Method for determining content of bis (2-ethylhexyl) adipate in liquid paraffin

Abstract

The invention discloses a method for measuring the content of bis (2-ethylhexyl) adipate in liquid paraffin, which comprises the following steps: firstly, preparing a group of standard solutions with different mass concentrations, and respectively carrying out gas chromatography test on each standard solution by adopting a gas chromatography method; drawing a standard working curve corresponding to each standard solution by taking the mass concentration of the standard solution as an abscissa and the quantitative chromatographic peak area as an ordinate; and carrying out gas chromatography test on the sample solution to be tested, substituting the measured quantitative chromatographic peak area into the standard working curve, taking the mass concentration of the corresponding standard solution as the mass concentration of the sample solution to be tested, and combining with the mass of the added sample to be tested to obtain the content of bis (2-ethylhexyl) adipate in the liquid paraffin. According to the determination method disclosed by the invention, the content of the bis (2-ethylhexyl) adipate in the liquid paraffin can be rapidly and accurately determined.

Description

Technical Field

[0001] The invention relates to a method for determining the content of di(2-ethylhexyl) adipate in liquid paraffin, belonging to the technical field of gas chromatography analysis. Background Art

[0002] Bis(2-ethylhexyl) adipate is a widely used plasticizer, and long-term use will have adverse effects on the ecological environment and human life. Therefore, it is very necessary to establish a fast, simple and accurate method for determining bis(2-ethylhexyl) adipate. Currently, there is no method specifically for the content of bis(2-ethylhexyl) adipate in liquid paraffin on the market, and this patent studies this. Summary of the invention

[0003] The purpose of the invention is to solve the problem that the prior art cannot measure the content of di(2-ethylhexyl)adipate in liquid paraffin, and to provide a method for measuring the content of di(2-ethylhexyl)adipate in liquid paraffin.

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

[0005] A method for measuring the content of bis(2-ethylhexyl) adipate in liquid paraffin of the present invention, the specific measuring method is as follows:

[0006] 1) Select different masses of bis(2-ethylhexyl) adipate standard solutions, dilute them to the test volume with ethyl acetate, and obtain a set of standard solutions with different mass concentrations;

[0007] 2) using a gas chromatography method to perform gas chromatography tests on each portion of the standard solution with different mass concentrations, and obtaining a gas chromatography test graph of each standard solution;

[0008] 3) Using the mass concentration of the standard solution as the abscissa and the quantitative chromatographic peak area as the ordinate, draw a standard working curve corresponding to each standard solution;

[0009] 4) diluting the liquid paraffin to be tested with ethyl acetate to a test volume to obtain a sample solution to be tested;

[0010] 5) Performing a gas chromatography test on the sample solution to be tested by a gas chromatography method to obtain a gas chromatography test graph of the sample solution to be tested, substituting the quantitative chromatographic peak area of ​​the test graph into the standard working curve, the mass concentration of the corresponding standard solution is the mass concentration of the sample solution to be tested, and combining the mass of the added sample to be tested to obtain the content of di(2-ethylhexyl) adipate in liquid paraffin.

[0011] The test conditions of the gas chromatography method are as follows: a WondaCap 1701 chromatographic column with a size of 30 m×0.25 mm×0.25 μm; a carrier gas of high-purity nitrogen with a purity of >99.999%; a flow rate of 1.0 mL / min, split injection, a split ratio of 50:1, an injection volume of 1.0 μL, and an injection port temperature of 250° C.

[0012] The column temperature program of the gas chromatography method is as follows: initial temperature 90°C, maintained for 2 minutes; increased to 170°C at a rate of 10°C / min; then increased to 200°C at a rate of 8°C / min; continued to increase to 280°C at a rate of 15°C / min and maintained for 10 minutes. The detector temperature is 280°C.

[0013] Beneficial Effects

[0014] The determination method of the invention can realize the rapid and accurate determination of the content of di(2-ethylhexyl) adipate in liquid paraffin, the sample solution preparation process is simple, and no interference is generated in the determination process; the determination method of the invention has broad application prospects in the field of material analysis. DETAILED DESCRIPTION

[0015] The present invention will be further described below in conjunction with the embodiments.

