CN104215723B - Monomethyl amine, the method for monoethyl amine content in a kind of ion-chromatographic determination cigarette side-stream smoke - Google Patents
Monomethyl amine, the method for monoethyl amine content in a kind of ion-chromatographic determination cigarette side-stream smoke Download PDFInfo
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Abstract
The invention discloses monomethyl amine, the method for monoethyl amine content in a kind of ion-chromatographic determination cigarette side-stream smoke, comprise the following steps: the trapping of monomethyl amine and monoethyl amine, the preparation of cigarette smoke sample treatment, storing solution and standard working solution, supernatant liquor carries out ion chromatography respectively.Present invention achieves the Accurate Determining to the monomethyl amine in cigarette side-stream smoke and monoethyl amine, overcome the complex operation measuring the Derivative GC method existence using to monomethyl amine in cigarette mainstream flue gas and monoethyl amine for the prior art, waste time and energy, it is difficult to the drawback of accurate quantitative analysis, there is the advantages such as pre-treatment is simple, accurate, highly sensitive, reproducible.Gas phase and grain are separately processed detection by the distribution situation in gas phase and grain phase two mutually according to monomethyl amine in side-stream smoke and monoethyl amine, more reasonable in theory, and are easy to grasp monomethyl amine and distribution situation in gas phase and grain phase for the monoethyl amine.
Description
Technical field
The invention belongs to physical and chemical inspection technical field, be specifically related to the mensuration of organic amine in cigarette side-stream smoke.
Background technology
During result of combustion of tobacco, the thermal degradation of nicotine or other alkaloids is likely to generate monomethyl amine and monoethyl amine,
Monomethyl amine, monoethyl amine have strong foul smell, have stronger stimulation and corrosiveness to skin, eyes, the upper respiratory tract and lung,
During poisoning, central nervous system is impaired, may result in tracheitis, bronchitis, pneumonia, even pulmonary edema, in China's regulation air
The safe level of monomethyl amine is 5mg/m3.The existence in cigarette smoke of monomethyl amine and monoethyl amine removes the impact on cigarette odor-absorbing relatively
Outside great, its existence in side-stream smoke there is also negative effect to surrounding environment.
The current report to monomethyl amine and monoethyl amine for the document focuses mostly at samples such as water sample, cosmetics, beverages, to cigarette cigarette
In gas, the mensuration report of its content is less.The method using mainly has AAS, liquid chromatography, gas chromatography, top
Gas chromatography, the chromatography of ions etc..Wherein AAS disturbing factor is more, and reappearance is poor；Liquid chromatography and
Gas chromatography typically will be through derivation process, complex operation and time-consuming；Amine molecule easily absorber in headspace gas chromatography
Wall, sample size is difficult to accurately control.
Content of the invention
The present invention provides a kind of with methyl sulfonic acid for flowing phase Gradient elution, with 0.01mol/L hydrochloric acid solution for inhaling
Receiving liquid, the method for monomethyl amine and monoethyl amine in chromatography of ions rapid and accurate determination cigarette side-stream smoke, the method includes following
Step:
The trapping of monomethyl amine and monoethyl amine in A, side-stream smoke: by cigarette sample 22 DEG C ± 1 DEG C and relative humidity 60%
The environment of ± 2% balances after 48h, select average weight for ± 0.02g/and average resistance to suction for the cigarette that ± 49Pa/ props up be
Test cigarette, traps the granule phase substance of side-stream smoke, uses the absorption bottle of two series connection simultaneously with fish tail cover and glass fiber filter
Absorbing liquid is collected after absorbing the gas gas-phase objects in side-stream smoke successively with the watery hydrochloric acid of the flow velocity 0.01mol/L of 3000mL/min；
