CN103472159A - Method for measuring ammonia content in cigarette smoke through ion chromatography - Google Patents
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Abstract
The invention discloses a method for measuring ammonia content in cigarette smoke through ion chromatography. The method comprises the steps that an F319-04 filter leaf and an absorption bottle gather ammonia in main stream smoke, extract liquor is added to extract particulate matter in the F319-04 filter leaf, moderate extract liquor is mixed with absorption liquid in the absorption bottle, volume metering is conducted, an aqueous phase filter is used for filtering the mixed liquid, and an ion chromatograph is introduced to conduct measuring, wherein the extract liquor is aldehyde with strong acid. Filter leaf extraction is conducted by the aldehyde solvent with the strong acid, and therefore the stability of ammonia detection liquid can be effectively improved. The method for measuring the ammonia content in the cigarette smoke through the ion chromatography can measure the ammonia content in the sample solution accurately and fast through the ion chromatography, and is suitable for measurement of the ammonia content in large numbers of cigarette samples, good in practicability and beneficial to deep harm-reduction and tar-reduction research.
Description
Technical field
The present invention relates to technical field of tobacco, particularly a kind of method that adopts ammonia content in the ion chromatography cigarette smoke.
Background technology
In recent years, along with deepening continuously of " Chinese-style cigarette " research, State Bureau was adjusted into " lowering harm and decreasing coking " by " reducing tar and reducing harm " in time, and Jiao falls in emphasis harm reduction steadily.The compound identified in tobacco and flue gas at present has 5000 kinds, but be harmful to carcinogenic composition, only accounts for very small percentage.
HOFFMANN and HECHT have announced " 43 kinds of compositions " list in 1991, to calendar year 2001 HOFFMAN list, announced 69 kinds of objectionable constituent.1998, Canadian government was announced 46 kinds of objectionable constituent lists in cigarette mainstream flue gas.China, on " cigarette harmfulness Research on Index System " basis, has determined 7 objectionable constituent indexs that cigarette mainstream flue gas harmfulness is had the greatest impact: CO, HCN, NNK, NH first
3, B[a] P, phenol, crotonaldehyde.Excess of ammonia not only makes the jealous intensity of cigarette become large, and produces stimulation and acid, causes that contraction appears in smoker throat.Therefore reduce ammonia burst size in cigarette smoke and, to improving the cigarette quality, reduce cigarette harmfulness significant.
This standard method of industry standard method YC/T377-2010(that current tobacco business has been set up ammonia content in the Analysis by Chromatography main flume is identical with the CN102012418A method), but the ammonia content in the method and CN102012418A in ammonia liquid to be measured is unstable, the total amount of ammonia in extract can constantly rise, thereby be unfavorable for determining ammonia value accurately, more be unfavorable for the lowering harm and decreasing coking of cigarette.Therefore how the ammonia content in the Accurate Determining flue gas is to need at present the problem solved, and the problem most critical is how to make the ammonia content in sample solution keep stable, to reduce experimental error.Carried out in recent years the research work of this respect in industry, some research mainly lays particular emphasis on the interference detected to reduce ammonia that separates that the novel stratographic analysis post of application improves ammonia and methylamine, for example apply the CS16 chromatographic column and under hot conditions ammonia and methylamine can obtain preferably degree of separation to meet quantitative test, but the liquid to be measured of ammonia is still unstable; Some research application Flow Analyzers are analyzed the ammonia in main flume, but this method fails to solve the stability of ammonia liquid to be measured equally; In addition, the method for stable ammonia liquid to be measured is also inquired in some research, purify by application stone Graphon the stability that liquid to be measured can improve ammonia in liquid to be measured such as Shi Wenzhuan etc., but this method operation is relatively loaded down with trivial details.The Chinese patent that application number is 201210363076.1 discloses a kind of method of measuring the ammonia in cigarette mainstream flue gas with amino-acid analyzer, it is according to the selection selectivity of ammonia and triketohydrindene hydrate chromogenic reaction, utilize the design concept of amino-acid analyzer, by the improvement to amino acid analysis method, set up the analytical approach of using automatic derivatization device after amino-acid