CN115236256B - Determination method of 1, 3-propyl sultone - Google Patents
Determination method of 1, 3-propyl sultone Download PDFInfo
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- CN115236256B CN115236256B CN202210671104.XA CN202210671104A CN115236256B CN 115236256 B CN115236256 B CN 115236256B CN 202210671104 A CN202210671104 A CN 202210671104A CN 115236256 B CN115236256 B CN 115236256B
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- -1 3-propyl Chemical group 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 28
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 69
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 68
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000012360 testing method Methods 0.000 claims abstract description 27
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 5
- 238000002347 injection Methods 0.000 claims description 19
- 239000007924 injection Substances 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 18
- 150000002500 ions Chemical class 0.000 claims description 16
- 238000004817 gas chromatography Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004949 mass spectrometry Methods 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 21
- 238000002360 preparation method Methods 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 9
- 238000000605 extraction Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 4
- 238000002137 ultrasound extraction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- DZVSAHOHDQUFMZ-UHFFFAOYSA-N 2-hydroxyethyl 4-methylbenzenesulfonate Chemical compound CC1=CC=C(S(=O)(=O)OCCO)C=C1 DZVSAHOHDQUFMZ-UHFFFAOYSA-N 0.000 description 1
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011151 fibre-reinforced plastic Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- MHYFEEDKONKGEB-UHFFFAOYSA-N oxathiane 2,2-dioxide Chemical compound O=S1(=O)CCCCO1 MHYFEEDKONKGEB-UHFFFAOYSA-N 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The application relates to the technical field of chemical analysis, and particularly discloses a method for measuring 1, 3-propyl sultone. The method specifically comprises the following steps: (1) Adding an extractant into a sample to be detected, and performing ultrasonic treatment to obtain an extract; (2) Testing the extract by adopting a gas chromatograph-mass spectrometer, and calculating the content of 1, 3-propyl sultone in the sample to be tested according to the test result; wherein the extractant is a mixed solution of n-hexane, acetone and ethyl acetate. The detection method provided by the application can effectively improve the accuracy of the determination of the 1, 3-propyl sultone.
Description
Technical Field
The application relates to the technical field of chemical analysis, in particular to a method for measuring 1, 3-propyl sultone.
Background
The 1, 3-propyl sultone is an excellent general sulfonating agent, belongs to a new functional fine chemical material, can react with a plurality of compounds under very mild conditions to provide sulfonic acid groups, thereby endowing the compounds with new properties, and is commonly used in the industries of leather making, spinning, printing ink, sensitizing dye and the like. However, 1, 3-propylsultone is a toxic substance, and 1, 3-propylsultone in industrial products is extremely liable to contact human body, thereby endangering human health, so that quantitative determination of the content of 1, 3-propylsultone in industrial products is necessary.
At present, gas chromatography is an effective method for measuring 1, 3-propyl sultone in industrial products, inert gas is used as a mobile phase, and the distribution coefficients of gas phase and fixed phase of each component in a sample to be measured in a chromatographic column are different, so that each component in the sample to be measured presents different chromatographic peaks in a chromatogram. According to the peak position and the peak area of the sample to be detected, the content of the 1, 3-propyl sultone in the sample to be detected can be determined. However, when the content of 1, 3-propylsultone in the sample to be measured is low, it is difficult for the gas chromatography to effectively enrich the 1, 3-propylsultone in the sample to be measured, so that the accuracy of the measurement result is low.
Disclosure of Invention
In order to improve the accuracy of 1, 3-propylsultone measurement, the present application provides a method for measuring 1, 3-propylsultone.
The method for measuring the 1, 3-propyl sultone specifically comprises the following steps:
(1) Adding an extractant into a sample to be detected, and performing ultrasonic treatment to obtain an extract;
(2) Testing the extract by adopting a gas chromatograph-mass spectrometer, and calculating the content of 1, 3-propyl sultone in the sample to be tested according to a test result;
the extractant is a mixed solution of n-hexane, acetone and ethyl acetate.
