CN104931573A - Analysis method of light tar in biomass gas - Google Patents
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- 238000003795 desorption Methods 0.000 claims abstract description 15
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 11
- 238000011084 recovery Methods 0.000 claims abstract description 7
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 5
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- 239000000567 combustion gas Substances 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000003463 adsorbent Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
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- 238000006073 displacement reaction Methods 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 239000012086 standard solution Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 238000001819 mass spectrum Methods 0.000 claims description 3
- 238000012113 quantitative test Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 19
- 238000005070 sampling Methods 0.000 abstract description 14
- 238000004445 quantitative analysis Methods 0.000 abstract description 4
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- 238000001514 detection method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
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- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 230000002265 prevention Effects 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 239000012855 volatile organic compound Substances 0.000 abstract 1
- 239000011269 tar Substances 0.000 description 47
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 14
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 12
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 12
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 10
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- 239000000243 solution Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 5
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
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- 239000012634 fragment Substances 0.000 description 3
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 239000011286 gas tar Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 125000003454 indenyl group Chemical class C1(C=CC2=CC=CC=C12)* 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
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- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthrene Natural products C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
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- 238000000769 gas chromatography-flame ionisation detection Methods 0.000 description 1
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- 229930195733 hydrocarbon Natural products 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
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- 239000003317 industrial substance Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 1
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- 239000005416 organic matter Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
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- 239000002910 solid waste Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention relates to a method for analyzing light tar in biomass gas, which comprises 5 steps of light tar collection, tar desorption, mass spectrometry, standard curve preparation and quantitative analysis; the method has simple and convenient sampling and high sampling efficiency; the desorption efficiency in the desorption process by means of sample solvent replacement auxiliary ultrasound and the like is high; the analysis process is simple, convenient and sensitive to operate and has good separation effect; the recovery rate of the light polycyclic aromatic hydrocarbon tar is high, the repeatability is good, the detection limit is low, and reliable data are provided for the tar separation process and the prevention and the treatment of environmental pollution; the method can be popularized and used for sampling and rapid qualitative and quantitative analysis of medium and light volatile organic compounds.
Description
Technical field
The present invention relates to the analytical approach of light tar in a kind of biological fuel gas, be specifically related to light tar sampling and GC-MS (gas chromatography-mass spectrum) analytical approach in a kind of biological fuel gas, belong to the interleaving techniques fields such as biomass thermal chemical conversion and chemical analysis.
Background technology
Biomass gasification process is association tar inevitably.Tar is in the follow-up use procedure of combustion gas, and the impurity such as Yi Yushui, dust and charcoal particle combine, blocking gas piping and valve, corroding metal; Be difficult to burn completely, produce the particles such as carbon black, combustion motor and gas-turbine wheel infringement are seriously; Its energy generally accounts for 5 ~ 15% of combustion gas gross energy, is difficult to utilization of burning together with combustion gas, reduces gasification efficiency.Therefore, the tar in combustion gas must carry out deep purifying.
Biomass gas tar oil may be defined as biomass thermal chemical conversion process and produces, the complex mixture be made up of fragrant hydrocarbons and their derivates.Namely the component that can detect reaches kind more than 100, wherein, massfraction be greater than 5% about have 7 kinds, be benzene,toluene,xylene, styrene, naphthalene, phenol and indenes respectively.Tar in gaseous state, is progressively condensed into liquid lower than 200 DEG C more than 300 DEG C.
Tar ingredients is complicated, to its carry out composition and structure resolve can be its be separated and comprehensive utilization basic data is provided, solve its environmental problem brought and problem of resource waste, the valuable industrial chemicals such as phenols can be extracted further or be processed into various fuel oil or solvent.Therefore, for the high value added utilization of tar, will directly affect the cost of combustion-gas jet test process.In order to utilize tar better, develop GC-MS and LC-MS (HPLC-MS) method of the full constituent analysis of tar.But these class methods are comparatively complicated, the semigel shape tar that normally condensation of sampling obtains, sample needs to carry out solvent extraction, soda acid is separated the measure such as phenol and chromatography segmentation, could go analysis again; Often also to assist infrared and ultimate analysis, just can carry out comparatively complete quantitative and qualitative analysis.
