CN104713903B - A kind of method of aroma component residual quantity in detection cigarette filter tip - Google Patents
A kind of method of aroma component residual quantity in detection cigarette filter tip Download PDFInfo
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- CN104713903B CN104713903B CN201510143543.3A CN201510143543A CN104713903B CN 104713903 B CN104713903 B CN 104713903B CN 201510143543 A CN201510143543 A CN 201510143543A CN 104713903 B CN104713903 B CN 104713903B
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- mouth rod
- fragrant mouth
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- fragrant
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Abstract
A kind of method of aroma component residual quantity in detection cigarette filter tip, including：Step one, sample cell are put into the fragrant mouth rod of cause, are put into the grade metering jet rod for not adding volatile spice in reference cell；Step 2, under the storage temperature for causing fragrant mouth rod, measure the Endothermic power P versus time curves in the spices volatilization process for causing fragrant mouth rod；Step 3, Endothermic power versus time curve is integrated obtain recept the caloric Qt, the spices rate of volatilization dc/dt for causing fragrant mouth rod is integrated the concentration c for obtaining causing fragrant mouth rod to be volatilized within a certain period of time to the timet；Step 4, fragrant caloric receptivity Q of the mouth rod in certain time period of causetWith total caloric receptivity QAlwaysRatio be equal to the concentration c for causing the spices volatilization in the certain time period of fragrant mouth rodtWith total concentration c0Ratio, obtain residual quantity c for causing spices in fragrant mouth rodSurplus=c0‑(Qt/QAlways)c0.The present invention can achieve the evaporation rate and residual concentration that continuous dynamic detection causes fragrant mouth rod essence and flavoring agent during storage, and easy to operate, testing result is accurately and reliably.
Description
Technical field
The present invention relates to a kind of method for detecting aroma component residual quantity in cigarette filter tip.
Background technology
Cigarette is a kind of by sucking the Special food for obtaining physiology and psychic gratification, and the fragrance of cigarette is to affect cigarette to inhale
Food matter and flavour characteristic key factor.
Fragrance is sucked for obtaining with necessarily flavour characteristic, generally accurately will add essence and flavoring agent in cigarette.To volume
The approach for adding essence and flavoring agent in cigarette is divided into two kinds, and the first approach is added to pipe tobacco, in aspiration procedure, the essence of interpolation
Burning of the spices by cigarette, with oral cavity and nasal cavity that flue gas reaches smoker.Thus the essence and flavoring agent one added in pipe tobacco
As be high boiling aroma component, or by burning, there is chemical reaction, produce aroma component.Second approach be by
Essence and flavoring agent is added in the mouth rod of cigarette, first prepares and causes fragrant mouth stick, then will cause fragrant mouth rod and pipe tobacco and other
Auxiliary material obtains final finished cigarettes by rolling up bag.In aspiration procedure, essence and flavoring agent is reached with flue gas and is taken out by directly volatilizing
The oral cavity of suction person and nasal cavity.As mouth rod does not burn, thus, it is low that the essence and flavoring agent composition being added in cigarette filter tip is required
The volatile composition of boiling point.The volatile essence and flavoring agent composition of these low boilings undoubtedly can bring not true to the quality control of product
Fixed factor, is to obtain stable product quality, and the production technology for cigarette provides accurate parameter, it is necessary to causing fragrant mouth rod
The change of essence and flavoring agent concentration during storage, is detected and is monitored.
The change of fragrant essence and flavoring agent concentration of the mouth rod during storage of cause is detected in prior art and monitored
One of method is sensory evaluating smoking's method, and the method is to allow the person of smokeing panel test, by sucking after sensory experience, judge to cause fragrant mouth rod in warp
Cross the concentration of remaining essence and flavoring agent after storing.It will be apparent that the method will put into larger manpower, need input a large amount of through tight
Teacher of the smokeing panel test of sensory evaluating smoking's training of lattice, and the physiological status of the person of smokeing panel test and disturbing for psychological condition is subject to easily, so as to bring
Larger error, and the method is difficult to 24 hours continuously smoke panel test and monitor, thus be difficult to obtain and cause the fragrant mouth rod to store
The complete information of essence and flavoring agent change in concentration in journey.