The mixed solution of n-hexane, acetone and ethyl acetate is used as an extraction solvent to carry out ultrasonic extraction on the 1, 3-propyl sultone in the sample to be detected, so that the 1, 3-propyl sultone in the sample to be detected can be fully enriched in the extraction agent; then, the extraction liquid is tested by adopting a gas chromatograph-mass spectrometer, the content of the 1, 3-propyl sultone in the sample to be tested is calculated, and the detection accuracy of the 1, 3-propyl sultone in the sample to be tested can be effectively improved by adopting the method.
Test analysis shows that compared with the method of selecting methanol as an extractant to extract a sample to be tested, the method of selecting n-hexane, acetone and ethyl acetate as the extractants to extract the sample to be tested simultaneously, so that the accuracy of measuring the 1, 3-propyl sultone in the sample to be tested is obviously improved.
In addition, experimental analysis shows that the method for measuring the 1, 3-propyl sultone in the sample to be measured is low in accuracy by selecting n-hexane as an extracting agent, acetone as an extracting agent or ethyl acetate as an extracting agent; two of normal hexane, acetone and ethyl acetate are selected to be fully mixed to be used as an extracting agent, and the extracting agent is used for the method for measuring the 1, 3-propyl sultone in the sample to be measured, so that the accuracy of a measuring result is slightly improved. The method for measuring the 1, 3-propyl sultone in the sample to be measured adopts n-hexane, acetone and ethyl acetate as the extracting agents, so that the accuracy of the measuring result is obviously improved.
Preferably, the weight ratio of the sample to be tested to the extractant is 1: (20-30).
Further, the weight ratio of the sample to be tested to the extractant is 1: (23-27).
In a specific embodiment, the weight ratio of the test sample to the extractant may be 1: 20. 1: 23. 1: 25. 1: 27. 1:30.
in some specific embodiments, the weight ratio of the test sample to the extractant may also be 1: (20-23), 1: (20-25), 1: (20-27), 1: (23-25), 1: (23-30), 1: (25-27), 1: (25-30), 1: (27-30).
As is clear from experimental analysis, when the weight ratio of the sample to be measured to the extractant is controlled within the above range, the accuracy of measuring 1, 3-propylsultone in the sample to be measured is further improved. Therefore, the present application controls the weight ratio of the test sample to the extractant within the above range.
Preferably, the extractant comprises the following components in parts by weight: 12-16 parts of n-hexane; 1.5-2.5 parts of acetone; ethyl acetate 0.5-1.0 parts.
In a specific embodiment, the n-hexane may be added in an amount of 12 parts, 14 parts, 16 parts.
In some specific embodiments, the n-hexane may also be added in an amount of (12-14) parts, (14-16) parts.
In a specific embodiment, the acetone may be added in an amount of 1.5 parts, 2 parts, 2.5 parts.
In some specific embodiments, the acetone may also be added in an amount of (1.5-2) parts, (2-2.5) parts.
In a specific embodiment, the ethyl acetate may be added in an amount of 0.5 parts, 0.8 parts, 1.0 parts.
In some specific embodiments, the ethyl acetate may also be added in an amount of (0.5-0.8) parts, (0.8-1.0) parts.
According to experimental analysis, when the addition amount of each component in the extractant is controlled within the range, the accuracy of measuring the 1, 3-propyl sultone in the sample to be tested is further improved after the sample to be tested is extracted. Therefore, the present application controls the addition amount of each component in the extractant within the above-described range.
Preferably, the conditions of the ultrasonic treatment are: the working frequency is 20-40KHZ; the temperature is 30-50 ℃; the time is 20-40min.
Preferably, the parameters of the gas chromatograph-mass spectrometer are:
(1) The conditions of the gas chromatography are as follows: chromatographic column: DB-5MS,30m x 0.25mm x 0.25 μm; carrier gas: helium (purity is more than or equal to 99.999 percent) with the flow rate of 0.5-1.5mL/min; sample inlet temperature: 220-250 ℃; column flow rate: 1.0-2.0mL/min; column box temperature rise program: the initial column temperature is 40-60 ℃, the temperature is kept for 2min, then the temperature is increased to 100-140 ℃ at the speed of 15 ℃/min, the temperature is kept for 2min, the temperature is increased to 280-320 ℃ at the speed of 15 ℃/min, and the temperature is kept for 10min;
(2) The conditions of the mass spectrometer are: transmission line temperature: 220 ℃; ion source temperature: 240 ℃; EI source bombardment energy: 70eV; mass scan range: 10-200m/z; solvent delay time: 5min; mass spectrometry run time: 15min; scanning mode: full scan and selective ion scan; ions 58, 64, 122m/z were monitored, with 58m/z selected as the quantitative ion.
