Detection method of No. 120 solvent oil in light stabilizer-123
阅读说明：本技术 一种光稳定剂-123中120号溶剂油的检测方法 (Detection method of No. 120 solvent oil in light stabilizer-123 ) 是由 郭强 贺佩 贾志军 于 2021-08-20 设计创作，主要内容包括：本发明属于物质分析检测技术领域,提供了一种光稳定剂-123中120号溶剂油的检测方法。本发明对所述不同浓度的系列120号溶剂油标准溶液进行红外扫描,筛选出特征红外波段；将系列120号溶剂油标准溶液的吸光度与浓度进行拟合,得到系列模型；以相关系数最大的模型为检测模型；将待测光稳定剂-123分馏,得到待测120号溶剂油；对所述待测120号溶剂油进行红外扫描,将所述待测120号溶剂油的红外信息代入检测模型中。本发明的检测方法的结果与气相色谱法检测结果偏差值在±0.02％之间,表明了本发明提供的检测方法重复性好、准确度高、操作简便快速高效,分析结果对光稳定剂在生产过程中质量控制有明显的指导意义。(The invention belongs to the technical field of substance analysis and detection, and provides a method for detecting No. 120 solvent oil in a light stabilizer-123. The invention carries out infrared scanning on the serial No. 120 solvent oil standard solutions with different concentrations to screen out a characteristic infrared band; fitting the absorbance and concentration of the serial No. 120 solvent oil standard solution to obtain a serial model; taking the model with the maximum correlation coefficient as a detection model; fractionating the light stabilizer-123 to be detected to obtain No. 120 solvent oil to be detected; and carrying out infrared scanning on the No. 120 solvent oil to be detected, and substituting the infrared information of the No. 120 solvent oil to be detected into a detection model. The deviation value of the result of the detection method and the detection result of the gas chromatography is +/-0.02%, which shows that the detection method provided by the invention has good repeatability, high accuracy, simple, convenient, rapid and efficient operation, and the analysis result has obvious guiding significance for the quality control of the light stabilizer in the production process.)
1. A detection method of No. 120 solvent oil in a light stabilizer-123 is characterized by comprising the following steps:
preparing a No. 120 solvent oil standard sample into a series of No. 120 solvent oil standard solutions with different concentrations;
carrying out infrared scanning on the serial No. 120 solvent oil standard solutions with different concentrations to screen out a characteristic infrared band;
carrying out linear fitting on the absorbance and the concentration of the characteristic infrared band of the serial No. 120 solvent oil standard solutions with different concentrations to obtain a serial model; selecting a model with the maximum correlation coefficient as a detection model;
fractionating light stabilizer-123 to be detected to obtain No. 120 solvent naphtha to be detected;
and carrying out infrared scanning on the No. 120 solvent oil to be detected, and substituting the infrared information of the No. 120 solvent oil to be detected into the detection model to obtain the content of the No. 120 solvent oil in the light stabilizer-123 to be detected.
2. The detection method according to claim 1, wherein the concentration of the series of No. 120 solvent oil standard solutions is 4mg/kg, 8mg/kg, 10mg/kg, 20mg/kg and 50mg/kg respectively.
3. The assay of claim 1 or 2, wherein the solvent formulated into a series of 120-gauge solvent oil standard solutions of varying concentrations is toluene.
4. The detection method according to claim 1, wherein the range of the infrared scan is 600cm-1～4000cm-1。
5. The detection method according to claim 1, wherein the principle of screening out the characteristic infrared band is as follows: the absorbance value of the infrared band is more than or equal to 0.1A.
6. The detection method according to claim 1, wherein the correlation coefficient of the detection model is not less than 0.999.
7. The detection method according to claim 1, wherein the temperature of the fractionation is 100 to 150 ℃.
8. The detection method according to claim 1 or 7, wherein the fractionation is performed under a stirring condition, and the rotation speed of the stirring is 20 to 40 rpm.
9. The detection method according to claim 1, wherein the process of substituting the infrared information of the number 120 solvent oil to be detected into the detection model to obtain the content of the number 120 solvent oil in the light stabilizer-123 to be detected comprises the following steps:
opening Spectrum Quant Beer's Law quantitative software, and calling out the detection model; and opening the infrared information of the No. 120 solvent oil to be detected, and clicking quant to obtain the content of the No. 120 solvent oil in the light stabilizer-123 to be detected.
Technical Field
The invention relates to the technical field of substance analysis and detection, in particular to a method for detecting No. 120 solvent oil in a light stabilizer-123.
