Method for detecting content of volatile substances in textile based on headspace-gas chromatography / mass spectrometer

Abstract

The invention discloses a method for detecting the content of volatile substances in a textile based on headspace-gas chromatography / mass spectrograph, and belongs to the technical field of volatile organic compound detection, and the method comprises the following steps: S1, cutting a sample to be detected into a proper size; s2, weighing a to-be-detected sample, putting the to-be-detected sample into a headspace bottle, adding the internal standard intermediate solution, and immediately pressing a cover; s3, placing the headspace bottle filled with the sample to be detected in a headspace-gas chromatography-mass spectrometer (HS-GC / MS) for analysis; s4, analyzing through an internal standard method to obtain the content of each volatile organic compound; the internal standard intermediate solution is prepared from an internal standard substance, and the internal standard substance is deuterated toluene. According to the method for detecting the content of the volatile substances in the textile based on the headspace-gas chromatography / mass spectrometer, the content of 21 volatile organic compounds in the textile can be rapidly detected, redundant pretreatment steps are not needed, and the method is convenient to operate, high in sensitivity and good in repeatability.

Description

Technical Field

[0001] The present invention relates to the field of volatile organic compound detection, and in particular to a method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry. Background Art

[0002] As people's living standards continue to improve, textiles are used more and more widely in daily life. From clothing to household items, textiles are in close and frequent contact with people. The quality and safety of textiles have attracted much attention, and the content of volatile substances is one of the important indicators for measuring the quality and safety of textiles.

[0003] At present, there are many standards for the limit values ​​of volatile organic compounds (VOCs) in daily textiles. For example, according to the OEKO-TEX standard, the formaldehyde limit value for baby textiles is 16mg / kg; the formaldehyde limit value for textiles that directly contact the skin is 275mg / kg, and the formaldehyde limit value for textiles and home furnishing materials that do not directly contact the skin is 300mg / kg. From the EU Directive 2002 / 231 / EC, which has different limits of 20 to 25g / pair for different types of shoes, to the 2009 Directive 2009 / 563 / EC, which has all shoes at 20g / pair, it can be seen that the EU's requirements for footwear VOCs are becoming more and more stringent.

[0004] In China, the control of VOCs in textiles, especially footwear products, relies solely on human senses to establish the odor level. This detection method is highly subjective, cannot accurately determine the type of VOCs, and is harmful to the health of test personnel. In addition, there are many types of VOCs in textiles, and how to quickly and quantitatively detect as many VOCs as possible has become a technical problem that needs to be overcome. Summary of the invention

[0005] The present invention aims to provide a method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry, which can quickly detect the content of 21 VOCs in textiles, especially footwear products, to solve the problem that VOCs cannot be quickly quantified in the prior art.

[0006] To achieve the above object, the present invention provides a method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry, comprising the following steps:

[0007] S1, cutting the sample to be tested into a suitable size;

[0008] S2, weigh the sample to be tested into the headspace bottle, add the internal standard intermediate solution, and immediately press the cap;

[0009] S3, placing the headspace bottle containing the sample to be tested in a headspace-gas chromatography-mass spectrometer (HS-GC / MS) for analysis;

[0010] S4, the content of each volatile organic compound was obtained by internal standard analysis;

[0011] The internal standard intermediate solution is prepared from an internal standard substance, and the internal standard substance is deuterated toluene.

[0012] In one embodiment, the temperature of the headspace treatment in step S3 is 120°C, the treatment time is 45 minutes, and the transfer line temperature is 140°C.

[0013] In one embodiment, the parameters of the gas chromatograph are set as follows: a DB-624 chromatographic column, an injection port temperature of 220°C, a split ratio of 100:1, a flow rate of 1.2 mL / min, a program temperature rise, an initial temperature of 40°C, maintained for 5 min, raised to 100°C at a rate of 15°C / min and maintained for 1 min, and then heated at a rate of 10°C / min.

[0014] The temperature was then raised to 150°C at a rate of 1°C / min, then immediately raised to 240°C at a rate of 20°C / min and maintained for 5 min.

[0015] In one embodiment, the parameters of the mass spectrometer are set as follows: ion source temperature 230°C, transfer line temperature 230°C.

[0016] In one embodiment, the volatile organic compounds include benzene, ethylbenzene, styrene, toluene, m-xylene, p-xylene, o-xylene, chloroform, carbon tetrachloride, 1,2-dichloroethane, 1,1,1-trichloroethane, 1,1,2-trichloroethane, 1,1,1,2-tetrachloroethane, 1,1,2,2-tetrachloroethane, pentachloroethane, 1,1-dichloroethylene, trichloroethylene, tetrachloroethylene, cyclohexanone, carbon disulfide, and hexachlorobutadiene.

