Method for measuring benzene and benzene, toluene, ethylbenzene and xylenes(BTEX) content of polypropylene fiber bundles and filter rods of cigarettes

Abstract

The invention discloses a method for measuring the benzene and BTEX content of polypropylene fiber bundles and filter rods of cigarettes, which comprises the steps of preparation of internal standard extraction liquid, standard working solution and sample solution, gas chromatography-mass spectrometry, calculation of measurement results and the like. The measurement method, which is improved and optimized, has the advantages of simple and accurate operation, high sensitivity, high recovery rate, high repeatability and the like. The method of the invention has the advantages that: the quantityis fixed according to internal standards, so errors caused by pretreatment or the precision of instruments are reduced effectively; the adopted chromatographic conditions ensure high separation degrees and high linear correlation of both six target compounds and internal standard chromatographic peaks, and the detection limit is between 0.01 and 0.02mu g / g; and the sample recovery rate is between95 and 101 percent and the average relative standard deviation is between 4.1 and 5.0.

Description

technical field

[0001] The invention relates to a method for measuring the content of benzene and benzene series in acrylic fiber tow and a filter rod for cigarettes, and belongs to the technical field of physical and chemical inspection of cigarette materials. Background technique

[0002] With the increasing progress of manufacturing technology, filter rods made of polypropylene fiber tow (hereinafter referred to as polypropylene fiber filter rods) are more and more widely used in tobacco companies. However, in the manufacturing process of propylene fiber filter rods, in order to improve the properties such as hardness, elasticity and forming rate of propylene fiber filter rods, it is necessary to add some special curing adhesives, and these special adhesives are often accompanied by different degrees of peculiar smell, even There are volatile harmful components, among which benzene substances, especially benzene, are extremely toxic, and benzene can greatly damage the bon...

Examples

Embodiment 1

[0035] The method for measuring the content of benzene and benzene series in the propylene fiber tow for cigarettes in this embodiment is as follows (the flow chart of the measurement method is as follows: figure 1 shown)

[0036] 1. Preparation of internal standard extract:

[0037] (1) Preparation of internal standard stock solution I: Accurately weigh 100.0mg of naphthalene in a 100mL volumetric flask, dissolve it with n-pentane, adjust the volume to the mark and mix well to obtain internal standard stock solution I with a concentration of 1mg / mL; The internal standard stock solution I is stored in a sealed refrigerator at 4°C, and the validity period is 3 months;

[0038] (2) Preparation of internal standard stock solution II: Accurately pipette 1 mL of internal standard stock solution I into a 50 mL volumetric flask, dilute to the mark with n-pentane and mix well to obtain internal standard solution II with a concentration of 20 μg / mL; The internal standard stock soluti...

Embodiment 2

[0062] The method for determining the content of benzene and benzene series in the propylene fiber filter stick for cigarettes in this embodiment is as follows

[0063] 1. Preparation of sample solution

[0064] Accurately weigh 4.00g of propylene fiber filter stick, cut the filter stick sample with scissors, then put it into a 100mL Erlenmeyer flask, add 50mL of internal standard extract (internal standard extract prepared in Example 1) and shake After extracting for 1 hour, the supernatant was the sample solution, and 2 mL of the supernatant was used for gas chromatography-mass spectrometry analysis;

[0065] 2, adopt the chromatographic mass spectrometry condition analysis sample solution among the embodiment 1;

[0066] 3. The chromatographic peak area ratios of 6 kinds of benzene and benzene series and internal standard naphthalene will be recorded, and substituted into the standard curve drawn in Example 1 to obtain the content of benzene and benzene series in the sa...