In order to ensure the safe handling of biological fuel gas, must carry out degree of depth decoking to it, except defocused, in combustion gas, tar content is generally lower than 200mg/Nm
3(about 200ppm).Now, in combustion gas, the number of components of tar significantly reduces, and mainly concentrates on the light multiring aromatic hydrocarbon tar being less than 4 phenyl ring.For the tar of trace in the combustion gas after purification, above-mentioned analytical approach seems too complicated, poor universality.Absorption-thermal desorption chromatography is the important method analyzed for this kind of micro-content organism.But these class methods, thermal desorption temperature is generally no more than 250 DEG C (tar of 3 or 4 phenyl ring is difficult to effective desorb), and desorption time is long, desorption efficiency is low, and the general recovery is lower than 90%.Japan Yoshikawa team (Son Y, Sato M, Namioka T, Yoshikawa K.A study onmeasurement of light tar content in the fuel gas produced in small-scale gasificationand power generation systems for solid wastes.J Environ Eng 2009,4:12-23.) establish the GC-FID (FID of gas tar oil absorption-thermal desorption, hydrogen flame) method, shortcoming is that thermal desorption efficiency is low, meanwhile, also there is limitation for the qualitative of tar ingredients in simple chromatogram.
Summary of the invention
The object of the invention is the analytical approach that light tar in a kind of biological fuel gas is provided to improve the deficiencies in the prior art.
Technical scheme of the present invention is: the analytical approach of light tar in a kind of biological fuel gas, and its concrete steps are as follows:
(1) tar collection: utilize adsorbent is housed stopple coupon at room temperature (general 0-25 DEG C) carry out tar sample collection, collect rearmounted refrigerator cold-storage and store;
(2) tar desorb: utilize organic solvent, carries out displacement desorption, centrifuging adsorbent dust after desorb under heating and ultrasonic measure;
(3) mass spectrometry: the tar that desorb obtains, utilizes mass spectrum to carry out qualitative analysis;
(4) typical curve prepares: utilize step (3) composition qualitatively, and the standard solution of configuration variable concentrations, carries out stratographic analysis, and drawing standard curve;
(5) quantitative test, the tar utilizing step (2) desorb to obtain carries out stratographic analysis, and compares with the typical curve that step (4) obtains, and calculates the content obtaining tar in combustion gas.
Gas recovery flow described in preferred steps (1) is 10 ~ 1000ml/min, and acquisition time is 1 ~ 10min.
Adsorbent described in preferred steps (1) is activated charcoal or commercial Tenax TA (the porous type polymkeric substance based on 2,6-diphenyl furans); Described adsorbent specific surface area is preferably greater than 800m
2/ g, micropore, mesoporous and macropore are crossed in pore size distribution.
Organic solvent described in preferred steps (2) is at least one in methyl alcohol, acetone or chloroform; Organic molten
Agent and adsorbent mass ratio are 10 ~ 30 ﹕ 1.
The ultrasonic frequency of preferred steps (2) is 30 ~ 100kHz, and ultrasonic time is 5 ~ 20min; Displacement desorption temperature is 30 ~ 50 DEG C; Described centrifuging condition is: centrifugal rotational speed is 3000 ~ 8000 turns/s, and centrifugation time is 3 ~ 5min.
Mass spectrometry condition described in preferred steps (3) is: ion source temperature 230 ~ 300 DEG C, and transmission line temperature is 250 ~ 300 DEG C; Scan pattern is electron scanning, electronics bombarding energy 60 ~ 80eV.
Chromatographic condition described in preferred steps (4) is: the capillary chromatographic column adopting nonpolar or medium note polarity; 35 ~ 50 DEG C of column temperatures keep 1min, 10 DEG C/min heating rate to rise to 150 DEG C, keep 1min, then rise to 250 ~ 320 DEG C with the heating rate of 20 DEG C/min, keep 2min; Injector temperature is 230 DEG C, and carrier gas is helium, and flow is 1ml/min, and pressure is 3kPa, and split ratio is 10 ﹕ 1; Sample size is 1 μ L.Capillary chromatographic column described in preferred steps (4) is DB-5, HP-5 or DB-17.
