CN113203802A - Method for determining content of organic components in pentachloropropane synthesis process - Google Patents
Method for determining content of organic components in pentachloropropane synthesis process Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 63
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 22
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 22
- FTCVHAQNWWBTIV-UHFFFAOYSA-N 1,1,1,2,2-pentachloropropane Chemical compound CC(Cl)(Cl)C(Cl)(Cl)Cl FTCVHAQNWWBTIV-UHFFFAOYSA-N 0.000 title claims abstract description 18
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- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 22
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 claims description 13
- 229960003750 ethyl chloride Drugs 0.000 claims description 13
- 239000012224 working solution Substances 0.000 claims description 13
- 229940050176 methyl chloride Drugs 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- VVWFZKBKXPXGBH-UHFFFAOYSA-N 1,1,1,3,3-pentachloropropane Chemical compound ClC(Cl)CC(Cl)(Cl)Cl VVWFZKBKXPXGBH-UHFFFAOYSA-N 0.000 claims description 7
- UBOXGVDOUJQMTN-UHFFFAOYSA-N 1,1,2-trichloroethane Chemical compound ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
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- 239000012086 standard solution Substances 0.000 claims description 4
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- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 claims description 3
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 3
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 229960001701 chloroform Drugs 0.000 claims description 3
- 230000005526 G1 to G0 transition Effects 0.000 claims description 2
- 229950005499 carbon tetrachloride Drugs 0.000 claims description 2
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
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- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 229940073584 methylene chloride Drugs 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims 1
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- KYKAJFCTULSVSH-UHFFFAOYSA-N chloro(fluoro)methane Chemical compound F[C]Cl KYKAJFCTULSVSH-UHFFFAOYSA-N 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
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- 238000004817 gas chromatography Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- MSSNHSVIGIHOJA-UHFFFAOYSA-N pentafluoropropane Chemical compound FC(F)CC(F)(F)F MSSNHSVIGIHOJA-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
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- GOLXNESZZPUPJE-UHFFFAOYSA-N spiromesifen Chemical compound CC1=CC(C)=CC(C)=C1C(C(O1)=O)=C(OC(=O)CC(C)(C)C)C11CCCC1 GOLXNESZZPUPJE-UHFFFAOYSA-N 0.000 description 1
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- 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
-
- 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
-
- 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
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a method for determining the content of organic components in the synthesis process of pentachloropropane, which comprises the following steps: s1, collecting a sample, mixing the sample with deionized water, uniformly mixing the mixture in a vibration mode, and then carrying out centrifugal liquid separation; then taking the organic phase after liquid separation, dehydrating the organic phase, taking the supernatant, and filtering to obtain a sample to be detected; s2, determining the content of organic components in the sample to be detected by adopting a gas chromatograph; wherein, nitrogen is selected as carrier gas in the testing process, the column temperature program is set to be 40-80 ℃ for 5-15 min, the temperature is increased to 120-180 ℃ for 3-10 min at 5-20 ℃/min, the temperature is increased to 220-260 ℃ for 5-20 min at 10-30 ℃/min, and meanwhile, the temperature of the sample inlet is controlled to be 200-300 ℃ and the pressure is controlled to be 15-30 psi. The method for measuring the content of the organic components in the synthesis process of the pentachloropropane can simultaneously measure the content of other components generated in the synthesis process, and can be used for quality control of the synthesis process.
Description
Technical Field
The invention relates to the technical field of organic component determination, in particular to a method for determining the content of organic components in the synthesis process of pentachloropropane.
