CN111929384A - Method for determining content of residual methyl siloxane in organic silicon softening agent by using HS-GC external standard method - Google Patents
Method for determining content of residual methyl siloxane in organic silicon softening agent by using HS-GC external standard method Download PDFInfo
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- -1 methyl siloxane Chemical class 0.000 title claims abstract description 43
- 238000010812 external standard method Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 8
- 239000010703 silicon Substances 0.000 title claims abstract description 8
- 239000004902 Softening Agent Substances 0.000 title claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 20
- 238000004458 analytical method Methods 0.000 claims abstract description 10
- 239000012159 carrier gas Substances 0.000 claims abstract description 4
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 33
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 20
- 239000012086 standard solution Substances 0.000 claims description 15
- 239000004671 silicon softener Substances 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 229920001296 polysiloxane Polymers 0.000 claims description 7
- 239000012488 sample solution Substances 0.000 claims description 7
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 239000011550 stock solution Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- IUMSDRXLFWAGNT-UHFFFAOYSA-N Dodecamethylcyclohexasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 IUMSDRXLFWAGNT-UHFFFAOYSA-N 0.000 claims description 5
- HTDJPCNNEPUOOQ-UHFFFAOYSA-N hexamethylcyclotrisiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 claims description 5
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 239000013043 chemical agent Substances 0.000 claims description 2
- 238000004817 gas chromatography Methods 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- 238000004445 quantitative analysis Methods 0.000 claims description 2
- 239000012898 sample dilution Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 238000000638 solvent extraction Methods 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000012491 analyte Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000219 mutagenic Toxicity 0.000 description 1
- 230000003505 mutagenic effect Effects 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001850 reproductive effect Effects 0.000 description 1
- 210000004994 reproductive system Anatomy 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000009988 textile finishing Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- 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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
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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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
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Abstract
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for determining the content of residual methyl siloxane in an organic silicon softening agent by using an HS-GC external standard method. Detecting by using a headspace gas chromatograph, and quantitatively analyzing by using an external standard method, wherein the gas chromatograph is an Agilent gas chromatograph 7890B, and the gas chromatographic analysis conditions are as follows: the chromatographic column is DB-1701 or chromatographic column with equivalent polarity, the column length is 30m, the column inner diameter is 320 μm, the initial column temperature is 100 deg.C, maintaining for 2min, then heating to 260 deg.C at the rate of 10 deg.C/min, maintaining for 10min, and the carrier gas flow rate is 3 mL/min. The method has the advantages of high precision, good reproducibility, no need of any solvent extraction pretreatment operation on the sample, reduced organic solvent consumption, shortened analysis time, and simple and safe method.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for determining the content of residual methyl siloxane in an organic silicon softening agent by using an HS-GC external standard method.
Background
Because the organic silicon has the advantages of good lubricity, softness, hydrophobicity and the like, the organic silicon softener has wide application in textile finishing and is a softener with outstanding performance and effect. The main raw materials for synthesizing the organosilicon softener are octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane and the like. However, it has been found that hexamethylcyclotrisiloxane (hereinafter referred to as D3), octamethylcyclotetrasiloxane (hereinafter referred to as D4), decamethylcyclopentasiloxane (hereinafter referred to as D5) and dodecamethylcyclohexasiloxane (hereinafter referred to as D6) have long-term harmful effects on the aquatic environment and have a potential risk of impairing reproductive ability. Methylsiloxane has been reported in the literature to be toxic to the nervous, immune and reproductive systems of the human body, being carcinogenic and mutagenic. And methyl siloxane such as D3, D4, D5, D6 and the like also has high volatility and high diffusion coefficient, and is easy to diffuse out of the organic silicon product, so that the organic silicon product enters human bodies and the environment to cause damage.
However, the residual amounts of D3, D4, D5 and D6 in the silicone softener are analyzed at present, and in the existing few analysis methods, a large amount of organic solvent is required for extraction, so that the operation process is complex, the error is large, and the method has certain harm to the bodies of analysis experimenters.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method for determining the content of the residual methyl siloxane in the organic silicon softener by using the HS-GC external standard method has the advantages of high precision, good reproducibility, capability of realizing direct quantification of a sample, avoidance of using a large amount of solvents, short analysis time, simplicity, practicability, safety and reliability.