Beneficial effect:
(1) this method sampling is easy, and sampling efficiency is high;
(2) means desorption process desorption efficiency such as sample solvent displacement assisting ultrasonic etc. is high;
(3) analytic process sensitive, good separating effect easy and simple to handle;
(4) the light palycyclic aromatic tar recovery is high, reproducible, detection limit is low, for tar separation process and control environmental pollution provide reliable data;
(5) method of the present invention can be promoted for the sampling of middle lightweight volatile organic matter and fast qualitative and quantitative test.
Accompanying drawing explanation
Fig. 1 is the qualitative spectrogram of embodiment 1 sample chromatogram.
Embodiment
The present invention is effectively realized by the following example, but does not therefore limit the scope of application of the present invention.
Embodiment 1
Step (1), utilize the adsorption tube that 1g activated charcoal is housed to gather the tar in combustion gas, acquisition time 5min, gather flow 1000ml/min, collecting temperature is 35 DEG C; After collection completes, by sampling pipe two ends, it is characterized in that utilizing the stopple coupon that adsorbent is housed at room temperature to carry out tar sample collection, collect rearmounted refrigerator cold-storage and store 5 days.
Step (2), by sampling, the adsorption tube obtained blocks, and is transferred to by activated charcoal in centrifuge tube, adds acetone 20ml; By centrifuge tube at 35 DEG C, ultrasonic 10min under 40kHz condition; After ultrasonic, the tar transfer of charcoal absorption enters in acetone, but activated charcoal is also by partial crushing, and dust enters in acetone, therefore by centrifuge tube centrifugal 3min under 5000 turns/s condition, is separated by dust with solution.
Step (3), gets above-mentioned solution 1ml, and send into GC-MS and scan, mass spectrometry condition is: ion source temperature 250 DEG C, and transmission line temperature is 270 DEG C; Scan pattern is electron scanning, electronics bombarding energy 70eV.Full scan determination fragment ion scope, by qualitative for sample for benzene,toluene,xylene, styrene, phenol, pyridine, indenes, naphthalene, phenanthrene, anthracene and pyrene (qualitative results sees attached list 1), the above-mentioned tar molecules be within containing 4 Benzene Molecules.Carry out characteristic ion scanning again after qualitative, scanning result is shown in accompanying drawing 1, and each composition obtains and to be effectively separated and qualitative.
Step (4), utilizes step (3) composition qualitatively, and the standard solution of configuration variable concentrations, carry out stratographic analysis, and the chromatographic condition that above-mentioned mass spectrometry coordinates is: chromatographic column adopts DB-5 capillary chromatographic column; 50 DEG C of column temperatures keep 1min, 10 DEG C/min heating rate to rise to 150 DEG C, keep 1min, then rise to 280 DEG C with the heating rate of 20 DEG C/min, keep 2min; Injector temperature is 230 DEG C, and carrier gas is helium, and flow is 1ml/min, and pressure is 3kPa, and split ratio is 10 ﹕ 1; Sample size is 1 μ L.According to peak area or peak height, drawing standard curve, in Table 1-1.
Step (5), the tar sample that desorb obtains carries out stratographic analysis, and chromatographic condition is consistent with step (4), peak area per sample or peak height,
Compare with typical curve, calculate the content obtaining tar in combustion gas, content results is as shown in table 1-2.
Embodiment 2
Step (1), utilize the adsorption tube that 1.5g adsorbent Tenax TA is housed to gather the tar in combustion gas, acquisition time 10min, gather flow 10ml/min, collecting temperature is 35 DEG C; After collection completes, by sampling pipe two ends, it is characterized in that utilizing the stopple coupon that adsorbent is housed at room temperature to carry out tar sample collection, collect rearmounted refrigerator cold-storage and store 10 days.
Step (2), by sampling, the adsorption tube obtained blocks, and is transferred to by activated charcoal in centrifuge tube, adds methyl alcohol 10ml; By centrifuge tube at 30 DEG C, ultrasonic 18min under 30kHz condition; After ultrasonic, the tar transfer of Tenax absorption enters in methyl alcohol, but Tenax is also by partial crushing, and dust enters in methyl alcohol, therefore by centrifuge tube centrifugal 4min under 3000 turns/s condition, is separated by dust with solution.
