CN104931301B - A kind of detection method of stacte smoke gathering device and stacte flue gas volatile ingredient - Google Patents
A kind of detection method of stacte smoke gathering device and stacte flue gas volatile ingredient Download PDFInfo
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Abstract
The invention discloses the detection method of a kind of stacte smoke gathering device and stacte flue gas volatile ingredient, the device includes gas gathering mask, cigarette smoke collector, the bottle,suction and vacuum pump for filling lyosoption being sequentially communicated with suction filtering tube, and the vacuum pump is used to the gas that trap is collected being extracted into the lyosoption of bottle,suction.Apparatus structure is simple, and raw material are easy to get, and builds of low cost, and applicability is wide, can not only trap gas phase and granule phase substance, but can independent trapped whole smoke, it is flexible and convenient to use.This method can analyze the volatile materials produced after stacte burning comprehensively, or the volatile ingredient in independent analysis gas phase and granule phase substance, it is easy to operate, high sensitivity, it is applicable not only to the volatile ingredient measure of combustion product gases in stacte industry, the fingerprint map analyzing of stacte can be also carried out, solid foundation is established for stacte quality control.
Description
Technical field
The invention belongs to stacte detection technique field, and in particular to a kind of stacte smoke gathering device and measure stacte cigarette
The method of volatile ingredient in gas.
Background technology
, that is, there is the applicating history of natural perfume material in day since human civilization, and even to this day, natural perfume material is being eaten
The fields such as product, beverage, medicine, cigarette, daily chemicals are more and more widely used.The use of natural perfume material is more with straight
Connect addition or extract essential oil addition mode apply based on, this two kinds of application forms, educational circles is to spices volatile component and essential oil
Into being allocated as a large amount of further investigations, but should in traditional industries --- the fragrant road that another natural perfume material is widely applied, natural perfume material
It is less with data accumulation.
Stacte raw material sources are extensive used by fragrant road, more using the fragrant medium-height grass such as santal, agalloch eaglewood, wrinkled giant hyssop, cloves, root of Dahurain angelica
The single formula of the crops such as medicine and fish-skin point, folium artemisiae argyi, stalk follows the compound spices that drug matching principle carries out compatibility.It is above-mentioned
Natural perfume material discharges a large amount of fragrance matters after burning, reaches purification air and beneficial to physically and mentally healthy effect, but due to basis
Data deficiency, the compatibility formulating options tradition of spices, more rule of thumb, therefore a kind of science, efficient and comprehensive detect are smoked
Development of the method for fragrant combustible substance for the sector, which has, greatly facilitates effect.
At present, the domestic detection report for stacte combustible substance is less, especially in combustible substance capturing device and method
Aspect is particularly short of.
The content of the invention
The present invention is in view of the shortcomings of the prior art, provide a kind of simple in structure, common stacte smoke gathering device of raw material
And the volatile ingredient in stacte flue gas is measured comprehensively.
In order to realize foregoing invention purpose, the present invention adopts the following technical scheme that：
A kind of stacte smoke gathering device, including be sequentially communicated with suction filtering tube gas gathering mask, cigarette smoke collector, be used for
The bottle,suction and vacuum pump of lyosoption are filled, the absorption that the vacuum pump is used to the gas that trap is collected being extracted into bottle,suction is molten
In agent.
The bottleneck of the bottle,suction is sealed with being inserted into the rubber stopper of long glass tube；The long glass tube for filtering bottleneck passes through
Suction filtering tube is connected with trap.
The bottle,suction is externally provided with low-temperature control device, i.e., controls low temperature outside bottle,suction with dry ice.
The lyosoption is mixing more than one or both of dichloromethane, n-hexane, methanol, ethanol and acetone
Thing.
The gas gathering mask is funnel.
A kind of detection method of stacte flue gas volatile ingredient, comprises the following steps：
Step 1：With cambridge filter trap granule phase substance, with equipped with lyosoption bottle,suction trap gas gas-phase objects, or directly with
Bottle,suction trapped whole smoke equipped with lyosoption；
Step 2：The granule phase substance trapped is put into concussion or ultrasonic extraction 20-60min in lyosoption；
Step 3：Progress low temperature is low after adding internal standard in lyosoption in step 2 resulting solution or step (1) bottle,suction
Press rotary evaporation；
Step 4：Solution after revolving described in step 3 is detected into GC-MS instruments, testing conditions are as follows：Chromatographic column is
DB-5MS, specification are：60m×0.25mm i.d×0.25μm；Carrier gas is He, flow 1.0mL/min；Split ratio is 30:1；Into
Sample amount is 1 μ L；Injector temperature is 280 DEG C；Heating schedule is 40 DEG C of initial temperature, and 280 DEG C of holdings are risen to 1.5 DEG C/min
20min；Transmission line temperature is 280 DEG C；Ion source temperature is 230 DEG C；Level Four bar temperature is 150 DEG C；Electron impact ionization voltage
For 70eV；Mass number scope is 50~550amu.
