CN106872597B - The content assaying method of a variety of cations in a kind of cigarette mainstream flue gas - Google Patents
The content assaying method of a variety of cations in a kind of cigarette mainstream flue gas Download PDFInfo
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- CN106872597B CN106872597B CN201710110665.1A CN201710110665A CN106872597B CN 106872597 B CN106872597 B CN 106872597B CN 201710110665 A CN201710110665 A CN 201710110665A CN 106872597 B CN106872597 B CN 106872597B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses a kind of content assaying methods of cations a variety of in cigarette mainstream flue gas.The method comprises the following steps: (1) trapping of the cation in cigarette mainstream flue gas；(2) cationic extraction and the preparation of testing sample solution；(3) it is detected using ion chromatography；Wherein, the trapping and extraction of the cation in step (1) in cigarette mainstream flue gas method particularly includes: trapped using the cambridge filter of cambridge filter and preprocessed mistake；The preprocess method of the cambridge filter of the preprocessed mistake are as follows: trapping solution is added in cambridge filter first, being then placed in temperature is 22 ± 2 DEG C, and relative humidity balances 0-4hr in the environment of being 60 ± 5%.This method can measure Li in cigarette mainstream flue gas simultaneously+、Na+、NH4+、K+、Mg2+、Ca2+Deng the content of 6 kinds of cationic ions, this method has filled up prior art blank；In addition, this method also has sample analysis flux big, and accuracy, reproducible feature.
Description
Technical field
The present invention relates to tobacco detection technique fields, and in particular to the content of a variety of cations in a kind of cigarette mainstream flue gas
Measuring method.
Background technique
It is known as main flume from the flue gas that the filter end of cigarette is sucked out when suction.Main flume is divided into gaseous substance and grain phase
Substance.Usually at room temperature can (filter disc made of a kind of glass fibre can filter out diameter greater than 0.2 μm cambridge filter
Particle) flue gas partial be known as gaseous substance, gaseous substance accounts for about 92% of amount of flue gas emission or so；It can be cut by cambridge filter
The flue gas partial of stream is known as granule phase substance matter, and granule phase substance matter accounts for about 8% of amount of flue gas emission or so.
Ammonia is the important finger of one of harmful ingredients in flue gas and Chinese cigarette safety evaluatio in Hoffman list
One of mark.Amino acid, protein, nitrate and ammonium salt etc. of the ammonia in tobacco in flue gas, has cigarette smell larger
It influences.
Due to containing Na in the main and supplementary materials of the production cigarette such as tobacco leaf, cigarette paper+、NH4+、K+、Mg2+、Ca2+Etc. it is a variety of sun from
Son.Meanwhile lithium is effective mood stabilizer, lithium is to treat most having for acute mania and Manic-depressive disease prophylactic administration
Effect measure.Many studies demonstrate that lithium has the function of required or beneficial effect to animal and people.Animal, which lacks lithium, can lead to service life contracting
Short, reproduction abnormality, behavior change and other exceptions.Therefore, Li is paid close attention to+、Na+、NH4+、K+、Mg2+、Ca2+Ion is in cigarette smoke
In content, the pass to explore the behavior that many people in agitation are accustomed to smoking, between the ingredient and its content of cigarette smoke
System, provides a kind of direction.
But blank is still belonged to the research of lithium content in tobacco at present, more lack a kind of while measuring Li+、Na+、NH4+、K+、
Mg2+、Ca2+The method of ion.
Existing tobacco business standard YC/T 377-2010 " the measurement chromatography of ions of ammonia of main stream smoke of cigarette " is concerned only with
The content of ammonia of main stream smoke of cigarette, and this method is faced with the cumbersome disadvantage time-consuming, organic solvent consumption is more of pre-treatment, and
The problems such as sensitivity of method and selectivity are low, and matrix interference is serious.The various sides of the standard and existing literature, patent report
Method is the ammonia collected in granule phase substance using cambridge filter in pretreatment process, while utilizing the trapping that trapping solution is added
Trap collects the ammonia in gas gas-phase objects, pipettes cambridge filter extract liquor and each 5mL of gas phase adsorption liquid, is settled to 25mL, prepares to be measured
Sample.In detection process, flue gas trapping is step relatively complicated in the primary link and ammonia detection work of ammonia detection work
Suddenly, the device used is collecting trap.But it is hinged with the process of collecting trap, time-consuming and laborious, conventional efficient is low, gives detection work belt
Inconvenience is carried out.More very, the installation for trapping hydrazine has directionality, if connection is anti-, will lead to trapping solution and enters smoking machine, may
Smoking machine can be damaged.In addition, the sample preparation of " cambridge filter extract liquor and gas phase adsorption liquid respectively pipette 5mL and is settled to 25mL "
Process is troublesome time-consuming.