Embodiment 3

[0069] The present embodiment is as follows to the detection method of the repeatability of the inventive method and the standard addition recovery rate

[0070] Add 3 different concentrations of standard working solutions to the sample (the concentration of each component in the standard solution is 0.002 μg / mL, 0.01 μg / mL, 0.05 μg / mL), the concentration of the internal standard is 0.02 μg / mL, Each sample is measured 5 times respectively, and the condition of chromatographic mass spectrometry analysis is with the chromatographic mass spectrometry analysis condition of embodiment 1, calculates according to the analysis result the standard addition recovery rate of benzene and benzene series in this method cigarette propylene fiber tow and filter stick and The relative standard deviation of measured value after adding the standard, the result is as shown in table 5;

[0071]

[0072] It can be seen from Table 5 that the recoveries of the six compounds are between 95% and 101...

technical field

[0001] The invention relates to a method for measuring the content of benzene and benzene series in acrylic fiber tow and a filter rod for cigarettes, and belongs to the technical field of physical and chemical inspection of cigarette materials. Background technique

[0002] With the increasing progress of manufacturing technology, filter rods made of polypropylene fiber tow (hereinafter referred to as polypropylene fiber filter rods) are more and more widely used in tobacco companies. However, in the manufacturing process of propylene fiber filter rods, in order to improve the properties such as hardness, elasticity and forming rate of propylene fiber filter rods, it is necessary to add some special curing adhesives, and these special adhesives are often accompanied by different degrees of peculiar smell, even There are volatile harmful components, among which benzene substances, especially benzene, are extremely toxic, and benzene can greatly damage the bon...

Examples

Embodiment 1

[0035] The method for measuring the content of benzene and benzene series in the propylene fiber tow for cigarettes in this embodiment is as follows (the flow chart of the measurement method is as follows: figure 1 shown)

[0036] 1. Preparation of internal standard extract:

[0037] (1) Preparation of internal standard stock solution I: Accurately weigh 100.0mg of naphthalene in a 100mL volumetric flask, dissolve it with n-pentane, adjust the volume to the mark and mix well to obtain internal standard stock solution I with a concentration of 1mg / mL; The internal standard stock solution I is stored in a sealed refrigerator at 4°C, and the validity period is 3 months;

[0038] (2) Preparation of internal standard stock solution II: Accurately pipette 1 mL of internal standard stock solution I into a 50 mL volumetric flask, dilute to the mark with n-pentane and mix well to obtain internal standard solution II with a concentration of 20 μg / mL; The internal standard stock soluti...

Embodiment 2

[0062] The method for determining the content of benzene and benzene series in the propylene fiber filter stick for cigarettes in this embodiment is as follows

[0063] 1. Preparation of sample solution

[0064] Accurately weigh 4.00g of propylene fiber filter stick, cut the filter stick sample with scissors, then put it into a 100mL Erlenmeyer flask, add 50mL of internal standard extract (internal standard extract prepared in Example 1) and shake After extracting for 1 hour, the supernatant was the sample solution, and 2 mL of the supernatant was used for gas chromatography-mass spectrometry analysis;

[0065] 2, adopt the chromatographic mass spectrometry condition analysis sample solution among the embodiment 1;

[0066] 3. The chromatographic peak area ratios of 6 kinds of benzene and benzene series and internal standard naphthalene will be recorded, and substituted into the standard curve drawn in Example 1 to obtain the content of benzene and benzene series in the sa...

Embodiment 3

[0069] The present embodiment is as follows to the detection method of the repeatability of the inventive method and the standard addition recovery rate

[0070] Add 3 different concentrations of standard working solutions to the sample (the concentration of each component in the standard solution is 0.002 μg / mL, 0.01 μg / mL, 0.05 μg / mL), the concentration of the internal standard is 0.02 μg / mL, Each sample is measured 5 times respectively, and the condition of chromatographic mass spectrometry analysis is with the chromatographic mass spectrometry analysis condition of embodiment 1, calculates according to the analysis result the standard addition recovery rate of benzene and benzene series in this method cigarette propylene fiber tow and filter stick and The relative standard deviation of measured value after adding the standard, the result is as shown in table 5;

[0071]

[0072] It can be seen from Table 5 that the recoveries of the six compounds are between 95% and 101...

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