The method for determining the content of the residual methyl siloxane in the organic silicon softener by using the HS-GC external standard method adopts a headspace gas chromatograph to carry out detection and quantitative analysis by using the external standard method, wherein the gas chromatograph is an Agilent gas chromatograph 7890B, and the gas chromatographic analysis conditions are as follows: the chromatographic column is DB-1701 or chromatographic column with equivalent polarity, the column length is 30m, the column inner diameter is 320 μm, the initial column temperature is 100 deg.C, maintaining for 2min, then heating to 260 deg.C at the rate of 10 deg.C/min, maintaining for 10min, and the carrier gas flow rate is 3 mL/min.
Wherein:
the gas chromatography conditions further include: the temperature of a sample inlet is 250 ℃, split-flow sample injection is adopted, the split-flow ratio is 25:1, and the sample injection amount is 20 mu L; a hydrogen flame detector is adopted, the temperature of the detector is 260 ℃, the hydrogen flow rate is 30mL/min, and the air flow rate is 300 mL/min.
The sampling mode is headspace sampling, the headspace sampler used for headspace sampling is an Agilent 7697A headspace sampler, and the using conditions are as follows: equilibrate at 130 ℃ for 30 min.
The methyl siloxane is one or more than one of hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane or dodecamethylcyclohexasiloxane.
The method for determining the content of the residual methyl siloxane in the organosilicon softener by using an HS-GC external standard method comprises the following specific steps:
(1) preparing a standard solution: respectively weighing 50.0mg of each methylsiloxane component standard substance in a beaker, diluting with n-hexane, transferring into a 500mL volumetric flask, and adding the n-hexane to a constant volume to a scale to prepare 100mg/L stock solution VI; then accurately transferring 10.00mL, 20.00mL, 30.00mL, 40.00mL and 50.00mL of each stock solution VI into 5 100mL volumetric flasks, fixing the volume of normal hexane to a scale, and obtaining standard solutions I, II, III, IV and V from each methyl siloxane component, wherein the concentrations of the standard solutions are 10.0mg/L, 20.0mg/L, 30.0mg/L, 40.0mg/L and 50.0mg/L respectively;
(2) preparing an organic silicon softener sample solution: accurately weighing a certain amount of sample in a 100mL volumetric flask according to the content range of the methyl siloxane in the sample, and fixing the volume of normal hexane to ensure that the concentration of each methyl siloxane component is 10-50 mg/L during measurement;
(3) analysis by a headspace gas chromatograph: analysis by a headspace gas chromatograph: shaking up standard solutions I, II, III, IV and V of each methylsiloxane component, precisely measuring 10mL of the standard solutions respectively in a special headspace sample introduction bottle, balancing headspace at 130 ℃ for 30min, analyzing the headspace samples by using a gas chromatograph, simultaneously recording the peak area of each methylsiloxane component, and drawing a content-peak area standard curve of each methylsiloxane component by using an external standard method to obtain a standard curve regression equation; and then analyzing the organic silicon softener sample solution, recording the peak area of each methyl siloxane component, and calculating the corresponding methyl siloxane content, namely the mass fraction of the methyl siloxane according to a standard curve regression equation.
The standard curve regression equation is X N C V/m, wherein:
x is the content of methyl siloxane monomer in the sample, and the unit is g/Kg;
n is sample dilution times;
c-methylsiloxane content, in mg/mL, read from a standard working curve;
v is the volume of the sample solution in mL;
m is the mass of the sample in g.
The standard product of the methylsiloxane component described in step (1) was produced by the national pharmaceutical group chemical agents limited.
Linear correlation coefficient R of standard curve of method2≥99.9％。
A medium concentration standard solution should be added after every 50 sample measurements, and if the measured data differ from the original value by more than 3%, the standard curve should be reproduced.
After the sample is heated and balanced by a headspace sample injector, the sample is detected by a hydrogen flame ionization detector, and qualitative retention time and quantitative determination are carried out by an external standard method.
And (3) qualitative confirmation: under the instrument conditions, chromatographic peaks of the sample solution to be tested and the standard appear at the same retention time (+ -0.1 min), at which time the target analyte can be qualitatively confirmed.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention has high precision, good reproducibility, high accuracy and good repeatability, and can realize accurate test on samples.