Preferably, the sample injection mode in the gas chromatograph adopts split-flow sample injection.
In the application, when the gas chromatography is adopted to test the extraction liquid to be tested, the sample loading amount of the chromatographic column is limited, and excessive extraction liquid to be tested enters the chromatographic column to generate overload phenomenon, so that the separation efficiency of the 1, 3-propyl sultone is reduced, and the accuracy of the measurement result is influenced. Therefore, the method and the device detect the sample to be detected in a split-flow sample injection mode, and are favorable for further improving the accuracy of the measurement result.
Further, the split ratio of the split sample injection is (10-20): 1.
further, the split ratio of the split sample injection is (13-17): 1.
in a specific embodiment, the split ratio of the split sample injection may be 10: 1. 13: 1. 15:1. 17: 1. 20: 1. a. The invention relates to a method for producing a fibre-reinforced plastic composite
In some specific embodiments, the split ratio of the split sample may also be (10-13): 1. (10-15): 1. (10-17): 1. (13-15): 1. (13-20): 1. (15-17): 1. (15-20): 1. (17-20): 1.
according to experimental analysis, when the gas chromatograph-mass spectrometer is adopted to test the sample to be tested, when the split ratio of the split sample injection is controlled within the range, the accuracy of measuring the 1, 3-propyl sultone in the sample to be tested is further improved. Therefore, the split ratio of split injection is controlled in the range.
In summary, the technical scheme of the application has the following specific effects:
according to the method, the mixed solution of n-hexane, acetone and ethyl acetate is used as an extraction solvent, the 1, 3-propyl sultone in the sample to be detected is subjected to ultrasonic extraction, then the extraction liquid is tested by adopting a gas chromatography-mass spectrometer, the content of the 1, 3-propyl sultone in the sample to be detected is calculated, and the detection accuracy of the 1, 3-propyl sultone in the sample to be detected can be effectively improved by using the method.
Detailed Description
The application provides a method for measuring 1, 3-propyl sultone, which specifically comprises the following steps:
(1) Adding an extractant into a sample to be detected, and then treating the sample to be detected for 20-40min by adopting an ultrasonic condition with the working frequency of 20-40KHZ at the temperature of 30-50 ℃ to obtain an extract;
(2) And testing the extract by adopting a gas chromatograph-mass spectrometer, and calculating the content of 1, 3-propyl sultone in the sample to be tested according to the test result.
Wherein the extractant is a mixed solution of n-hexane, acetone and ethyl acetate.
Specifically, the weight ratio of the sample to be tested to the extractant is 1: (20-30). Further, the weight ratio of the sample to be tested to the extractant is 1: (23-27).
Further, the extractant comprises the following components in parts by weight: 12-16 parts of n-hexane; 1.5-2.5 parts of acetone; ethyl acetate 0.5-1.0 parts.
Wherein, the parameters of the gas chromatograph-mass spectrometer are:
(1) The conditions of the gas chromatography were: chromatographic column: DB-5MS,30m x 0.25mm x 0.25 μm; carrier gas: helium (purity is more than or equal to 99.999 percent) with the flow rate of 0.5-1.5mL/min; sample inlet temperature: 220-250 ℃; column flow rate: 1.0-2.0mL/min; column box temperature rise program: the initial column temperature is 40-60 ℃, the temperature is kept for 2min, then the temperature is increased to 100-140 ℃ at the speed of 15 ℃/min, the temperature is kept for 2min, the temperature is increased to 280-320 ℃ at the speed of 15 ℃/min, and the temperature is kept for 10min;
the sample injection mode in the gas chromatograph adopts split-flow sample injection.
Specifically, the split ratio of split sample injection is (10-20): 1. further, the split ratio of the split sample injection is (13-17): 1.