Therefore, have and develop a kind of content of a variety of cations and easy to operate of capable of measuring simultaneously in cigarette mainstream flue gas
Fast, the simple detection method of pre-treatment is not only to comply with " World Health Organization's Framework Convention on Tobacco Control " (WHO FCTC)
The status that dynamics constantly enhances carries out technological reserve to monitor more smoke components, also embodies tobacco as conscientious
Enterprise, the attitude that consumer is responsible for.
Summary of the invention
The purpose of the present invention is to provide a kind of content assaying methods of cations a variety of in cigarette mainstream flue gas, to solve
Certainly the prior art cannot detect the problem of a variety of cations in cigarette mainstream flue gas simultaneously.
To achieve the above object, the method for the present invention is achieved by the following technical programs:
The content assaying method of a variety of cations in a kind of cigarette mainstream flue gas, which is characterized in that comprise the following steps:
(1) trapping of the cation in cigarette mainstream flue gas；
(2) cationic extraction and the preparation of testing sample solution；
(3) it is detected using ion chromatography；
Wherein, the trapping and extraction of the cation in step (1) in cigarette mainstream flue gas method particularly includes: using common
Cambridge filter and the cambridge filter of preprocessed mistake are trapped；
The preprocess method of the cambridge filter of the preprocessed mistake are as follows: trapping is added first in common cambridge filter
Liquid, being then placed in temperature is 22 ± 2 DEG C, and relative humidity balances 0-4hr in the environment of being 60 ± 5%；The trapping solution includes
Following component: stabilizer, alcohol, acid and water.
When detecting the specific ingredient in different samples using ion chromatography, several ingredients, pre-treatment can be measured simultaneously
Journey is particularly significant.How to be extracted from the sample of complicated component need the ingredient that measures be can realize while check it is a variety of at
The key divided.And in the present invention, the ingredient in cigarette mainstream flue gas is sufficiently complex, how and meanwhile successfully trapping and extraction make the test
Li in cigarette main flume+、Na+、NH4 +、K+、Mg2+、Ca2+Ion is the problem that must be broken through first when detection, and inventor is through big
The experiment of amount is groped, we are using the cation using common cambridge filter trapping cigarette mainstream flue gas grain phase part, using warp
The cation of pretreated cambridge filter trapping gaseous phase of main stream smoke of cigarette part, while having extracted in cigarette mainstream flue gas
6 kinds of cation Li+、Na+、NH4 +、K+、Mg2+、Ca2+Ion, and then realizing can be using ion chromatography while measuring cigarette master
Flow the Li in flue gas+、Na+、NH4 +、K+、Mg2+、Ca2+Ion.This method overcomes the prior art that can only analyze in cigarette mainstream flue gas
A kind of deficiency of cation, has filled up prior art blank.It is caught in addition, this method has abandoned use during cation trapping
Collect trap, simplify operation, so that pre-treating method becomes very simple.
Preferably, the stabilizer in trapping solution selects liquid stabilisers or Pickering agent；
When stabilizer selects liquid stabilisers, liquid stabilisers: alcohol: acid: water=0-1000mL:0-1000mL:0-
100mL:1000mL；
When stabilizer selects Pickering agent, Pickering agent: alcohol: acid: water=0-5g:0-1000mL:0-100mL:
1000mL；
The liquid stabilisers are selected from alcohols, ketone or aldehydes；The alcohols is selected from methanol, ethyl alcohol and/or the third three
Alcohol, the ketone are selected from acetone and/or butanone, and the aldehydes is selected from formaldehyde, acetaldehyde and/or propionic aldehyde；
The Pickering agent is selected from paraformaldehyde；
The alcohol is selected from methanol, ethyl alcohol and/or glycerine；
The acid is selected from nitric acid, hydrochloric acid, sulfuric acid and/or perchloric acid.
Preferably, the additional amount of trapping solution is 0.1-100mL/cm2Cambridge filter, or cambridge filter is fully immersed in
1-2min in trapping solution.
It is further preferred that the trapping and extraction of the cation in step (1) in cigarette mainstream flue gas method particularly includes:
The cambridge filter of common cambridge filter and preprocessed mistake is placed in cigarette clamper, wherein the cambridge filter of preprocessed mistake
It is placed in the front end of cigarette clamper, is trapped.
