CN111189953A - Method for determining content of organic peroxide - Google Patents
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- CN111189953A CN111189953A CN202010031819.XA CN202010031819A CN111189953A CN 111189953 A CN111189953 A CN 111189953A CN 202010031819 A CN202010031819 A CN 202010031819A CN 111189953 A CN111189953 A CN 111189953A
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Abstract
The invention relates to the field of organic peroxide analysis, and discloses a method for determining the content of organic peroxide, which comprises the steps of firstly drawing a standard curve of the organic peroxide by using a reversed phase C18 chromatographic column through an HPLC method, and then obtaining the content of the organic peroxide in a sample to be detected under the same condition according to the standard curve, wherein the organic peroxide is at least one selected from tert-butyl peroxy-2-ethylhexanoate, tert-butyl peroxyisononanoate, tert-butyl peroxypivalate and di-tert-butyl peroxide. The method for measuring the content of the organic peroxide has the advantages of time saving, labor saving, high accuracy and good repeatability, can overcome errors in iodometry measurement, and can avoid the problem that the organic peroxide is easily decomposed at high temperature and cannot be accurately measured in gas chromatography.
Description
Technical Field
The invention relates to the field of organic peroxide analysis, and discloses a method for determining the content of organic peroxide.
Background
At present, four organic peroxides, i.e., tert-butyl peroxy-2-ethylhexanoate (TBPEH), tert-butyl peroxyisononanoate (TBPIN), tert-butyl peroxypivalate (TBPPI) and di-tert-butyl peroxide (DTBP), are used as polymerization initiators for high-pressure polyethylene. Among the four organic peroxides, TBPPI has the worst stability, the automatic accelerated degradation temperature is 20 ℃, and the storage temperature is below minus 5 ℃. In the measuring process, degradation is easy to occur, so that the measuring result has large errors.
The current analytical methods employ iodometry to quantify organic peroxides. Since the organic peroxide has by-products and unreacted raw materials during the synthesis reaction, and the contents of the by-products and the unreacted raw materials are calculated into the content of the organic peroxide during the iodometric analysis, the contents of the components in the organic peroxide cannot be accurately measured when the content of each organic peroxide is analyzed by the iodometric method.
The content of each component of the peroxide is analyzed by adopting a gas chromatography, the contained peroxide is required to have better stability, and can still be kept not to be decomposed at the analysis temperature of the gas chromatography, so that the accurate analysis of the content of the peroxide can be ensured. Among the four peroxides, only DTBP had good stability, and the auto-accelerated degradation temperature was 80 ℃. There are studies on the analysis of the DTBP content of organic peroxides by gas chromatography, but the content of each peroxide in the mixture of the above four peroxides cannot be determined by gas chromatography because the higher vaporization temperature decomposes the three peroxides except for DTBP and cannot be analyzed.
Therefore, it is required to develop a method capable of measuring the organic peroxide, particularly a method capable of measuring a mixture of a plurality of organic peroxides.
Disclosure of Invention
The invention aims to overcome the problem of large error in the determination of organic peroxide in the prior art, and provides a method for determining the content of organic peroxide, which has the effect of accurately and precisely determining the content of organic peroxide and can determine at least one of tert-butyl peroxy-2-ethylhexanoate, tert-butyl peroxyisononanoate, tert-butyl peroxypivalate and di-tert-butyl peroxide.
In order to achieve the above object, one aspect of the present invention provides a method for determining the content of an organic peroxide, the method comprising:
(1) taking an organic peroxide standard sample, preparing organic peroxide standard solutions with different concentration gradients, detecting by using an HPLC method to obtain the peak area of the organic peroxide, and drawing a standard curve according to the concentration of the organic peroxide standard solution and the peak area of the organic peroxide;
(2) taking a sample to be detected, preparing a sample solution to be detected, detecting by using an HPLC method under the same condition as the step (1), obtaining the peak area of the organic peroxide in the sample solution to be detected, and calculating the content of the organic peroxide in the sample to be detected according to a standard curve;
wherein the organic peroxide is at least one selected from tert-butyl peroxy-2-ethylhexanoate, tert-butyl peroxyisononanoate, tert-butyl peroxypivalate and di-tert-butyl peroxide;
wherein, the chromatographic column used for HPLC detection is a reversed phase C18 chromatographic column.
Preferably, the solvent of the organic peroxide standard solution and the sample solution to be detected is methanol and/or isopropanol;
when the HPLC method is used for detection, the concentration of the organic peroxide in the organic peroxide standard solution is 0.5-10 wt%; and/or
When the HPLC method is used for detection, the concentration of the organic peroxide in the sample solution to be detected is 0.5-10 wt%.