(2) The conditions of the mass spectrometer were: transmission line temperature: 220 ℃; ion source temperature: 240 ℃; EI source bombardment energy: 70eV; mass scan range: 10-200m/z; solvent delay time: 5min; mass spectrometry run time: 15min; scanning mode: full scan and selective ion scan; ions 58, 64, 122m/z were monitored, with 58m/z selected as the quantitative ion.
The present application is described in further detail below in connection with preparations 1-19, examples 1-25, comparative examples 1-6, and performance measurement tests, which should not be construed as limiting the scope of the claimed application.
Preparation example
Preparation examples 1 to 13
Preparation examples 1 to 13 each provide an extractant.
The preparation examples are different in that: the addition amount of each component in the extractant. As shown in table 1.
The preparation method of each preparation example comprises the following steps: according to Table 1, n-hexane, acetone and ethyl acetate were weighed in corresponding weights and thoroughly mixed to prepare an extractant.
TABLE 1 addition amount of each component in the extractant of preparation examples 1 to 13
Preparation examples 14 to 19
Preparation examples 14-19 each provide an extractant.
Each of the above preparation examples is different from preparation example 3 in that: the types of the components in the extractant. As shown in table 2.
TABLE 2 kinds of respective components in the extractants in preparation examples 3, 14-19
Examples
Examples 1 to 13
Examples 1-13 provide a method for measuring 1, 3-propylsultone, respectively.
The above embodiments differ in that: the type of extractant in step (1). Specifically, the results are shown in Table 3.
The specific steps of the above embodiments are as follows:
1. respectively weighing 0.5g of 1, 3-propyl sultone, 1g of hydroxyethyl p-toluenesulfonate, 1.5g of 1, 4-butane sultone and 997g of deionized water, and fully and uniformly mixing to obtain a sample to be tested;
2. adding 0.1g of a sample to be tested into 2.5g of an extractant, and then treating the sample to be tested for 30min at the temperature of 40 ℃ under the ultrasonic condition of the working frequency of 30KHZ to obtain an extract;
3. preparing 0.01%, 0.1%, 0.5%, 1% and 5% of serial standard solutions of the 1, 3-propyl sultone standard substances according to the steps (1) and (2), testing the standard solutions by adopting a gas chromatograph-mass spectrometer, and drawing a standard curve according to test results;
4. testing the extract to be tested by adopting a gas chromatograph-mass spectrometer, and calculating the content of 1, 3-propyl sultone in the sample to be tested according to a test result and a standard curve;
wherein, the parameters of the gas chromatograph-mass spectrometer are:
(1) the conditions of the gas chromatography were: chromatographic column: DB-5MS,30m x 0.25mm x 0.25 μm; carrier gas: helium (purity is more than or equal to 99.999 percent) with a flow rate of 1mL/min; sample inlet temperature: 230 ℃; column flow rate: 1.5mL/min; column box temperature rise program: the initial column temperature is 50 ℃, kept for 2min, then heated to 120 ℃ at the speed of 15 ℃/min, kept for 2min, heated to 300 ℃ at the speed of 15 ℃/min, and kept for 10min; split sample injection is adopted, and the split ratio is 15:1.
(2) the conditions of the mass spectrometer were: transmission line temperature: 220 ℃; ion source temperature: 240 ℃; EI source bombardment energy: 70eV; mass scan range: 10-200m/z; solvent delay time: 5min; mass spectrometry run time: 15min; scanning mode: full scan and selective ion scan; ions 58, 64, 122m/z were monitored, with 58m/z selected as the quantitative ion.
TABLE 3 types of extractants in examples 1-13
Examples 14 to 19
Examples 14-19 provide a method for measuring 1, 3-propylsultone, respectively.
The above embodiments differ from embodiment 3 in that: the weight ratio of the sample to be tested to the extractant. As shown in table 4.
Table 4 weight ratio of the test sample to the extractant in examples 3, 14 to 19
Examples 20 to 25
Examples 20-25 provide a method for measuring 1, 3-propylsultone, respectively.
The above embodiments differ from embodiment 3 in that: split ratio of split sample introduction in gas chromatography conditions. As shown in table 5.