Preferably, the preparation of extraction and testing sample solution cationic in step (2) method particularly includes: will be common
The cation that cambridge filter and the cambridge filter of preprocessed mistake trap is extracted with extractant, molten up to sample to be tested after filtering
Liquid；The extractant includes stabilizer, alcohol, acid and water；
The stabilizer selects liquid stabilisers or Pickering agent；
When stabilizer selects liquid stabilisers, liquid stabilisers: alcohol: acid: water=0-1000mL:0-1000mL:0-
100mL:1000mL；
When stabilizer selects Pickering agent, Pickering agent: alcohol: acid: water=0-5g:0-1000mL:0-100mL:
1000mL；
The liquid stabilisers are selected from alcohols, ketone or aldehydes；The alcohols is selected from methanol, ethyl alcohol and/or the third three
Alcohol, the ketone are selected from acetone and/or butanone, and the aldehydes is selected from formaldehyde, acetaldehyde and/or propionic aldehyde；
The Pickering agent is selected from paraformaldehyde；
The alcohol is selected from methanol, ethyl alcohol and/or glycerine；
The acid is selected from nitric acid, hydrochloric acid, sulfuric acid and/or perchloric acid.
Preferably, nitric acid described in trapping solution and extractant refers to that mass fraction is the concentrated nitric acid of 60-65%；Described
Hydrochloric acid refers to that mass fraction is the concentrated hydrochloric acid of 30-38%；The sulfuric acid refers to the concentrated sulfuric acid that mass fraction is about 90-98%；
The perchloric acid refers to the perchloric acid that mass fraction is about 65-75%.
Above-mentioned trapping solution and extract liquor are that inventor screens through many experiments, use above-mentioned trapping solution and extraction
Liquid can allow a variety of cation constituent trappings in cigarette mainstream flue gas abundant completely, and extract completely, while can stablize sample
Middle NH4+The effect of ion, assay result is stablized in sample in r for 24 hours, extends the holding time of effective sample solution,
Greatly increase daily sample amount detection.
Preferably, the extraction is placed in the container made of acid-fast alkali-proof plastics and carries out, the acid-fast alkali-proof modeling
Material is polyethylene or polytetrafluoroethylene (PTFE).
Above-mentioned acid-fast alkali-proof plastics are selected to can avoid introducing Na due to the factor of container material quality during the experiment+Ion
Equal interfering substances, influence the accuracy of detection, lead to the Na in packaging bag containing cigarette+The content detection of ion is worth higher system and misses
Difference.
Preferably, the filtering uses aperture to carry out for 0.22 or 0.45 μm of filter membrane, filter membrane material selection polyether sulfone
(PES) filter membrane, hydrophilic Kynoar (PVDF) filter membrane or nylon66 fiber filter membrane.
Preferably, the specific testing conditions of ion chromatography described in step (3) are as follows: chromatographic column selects cation analysis
Column；Flow velocity is 0.5-2mL/min；Sample volume is 25-100 μ L；Column temperature is 20-39 DEG C；Detection cell temperature is 20-39 DEG C；Inhibit
Device electric current is 2-300mA；Gradient is 0.001-0.035mol/LMAS isocratic elution or gradient elution program.
It is further preferred that the specific testing conditions of ion chromatography described in step (3) are as follows: chromatographic column selection CS12A,
CS16 or CS19 cation analysis column；Flow velocity is 0.6-1.2mL/min；Column temperature is 30-35 DEG C；Detection cell temperature is 30-35 DEG C；
Suppressor electric current is 2-120mA；Detector selects electric conductivity detector；Suppressor selects CSRS-II；Guard column selection CG12A,
CG16 or CG19 cation guard column；Instrument model is ICS-5000 or ICS-3000 plasma chromatography instrument, and the gradient is washed
De- program are as follows: when 0min, the concentration of MAS is 15.0mmol/L；When 6.0min, the concentration of MAS is 15.0mmol/L；6.1min
When, the concentration of MAS is 30.0mmol/L；When 8.5min, the concentration of MAS is 30.0mmol/L；When 12.6min, the concentration of MAS is
16.0mmol/L；When 15.0min, the concentration of MAS is 16.0mmol/L.
MAS of the present invention refers to Loprazolam aqueous solution.
