CN104122171B - A kind of selection is used for the method for the extraction system of measuring cigarette smoke granule phase substance acid-base value - Google Patents
A kind of selection is used for the method for the extraction system of measuring cigarette smoke granule phase substance acid-base value Download PDFInfo
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Abstract
The invention discloses a kind of selection for measuring the method for extraction system of cigarette smoke granule phase substance acid-base value; The method is to adopt various water/organic extraction systems to pass through trial and error method, measure the buffering equivalent β of water/organic solvent system, determine best extraction system by β again, and by verifying that the mensuration of pH value can not be subject to CO after selected extraction system extraction Smoke Particulate2Impact; Obtain the best extraction system for measuring cigarette smoke granule phase substance acid-base value; The method is simple, can obtain fast the best, the most effective extraction system pH value for Accurate Determining Smoke Particulate; So that set up a kind of standard detecting method of unified cigarette smoke granule phase substance pH.
Description
Technical field
The present invention relates to a kind of selection for measuring the method for extraction system of cigarette smoke granule phase substance acid-base value, belong toIn flue gas analysis detection field.
Background technology
Smoke pH is one of overall target of cigarette total quality reflection, can in concentrated expression cigarette composition, changeLearn composition and chemical balance, especially can reflect the form that exists of nicotine in flue gas. The 1950's, tobaccoChemists have started to notice the importance of flue gas pH.
The original definition of pH value: a kind of scale of hydrogen ion activity in the aqueous solution, namely molten on ordinary meaningThe criterion of liquid soda acid degree. Conventionally pH value is a number between 0 and 14, in the time that pH is greater than 7Wait, solution is alkalescence, and in the time of pH=7, it is neutral that solution is. but at non-aqueous solution or non-standard temperature and pressureUnder condition, pH=7 may not represent that solution is neutral, and this need to be by calculating this solvent under this conditionDissociation constant to decide pH be neutral value. So adopt different solvents pH value to compare to be do not have assortedMeaning. In pure non-aqueous solution and part non-aqueous solution, adopt pH determination of electrode pH to electrodeRequirement also very high, as the kind of electrode, response range etc. will be consistent. Find according to a large amount of literature surveys,The assay method of cigarette smoke pH value adopts electrode method more, and pH combination electrode is being measured operation letter on pHEasy row. And substantially can be divided three classes in the sample pre-treatments of cigarette smoke: the one, adopt pure aquatic systemAbsorb flue gas or extraction granule phase substance, then measure the pH value of the aqueous solution; The 2nd, adopt water/organic solvent systemAbsorb flue gas or extraction granule phase substance, and then measure the pH value of this solution; The 3rd, by apply one on electrodeLayer cushioning liquid absorbs flue gas and directly measures and obtain pH value. Two kinds of methods are the most universal above. According to determining of pH valueJustice and the feature of pH electrode, employing above two kinds of methods has comparison because of the pH value that the difference of extraction system obtainsLarge difference, and in the processing of pure water, different researchers also has diverse ways, has pure water is removed to CO2Process, have pure water furnishing pH=7 is processed, or the two is joined together, this is because in water and surrounding airCO2Also can affect the acid-base value of solution. These different processing methods cause adopting determination of electrode to obtainPH value is also different. Therefore in the time setting up the detection method of cigarette smoke granule phase substance pH, How to choose extractsThe system of getting is one of key point.
Summary of the invention
The object of the invention is to be to provide a kind of concept that adopts solution buffering equivalent to select the best, the most effectiveFor extracting the method for extraction system of its pH value of Smoke Particulate Accurate Determining, so that set up a kind of systemThe standard detecting method of one cigarette smoke granule phase substance pH.
The invention provides a kind of selection for measuring the method for extraction system of cigarette smoke granule phase substance acid-base value,The method comprises the following steps:
Step is a): hydrochloric acid solution is joined respectively to some groups of identical water/organic solvents with different volumesAfter in system, measure the pH value of each group of water/organic solvent system, the pH value recording is converted into [H+] concentration,With [H+] concentration is abscissa, the molar concentration of respectively organizing hydrochloric acid solution in water/organic solvent system is that ordinate carries outOne-variable linear regression, is defined as the slope of equation of linear regression the buffering equivalent of described water/organic solvent systemβ i, wherein, i represents the volumn concentration of water in water/organic solvent system;
Step is b): i is got in 0～100 to different values, repeating step process a), records different β iValue, makes β i relation curve corresponding to i value; On relation curve, select the β i of i >=50 correspondence, select β iWater/the organic solvent system of little correspondence is best extraction system;
Step is c): aspirate some groups of identical cigarette, after collecting with cambridge filter respectively, respectively with and stepA) some groups of water/organic solvent systems identical in are as extract ultrasonic extraction 30.0min～35.0min; By saltAfter acid solution joins respectively in described each group of extract with different volumes, measure the pH of each group of extractValue, is converted into [H by pH value+] concentration, with [H+] concentration is abscissa, respectively organizes the hydrochloric acid solution in extractMolar concentration be that ordinate carries out one-variable linear regression, the slope of equation of linear regression is defined as to described extractionThe buffering equivalent β Ei of liquid, wherein, i represents the volumn concentration of water in extract;
Steps d): the size of the β i that each different β Ei that comparison step c) obtains and step b) record,β Ei is far longer than β i, and the extract buffer capacity that has shown to extract Smoke Particulate is very large, extraction system and ringCO in border2Can not affect the pH value of extract, therefore can get rid of CO2The best body that step b) is selectedInterference to pH pH-value determination pH after system's extraction cigarette smoke granule phase substance.