Background
Chlorofluorocarbon is a main substance which destroys the ozone layer of the atmosphere and generates greenhouse effect, and in order to protect the ecological environment in which human beings depend for survival, the international society decides to phase out and forbid the use of chlorofluorocarbon. At present, all countries in the world strive to develop foaming agents with low Ozone Depletion Potential (ODP) and low greenhouse effect potential (GWP) and less environmental impact. Research proves that 1,1,1,3, 3-pentafluoropropane (HFC-245 fa for short) is environment-friendly and gradually becomes the best substitute of chlorofluorocarbon. 1,1,1,3, 3-pentachloropropane (HCC-240 fa for short) is used as an important raw material for synthesizing HFC-245fa, and a brand new measuring method needs to be established for measuring other components generated in the synthesizing process so as to comprehensively and reliably control the quality of the HCC-240fa synthesizing process.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for measuring the content of organic components in the synthesis process of pentachloropropane, which can simultaneously measure the content of other components generated in the synthesis process and can be used for quality control of the synthesis process.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a method for determining the content of organic components in the synthesis process of pentachloropropane, which comprises the following steps:
s1, collecting a sample, mixing the sample with deionized water, uniformly mixing the mixture in a vibration mode, and then carrying out centrifugal liquid separation; then taking the organic phase after liquid separation, dehydrating the organic phase, taking the supernatant, and filtering to obtain a sample to be detected;
s2, determining the content of organic components in the sample to be detected by adopting a gas chromatograph; wherein, nitrogen is selected as carrier gas in the testing process, the column temperature program is set to be 40-80 ℃ for 5-15 min, the temperature is increased to 120-180 ℃ for 3-10 min at 5-20 ℃/min, the temperature is increased to 220-260 ℃ for 5-20 min at 10-30 ℃/min, and meanwhile, the temperature of the sample inlet is controlled to be 200-300 ℃ and the pressure is controlled to be 15-30 psi.
Further, in step S1, the rotation speed of the centrifugation is 1500-5000 rpm, and the centrifugation time is 2-10 min.
Further, in step S1, the organic phase is dehydrated by using a combination of one or more of calcium chloride, magnesium sulfate, and molecular sieve.
Further, in step S2, the stationary phase used in the gas chromatograph is 6% cyanopropyl phenyl methyl polysiloxane, and the gas chromatographic column with a length of 30-100 m, an inner diameter of 100-530 μm and a coating thickness of 0.1-3 μm is used as a separation column.
Further, in step S2, the column temperature program is set to 80 ℃ for 5min, 20 ℃/min to 180 ℃, 30 ℃/min to 260 ℃ for 5min, while the injection port temperature is set to 200 ℃ and the pressure is set to 15 psi.
Further, in step S2, the organic component includes methyl chloride and ethyl chloride, and the detected mass fraction range is 0.1-20%.
Further, in step S2, the specific steps of determining the content of the organic component in the pretreated sample by using a gas chromatograph include:
injecting a sample to be detected into a gas chromatograph, obtaining the chromatographic peak area of each component of the sample, and respectively calculating the mass fraction of each component in the sample to be detected according to the established standard curve of each component.
Further, in step S2, the analytical instrument used was composed of a gas chromatograph (Agilent 7890B) and an auto-sampler (Agilent G4513A).
Further, in step S2, a capillary column of type Agilent J & W DB-1301, 30 m.times.0.25 mm.times.1 μm was used.
Further, the method also comprises the steps of preparing a standard curve working solution and establishing a standard curve of various organic components.
Further, the specific steps of preparing the standard curve working solution are as follows:
preparing 3-5 groups of standard substance solutions with different mass fractions of known components by taking 1,1,1,3, 3-pentachloropropane as a background, wherein the mass fraction of each component is 0.1-20%; wherein the known component comprises one or more of methyl chloride, methylene chloride, trichloromethane, carbon tetrachloride, ethyl chloride, 1, 1-dichloroethane, 1, 2-dichloroethane, 1,1, 1-trichloroethane, 1,1, 2-trichloroethane.
Further, the known components comprise methyl chloride and ethyl chloride, the mass fractions of the methyl chloride standard solution are respectively 0.5%, 2%, 5%, 8% and 10%, and the mass fractions of the ethyl chloride standard solution are respectively 1%, 5%, 10%, 15% and 20%.