analyzer and post thereof to measure ammonia of main stream smoke of cigarette, solved the sodion interference problem of chromatography of ions.The Chinese patent that application number is 201010530910.2 discloses a kind of method of measuring ammonia of main stream smoke of cigarette, comprises the following steps: the trapping of a, ammonia of main stream smoke of cigarette: the ammonia that adopts granule phase substance in cambridge filter trapping main flume; B, sample pre-treatments: the cambridge filter that will trap Smoke Particulate is put into container, adds HCl concussion, then gets respectively the granule phase substance extract and the gas phase absorption liquid is mixed in container, obtains the liquid for preparing of ammonia of main stream smoke of cigarette; C, ammonia prepare liquid after mocromembrane filters, can directly with the Continuous Flow Analysis instrument, analyze, each sample determination only needs 2min, can determine the burst size of ammonia of main stream smoke of cigarette.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that adopts ammonia content in the ion chromatography cigarette smoke, and the method is easy to operate, detection sensitivity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposals:
A kind of method that adopts ammonia content in the ion chromatography cigarette smoke, ammonia in application cambridge filter and absorption bottle trapping main flume, after adding the granule phase substance in extract extraction cambridge filter, get appropriate extract and the merging of the absorption liquid in absorption bottle, constant volume, introduce ion chromatograph after filtering by the water filtrator and measured; Described extract is the aldehyde solution that contains strong acid.
Further, comprise the following steps:
(1) according to YC/T377-2010 smoking cigarette, with cambridge filter, trap mainstream smoke total particulate matter, collect the ammonia of gas phase part with the absorption bottle that trapping solution is housed; Aspirating 4 cigarette trapping solvent volume is 20ml, and aspirating 20 cigarette trapping solvent volume is 50ml;
(2) aspirate complete, the cambridge filter that contains granule phase substance with the aldehyde solution extraction that contains strong acid;
(3) accurately pipette the gas phase absorption liquid that extract that 5ml step (2) obtains and 5ml step (1) obtain, with aldehyde solution dilution constant volume, filter by the water filtrator after merging, obtain the liquid to be measured of ammonia, then use ion chromatography;
Ion Chromatographic Method and condition are as follows: mobile phase: the 0.020mol/L pyrovinic acid; Flow velocity: 1.0mL/min; Sample size: 25 μ L; Column temperature: 30 ℃; Conductance cell temperature: 35 ℃; Rejector electric current: 59mA.
Further, described aldehyde solution is one or several the mixed liquor in formaldehyde, acetaldehyde and propionic aldehyde.
Further, the concentration of described aldehyde solution is 0.3mmol/L-9mmol/L.
Further, described strong acid is hydrochloric acid or sulfuric acid.
Further, described strong acid concentration is 5mmol/L-200mmol/L.
Further, the time of described extraction is 10-40 minute.
Further, described extraction mode is vibration and ultrasonic.
Further, the lyosorption of described gas phase is deionized water and strong acid.
Beneficial effect of the present invention
The aldehydes solvent extraction filter disc that employing contains strong acid, can effectively improve the stability that ammonia detects liquid.Use the present invention to determine accurately and rapidly the content of ammonia in sample solution by the chromatography of ions, be applicable to ammonia content in cigarette sample in enormous quantities and measure, good practicality is arranged, be conducive to carry out in a deep going way lowering harm and decreasing coking research.
The accompanying drawing explanation
Fig. 1 is ammonium ion standard solution working curve.
Embodiment
By commercial cigarettes A balance 48 hours under (22 ± 1) ℃, relative humidity (60 ± 3) % condition, then determine and the stub length of mark smoking cigarette, aspirate 4 cigarette.
Trap mainstream smoke total particulate matter with cambridge filter, collect the ammonia of gas phase part with the trapping bottle of trapping solution that 20 ml deionized water are housed.
There is the filter disc of the main flume of 4 cigarette to put into the 100mL conical flask trapping, add extract 20mL, in extract, concentration of formaldehyde is that 3mmol/L, concentration of hydrochloric acid are 100mmol/L, then conical flask is placed on velocity-modulated oscillator and vibrates 40 minutes, and oscillator frequency is made as 160r/min.Accurately pipette respectively 5mL above-mentioned grain phase extract and gas phase trapping solution in the volumetric flask of 25mL, use the extract constant volume, shake up 0.45 micron water syringe filters of rear use and filter to be measured.