Described organic solvent is the conventional organic solvent of extraction.
In described method, β i is less, shows that the buffer capacity of system is more weak, and this system is more easily subject to additionalThe impact of material and cause the variation of pH, β i is larger, shows that the buffer capacity of system is stronger, and this system is not moreEasily be subject to the impact of additional substance and cause the variation of pH.
The extraction system that the inventive method is selected is used for extracting Smoke Particulate, measures volume by pH combination electrodeCigarette Smoke Particulate acid-base value.
The combination electrode of surveying pH value in method of the present invention is to measure on the basis based on the aqueous solution,Water/the organic solvent system of i < 50 is that organic phase is main solution, is not suitable for measuring pH value with combination electrode; InstituteSelect the β i with i >=50 correspondence with the present invention, the minimum corresponding water/organic solvent system of selection β i is bestExtraction system.
Beneficial effect of the present invention is: can be rapidly and accurately from a large amount of extraction system by method of the present inventionSelect the extraction system of the most applicable extraction cigarette smoke granule phase substance, can Accurate Determining cigarette smoke granule phase substance soda acidProperty; So that set up a kind of standard detecting method of unified cigarette smoke granule phase substance pH.
Brief description of the drawings
[Fig. 1] is [H in water/isopropyl alcohol extraction system of embodiment 1+] buffering equivalent β corresponding to concentrationiCurve.
[Fig. 2] is [H in water/ethanol extraction system of embodiment 2+] buffering equivalent β corresponding to concentrationiCurve.
[Fig. 3] is [H in water/methanol extraction system of embodiment 3+] buffering equivalent β corresponding to concentrationiCurve.
After [Fig. 4] is water/isopropyl alcohol extraction system extraction Smoke Particulate of embodiment 4, its [H+] concentration is correspondingBuffering equivalent β EiCurve.
Detailed description of the invention
Following examples are intended to further illustrate content of the present invention, instead of limit the scope of the invention.
Embodiment 1
For example, prepare in advance 0.1mol/L with 75% pure water-25% Isopropanol Solvent (volume fraction, v/v)Hydrochloric acid solution, add respectively 0,1 μ L, 5 μ L, 10 μ L, 50 μ L, 80 μ L, 100 μ L, 200 μ LIn 75% pure water-25% Isopropanol Solvent of 20.0mL, measure respectively its pH value conversion and obtain different [H+]Concentration, with [the H obtaining+] concentration does X-axis, the concentration of the hydrochloric acid solution adding be (material of the hydrochloric acid addingThe concentration that obtains divided by 20mL of amount, taking mol/L) carry out one-variable linear regression, regression equation as ordinateSlope be defined as the buffering equivalent β of this systemi(wherein i=0,1,2 ... 100, i represents water-isopropyl alcoholThe percentage composition of water in volume ratio). Calculate β75, Here it is 75% water-25% Isopropanol SolventBuffering equivalent value. According to above-mentioned steps, measure respectively pure aquatic system, 65% water-35% Isopropanol Solvent, 50%Water-50% Isopropanol Solvent, 35% water-65% Isopropanol Solvent, 15% water-85% Isopropanol Solvent, 10% waterThe β i value of-90% Isopropanol Solvent, pure Isopropanol Solvent. Water content with system is mapped and is obtained Fig. 1 β i,Be exactly water-Isopropanol Solvent water content and the graph of a relation that cushions equivalent β. As shown in Figure 1, the water below 15%-The buffering equivalent minimum of Isopropanol Solvent, is secondly pure water, illustrates that their antiacid alkali ability is more weak, along withThe increase of water content in system, buffering equivalent β slowly increases, in the time of 35% water-65% isopropyl alcohol (v/v)β35Maximum.