The opposing party change for causing fragrant essence and flavoring agent concentration of the mouth rod during storage detected in prior art
Method is chromatography, i.e., first to causing fragrant mouth rod to carry out pre-treatment, the essence and flavoring agent in fragrant mouth rod will be caused to be extracted with solvent, then
With chromatograph to extract in aroma component carry out quantitative analysis detection.Although the method sensitivity is high, pre-treatment is walked
Suddenly need to be accomplished manually, and time-consuming, thus larger human cost will be put into.Additionally, chromatography cannot also realize 24 hours continuously
Sampling, thus be difficult to obtain the complete information for causing fragrant mouth rod essence and flavoring agent change in concentration during storage.
Content of the invention
The method that the present invention provides aroma component residual quantity in a kind of detection cigarette filter tip, can achieve continuously dynamic detection
The evaporation rate and residual concentration of fragrant mouth rod essence and flavoring agent during storage is caused, easy to operate, it is not necessary to add any other
Reagent and medicine, saved the consumption of reagent cost, it is to avoid because of the environmental pollution that the consumption of reagent causes, and testing result
Accurately and reliably.
A kind of method of aroma component residual quantity in detection cigarette filter tip, is detected using the hot instrument of thermal conductivity type micro,
The hot instrument of the thermal conductivity type micro includes the measuring cell being made up of sample cell and reference cell, the thermoelectricity being distributed in around measuring cell unit
The number of part, the heat abstractor being arranged on around measuring cell, the thermostat being arranged on around heat abstractor and thermoelectric element connection
According to analyzer, on sample cell and reference cell, be arranged with sleeve pipe, the one side of thermoelectric element is brought into close contact with sleeve pipe, thermoelectric element another
Simultaneously it is brought into close contact with heat abstractor, methods described comprises the steps：
The fragrant mouth rod of cause is put in step one, sample cell, is put into the grade metering jet rod for not adding volatile spice in reference cell；
Step 2, under the storage temperature for causing fragrant mouth rod, the spices of the fragrant mouth rod of the cause that measured with the hot instrument of thermal conductivity type micro is waved
Endothermic power P versus time curves during sending out, Endothermic power P versus time curves reflect the fragrant mouth rod of cause
Spices rate of volatilization dc/dt is over time；
Step 3, by step 2 obtain Endothermic power P versus time curves be integrated, that is, recepted the caloric
Qt, the spices rate of volatilization dc/dt for causing fragrant mouth rod was integrated to the time and obtains causing fragrant mouth rod to be volatilized within a certain period of time
Concentration ct；
Step 4, the speed for causing fragrant mouth bar spices material volatilization due to causing the Endothermic power P of the spices volatilization of fragrant mouth rod to be proportional to
Rate dc/dt, therefore causes fragrant caloric receptivity Q of the mouth rod in certain time periodtWith total caloric receptivity QAlwaysRatio be equal to and cause fragrant mouth rod to exist
The concentration c of spices volatilization in certain time periodtWith the ratio of total concentration, wherein c0For the initial concentration of spices, i.e. Qt/QAlways=ct/
c0, and then residual quantity c for obtaining causing spices in fragrant mouth rodSurplus=c0-(Qt/QAlways)c0.
The method of aroma component residual quantity in detection cigarette filter tip as above, the step 2 are specially：In test
During, cause fragrant mouth rod that heat absorption occurs in sample cell and cause the temperature of sample cell to reduce, so as to sample cell and heat abstractor it
Between form temperature difference Δ T, temperature difference Δ T is converted into voltage signal U by thermoelectric element by Seebeck effect and exports to data point
Analyzer, data analyzer are caused accordingly according to the data for testing collected voltage signal U and corresponding time t
Endothermic power P versus time curves in the spices volatilization process of fragrant mouth rod.