When detecting the specific ingredient in different samples using ion chromatography, the selection of testing conditions is also extremely important, detection
Condition selection is incorrect or selection testing conditions have differences, and can all cause ingredient to be measured to be surveyed ineffective；Such as quasi-molecular ions point
It does not open, the problems such as sensitivity is not high.Inventor has found after a lot of trial and error, under above-mentioned specific testing conditions simultaneously
Detect cation Li in 6 in cigarette mainstream flue gas+、Na+、NH4 +、K+、Mg2+、Ca2+The content of ion has optimal ion
Peak separating degree, sensitivity and selectivity.
Preferably, the content assaying method, further includes quantitative analysis step, and the quantitative analysis uses external standard method
Or internal standard method.
Most preferably, the present invention is carried out using external standard method, and the specific method is as follows:
A series of standard working solution for preparing reference substances containing various concentration object establishes standard work using IC method
Make curve, the quantitative detection for sample；Cations in sample are calculated by formula (1)；
Ci=CI is surveyed*V/n...........................................(1)
In formula, CiFor the quality of cationic substance i in the main flume of every cigarette, unit is μ g/cig, as a result accurately
To 0.1 μ g/cig；
CI is surveyedThe content of resulting cationic substance i is measured for IC, unit is μ g/mL；
V is solvent volume used in extraction cambridge filter, unit mL；
N is the number for carrying out the cigarette of this analysis, unit cig；
Take the arithmetic mean of instantaneous value of two parallel samples as test result to get the Li into cigarette mainstream flue gas to be measured+、Na+、NH4 +、K+、Mg2+、Ca2+The content of ion.
In addition, the content of ammonia of main stream smoke of cigarette can also be calculated by formula (2)；
Ci=CI is surveyed*V*17.03/n/18.04........................................(2)
In formula, CiFor NH in the main flume of every cigarette4 +The quality of ion, unit are μ g/cig, are as a result accurate to 0.1
μg/cig；
CI is surveyedResulting NH is measured for IC4 +The content of ion, unit are μ g/mL；
V is solvent volume used in extraction cambridge filter, unit mL；
N is the number for carrying out the cigarette of this analysis, unit cig；
Take the arithmetic mean of instantaneous value of two parallel samples as test result to get the NH into cigarette mainstream flue gas to be measured4 +From
The content of son.
The final result of all samples Positive Ion Content subtracts in blank filter disc for the calculated value of the cations
The cations value.
The method of the present invention has the advantages that (1) content assaying method of the present invention using IC method while measuring volume
In cigarette main flume 6 in cation Li+、Na+、NH4 +、K+、Mg2+、Ca2+The content of ion, this method have filled up the prior art
Blank；(2) this invention simplifies trappings cationic in cigarette mainstream flue gas so that liquid relief in sample pretreatment process, merging,
These three steps of constant volume are also omitted therewith, only by single extraction and filtering, are just completed sample pretreatment process, are greatly simplified
Sample preparation procedure, improves detection efficiency；(3) trapping solution and extract liquor of the present invention, can allow cigarette master completely
It is abundant to flow a variety of cation constituent trappings in flue gas, and extracts completely, while NH in sample can be stablized4 +The effect of ion,
Assay result is stablized in sample in r for 24 hours, extends the holding time of effective sample solution, greatly increases daily sample
Product examine quantitation；(4) this method has sample analysis flux big, and accuracy, reproducible feature.
Detailed description of the invention
Fig. 1 is the Li in cigarette mainstream flue gas+、Na+、NH4 +、K+、Mg2+、Ca2+The standard solution chromatography of determination of ion content
Figure.
Fig. 2 is Li in the main flume of cigarette sample A+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content chromatogram.
Fig. 3 is Li in the main flume of cigarette sample B+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content chromatogram.
Fig. 4 is Li in the main flume of cigarette sample C+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content chromatogram.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Li in 1 cigarette mainstream flue gas standard solution of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) standard solution sample preparation condition:
Polytetrafluoro is used with trapping solution/extract liquor (when preparing standard solution sample, trapping solution and extract liquor are consistent)
Ethylene (PETT) volumetric flask prepares Li+、Na+、NH4 +、K+、Mg2+、Ca2+Ion concentration is the standard solution of 2 μ g/mL；
Trapping solution/extract liquor are as follows:
Acetone: methanol: ethyl alcohol: sulfuric acid (selects the concentrated sulfuric acid that mass fraction is about 98%): water, by 2mL:500mL:
500mL:3mL:1000mL mixing.
After shaken at room temperature 10min, extract liquor is collected filtered extract liquor and is made by 0.45 μm of polyether sulfone (PES) filter membrane
It is placed in ion chromatography bottle for sample, it is to be detected.