Embodiment 2
For example, prepare in advance 0.1mol/L's with 75% pure water-25% ethanol system (volume fraction, v/v)Hydrochloric acid solution, adds respectively 0,1 μ L, 5 μ L, 10 μ L, 50 μ L, 80 μ L, 100 μ L, 200 μ LIn 75% pure water-25% ethanol system of 20.0mL, measure respectively its pH value conversion and obtain different [H+]Concentration, does X-axis with [H+] concentration obtaining, the concentration (material of the hydrochloric acid adding of the hydrochloric acid solution addingThe concentration that obtains divided by 20mL of amount, taking mol/L) carry out one-variable linear regression, recurrence side as ordinateThe slope of journey is defined as buffering equivalent β i (wherein i=0,1,2 of this system ... 100, i represents water-ethanol volumeThe percentage composition of water in ratio). Calculate β75, the buffering equivalent value of Here it is 75% water-25% ethanol system.According to above-mentioned steps, measure respectively pure aquatic system, 65% water-35% ethanol system, 50% water-50% ethanol system,35% water-65% ethanol system, 15% water-85% ethanol system, 10% water-90% ethanol system, straight alcohol systemβ i value. Water content with system is mapped and is obtained Fig. 2 β i, is exactly that water-ethanol system water content is worked as with bufferingThe graph of a relation of amount β. As shown in Figure 2, the buffering equivalent minimum of straight alcohol system, is secondly pure water, and it is describedAntiacid alkali ability more weak, along with the increase of water content in system, buffering equivalent β slowly increases,15% water-85% ethanol (v/v) during to 35% water-65% ethanol (v/v) β in maximum.
Embodiment 3
For example, prepare in advance 0.1mol/L's with 75% pure water-25% methanol system (volume fraction, v/v)Hydrochloric acid solution, adds respectively 0,1 μ L, 5 μ L, 10 μ L, 50 μ L, 80 μ L, 100 μ L, 200 μ LIn 75% pure water-25% methanol system of 20.0mL, measure respectively its pH value conversion and obtain different [H+]Concentration, with [the H obtaining+] concentration does X-axis, the concentration of the hydrochloric acid solution adding be (material of the hydrochloric acid addingThe concentration that obtains divided by 20mL of amount, taking mol/L) carry out one-variable linear regression, regression equation as ordinateSlope be defined as the buffering equivalent β of this systemi(wherein i=0,1,2 ... 100, i represents water-methanol bodyThe percentage composition of water in long-pending ratio). Calculate β75, the buffering of Here it is 75% water-25% methanol system is worked asValue. According to above-mentioned steps, measure respectively pure aquatic system, 65% water-35% methanol system, 50% water-50% firstAlcohol system, 35% water-65% methanol system, 15% water-85% methanol system, 10% water-90% methanol system, pureThe β of methanol systemiValue. With the water content of system to βiMapping obtains Fig. 3, is exactly that Water-Methanol System containsThe water yield and the graph of a relation that cushions equivalent β. As shown in Figure 3, the buffering of the Water-Methanol System below 15% is worked asAmount is minimum, is secondly pure water, illustrates that their antiacid alkali ability is more weak, along with moisture in systemThe increase of amount, buffering equivalent β slowly increases, β in the time of 35% water-65% methyl alcohol (v/v)35Maximum.
Embodiment 4
Aspirate 4 identical cigarette as one group of sample, aspirate 8 groups, after cigarette smoking, take off collectionThere is the cambridge filter of Smoke Particulate, enter as extractant with 20.0mL75% water-25% Isopropanol Solvent respectivelyRow ultrasonic extraction 30.0min-35.0min, measures its pH value. In 8 groups of extracts, add respectively different volumes0.1mol/L hydrochloric acid solution (be respectively 0,1 μ L, 5 μ L, 10 μ L, 50 μ L, 80 μ L, 100 μ L,200 μ L), measure and added 8 groups of extract pH values after hydrochloric acid. The pH value obtaining is converted and becomes [H+]Concentration, does X-axis with [H+] concentration, and the amount (taking mol/L) of the different hydrochloric acid solutions that add is ordinateCarry out one-variable linear regression, the buffering equivalent β Ei that the slope of regression equation is defined as this extract (whereinI=0,1,2 ... 100, i represents the percentage composition of water in water/isopropyl alcohol volume ratio). Calculate β E75, thisThe buffering equivalent value of the extract that 75% water-25% Isopropanol Solvent obtains as extractant exactly. According to above-mentioned stepSuddenly measure respectively pure aquatic system, 65% pure water-35% Isopropanol Solvent, 50% pure water-50% Isopropanol Solvent, 35%Pure water-65% Isopropanol Solvent, 15% pure water-85% Isopropanol Solvent, 10% pure water-90% Isopropanol Solvent,Pure Isopropanol Solvent is made the β Ei value of extractant. Fig. 4 is the extraction after water/Isopropanol Solvent extraction Smoke ParticulateGet liquid buffering equivalent and water/Isopropanol Solvent buffering equivalent comparison diagram. As seen from Figure 4, different water/isopropylsExtract after alcohol extraction system extraction Smoke Particulate adds after hydrochloric acid, and concentration of hydrochloric acid does not become with [H+] concentrationLinear relationship, from its trend, the buffering equivalent of each system extract is more much bigger than pure aquatic system, thanThe buffering equivalent of 35% water-65% isopropyl alcohol (v/v) system is also much bigger. Same water-ethanol system and water-The extract buffering equivalent of methanol system is also much bigger than pure aquatic system. Therefore can illustrate in water and environment inCO2Being very little on the impact of measurement result, is negligible.