B, blank assay: take identical cigarette, under not lighting state, every carries out corresponding average mouth number suction, obtains reality
Test room room air blank and filter disc blank sample；
C, cigarette smoke sample treatment: a, effluent gas gas-phase objects (fish tail cover+absorption bottle): trapping is had the fish tail cover of gas gas-phase objects
Inwall is with in 0.01mol/L hydrochloric acid solution drip washing container, then by after in two GAS ABSORPTION bottles, absorbing liquid is transferred to said vesse,
Respectively by the hydrochloric acid solution washing absorption bottle of 0.01mol/L and side-stream smoke contact portion, cleaning solution is proceeded in the lump above-mentioned appearance
Device, then shake up after being settled to scale with hydrochloric acid solution, pipette supernatant liquor after standing and treat ion chromatography；B, granule phase substance (filter
Piece): aspirate after cigarette terminates, taken out glass fiber filter, after trap inwall filter disc is cleaned, by this filter disc and glass
Fiber filter disc together puts into Erlenmeyer flask, adds the hydrochloric acid solution of 0.01mol/L, pipettes supernatant liquor, warp after ultrasonic extraction 50min
After 0.22 m aqueous phase membrane filtration, collect filtrate and treat ion chromatography；
The storing solution of D, monomethyl amine and monoethyl amine and the preparation of standard working solution: accurately weigh 0.1g40% mass respectively
Concentration monomethylamine aqueous solution, 0.06g65%～70% mass concentration the monoethyl amine aqueous solution in container, use 0.01mol/L hydrochloric acid
It after solution is settled to scale, is configured to the hybrid standard storing solution of monomethyl amine, monoethyl amine, then standard inventory described in stepwise dilution
Liquid, after being configured to the series standard working solution that the 0.02nd, concentration be respectively the 0.04th, the 0.08th, the 0.2nd, the 0.4th, the 0.8th, 2.0 g/mL, warp
Ion chromatography obtains the linear equation coefficient R of monomethyl amine ion and monoethyl amine ion2It is 0.9999；
E, the supernatant liquor by above-mentioned a, b step carry out ion chromatography respectively, chromatography of ions condition: chromatographic column:
CS16 (4 × 250 mm) splitter, CGl6 (4 × 50 mm) guard column；Electric conductivity detector, wears peace CSRS ULTRA-II (4
Mm) suppressor；Flowing phase: 10mmol/L methyl sulfonic acid, Gradient elution, elution time is 40min；Flow velocity: 1.0 mL/
min；Sample size: 25uL；Column temperature: 60 DEG C；Autosynthesis suppressor electric current: 39mA.
The side-stream smoke grain obtaining after above-mentioned ion chromatography is neutralized mutually the content of monomethyl amine and monoethyl amine in gas phase
Substitute into below equation (1) respectively and formula (2) calculates, then the total amount of monomethyl amine in side-stream smoke and monoethyl amine is substituted into formula
(3) content of monomethyl amine and monoethyl amine in rapid and accurate determination cigarette side-stream smoke is got final product.
In above formula: M1Determinand content in cigarette side-stream smoke gas phase, unit is microgram every (μ g/ props up)；
C1The mensuration concentration of determinand ion in gas phase liquid to be measured, unit is micrograms per millilitre (μ g/mL)；
C01The mensuration concentration of determinand ion in gas phase blank solution, unit is micrograms per millilitre (μ g/mL)；
M2Determinand content in cigarette side-stream smoke grain phase, unit is microgram every (μ g/ props up)；
C2The mensuration concentration of determinand ion in grain liquid mutually to be measured, unit is micrograms per millilitre (μ g/mL)；
C02The mensuration concentration of determinand ion in grain phase blank solution, unit is micrograms per millilitre (μ g/mL)；
M determinand molecule formula weight, monomethyl amine is 31, and monoethyl amine is 45；
Determinand content in M cigarette side-stream smoke, unit is microgram every (μ g/ props up)；
The number of n suction cigarette, unit:.