Background
The light stabilizer-123 is produced by using 2,2,6, 6-tetramethyl piperidinol as main material and through oxidation, free radical and ester exchange reaction. A small amount of No. 120 solvent oil is added during the preparation of the light stabilizer-123, so that a finished product generated after the reaction contains a small amount of No. 120 solvent oil, the No. 120 solvent oil needs to be recycled by a fractionation method, and the influence on the subsequent processes is reduced. The residual No. 120 solvent oil in the light stabilizer-123 can affect the performance of the light stabilizer-123. The current industry common detection and analysis method is a gas chromatography method. However, the analysis of No. 120 solvent oil in the light stabilizer by gas chromatography has the following defects: firstly, the detection time for determining the content of the solvent oil is long, the time is consumed for about 1 hour, hysteresis exists, and the requirement for guiding industrial production cannot be met; secondly, a gas chromatography instrument is required to be used in the experimental process, so that the cost is too high.
Therefore, establishing a method for detecting the content of the solvent oil in the light stabilizer, which is simple and rapid to operate, becomes an urgent research topic to be overcome in the detection and analysis of the residual solvent oil in the light stabilizer.
Disclosure of Invention
In view of the above, the invention aims to provide a method for detecting No. 120 solvent oil in a light stabilizer-123. The detection method provided by the invention is simple to operate and high in accuracy.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for detecting No. 120 solvent oil in a light stabilizer-123, which comprises the following steps:
preparing a No. 120 solvent oil standard sample into a series of No. 120 solvent oil standard solutions with different concentrations;
carrying out infrared scanning on the serial No. 120 solvent oil standard solutions with different concentrations to screen out a characteristic infrared band;
carrying out linear fitting on the absorbance and the concentration of the characteristic infrared band of the serial No. 120 solvent oil standard solutions with different concentrations to obtain a serial model; selecting a model with the maximum correlation coefficient as a detection model;
fractionating light stabilizer-123 to be detected to obtain No. 120 solvent naphtha to be detected;
and carrying out infrared scanning on the No. 120 solvent oil to be detected, and substituting the infrared information of the No. 120 solvent oil to be detected into the detection model to obtain the content of the No. 120 solvent oil in the light stabilizer-123 to be detected.
Preferably, the concentration of the series 120 solvent oil standard solution is 4mg/kg, 8mg/kg, 10mg/kg, 20mg/kg and 50mg/kg respectively.
Preferably, the solvent formulated into the series of 120 # mineral spirit standard solutions of varying concentrations is toluene.
Preferably, the range of the infrared scan is 600cm-1～4000cm-1。
Preferably, the principle of screening out the characteristic infrared band is as follows: the absorbance value of the infrared band is more than or equal to 0.1A.
Preferably, the correlation coefficient of the detection model is more than or equal to 0.999.
Preferably, the temperature of the fractionation is 100 to 150 ℃.
Preferably, the fractionation is carried out under the condition of stirring, and the rotating speed of the stirring is 20-40 rpm.
Preferably, the process of substituting the infrared information of the number 120 solvent oil to be detected into the detection model to obtain the content of the number 120 solvent oil in the light stabilizer-123 to be detected comprises the following steps:
opening Spectrum Quant Beer's Law quantitative software, and calling out the detection model; and opening the infrared information of the No. 120 solvent oil to be detected, and clicking quant to obtain the content of the No. 120 solvent oil in the light stabilizer-123 to be detected.
The invention provides a method for detecting No. 120 solvent oil in a light stabilizer-123, which comprises the following steps: preparing a No. 120 solvent oil standard sample into a series of No. 120 solvent oil standard solutions with different concentrations; carrying out infrared scanning on the serial No. 120 solvent oil standard solutions with different concentrations to screen out a characteristic infrared band; carrying out linear fitting on the absorbance and the concentration of the characteristic infrared band of the serial No. 120 solvent oil standard solutions with different concentrations to obtain a serial model; selecting a model with the maximum correlation coefficient as a detection model; fractionating light stabilizer-123 to be detected to obtain No. 120 solvent naphtha to be detected; and carrying out infrared scanning on the No. 120 solvent oil to be detected, and substituting the infrared information of the No. 120 solvent oil to be detected into the detection model to obtain the content of the No. 120 solvent oil in the light stabilizer-123 to be detected.
The deviation value of the detection result of the detection method provided by the invention and the detection result of the gas chromatography is +/-0.02%, the feasibility of the method is further verified, the detection method provided by the invention is good in repeatability, high in accuracy, simple, convenient, rapid and efficient to operate, and the analysis result has obvious guiding significance for quality control of the light stabilizer in the production process.
