CN103675089B - A kind of method analyzing coal tar pyrolysis low molecule product - Google Patents
A kind of method analyzing coal tar pyrolysis low molecule product Download PDFInfo
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- CN103675089B CN103675089B CN201310655604.5A CN201310655604A CN103675089B CN 103675089 B CN103675089 B CN 103675089B CN 201310655604 A CN201310655604 A CN 201310655604A CN 103675089 B CN103675089 B CN 103675089B
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Abstract
Analyzing a method for coal tar pyrolysis low molecule product, the method adopts the steps such as sample acquisition, original position pyrolysis flying time mass spectrum analysis, data analysis. Through temperature programming flying time mass spectrum analysis after tar is obtained, it is possible to the composition of detection coal tar main low molecule product in pyrolytic process and occuring regularity, system is highly sensitive, good resolution. Utilize ultraviolet light photo from (PI) source as ionizer, ionization process can not produce fragment ion, to understanding coal tar structure with instruct tar to utilize there is important meaning.
Description
Technical field
The invention belongs to mass spectroscopy field, it is specifically related to a kind of method utilizing temperature programming flying time mass spectrum analysis coal tar pyrolysis low molecule product.
Background technology
Coal tar is a kind of black or brown thick liquid, is the by product when dry distillation of coal coke and coal gas. Its pyrolysis product not only directly can burn as fuel, also can be used for fractionation phenols, aromatic hydrocarbon, alkane class etc., and can be used for manufacturing other dyestuff or medicines etc. Therefore, its pyrolysis product is precipitated out to the research of rule, contribute to the utilization ratio improving coal tar to have important meaning.
Research for coal tar group part mainly contains nuclear magnetic resonance method (H-NMR), GC-MS, the methods such as Ultraluminescence spectrum, but these methods can only detect the composition of tar, and can not reflect composition and the occuring regularity of tar main low molecule product in pyrolytic process, and sample needs responsible pre-treatment process. And the group part for coal tar pyrolysis product studies mainly thermogravimetry, by the variation relation of measure sample quality and temperature, determine group part of sample, but its temperature rise rate is very fast, easily cause starting temperature and final temperature higher, it is unfavorable for measuring of intermediate product.
Summary of the invention
In order to solve the problem, it is an object of the invention to provide a kind of method utilizing temperature programming flying time mass spectrum analysis coal tar pyrolysis low molecule product.
The present invention provides a kind of method utilizing temperature programming flying time mass spectrum analysis coal tar pyrolysis low molecule product, and the method concrete steps are as follows:
(1) sample obtains
Coal sample is pulverized, mixed even after cross 100 orders sieves, dry 12��24h at 70 DEG C, be placed in encloses container, dry vacuum distillation is warming up to 1000 DEG C, cold go after tar sample, be put in dry place stand-by;
(2) temperature programming flying time mass spectrum analysis
Getting 5��15mg tar sample is positioned in ion source, and with ramp to 700��800 DEG C of 5��10 DEG C/min, mass spectrum adds up frequency 10000Hz, every second record 1 spectrogram;
(3) data analysis
The mass spectrum obtained is utilized origin8.0 process.
The described method utilizing temperature programming flying time mass spectrum analysis coal tar pyrolysis low molecule product provided by the invention, the working conditions of described temperature programming flight time mass spectrum: vacuum tightness is 10-5Pa, ionization mode adopts PI source, and electron energy is 8��12eV.
The described method utilizing temperature programming flying time mass spectrum analysis coal tar pyrolysis low molecule product provided by the invention, sample hose is directly inlayed in an ion source, when tar is in sample hose during pyrolysis, pyrolysis product directly enters into the mass analyzer of temperature programming flight time mass spectrum.
The present invention can detect coal tar pyrolysis low molecule product fast.
Advantage of the present invention: by after tar sample preparation through temperature programming flying time mass spectrum analysis, intensification is controlled well, it is possible to the detection composition of tar main low molecule product in pyrolytic process and occuring regularity, and system is highly sensitive, good resolution; Utilize PI source can not produce fragment ion in ionization process as ionizer, and sample does not need to do any process.