Experimental result requires that being accurate to 0.1 μ g/ props up；
The technological progress that the present invention obtains:
Owing to using technique scheme of the present invention, the technological progress that the present invention obtains is:
1st, the present invention uses the chromatography of ions to achieve the accurate survey to the monomethyl amine in cigarette side-stream smoke and monoethyl amine
Fixed, overcome the derivatization-gas chromatography measuring employing to monomethyl amine in cigarette mainstream flue gas and monoethyl amine for the prior art
The complex operation existing, wastes time and energy, it is difficult to the drawback of accurate quantitative analysis, and Comparatively speaking, the chromatography of ions of the present invention has front place
Manage the advantages such as simple, accurate, highly sensitive, reproducible, it is achieved that the standard to monomethyl amine in cigarette side-stream smoke and monoethyl amine
Really measure.
2nd, in the present invention, the linear concentration scope of monomethyl amine and monoethyl amine is 0.02～2.0 g/mL, and the range of linearity is wider,
Linear equation coefficient R2It is 0.9999, linearly preferably.And the concentration range of monomethyl amine in actual sample gas phase and grain phase
Being about 0.1～1.0 g/mL, the concentration range of monoethyl amine is about 0.05～0.5 g/mL, thus linearly the fully meeting of the present invention
The mensuration of actual sample.
3rd, in the present invention in cigarette side-stream smoke gas phase monomethyl amine and monoethyl amine detection limit be respectively 0.25 μ g/ prop up,
0.28 μ g/ props up；In grain phase, the detection limit of monomethyl amine and monoethyl amine is respectively that 0.038 μ g/ props up, 0.054 μ g/ props up, far below reality
The measured value of monomethyl amine and monoethyl amine in sample gas phase and grain phase, thus the accurate quantitative analysis to monomethyl amine and monoethyl amine can be realized.
4th, in the present invention rate of recovery of monomethyl amine between 80.7%～102.9%, the rate of recovery of monoethyl amine 85.1%～
Between 102.1%, the rate of recovery is preferable, illustrates that accuracy of the present invention is higher.The parallel determination 5 under identical conditions of same cigarette sample
Secondary, the precision (RSD) of calculated monomethyl amine and monoethyl amine is respectively less than 3%, present invention repeatability is described preferably.
5th, the present invention according to monomethyl amine in side-stream smoke and monoethyl amine the distribution situation in gas phase and grain phase two, by gas
Separately process detection with grain mutually mutually, more reasonable in theory, and be easy to grasp monomethyl amine and monoethyl amine in gas phase and grain phase
Distribution situation.
Brief description
Fig. 1 is side-stream smoke capturing device schematic diagram of the present invention.
Fig. 2 is monomethyl amine and monoethyl amine standard sample chromatography of ions figure in cigarette side-stream smoke.
Fig. 3 is typical sample chromatography of ions figure.
Fig. 4 is that methyl sulfonic acid concentrations affects figure to determinand separating degree.
Fig. 5 is that column temperature affects figure to determinand separating degree.
What Fig. 6 was ultrasonic time on monomethyl amine in granule phase substance and monoethyl amine content affects figure.
Fig. 7 is that in liquid to be measured, monomethyl amine and monoethyl amine content change over tendency chart.
Detailed description of the invention
The present embodiment key instrument: use the five duct effluents that German Borg.waldt.KC company as shown in Figure 1 produces
Smoking machine, wherein connects main flume trap 5, installing cambridge filter, trap 5 arrival end in trap 5 bottom fish tail cover 1
Being passed through main flume 6, fish tail cover 1 top connects side-stream smoke trap 2, and side-stream smoke trap 2 port of export concatenation gas is inhaled
Receive bottle the 3rd, 4；Dai An company of U.S. IC-3000 ion chromatograph, joins electric conductivity detector and gradient elution pump；City of Kunshan's ultrasonic instrument
The KQ-500 type ultrasonic washing instrument that Co., Ltd produces；The 0.0001g AB204-that Mettler Toledo company of Switzerland produces
The Elix Milli-Q ultrapure water machine that S type electronic balance and MILLIPORE SAS company of the U.S. produce.
