weight ratio of 50:5:45 to obtain a test seam beautifying agent. The content of hydrogenated bisphenol A epoxy resin was 5%.

[0049] Example 1

[0050] 1. Parameter setting of pyrolysis-gas chromatography-mass spectrometry

[0051] Pyrolysis parameters: double click mode

[0052]

[0053] Gas chromatography parameters: The model of the capillary column is HP-INNOWax, purchased from Agilent Technologies, with a length of 30 m, an inner diameter of 0.25 mm, a film thickness of 0.25 μm, and a filler of polyethylene glycol; injection port temperature: 220 °C; flow rate: 1 mL / min; injection mode: split injection, split ratio: 10:1; programmed temperature was used according to the following parameters:

[0054]

[0055] Mass spectrometry parameters: transfer line temperature: 250°C; ion source temperature: 300°C; acquisition mode: SCAN∼ solvent delay time: 4 min; SCAN mode: 29-600 amu; SIM mode: quantitative ion (M / Z): 123; qualitative ion (M / Z): 67, 81, 141;

[0056] 2. Standard working curve

[0057] Accurately weigh 0.5g of hydrogenated bisphenol A epoxy resin standard substance, dilute to 25mL with ethyl acetate, and prepare a standard stock solution with a concentration of 20000mg / L. Use graduated pipettes of different ranges to draw a certain amount of standard stock solution into a volumetric flask, and then add ethyl acetate to prepare standard solutions with concentrations of 400, 600, 800, 1000, and 2000mg / L.

[0058] 20 μL of standard solutions of different concentrations were taken and placed in a pyrolysis vessel for pyrolysis-gas chromatography-mass spectrometry detection. The standard working curve was drawn with the chromatographic peak area of ​​hydrogenated bisphenol A epoxy resin as the ordinate and the concentration of the standard solution as the abscissa. The curve equation was: Y = 1.5993X-35.8278, and the correlation coefficient R 2 =0.999, where X is the concentration and Y is the chromatographic peak area.

[0059] 3. Sample solution test

[0060] Weigh 0.2544 g of the sample into a 10 mL volumetric flask, dissolve it in ethyl acetate and make up to volume, and ultrasonicate for 10 minutes to obtain a sample solution.

[0061] The solution was transferred with a 1 mL syringe, filtered with hydrophobic PTFE, and 20 μL of the sample solution was drawn onto a sample cup with a pipette. The sample was tested by thermal pyrolysis-gas chromatography-mass spectrometry, and the peak area of ​​the sample was 1954.981. The concentration of hydrogenated bisphenol A epoxy resin was 1244.8 mg / L from the standard working curve.

[0062] According to the following formula

[0063]

[0064] The calculated content of hydrogenated bisphenol A epoxy resin in the sample was 4.89%, which was in line with expectations.

[0065] like Figure 1 As shown in the figure, the retention times of the three isomers of hydrogenated bisphenol A in the gas chromatogram are 30.299min, 32.116min, and 34.185min, respectively. The separation between the three peaks is 8.86 and 8.91, which is much greater than 1.5. The components are completely separated. The greater the separation, the better the separation effect of the two adjacent peaks. In general, when the separation is 1.5, it can be considered that the two adjacent components are completely separated.

[0066] Figure 2 The mass spectrum of hydrogenated bisphenol A, a cleavage product of hydrogenated epoxy resin, is shown, wherein the abscissa is the mass-to-charge ratio (M / Z value) and the ordinate is the ion intensity.

[0067] Example 2

[0068] The steps of Example 1 were repeated, except that:

[0069] The gas chromatography column was replaced with a DB-17 column (purchased from Agilent Technologies) filled with (50%-phenyl)-methylpolysiloxane, 30 m in length, 0.25 mm in inner diameter, and 0.25 μm in film thickness; the obtained standard working curve was Y=1.4735X-30.7583, with a correlation coefficient R 2 =0.995;

[0070] 0.2512 g of the caulking agent sample was weighed, and the peak area of ​​the sample was 1730.427. The concentration of hydrogenated bisphenol A epoxy resin was obtained from the standard working curve to be 1195.2 mg / L. The hydrogenated bisphenol A epoxy resin content was calculated to be 4.76%, which was in line with expectations.

[0071] like Figure 3 The retention times of the three isomers of hydrogenated bisphenol A in the gas chromatogram shown are 15.791 min, 15.889 min, and 15.982 min, and the separation degrees between the three peaks are: 1.51 and 1.48, which are basically equivalent to 1.5, and the components are basically completely separated.

[0072] Comparative Example 1

[0073] The steps of Example 1 were repeated, except that:

[0074] The gas chromatography column was replaced with a chromatographic column Ultra 2 (purchased from Agilent Technologies) filled with (5%-phenyl)-methylpolysiloxane, with a length of 25 m, an inner diameter of 0.20 mm, and a film thickness of 0.33 μm; the obtained standard working curve was Y=1.3121X-28.9932, and the correlation coefficient R2 =0.989, and its correlation coefficient is lower than 0.995.

[0075] 0.2574 g of the caulking agent sample was weighed, and the peak area of ​​the sample was 1342.863. The concentration of hydrogenated bisphenol A epoxy resin was obtained from the standard working curve to be 1045.5 mg / L. The content of hydrogenated bisphenol A epoxy resin in the sample was calculated to be 4.06%, which was quite different from the actual content.

[0076] like Figure 4 The retention times of the three isomers of hydrogenated bisphenol A in the gas chromatogram shown are 13.462 min, 13.610 min, and 13.745 min, and the separation degrees between the peaks are: 1.70 and 1.72, which are basically equivalent to 1.5, and the components are basically completely separated.

