CN106370609A - Method for measuring acid value of tobacco essence - Google Patents
Method for measuring acid value of tobacco essence Download PDFInfo
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- CN106370609A CN106370609A CN201610757408.2A CN201610757408A CN106370609A CN 106370609 A CN106370609 A CN 106370609A CN 201610757408 A CN201610757408 A CN 201610757408A CN 106370609 A CN106370609 A CN 106370609A
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- tobacco
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- acid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/314—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry with comparison of measurements at specific and non-specific wavelengths
- G01N2021/3155—Measuring in two spectral ranges, e.g. UV and visible
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- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a method for measuring the acid value of tobacco essence. The to-be-measured essence is dissolved with a 50% ethanol water solution, active carbon powder is added for treatment, and then the materials are filtered; a potassium iodate water solution and a potassium iodide water solution are added into filtrate for reacting, the materials are diluted with 50% ethanol water, and then a spectrophotometer is used for analysis at the 352nm wavelength. The result is obtained after drawing of a standard curve and calculating. The spectrophotometric method is applied to measuring the acid value of the essence for the first time. The recovery rate range ranges from 93.6% to 95.8%, and variable coefficients of three continuous measuring results are 0.00%. The method is easy and convenient to operate, high in analysis speed and high in accuracy and precision degree, and has good application prospects.
Description
Technical field
The invention belongs to flavouring essence for tobacco physical and chemical index detection technique field is and in particular to one kind being capable of Accurate Determining cigarette perfume
The method of smart acid number.
Background technology
The stability of flavouring essence for tobacco, can keep the concordance of Medicated cigarette fragrance characteristic, fragrance quality, so flavouring essence for tobacco
Quality stability is directly connected to the quality stability of cigarette product.At present the quality of flavouring essence for tobacco is mainly referred to by refractive power
Physical and chemical indexs such as number, relative density, acid number, volatility total amount and manually smell this two links fragrant and to control.Due to essence composition
Complexity, essence spice for cigarette produce, storage, transport, and allotment after storage, apply during, because of temperature
The reasons such as degree, humidity change and oxidation lead to the parameters such as density, refraction index, acid number, volatile ingredient total amount to change.For
Ensure the quality of flavouring essence for tobacco, tobacco business adopts automatical potentiometric titrimeter Deca titrant, ph electrode to indicate titration end-point
Method measure the acid number of flavouring essence for tobacco, but the method complex steps, determination efficiency is low.
Spectrophotography is a kind of common analysis method, and it is contained with measuring material to the selective absorbing of light based on material
Amount, has the advantages that analyze speed is fast, accuracy and precision is high, easy and simple to handle, highly versatile.If the method is applied to
The measuring it should can overcome the shortcomings of that existing detection method exists well of tobacco essence acid value, but in prior art not yet
There is successful report.
Content of the invention
Present invention aims to the deficiencies in the prior art, provide a kind of method measuring tobacco essence acid value, fortune
With spectrophotography, on the premise of ensureing accuracy in detection and precision, simplify the process measuring.
The purpose of the present invention is achieved by the following technical programs.
Unless otherwise stated, percent of the present invention is percentage by volume.
A kind of method measuring tobacco essence acid value, comprises the following steps:
(1) weigh essence sample for tobacco 0.5g to be measured, dissolved with concentration volume ratio 50% ethanol water, constant volume arrives
50ml, shakes up, and then moves in 100ml conical flask, plus 5g activated carbon powder concussion 30min, is transferred to centrifuge tube centrifugation 20min, mistake
Clear filtrate is taken after filter；
(2) take clear filtrate 5ml in 25ml color comparison tube, sequentially add 5g/l iodic acid aqueous solutions of potassium 4.0ml, 50g/l iodine
Change aqueous solutions of potassium 2.0ml, be settled to scale with concentration volume ratio 50% ethanol water, mix, after reaction 40s, use light splitting light
Degree counts the absorbance measuring essence sample for tobacco to be measured at wavelength 352nm；
(3) draw standard curve: with liquid-transfering gun pipette successively proven hydrochloric acid solution 8.0,10.0,12.0,14.0,
16.0th, 18.0,20.0,22.0 μ l are placed in the color comparison tube of 8 25ml, respectively refer to the described operation of step (2) and develop the color and measure
Afterwards, with absorbance as abscissa, hydrogen ion concentration draws standard working curve for vertical coordinate；
(4) result calculates: according to the absorbance of essence sample for tobacco to be measured, reads data, button from standard working curve
The hydrogen ion concentration of essence sample for tobacco to be measured is obtained after removing blank, then the hydrogenion concentration value band by essence sample for tobacco to be measured
Enter formula (1) to calculate, obtain the acid number of essence sample for tobacco to be measured, and using the meansigma methodss of parallel assay twice as final survey
Determine result；
Tobacco essence acid value is pressed formula (1) and is calculated:
In formula:
The acid number of av flavouring essence for tobacco, i.e. the milligram number of potassium hydroxide needed for neutralization 1g flavouring essence for tobacco, unit is milligram
(mg)；
The molal weight of 56.1 potassium hydroxide, unit is gram every mole (g/mol)；
chThe h of essence sample for tobacco to be measured+Concentration, unit is mM every liter (mmol/l)；
vhThe constant volume of chromogenic reaction, unit is milliliter (ml)；
N takes extension rate during clear filtrate colour developing；
1000 volume conversion factors, will be transformed into liter (l) with the volume that milliliter (ml) represents；
G essence sample for tobacco to be measured quality, unit is gram (g).