Detailed Description
The invention provides a method for detecting No. 120 solvent oil in a light stabilizer-123, which comprises the following steps:
preparing a No. 120 solvent oil standard sample into a series of No. 120 solvent oil standard solutions with different concentrations;
carrying out infrared scanning on the serial No. 120 solvent oil standard solutions with different concentrations to screen out a characteristic infrared band;
carrying out linear fitting on the absorbance and the concentration of the characteristic infrared band of the serial No. 120 solvent oil standard solutions with different concentrations to obtain a serial model; selecting a model with the maximum correlation coefficient as a detection model;
fractionating light stabilizer-123 to be detected to obtain No. 120 solvent naphtha to be detected;
and carrying out infrared scanning on the No. 120 solvent oil to be detected, and substituting the infrared information of the No. 120 solvent oil to be detected into the detection model to obtain the content of the No. 120 solvent oil in the light stabilizer-123 to be detected.
The invention prepares the No. 120 solvent oil standard sample into the series No. 120 solvent oil standard solution with different concentrations.
In the present invention, the solvent formulated into the series of 120 # solvent oil standard solutions of different concentrations is preferably toluene. In the invention, the concentration of the serial No. 120 solvent oil standard solution is 4mg/kg, 8mg/kg, 10mg/kg, 20mg/kg and 50mg/kg respectively. The preparation method of the series No. 120 solvent oil standard solution is not particularly limited, and a mixed solution preparation method known to a person skilled in the art can be adopted.
After series No. 120 solvent oil standard solutions with different concentrations are obtained, the infrared scanning method carries out infrared scanning on the series No. 120 solvent oil standard solutions with different concentrations, and a characteristic infrared band is screened out.
In the present invention, theThe infrared scanning method is preferably an ATR method, and the range of the infrared scanning is preferably 600cm-1～4000cm-1. In the present invention, the principle of screening out the characteristic infrared band is preferably: the absorbance value of the infrared band is more than or equal to 0.1A.
After a specific characteristic infrared band is screened out, carrying out linear fitting on the absorbance and the concentration of the characteristic infrared band of the serial No. 120 solvent oil standard solution with different concentrations to obtain a serial model; and selecting the model with the maximum correlation coefficient as the detection model.
In the invention, a plurality of peaks with high absorbance values may exist in the characteristic infrared band, and preferably, the plurality of absorbance values are respectively subjected to linear fitting with the concentrations of the serial No. 120 solvent oil standard solutions with different concentrations to obtain a serial model. The linear fitting method is not particularly limited in the present invention, and a linear fitting method known to those skilled in the art may be adopted.
In the present invention, the correlation coefficient of the detection model is preferably not less than 0.999.
The method fractionates the light stabilizer-123 to be detected to obtain the No. 120 solvent naphtha to be detected.
In the present invention, the temperature of the fractionation is preferably 100 to 150 ℃, the fractionation is preferably performed under a stirring condition, and the rotation speed of the stirring is preferably 20 to 40rpm, and particularly preferably 20 rpm.
In the present invention, the fractionation preferably comprises the steps of:
placing the light stabilizer-123 to be measured into a three-neck round-bottom flask, simultaneously placing a rotor, heating to the fractionation temperature, and simultaneously stirring for fractionation; the round flask is externally connected with a condenser pipe, the condenser pipe is connected with a ox horn pipe, the ox horn pipe is placed downwards into the conical flask, and the No. 120 solvent naphtha to be detected is collected by a fractionation method.
In the present invention, the fractionation can fractionate the No. 120 solvent oil from the light stabilizer-123 to be measured.
After the No. 120 solvent oil to be detected is obtained, the invention carries out infrared scanning on the No. 120 solvent oil to be detected, and substitutes the infrared information of the No. 120 solvent oil to be detected into the detection model to obtain the content of the No. 120 solvent oil in the light stabilizer-123 to be detected.
In the present invention, the operation of determining the infrared scanning of the 120 # solvent oil to be measured is consistent with the parameters of the infrared scanning performed in the above technical scheme, and is not described herein again. In the present invention, in order to reduce the workload, it is preferable to measure only a specific infrared band at the time of establishing the detection model.
In the invention, the process of substituting the infrared information of the No. 120 solvent oil to be detected into the detection model to obtain the content of the No. 120 solvent oil in the light stabilizer-123 to be detected preferably comprises the following steps:
opening Spectrum Quant Beer's Law quantitative software, and calling out the detection model; and opening the infrared information of the No. 120 solvent oil to be detected, and clicking quant to obtain the content of the No. 120 solvent oil in the light stabilizer-123 to be detected.