Preferably, the mobile phase used in the HPLC detection process is water and an organic solvent; the organic solvent is selected from methanol and/or isopropanol, and the weight ratio of water to the organic solvent is 30-10: 70-90.
Preferably, the sample size is 5-30. mu.L as determined by HPLC.
Preferably, the detection wavelength detected by the HPLC method is 240-260 nm; the column temperature is 30-45 ℃.
By adopting the method, the content of at least one of tert-butyl peroxy-2-ethylhexanoate (TBPEH), tert-butyl peroxyisononanoate (TBPIN), tert-butyl peroxypivalate (TBPPI) and di-tert-butyl peroxide (DTBP) is measured by an HPLC method, so that the method has high accuracy and precision, and the problem of decomposition of the organic peroxide in the measuring process is basically avoided.
Drawings
FIG. 1 is a chromatogram of a TBPPI standard in example 1 of the present invention;
FIG. 2 is a chromatogram of a TBPEH standard in example 1 of the present invention;
FIG. 3 is a chromatogram of a TBPIN standard in example 1 of the present invention;
FIG. 4 is a chromatogram of a DTBP standard in example 1 of the present invention.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a method for determining the content of organic peroxide, which comprises the following steps:
(1) taking an organic peroxide standard sample, preparing organic peroxide standard solutions with different concentration gradients, detecting by using an HPLC method to obtain the peak area of the organic peroxide, and drawing a standard curve according to the concentration of the organic peroxide standard solution and the peak area of the organic peroxide;
(2) taking a sample to be detected, preparing a sample solution to be detected, detecting by using an HPLC method under the same condition as the step (1), obtaining the peak area of the organic peroxide in the sample solution to be detected, and calculating the content of the organic peroxide in the sample to be detected according to a standard curve;
wherein the organic peroxide is at least one selected from tert-butyl peroxy-2-ethylhexanoate (TBPEH), tert-butyl peroxyisononanoate (TBPIN), tert-butyl peroxypivalate (TBPPI) and di-tert-butyl peroxide (DTBP);
wherein, the chromatographic column used for HPLC detection is a reversed phase C18 chromatographic column.
It is to be understood that organic peroxides having properties similar to those of the organic peroxide can also be measured using the method of the present invention.
In the present invention, before the organic peroxide standard sample is prepared into the organic peroxide standard solution with different concentration gradients, the organic peroxide standard sample may be subjected to solution or dilution, or may not be subjected to any treatment, and in a preferred case, isododecane is used as a solvent for dissolution to obtain the organic peroxide standard sample-isododecane solution, so that the content of the organic peroxide in the organic peroxide standard sample-isododecane solution is 10 to 80 wt%, for example, 10, 20, 30, 40, 50, 60, 70, 80 wt% and any range between any two values, and preferably 20 to 50 wt%. In the preferred case, the accuracy and precision of the analysis of the organic peroxide content can be improved.
In the present invention, the content of the organic peroxide in the sample to be tested is preferably 10 to 80 wt%, and may be, for example, 10, 20, 30, 40, 50, 60, 70, 80 wt% or any range of composition between any two values, and is preferably 20 to 50 wt%. In the preferred case, the accuracy and precision of the analysis of the organic peroxide content can be improved.
In the present invention, preferably, the sample to be tested further contains isododecane.
In the invention, under the condition that the organic peroxide standard solution and the sample solution to be detected both contain organic peroxide and isododecane, the accuracy and precision of analyzing the content of the organic peroxide can be improved.
In the present invention, the solvent used for preparing the organic peroxide standard solution and the sample solution to be tested may be a solvent that is conventionally used in the art and is miscible with the organic peroxide, and preferably, the solvent of the organic peroxide standard solution and the sample solution to be tested is methanol and/or isopropanol, and more preferably methanol. The solvent may be the same or different, preferably the same, as the organic solvent used in the mobile phase during the detection by HPLC.
In the present invention, the concentration of the organic peroxide in the organic peroxide standard solution can be selected from a wide range in the HPLC method, and preferably, the concentration of the organic peroxide in the organic peroxide standard solution is 0.5 to 10 wt%, for example, 0.5, 1, 2, 4, 6, 8, 10 wt% and any range of composition between any two values, and more preferably 1 to 8 wt%. Within the preferred range, a better peak pattern can be obtained, further improving the accuracy and precision of the analysis.