Final measurement result is accurate to 0.1mg；The tolerance of parallel determinations is twice: acid number 10 (containing) below
For 0.2；Acid number is 0.5 10～100；Acid number 100 (containing) more than be 1.0.
With respect to prior art, the invention has the advantages that spectrophotography is applied to cigarette by the present invention initiatively
Mensure with essence acid number.Its response rate scope is 93.6%～95.9%, 5 samples, the Variation Lines of continuous 3 measurement results
Number is 0.00%.The method is easy and simple to handle, analyze speed is fast, and accuracy and precision are high, have a good application prospect.
Brief description
The impact to sample solution absorbance for Fig. 1 potassium iodate solution addition；
The impact to sample solution absorbance for Fig. 2 liquor kalii iodide addition；
Fig. 3 standard working curve.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples, but drawings and Examples are not right
The restriction of technical solution of the present invention, all based on present invention teach that the change made, all should belong to protection scope of the present invention.
Embodiment 1
1. experimental principle, material and method
1.1 experimental principle
Essence sample for tobacco after chromogenic reaction, with spectrophotography at 352nm mensuration absorbance, in solution hydrogen from
The concentration of son is directly proportional to absorbance, can draw hydrogen ion concentration by absorbance, thus extrapolating the acid number of flavouring essence for tobacco.
1.2 materials and instrument
Potassium iodate (ar, Shanghai Run Jie chemical reagent company limited)；Potassium iodide (ar, Solution on Chemical Reagents in Shanghai company limited),
Hydrochloric acid (ar, Shantou, Guangdong city Xi Long chemical plant)；The distilled water (making by oneself) of removing carbon dioxide；Activated carbon powder (ar, Jining of Shandong Province sea
Receive environmental protection company limited)；5 essence sample for tobacco supervise sampling observation product for Yunnan Province's flavouring essence for tobacco.
Ja5002 balance (sensibility reciprocal 0.01g, Shanghai balance equipment factory)；Metler ae200 analytical balance (sensibility reciprocal:
0.0001g, metler toledo company of Switzerland)；Hp5873 ultraviolet-uisible spectrophotometer (hp company of the U.S.)；
1.3 sample treatment and analysis
1.3.1 sample pre-treatments
Claim essence sample for tobacco 0.5g to be measured, with 50% ethanol water dissolve (volume ratio), constant volume to 50ml, shake up,
Then move in 100ml conical flask, plus 5g activated carbon powder concussion 30min, it is transferred to centrifuge tube centrifugation 20min, after filtration, take clarification
Filtrate；
1.3.2 colour developing and mensure
Take clear filtrate 5ml in 25ml color comparison tube, sequentially add 5g/l iodic acid aqueous solutions of potassium 4.0ml, 50g/l potassium iodide
Aqueous solution 2.0ml, is settled to scale with 50% ethanol water (volume ratio), mix, reaction 40s after, with spectrophotometer in
352nm wavelength is measured.
2. result and discussion
2.1 choice of experimental conditions
2.1.1 wavelength selects
With 1nm for interval, from 200nm to 700nm, the hydrochloric acid solution after colour developing is scanned, gained absorption curve shows
There are two absworption peaks, respectively 280nm and 352nm, it is contemplated that 280nm chaff interference is more, therefore selects more distinctive
352nm does the optimal wavelength analyzed.
2.1.2 the impact to sample solution absorbance for the potassium iodate solution consumption
Keep other conditions constant, add different amounts of 5g/l iodic acid aqueous solutions of potassium, the trap of sample solution changes such as
Fig. 1.Result shows, when potassium iodate amount of aqueous solution used is in the range of 4.0ml, sample solution absorbance is maximum.Therefore this experimental selection
4.0ml.
2.1.3 the impact to sample solution absorbance for the liquor kalii iodide consumption
Other conditions are constant, be separately added into 50g/l liquor kalii iodide 1.2,1.6,1.8,2.0,3.0,4.0,5.0 and
8.0ml, surveys absorbance, as shown in Fig. 2 absorbance change is less when the addition of liquor kalii iodide is within 2ml.This experiment is selected
Select the addition that 2.0ml is liquor kalii iodide.
2.1.4 the impact to absorbance for the response time
After three kinds of reagent mixing, reaction occurs immediately, and solution is in faint yellow, and different reaction durations produces different extinctions
Degree.Keep other conditions constant, observe the absorbance change after 0s, 20s, 30s, 40s, 50s, 60s respectively, result shows, changes
Learn reaction very fast, reaction after 40s reaches and stablizes, the therefore selective response time is 40s.