(2) sample ions chromatography IC testing conditions:
Chromatographic column: CS12A analytical column is equipped with CG12A guard column；Flow velocity: 1.0mL/min；Sample volume: 100 μ L；Column temperature: 35
℃；Detection cell temperature: 35 DEG C；Detector: electric conductivity detector；Suppressor: CSRS-II；Suppressor electric current: 80mA；Gradient:
(MSA) 0.020mol/L MAS isocratic elution.The Li in cigarette mainstream flue gas measured+、Na+、NH4 +、K+、Mg2+、Ca2+Ion
The standard solution chromatogram of assay is shown in Fig. 1.
Li in the main flume of 2 cigarette sample A of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) trapping of the cation in cigarette mainstream flue gas；
(2) cationic extraction and the preparation of testing sample solution；
(3) it is detected using ion chromatography；
(4) quantitative analysis；
The trapping of cation in step (1) in cigarette mainstream flue gas method particularly includes: by two cambridge filter (1
The cambridge filter of untreated common cambridge filter and 1 preprocessed mistake, untreated common cambridge filter trap cigarette
The cation of main flume grain phase part, using the sun of the cambridge filter trapping gaseous phase of main stream smoke of cigarette part of preprocessed mistake
Ion) it is placed in cigarette clamper, wherein the cambridge filter of preprocessed mistake is placed in the front end of cigarette clamper, and matte court
Before, using linear type smoking machine, under ISO mode, 4 cigarette are aspirated, carry out cationic trapping；
The preprocess method of the cambridge filter of the preprocessed mistake are as follows: trapping solution is added in cambridge filter first,
The additional amount of trapping solution is 0.3mL/cm2, being then placed in temperature is 22 DEG C, and relative humidity balances 1hr in the environment of being 60%；Institute
The composition for the trapping solution stated are as follows: methanol: nitric acid (selects the concentrated nitric acid that mass fraction is about 65%): water, by 500mL:1mL:
1000mL mixing；
The preparation of cationic extraction and testing sample solution in step (2) method particularly includes:
Trapping is had to the cambridge filter of flue gas grain phase part, and passes through the pretreated sword for having trapped flue gas gas phase portion
Bridge filter disc is put into 250mL tool plug polyethylene triangular flask, 100mL extractant is added, and shaken at room temperature extracts 30min, places 2min
Afterwards, extract liquor is collected filtered extract liquor and is placed in ion chromatography bottle as sample by 0.22 μm of nylon66 fiber membrane filtration,
Obtain testing sample solution；Wherein, the composition of extractant are as follows: methanol: ethyl alcohol: nitric acid: water, by 100mL:400mL:0.7mL:
1000mL mixing；
The specific testing conditions of ion chromatography described in step (3) are as follows: chromatographic column: CS12A analytical column is equipped with CG12A and protects
Guard post；Flow velocity: 1.2mL/min；Sample volume: 100 μ L；Column temperature: 35 DEG C；Detection cell temperature: 35 DEG C；Detector: electric conductivity detector；
Suppressor: CSRS-II；Suppressor electric current: 106mA；Gradient elution program is shown in Table 1, and obtained chromatogram is shown in Fig. 2；
1. gradient elution program of table
Quantitative analysis described in step (4) is carried out using external standard method, and the specific method is as follows: preparation is a series of to contain difference
The standard working solution of the reference substance of concentration target object establishes standard working curve using IC method, the quantitative detection for sample；
Cations in sample can be by being calculated in Summary by formula (1)；The content of ammonia can also be by summary of the invention
Formula (2) in part calculates, and testing result is shown in Table 2；
2. assay result of table
As can be seen that this method can detect the Li in cigarette mainstream flue gas simultaneously from table 2 and Fig. 2+、Na+、NH4 +、
K+、Mg2+、Ca2+Deng 6 kinds of cations, and Gradient program elution cationic peak separating degree each compared with Gradient elution is more preferable, detects base
Line is more smooth, and detection limit is low.In addition, this method pre-treating method is simple, significantly simplifies sample preparation procedure, inspection is improved
Survey efficiency.
Li in the main flume of 3 cigarette sample A of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) trapping of the cation in cigarette mainstream flue gas；
(2) cationic extraction and the preparation of testing sample solution；
(3) it is detected using ion chromatography；
(4) quantitative analysis；
The specific method of step (1), (2), (3) and (4) is same as Example 2, the difference is that step (2) is prepared into
To testing sample solution place 12hr after detected again, specific testing result is shown in Table 3,
3. assay result of table
As can be seen from Table 3, the testing result after testing sample solution placement 12hr and embodiment 2 detect immediately
As a result almost consistent, this illustrates, the cation in sample to be tested can be stablized under the protective effect of trapping solution and extractant to be deposited
Content assaying method of the present invention extends the holding time of effective sample solution, greatly increases daily sample
Amount detection.
