Method for detecting purity of high polymer material plasticizer lauryl octanoate

Abstract

The invention discloses a method for detecting the purity of a polymer material plasticizer lauryl octanoate, which comprises the following steps: firstly, extracting the plasticizer lauryl octanoate by using tetrahydrofuran to obtain a liquid to be detected; then detecting the to-be-detected liquid according to liquid chromatogram detection conditions, and obtaining a chromatogram by taking time as a horizontal coordinate and an instrument detection electric signal as a vertical coordinate; and finally, calculating the purity of the plasticizer lauryl octanoate in the liquid to be detected according to the following formula: X2: # imgabs0 #, wherein At is the average value of the peak area of the plasticizer lauryl octanoate in the sample; ai is the value of the peak area of all components in the sample. According to the detection method disclosed by the invention, the plasticizer lauryl octanoate is extracted by utilizing tetrahydrofuran, so that the purity of the plasticizer lauryl octanoate can be rapidly detected, and the detection accuracy is high.

Description

Technical Field

[0001] The invention belongs to the technical field of effective component detection in polymer materials, and relates to a method for detecting the purity of lauryl octanoate, a plasticizer in polymer materials. Background Art

[0002] There are currently no publicly published literature on the purity analysis method of the plasticizer lauryl octanoate in China. The high viscosity and insoluble properties of the polymer plasticizer lauryl octanoate make it poorly soluble in acetone and ethanol. The sample will precipitate at the column head, affecting purification and separation. This patent studies the analysis method for this. Summary of the invention

[0003] The purpose of the invention is to provide a method for detecting the purity of lauryl octanoate, a polymer material plasticizer, so as to improve the detection accuracy of the plasticizer lauryl octanoate.

[0004] The objective of the present invention is achieved through the following technical solutions:

[0005] The present invention provides a method for detecting the purity of lauryl octanoate, a polymer material plasticizer, comprising the following steps:

[0006] 1) extracting the plasticizer lauryl octanoate using tetrahydrofuran to obtain a test solution;

[0007] 2) The liquid to be tested is tested according to the liquid chromatography detection conditions, with time as the horizontal axis and the instrument detection electrical signal as the vertical axis, to obtain the chromatogram.

[0008] 3) Calculate the purity X2 of the plasticizer lauryl octanoate in the test solution in terms of mass fraction according to the following formula;

[0009]

[0010] Where:

[0011] A t ——The average value of the peak area of ​​plasticizer lauryl octanoate in the sample;

[0012] A i ——The numerical value of the peak area of ​​all components in the sample.

[0013] Preferably, the extraction operation in step 1) is ultrasonic extraction, the frequency of the ultrasonic extraction is (15-25) MHz, and the time of the ultrasonic extraction is preferably 60-90 min.

[0014] Preferably, the liquid chromatography detection conditions include: the solvent and mobile phase are tetrahydrofuran; the elution method is isocratic elution; the column temperature is 30°C; the detector is an ultraviolet detector; the detection wavelength is 210nm; the chromatographic column for liquid chromatography detection is C 18 column; the injection volume of the liquid chromatography detection is 25 μL; the flow rate of the mobile phase is 0.5 mL / min.

[0015] Preferably, the volume ratio of the plasticizer lauryl octanoate to tetrahydrofuran is 1 mL:29 mL.

[0016] Beneficial Effects

[0017] The detection method of the invention can realize rapid detection of the purity of the plasticizer lauryl octanoate by using tetrahydrofuran to extract the plasticizer lauryl octanoate, and has high detection accuracy. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is a liquid chromatography detection chart of the test liquid obtained in step 2) of the embodiment. DETAILED DESCRIPTION

[0019] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0020] Example

[0021] The present invention provides a method for detecting the purity of lauryl octanoate, a polymer material plasticizer, comprising the following steps:

[0022] 1) Measure 1 mL ± 0.1 mL of the plasticizer lauryl octanoate into a 30 mL volumetric flask to obtain a sample to be tested;

[0023] 2) The sample to be tested is diluted to the mark with tetrahydrofuran solvent and then shaken to obtain a test solution for liquid chromatography testing. The obtained test solution is filtered through a 0.45 μm microporous filter membrane, and then the obtained test solution is tested using an Agilent 1260Ⅱ liquid chromatograph according to the detection conditions of liquid chromatography to obtain a chromatogram of the plasticizer lauryl octanoate.

[0024] 3) The liquid to be tested is tested according to the liquid chromatography detection conditions, with time as the horizontal axis and the instrument detection electrical signal as the vertical axis, to obtain a liquid chromatography detection graph of the liquid to be tested, such as Figure 1 shown.

[0025] The liquid chromatography detection conditions include: the solvent and mobile phase are tetrahydrofuran; the elution method is isocratic elution; the column temperature is 30°C; the detector is an ultraviolet detector; and the detection wavelength is 210nm. The chromatographic column for liquid chromatography detection is C 18The injection volume of the liquid chromatography detection is 25 μL. The flow rate of the mobile phase is 0.5 mL / min.

[0026] The volume ratio of the plasticizer lauryl octanoate to tetrahydrofuran is 1 mL:29 mL.

[0027] 4) Calculate the purity X2 of the plasticizer lauryl octanoate in the test solution in terms of mass fraction according to the following formula;

[0028]

[0029] Where:

[0030] A t ——The average value of the peak area of ​​plasticizer lauryl octanoate in the sample;

[0031] A i ——The numerical value of the peak area of ​​all components in the sample.

[0032] According to the liquid chromatography detection chart of the test liquid, a peak appears at a retention time of 5.32667 min, the peak area (mV.sec): 6937.63, and the integrated area of ​​the peak is 100%. It can be considered that the purity of the sample is 100%.

[0033] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for detecting the purity of lauryl octanoate, a polymer plasticizer, characterized in that: The following steps are involved: 1) extracting the plasticizer lauryl octanoate using tetrahydrofuran to obtain a test solution; 2) detecting the liquid to be tested according to the liquid chromatography detection conditions, with time as the horizontal axis and the instrument detection electrical signal as the vertical axis, to obtain the chromatogram; 3) Calculate the purity X2 of the plasticizer lauryl octanoate in the test solution in terms of mass fraction according to the following formula; Where: A t ——The average value of the peak area of ​​plasticizer lauryl octanoate in the sample; A i ——The numerical value of the peak area of ​​all components in the sample.

2. A method for detecting the purity of lauryl octanoate, a polymer plasticizer, as claimed in claim 1, characterized in that: The extraction operation in step 1) is ultrasonic extraction, the frequency of the ultrasonic extraction is 15-25 MHz, and the time of the ultrasonic extraction is preferably 60-90 min.

3. A method for detecting the purity of lauryl octanoate, a polymer plasticizer, as claimed in claim 1, characterized in that: The liquid chromatography detection conditions include: the solvent and mobile phase are tetrahydrofuran; the elution method is isocratic elution; the column temperature is 30°C; the detector is an ultraviolet detector; the detection wavelength is 210nm; the chromatographic column for liquid chromatography detection is C 18 column; the injection volume of the liquid chromatography detection is 25 μL; the flow rate of the mobile phase is 0.5 mL / min.

4. A method for detecting the purity of lauryl octanoate, a polymer plasticizer, as claimed in claim 1, characterized in that: The volume ratio of the plasticizer lauryl octanoate to tetrahydrofuran is 1 mL:29 mL.

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