In the present invention, the concentration of the organic peroxide in the sample solution to be tested can be selected from a wide range during HPLC detection, and preferably, the concentration of the organic peroxide in the sample solution to be tested is 0.5 to 10 wt%, for example, 0.5, 1, 2, 4, 6, 8, 10 wt% and any range between any two values, and more preferably 1 to 8 wt%. Within the preferred range, a better peak pattern can be obtained, further improving the accuracy and precision of the analysis.
In the present invention, preferably, before the HPLC detection is performed on the organic peroxide standard solution and the sample solution to be detected, a filter membrane is used to filter the organic peroxide standard solution and the sample solution to be detected, respectively; the filter membrane is a 0.45 μm filter membrane. The filtered organic peroxide standard solution and the solution of the sample to be detected can be fed into a chromatographic column for HPLC analysis.
It should be understood that the HPLC method and the equipment used for determining the organic peroxide standard solution and the sample solution to be tested are the same.
In the present invention, the standard solution and the sample solution can be analyzed using a liquid chromatograph which is conventional in the art, and preferably, the high performance liquid chromatograph of the HPLC method is shimadzu LC-2030 or siemer femplc.
It is known that the high performance liquid chromatograph is also equipped with a manual or automated sample injection system, preferably an automated sample injection system.
Wherein, the high performance liquid chromatograph can be operated according to the operation method of the high performance liquid chromatograph which is conventionally used in the field by the person skilled in the art.
In the present invention, the amount of sample detected by HPLC can be selected from a wide range, and the amount of sample detected by HPLC is preferably 5 to 30. mu.L, for example, may be 5, 8, 10, 15, 20, 25, 30. mu.L, or any range of any two values, and more preferably 8 to 15. mu.L. In the preferable range, the chromatographic peak has good peak type symmetry, basically no tailing, and higher accuracy and precision of an analysis result.
In the present invention, the high performance liquid chromatograph is also equipped, as is well known, with a column that is a reversed-phase C18 column conventionally used in the art, preferably a poroshell 120 column.
In the present invention, the high performance liquid chromatograph is further equipped with a column oven for providing a stable working environment to the chromatographic column, especially maintaining a stable column temperature, preferably, the column temperature is 20-35 ℃. Within the preferred ranges, the accuracy and precision of the analysis of the organic peroxide content can be improved.
It is known to use mobile phases in the detection process by HPLC. Preferably, the mobile phase used in the HPLC detection process is water and an organic solvent. Preferably, the organic solvent is selected from methanol and/or isopropanol. More preferably methanol. Preferably, the weight ratio of water to organic solvent is 30-10: 70-90, such as 10:90, 12:88, 14:86, 16:84, 18:82, 20:80, 22:78, 24:76, 26:74, 28:72, 30:70, and any range between any two values, and more preferably 24-16: 76-84.
In the present invention, the flow rate of the mobile phase can be selected within a wide range, preferably 0.5 to 2mL/min, as measured by HPLC.
As is known, the hplc is also equipped with a detector, preferably an ultraviolet detector; the high performance liquid chromatograph is used together with an ultraviolet detector for detection.
In the present invention, the detection wavelength can be selected in a wide range, and preferably, the detection wavelength detected by HPLC method is 240-260nm, such as 240nm, 242nm, 244nm, 246nm, 248nm, 250nm, 252nm, 254nm, 256nm, 258nm, 260nm and any range composed of any two values, more preferably 250-256 nm. Within the preferred ranges, the accuracy and precision of the analysis of the organic peroxide content can be improved.
In the invention, a standard curve is drawn according to the concentration of the organic peroxide standard solution and the peak area of the organic peroxide; and then substituting the peak area of the organic peroxide in the sample to be detected, which is determined by the HPLC method, into the standard curve to calculate the content of the organic peroxide in the sample to be detected.
The present invention will be described in detail below by way of examples.
In the following examples, isododecane is chromatographically pure isododecane of alpha reagent, 80% pure.
The DTBP standard was 99.7% pure DTBP available from Lamzhou auxiliary Agents company, Inc.
The TBPPI standard is a 98.5% pure TBPPI available from lanzhou auxiliary factory, llc.
The TBPEH standard is 98.5% pure TBPEH available from Lanzhou auxiliary Agents Co., Ltd.
The TBPIN standard is 99.3% pure TBPIN available from lanzhou auxiliary agents, llc.
The data obtained were analyzed using Excel software.