[0077] Comparative Example 2

[0078] The steps of Example 1 were repeated, except that:

[0079] The gas chromatography column was replaced with a chromatographic column DB-1 (purchased from Agilent Technologies) filled with 100% methyl polysiloxane, with a length of 30 m, an inner diameter of 0.25 mm, and a film thickness of 0.25 μm; the obtained standard working curve was Y=1.3027X-28.2547, and the correlation coefficient R 2 =0.987, and its correlation coefficient is lower than 0.995.

[0080] 0.2526 g of the caulking agent sample was weighed, and the peak area of ​​the sample was 1248.456. The concentration of hydrogenated bisphenol A epoxy resin was obtained from the standard working curve to be 980.0 mg / L. The content of hydrogenated bisphenol A epoxy resin in the sample was calculated to be 3.88%, which was quite different from the actual content.

[0081] like Figure 5 The retention times of the three isomers of hydrogenated bisphenol A in the gas chromatogram shown are 15.142 min, 15.188 min, and 15.235 min, and the separation degrees between the peaks are: 1.45 and 1.57, which are basically equivalent to 1.5, and the components are basically completely separated.

[0082] Although Comparative Example 1-2 can completely separate the three isomers of hydrogenated bisphenol A, the correlation coefficient of the standard working curve obtained is small, and the content of the obtained hydrogenated bisphenol A epoxy resin is greatly different from the actual content.

[0083] According to the technical solution of the embodiment of the present invention, the method of the present invention can completely distinguish the isomers of hydrogenated bisphenol A, and the correlation coefficient of the obtained standard working curve is at least 0.995, thereby enabling accurate quantitative analysis of hydrogenated bisphenol A epoxy resin.

[0084] The above specific implementations do not constitute a limitation on the protection scope of the present invention. It should be understood by those skilled in the art that various modifications, combinations, sub-combinations and substitutions may occur depending on design requirements and other factors. Any modification, equivalent substitution and improvement made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for determining the content of hydrogenated bisphenol A epoxy resin in a sample, It is characterized in that The method comprises adopting a pyrolysis-gas chromatography-mass spectrometer to determine a hydrogenated bisphenol A epoxy resin standard solution and draw a standard working curve, wherein the hydrogenated bisphenol A epoxy resin in a sample is determined by detecting hydrogenated bisphenol A, and wherein the gas chromatography column is a capillary column chromatographic column filled with (50%-phenyl)-methyl polysiloxane or a capillary column chromatographic column filled with polyethylene glycol; the sample is tested by adopting the same steps as those for determining the hydrogenated bisphenol A epoxy resin standard solution; and the content of the hydrogenated bisphenol A epoxy resin in the sample is calculated according to the obtained standard working curve.

2. The method according to claim 1, It is characterized in that The correlation coefficient of the obtained standard working curve was at least 0.

995.

3. The method according to claim 1 or 2, It is characterized in that In the gas chromatography, the capillary chromatographic column has a length of 10-60m, an inner diameter of 0.18-0.53mm, and a film thickness of 0.18-0.53μm; wherein the gas chromatographic column is a capillary column chromatographic column whose filler is polyethylene glycol.

4. The method according to claim 1 or 2, It is characterized in that The gas chromatograph has an injection port temperature of 200-240°C, a flow rate of 0.8-1.5 mL / min, an injection mode of split injection, and a split ratio of (8-15):

1. The temperature is programmed to rise from 90-110°C to 260-270°C at a heating rate of 5-15°C / min and maintained for 20-40 minutes.

5. The method according to claim 1 or 2, It is characterized in that The thermal cracking adopts a double-click mode, and the thermal cracking heating program is: starting from 50-70°C, heating to 100-130°C at a heating rate of 20-40°C / min, maintaining for 0.1-0.3min, and then heating to 480-520°C at a heating rate of 30-50°C / min, maintaining for 0.5-2min.

6. The method according to claim 1 or 2, It is characterized in that In the mass spectrometry detection, the transmission line temperature is: 23-270°C; the ion source temperature is: 280-320°C; the acquisition mode is: SCAN∼ and the solvent delay time is: 2-5min.

7. The method according to claim 1 or 2, It is characterized in that When the gas chromatography column is a capillary column whose filler is (50%-phenyl)-methylpolysiloxane, in the gas chromatogram, the retention time of hydrogenated bisphenol A is 15.79-15.99 min.

8. The method according to claim 1 or 2, It is characterized in that When the gas chromatography column is a capillary column whose filler is polyethylene glycol, in the gas chromatogram, the retention time of hydrogenated bisphenol A is 30.29-34.19 min.

9. The method according to claim 1 or 2, It is characterized in that The steps of using a pyrolysis-gas chromatography-mass spectrometer to measure a hydrogenated bisphenol A epoxy resin standard solution and draw a standard working curve include using an organic solvent to configure a hydrogenated bisphenol A epoxy resin standard substance into a series of hydrogenated bisphenol A epoxy resin standard solutions of concentration; using a pyrolysis-gas chromatography-mass spectrometer to test the obtained standard solution, and then drawing a standard working curve with the chromatographic peak area of ​​the hydrogenated bisphenol A epoxy resin as the ordinate and the concentration of the standard solution as the abscissa; wherein the organic solvent includes one or more of toluene, dichloromethane, chloroform, ether, ethyl acetate, methyl acetate, acetone, and n-propanol.

10. The method according to any one of claims 1 to 9 is used to determine the use of hydrogenated bisphenol A epoxy resin in a seam beauty agent.

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