Li in the main flume of 4 cigarette sample A of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) trapping of the cation in cigarette mainstream flue gas；
(2) cationic extraction and the preparation of testing sample solution；
(3) it is detected using ion chromatography；
(4) quantitative analysis；
The specific method of step (1), (2), (3) and (4) is same as Example 2, the difference is that step (2) is prepared into
To testing sample solution place and detected after r again for 24 hours, specific testing result is shown in Table 4,
4. assay result of table
As can be seen from Table 4, testing sample solution places what the testing result after r and embodiment 2 for 24 hours detected immediately
As a result almost consistent, this illustrates, the cation in sample to be tested can be stablized under the protective effect of trapping solution and extractant to be deposited
Content assaying method of the present invention extends the holding time of effective sample solution, greatly increases daily sample
Amount detection.
Li in the main flume of 5 cigarette sample A of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) trapping of the cation in cigarette mainstream flue gas；
(2) cationic extraction and the preparation of testing sample solution；
(3) it is detected using ion chromatography；
(4) quantitative analysis；
The specific method of step (1), (2), (3) and (4) is same as Example 4, the difference is that step (1) and (2)
In trapping solution and extractant composition it is different.Specific testing result is shown in Table 5.
The composition of the trapping solution are as follows: paraformaldehyde: ethyl alcohol: nitric acid (selects the dense nitre that mass fraction is about 65%
Acid): water is mixed by 3g:400mL:10mL:1000mL；
The composition of extractant are as follows: paraformaldehyde: ethyl alcohol: nitric acid: water is mixed by 3g:400mL:10mL:1000mL；
5. assay result of table
As can be seen from Table 5, the result of the detection of the testing result Yu embodiment 4 of testing sample solution almost one
It causes, this explanation, the cation in sample to be tested is using paraformaldehyde as the protective effect of the trapping solution of stabilizer and extractant
It can equally be stabilized down, content assaying method of the present invention extends the holding time of effective sample solution, significantly
Ground improves daily sample amount detection.
Li in the main flume of 6 cigarette sample B of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) trapping of the cation in cigarette mainstream flue gas；
(2) cationic extraction and the preparation of testing sample solution；
(3) it is detected using ion chromatography；
(4) quantitative analysis；
The trapping of cation in step (1) in cigarette mainstream flue gas method particularly includes: by two cambridge filter (1
The cambridge filter of untreated cambridge filter and 1 preprocessed mistake, untreated cambridge filter trap cigarette mainstream flue gas
The cation of grain phase part, using the cation of the cambridge filter trapping gaseous phase of main stream smoke of cigarette part of preprocessed mistake) it sets
In cigarette clamper, wherein the cambridge filter of preprocessed mistake is placed in the front end of cigarette clamper, and matte is facing forward, using turn
Dish-type smoking machine aspirates 10 cigarette under ISO mode, carries out cationic trapping；
The preprocess method of the cambridge filter of the preprocessed mistake are as follows: trapping solution is added in cambridge filter first,
The additional amount of trapping solution is 2mL/cm2, being then placed in temperature is 22 DEG C, and relative humidity balances 2hr in the environment of being 60%；It is described
Trapping solution composition are as follows: hydrochloric acid (select mass fraction be about 35.5% concentrated hydrochloric acid): water, by 2mL:1000mL mixing；
The preparation of cationic extraction and testing sample solution in step (2) method particularly includes:
Trapping is had to the cambridge filter of flue gas grain phase part, and passes through the pretreated sword for having trapped flue gas gas phase portion
Bridge filter disc is put into 250mL tool plug polyethylene triangular flask, 200mL extractant is added, and shaken at room temperature extracts 30min, places 2min
Afterwards, extract liquor is collected filtered extract liquor and is placed in ion chromatography bottle as sample by 0.45 μm of polyethersulfone membranes filtering,
Obtain testing sample solution；Wherein, the composition of extractant are as follows: acetone: ethyl alcohol: the concentrated sulfuric acid: water, by 1mL:400mL:2mL:1000mL
Mixing；
The specific testing conditions of ion chromatography described in step (3) are as follows: chromatographic column: CS19 analytical column is equipped with CG19 protection