The method of aroma component residual quantity, the temperature of thermostat in thermostat in detection cigarette filter tip as above
The electric potential signal that fluctuation is produced produces identical interference signal between the two in sample cell and reference cell, in step 2, by two
Both are offset by carrying out subtractive on circuit by individual interference signal, to eliminate the shadow of the fluctuation to measurement result of ambient temperature
Ring.
The invention has the advantages that：
1. the physical holding of the stock process for causing fragrant mouth rod can be simulated, it is not necessary to add any other reagent, will not introduce interference because
Element, so that realize that continuous dynamic detection causes the evaporation rate and residual concentration of fragrant mouth rod essence and flavoring agent during storage.
2. easy to operate, it is not necessary in specific time point sampling and analysis, save artificial running cost.
3. any other reagent and medicine need not be added, the consumption of reagent cost has been saved, it is to avoid disappearing because of reagent
The environmental pollution that consumption causes.
4. detecting system adopts the presence of twin docking, reference to reduce ambient temperature influence of fluctuations, and sensitivity is high, reappears
Property is good, can detect microwatt and even lower thermal signal, and minimum temperature difference is 10-7DEG C, testing result is accurately and reliably.
5. can realize 24 hours continuous dynamic detect, cause fragrant mouth rod essence and flavoring agent during storage to wave so as to obtain
The complete information of speed and residual concentration is sent out, is the quality control and the determination of technological parameter of cigarette product, there is provided accurately comprehensively
Information and guidance.
The present invention obtains electric signal over time by microcalorimeter measurement, intuitively can reflect fragrant in the fragrant mouth rod of cause
The change of the rate of volatilization of smart fragrance component, discloses fragrant dynamic information of the mouth rod during storage of cause, is to cause fragrant mouth rod
Condition of storage provide reference, be that the quality control of cigarette product and the selection of cigarette producing process lay the foundation.
Description of the drawings
Fig. 1 is the structural representation of the device of aroma component residual quantity in present invention detection cigarette filter tip；
Fig. 2 is that the present invention causes the Endothermic power versus time curve figure in the spices volatilization process of fragrant mouth rod；
Fig. 3 is that the present invention causes the total caloric receptivity Q in the spices volatilization process of fragrant mouth rodAlwaysIntegration schematic diagram；
Fig. 4 is the caloric receptivity Q of the spices volatilization for causing fragrant mouth rod in the t times of the present inventiontIntegration schematic diagram.
In figure：1 thermostat, 2 heat abstractors, 3 sample cells, 4 reference cells, 5 thermoelectric elements, 6 sleeve pipes,
7 data analyzers.
Specific embodiment
Accompanying drawing in below in conjunction with the present invention, to the present invention in technical scheme be clearly and completely described.
The present invention provide a kind of detection cigarette filter tip in aroma component residual quantity method, its adopt Fig. 1 shown devices come
Detected, described device be the hot instrument of thermal conductivity type micro, including be made up of sample cell 3 and reference cell 4 measuring cell, be distributed in survey
Thermoelectric element 5, the heat abstractor 2 being arranged on around measuring cell around amount pond, the thermostat being arranged on around heat abstractor 2
1 and thermoelectric element 5 connection data analyzer 7, be arranged with sleeve pipe 6 on sample cell 3 and reference cell 4.
The metal derby that heat abstractor 2 can adopt one piece of quality very big, because quality is big, thermal capacitance is big, absorbs or releases
Some heats are put, its temperature changes very little, therefore its temperature change is fluctuated by ambient temperature and affected less, and heat abstractor 2 is put
In the thermostat of thermostat 1, the temperature fluctuation of heat abstractor 2 is less than the temperature fluctuation of thermostat, and temperature persistance is more preferable.