The following examples are provided to describe the detection method of 120 # solvent oil in light stabilizer-123 of the present invention in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Preparation of a standard sample: no. 120 solvent oil standard samples (1000mg/kg) are taken, and xylene is used as a solvent to prepare No. 120 solvent oil standard solutions with the concentrations of 4mg/kg, 8mg/kg, 10mg/kg, 20mg/kg and 50mg/kg respectively.
(2) And (3) measuring a standard sample by an ATR method: selecting ATR method to perform infrared scanning on standard sample, with xylene as background, and scanning spectrum range of 600cm-1～4000cm-1In the meantime.
(3) Selecting a characteristic infrared band: the wave band is 2500cm-1～3000cm-1。
(4) Drawing a standard curve: selecting 2500cm-1～3000cm-12930cm in the wave band-1And (3) the absorbance under the wavelength, and drawing a positive correlation curve of the absorbance and the concentration of the standard solution, wherein the value of the correlation coefficient R is 0.9997.
(5) Pretreatment of the light stabilizer-123 to be detected: 1.0005g of light stabilizer-123 to be detected is placed in a three-mouth round-bottom flask, and simultaneously a rotor is placed in the flask; heating at 120 deg.C while stirring at a rotation speed of 50 r/min; the round flask is externally connected with a condenser pipe, the condenser pipe is connected with a ox horn pipe, the ox horn pipe is placed downwards into the conical flask, and the No. 120 solvent naphtha to be detected is collected by a fractionation method.
(6) ATR test of samples to be tested: dripping No. 120 solvent oil to be detected into a Fourier infrared spectrometer, selecting an ATR mode to sweep spectrum, wherein the sweep spectrum waveband is 2500cm-1～3000cm-1。
(7) Quantitative analysis: opening Spectrum Quant Beer's Law quantitative software, calling 2930cm in step (4)-1And (5) opening the infrared information of the characteristic infrared band of the 120 # solvent oil to be detected, which is scanned in the step (6), of the standard curve under the wavelength, and clicking quant to obtain a calculation result.
Example 2
(1) Preparation of a standard sample: no. 120 solvent oil standard samples (1000mg/kg) are taken, and xylene is used as a solvent to prepare No. 120 solvent oil standard solutions with the concentrations of 4mg/kg, 8mg/kg, 10mg/kg, 20mg/kg and 50mg/kg respectively.
(2) And (3) measuring a standard sample by an ATR method: selecting ATR method to perform infrared scanning on standard sample, with xylene as background, and scanning spectrum range of 600cm-1～4000cm-1In the meantime.
(3) Selecting a characteristic infrared band: the sweep spectrum selection waveband is 2700cm-1～3200cm-1。
(4) Drawing a standard curve: selecting 2700cm-1～3200cm-12930cm in the wave band-1And (3) the absorbance under the wavelength, and drawing a positive correlation curve of the absorbance and the concentration of the standard solution, wherein the value of the correlation coefficient R is 0.9991.
(5) Pretreatment of the light stabilizer-123 to be detected: 1.0005g of light stabilizer-123 to be detected is placed in a three-mouth round-bottom flask, and simultaneously a rotor is placed in the flask; heating at 120 deg.C while stirring at a rotation speed of 20 r/min; the round flask is externally connected with a condenser pipe, the condenser pipe is connected with a ox horn pipe, the ox horn pipe is placed downwards into the conical flask, and the No. 120 solvent naphtha to be detected is collected by a fractionation method.
(6) ATR test of samples to be tested: dripping No. 120 solvent oil to be detected into a Fourier infrared spectrometer, selecting an ATR mode to sweep spectrum, wherein the sweep spectrum waveband is 2700cm-1～3200cm-1。
(7) Quantitative analysis: opening Spectrum Quant Beer's Law quantitative software, calling 2930cm in step (4)-1And (5) opening the infrared information of the characteristic infrared band of the 120 # solvent oil to be detected, which is scanned in the step (6), of the standard curve under the wavelength, and clicking quant to obtain a calculation result.
Example 3
(1) Preparation of a standard sample: no. 120 solvent oil standard samples (1000mg/kg) are taken, and xylene is used as a solvent to prepare No. 120 solvent oil standard solutions with the concentrations of 4mg/kg, 8mg/kg, 10mg/kg, 20mg/kg and 50mg/kg respectively.
(2) And (3) measuring a standard sample by an ATR method: selecting ATR method to perform infrared scanning on standard sample, with xylene as background, and scanning spectrum range of 600cm-1～4000cm-1In the meantime.
