CN103472159B - 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 adopting ammonia content in ion chromatography cigarette smoke.
Background technology
In recent years, that studies along with " Chinese-style cigarette " deepened continuously, and " reducing tar and reducing harm " is adjusted to " lowering harm and decreasing coking " by State Bureau in time, and emphasis harm reduction, falls Jiao steadily.The compound identified in tobacco and flue gas at present has 5000 kinds, but harmful and carcinogenic composition only accounts for very small percentage.
HOFFMANN and HECHT disclosed " 43 kinds of compositions " list in 1991, disclose 69 kinds of objectionable constituent to calendar year 2001 HOFFMAN list.1998, Canadian government disclosed 46 kinds of objectionable constituent lists in cigarette mainstream flue gas.China, on " cigarette harmfulness Research on Index System " basis, determines 7 objectionable constituent indexs had the greatest impact to cigarette mainstream flue gas harmfulness: 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 smoker throat to occur contraction.Therefore reduce ammonia burst size in cigarette smoke and, to improving cigarette quality, reduce cigarette harmfulness significant.
This standard method of industry standard methods YC/T377-2010(that current tobacco business has established ammonia content in Analysis by Chromatography main flume is identical with 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, thus be unfavorable for determining ammonia value accurately, be more unfavorable for the lowering harm and decreasing coking of cigarette.Therefore the ammonia content how in Accurate Determining flue gas is the problem needing at present to solve, and problem most critical how to make the ammonia content in sample solution keep stable, to reduce experimental error.The research work of this respect has been carried out in recent years in industry, some research mainly lays particular emphasis on the interference be separated to reduce ammonia detection that the novel stratographic analysis post of application improves ammonia and methylamine, such as apply CS16 chromatographic column and ammonia and methylamine can obtain good degree of separation to meet quantitative test under the high temperature conditions, but the liquid to be measured of ammonia is still unstable; Some research application Flow Analyzers analyze the ammonia in main flumes, 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, and the such as Shi Wen village etc. purify by application stone Graphon the stability that liquid to be measured can improve ammonia in liquid to be measured, but the operation of this method is relatively loaded down with trivial details.Application number be 201210363076.1 Chinese patent disclose a kind of method that amino-acid analyzer measures the ammonia in cigarette mainstream flue gas, 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, establish automatic derivatization device after using amino-acid analyzer and post thereof and measure the analytical approach of ammonia of main stream smoke of cigarette, solve the sodion interference problem of chromatography of ions.Application number be 201010530910.2 Chinese patent disclose a kind of method measuring ammonia of main stream smoke of cigarette, comprise the following steps: the trapping of a, ammonia of main stream smoke of cigarette: adopt the ammonia of granule phase substance in cambridge filter trapping main flume; B, sample pre-treatments: the cambridge filter of trapping Smoke Particulate is put into container, add HCl concussion, then get granule phase substance extract respectively and gas phase adsorption liquid is mixed in container, what obtain ammonia of main stream smoke of cigarette prepares liquid; C, ammonia prepare liquid through mocromembrane filter after, can directly with 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 adopting ammonia content in 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 adopting ammonia content in ion chromatography cigarette smoke, application cambridge filter and absorption bottle trap the ammonia in main flume, after adding the granule phase substance in extract extraction cambridge filter, the absorbing liquid got in appropriate extract and absorption bottle merges, constant volume, measures by introducing ion chromatograph after aqueous phase metre filter; Described extract is the aldehyde solution containing strong acid.
Further, comprise the following steps:
(1) according to YC/T377-2010 smoking cigarette, trap mainstream smoke total particulate matter with cambridge filter, collect the ammonia of gas phase portion with the absorption bottle that trapping solution is housed; Aspirating 4 cigarette trapping solvent volumes is 20ml, and aspirating 20 cigarette trapping solvent volumes is 50ml;
(2) aspirate complete, with the cambridge filter containing granule phase substance containing the aldehyde solution extraction of strong acid;
(3) accurately pipette extract that 5ml step (2) obtains and the gas phase adsorption liquid that 5ml step (1) obtains, with aldehyde solution dilution constant volume after merging, by aqueous phase metre filter, obtain the liquid to be measured of ammonia, then use ion chromatography;
Ion Chromatographic Method and condition as follows: mobile phase: 0.020mol/L pyrovinic acid; Flow velocity: 1.0mL/min; Sample size: 25 μ L; Column temperature: 30 DEG C; Conductance cell temperature: 35 DEG C; 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 for vibration and ultrasonic.
Further, the lyosorption of described gas phase is deionized water and strong acid.
Beneficial effect of the present invention
Adopt the aldehydes solvent extraction filter disc containing strong acid, effectively can improve the stability that ammonia detects liquid.Use the present invention can determine the content of ammonia in sample solution accurately and rapidly by the chromatography of ions, be applicable to ammonia content in cigarette sample in enormous quantities and measure, have good practicality, be conducive to carrying out lowering harm and decreasing coking research in a deep going way.
Accompanying drawing explanation
Fig. 1 is ammonium ion standard solution working curve.
Embodiment
Embodiment 1
By commercial cigarettes A balance 48 hours under (22 ± 1) DEG C, relative humidity (60 ± 3) % condition, then determine and mark the stub length of smoking cigarette, aspirate 4 cigarette.
Trap mainstream smoke total particulate matter with cambridge filter, collect the ammonia of gas phase portion with the trapping bottle that the trapping solution of 20 ml deionized water is housed.