Thermoelectric element 5 is the temperature sensor being together in series by some thermocouples, the one side of thermoelectric element 5 and sample cell 2
Or the sleeve pipe 6 of reference cell 4 is brought into close contact, the another side of thermoelectric element 5 is brought into close contact with heat abstractor 2.The effect of sleeve pipe 6 is
Thermoelectric element 5 is fixed, and good contact is formed between sample cell 2.Because sample cell 2 must fill sample after taking out, it is not
May maintain static, so it directly can not possibly form and closely fit with thermoelectric element 5.Covered with one outside sample cell 2
Pipe 6, makes the outer wall of sleeve pipe 6 post and fix with the one side of thermoelectric element 5, it is ensured that good heat conductivility.Reference cell 4 and sample
The structure in product pond 3 is just the same, during measurement, is put into the material of thermal inertia corresponding with measurement sample (such as embodiment in reference cell 4
In, sample cell 3 be put into for causing fragrant mouth rod, be then put in reference cell 4 do not add volatile spice wait metering jet rod), surveying
There is no neither endothermic nor exothermic in reference cell 4 in examination temperature range.In test process, the temperature of thermostat is not definitely to fix not
Become, have a small temperature fluctuation, cause the temperature of heat abstractor 2 also and then to fluctuate together, this temperature fluctuation
Electric potential signal can be produced, and this electric potential signal is unrelated with the suction/heat release of sample, be the undesirable interference signal for obtaining.
As sample cell 3 and reference cell 4 are connected by thermoelectric element 5 with same heat abstractor 2, so, will be in sample cell 3
Identical interference signal is produced between the two with reference cell 4, two interference signals are carried out subtractive on circuit, can be by both
Offset, interference is minimized, so as to eliminate the impact of the fluctuation to measurement result of ambient temperature, the measurement of instrument is improve
Precision.
In test process, sample it may happen that neither endothermic nor exothermic reaction, causes sample cell in sample cell 3
3 temperature reduces or raises.So as to form the temperature difference Δ T of a very little between sample cell 3 and heat abstractor 1.This
Temperature difference is converted into voltage signal U by thermoelectric element 5 by Seebeck (Seebeck) effect and exports to data analyzer 7.U and
Relation between Δ T can be formulated：U=S Δ T
S is the Seebeck coefficients of sensor (i.e. thermoelectric element 5), unit：V/K, to a sensor, in uniform temperature
It is constant down, because test is carried out under constant temperature, S is constant, then be linear relationship between U and Δ T.
Temperature difference between sample cell 3 and heat abstractor 5 can cause heat transfer, when heat transfer reaches stable state, this heat transfer
Power and sample neither endothermic nor exothermic power equal.According to Newton's law of cooling (Newton's Law of Cooling), pass
Relation between thermal power P and temperature difference T can be formulated：P=λ Δ TA/ Δ x
In formula, λ is thermal conductivity, is constant；Δ x is the distance of heat transfer；A is heat transfer area；Because calorimeter
Structure and material is all fixed, so λ, A and Δ x are constants, then P=k Δs T, i.e. P are also linear with Δ T.
Therefore the voltage signal of sensor is also linear, i.e. P ∝ U with the neither endothermic nor exothermic power of sample in sample cell 3.Institute
With by the data for testing collected U (voltage signal) and corresponding t (time), so that it may obtain corresponding P (thermal power)
With the data of t (time), can be drawn by software and obtain corresponding figure, i.e. P-t curves, as shown in Figure 2.
Fig. 2 is the spices volatilization of the cause perfume mouth rod under the storage temperature for causing fragrant mouth rod, being measured with the hot instrument of thermal conductivity type micro
During Endothermic power versus time curve.The curve has intuitively reacted the fragrant mouth rod spices during storage of cause and has waved
The Endothermic power that sends out changes over complete information.And the Endothermic power of spices volatilization is proportional to the speed of spices volatilization, because
This Fig. 2 completely can intuitively reflect the spices rate of volatilization of the fragrant mouth rod of cause over time.As seen from Figure 2, cause
The rate of volatilization of the spices of fragrant mouth rod is larger in first 24 hours, maximum occurs at 5 hours.After 24 hours, fragrant mouth is caused
The spices rate of volatilization of rod is gradually reduced.