Column；Flow velocity: 1.0mL/min；Sample volume: 100 μ L；Column temperature: 35 DEG C；Detection cell temperature: 35 DEG C；Detector: electric conductivity detector；Suppression
Device processed: CSRS-II；Suppressor electric current: 24mA；Gradient elution program is shown in Table 6, and obtained chromatogram is shown in Fig. 3；
6. gradient elution program of table
Quantitative analysis described in step (4) is carried out using external standard method, and the specific method is as follows: preparation is a series of to contain difference
The standard working solution of the reference substance of concentration target object establishes standard working curve using IC method, the quantitative detection for sample；
Cations in sample can be by being calculated in Summary by formula (1)；The content of ammonia can also be by summary of the invention
Formula (2) in part calculates, and testing result is shown in Table 7；
7. assay result of table
Li in the main flume of 7 cigarette sample C of embodiment+、Na+、NH4 +、K+、Mg2+、Ca2+Determination of ion content
(1) trapping of the cation in cigarette mainstream flue gas；
(2) cationic extraction and the preparation of testing sample solution；
(3) it is detected using ion chromatography；
(4) quantitative analysis；
The trapping of cation in step (1) in cigarette mainstream flue gas method particularly includes: by two cambridge filter (1
The cambridge filter of untreated cambridge filter and 1 preprocessed mistake, untreated cambridge filter trap cigarette mainstream flue gas
The cation of grain phase part, using the cation of the cambridge filter trapping gaseous phase of main stream smoke of cigarette part of preprocessed mistake) it sets
In cigarette clamper, wherein the cambridge filter of preprocessed mistake is placed in the front end of cigarette clamper, and matte is facing forward, using straight
Line style smoking machine aspirates 2 cigarette under HC mode, carries out cationic trapping；
The preprocess method of the cambridge filter of the preprocessed mistake are as follows: trapping solution is added in cambridge filter first,
The additional amount of trapping solution is 0.6mL/cm2, being then placed in temperature is 22 DEG C, and relative humidity balances 4hr in the environment of being 60%；Institute
The composition for the trapping solution stated are as follows: sulfuric acid (selects the concentrated sulfuric acid that mass fraction is about 98%): water is mixed by 2mL:1000mL；
The preparation of cationic extraction and testing sample solution in step (2) method particularly includes:
Trapping is had to the cambridge filter of flue gas grain phase part, and passes through the pretreated sword for having trapped flue gas gas phase portion
Bridge filter disc is put into 250mL tool plug polyethylene triangular flask, 200mL extractant is added, and shaken at room temperature extracts 30min, places 2min
Afterwards, extract liquor is collected filtered extract liquor and is placed in ion chromatography bottle as sample by 0.45 μm of polyethersulfone membranes filtering,
Obtain testing sample solution；Wherein, the composition of extractant are as follows: ethyl alcohol: concentrated hydrochloric acid (selects the dense salt that mass fraction is about 35.5%
Acid): water is mixed by 998mL:1.7mL:1000mL；
The specific testing conditions of ion chromatography described in step (3) are as follows: chromatographic column: CS12A analytical column is equipped with CG12 and protects
Guard post；Flow velocity: 1.5mL/min；Sample volume: 100 μ L；Column temperature: 25 DEG C；Detection cell temperature: 35 DEG C；Detector: electric conductivity detector；
Suppressor: CSRS-II；Suppressor electric current: 90mA；Gradient elution program is shown in Table 8, and obtained chromatogram is shown in Fig. 4；
8. gradient elution program of table
Quantitative analysis described in step (4) is carried out using external standard method, and the specific method is as follows: preparation is a series of to contain difference
The standard working solution of the reference substance of concentration target object establishes standard working curve using IC method, the quantitative detection for sample；
Cations in sample can be by being calculated in Summary by formula (1)；The content of ammonia can also be by summary of the invention
Formula (2) in part calculates, and testing result is shown in Table 9；
9. assay result of table
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (6)
1. the content assaying method of a variety of cations in a kind of cigarette mainstream flue gas, which is characterized in that comprise the following steps:
(1) trapping of the cation in cigarette mainstream flue gas；
(2) cationic extraction and the preparation of testing sample solution；
(3) it is detected using ion chromatography；
