CN114062549A - Rapid detection method for methyl cyclosiloxane in textile - Google Patents
Rapid detection method for methyl cyclosiloxane in textile Download PDFInfo
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- CN114062549A CN114062549A CN202111354333.0A CN202111354333A CN114062549A CN 114062549 A CN114062549 A CN 114062549A CN 202111354333 A CN202111354333 A CN 202111354333A CN 114062549 A CN114062549 A CN 114062549A
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 title claims abstract description 43
- 239000004753 textile Substances 0.000 title claims abstract description 38
- 238000001514 detection method Methods 0.000 title abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 17
- 238000005303 weighing Methods 0.000 claims abstract description 13
- 230000014759 maintenance of location Effects 0.000 claims abstract description 9
- 239000012634 fragment Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 4
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 15
- 239000012224 working solution Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000011550 stock solution Substances 0.000 claims description 8
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000004904 shortening Methods 0.000 abstract description 2
- 238000000638 solvent extraction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 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 description 2
- 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 description 2
- 239000004902 Softening Agent Substances 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229920006052 Chinlon® Polymers 0.000 description 1
- 229920000433 Lyocell Polymers 0.000 description 1
- 229920002334 Spandex Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- UXOLDCOJRAMLTQ-UHFFFAOYSA-N ethyl 2-chloro-2-hydroxyiminoacetate Chemical compound CCOC(=O)C(Cl)=NO UXOLDCOJRAMLTQ-UHFFFAOYSA-N 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000003988 headspace gas chromatography Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 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 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001850 reproductive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000009988 textile finishing Methods 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
Images
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
-
- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
-
- 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
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention provides a method for rapidly detecting methyl cyclosiloxane in textiles, which adopts a headspace-gas chromatograph to detect the methyl cyclosiloxane and comprises the following steps: (1) preparing a standard product of methyl cyclosiloxane and placing the standard product at the bottom of a headspace bottle; (2) crushing a sample to be tested into fragments with the particle size of less than 0.5mm, uniformly mixing, weighing a proper amount of the sample to be tested, and then placing the sample to be tested at the bottom of a headspace bottle; (3) and (3) respectively detecting the methylcyclosiloxane in the standard substance and the sample to be detected in the steps (1) and (2) by adopting a headspace-gas chromatograph, and carrying out qualitative and quantitative analysis according to the comparison between the retention time and the peak area of the methylcyclosiloxane. The method can quickly detect whether the textile contains the methyl cyclosiloxane, thereby shortening the detection period; and the sample does not need chemical solvent extraction pretreatment, and the detection process is simpler and more environment-friendly.
Description
Technical Field
The invention relates to the field of textile detection, in particular to a rapid detection method of methyl cyclosiloxane in textiles.
Background
The organic silicon softening agent is a commonly used after-finishing agent in the textile printing and dyeing industry, and can endow fabrics with the performances of softness, smoothness and static resistance. The use of the organic silicon softening agent can improve the wearability of textile products and improve the quality and added value of the textile products to play an important role. Octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6) are important raw materials for synthesizing organic silicon textile finishing aids, and researches show that D4 has long-term harm effect on aquatic environment and danger of weakening reproductive capacity, enters the environment mainly through modes of volatilization, waste water and the like, is enriched in organisms and generates biological harm, and D5 and D6 have similar harm. On 27.6.2018, ECHA published batch 19 high interest (SVHC), and D4, D5, D6 entered the REACH high interest (SVHC) list, and in addition, the Children Safety Product Act (CSPA) of washington, usa has listed D4 as a children high interest chemical list (CHCC). The international STANDARDs for textile product certification STANDARD 100by OEKO-TEX, Bluesign, GOTS, etc. also all incorporate the D4, D5, D6 restrictions therein. At present, the current national standard adopts a gas chromatography-mass spectrometry combined method, and the pretreatment needs to be carried out by using an organic solvent of n-hexane or tetrahydrofuran for ultrasonic extraction. The time consumption is high and the organic solvent has certain harm.
Considering that the detection rate of the methyl cyclosiloxane in the textile is relatively low in actual detection, an accurate and efficient rapid detection method is very necessary to be established for shortening the detection period, accelerating the detection speed and reducing or even avoiding the use of organic reagents.
Disclosure of Invention
The invention provides a rapid detection method for methylcyclosiloxane in textiles, aiming at the problems of long pretreatment time, adoption of an organic reagent as an extraction solvent, complex process, time consumption and the like of the existing detection method.