(2) The method can be used for directly testing the content of each methyl siloxane component in the organic silicon softener, does not need to perform any solvent extraction pretreatment operation on a sample, shortens the analysis time, and is simple, safe, convenient and reliable.
Drawings
FIG. 1 is a standard curve of the content-peak area of hexamethylcyclotrisiloxane (D3);
FIG. 2 is a content-peak area standard curve of octamethylcyclotetrasiloxane (D4);
FIG. 3 is a content-peak area standard curve for decamethylcyclopentasiloxane (D5);
FIG. 4 is a content-peak area standard curve for dodecamethylcyclohexasiloxane (D6);
FIG. 5 is a standard chromatogram;
FIG. 6 is a chromatogram for detection of a sample in example 1.
Detailed Description
The invention is further described below with reference to the accompanying drawings and examples.
Example 1
1. Preparing an instrument:
adopting Agilent 7890B gas chromatograph, 7697A headspace sample injector to perform headspace sample injection, and balancing at 130 deg.C for 30 min; the chromatographic column is DB-1701 (or chromatographic column with equivalent polarity), the column length is 30m, the column inner diameter is 320 μm, the initial column temperature is 100 ℃, the temperature is kept for 2min, then the temperature is raised to 260 ℃ at the speed of 10 ℃/min, the temperature is kept for 10min, and the flow rate of carrier gas is 3 mL/min; the temperature of a sample inlet is 250 ℃, split-flow sample injection is adopted, the split-flow ratio is 251, and the sample injection amount is 20 mu L; and the hydrogen flame detector detects that the temperature is 260 ℃, the hydrogen flow rate is 30mL/min, and the air flow rate is 300 mL/min.
2. Drawing of standard curve
Preparing a standard solution: respectively and accurately weighing 50mg of standard substances of D3, D4, D5 and D6 in a beaker, diluting the standard substances with n-hexane, transferring the diluted standard substances into a 500mL volumetric flask, and adding the n-hexane to a constant volume to a scale to prepare 100mg/L stock solution VI; then accurately transferring 10.00mL, 20.00mL, 30.00mL, 40.00mL and 50.00mL from each stock solution VI into 5 100mL volumetric flasks, metering the volume to scale by using n-hexane, and obtaining standard solutions I, II, III, IV and V by using D3, D4, D5 and D6 respectively, wherein the concentrations of the standard solutions D3, D4, D5 and D6 are respectively 10.0mg/L, 20.0mg/L, 30.0mg/L, 40.0mg/L and 50.0 mg/L;
taking 10mL of standard solutions of D3, D4, D5 and D6 in a special headspace sample bottle respectively, injecting samples under the chromatographic conditions and obtaining standard working curves of D3, D4, D5 and D6 respectively, and the standard working curves are shown in figures 1-4.
3. The standard chromatogram is shown in FIG. 5.
4. Determination of samples
Accurately weighing 2.0253g of an organosilicon softener sample into a 100mL volumetric flask, carrying out constant volume on n-hexane, putting 10mL of a solution to be tested into a special headspace sample feeding bottle, carrying out sample feeding under the chromatographic condition to obtain a sample curve chart 6, and directly calculating the result by an external standard method, wherein the contents of residual D3, D4, D5 and D6 are respectively 0ppm, 1065ppm, 747ppm and 982 ppm.
5. The results show that: the method is adopted to carry out quantitative determination on the contents of D3, D4, D5 and D6 remained in the organosilicon softener, and has accurate analysis, simple operation and high precision.
Claims (7)
1. A method for determining the content of residual methyl siloxane in an organic silicon softening agent by using an HS-GC external standard method is characterized by comprising the following steps: detecting by using a headspace gas chromatograph, and quantitatively analyzing by using an external standard method, wherein the gas chromatograph is an Agilent gas chromatograph 7890B, and the gas chromatographic analysis conditions are as follows: the chromatographic column is DB-1701 or chromatographic column with equivalent polarity, the column length is 30m, the column inner diameter is 320 μm, the initial column temperature is 100 deg.C, maintaining for 2min, then heating to 260 deg.C at the rate of 10 deg.C/min, maintaining for 10min, and the carrier gas flow rate is 3 mL/min.