Step (3), gets above-mentioned solution 1ml, and send into GC-MS and scan, mass spectrometry condition is: ion source temperature 230 DEG C, and transmission line temperature is 250 DEG C; Scan pattern is electron scanning, electronics bombarding energy 60eV.Full scan determination fragment ion scope, by qualitative for sample be benzene,toluene,xylene, styrene, phenol, pyridine, naphthalene and phenanthrene, the above-mentioned tar molecules be within containing 4 Benzene Molecules.Carry out characteristic ion scanning again after qualitative, each composition obtains and to be effectively separated and qualitative.
Step (4), utilizes step (3) composition qualitatively, and the standard solution of configuration variable concentrations, carry out stratographic analysis, and the chromatographic condition that above-mentioned mass spectrometry coordinates is: chromatographic column adopts HP-5 capillary chromatographic column; 40 DEG C of column temperatures keep 1min, 10 DEG C/min heating rate to rise to 150 DEG C, keep 1min, then rise to 250 DEG C with the heating rate of 20 DEG C/min, keep 2min; Injector temperature is 230 DEG C, and carrier gas is helium, and flow is 1ml/min, and pressure is 3kPa, and split ratio is 10 ﹕ 1; Sample size is 1 μ L.According to peak area or peak height, drawing standard curve, in Table 2-1.
Step (5), the tar sample that desorb obtains carries out stratographic analysis, and chromatographic condition is consistent with step (4), peak area per sample or peak height, compare with typical curve, calculate the content obtaining tar in combustion gas, content results is as shown in table 2-2.
Embodiment 3
Step (1), utilize the adsorption tube that 2g activated charcoal is housed to gather the tar in combustion gas, acquisition time 1min, gather flow 500ml/min, collecting temperature is 25 DEG C; After collection completes, by sampling pipe two ends, it is characterized in that utilizing the stopple coupon that adsorbent is housed at room temperature to carry out tar sample collection, after collection, directly carry out qualitative and quantitative analysis.
Step (2), by sampling, the adsorption tube obtained blocks, and is transferred to by activated charcoal in centrifuge tube, adds chloroform 30ml; By centrifuge tube at 48 DEG C, ultrasonic 4min under 95kHz condition; After ultrasonic, the tar transfer of charcoal absorption enters in chloroform, but activated charcoal is also by partial crushing, and dust enters in chloroform, therefore by centrifuge tube centrifugal 5min under 8000 turns/s condition, is separated by dust with solution.
Step (3), gets above-mentioned solution 1ml, and send into GC-MS and scan, mass spectrometry condition is: ion source temperature 290 DEG C, and transmission line temperature is 295 DEG C; Scan pattern is electron scanning, electronics bombarding energy 80eV.Full scan determination fragment ion scope, by qualitative for sample be benzene,toluene,xylene, styrene, phenol, pyridine and naphthalene, the above-mentioned tar molecules be within containing 4 Benzene Molecules.Carry out characteristic ion scanning again after qualitative, each composition obtains and to be effectively separated and qualitative.
Step (4), utilizes step (3) composition qualitatively, and the standard solution of configuration variable concentrations, carry out stratographic analysis, and the chromatographic condition that above-mentioned mass spectrometry coordinates is: chromatographic column adopts DB-17 capillary chromatographic column; 35 DEG C of column temperatures keep 1min, 10 DEG C/min heating rate to rise to 150 DEG C, keep 1min, then rise to 320 DEG C with the heating rate of 20 DEG C/min, keep 2min; Injector temperature is 230 DEG C, and carrier gas is helium, and flow is 1ml/min, and pressure is 3kPa, and split ratio is 10 ﹕ 1; Sample size is 1 μ L.According to peak area or peak height, drawing standard curve, in Table 3-1.
Step (5), the tar sample that desorb obtains carries out stratographic analysis, and chromatographic condition is consistent with step (4), peak area per sample or peak height, compare with typical curve, calculate the content obtaining tar in combustion gas, content results is as shown in table 3-2.