And cause the P (thermal power) of fragrant mouth bar spices material volatilization and the linear phase that causes spices volatilizees in fragrant mouth rod speed dc/dt
Close, i.e.,P-t curves in Fig. 2 are integrated, that is, obtain quantity of heat production, as shown shaded in figure 3.
The spices rate of volatilization (dc/dt) for causing fragrant mouth rod was integrated to the time and just obtains causing fragrant mouth rod in certain time
Interior volatilized concentration ct.
Cause the speed of fragrant mouth bar spices material volatilization due to causing the Endothermic power of the spices volatilization of fragrant mouth rod to be proportional to, institute so that
Caloric receptivity Q of the fragrant mouth rod in certain time periodtWith total caloric receptivity QAlwaysRatio be equal to and cause fragrant mouth rod fragrant in certain time period
The concentration c of material volatilizationtWith total concentration (i.e. initial concentration c0, be, it is known that) ratio,
I.e.：Qt/QAlways=ct/c0(1)
cSurplus=c0-(Qt/QAlways)c0(2)
In formula (1), QtWith QAlwaysCan be integrated by the measured curve of Fig. 2 experiments and be calculated, thus, can by formula (1)
To obtain causing the ratio c of the concentration volatilized in section at any time by fragrant mouth rod and initial concentrationt/c0, table 1 gives different storages
Deposit the c corresponding to time tt/c0.Process design for cigarette is provided accurate parameter by the ratio, is the quality control of cigarette
System and production cost control provide foundation.
Table 1 causes the ratio c of fragrant mouth bar spices material volatile concentrations and total concentration (initial concentration)t/c0Relation over time
According to YC/T 138 1998《Tobacco and tobacco product sensory evaluation method》Method, at interval of 6 hours to cause
Fragrant mouth rod has carried out sensory evaluating smoking, and emphasis scores to the perfume quantity for causing fragrant mouth rod.The results are shown in Table 2:
Table 2 causes sensory evaluating smoking's result of fragrant mouth rod
The residual of the aroma component that the score value of the perfume quantity that sensory evaluating smoking is given is drawn with this programme in table 1 in comparison sheet 2
Amount and the ratio of original concentration, as a result unanimously, so that demonstrate the accurate reliability of this programme method acquired results.
The above, the only specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, any
Belong to those skilled in the art the invention discloses technical scope in, the change or replacement that can readily occur in all are answered
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be defined by scope of the claims.
Claims (3)
1. a kind of detection cigarette filter tip in aroma component residual quantity method, it is characterised in that：Using the hot instrument of thermal conductivity type micro come
Detected, the hot instrument of the thermal conductivity type micro includes the measuring cell being made up of sample cell (3) and reference cell (4), is distributed in measurement
Thermoelectric element (5), the heat abstractor (2) being arranged on around measuring cell, the constant temperature being arranged on around heat abstractor (2) around pond
Sleeve pipe (6) is arranged with the data analyzer (7) that device (1) and thermoelectric element (5) connect, sample cell (3) and reference cell (4),
The one side of thermoelectric element (5) is brought into close contact with sleeve pipe (6), and the another side of thermoelectric element (5) is brought into close contact with heat abstractor (2),
Methods described comprises the steps：
The fragrant mouth rod of cause is put in step one, sample cell (3), is put into the grade metering jet for not adding volatile spice in reference cell (4)
Rod；
Step 2, under the storage temperature for causing fragrant mouth rod, measure the spices volatilization process for causing fragrant mouth rod with the hot instrument of thermal conductivity type micro
In Endothermic power P versus time curves, Endothermic power P versus time curves reflect that the spices for causing fragrant mouth rod is waved
Send out speed dc/dt over time；
Step 3, by step 2 obtain Endothermic power P versus time curves be integrated, that is, obtain recept the caloric Qt, will cause
The spices rate of volatilization dc/dt of fragrant mouth rod is integrated the concentration for obtaining causing fragrant mouth rod to be volatilized within a certain period of time to the time
ct；
Step 4, speed dc/ for causing fragrant mouth bar spices material volatilization due to causing the Endothermic power P of the spices volatilization of fragrant mouth rod to be proportional to
Dt, therefore causes fragrant caloric receptivity Q of the mouth rod in certain time periodtWith total caloric receptivity QAlwaysRatio be equal to cause fragrant mouth rod at certain for the moment
Between in section spices volatilization concentration ctWith the ratio of total concentration, wherein c0For the initial concentration of spices, i.e. Qt/QAlways=ct/c0, and then
Obtain residual quantity c for causing spices in fragrant mouth rodSurplus=c0-(Qt/QAlways)c0.