The lyosoption is mixing more than one or both of dichloromethane, n-hexane, methanol, ethanol and acetone
Thing.
The low-temp low-pressure is 30~50 DEG C, 500~700mbar.
The low-temp low-pressure is 40 DEG C, 600mbar.
Relatively existing technology, the present invention have the following advantages：
1. stacte smoke gathering device is simple in structure, raw material are easy to get, and build of low cost, and applicability is wide, can both trap
Gas phase and granule phase substance, but can independent trapped whole smoke, it is flexible and convenient to use.
2. the present invention can be detected efficiently and comprehensively using the volatile ingredient of GC-MS analysis stacte flue gases, this method
The volatile materials produced after stacte burning, or the volatile ingredient in independent analysis gas phase and granule phase substance.Pre-treatment is simple, peak
Separating degree is high, and finger-print contains much information, and reproducible, high sensitivity, and the amount of substance identified in this approach is enriched, and is smoked
Solid foundation is established in fragrant quality control.
Brief description of the drawings
Fig. 1 is the structure diagram of stacte smoke gathering device of the present invention；1 is funnel；2 be cigarette smoke collector；3 are
Bottle,suction；4 be vacuum pump.
Fig. 2 sinks sample chromatogram figure for star continent water.
Fig. 3 is agalloch eaglewood sample chromatogram figure.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and embodiments.It is it should be appreciated that described herein
Specific embodiment only to explain analysis condition technical essential of the present invention, is not intended to limit the present invention.
Embodiment 1
Used main agents and instrument：
Agalloch eaglewood (Guangdong Zhuhai Yu Feng agalloch eaglewood Industries, Ltd)；Star continent water sinks (commercially available)；44mm cambridge filters (Britain
Whatman companies)；Dichloromethane (AR, Aladdin)；Internal standard phenylethyl propionate (SP, Sigma-Aldrich)
7890 gas chromatographs and 5975C mass spectrographs (Agilent companies of the U.S.)；CP2245 electronic balance (sensibility reciprocals
0.0001g, German Sartorius companies)；One channel smoke sucking machine (rich watt Kai Xi companies of LM1 Germany)；Rotary Evaporators (R-
210 Bu Qi Co., Ltds of Switzerland)；Stacte smoke gas collecting apparatus is shown in Fig. 1.
The side of volatile ingredient in the granule phase substance trapped by above-mentioned stacte smoke gathering device is measured in the present embodiment
Method, comprises the following steps：
Step 1：Vacuum pump is opened, agalloch eaglewood is lighted under funnel, fires to a period of time, takes trap to weigh and calculates grain
Phase thing weight；
Step 2：Cambridge filter is moved into 50mL conical flasks, adds 30mL dichloromethane, and it is interior to add phenethyl acetate
Mark, shakes 30min with the speed of 180r/min, rear to move into revolving bottle；
Step 3：Revolving bottle is connected to rotary evaporator, 40 DEG C, rotary evaporation solution is left to 1mL under the conditions of 600mbar
The right side, moves into sample injection bottle, and machine is analyzed in wait, and each sample is parallel to be repeated 3 times；
GC conditions are as follows：Chromatographic column：DB-5MS(60m×0.25mm i.d×0.25μm)；Carrier gas：He, flow 1.0mL/
min；Split ratio：30:1；Sample size：1μL；Injector temperature：280℃；Temperature programming：40℃→1.5℃/min→280℃
(20min).MS conditions are as follows：Transmission line temperature：280℃；Ion source temperature：230℃；Level Four bar temperature：150℃；Electronics bangs
Hit (EI) ionization voltage：70eV；Mass number scope：50~550amu.
Step 4：Wiley05+Nist08 connects retrieval analysis spectrogram, and scalar slightly quantifies each target peak, meter in contrast
Calculate the amount of every kind of volatile matter in Unit Weight granule phase substance.
Volatile ingredient is qualitative in two kinds of agalloch eaglewood sample combustion granule phase substances in the present embodiment and quantitative result is shown in Table 1.