Further, the specific steps of establishing the standard curves of various organic components are as follows:
under the same chromatographic conditions as the sample test, respectively injecting 0.1-5 mu L of standard curve working solution into a gas chromatograph to obtain the chromatographic peak area of each component; and respectively establishing a standard curve of each component by taking the peak area of the chromatographic peak of each component as a vertical coordinate and the mass fraction of each component as a horizontal coordinate.
Compared with the prior art, the invention has the beneficial effects that:
1. the method for determining the content of the organic components in the synthesis process of the pentachloropropane has the advantages of less sample usage amount, simple operation, short analysis time, increased test sensitivity, good linearity maintenance, improved method reliability, small instrument loss and low cost consumption.
2. According to the method for determining the content of the organic components in the pentachloropropane synthesis process, the sample treatment process is completed in a closed space, so that the damage to testing personnel and the environment caused by volatilization of the sample in the pretreatment process is avoided.
Drawings
FIG. 1 is a gas chromatogram of a standard curve working solution of 9 organic components;
the reference numbers in the figures illustrate: 1. methyl chloride; 2. dichloromethane; 3. chloroform; 4. 1,1, 1-trichloroethane; 5. ethyl chloride; 6. carbon tetrachloride; 7. 1, 2-dichloroethane; 8. 1, 1-dichloroethane; 9. 1,1, 2-trichloroethane.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The experimental methods used in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used therein are commercially available without otherwise specified.
The invention provides a method for measuring the content of organic components in the synthesis process of pentachloropropane, which adopts a gas chromatograph to simultaneously measure the content of various known organic components, and comprises the following steps:
the method comprises the following steps: sample pretreatment
After the sample is collected, mixing the sample with deionized water, fully oscillating and uniformly mixing, placing the treated sample in a centrifuge, separating liquid after high-speed centrifugation (4000rpm) for 5 minutes, taking an organic phase in a sample bottle, adding calcium chloride for dewatering, and taking supernatant for filtering and storing;
step two: preparation of standard curve working solution
Preparing 5 mixed standard substance solutions with different mass fractions of known components by using 1,1,1,3, 3-pentachloropropane as a background in a standard curve working solution; wherein, the mass fractions of the chloromethane are respectively 0.5%, 2%, 5%, 8% and 10%, and the mass fractions of the chloroethane are respectively 1%, 5%, 10%, 15% and 20%;
step three: GC analysis
Selecting nitrogen as carrier gas, setting the column temperature program to 80 deg.C for 5min, raising the temperature to 180 deg.C at 20 deg.C/min, raising the temperature to 260 deg.C at 30 deg.C/min for 5min, setting the injection port temperature to 200 deg.C, and setting the pressure to 15 psi;
step four: establishing a standard curve of each component
Under the chromatographic conditions, respectively injecting 1 mu L of standard curve working solution into a gas chromatograph to obtain the chromatographic peak area of each component; respectively establishing a standard curve of each component by taking the peak area of each component chromatographic peak as a vertical coordinate and the mass fraction of each component as a horizontal coordinate;
step five: determining the content of each component in the sample to be tested
Under the chromatographic conditions, injecting a sample to be detected with the same volume into a gas chromatograph to obtain the chromatographic peak area of each component of the sample to be detected, and respectively calculating the mass fraction of each component in the sample to be detected according to the established standard curve of each component;
step six: method verification
The method is subjected to the verification of standard curve, accuracy, repeatability and reproducibility and the standard addition recovery rate.
Example 1: establishing a standard curve
Accurately weighing appropriate amounts of methyl chloride and ethyl chloride, and preparing standard curve working solutions with different mass fractions by taking 1,1,1,3, 3-pentachloropropane as a solvent, wherein the mass fractions of the methyl chloride are respectively 0.5%, 2%, 5%, 8% and 10%, and the mass fractions of the ethyl chloride are respectively 1%, 5%, 10%, 15% and 20%. And (4) sampling the solution with each concentration for 1 mu L analysis according to the chromatographic conditions of the step three to obtain a gas chromatogram of the working solution of each standard curve. The peak area of the object to be measured is used as the ordinate, the mass fraction of the object to be measured is used as the abscissa, regression calculation is carried out by using a weighted least square method, and the regression equation and the correlation coefficient of each compound are obtained, and the result is shown in table 1.