Chromatography of ions condition: mobile phase: the 20mM Loprazolam, flow velocity: 1.0ml/min, chromatographic column: CS12A, sample size: 25 μ L, column temperature: 30 ℃, autosynthesis rejector electric current: 59mA.
In different chronometry ammonia solution to be measured, the content results of ammonia is as shown in table 1 respectively, apply as seen from the table significant variation of the relatively stable generation of ammonia content that the inventive method records, and the ammonia content that uses primary standard method YC/T377-2010 to record changes greatly.
Prepare the ammonia series standard working solution of 0.1 μ g/mL～1 μ g/mL, concentration gradient is more than 5 and distribute relatively evenly, utilizes ion chromatograph to be detected standard solution, adopts peak area to carry out linear fit: y=k*x+b to concentration, weight factor is 1/x, the curve r obtained
20.99, and obtaining regression equation, typical curve is shown in Fig. 1.
Table 1 embodiment 1 test cigarette sample adopts new method and standard method YC/T377-2010 ammonia content stability analysis result
1.(unit: μ g/cig)
Annotate 1.: " A " means the variation of the ammonia content that employing this patent method records; " B " means the variation of the ammonia content that employing standard method YC/T377-2010 records
The recovery result of embodiment 1
According to the burst size of ammonia in the method analysis of cigarette A main flume, record the ammonia content value under blank, basic, normal, high four levels, calculate low mark, acceptance of the bid and the high standard recovery of embodiment 1, the results are shown in Table 2.The recovery data that can obtain the mark-on experiment of basic, normal, high three levels from experimental data all are greater than 90%, and the recovery of this experimental technique is good.
The computing formula of the recovery is as follows:
The % recovery=100 * (mark-on measure mean value-mark-on is measured mean value)/add scalar
Table 2 recovery of standard addition (unit: μ g/cig)
| Title | The standard specimen measured value added | Detected value after mark-on | The % recovery |
| Mark-on not | - | 6.05 | - |
| Low mark | 4.99 | 11.16 | 102.4 |
| Acceptance of the bid | 7.81 | 13.70 | 97.9 |
| High standard | 13.57 | 19.22 | 97.05 |
Embodiment 2
By 2 kinds of Virginian-type cigarette B and C and a kind of blended type cigarette D balance 48 hours under (22 ± 1) ℃, relative humidity (60 ± 3) % condition, then determine and the stub length of mark smoking cigarette, aspirate 4 cigarette.
Trap mainstream smoke total particulate matter with cambridge filter, collect the ammonia of gas phase part with the trapping bottle that 20 milliliters of 5mmol/L strong acid trapping solution are housed.
Accurately pipette sulfuric acid mixture liquid (volumetric molar concentration of formaldehyde, acetaldehyde and sulfuric acid is respectively 1mmol/L, 1mmol/L, 50mmol/L) the extract extraction cambridge filter that 20ml contains formaldehyde and acetaldehyde, ultrasonic extraction 40min, merge 5ml gas phase absorption liquid and 5ml grain phase extract, be settled to 25ml with formaldehyde and acetaldehyde mixed solution (formaldehyde, acetaldehyde volumetric molar concentration are respectively 1mmol/L, 1mmol/L), after crossing 0.45 micron filter membrane, analyze at regular intervals ammonia content in liquid to be measured, and investigate ammonia content in dissimilar cigarette and whether stablize.
Visible by table 3, fire-cured tobacco type and hybrid cigarette all can be stablized the ammonia content of liquid to be measured in the regular hour scope, so this method has good universality.
Time dissimilar cigarette ammonia content stability analysis result of table 2 (unit: μ g/cig)
| The sample trade mark | 0h | 2h | 4h | 5h | 24h |
| A | 5.74 | 6.00 | 6.19 | 5.64 | 5.56 |
| B | 8.16 | 8.94 | 9.52 | 9.75 | 10.80 |
| C | 4.88 | 5.05 | 4.88 | 5.10 | 5.11 |
Embodiment 3
Repeat embodiment 1, its difference only is, extract changes the formalin that 20mL concentration is 10% into.