Table 1-1 sample standard curve
Table 1-2 sample amounts table
Table 2-1 sample standard curve
Table 2-2 sample amounts table
| Title | Characteristic ion | Content, mg/Nm 3 | Recovery of standard addition, % |
| Benzene | 78,77,51 | 12.26 | 92.43 |
| Pyridine | 79,52,39 | 9.21 | 94.49 |
| Toluene | 91,92,65,51 | 7.17 | 98.66 |
| Dimethylbenzene | 91,106,77,51 | 6.40 | 91.20 |
| Styrene | 104,103,78,51 | 12.05 | 100.66 |
| Phenol | 94,66,39,55 | 14.88 | 100.11 |
| Naphthalene | 128,102,64,51 | 1.67 | 97.02 |
| Luxuriant and rich with fragrance | 178,152,76,89 | 9.64 | 90.56 |
Table 3-1 sample standard curve
Table 3-2 sample amounts table
| Title | Characteristic ion | Content, mg/Nm 3 | Recovery of standard addition, % |
| Benzene | 78,77,51 | 0.76 | 95.90 |
| Pyridine | 79,52,39 | 2.37 | 92.02 |
| Toluene | 91,92,65,51 | 4.71 | 90.11 |
| Dimethylbenzene | 91,106,77,51 | 0.95 | 101.96 |
| Styrene | 104,103,78,51 | 2.16 | 91.70 |
| Phenol | 94,66,39,55 | 3.93 | 90.73 |
| Naphthalene | 128,102,64,51 | 4.77 | 101.92 |
Claims (8)
1. the analytical approach of light tar in biological fuel gas, its concrete steps are as follows:
(1) tar collection: utilize the stopple coupon that adsorbent is housed at room temperature to carry out tar sample collection, collects rearmounted refrigerator cold-storage and stores;
(2) tar desorb: utilize organic solvent, carries out displacement desorption, centrifuging adsorbent dust after desorb under heating and ultrasonic measure;
(3) mass spectrometry: the tar that desorb obtains, utilizes mass spectrum to carry out qualitative analysis;
(4) typical curve prepares: utilize step (3) composition qualitatively, and the standard solution of configuration variable concentrations, carries out stratographic analysis, and drawing standard curve;
(5) quantitative test, the tar utilizing step (2) desorb to obtain carries out stratographic analysis, and compares with the typical curve that step (4) obtains, and calculates the content obtaining tar in combustion gas.
2. analytical approach according to claim 1, it is characterized in that the gas recovery flow described in step (1) is 10 ~ 1000ml/min, acquisition time is 1 ~ 10min.
3. analytical approach according to claim 1, is characterized in that the adsorbent described in step (1) is activated charcoal or commercial Tenax TA.
4. analytical approach according to claim 1, the organic solvent that it is characterized in that described in step (2) is at least one in methyl alcohol, acetone or chloroform; Organic solvent and adsorbent mass ratio are 10 ~ 30 ﹕ 1.
5. analytical approach according to claim 1, it is characterized in that the ultrasonic frequency of step (2) is 30 ~ 100kHz, ultrasonic time is 5 ~ 20min; Displacement desorption temperature is 30 ~ 50 DEG C; Described centrifuging condition is: centrifugal rotational speed is 3000 ~ 8000 turns/s, and centrifugation time is 3 ~ 5min.
6. analytical approach according to claim 1, it is characterized in that the mass spectrometry condition described in step (3) is: ion source temperature 230 ~ 300 DEG C, transmission line temperature is 250 ~ 300 DEG C; Scan pattern is electron scanning, electronics bombarding energy 60 ~ 80eV.
7. analytical approach according to claim 1, is characterized in that the chromatographic condition described in step (4) is: the capillary chromatographic column adopting nonpolar or medium note polarity; 35 ~ 50 DEG C of column temperatures keep 1min, 10 DEG C/min heating rate to rise to 150 DEG C, keep 1min, then rise to 250 ~ 320 DEG C with the heating rate of 20 DEG C/min, keep 2min; Injector temperature is 230 DEG C, and carrier gas is helium, and flow is 1ml/min, and pressure is 3kPa, and split ratio is 10 ﹕ 1; Sample size is 1 μ L.
8. analytical approach according to claim 7, is characterized in that the capillary chromatographic column described in step (4) is DB-5, HP-5 or DB-17.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110658265A (en) * | 2018-06-29 | 2020-01-07 | 宝武炭材料科技有限公司 | Method for simultaneously measuring contents of benzene, toluene, xylene and naphthalene in coal gas |
| CN111892937A (en) * | 2020-06-16 | 2020-11-06 | 浙江大学 | Characterization method for distribution of all components of aromatic compounds in light components of coal tar |
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