2. as claimed in claim 1 detection cigarette filter tip in aroma component residual quantity method, it is characterised in that the step
Two are specially：In test process, cause fragrant mouth rod that heat absorption occurs in sample cell (3) and cause the temperature of sample cell (3) to reduce, so as to
Temperature difference Δ T is formed between sample cell (3) and heat abstractor (1), and temperature difference Δ T is imitated by Seebeck by thermoelectric element (5)
Voltage signal U should be converted into export to give data analyzer (7), data analyzer (7) is according to testing collected voltage letter
The data of number U and corresponding time t, obtain the Endothermic power P in the corresponding spices volatilization process for causing fragrant mouth rod with the time
Change curve.
3. as claimed in claim 1 or 2 detection cigarette filter tip in aroma component residual quantity method, it is characterised in that：In perseverance
The electric potential signal that the temperature fluctuation of thermostat is produced in warm device produces identical between the two in sample cell (3) and reference cell (4)
Interference signal, in step 2, both are offset by two interference signals are carried out subtractive on circuit, to eliminate the external world
Impact of the fluctuation of temperature to measurement result.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510143543.3A CN104713903B (en) | 2015-03-30 | 2015-03-30 | A kind of method of aroma component residual quantity in detection cigarette filter tip |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510143543.3A CN104713903B (en) | 2015-03-30 | 2015-03-30 | A kind of method of aroma component residual quantity in detection cigarette filter tip |
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| CN104713903A CN104713903A (en) | 2015-06-17 |
| CN104713903B true CN104713903B (en) | 2017-03-15 |
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| CN107402230B (en) * | 2017-08-01 | 2023-09-26 | 昆明理工大学 | Tobacco product smoke concentration measuring device and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0420852A (en) * | 1990-05-15 | 1992-01-24 | Showa Electric Wire & Cable Co Ltd | Method for measuring rate of content of foaming agent in synthetic resin containing foaming agent |
| FR2664058B1 (en) * | 1990-06-27 | 1996-09-20 | Fondis Sa | DETECTOR OF IMBULATED VOLATILE MATERIAL, IN PARTICULAR FOR A HEATING APPARATUS. |
| CN2501047Y (en) * | 2001-07-10 | 2002-07-17 | 武汉亿胜科技有限公司 | Tester for coal content in cement raw material |
| CN2519909Y (en) * | 2001-09-26 | 2002-11-06 | 上海理工大学 | Heat-measuring type biosensor for detecting residul pesticide |
| CN1995998A (en) * | 2006-01-06 | 2007-07-11 | 胜光科技股份有限公司 | Concentration monitoring device and method therefor |
| CN201340401Y (en) * | 2009-01-06 | 2009-11-04 | 上海理工大学 | Detection device used for general-purpose pesticide residue rapid detecting biosensor |
| DE102010048748A1 (en) * | 2010-10-16 | 2012-04-19 | Man Truck & Bus Ag | Method and device for determining the soot concentration in the engine oil of internal combustion engines |
| CN104181078B (en) * | 2014-09-01 | 2016-05-25 | 中国工程物理研究院化工材料研究所 | A kind of method and device of testing volatile matter content in explosive |
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