The filter disc of the main flume of 4 cigarette is had to put into 100mL conical flask trapping, add extract 20mL, in extract, concentration of formaldehyde is 3mmol/L, concentration of hydrochloric acid is 100mmol/L, and be then placed in by conical flask on velocity-modulated oscillator and vibrate 40 minutes, oscillator frequency is set to 160r/min.Accurately pipette 5mL above-mentioned grain phase extract and gas phase trapping solution respectively in the volumetric flask of 25mL, use extract constant volume, shake up rear use 0.45 micron of aqueous phase syringe filters and filter to be measured.
Chromatography of ions condition: mobile phase: 20mM Loprazolam, flow velocity: 1.0ml/min, chromatographic column: CS12A, sample size: 25 μ L, column temperature: 30 DEG C, 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 that the ammonia content that records of the inventive method is relatively stable, and significant change does not occur as seen from the table, and the ammonia content using 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 more than 5 and distribute relatively uniform, utilizes ion chromatograph to detect standard solution, adopts peak area to carry out linear fit to concentration: y=k*x+b, weight factor is 1/x, the curve r obtained
2>0.99, and obtain regression equation, typical curve is shown in Fig. 1.
Table 1 embodiment 1 is tested cigarette sample and is adopted new method and standard method YC/T377-2010 ammonia content stability analysis result
1.(unit: μ g/cig)
Note 1.: " A " represents the change of the ammonia content adopting this patent method to record; " B " represents the change of the ammonia content adopting standard method YC/T377-2010 to record
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 the low mark of embodiment 1, acceptance of the bid and the high standard recovery, 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 are all 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 measures mean value-non-mark-on and measures 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 |
| Non-mark-on | - | 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) DEG C, relative humidity (60 ± 3) % condition, then determine and mark the stub length of smoking cigarette, aspirate 4 cigarette.
Trap mainstream smoke total particulate matter with cambridge filter, collect the ammonia of gas phase portion 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 adsorption liquid and 5ml grain phase extract, 25ml is settled to formaldehyde and acetaldehyde mixed solution (formaldehyde, acetaldehyde volumetric molar concentration are respectively 1mmol/L, 1mmol/L), after crossing 0.45 micron membrane filter, analyze ammonia content in liquid to be measured at regular intervals, and investigate ammonia content in dissimilar cigarette and whether stablize.
Visible by table 3, fire-cured tobacco type and hybrid cigarette all can stablize the ammonia content of liquid to be measured within the regular hour, and therefore this method has good universality.
Table 2 time dissimilar cigarette ammonia content stability analysis result (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 is only, extract changes the formalin that 20mL concentration is 10% into.
Embodiment 4
Repeat embodiment 1, its difference is only, extract changes the hydrochloric acid solution of the 100mmol/L of 20mL into.
Embodiment 5
Repeat embodiment 1, its difference is only, extract changes 1% acetaldehyde solution of 20mL and the sulfuric acid solution of 200mmol/L into.
Embodiment 6
Repeat embodiment 1, its difference is only, 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 is clearly described, the restriction not 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 cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (4)
1. adopt a method for ammonia content in ion chromatography cigarette smoke, it is characterized in that, comprise the following steps:
(1) according to YC/T 377-2010 smoking cigarette, trap mainstream smoke total particulate matter with cambridge filter, collect the ammonia of gas phase portion with the absorption bottle that absorbing liquid is housed; Aspirating 4 cigarette trapping solvent volumes is 20ml, and aspirating 20 cigarette trapping solvent volumes is 50ml;
(2) aspirate complete, with the cambridge filter containing granule phase substance containing the aldehyde solution extraction of strong acid;
(3) accurately pipette that 5ml step (2) obtains extract and 5ml step (1) obtain gas phase adsorption liquid, with the described aldehyde solution dilution constant volume containing strong acid after merging, by aqueous phase metre filter, obtain the liquid to be measured of ammonia, then use ion chromatography;
Ion Chromatographic Method and condition as follows: mobile phase: 0.020mol/L pyrovinic acid; Flow velocity: 1.0mL/min; Chromatographic column: CS12A; Sample size: 25 μ L; Column temperature: 30 DEG C; Conductance cell temperature: 35 DEG C; Rejector electric current: 59mA;
Described aldehyde solution is one or several the mixed liquor in formaldehyde, acetaldehyde and propionic aldehyde;
Described aldehyde solution concentration is 0.3mmol/L-9mmol/L;
Described strong acid is hydrochloric acid or sulfuric acid;
Described strong acid concentration is 5mmol/L-200mmol/L.
2. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 1, is characterized in that: the time of described extraction is 10-40 minute.
3. 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.
4. the method for ammonia content in employing ion chromatography cigarette smoke according to claim 1, is characterized in that: described absorbing liquid is deionized water or strong acid.
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| 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 |
| CN105067390B (en) * | 2015-08-18 | 2019-11-22 | 福建中烟工业有限责任公司 | A method of measurement ammonia of main stream smoke of cigarette content |
| 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 |
| CN108508132B (en) * | 2017-02-28 | 2020-12-29 | 云南省烟草质量监督检测站 | Method for simultaneously measuring contents of various cations in tobacco |
| CN108508100B (en) * | 2017-02-28 | 2021-06-08 | 云南省烟草质量监督检测站 | Method for simultaneously measuring contents of Li +, Na +, NH4+, K +, Mg2+ and Ca2+ in reconstituted tobacco |
| 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 |
| CN106645503B (en) * | 2017-02-28 | 2019-11-01 | 云南省烟草质量监督检测站 | Li in packaging bag containing cigarette+、Na+、NH4+、K+、Mg2+、Ca2+The content assaying method of ion |
| 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 |
| CN108195966B (en) * | 2018-01-09 | 2020-10-13 | 湖北中烟工业有限责任公司 | Method for detecting ammonia content in aqueous gloss oil of cigarette tipping paper |
| CN110988188B (en) * | 2019-12-23 | 2022-12-23 | 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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