[0016] Example

[0017] A method for measuring the content of bis(2-ethylhexyl) adipate in liquid paraffin, the specific measuring method is as follows:

[0018] 1) Select different masses of bis(2-ethylhexyl) adipate standard solutions, dilute them to the test volume with ethyl acetate, and obtain a set of standard solutions with different mass concentrations;

[0019] 2) using a gas chromatography method to perform gas chromatography tests on each portion of the standard solution with different mass concentrations, and obtaining a gas chromatography test graph of each standard solution;

[0020] 3) Using the mass concentration of the standard solution as the abscissa and the quantitative chromatographic peak area as the ordinate, draw a standard working curve corresponding to each standard solution;

[0021] 4) Weigh the test sample into a 100 mL volumetric flask and dilute the test sample with ethyl acetate to the test volume to obtain a test sample solution;

[0022] 5) The sample solutions to be tested are respectively subjected to gas chromatography tests by gas chromatography method to obtain gas chromatography test graphs of the sample solutions to be tested, and the quantitative chromatographic peak area of ​​the test graph is brought into the standard working curve, and the mass concentration of the corresponding standard solution is the mass concentration of the sample solution to be tested. Combined with the mass of the added sample to be tested, the content of di(2-ethylhexyl) adipate in liquid paraffin can be obtained.

[0023] Test conditions: WondaCap 1701 chromatographic column (30m×0.25mm×0.25μm), carrier gas is high-purity nitrogen (>99.999%), flow rate 1.0mL / min, split injection, split ratio 50:1, injection volume 1.0μL, injection port temperature 250℃, column temperature program: initial temperature 90℃, hold for 2min; increase to 170℃ at a rate of 10℃ / min; then increase to 200℃ at a rate of 8℃ / min; continue to increase to 280℃ at a rate of 15℃ / min and hold for 10min. Detector temperature 280℃.

Claims

1. A method for determining the content of bis(2-ethylhexyl) adipate in liquid paraffin, characterized in that: The specific determination method is as follows: 1) Select different masses of bis(2-ethylhexyl) adipate standard solutions, dilute them to the test volume with ethyl acetate, and obtain a set of standard solutions with different mass concentrations; 2) using a gas chromatography method to perform gas chromatography tests on each portion of the standard solution with different mass concentrations, and obtaining a gas chromatography test graph of each standard solution; 3) Using the mass concentration of the standard solution as the abscissa and the quantitative chromatographic peak area as the ordinate, draw a standard working curve corresponding to each standard solution; 4) diluting the liquid paraffin to be tested with ethyl acetate to a test volume to obtain a sample solution to be tested; 5) Performing a gas chromatography test on the sample solution to be tested by a gas chromatography method to obtain a gas chromatography test graph of the sample solution to be tested, substituting the quantitative chromatographic peak area of ​​the test graph into the standard working curve, the mass concentration of the corresponding standard solution is the mass concentration of the sample solution to be tested, and combining the mass of the added sample to be tested to obtain the content of di(2-ethylhexyl) adipate in liquid paraffin.

2. A method for determining the content of bis(2-ethylhexyl) adipate in liquid paraffin according to claim 1, characterized in that: The test conditions of the gas chromatography method are as follows: a WondaCap 1701 chromatographic column with a size of 30 m×0.25 mm×0.25 μm; a carrier gas of high-purity nitrogen with a purity of >99.999%; a flow rate of 1.0 mL / min, split injection, a split ratio of 50:1, an injection volume of 1.0 μL, and an injection port temperature of 250° C. The column temperature program of the gas chromatography method is as follows: initial temperature 90°C, maintained for 2 minutes; increased to 170°C at a rate of 10°C / min; then increased to 200°C at a rate of 8°C / min; continued to increase to 280°C at a rate of 15°C / min and maintained for 10 minutes. The detector temperature is 280°C.