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Online trapping and analyzing method for benzo[a]pyrene in thermal cracking products, and apparatus thereof

An analytical method and thermal cracking technology, applied in analytical materials, material separation, measurement devices, etc., can solve problems such as unpublished reports, and achieve the effects of improving sensitivity and selectivity, simplifying the determination method and reducing experimental errors.

Active Publication Date: 2014-04-16
YUNNAN RES INST OF TOBACCO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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  • Online trapping and analyzing method for benzo[a]pyrene in thermal cracking products, and apparatus thereof
  • Online trapping and analyzing method for benzo[a]pyrene in thermal cracking products, and apparatus thereof
  • Online trapping and analyzing method for benzo[a]pyrene in thermal cracking products, and apparatus thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1 Experimental part

[0034] 1.1 Instruments and reagents

[0035] Benzo[a]pyrene (standard substance, purity ≥99%, Chem Service Company), D 12 - Benzo[a]pyrene (standard substance, purity ≥99%, Chem Service Company).

[0036] 7890A / 5975C gas chromatography-mass spectrometry (Agilent, USA), with CIS-4 large-volume cold inlet (GERSTEL, Germany); Pyroprobe 5200 thermal cracking instrument (CDS, USA); AG204 electronic balance (sense Quantity 0.0001 g, Switzerland METTLER TOLEDO company).

[0037] 1.2 Thermal cracking conditions

[0038] Pyrolysis atmosphere: nitrogen-oxygen mixed gas containing 9% oxygen. Total pyrolysis gas flow: 4.6 mL / s

[0039] The pyrolysis probe (pyrolysis head) had an initial temperature of 300 °C, maintained for 5 s, then increased from 30 °C to 900 °C, and maintained for 5 s.

[0040] 1.3 GC-MS analysis conditions

[0041] CIS cold inlet conditions: keep at -30°C for 0.5 min, raise to 260°C at 12°C / s and hold for 1 min, then rise to 350°C a...

Embodiment 2

[0062] Embodiment two: the optimal selection of gas flow rate of pyrolyzer

[0063] Effect of different flow rates on the content of benzo[a]pyrene in the pyrolysis product. With other conditions unchanged, the flow rates of the pyrolysis gas were set to 80, 120, 160, 200, and 276 mL / min, respectively, and the content of benzo[a]pyrene in the pyrolysis products of the same sample was detected. The results are shown in Table 1. From Table 1, it can be seen that the change of different gas flow rates of the pyrolysis instrument has no significant impact on the analysis results of benzo[a]pyrene, so the pyrolysis reaction gas flow rate is selected from Baker et al. of formalaldehyde from sugars and tobacco [J]. J. Anal. Appl. Pyrolysis, 2006, 77(1): 12-21) recommended 276 mL / min.

[0064] Table 1 Contents of benzo[a]pyrene in pyrolysis products at different gas flow rates

[0065]

Embodiment 3

[0066] Embodiment three: the repeatability and detection limit of the method

[0067] The same sample was measured 5 times in parallel according to the established method. The results are shown in Table 2. The relative standard deviation (RSD) of this experimental method was 4.17%, indicating that the repeatability of the method met the experimental requirements.

[0068] Table 2 Repeatability and detection limit of the method

[0069]

[0070] Use the standard sample with the lowest concentration, repeat the sample injection 5 times, calculate the standard deviation from the measured concentration value, take 3 times the standard deviation as the detection limit of the method, and take 10 times the standard deviation as the quantitative limit of the method, the data are shown in the table 2. The detection limit of benzo[a]pyrene in this detection method is 15.30 ng / mL, and the quantification limit is 51.00 ng / mL.

[0071] From the measurement results of reproducibility, l...

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Abstract

The invention discloses an online trapping and analyzing method for benzo[a]pyrene in thermal cracking products, and an apparatus thereof, and belongs to the technical field of analytic detection. The method comprises the following steps: filling a sample into a thermal cracking chamber, carrying out aerobic thermal cracking under a programmed heating condition, directly introducing the thermal cracking products to the cold injection port of a gas chromatograph through a transmission pipeline, and trapping through refrigerating by liquid nitrogen; and carrying out programmed heating on the cold injection port after finishing the thermal cracking, allowing the thermal cracking products to be gasified and to enter a gas chromatograph-mass spectrometer, and quantitatively analyzing the benzo[a]pyrene in the thermal cracking products through adopting a selected ion mode. The apparatus comprises helium (1), a nitrogen-oxygen gas mixture (2), a triple valve (3), a flow controller (4), a flow controller (5), a handle (6), a thermal cracker (7), the transmission pipeline (8), a nut (9), an injection isolation pad (10), the cold injection port (11) and the gas chromatograph-mass spectrometer (12). According to the invention, the method has the advantages of good reappearance, high recovery rate, simple operation, and experiment error reduction; and the apparatus has a simple structure.

Description

Technical field: [0001] The invention relates to an online capture and analysis method and device for benzo[a]pyrene in thermal cracking products of additives and tobacco components, belonging to the technical field of analysis and detection. Background technique [0002] Polycyclic Aromatic Hydrocarbons (PAHs), also known as polycyclic aromatic hydrocarbons, refers to a class of compounds in which two or more benzene rings are connected in the form of condensed rings. The fused-ring aromatic hydrocarbons are mainly formed during the incomplete combustion of organic matter such as fossil fuels (such as carbon). Widely present in soil, air, plants, food, sewage, automobile exhaust and cigarette smoke. Most fused-ring aromatic hydrocarbons are toxic and carcinogenic. Since the carcinogenic effect of benzo[a]pyrene (BaP) is higher than that of other fused-ring aromatic hydrocarbons, BaP has become a hot spot of concern. [0003] Fresh tobacco leaves themselves do not contain ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 杨叶昆李雪梅徐济仓缪恩铭魏玉玲陈建华缪明明
Owner YUNNAN RES INST OF TOBACCO SCI
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