In order to achieve the purpose, the technical scheme of the invention is as follows: a method for rapidly detecting methyl cyclosiloxane in textiles by adopting a headspace-gas chromatograph comprises the following steps:
(1) preparing a standard product of methyl cyclosiloxane and placing the standard product at the bottom of a headspace bottle;
(2) crushing a sample to be tested into fragments with the particle size of less than 0.5mm, uniformly mixing, weighing a proper amount of the sample to be tested, and then placing the sample to be tested at the bottom of a headspace bottle;
(3) and (3) respectively detecting the methylcyclosiloxane in the standard substance and the sample to be detected in the steps (1) and (2) by adopting a headspace-gas chromatograph, and carrying out qualitative and quantitative analysis according to the comparison between the retention time and the peak area of the methylcyclosiloxane.
The invention is further set that the mass of the sample to be tested is 1-2 g, and the accuracy is 0.01 g.
The invention is further arranged that the chromatograph operating conditions of the headspace gas chromatograph are:
the chromatographic column is DB-5MS, 30.0 mm × 0.25 μm or other similar capillary columns; the column temperature is 60-80 ℃, the carrier gas is high-purity nitrogen, the column flow is 1.0-1.5 mL/min, the injection port temperature is 250-300 ℃, and no shunt injection is performed;
temperature programming: the initial temperature is 40-80 ℃, the temperature is kept for 0-5 min, the temperature is raised to 150 ℃ at the speed of 10-50 ℃/min, the temperature is raised to 280-330 ℃ at the speed of 40-80 ℃/min, and the temperature is kept for 5-10 min;
a detector: an FID detector is adopted, and the temperature of the detector is 280-330 ℃; the hydrogen flow rate is 30-60 mL/min.
The invention is further arranged that the conditions of the headspace are: the headspace temperature of the headspace automatic sample injector is 90-120 ℃, the headspace time is 30-60 min, the temperature of a gas transmission system is 100-120 ℃, the temperature of a transmission pipe is 100-120 ℃, and the sample injection interval is 10-30 min.
The invention is further configured that the preparation method of the standard substance comprises the following steps: weighing 1g of cut blank textile in a headspace bottle, sucking a standard working solution of methyl cyclosiloxane, injecting the standard working solution onto the blank textile, and obtaining a standard product of methyl cyclosiloxane after the solvent is volatilized to dry.
The invention is further configured such that the method of preparing the standard working solution comprises: accurately weighing a standard substance of methyl cyclosiloxane, taking normal hexane as a solvent, preparing a standard stock solution with the concentration of 1000-2000 +/-50 mu g/mL, and diluting the standard stock solution to prepare a standard working solution with the concentration of 0.1-200 +/-2 mu g/mL.
The invention further provides that the content of the methylcyclosiloxane is calculated according to the following formula:
X＝(Ai-Aj)×Cis/(Ais×m) (1)
wherein: x is the content of the methyl cyclosiloxane in milligrams per kilogram (mg/kg) in the sample to be tested;
Cisis the absolute mass of methylcyclosiloxane in the standard in grams (g);
Aithe area of the response peak of the methyl cyclosiloxane in the sample to be measured;
Ajthe area of the response peak of the methyl cyclosiloxane in the blank test;
Aisis the area of the response peak of the methyl cyclosiloxane in the standard;
m is the sample weight of the sample to be measured and has the unit of gram (g).
The qualitative analysis method of the methyl cyclosiloxane comprises the following steps: after detection using a headspace gas chromatography detector, the retention times of the chromatographic peaks of the sample to be detected and the standard mass are compared. And if the retention time of the mass spectrometry peak of the substance to be detected in the sample is consistent with that of the standard substance, and the allowable deviation is less than +/-2.5%, judging that the corresponding object to be detected exists in the sample.
Compared with the prior art, the detection method can quickly detect whether the textile contains the methyl cyclosiloxane, and the sample does not need chemical solvent extraction pretreatment, so that the detection is simpler; the process has no organic solvent pollution, and is more environment-friendly and healthy; the quantitative and qualitative detection of the methyl cyclosiloxane can be carried out by combining a headspace-gas chromatograph trace analysis technology, and the detection limit is 2 mg/kg; the method shortens the detection period to the maximum extent.
Drawings
FIG. 1 is a chromatogram of a methylcyclosiloxane standard (40mg/kg) in example 1.
FIG. 2 is a chromatogram of a sample to be tested in example 1.
FIG. 3 is a chromatogram of a sample to be tested in example 2.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that this example is for illustrative purposes only and is not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
EXAMPLE 1 measurement of the content of methylcyclosiloxane in textiles
(1) Weighing a standard substance of the methyl cyclosiloxane by using normal hexane as a solvent to prepare a standard stock solution with the concentration of 1000 +/-50 mg/L, and diluting the standard stock solution into standard working solutions with the low concentrations of 5mg/L, 10mg/L, 20mg/L, 30mg/L and 40mg/L step by step; weighing 1g of the cut blank textile in a headspace bottle, respectively transferring 1mL of the five standard working solutions with different concentrations, injecting the five standard working solutions into the textile in the headspace bottle, and after the solvent is volatilized to dry, obtaining a standard product of the methyl cyclosiloxane, wherein the absolute contents of the methyl cyclosiloxane in the headspace bottle are respectively: 5mg/kg, 10mg/kg, 20mg/kg, 30mg/kg, 40 mg/kg.