Main agents and material: analyze single methylamine, 40% aqueous solution, analyze single ethamine 65%～70% aqueous solution, top grade
Pure hydrochloric acid；Φ 44 cambridge filter；80ml GAS ABSORPTION bottle；10 kinds of cigarette samples purchased from local market；Absorbing liquid is
The aqueous hydrochloric acid solution of 0.01mol/L.
Realize the method for monomethyl amine and monoethyl amine content in ion-chromatographic determination cigarette side-stream smoke of the present invention, including with
Lower step:
The trapping of monomethyl amine and monoethyl amine in A, side-stream smoke: by cigarette sample 22 DEG C ± 1 DEG C and relative humidity 60%
The environment of ± 2% balances after 48h, select average weight for ± 0.02g/and average resistance to suction for the cigarette that ± 49Pa/ props up be
Test cigarette, traps the granule phase substance of side-stream smoke with fish tail cover and glass fiber filter, uses each addition of two series connection simultaneously
Have the hydrochloric acid solution of 30mL0.01mol/L as the flow velocity 0.01mol/L with 3000mL/min for the absorbing liquid watery hydrochloric acid successively
Absorbing liquid is collected after absorbing the gas gas-phase objects in side-stream smoke；Had a suck of according to every 60 seconds, every mouthful of puff duration 2s, take out for every mouthful
Inhale capacity 35ml, then collect cigarette side-stream smoke granule phase substance with the cambridge filter of Φ 44mm, on five duct effluent smoking machines
Four cigarette are aspirated in each duct, after cigarette smoking terminates, take out fish tail cover, side-stream smoke trap and two after suction 2 mouthfuls
The absorption bottle of series connection, carries out sample pre-treatments immediately；
B, blank assay: take identical cigarette, do not light, every carries out corresponding average mouth number suction, obtains not lighting shape
Laboratory room air blank under state and filter disc blank sample, carry out blank deduction in last measurement result after process；
C, cigarette smoke sample treatment: a, effluent gas gas-phase objects (fish tail cover+absorption bottle): fish tail cover inwall 60mL concentration is
The hydrochloric acid solution drip washing of 0.01mol/L is in 200mL volumetric flask, then is transferred to above-mentioned by absorbing liquid in two GAS ABSORPTION bottles
After in 200mL volumetric flask, respectively with the hydrochloric acid solution washing absorption bottle that 30mL concentration is 0.01mol/L and side-stream smoke contact site
Point, after each absorption bottle respectively washs 2 times～3 times, proceed to cleaning solution in 200mL volumetric flask in the lump, then with salt acid extraction solution
Shake up after being settled to scale, pipette 1mL supernatant liquor after standing 2min and treat ion chromatography；B, granule phase substance (filter disc): suction
After complete cigarette terminates, take out glass fiber filter, trap inwall wiped clean with clean 1/4th filter discs, by this filter disc and
Glass fiber filter is together put in 100mL Erlenmeyer flask, the hydrochloric acid solution accurately adding 30mL concentration to be 0.01mol/L, ultrasonic
Pipetting about 2mL supernatant liquor after extraction 50min, after 0.22 m aqueous phase membrane filtration, filtrate treats ion chromatography；
The storing solution of D, monomethyl amine and monoethyl amine and the preparation of standard working solution: accurately weigh 0.1g40% mass respectively
Concentration monomethylamine aqueous solution, 0.06g65%～70% mass concentration the monoethyl amine aqueous solution in 100mL volumetric flask, use
It after 0.01mol/L hydrochloric acid solution is settled to scale, is configured to the hybrid standard storing solution of monomethyl amine, monoethyl amine, then dilute step by step
Release described standard reserving solution, be configured to concentration be respectively the 0.02nd, the 0.04th, the 0.08th, the 0.2nd, the 0.4th, the 0.8th, 2.0 g/mL series mark
After quasi-working solution, obtain the linear equation coefficient R of monomethyl amine ion and monoethyl amine ion through ion chromatography2It is
0.9999；
E, the supernatant liquor by above-mentioned a, b step carry out ion chromatography respectively, chromatography of ions condition: chromatographic column:
CS16 (4 × 250 mm) splitter, CGl6 (4 × 50 mm) guard column；Electric conductivity detector, wears peace CSRS ULTRA-II (4
Mm) suppressor；Flowing phase: 10mmol/L methyl sulfonic acid, Gradient elution, elution time is 40min；Flow velocity: 1.0 mL/
min；Sample size: 25uL；Column temperature: 60 DEG C；Autosynthesis suppressor electric current: 39mA.