Wherein, the trapping and extraction of the cation in step (1) in cigarette mainstream flue gas method particularly includes: use cambridge filter
It is trapped with the cambridge filter of preprocessed mistake；
The preprocess method of the cambridge filter of the preprocessed mistake are as follows: trapping solution is added in cambridge filter first, then
Being put into temperature is 22 ± 2 DEG C, and relative humidity balances 0-4hr in the environment of being 60 ± 5%；The trapping solution includes such as the following group
Point: stabilizer, alcohol, acid and water；
Stabilizer in the trapping solution selects liquid stabilisers or Pickering agent；
When stabilizer selects liquid stabilisers, liquid stabilisers: alcohol: acid: water=0-1000mL:0-1000mL:0-100mL:
1000mL；
When stabilizer selects Pickering agent, Pickering agent: alcohol: acid: water=0-5g:0-1000mL:0-100mL:
1000mL；
The liquid stabilisers are ketone；The ketone is selected from acetone and/or butanone；
The Pickering agent is selected from paraformaldehyde；
The alcohol is selected from methanol, ethyl alcohol and/or glycerine；
The acid is selected from nitric acid, hydrochloric acid, sulfuric acid and/or perchloric acid；
The specific testing conditions of the ion chromatography are as follows: chromatographic column selects CS12A, CS16 or CS19 cation analysis column；Stream
Speed is 0.6-1.5mL/min；Column temperature is 30-35 DEG C；Detection cell temperature is 30-35 DEG C；Suppressor electric current is 2-120mA；Detection
Device selects electric conductivity detector；Suppressor selects CSRS-II；Guard column selects CG12A, CG16 or CG19 cation guard column；Instrument
Device model ICS-5000 or ICS-3000 plasma chromatography instrument；Gradient elution program are as follows: when 0min, Loprazolam aqueous solution
Concentration is 15.0mmol/L；When 6.0min, the concentration of Loprazolam aqueous solution is 15.0mmol/L；When 6.1min, Loprazolam
The concentration of aqueous solution is 30.0mmol/L；When 8.5min, the concentration of Loprazolam aqueous solution is 30.0mmol/L；12.6min when,
The concentration of Loprazolam aqueous solution is 16.0mmol/L；When 15.0min, the concentration of Loprazolam aqueous solution is 16.0mmol/L；
The cation is Li+、Na+、NH4 + 、K+、Mg2+And Ca2+Ion；
The preparation of cationic extraction and testing sample solution in the step (2) method particularly includes: filter common Cambridge
The cation that piece and the cambridge filter of preprocessed mistake trap is extracted with extractant, up to testing sample solution after filtering；Institute
The extractant stated includes stabilizer, alcohol, acid and water；
The stabilizer selects liquid stabilisers or Pickering agent；
When stabilizer selects liquid stabilisers, liquid stabilisers: alcohol: acid: water=0-1000mL:0-1000mL:0-100mL:
1000mL；
When stabilizer selects Pickering agent, Pickering agent: alcohol: acid: water=0-5g:0-1000mL:0-100mL:
1000mL；
The liquid stabilisers are selected from alcohols, ketone or aldehydes；The alcohols is selected from methanol, ethyl alcohol and/or glycerine, institute
The ketone stated is selected from acetone and/or butanone, and the aldehydes is selected from formaldehyde, acetaldehyde and/or propionic aldehyde；
The Pickering agent is selected from paraformaldehyde；
The alcohol is selected from methanol, ethyl alcohol and/or glycerine；
The acid is selected from nitric acid, hydrochloric acid, sulfuric acid and/or perchloric acid.
2. content assaying method according to claim 1, which is characterized in that the additional amount of trapping solution is 0.1-100mL/cm2
Cambridge filter, or cambridge filter is fully immersed in 1-2min in trapping solution.
3. content assaying method according to claim 1, which is characterized in that the trapping of the cation in cigarette mainstream flue gas
With extraction method particularly includes: the cambridge filter of common cambridge filter and preprocessed mistake is placed in cigarette clamper, wherein
The cambridge filter of preprocessed mistake is placed in the front end of cigarette clamper, is trapped.
4. content assaying method according to claim 1, which is characterized in that the extraction is placed in by acid-fast alkali-proof plastics
It is carried out in manufactured container, the acid-fast alkali-proof plastics are polyethylene or polytetrafluoroethylene (PTFE).
5. content assaying method according to claim 1, which is characterized in that the filtering use aperture for 0.22 or
0.45 μm of filter membrane carries out, filter membrane material selection polyether sulfone (PES) filter membrane, hydrophilic Kynoar (PVDF) filter membrane or nylon
66 filter membranes.
6. content assaying method according to claim 1, which is characterized in that further include quantitative analysis step, described determines
Amount analysis uses external standard method or internal standard method.
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