Because aqueous buffer solution is demarcated for the pH meter using, when it is when measuring non-aqueous solution pH value,The dissociation constant of acid or alkali, the constant of medium, liquid junction potential (may produce the error of approximately 1 pH unit),The hydrogen ion response value of glass electrode all can change, and the value recording in this case can only be called apparentPH value. So according to the feature of pH electrode, be the requirement that does not meet us taking organic phase as main system,Therefore selecting pure water is the Acidity of Aikalinity that best extraction system is carried out evaluating cigarette flue gas granule phase substance.
Claims (3)
1. selection is used for a method for the extraction system of measuring cigarette smoke granule phase substance acid-base value, it is characterized in that,Comprise the following steps:
Step is a): hydrochloric acid solution is joined respectively to some groups of identical water/organic solvents with different volumesAfter in system, measure the pH value of each group of water/organic solvent system, the pH value recording is converted into [H+] concentration,With [H+] concentration is abscissa, the molar concentration of respectively organizing hydrochloric acid solution in water/organic solvent system is that ordinate carries outOne-variable linear regression, is defined as the slope of equation of linear regression the buffering equivalent of described water/organic solvent systemβ i, wherein, i represents the volumn concentration of water in water/organic solvent system;
Step is b): i is got in 0～100 to different values, repeating step process a), records different β iValue, makes β i relation curve corresponding to i value; On relation curve, select the β i of i >=50 correspondence, select β iWater/the organic solvent system of little correspondence is best extraction system;
Step is c): aspirate some groups of identical cigarette, after collecting with cambridge filter respectively, respectively with and stepA) some groups of water/organic solvent systems identical in are as extract ultrasonic extraction 30.0min～35.0min; By saltAfter acid solution joins respectively in described each group of extract with different volumes, measure the pH of each group of extractValue, is converted into [H by pH value+] concentration, with [H+] concentration is abscissa, respectively organizes the hydrochloric acid solution in extractMolar concentration be that ordinate carries out one-variable linear regression, the slope of equation of linear regression is defined as to described extractionThe buffering equivalent β Ei of liquid, wherein, i represents the volumn concentration of water in extract;
Steps d): the size of the β i that each different β Ei that comparison step c) obtains and step b) record,β Ei is far longer than β i, and the extract buffer capacity that has shown to extract Smoke Particulate is very large, extraction system and ringCO in border2Can not affect the pH value of extract, therefore can get rid of CO2The best body that step b) is selectedInterference to pH pH-value determination pH after system's extraction cigarette smoke granule phase substance.
2. the method for claim 1, is characterized in that, described organic solvent is to extract commonly use organicSolvent.
3. the method for claim 1, is characterized in that, β i is less, shows that the buffer capacity of system is more weak,This system is more easily subject to the impact of additional substance and causes the variation of pH, and β i is larger, shows the buffering of systemAbility is stronger, and this system is more not easy to be subject to the impact of additional substance and the variation that causes pH.
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| US5131415A (en) * | 1991-04-04 | 1992-07-21 | R. J. Reynolds Tobacco Company | Tobacco extraction process |
| JP2780513B2 (en) * | 1991-05-29 | 1998-07-30 | 日本電気株式会社 | Buffer capacity design method |
| JPH07319630A (en) * | 1994-05-27 | 1995-12-08 | Nec Corp | Buffer capacity determination system |
| DE19809829A1 (en) * | 1998-02-27 | 1999-09-02 | Merkel | Liquid chromatographic analysis of meconium for determination of nicotine and cotinine |
| CN102401816A (en) * | 2010-09-09 | 2012-04-04 | 上海海帝园艺有限公司 | Method for detecting alkaloid in tobacco |
| EP2607880A1 (en) * | 2011-12-21 | 2013-06-26 | Philip Morris Products S.A. | Method of producing an extract of a smokeless tobacco product |
| CN103852500B (en) * | 2014-01-20 | 2016-02-17 | 四川大学 | A kind of method of pH electrode the real time measure gas pH value |
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