Obtain monomethyl amine as shown in Figure 2 and monoethyl amine standard sample chromatography of ions figure and typical sample as shown in Figure 3
Chromatography of ions figure, in Fig. 2, a represents monomethyl amine ion, and b represents monoethyl amine ion；In Fig. 3, c represents monomethyl amine ion, and d represents one
Ethamine ion.
The side-stream smoke grain obtaining after above-mentioned ion chromatography is neutralized mutually the content of monomethyl amine and monoethyl amine in gas phase
Substitute into below equation (1) respectively and formula (2) calculates, then the total amount of monomethyl amine in side-stream smoke and monoethyl amine is substituted into formula
(3) content of monomethyl amine and monoethyl amine in rapid and accurate determination cigarette side-stream smoke is got final product.
In above formula: M1Determinand content in cigarette side-stream smoke gas phase, unit is microgram every (μ g/ props up)；
C1The mensuration concentration of determinand ion in gas phase liquid to be measured, unit is micrograms per millilitre (μ g/mL)；
C01The mensuration concentration of determinand ion in gas phase blank solution, unit is micrograms per millilitre (μ g/mL)；
M2Determinand content in cigarette side-stream smoke grain phase, unit is microgram every (μ g/ props up)；
C2The mensuration concentration of determinand ion in grain liquid mutually to be measured, unit is micrograms per millilitre (μ g/mL)；
C02The mensuration concentration of determinand ion in grain phase blank solution, unit is micrograms per millilitre (μ g/mL)；
M determinand molecule formula weight, monomethyl amine is 31, and monoethyl amine is 45；
Determinand content in M cigarette side-stream smoke, unit is microgram every (μ g/ props up).
The number of n suction cigarette, unit:.
Experimental result requires that being accurate to 0.1 μ g/ props up.
Have studied with methyl sulfonic acid for flowing phase Gradient elution herein, with the hydrochloric acid solution of 0.01mol/L for absorbing
Liquid, the chromatography of ions quickly measures monomethyl amine and monoethyl amine in cigarette side-stream smoke, and is optimized the method condition
And evaluation.
Condition determination of the present invention is analyzed
1st, the selection of ion chromatographic column
Owing in cigarette smoke, ammonium ion, monomethyl amine ion, monoethyl amine ion interfere with each other, for being kept completely separate three
Open, selected CS12 (4 × 250mm) splitter, CGl2 (4 × 50mm) guard column and CS16 (4 × 250mm) splitter,
Two kinds of chromatographic columns of CGl6 (4 × 50 mm) guard column, it is found that CS16 post separating effect is preferable.
2nd, the selection of methyl sulfonic acid concentrations
Selecting methyl sulfonic acid to elute test substance mutually for flowing, can the concentration of flowing phase outstanding to be kept completely separate determinand
It for key, is that the ammonium ion in cigarette side-stream smoke, monomethyl amine ion and monoethyl amine ion isolation is complete, have selected
10mmol/L, 20 mmol/L, 30 mmol/L methyl sulfonic acid Gradient elutions, as shown in Figure 4, wherein a1Represent a first
Amine ion, b1 represents monoethyl amine ion.As shown in Figure 4, during 10mmol/L methyl sulfonic acid Gradient elution, can by ammonium ion,
Monomethyl amine ion and monoethyl amine ion are kept completely separate.
3rd, the selection of column temperature
Separating degree that column temperature looks for spectral peak to be measured, retention time, post pressure etc. all have an impact, and test column temperature and are respectively 30
DEG C, 40 DEG C, 50 DEG C, 60 DEG C when each determinand separation situation, as it is shown in figure 5, wherein c1 represents monomethyl amine ion, d1 represents one
Ethamine ion, Fig. 5 shows that the separating effect of each determinand when 60 DEG C is best, thus selects column temperature to be 60 DEG C in embodiment.