Volatile ingredient in 1 two kinds of agalloch eaglewood sample combustion granule phase substances of table
Note：N.D. it is not detect
In the present embodiment, isolate and identify 123 kinds of materials, content is more for 4 sugared catabolites, 9 monoterpenes
Compound, 8 contain methoxy compound, and monoterpenes compound is primarily present in the secretory tissue of higher plant, methoxylation
Produced by compound is mainly lignin degradation.It is mainly that sesquiterpenoids is different from the agilawood essential oil component of document report,
In volatile ingredient in agalloch eaglewood burning smoke granule phase substance, sesquiterpenoids seldom detects.
Embodiment 2
Implementation column 1 is repeated, there is following difference：Load 30mL dichloromethane in bottle,suction and collect agalloch eaglewood sample combustion
Gas gas-phase objects, add upper machine analysis after internal standard rotary evaporation.
The result shows that：Volatile content in agalloch eaglewood gas gas-phase objects is far below granule phase substance.
Embodiment 3
Embodiment 1 is repeated, there is following difference：Remove the cigarette trap in collection device, load in bottle,suction
30mL dichloromethane collects the volatile ingredient in the full flue gas of agalloch eaglewood sample combustion, adds upper machine point after internal standard rotary evaporation
Analysis.
The result shows that：Volatile ingredient quantity in full flue gas is roughly the same with granule phase substance, but fractions content is bright
It is aobvious higher.
Claims (3)
1. a kind of detection method of stacte flue gas volatile ingredient, it is characterised in that comprise the following steps：
Step 1：With cambridge filter trap granule phase substance, with equipped with lyosoption bottle,suction trap gas gas-phase objects, or directly with equipped with
The bottle,suction trapped whole smoke of lyosoption；
Step 2：The granule phase substance trapped is put into concussion or ultrasonic extraction 20-60min in lyosoption；
Step 3：Low-temp low-pressure rotation is carried out after internal standard is added in lyosoption in step 2 resulting solution or step 1 bottle,suction
Evaporation, the low-temp low-pressure are 30~50 DEG C, 500~700mbar；
Step 4：Solution after step 3 rotary evaporation is detected into GC-MS instruments, testing conditions are as follows：Chromatographic column is DB-
5MS, specification are：60m×0.25mm i.d×0.25μm；Carrier gas is He, flow 1.0mL/min；Split ratio is 30:1；Sample size
For 1 μ L；Injector temperature is 280 DEG C；Heating schedule is 40 DEG C of initial temperature, and 280 DEG C of holding 20min are risen to 1.5 DEG C/min；
Transmission line temperature is 280 DEG C；Ion source temperature is 230 DEG C；Level Four bar temperature is 150 DEG C；Electron impact ionization voltage is 70eV；
Mass number scope is 50~550amu.
2. detection method according to claim 1, it is characterised in that the lyosoption is dichloromethane, n-hexane, first
Mixture more than one or both of alcohol, ethanol and acetone.
3. detection method according to claim 1 or 2, it is characterised in that the low-temp low-pressure is 40 DEG C, 600mbar.
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| CN106501418A (en) * | 2016-12-30 | 2017-03-15 | 中国烟草总公司广东省公司 | A kind of flue gas causes perfumery to build method and the application of Nicotiana tabacum L. finger printing |
| CN106645537B (en) * | 2017-01-23 | 2018-06-15 | 中国烟草总公司郑州烟草研究院 | The method for measuring 19 kinds of sootiness perfume (or spice) ingredients in cigarette mainstream flue gas simultaneously |
| CN106932238A (en) * | 2017-04-24 | 2017-07-07 | 云南中烟工业有限责任公司 | A kind of olfactory substance capturing device and application |
| CN107156897B (en) * | 2017-07-07 | 2019-03-19 | 重庆中烟工业有限责任公司 | A kind of device and method preparing tobacco tar |
| CN108037236B (en) * | 2017-11-21 | 2023-03-03 | 中国科学院西北生态环境资源研究院 | Experimental device for collecting quantitative analysis gas of methane conversion rate in torch discharge |
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| CN102645496A (en) * | 2012-05-11 | 2012-08-22 | 广东中烟工业有限责任公司 | Discriminant analysis method for distribution ratio of volatile and semi-volatile component in gas phase and particle phase in cigarette mainstream smoke |
| CN104458331A (en) * | 2014-12-23 | 2015-03-25 | 浙江诺睿特生物科技有限公司 | Sampling device for spice distillation |
| CN104569197B (en) * | 2014-12-30 | 2016-10-26 | 广东中烟工业有限责任公司 | The silanization GC/MS detection method of sugar, 1,2-propylene glycol and the glycerol in mensuration Nicotiana tabacum L. simultaneously |
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