(3) Selecting a characteristic infrared band: the wave band is 2500cm-1～3200cm-1。
(4) Drawing a standard curve: selecting 2500cm-1～3200cm-12930cm in the wave band-1And (3) the absorbance under the wavelength, and drawing a positive correlation curve of the absorbance and the concentration of the standard solution, wherein the value of the correlation coefficient R is 0.9996.
(5) Pretreatment of the light stabilizer-123 to be detected: putting 1.0007g of a sample to be detected in a three-mouth round-bottom flask, and simultaneously putting a rotor; heating at 120 deg.C while stirring at a rotation speed of 30 r/min; the round flask is externally connected with a condenser pipe, the condenser pipe is connected with a ox horn pipe, the ox horn pipe is placed downwards into the conical flask, and the No. 120 solvent naphtha to be detected is collected by a fractionation method.
(6) ATR test of samples to be tested: dripping No. 120 solvent oil to be detected into a Fourier infrared spectrometer, selecting an ATR mode to perform infrared spectrum scanning, wherein the spectrum scanning waveband is 2500cm-1～3200cm-1。
(7) Quantitative analysis: opening Spectrum Quant Beer's Law quantitative software, calling 2930cm in step (4)-1And (5) opening the infrared information of the characteristic infrared band of the 120 # solvent oil to be detected, which is scanned in the step (6), of the standard curve under the wavelength, and clicking quant to obtain a calculation result.
Example 4
(1) Preparation of a standard sample: no. 120 solvent oil standard samples (1000mg/kg) are taken, and xylene is used as a solvent to prepare No. 120 solvent oil standard solutions with the concentrations of 4mg/kg, 8mg/kg, 10mg/kg, 20mg/kg and 50mg/kg respectively.
(2) And (3) measuring a standard sample by an ATR method: selecting ATR method to perform infrared scanning on standard sample, with xylene as background, and scanning spectrum range of 600cm-1～4000cm-1In the meantime.
(3) Selecting a characteristic infrared band: the wave band is 2700cm-1～3400cm-1。
(4) Drawing a standard curve: selecting 2700cm-1～3400cm-12930cm in the wave band-1And (3) the absorbance under the wavelength, and drawing a positive correlation curve of the absorbance and the concentration of the standard solution, wherein the value of the correlation coefficient R is 0.9996.
(5) Pretreating a light stabilizer-123 to be detected: 1.0005g of light stabilizer-123 to be detected is placed in a three-mouth round-bottom flask, and simultaneously a rotor is placed in the flask; heating at 120 deg.C while stirring (rotation speed of 30 r/min); the round flask is externally connected with a condenser pipe, the condenser pipe is connected with a ox horn pipe, the ox horn pipe is placed downwards into the conical flask, and the No. 120 solvent naphtha to be detected is collected by a fractionation method.
(6) ATR test of samples to be tested: dripping No. 120 solvent oil to be detected into a Fourier infrared spectrometer, selecting an ATR mode to perform infrared spectrum scanning, wherein the spectrum scanning waveband is 2700cm-1～3400cm-1。
(7) Quantitative analysis: opening Spectrum Quant Beer's Law quantitative software, calling 2930cm in step (4)-1And (5) opening the infrared information of the characteristic infrared band of the 120 # solvent oil to be detected, which is scanned in the step (6), of the standard curve under the wavelength, and clicking quant to obtain a calculation result.
Detecting the light stabilizer-123 to be detected by adopting a gas chromatography, wherein the test conditions are as follows: the temperature of the detector is 250 ℃, the temperature of the injection port is 150 ℃, the carrier gas is nitrogen, the split ratio is 100: 1; the sample introduction volume is 1 mL; the programmed temperature is maintained at 50 deg.C for 1min, and increased to 64 deg.C at a rate of 2 deg.C/min, then increased to 100 deg.C at a rate of 20 deg.C/min, then increased to 220 deg.C at a rate of 30 deg.C/min, and maintained for 6 min.
TABLE 1 comparative analysis of the results of the detection of residual amounts of solvent oil according to the invention and the prior art
As can be seen from Table 1, the detection method provided by the invention has good repeatability, and compared with a gas chromatography method, the pretreatment is selected at 30rpm, and the wavelength is selected from 2700-3400 cm-1Wave band 2930cm-1The detection is closer at the wavelength.
In conclusion, the deviation value of the detection result of the detection method provided by the invention and the detection result of the gas chromatography is less than 2%, the feasibility of the detection method is further verified, the detection method provided by the invention is good in repeatability, high in accuracy, simple, convenient, rapid and efficient to operate, and the analysis result has obvious guiding significance for quality control of the light stabilizer in the production process.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.