4th, the selection of flow velocity
Flow rate of mobile phase has influence on the appearance time of ion, separating degree, when flow rate of mobile phase is too high, and interionic separating degree
Being deteriorated, flow rate of mobile phase is too low, and minute is long.The flowing phase of the 0.5th, the 0.8th, the 1.0th, 1.2mL/min by experimental selection
Flow velocity, comprehensive separating degree and the retention time analyzed, the flow velocity of more suitable 1.0 mL/min of present invention selection.
5th, the selection of absorbing liquid concentration
For guaranteeing that monomethyl amine in cigarette side-stream smoke gas gas-phase objects and granule phase substance, monoethyl amine are completely absorbed and extract, examination
Test the hydrochloric acid that have selected the 0.005th, the 0.01st, tri-kinds of variable concentrations of 0.02mol/L as absorbing liquid and extract, added absorbing liquid and
Extract volume is 30mL, knows that 0.01mol/L aqueous hydrochloric acid solution can reach satisfied result from table 1.
The impact on determinand content for the table 1 absorbing liquid concentration
6th, the selection of absorption bottle series connection number
For guaranteeing that monomethyl amine in components in cigarette smoke gas phase thing, monoethyl amine are completely absorbed, 3 difference of connecting after trap
Equipped with the absorption bottle that 30mL concentration is 0.01mol/L aqueous hydrochloric acid solution, gas phase composition is trapped, after aspirating 4 cigarette, will
Solution in three absorption bottles shakes up, and crosses 0.22 m aqueous phase filter membrane and carries out ion chromatography, by analyzing three absorption bottles
Absorption efficiency, it was found that preposition absorption bottle, in put the concentration of monomethylamine in absorption bottle and rearmounted absorption bottle and be respectively the 0.339th,
0.0513rd, 0.0066 μ g/mL, accounting for the ratio of total concentration respectively is the 85.4%th, the 12.9%th, 1.7%；Monoethyl amine in three absorption bottles
The 0.157th, concentration be respectively the 0.0144th, 0 μ g/mL, accounts for the 91.6%th, the 8.4%th, the 0% of total concentration ratio respectively.Data show cigarette side
In stream flue gas, monomethyl amine and the monoethyl amine of more than 98% are all absorbed by the first two absorption bottle, therefore test selects the absorption of two series connection
The gas gas-phase objects of bottle trapping side-stream smoke, each loading 30mL absorbing liquid in absorption bottle.
7th, the selection of mode and extraction time is extracted
Test have selected ultrasonic and two kinds of extraction modes of vibration, as a example by 1# cigarette, after oscillation extraction 50min sample introduction is analyzed
Monomethyl amine, the content of monoethyl amine are respectively that 8.4 μ g/ prop up, 1.6 μ g/ prop up, ultrasonic extraction 50min sample introduction analyze after monomethyl amine, a second
The content of amine is respectively that 9.1 μ g/ prop up, 1.8 μ g/ prop up, and ultrasonic extraction rate is slightly above oscillation extraction.Test selects ultrasonic extraction side
Formula, for optimizing the ultrasonic extraction time, test have selected the 20th, the 30th, the 40th, the 50th, 60min different extraction time when determinand extraction effect
Rate, as shown in Figure 6, wherein "" represent monomethyl amine, "" represent monoethyl amine.It will be appreciated from fig. 6 that when extraction
Between reach 50min after, the determinand content in extract is not changed in substantially, and therefore extraction time is chosen as 50min.