2.2 standard curve
Prepare and demarcate hydrochloric acid solution, pipetted successively with pipet and demarcate the hydrochloric acid solution that concentration is 0.1032mol/l
8.0th, 10.0,12.0,14.0,16.0,18.0,20.0 and 22.0 μ l, is settled to 25ml, after developing the color and measure according to 1.3.2, obtains
To the standard working curve as Fig. 3, x-axis is the absorbance of solution, and y-axis is hydrion content, and equation of linear regression is y=
13.314x-0.3700, correlation coefficient r=0.9996.
2.3 the response rate
Add known quantity hydrochloric acid in the sample filtrate of known content (meansigma methodss of 3 mensure), measure its hydrion dense
Degree, the response rate is respectively 93.6%, 95.9% (being shown in Table 1), and the accuracy of illustration method is good, and testing result is reliable.
Table 1 response rate
2.4 it is repeated
By continuous detecting 3 times respectively of five samples of a, b, c, d, e, the results are shown in Table 2.The coefficient of variation is 0.00%, explanation
The precision of the method is high.
The reperformance test result of table 2 spectrophotography
3rd, conclusion
Using the acid number of spectrophotometry flavouring essence for tobacco easy and simple to handle, result is accurate, precision is high, is a kind of to expire
The method that foot modernizes flavouring essence for tobacco supervisory detection.
Claims (2)
1. a kind of method measuring tobacco essence acid value, comprises the following steps:
(1) weigh essence sample for tobacco 0.5g to be measured, dissolved with concentration volume ratio 50% ethanol water, constant volume, to 50ml, shakes
Even, then move in 100ml conical flask, plus 5g activated carbon powder concussion 30min, it is transferred to centrifuge tube centrifugation 20min, take clear after filtration
Clear filtrate；
(2) take clear filtrate 5ml in 25ml color comparison tube, sequentially add 5g/l iodic acid aqueous solutions of potassium 4.0ml, 50g/l potassium iodide
Aqueous solution 2.0ml, is settled to scale with concentration volume ratio 50% ethanol water, mixes, and after reaction 40s, uses spectrophotometer
The absorbance of essence sample for tobacco to be measured is measured at wavelength 352nm；
(3) draw standard curve: with liquid-transfering gun pipette successively proven hydrochloric acid solution 8.0,10.0,12.0,14.0,16.0,
18.0th, 20.0,22.0 μ l are placed in the color comparison tube of 8 25ml, respectively refer to after the described operation of step (2) develops the color and measure, with
Absorbance is abscissa, and hydrogen ion concentration draws standard working curve for vertical coordinate；
(4) result calculates: according to the absorbance of essence sample for tobacco to be measured, reads data from standard working curve, deduction is empty
Obtain the hydrogen ion concentration of essence sample for tobacco to be measured after white, then the hydrogenion concentration value of essence sample for tobacco to be measured is brought into public affairs
Formula (1) calculates, and obtains the acid number of essence sample for tobacco to be measured, and using the meansigma methodss of parallel assay twice as final mensure knot
Really；
Tobacco essence acid value is pressed formula (1) and is calculated:
In formula:
The acid number of av flavouring essence for tobacco, i.e. the milligram number of potassium hydroxide needed for neutralization 1g flavouring essence for tobacco, unit is milligram (mg)；
56.1 the molal weight of potassium hydroxide, unit is gram every mole (g/mol)；
chThe h of essence sample for tobacco to be measured+Concentration, unit is mM every liter (mmol/l)；
vhThe constant volume of chromogenic reaction, unit is milliliter (ml)；
N takes extension rate during clear filtrate colour developing；
1000 volume conversion factors, will be transformed into liter (l) with the volume that milliliter (ml) represents；
G essence sample for tobacco to be measured quality, unit is gram (g).
2. the method measuring tobacco essence acid value according to claim 1 it is characterised in that: parallel determinations twice
Tolerance is: it is 0.2 that acid number contains 10 below 10；Acid number is 0.5 10～100；It is 1.0 that acid number contains 100 more than 100；?
Whole measurement result is accurate to 0.1mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610757408.2A CN106370609A (en) | 2016-08-29 | 2016-08-29 | Method for measuring acid value of tobacco essence |
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| CN201610757408.2A CN106370609A (en) | 2016-08-29 | 2016-08-29 | Method for measuring acid value of tobacco essence |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109298129A (en) * | 2018-11-20 | 2019-02-01 | 四川中烟工业有限责任公司 | A method of measurement essence spice for cigarette acid value |
| CN110412026A (en) * | 2019-08-13 | 2019-11-05 | 张家口卷烟厂有限责任公司 | A kind of tobacco aromaticss preparation accuracy method for quickly detecting |
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Cited By (3)
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|---|---|---|---|---|
| CN109298129A (en) * | 2018-11-20 | 2019-02-01 | 四川中烟工业有限责任公司 | A method of measurement essence spice for cigarette acid value |
| CN110412026A (en) * | 2019-08-13 | 2019-11-05 | 张家口卷烟厂有限责任公司 | A kind of tobacco aromaticss preparation accuracy method for quickly detecting |
| CN110412026B (en) * | 2019-08-13 | 2022-03-18 | 张家口卷烟厂有限责任公司 | Method for rapidly testing preparation accuracy of tobacco flavor |
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