[0017] Beneficial effect: The method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry provided by the present invention can quickly detect the content of 21 volatile organic compounds in textiles, does not require additional pre-treatment steps, is easy to operate, has high sensitivity and good repeatability.

[0018] In order to make the above features and advantages of the invention more obvious and easy to understand, embodiments are given below and described in detail with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 Schematic diagram of the detection results of Example 1 of the present invention.

[0020] Figure 2 This is a schematic diagram of the detection results of Example 2 of the present invention. DETAILED DESCRIPTION

[0021] In order to make the purpose and technical solution of the embodiment of the present invention clearer, the technical solution of the embodiment of the present invention will be clearly and completely described below in conjunction with the drawings of the embodiment of the present invention. Obviously, the described embodiment is a part of the embodiment of the present invention, not all of the embodiments. Based on the described embodiment of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0022] The present invention provides a method for detecting the content of 21 VOCs in textiles based on headspace-gas chromatography / mass spectrometry. The information of the 21 VOCs to be tested is shown in Table 1:

[0023] Table 1 Information of the object to be tested

[0024] No. Compound CAS No. Quantitative ion Qualifier ions 1 benzene 71-43-2 78 77 / 51 2 Ethylbenzene 100-41-4 91 106 / 92 3 Styrene 100-42-5 104 103 / 78 / 51 4 Toluene 108-88-3 91 92 / 89 5 Meta-Xylene 108-38-3 91 106 / 105 6 p-Xylene 106-42-3 91 106 / 105 7 o-Xylene 95-47-6 91 106 / 78 8 Chloroform 67-66-3 83 85 / 47 9 Carbon tetrachloride 56-23-5 117 118 / 119 / 82 10 1,2-Dichloroethane 107-06-2 62 64 / 49 / 98 11 1,1,1-Trichloroethane 71-55-6 97 99 / 61 / 117 12 1,1,2-Trichloroethane 79-00-5 97 83 / 61 13 1,1,1,2-Tetrachloroethane 630-20-6 131 117 / 95 14 1,1,2,2-Tetrachloroethane 79-34-5 97 83 / 99 / 61 15 Pentachloroethane 76-01-7 167 171 / 130 16 1,1-Dichloroethylene 75-35-4 96 98 / 63 17 Trichloroethylene 79-01-6 95 130 / 132 18 Tetrachloroethylene 127-18-4 166 164 / 131 19 Cyclohexanone 108-94-1 55 98 / 42 20 Carbon disulfide 75-15-0 76 78 / 44 / 32 21 Hexachlorobutadiene 87-68-3 225 190 / 118

[0025] The headspace gas chromatography mass spectrometry (HS-GC / MS) analysis includes the following steps:

[0026] S1, cutting the sample to be tested into a suitable size, preferably 3mm*3mm;

[0027] S2, weigh the sample to be tested into the headspace bottle, add the internal standard intermediate solution, and immediately press the cap;

[0028] S3, the headspace bottle containing the sample to be tested is analyzed by headspace gas chromatography-mass spectrometry (HS-GC / MS);

[0029] S4, the content of each volatile organic compound was obtained by internal standard analysis.

[0030] In this method, the internal standard is deuterated toluene, and the information is shown in Table 2:

[0031] Table 2 Internal standard information

[0032] No. Compound CAS No. Quantitative ion Qualifier ions 1 Deuterated toluene 2037-26-5 98 100

[0033] In step S3, the headspace-gas chromatography-mass spectrometry (HS-GC / MS) parameters are set as shown in Table 3:

[0034] Table 3 HS-GC / MS instrument parameters

[0035]

[0036]

[0037] The present invention will be further described below in conjunction with specific embodiments:

[0038] Example 1

[0039] This embodiment provides a method for detecting the content of 21 VOCs in footwear products based on headspace-gas chromatography / mass spectrometry, comprising the following steps:

[0040] S1, cut the footwear sample into 3mm*3mm size;

[0041] S2, weigh (1.000±0.001) g of the sample to be tested into a 20 mL headspace bottle, add 10 μL of the internal standard intermediate solution, and immediately cap it;

[0042] S3, the headspace sample containing the sample to be tested is analyzed by headspace gas chromatography-mass spectrometry (HS-GC / MS), and the instrument parameters are set as follows:

[0043] The temperature of the headspace treatment was 120°C, the treatment time was 45 min, and the transfer line temperature was 140°C;

[0044] The parameters of the gas chromatograph were set as follows: DB-624 (60m×0.25mm×1.4μm) chromatographic column, injection port temperature 220℃, split ratio 100:1, flow rate 1.2mL / min. The temperature was programmed: the initial temperature was 40℃, maintained for 5min, then increased to 100℃ at a rate of 15℃ / min and maintained for 1min, then increased to 150℃ at a rate of 10℃ / min, and immediately increased to 240℃ at a rate of 20℃ / min, and maintained for 5min;

[0045] The parameters of the mass spectrometer were set as follows: ion source temperature 230°C, transfer line temperature 230°C.