Embodiment 4
Repeat embodiment 1, its difference only is, extract changes the hydrochloric acid solution of the 100mmol/L of 20mL into.
Embodiment 5
Repeat embodiment 1, its difference only is, extract changes 1% acetaldehyde solution of 20mL and the sulfuric acid solution of 200mmol/L into.
Embodiment 6
Repeat embodiment 1, its difference only is, extract changes the 25% propionic aldehyde solution of 20mL and the hydrochloric acid solution of 5mmol/L into.
The above embodiment of the present invention is only for example of the present invention clearly is described, is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give all embodiments exhaustive.Every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention extends out or change that belong to.
Claims (9)
1. a method that adopts ammonia content in the ion chromatography cigarette smoke, it is characterized in that: the ammonia in application cambridge filter and absorption bottle trapping main flume, after adding the granule phase substance in extract extraction cambridge filter, get appropriate extract and the merging of the absorption liquid in absorption bottle, constant volume, introduce ion chromatograph after filtering by the water filtrator and measured; Described extract is the aldehyde solution that contains strong acid.
2. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 1 is characterized in that: comprise the following steps:
(1) according to YC/T377-2010 smoking cigarette, with cambridge filter, trap mainstream smoke total particulate matter, collect the ammonia of gas phase part with the absorption bottle that absorption liquid is housed; Aspirating 4 cigarette trapping solvent volume is 20ml, and aspirating 20 cigarette trapping solvent volume is 50ml;
(2) aspirate complete, the cambridge filter that contains granule phase substance with the aldehyde solution extraction that contains strong acid;
(3) accurately pipette that 5ml step (2) obtains extract and 5ml step (1) obtain the gas phase absorption liquid, after merging, with aldehyde solution dilution constant volume, by the water filtrator, filter, obtain the liquid to be measured of ammonia, then use ion chromatography;
Ion Chromatographic Method and condition are as follows: mobile phase: the 0.020mol/L pyrovinic acid; Flow velocity: 1.0mL/min; Sample size: 25 μ L; Column temperature: 30 ℃; Conductance cell temperature: 35 ℃; Rejector electric current: 59mA.
3. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 1 is characterized in that: described aldehyde solution is one or several the mixed liquor in formaldehyde, acetaldehyde and propionic aldehyde.
4. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 1, it is characterized in that: described aldehyde solution concentration is 0.3mmol/L-9mmol/L.
5. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 1, it is characterized in that: described strong acid is hydrochloric acid or sulfuric acid.
6. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 1, it is characterized in that: described strong acid concentration is 5mmol/L-200mmol/L.
7. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 1, it is characterized in that: the time of described extraction is 10-40 minute.
8. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 1 is characterized in that: described extraction mode is vibration and ultrasonic.
9. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 2, it is characterized in that: described absorption liquid is deionized water or strong acid.