(2) Taking a blue-white alternate stripe textile sample, wherein the textile fiber component is 100% lyocell, shearing the textile sample into fragments or powder with the particle size of less than 0.5mm by using scissors, uniformly mixing, weighing 1g of the sheared sample to be tested, and placing the sample in another headspace bottle.
(3) And (3) respectively placing the headspace bottles filled with the standard substance and the sample to be detected in the steps (1) and (2) on a headspace-gas chromatograph for headspace-gas chromatographic analysis, wherein:
chromatographic conditions are as follows: the chromatographic column is DB-5MS, 30.0 mm multiplied by 0.25 mu m; the carrier gas is nitrogen; column temperature: 60 ℃; the column flow rate is 1.0 mL/min; the temperature of a sample inlet is 250 ℃; no shunt sampling; temperature programming: the initial temperature is 60 ℃, the temperature is kept for 3min, the temperature is increased to 150 ℃ at the speed of 40 ℃/min, and the temperature is increased to 300 ℃ at the speed of 60 ℃/min and kept for 5 min.
Headspace conditions: head space temperature: 100 ℃; headspace time: 40 min; the temperature of the gas delivery system is 120 ℃; transfer tube temperature: 120 ℃; sampling intervals: and 20 min.
A detector: a FID detector; detector temperature: 300 ℃; the hydrogen flow rate was 40 mL/min.
In this embodiment, the detection results of the standard sample and the sample to be detected are shown in fig. 1 and fig. 2, respectively, fig. 1 shows a selective ion chromatogram of the reference standard sample, in which the peaks can be separated from each other, and the peaks have sharp shapes and good symmetry; the selected monitoring ions have high sensitivity, good selectivity, less interference, wide linear range, accurate qualitative determination and low quantitative limit. The sample's selective monitoring ion chromatogram is shown in FIG. 2.
According to the detection results of the standard samples, linear equations of three substances D4, D5 and D6 are obtained, wherein y is the peak area and x is the content, as shown in Table 1.
Table 1 example 1 Retention time and Linear equation for methylcyclosiloxane
The sample to be tested and the standard sample have D4, D5 and D6 peaks at the same retention time of 5.7min, 6.5min and 7.2min, and the contents of the methyl cyclosiloxane D4, D5 and D6 in 1g of the textile sample are respectively calculated according to the formula (1): 30.41mg/kg, 30.68mg/kg, 27.04 mg/kg.
Example 2 measurement of the content of methylcyclosiloxane in textiles
(1) Weighing a standard substance of the methyl cyclosiloxane by using normal hexane as a solvent to prepare a standard stock solution with the concentration of 1000 +/-50 mg/L, and diluting the standard stock solution into standard working solutions with the low concentrations of 5mg/L, 10mg/L, 20mg/L, 30mg/L and 40mg/L step by step; weighing 1g of the cut blank textile in a headspace bottle, transferring 1mL of five standard working solutions with different concentrations respectively, injecting the five standard working solutions into the textile in the headspace bottle, and volatilizing the solvent to obtain the final product, wherein the absolute contents of the methyl cyclosiloxane in the headspace bottle are respectively as follows: 5mg/kg, 10mg/kg, 20mg/kg, 30mg/kg, 40 mg/kg.
(2) Taking a white-background red textile sample, wherein the fiber components of the sample are 9.98% of spandex and 90.02% of chinlon, shearing the sample into fragments or powder with the particle size of less than 0.5mm by using scissors, uniformly mixing, weighing 1g of the sheared sample to be detected, and placing the weighed sample in another headspace bottle.
(3) And (3) respectively placing the headspace bottles in the steps (1) and (2) on a headspace-gas chromatograph to perform headspace-gas chromatographic analysis, wherein:
chromatographic conditions are as follows: the chromatographic column is DB-5MS, 30.0 mm multiplied by 0.25 mu m; the carrier gas is nitrogen; column temperature: 60 ℃; the column flow rate is 1.0 mL/min; the temperature of a sample inlet is 250 ℃; no shunt sampling; temperature programming: the initial temperature is 60 ℃, the temperature is kept for 3min, the temperature is increased to 150 ℃ at the speed of 40 ℃/min, and the temperature is increased to 300 ℃ at the speed of 60 ℃/min and kept for 5 min.
Headspace conditions: head space temperature: 100 ℃; headspace time: 40 min; the temperature of the gas delivery system is 120 ℃; transfer tube temperature: 120 ℃; sampling intervals: and 20 min.