2. The method of determining the residual methylsiloxane content of silicone softener by HS-GC external standard method as claimed in claim 1, wherein: the gas chromatography conditions further include: the temperature of a sample inlet is 250 ℃, split-flow sample injection is adopted, the split-flow ratio is 25:1, and the sample injection amount is 20 mu L; a hydrogen flame detector is adopted, the temperature of the detector is 260 ℃, the hydrogen flow rate is 30mL/min, and the air flow rate is 300 mL/min.
3. The method of determining the residual methylsiloxane content of silicone softener by HS-GC external standard method as claimed in claim 1, wherein: the sampling mode is headspace sampling, the headspace sampler used for headspace sampling is an Agilent 7697A headspace sampler, and the using conditions are as follows: equilibrate at 130 ℃ for 30 min.
4. The method of determining the residual methylsiloxane content of silicone softener by HS-GC external standard method as claimed in claim 1, wherein: the methyl siloxane is one or more than one of hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane or dodecamethylcyclohexasiloxane.
5. The method of determining the residual methylsiloxane content of silicone softener by HS-GC external standard method as claimed in claim 1, wherein: the detection and external standard quantitative analysis by adopting a headspace gas chromatograph comprise the following specific steps:
(1) preparing a standard solution: respectively weighing 50.0mg of each methylsiloxane component standard substance in a beaker, diluting with n-hexane, transferring into a 500mL volumetric flask, and adding the n-hexane to a constant volume to a scale to prepare 100mg/L stock solution VI; then accurately transferring 10.00mL, 20.00mL, 30.00mL, 40.00mL and 50.00mL of each stock solution VI into 5 100mL volumetric flasks, fixing the volume of normal hexane to a scale, and obtaining standard solutions I, II, III, IV and V from each methyl siloxane component, wherein the concentrations of the standard solutions are 10.0mg/L, 20.0mg/L, 30.0mg/L, 40.0mg/L and 50.0mg/L respectively;
(2) preparing an organic silicon softener sample solution: accurately weighing a certain amount of sample in a 100mL volumetric flask according to the content range of the methyl siloxane in the sample, and fixing the volume of normal hexane to ensure that the concentration of each methyl siloxane component is 10-50 mg/L during measurement;
(3) analysis by a headspace gas chromatograph: analysis by a headspace gas chromatograph: shaking up standard solutions I, II, III, IV and V of each methylsiloxane component, precisely measuring 10mL of the standard solutions respectively in a special headspace sample introduction bottle, balancing headspace at 130 ℃ for 30min, analyzing the headspace samples by using a gas chromatograph, simultaneously recording the peak area of each methylsiloxane component, and drawing a content-peak area standard curve of each methylsiloxane component by using an external standard method to obtain a standard curve regression equation; and then analyzing the organic silicon softener sample solution, recording the peak area of each methyl siloxane component, and calculating the corresponding methyl siloxane content, namely the mass fraction of the methyl siloxane according to a standard curve regression equation.
6. The method of determining residual methyl siloxane content in silicone softener by HS-GC external standard method according to claim 5, characterized in that: the standard curve regression equation is X N C V/m, wherein:
x is the content of methyl siloxane monomer in the sample, and the unit is g/Kg;
n is sample dilution times;
c-methylsiloxane content, in mg/mL, read from a standard working curve;
v is the volume of the sample solution in mL;
m is the mass of the sample in g.
7. The method of determining residual methyl siloxane content in silicone softener by HS-GC external standard method according to claim 5, characterized in that: the standard product of the methylsiloxane component described in step (1) was produced by the national pharmaceutical group chemical agents limited.
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Cited By (3)
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| CN112924585A (en) * | 2021-01-28 | 2021-06-08 | 河南师范大学 | Qualitative analysis method of linear dimethyl siloxane in polydimethylsiloxane |
| CN113884602A (en) * | 2021-11-11 | 2022-01-04 | 扬州晨化新材料股份有限公司 | Method for detecting content of residual cyclosiloxane of organic silicon fabric finishing agent |
| CN114062549A (en) * | 2021-11-12 | 2022-02-18 | 上海市质量监督检验技术研究院 | Rapid detection method for methyl cyclosiloxane in textile |
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