8th, the stability of solution to be measured
Determinand in cigarette smoke is affected by environment and sample substrate itself, with the prolongation of standing time, to be measured
The content of thing is gradually increased, and with a sample liquid to be measured for analyzing object, places 0h, 1h, 2h, 4h, 8h, 12h, 16h, 24h respectively
And 48h, testing result is shown in accompanying drawing 7, wherein "" represent monomethyl amine, "" represent monoethyl amine.Can from Fig. 7
Discovery, in 12h, the measured value of monomethyl amine and monoethyl amine changes all within 5%, and the content of monomethyl amine and monoethyl amine gradually increases afterwards
Adding, after liquid to be measured placement 48h, the content of monomethyl amine and monoethyl amine increases by 10.6% and 14.6% respectively, therefore test requirements document sample palpus
After cigarette smoking completes, 12h completes detection.
9th, standard working curve, detection limit and quantitative limit
The concentration preparing is respectively the 0.02nd, the 0.04th, the 0.08th, the 0.2nd, the 0.4th, the 0.8th, 2.0 g/mL series standard work
Solution carries out ion chromatography, and with target concentration as abscissa, in chromatogram, determinand peak area is as ordinate, carries out
Regression analysis, obtains the linear equation of determinand.Minimum standard specimen solution repeats sample introduction 10 times, calculates the standard deviation of measured value,
Using 3 times of standard deviation scaling results as the detection limit of method, using 10 times of standard deviation scaling results as the quantitative limit of method,
Data see table 2.
The linear equation of table 2 method, coefficient correlation, detection limit and quantitative limit
10th, the rate of recovery and repeatability
Grain phase (filter disc) sample segment recovery of standard addition: respectively by basic, normal, high dense on the glass fiber filter having aspirated
Degree adds the standard liquid of 3 variable concentrations, adds 30mL0.01mol/L hydrochloric acid solution ultrasonic extraction 50min, takes after standing
Carry out ion chromatography after layer clear liquid filter membrane；Gas phase portion sample recovery of standard addition: proceeding to fish tail cover leacheate and suction
Receive in the 200mL volumetric flask of bottle leacheate, add the standard liquid of 3 variable concentrations respectively by basic, normal, high concentration, shake up, molten
Liquid filter membrane, carries out ion chromatography, and recovery test result see table 3.As shown in Table 3, the rate of recovery of monomethyl amine exists
Between 80.7%～102.9%, the rate of recovery of monoethyl amine is between 85.1%～102.1%, and the rate of recovery is preferable, illustrates that the method is accurate
Property is higher.Parallel determination 5 times under identical conditions of same cigarette sample, calculate the relative standard deviation of 5 parallel determinations
(RSD), measurement result see table 3.In table 3, result shows, the precision RSD of monomethyl amine and monoethyl amine is respectively less than 3%, and this is described
Method repeatability is preferably.
The rate of recovery of table 3 method and precision (RSD)
11st, the content of monomethyl amine and monoethyl amine in part cigarette side-stream smoke
Use the inventive method to 10 kinds of cigarettes types, different tar content sample in monomethyl amine and monoethyl amine contain
Amount detects, and the results are shown in Table 4.Result shows: 1. the monomethyl amine in side-stream smoke and monoethyl amine are primarily present in gas phase portion,
Account for about the 70% of total content；2., in 10 samples, in 2 blended type cigarettes, the content of monomethyl amine and monoethyl amine is above it
Yu 8 Virginian-type cigarettes.