Example 1
This example illustrates the establishment of a standard curve for organic peroxides
(1) Solution preparation
Preparation of a standard solution: 250mg of organic peroxide (DTBP, TBPPI, TBPEH or TBPIN) standard sample is weighed and dissolved in 250mg of isododecane, then different amounts of methanol are added, and the mixture is fully shaken and mixed to obtain standard solutions with the concentrations of 1 wt%, 5 wt% and 8 wt%.
The standard solutions were separately filtered using 0.45 μm filters before HPLC analysis.
(2) HPLC analysis
In this example, the standard curves of DTBP, TBPPI, TBPEH and TBPIN were sequentially established as follows
High performance liquid chromatograph: shimadzu LC-2030;
a chromatographic column: a reverse C18 column, Poroshell 120;
a detector: ultraviolet visible spectrophotometer LAMBDA25, wavelength 254 nm;
column temperature: 30 ℃;
mobile phase: formaldehyde and water (80: 20); the flow rate is 1.0mL/min, and the tail blowing flow is 20 mL/min;
sample introduction amount: 10 μ L.
(3) Establishment of a Standard Curve
Analyzing the chromatogram obtained in step (2) (as shown in fig. 1 to 4), calculating peak area, and calculating to obtain standard curve of each organic peroxide.
DTBP: the standard curve is that y is 98755x-864.83, R2＝0.9997。
TBPPI: the standard curve is that y is 185760x +702.81, R2＝0.9992。
TBPEH: the standard curve is that y is 528720x +2082.4, R2＝0.9993。
TBPIN: the standard curve is that y is 185760x +702.81, R2＝0.9995。
Example 2
This example illustrates the determination of the content of organic peroxide in a sample
Preparing a sample to be tested: organic peroxide (DTBP, TBPPI, TBPEH or TBPIN) standards were weighed and formulated with isododecane to 25.12 wt% TBPPI, 30.15 wt% TBPEH, 30.18 wt% TBPIN and 49.92 wt% DTBP, respectively.
And (3) fully and uniformly mixing 9 parts by weight of methanol and 1 part by weight of a sample to be detected to obtain a sample solution to be detected, and filtering the sample solution to be detected by using a 0.45-micrometer filter membrane before carrying out HPLC detection on the sample solution to be detected.
The concentration of the above test sample solutions was determined by HPLC analysis as described in example 1, with 8 replicates of each solution.
Taking TBPEH as an example, 30.15 wt% of samples to be tested for TBPEH are analyzed for 8 times, the analysis results are respectively 30.28%, 30.37%, 29.99%, 30.54%, 30.10%, 29.94%, 30.37% and 30.23%, the average value is calculated to be 30.23%, and the SD value is calculated to be 0.21%.
The result of 25.12 wt% TBPPI test sample was 24.95 ± 0.72 wt%.
The result of the 30.18 wt% TBPIN test sample was 30.68 ± 0.35 wt%.
49.92 wt% DTBP test sample gave a result of 50.11. + -. 0.41 wt%.
Example 3
This example illustrates the determination of the content of organic peroxide in a sample
Preparing a sample to be tested: organic peroxide (TBPPI, TBPEH and TBPIN) standards were weighed and formulated with isododecane to give a mixed sample of TBPPI (10 wt%), TBPEH (15 wt%) and TBPIN (20 wt%).
And (3) fully and uniformly mixing 9 parts by weight of methanol and 1 part by weight of a sample to be detected to obtain a sample solution to be detected, and filtering the sample solution to be detected by using a 0.45-micrometer filter membrane before carrying out HPLC detection on the sample solution to be detected.
The concentration of the above test sample solution was determined in 3 replicates according to the HPLC analysis method described in example 1.
And (3) analyzing by HPLC to obtain the following components in the sample to be detected: TBPPI 10.76. + -. 0.42 wt%, TBPEH 15.56. + -. 0.57 wt% and TBPIN 20.36. + -. 0.55 wt%.
Example 4
This example illustrates the determination of the content of organic peroxide in a sample
The procedure was followed as in example 2 except that the amount of the sample to be sampled was 30. mu.L.
The four peroxide samples were too broad in chromatographic peaks and exhibited tailing when analyzed by HPLC.
Example 5
This example illustrates the determination of the content of organic peroxide in a sample
A standard curve was established using TBPEH as described in example 1, except that the solvent used to prepare the solution to be tested was replaced by methanol to isopropanol and the type of organic solvent in the mobile phase was replaced by methanol to isopropanol.