Table 19 ingredient standard curve regression equation
Example two: experiment of accuracy
Accurately weighing a proper amount of methyl chloride and ethyl chloride, taking 1,1,1,3, 3-pentachloropropane as a solvent, preparing a quality control sample with a certain mass fraction, continuously injecting samples for 6 times according to the same chromatographic conditions of the example 1, recording the measurement results of 9 compounds, and calculating the relative error values, wherein the results are shown in a table 2. As can be seen from table 2, the accuracy of the method is good.
TABLE 29 relative errors of the ingredients
Example three: repeatability and reproducibility experiments
6 parts of the same sample to be detected, 10g of each part, are precisely weighed, a person prepares a sample solution to be detected according to the method of the step one, the sample solution is respectively measured according to the chromatographic conditions of the example 1, the peak areas of 9 components are recorded, and the RSD value of the component solution is calculated, and the result is shown in a table 3, which shows that the method has good repeatability.
Table 39 repeatability of ingredients (n ═ 6)
6 parts of the same sample to be tested is precisely weighed, 2 parts of the same sample to be tested are respectively taken by 10g of each part and 3 persons, the sample solution to be tested is prepared according to the method in the step one, the peak areas of 9 components are respectively measured according to the chromatographic conditions in the example 1, and the RSD value of the components is calculated, and the result is shown in a table 4, which indicates that the method has good reproducibility.
Table 49 reproducibility of ingredients (n ═ 6)
Example four: standard recovery rate experiment
Precisely weighing 6 parts of sample to be tested, adding 5g of standard curve working solution into each part, supplementing 1,1,1,3, 3-pentachloropropane to 10g, preparing sample solution to be tested according to the method in the step one, respectively measuring according to the chromatographic conditions of the example 1, and recording the standard recovery rates of 9 components, wherein the results are shown in Table 5.
TABLE 59 recovery of spiked ingredients
Example five: sample assay
And (3) taking 8 batches of samples to be detected, precisely weighing 10g of the samples to be detected, preparing a sample solution to be detected according to the method in the step one, respectively measuring according to the chromatographic conditions of the example 1, and respectively recording the content of 9 components in each batch of samples, wherein the result is shown in table 6.
TABLE 6 content of 9 Components (wt%) of different batches of samples
In conclusion, the gas chromatography analysis method established by the invention can simultaneously determine the content of various organic components in the synthesis process of pentachloropropane, and has the advantages of simple operation, short analysis time, high result reliability and little harm to personnel and environment.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. A method for measuring the content of organic components in the synthesis process of pentachloropropane is characterized by comprising the following steps:
s1, collecting a sample, mixing the sample with deionized water, uniformly mixing the mixture in a vibration mode, and then carrying out centrifugal liquid separation; then taking the organic phase after liquid separation, dehydrating the organic phase, taking the supernatant, and filtering to obtain a sample to be detected;
s2, determining the content of organic components in the sample to be detected by adopting a gas chromatograph; wherein, nitrogen is selected as carrier gas in the testing process, the column temperature program is set to be 40-80 ℃ for 5-15 min, the temperature is increased to 120-180 ℃ for 3-10 min at 5-20 ℃/min, the temperature is increased to 220-260 ℃ for 5-20 min at 10-30 ℃/min, and meanwhile, the temperature of the sample inlet is controlled to be 200-300 ℃ and the pressure is controlled to be 15-30 psi.