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| CN104090082A (en) * | 2014-07-24 | 2014-10-08 | 云南中烟工业有限责任公司 | Method for forecasting pH value of full smoke of cigarette |
| CN104569194A (en) * | 2014-12-26 | 2015-04-29 | 浙江中烟工业有限责任公司 | Ion chromatographic measurement method for ammonia content in flue gas of electronic cigarette |
| CN105067390A (en) * | 2015-08-18 | 2015-11-18 | 福建中烟工业有限责任公司 | Method for measuring ammonia content in mainstream smoke of cigarettes |
| CN106645503A (en) * | 2017-02-28 | 2017-05-10 | 云南省烟草质量监督检测站 | Measuring method of contents of Li<+>, Na<+>, NH4<+>, K<+>, Mg<2+> and Ca<2+> ions in smoke-laden packaging bag |
| CN106872597A (en) * | 2017-02-28 | 2017-06-20 | 云南省烟草质量监督检测站 | The content assaying method of various cations in a kind of cigarette mainstream flue gas |
| CN106908564A (en) * | 2017-02-28 | 2017-06-30 | 云南省烟草质量监督检测站 | Lithium, sodium, ammonia, potassium, magnesium, the method for calcium content in smoke-free tobacco product are determined simultaneously |
| CN108195966A (en) * | 2018-01-09 | 2018-06-22 | 湖北中烟工业有限责任公司 | The detection method of ammonia content in a kind of cigarette tipping paper water-based gloss oil |
| CN108508100A (en) * | 2017-02-28 | 2018-09-07 | 云南省烟草质量监督检测站 | Measure Li in reconstituted tobacco simultaneously+、Na+、NH4+、K+、Mg2+、Ca2+The method of content |
| CN108508101A (en) * | 2017-02-28 | 2018-09-07 | 云南省烟草质量监督检测站 | The content assaying method of a variety of alkalies and alkaline earth ions in a kind of cigarette paper |
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| CN104090082A (en) * | 2014-07-24 | 2014-10-08 | 云南中烟工业有限责任公司 | Method for forecasting pH value of full smoke of cigarette |
| CN104090082B (en) * | 2014-07-24 | 2015-10-28 | 云南中烟工业有限责任公司 | The Forecasting Methodology of the full smoke pH of a kind of cigarette |
| CN104569194A (en) * | 2014-12-26 | 2015-04-29 | 浙江中烟工业有限责任公司 | Ion chromatographic measurement method for ammonia content in flue gas of electronic cigarette |
| CN105067390A (en) * | 2015-08-18 | 2015-11-18 | 福建中烟工业有限责任公司 | Method for measuring ammonia content in mainstream smoke of cigarettes |
| CN108508100A (en) * | 2017-02-28 | 2018-09-07 | 云南省烟草质量监督检测站 | Measure Li in reconstituted tobacco simultaneously+、Na+、NH4+、K+、Mg2+、Ca2+The method of content |
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| CN106908564A (en) * | 2017-02-28 | 2017-06-30 | 云南省烟草质量监督检测站 | Lithium, sodium, ammonia, potassium, magnesium, the method for calcium content in smoke-free tobacco product are determined simultaneously |
| CN106645503A (en) * | 2017-02-28 | 2017-05-10 | 云南省烟草质量监督检测站 | Measuring method of contents of Li<+>, Na<+>, NH4<+>, K<+>, Mg<2+> and Ca<2+> ions in smoke-laden packaging bag |
| CN108508101A (en) * | 2017-02-28 | 2018-09-07 | 云南省烟草质量监督检测站 | The content assaying method of a variety of alkalies and alkaline earth ions in a kind of cigarette paper |
| CN108508132A (en) * | 2017-02-28 | 2018-09-07 | 云南省烟草质量监督检测站 | The method for measuring a variety of cations in tobacco simultaneously |
| CN106908564B (en) * | 2017-02-28 | 2019-04-05 | 云南省烟草质量监督检测站 | The method for measuring lithium in smoke-free tobacco product, sodium, ammonia, potassium, magnesium, calcium content simultaneously |
| CN106872597B (en) * | 2017-02-28 | 2019-10-25 | 云南省烟草质量监督检测站 | The content assaying method of a variety of cations in a kind of cigarette mainstream flue gas |
| CN108195966A (en) * | 2018-01-09 | 2018-06-22 | 湖北中烟工业有限责任公司 | The detection method of ammonia content in a kind of cigarette tipping paper water-based gloss oil |
| CN110967427A (en) * | 2019-12-23 | 2020-04-07 | 江苏中烟工业有限责任公司 | Method for high-stability determination of ammonia content in cigarette mainstream smoke by adopting ion chromatography |
| CN110988188A (en) * | 2019-12-23 | 2020-04-10 | 江苏中烟工业有限责任公司 | Method for detecting ammonia content in particulate matters of main stream smoke of cigarettes |
| CN110967427B (en) * | 2019-12-23 | 2022-09-30 | 江苏中烟工业有限责任公司 | Method for high-stability determination of ammonia content in cigarette mainstream smoke by adopting ion chromatography |
| CN113655167A (en) * | 2020-05-12 | 2021-11-16 | 国家烟草质量监督检验中心 | Method for measuring ammonia content in main stream smoke of cigarette by automatic filter disc liquid coating device |
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