Table 4 sample detection result (μ g/ props up)
Claims (1)
1. monomethyl amine, the method for monoethyl amine content in an ion-chromatographic determination cigarette side-stream smoke:
The trapping of monomethyl amine and monoethyl amine in A, side-stream smoke: by cigarette sample 22 DEG C ± 1 DEG C and relative humidity 60% ± 2%
Environment in after balance 48h, select average weight for ± 0.02g/and the cigarette propped up for ± 49Pa/ of average resistance to suction be test
Cigarette, traps the granule phase substance of side-stream smoke with fish tail cover and glass fiber filter, use simultaneously the absorption bottles of two series connection with
The watery hydrochloric acid of the flow velocity 0.01mol/L of 3000mL/min collects absorbing liquid after absorbing the gas gas-phase objects in side-stream smoke successively；
B, blank assay: take identical cigarette, under not lighting state, every carries out corresponding average mouth number suction, obtains laboratory
Room air blank and filter disc blank sample；
C, cigarette smoke sample treatment: a, effluent gas gas-phase objects: trapping is had the fish tail cover inwall 0.01mol/L hydrochloric acid of gas gas-phase objects
In solution drip washing container, then by after in two GAS ABSORPTION bottles, absorbing liquid is transferred to said vesse, respectively with the salt of 0.01mol/L
Cleaning solution is proceeded to said vesse by acid solution wash absorption bottle and side-stream smoke contact portion in the lump, then with salt acid extraction solution
Shaking up after being settled to scale, stirring pipettes supernatant liquor after standing and treats ion chromatography；B, granule phase substance filter disc: aspirated cigarette
After end, take out glass fiber filter, after trap inwall filter disc is cleaned, this filter disc and glass fiber filter are together put
Enter Erlenmeyer flask, add the hydrochloric acid solution of 0.01mol/L, pipette supernatant liquor after ultrasonic extraction 50min, through 0.22 m aqueous phase filter membrane
After filtration, collect filtrate and treat ion chromatography；
The storing solution of D, monomethyl amine and monoethyl amine and the preparation of standard working solution: accurately weigh 0.1g40% mass concentration respectively
Monomethylamine aqueous solution, 0.06g65%～70% mass concentration the monoethyl amine aqueous solution in container, use 0.01mol/L hydrochloric acid solution
It after being settled to scale, is configured to the hybrid standard storing solution of monomethyl amine, monoethyl amine, then standard reserving solution described in stepwise dilution,
After being configured to the series standard working solution that the 0.02nd, concentration be respectively the 0.04th, the 0.08th, the 0.2nd, the 0.4th, the 0.8th, 2.0 g/mL, through from
Sub-chromatography obtains the linear equation coefficient R of monomethyl amine ion and monoethyl amine ion2It is 0.9999；
E, the supernatant liquor by above-mentioned a, b step carry out ion chromatography, chromatography of ions condition: chromatographic column: CS16 divides respectively
From post, CGl6 guard column；Electric conductivity detector, wears peace CSRS ULTRA-II suppressor；Flowing phase: 10mmol/L methyl sulfonic acid,
Gradient elution, elution time is 40min；Flow velocity: 1.0 mL/min；Sample size: 25 L；Column temperature: 60 DEG C；Autosynthesis suppresses
Device electric current: 39mA；
The side-stream smoke grain obtaining after above-mentioned ion chromatography is neutralized mutually the content of monomethyl amine and monoethyl amine in gas phase respectively
Substitute into below equation (1) and formula (2) calculates, then the total amount of monomethyl amine in side-stream smoke and monoethyl amine is substituted into formula (3) i.e.
Can the content of monomethyl amine and monoethyl amine in rapid and accurate determination cigarette side-stream smoke:
In above formula: M1Determinand content in cigarette side-stream smoke gas phase, unit is microgram every (μ g/ props up)；
C1The mensuration concentration of determinand ion in gas phase liquid to be measured, unit is micrograms per millilitre (μ g/mL)；
C01The mensuration concentration of determinand ion in gas phase blank solution, unit is micrograms per millilitre (μ g/mL)；
M2Determinand content in cigarette side-stream smoke grain phase, unit is microgram every (μ g/ props up)；
C2The mensuration concentration of determinand ion in grain liquid mutually to be measured, unit is micrograms per millilitre (μ g/mL)；
C02The mensuration concentration of determinand ion in grain phase blank solution, unit is micrograms per millilitre (μ g/mL)；
M determinand molecule formula weight, monomethyl amine is 31, and monoethyl amine is 45；
Determinand content in M cigarette side-stream smoke, unit is microgram every (μ g/ props up)；
The number of n suction cigarette, unit:.
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| CN114689715B (en) * | 2020-12-29 | 2024-01-16 | 北京海浈医药科技有限公司 | Method for detecting trimethylamine or trimethylamine salt content |
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