Accompanying drawing explanation
Fig. 1 is temperature programming flight time mass spectrum; Wherein: 1 is ionization chamber; 2 is the ion source of integrated original position pyrolysis installation; 3 is time of flight mass analyzer; 4 is receptor; 5 is TDC acquisition module; 6 is ADC acquisition module; 7 is computer; 8 is vacuum system;
Fig. 2 is Firing Shenhua Coal tar PI source mass spectrum;
Embodiment
The present invention will be further described by the following examples, but not thereby limiting the invention.
One, sample obtains
Coal sample is pulverized, mixed even after cross 100 orders sieves, dry 12h at 70 DEG C, be placed in encloses container, dry vacuum distillation is warming up to 1000 DEG C, cold go after to be put in dry place stand-by.
Two, temperature programming flying time mass spectrum analysis
Temperature programming flight time mass spectrum working conditions: vacuum tightness is 10-5Pa, ionization mode adopts PI source, and electron energy is 10.6eV. Getting 10mg tar is positioned in in-situ heat solution ion source, and with the ramp to 800 DEG C of 5 DEG C/min, mass spectrum adds up frequency 10000Hz, every second record 1 spectrogram.
Three, data analysis
The mass spectrum obtained is utilized origin8.0 process.
Embodiment 1 Firing Shenhua Coal tar
Firing Shenhua Coal is pulverized, mixed even after cross 100 orders sieves, dry 12h at 70 DEG C, be placed in encloses container, dry vacuum distillation is warming up to 1000 DEG C, cold go after to be put in dry place stand-by.
Getting 10mg tar is positioned in temperature programming ion source, and with the ramp to 800 DEG C of 5 DEG C/min, mass spectrum adds up frequency 10000Hz, and every second record 1 spectrogram, flight time mass spectrum vacuum tightness is 10-5Pa��
Data are shown in Fig. 2 after origin8.0 processes.
This method utilizes temperature programming flight time mass spectrum, it is possible to for the real-time analysis of coal tar pyrolysis product, and system heats up and controls well, it is possible to the composition of detection tar main low molecule product in pyrolytic process and occuring regularity, highly sensitive, good resolution; Utilize PI source can not produce fragment ion in ionization process as ionizer, and sample does not need to do any process.
Claims (2)
1. analyze the method for coal tar pyrolysis low molecule product for one kind, it is characterised in that: the method concrete steps are as follows:
(1) sample obtains
Coal sample being pulverized, mix even rear 100 orders of crossing and sieve, dry 12��24h, be placed in encloses container at 70 DEG C, dry vacuum distillation is warming up to 1000 DEG C, obtains tar sample after cooling, is put in drying place stand-by;
(2) temperature programming flying time mass spectrum analysis
Getting 5��15mg tar sample is positioned in ion source, and with ramp to 700��800 DEG C of 5��10 DEG C/min, mass spectrum adds up frequency 10000Hz, every second record 1 spectrogram;
The working conditions of described temperature programming flight time mass spectrum: vacuum tightness is 10-5Pa, ionization mode adopts PI source, and electron energy is 8��12eV;
(3) data analysis
The mass spectrum obtained is utilized origin8.0 process.
2. according to the method analyzing coal tar pyrolysis low molecule product described in claim 1, it is characterized in that: sample hose is directly inlayed in an ion source, when tar is in sample hose during pyrolysis, pyrolysis product directly enters into the mass analyzer of temperature programming flight time mass spectrum.
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| CN105372360A (en) * | 2014-08-26 | 2016-03-02 | 中国科学院大连化学物理研究所 | Method for polymer pyrolysis gas-state volatile matter through in-situ pyrolysis flight time mass spectrometry |
| CN105372361A (en) * | 2014-08-26 | 2016-03-02 | 中国科学院大连化学物理研究所 | Method for polymer pyrolysis low-molecule product through in-situ pyrolysis flight time mass spectrometry |
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