2. The method for determining the content of organic components in the synthesis process of pentachloropropane according to claim 1, wherein in step S1, the rotation speed of the centrifugation is 1500-5000 rpm, and the centrifugation time is 2-10 min.
3. The method of claim 1, wherein in step S1, the organic phase is dehydrated by using a combination of one or more of calcium chloride, magnesium sulfate and molecular sieve.
4. The method of claim 1, wherein in step S2, the stationary phase used in the gas chromatograph is 6% cyanopropylphenyl-methyl polysiloxane, and the gas chromatographic column with a length of 30-100 m, an inner diameter of 100-530 μm and a coating thickness of 0.1-3 μm is used as the separation column.
5. The method of claim 1, wherein in step S2, the column temperature program is set to 80 ℃ for 5min, 20 ℃/min to 180 ℃, 30 ℃/min to 260 ℃ for 5min, the inlet temperature is set to 200 ℃, and the pressure is set to 15 psi.
6. The method for determining the content of the organic components in the synthesis process of pentachloropropane according to claim 1, wherein in step S2, the organic components include methyl chloride and ethyl chloride, and the mass fraction range of the detection is 0.1-20%.
7. The method for determining the content of organic components in the synthesis process of pentachloropropane according to claim 1, further comprising the steps of preparing a standard curve working solution and establishing a standard curve for each organic component.
8. The method for determining the content of organic components in the synthesis process of pentachloropropane according to claim 7, wherein the specific steps of preparing the standard curve working solution are as follows:
preparing 3-5 groups of standard substance solutions with different mass fractions of known components by taking 1,1,1,3, 3-pentachloropropane as a background, wherein the mass fraction of each component is 0.1-20%; wherein the known component comprises one or more of methyl chloride, methylene chloride, trichloromethane, carbon tetrachloride, ethyl chloride, 1, 1-dichloroethane, 1, 2-dichloroethane, 1,1, 1-trichloroethane, 1,1, 2-trichloroethane.
9. The method for determining the content of organic components in the synthesis process of pentachloropropane according to claim 8, wherein the known components comprise methyl chloride and ethyl chloride, the mass fraction of the methyl chloride standard solution is 0.5%, 2%, 5%, 8%, 10%, respectively, and the mass fraction of the ethyl chloride standard solution is 1%, 5%, 10%, 15%, 20%, respectively.
10. The method for determining the content of organic components in the synthesis process of pentachloropropane according to claim 7, wherein the specific steps of establishing the standard curves of various organic components are as follows:
under the same chromatographic condition with the test of a sample to be tested, respectively injecting 0.1-5 mu L of standard curve working solution into a gas chromatograph to obtain the chromatographic peak area of each component; and respectively establishing a standard curve of each component by taking the peak area of the chromatographic peak of each component as a vertical coordinate and the mass fraction of each component as a horizontal coordinate.
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| CN115876902A (en) * | 2021-09-29 | 2023-03-31 | 江苏正大清江制药有限公司 | Method for determining potential genotoxic impurities chloromethane and chloroethane in clohexine dry suspension |
Citations (4)
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| CN102998396A (en) * | 2012-12-18 | 2013-03-27 | 常州大学 | Method for determining epoxy chloropropane in water |
| CN104297397A (en) * | 2013-07-16 | 2015-01-21 | 广东省东莞市质量监督检测中心 | Detection method of content of halohydrocarbon organic substances in shoe-making treatment agent |
| CN106198775A (en) * | 2016-06-25 | 2016-12-07 | 江苏正大清江制药有限公司 | A kind of method measuring chloromethanes in gemcitabine hydrochloride, ethyl chloride |
| CN112014487A (en) * | 2019-05-30 | 2020-12-01 | 特丰制药有限公司 | Method for determining chloral hydrate or chloralkane content in preparation thereof |
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| CN115876902A (en) * | 2021-09-29 | 2023-03-31 | 江苏正大清江制药有限公司 | Method for determining potential genotoxic impurities chloromethane and chloroethane in clohexine dry suspension |
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