The standard curve for TBPEH was found to be y-428421 x +1283.6, R2＝0.9989。
Example 6
This example illustrates the determination of the content of organic peroxide in a sample
Example 6-1: the procedure is as in example 2, except that the weight ratio of water to methanol in the mobile phase is 30: 70.
Example 6-2: the procedure is as in example 2, except that the weight ratio of water to methanol in the mobile phase is 10: 90.
Upon HPLC analysis, an increase in methanol ratio resulted in a decrease in peroxide retention time when methanol: when water is 90:10, the peak area decreases, the retention time is short, and it is difficult to completely separate 4 peroxides.
When the ratio of methanol: when the water is 70:30, the retention time is too long, and the peak shape is wide.
Example 7
Taking TBPEH as an example, determining the influence of the TBPEH content in the solution to be detected
Example 7-1: the procedure was followed as in example 2, except that the concentration of the test sample solution of TBPEH was adjusted to 0.1 wt%.
When the concentration of the sample solution to be tested of TBPEH was 0.1 wt%, the result of 30.15 wt% TBPEH sample to be tested was 30.25 + -0.81 wt% as analyzed by HPLC.
Example 7-2: the procedure was followed as in example 2, except that the concentration of the test sample solution of TBPEH was adjusted to 12% by weight.
When the concentration of the test sample solution of TBPEH was 12 wt%, the result of the 30.15 wt% TBPEH test sample was 30.41 ± 0.90 wt%.
From the above examples, it can be seen that the method of the present invention can accurately and precisely analyze the content of organic peroxides.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for determining the content of an organic peroxide, the method comprising:
(1) taking an organic peroxide standard sample, preparing organic peroxide standard solutions with different concentration gradients, detecting by using an HPLC method to obtain the peak area of the organic peroxide, and drawing a standard curve according to the concentration of the organic peroxide standard solution and the peak area of the organic peroxide;
(2) taking a sample to be detected, preparing a sample solution to be detected, detecting by using an HPLC method under the same condition as the step (1), obtaining the peak area of the organic peroxide in the sample solution to be detected, and calculating the content of the organic peroxide in the sample to be detected according to a standard curve;
wherein the organic peroxide is at least one selected from tert-butyl peroxy-2-ethylhexanoate, tert-butyl peroxyisononanoate, tert-butyl peroxypivalate and di-tert-butyl peroxide;
wherein, the chromatographic column used for HPLC detection is a reversed phase C18 chromatographic column.
2. The assay of claim 1, wherein the organic peroxide standard is dissolved in isododecane as a solvent before formulating the organic peroxide standard into organic peroxide standard solutions with different concentration gradients, such that the organic peroxide content of the organic peroxide standard-isododecane solution is 10 to 80 wt%.
3. The assay of claim 1, wherein the sample to be assayed has an organic peroxide content of 10-80 wt%;
preferably, the sample to be tested also contains isododecane.
4. The assay method according to claim 1, wherein the solvent of the organic peroxide standard solution and the sample solution to be tested is methanol and/or isopropanol;
when the HPLC method is used for detection, the concentration of the organic peroxide in the organic peroxide standard solution is 0.5-10 wt%; and/or
When the HPLC method is used for detection, the concentration of the organic peroxide in the sample solution to be detected is 0.5-10 wt%.
5. The analytical method according to claim 1, wherein the HPLC-HPLC apparatus is Shimadzu LC-2030 or SamerfeUHPLC.
6. The analytical method according to claim 1, wherein the mobile phase used in the HPLC method detection process is water and an organic solvent; the organic solvent is selected from methanol and/or isopropanol, and the weight ratio of water to the organic solvent is 30-10: 70-90.
7. The assay of claim 6, wherein the flow rate of the mobile phase is 0.5-2mL/min as measured by HPLC.
8. The assay of claim 1, wherein the sample size is 5-30 μ L as measured by HPLC.
9. The analytical method according to claim 1, wherein the detection wavelength by HPLC method is 240-260 nm; the column temperature is 30-45 ℃.
10. The analytical method according to claim 1, wherein the organic peroxide standard solution and the sample solution to be tested are separately filtered using a filter membrane before HPLC detection of the organic peroxide standard solution and the sample solution to be tested;
the filter membrane is a 0.45 μm filter membrane.
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| CN112684058A (en) * | 2020-12-30 | 2021-04-20 | 国高材高分子材料产业创新中心有限公司 | Method for measuring DTBP content in polypropylene melt-blown material |
| CN113063865A (en) * | 2021-03-19 | 2021-07-02 | 陕西延长中煤榆林能源化工有限公司 | Analysis method of 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane in polypropylene melt-blown material |
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