[0046] S4, the content of each volatile organic compound was obtained by internal standard analysis.

[0047] Test results such as Figure 1 As shown, Figure 1 middle:

[0048] 1: 1,1-dichloroethylene; 2: carbon disulfide; 3: chloroform; 4: 1,1,1-trichloroethane; 5: carbon tetrachloride; 6: benzene; 7: 1,2-dichloroethane; 8: trichloroethylene; 9: toluene; 10: 1,1,2-trichloroethane; 11: tetrachloroethylene; 12: ethylbenzene; 13: 1,1,1,2-tetrachloroethane; 14: m-xylene; 15: p-xylene; 16: styrene; 17: o-xylene; 18: cyclohexanone; 19: 1,1,2,2-tetrachloroethane; 20: pentachloroethane; 21: hexachlorobutadiene; 22: deuterated toluene.

[0049] Example 2

[0050] This embodiment provides a method for detecting the content of 21 VOCs in textile products based on headspace-gas chromatography / mass spectrometry. The difference between this embodiment and embodiment 1 is only that the detection object is different.

[0051] Test results such as Figure 2 As shown, according to Figure 2 The results of carbon disulfide and toluene in textile products were 56μg / kg and 46μg / kg respectively.

[0052] Example 3

[0053] Using the method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry provided by the present invention, 21 compounds with a concentration of 20 μg were tested repeatedly 6 times. The results are shown in the following table. The results show that the method has good repeatability.

[0054]

[0055] In summary, the method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry provided by the present invention can quickly detect the content of 21 volatile organic compounds in textiles, does not require unnecessary pretreatment steps, is easy to operate, has high sensitivity and good repeatability.

[0056] Although the present invention has been disclosed as above by way of embodiments, it is not intended to limit the present invention. Any person having ordinary knowledge in the technical field may make some changes and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention shall be determined by the scope of the attached patent application.

Claims

1. A method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry, characterized in that: The following steps are involved: S1, cutting the sample to be tested into a suitable size; S2, weigh the sample to be tested into the headspace bottle, add the internal standard intermediate solution, and immediately press the cap; S3, placing the headspace bottle containing the sample to be tested in a headspace-gas chromatography-mass spectrometer (HS-GC / MS) for analysis; S4, the content of each volatile organic compound was obtained by internal standard analysis; The internal standard intermediate solution is prepared from an internal standard substance, and the internal standard substance is deuterated toluene.

2. The method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry according to claim 1, characterized in that: In step S3, the temperature of the headspace treatment is 120°C, the treatment time is 45 min, and the transfer line temperature is 140°C.

3. The method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry according to claim 2, characterized in that: The parameters of the gas chromatograph were set as follows: a DB-624 column, an injection port temperature of 220°C, a split ratio of 100:1, a flow rate of 1.2 mL / min, and a programmed temperature rise with an initial temperature of 40°C, maintained for 5 min, raised to 100°C at a rate of 15°C / min and maintained for 1 min, then raised to 150°C at a rate of 10°C / min, and immediately raised to 240°C at a rate of 20°C / min and maintained for 5 min.

4. The method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry according to claim 3, characterized in that: The parameters of the mass spectrometer were set as follows: ion source temperature 230°C, transfer line temperature 230°C.

5. The method for detecting the content of volatile substances in textiles based on headspace-gas chromatography / mass spectrometry according to claim 1, characterized in that: The volatile organic compounds include benzene, ethylbenzene, styrene, toluene, m-xylene, p-xylene, o-xylene, chloroform, carbon tetrachloride, 1,2-dichloroethane, 1,1,1-trichloroethane, 1,1,2-trichloroethane, 1,1,1,2-tetrachloroethane, 1,1,2,2-tetrachloroethane, pentachloroethane, 1,1-dichloroethylene, trichloroethylene, tetrachloroethylene, cyclohexanone, carbon disulfide, and hexachlorobutadiene.

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