A detector: a FID detector; detector temperature: 300 ℃; the hydrogen flow rate was 40 mL/min.
The selective ion chromatogram of the sample to be measured in this example is shown in fig. 3.
According to the detection results of the standard samples, linear equations of three substances D4, D5 and D6 are obtained, wherein y is the peak area and x is the content, as shown in Table 2.
Table 2 example 2 Retention time and Linear equation for methylcyclosiloxane
The sample to be tested and the standard sample have D4, D5 and D6 peaks at the same retention time of 5.7min, 6.5min and 7.2min, and the contents of the methyl cyclosiloxane D4, D5 and D6 in 1g of the textile sample are respectively calculated according to the formula (1): 15.67mg/kg, 16.94mg/kg, 30.13 mg/kg.
The method for detecting the content of the methyl cyclosiloxane in the textile can shorten the detection period to the maximum extent, and enables the detection process to be simpler and more environment-friendly.
Claims (7)
1. A method for rapidly detecting methyl cyclosiloxane in textiles is characterized in that a headspace-gas chromatograph is adopted to detect the methyl cyclosiloxane, and comprises the following steps:
(1) preparing a standard product of methyl cyclosiloxane and placing the standard product at the bottom of a headspace bottle;
(2) crushing a sample to be tested into fragments with the particle size of less than 0.5mm, uniformly mixing, weighing a proper amount of the sample to be tested, and then placing the sample to be tested at the bottom of a headspace bottle;
(3) and (3) respectively detecting the methylcyclosiloxane in the standard substance and the sample to be detected in the steps (1) and (2) by adopting a headspace-gas chromatograph, and carrying out qualitative and quantitative analysis according to the comparison between the retention time and the peak area of the methylcyclosiloxane.
2. The method for rapidly detecting methyl cyclosiloxane in textile according to claim 1, wherein the mass of the sample to be detected is 1-2 g, and is accurate to 0.01 g.
3. The method for rapidly detecting methyl cyclosiloxane in textile according to claim 1, wherein the working conditions of the chromatograph of the headspace gas chromatograph are as follows:
the chromatographic column is DB-5MS, 30.0 mm × 0.25 μm or other similar capillary columns; the column temperature is 60-80 ℃, the carrier gas is high-purity nitrogen, the column flow is 1.0-1.5 mL/min, the injection port temperature is 250-300 ℃, and no shunt injection is performed;
temperature programming: the initial temperature is 40-80 ℃, the temperature is kept for 0-5 min, the temperature is raised to 150 ℃ at the speed of 10-50 ℃/min, the temperature is raised to 280-330 ℃ at the speed of 40-80 ℃/min, and the temperature is kept for 5-10 min;
a detector: an FID detector is adopted, and the temperature of the detector is 280-330 ℃; the hydrogen flow rate is 30-60 mL/min.
4. The method for rapidly detecting methylcyclosiloxane in a textile according to claim 1, wherein the headspace conditions are as follows: the headspace temperature of the headspace automatic sample injector is 90-120 ℃, the headspace time is 30-60 min, the temperature of a gas transmission system is 100-120 ℃, the temperature of a transmission pipe is 100-120 ℃, and the sample injection interval is 10-30 min.
5. The method for rapidly detecting methyl cyclosiloxane in textile according to claim 1, wherein the preparation method of the standard substance is as follows: weighing 1g of cut blank textile in a headspace bottle, sucking a standard working solution of methyl cyclosiloxane, injecting the standard working solution onto the blank textile, and obtaining a standard product of methyl cyclosiloxane after the solvent is volatilized to dry.
6. The method for rapidly detecting methyl cyclosiloxane in textile according to claim 5, wherein the preparation method of the standard working solution is as follows: accurately weighing a standard substance of methyl cyclosiloxane, taking normal hexane as a solvent, preparing a standard stock solution with the concentration of 1000-2000 +/-50 mu g/mL, and diluting the standard stock solution to prepare a standard working solution with the concentration of 0.1-200 +/-2 mu g/mL.
7. The method for rapidly detecting methyl cyclosiloxane in textile according to claim 1, wherein the content of methyl cyclosiloxane is calculated according to the following formula:
X＝(Ai-Aj)×Cis/(Ais×m) (1)
wherein: x is the content of the methyl cyclosiloxane in milligrams per kilogram (mg/kg) in the sample to be tested;
Cisis the absolute mass of methylcyclosiloxane in the standard in grams (g);
Aithe area of the response peak of the methyl cyclosiloxane in the sample to be measured;
Ajis the response of methylcyclosiloxane in blank testPeak area;
Aisis the area of the response peak of the methyl cyclosiloxane in the standard;
m is the sample weight of the sample to be measured and has the unit of gram (g).
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