TABLE 5 split ratio of split feeds in examples 3, 20-25
Comparative example
Comparative examples 1 to 6
Comparative examples 1-6 each provide a method for measuring 1, 3-propylsultone.
Each of the above comparative examples is different from example 3 in that: type of extractant. As shown in table 6.
TABLE 6 types of extractants in comparative examples 1-6
Comparative example 7
Comparative example 7 provides a method for determining 1, 3-propylsultone.
This comparative example differs from example 3 in that: the extractant is methanol.
Performance measurement test
The accuracy of the measurement method provided in the present application was calculated by comparing the measured values of the 1, 3-propylsultone content in the test samples provided in examples 1 to 25 and comparative examples 1 to 6 with the actual value of the 1, 3-propylsultone content in the test sample of 0.5%o.
TABLE 7 detection results for examples 1-25 and comparative examples 1-6
Referring to Table 6, as can be seen from the results of comparative examples 1 to 25 and comparative examples 1 to 6, the present application uses a mixed solution of n-hexane, acetone and ethyl acetate as an extractant to perform ultrasonic extraction of 1, 3-propylsultone in a sample to be tested; obtaining an extract; and then, testing the extract by adopting a gas chromatograph-mass spectrometer, and calculating the content of the 1, 3-propyl sultone in the sample to be tested. By using the test method provided by the application, the accuracy of the measurement of the 1, 3-propyl sultone in the sample to be tested can be effectively improved.
As can be seen from the detection results of comparative examples 3 and 7, compared with the method of selecting methanol as the extractant to extract the sample to be tested, the method of selecting n-hexane, acetone and ethyl acetate as the extractants to extract the sample to be tested simultaneously, so that the accuracy of measuring the 1, 3-propylsultone in the sample to be tested is obviously improved.
As can be seen from the detection results of comparative example 3 and comparative examples 1 to 6, the accuracy of measuring 1, 3-propylsultone in the sample to be measured is lower than that in the sample to be measured which is extracted by using n-hexane alone, acetone alone or ethyl acetate alone; two of normal hexane, acetone and ethyl acetate are selected to be fully mixed to be used as an extractant, the sample to be tested is extracted, and the accuracy of measuring the 1, 3-propyl sultone in the sample to be tested is slightly improved. In the method, n-hexane, acetone and ethyl acetate are selected as the extracting agents at the same time, and the sample to be tested is extracted, so that the accuracy of measuring the 1, 3-propyl sultone in the sample to be tested is obviously improved.
As is clear from the results of comparative examples 1 to 5, when the amount of n-hexane added in the extractant is controlled within the range of 12 to 16 parts, the accuracy of measuring 1, 3-propylsultone in the sample to be measured is further improved after the sample to be measured is extracted. Therefore, the present application controls the addition amount of n-hexane in the extractant within the above-described range.
As is clear from the results of comparative examples 3 and 6 to 9, when the amount of acetone added in the extractant is controlled within the range of 1.5 to 2.5 parts, the accuracy of measuring 1, 3-propylsultone in the sample to be tested is further improved after the sample to be tested is extracted. Therefore, the present application controls the addition amount of acetone in the extractant within the above-described range.
As is clear from the results of comparative examples 3 and 10 to 13, when the amount of ethyl acetate added to the extractant is controlled within the range of 0.5 to 1.0 part, the accuracy of measuring 1, 3-propylsultone in the sample to be tested is further improved after the sample to be tested is extracted. Therefore, the present application controls the addition amount of ethyl acetate in the extractant within the above-described range.
As can be seen from the results of comparative examples 3 and 14 to 19, when the weight ratio of the sample to be tested to the extractant is controlled to be 1: when the ratio is within the range of (20-30), the accuracy of measuring 1, 3-propylsultone in the sample to be measured is further improved. Thus, the present application controls the weight ratio of the test sample to the extractant within the above range. Further, the present application controls the weight ratio of the test sample to the extractant to 1: (23-27).
As can be seen from the test results of comparative examples 3 and 20 to 25, when the sample to be tested is tested by a gas chromatograph-mass spectrometer, the split ratio of the split sample injection is controlled to be (10 to 20): when 1 is within the range, the accuracy of measuring 1, 3-propylsultone in the sample to be measured is further improved. Therefore, the split ratio of split injection is controlled in the range. Further, the split ratio of split sample injection is controlled to be (13-17): 1.
while the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (2)
1. The method for measuring the 1, 3-propyl sultone is characterized by comprising the following steps of:
(1) Adding an extractant into a sample to be detected, and performing ultrasonic treatment to obtain an extract; the weight ratio of the sample to be tested to the extractant is 1: (23-27), wherein the extractant is a mixed solution of n-hexane, acetone and ethyl acetate, and the extractant comprises the following components in parts by weight: 12-16 parts of n-hexane; 1.5-2.5 parts of acetone; 0.5-1.0 part of ethyl acetate;
(2) Testing the extract by adopting a gas chromatograph-mass spectrometer, and calculating the content of 1, 3-propyl sultone in the sample to be tested according to a test result;
the parameters of the gas chromatograph-mass spectrometer are:
the conditions of the gas chromatography are as follows: chromatographic column: DB-5MS,30m x 0.25mm x 0.25 μm; carrier gas: helium (purity is more than or equal to 99.999 percent) with the flow rate of 0.5-1.5mL/min; sample inlet temperature: 220-250 ℃; column flow rate: 1.0-2.0mL/min; column box temperature rise program: the initial column temperature is 40-60 ℃, the temperature is kept for 2min, then the temperature is increased to 100-140 ℃ at the speed of 15 ℃/min, the temperature is kept for 2min, the temperature is increased to 280-320 ℃ at the speed of 15 ℃/min, and the temperature is kept for 10min;
the sample injection mode in the gas chromatograph adopts split-flow sample injection, and the split-flow ratio of the split-flow sample injection is (13-17): 1, a step of;
the conditions of the mass spectrometer are: transmission line temperature: 220 ℃; ion source temperature: 240 ℃; EI source bombardment energy: 70eV; mass scan range: 10-200m/z; solvent delay time: 5min; mass spectrometry run time: 15min; scanning mode: full scan and selective ion scan; ions 58, 64, 122m/z were monitored, with 58m/z selected as the quantitative ion.
2. The method for measuring 1, 3-propylsultone according to claim 1, wherein the ultrasonic treatment conditions are: the working frequency is 20-40KHZ; the temperature is 30-50 ℃; the time is 20-40min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210671104.XA CN115236256B (en) | 2022-06-15 | 2022-06-15 | Determination method of 1, 3-propyl sultone |
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| CN202210671104.XA CN115236256B (en) | 2022-06-15 | 2022-06-15 | Determination method of 1, 3-propyl sultone |
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| CN115236256A CN115236256A (en) | 2022-10-25 |
| CN115236256B true CN115236256B (en) | 2024-02-09 |
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| CN110824043A (en) * | 2019-11-08 | 2020-02-21 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Method for measuring content of 1, 3-propane sultone in textile |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110824043A (en) * | 2019-11-08 | 2020-02-21 | 广东产品质量监督检验研究院（国家质量技术监督局广州电气安全检验所、广东省试验认证研究院、华安实验室） | Method for measuring content of 1, 3-propane sultone in textile |
Non-Patent Citations (4)
| Title |
|---|
| Anna Jeżewska.Determination of Propane-1,3-sultone in Workplace Air for Occupational Exposure Assessment.Int J Environ Res Public Health.2020,第17卷(第4期),第1414页. * |
| 国家市场监督管理总局/国家标准化管理委员会."纺织品α-溴代肉桂醛和1,3-丙烷磺酸内酯的测定".中华人民共和国国家标准GB/T 41416-2022.2022,第7.1节. * |
| 王成云 ; 周小琪 ; 林君峰 ; 谢堂堂 ; 褚乃清 ; .一种快速测定纺织品中1,3-丙烷磺内酯的方法.棉纺织技术.2018,第27卷(第11期),第1.2节、1.3节、2.2节. * |
| 王成云 ; 杨左军 ; 顾浩飞 ; 龙斌 ; 刘怡 ; 徐嵘 ; .软体家具用纺织品中1,3-丙烷磺内酯的测定.分析仪器.2018,(第04期),第30-34页. * |
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