CN103616453A - Determination method of ammonia content in cigarette mainstream smoke - Google Patents
Determination method of ammonia content in cigarette mainstream smoke Download PDFInfo
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- CN103616453A CN103616453A CN201310655480.0A CN201310655480A CN103616453A CN 103616453 A CN103616453 A CN 103616453A CN 201310655480 A CN201310655480 A CN 201310655480A CN 103616453 A CN103616453 A CN 103616453A
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Abstract
The invention provides a determination method of ammonia content in cigarette mainstream smoke. According to the determination method provided by the invention, by taking Li+ as an internal standard substance, ion chromatography detection of the ammonia content in the cigarette mainstream smoke is realized. The determination method provided by the invention avoids the interference of the environmental background to an electrical conductivity detector, under different environmental backgrounds, for different cigarette samples, the ammonia content in the cigarette mainstream smoke can be quantitatively obtained by adopting the same standard curve, and detection results have high accuracy and repeatability. Experimental results show that at different environment temperatures, the detection results obtained by the determination method provided by the invention have high repeatability, so that the stability and accuracy of detection are improved.
Description
Technical field
The present invention relates to technical field of cigarettes, relate in particular to a kind of method of measuring ammonia of main stream smoke of cigarette content.
Background technology
Ammonia is the natural component existing with proton form in tobacco, and excess of ammonia can produce strong impulse, makes flue gas coarse, generation is charred taste, and can produce a large amount of objectionable constituent, causes the contraction of smoker throat, make people feel to choke and cough, nasal cavity, tongue have pungent sensation unbearably.Therefore, ammonia plays an important role to controlling cigarette odor-absorbing.
Through long-term experiment, the ammonia content that the chromatography of ions (IC) is measured in cigarette mainstream flue gas is shown one's talent from the methods such as spectrophotometric method, electrochemical process, Capillary Electrophoresis, the advantage such as good with its selectivity, sensitive, quick, easy becomes the method for extensively promoting the use of in industry.But what the ion chromatograph using at present generally used is electric conductivity detector, and this detecting device is subject to extraneous thermal effect larger.The product in early stage of ion chromatograph does not have temperature-controlling system, gradient elution system and automatic sample handling system, has therefore caused the larger fluctuation of detector sensitivity.Thereby cause at every turn production standard curve again, eliminate as far as possible this impact.So both wasted the great many of experiments time, and in experiment, the variation of temperature still can cause the fluctuation of detector sensitivity, affect the repeatability of experimental data and accuracy and repeated.
Summary of the invention
The object of the present invention is to provide a kind of method of measuring ammonia of main stream smoke of cigarette content, the method provided by the invention impact of surperficial environment temperature on testing result effectively, the stability and the accuracy that improve testing result.
The invention provides a kind of method of measuring ammonia of main stream smoke of cigarette content, comprise the following steps:
A) gather the main flume of cigarette sample to be measured, obtain main flume solution;
C) described main flume solution is mixed with internal standard compound, obtain solution to be measured, described internal standard compound comprises Li
+;
D) described solution to be measured is carried out to chromatography of ions detection, obtain the chromatography of ions figure of described solution to be measured;
E), according to the chromatography of ions figure of described solution to be measured and predetermined typical curve, obtain the ammonia content of solution to be measured;
F), according to the quantity of the ammonia content of described solution to be measured and described cigarette to be measured, obtain the ammonia content in cigarette mainstream flue gas.
Preferably, the mass concentration of described internal standard compound in solution to be measured is 0.05 μ g/mL～0.5 μ g/mL.
The flow velocity of the mobile phase that preferably, described chromatography of ions detects is 0.5mL/min～5mL/min.
Preferably, described mobile phase is methanesulfonic acid solution, and the volumetric molar concentration of described methanesulfonic acid solution is 10mmol/L～25mmol/L.
Preferably, the rejector electric current that described chromatography of ions detects is 40mA～55mA.
Preferably, the quantitative ring volume that described chromatography of ions detects is 50 μ L～200 μ L.
Preferably, described step a) is specially:
A1) by cigarette sample to be measured balance in constant-temperature constant-humidity environment;
A2) cigarette sample after described balance is aspirated, adopt the granule phase substance of cambridge filter trapping main flume;
Adopt the gas gas-phase objects in extractant trapping main flume, obtain gas gas-phase objects solution;
A3) absorption there is is the cambridge filter of total particulate matter in mainstream smoke adopt extractant to extract, obtain granule phase substance solution;
A4) described gas gas-phase objects solution and described granule phase substance solution are mixed, obtain main flume solution.
Preferably, described extractant is hydrochloric acid solution.
Preferably, the volumetric molar concentration of described hydrochloric acid solution is 5mmol/L～20mmol/L.
Preferably, the temperature of described constant-temperature constant-humidity environment be 22 ℃ ± (1～5) ℃;
The relative humidity of described constant-temperature constant-humidity environment is 60% ± (1%～5%).
The invention provides a kind of method of measuring ammonia of main stream smoke of cigarette content, comprise the following steps: a) gather the main flume of cigarette sample to be measured, obtain main flume solution; C) described main flume solution is mixed with internal standard compound, obtain solution to be measured, described internal standard compound comprises Li
+; D) described solution to be measured is carried out to chromatography of ions detection, obtain the chromatography of ions figure of described solution to be measured; E), according to the chromatography of ions figure of described solution to be measured and predetermined typical curve, obtain the ammonia content of solution to be measured; F), according to the quantity of the ammonia content of described solution to be measured and described cigarette to be measured, obtain the ammonia content in cigarette mainstream flue gas.Assay method provided by the invention is with Li
+as internal standard compound, realized the chromatography of ions of ammonia of main stream smoke of cigarette content has been detected, method provided by the invention has been avoided the interference of environmental background to electric conductivity detector, under varying environment background, for different cigarette samples, adopt same typical curve just can quantitatively obtain the ammonia content in cigarette mainstream flue gas, and testing result have higher accuracy and repeatability.Experimental result shows, method provided by the invention is under different environment temperatures, and the testing result obtaining has higher repeatability, improved the stability and the accuracy that detect.
Accompanying drawing explanation
Fig. 1 is the standard substance that obtains of the embodiment of the present invention 1 and the chromatography of ions figure of cigarette sample;
Fig. 2 is the chromatography of ions figure of the standard solution of the series concentration that obtains of the embodiment of the present invention 2;
Fig. 3 is the canonical plotting that the embodiment of the present invention 2 obtains;
Fig. 4 is that the standard solution that the embodiment of the present invention 7 obtains is changing the chromatogram contrast quantitatively encircling after solvent.
Embodiment
The invention provides a kind of method of measuring ammonia of main stream smoke of cigarette content, comprise the following steps:
A) gather the main flume of cigarette sample to be measured, obtain main flume solution;
C) described main flume solution is mixed with internal standard compound, obtain solution to be measured, described internal standard compound comprises Li
+;
D) described solution to be measured is carried out to chromatography of ions detection, obtain the chromatography of ions figure of described solution to be measured;
E), according to the chromatography of ions figure of described solution to be measured and predetermined typical curve, obtain the ammonia content of solution to be measured;
F), according to the quantity of the ammonia content of described solution to be measured and described cigarette to be measured, obtain the ammonia content in cigarette mainstream flue gas.
Assay method provided by the invention is with Li
+as internal standard compound, realized the chromatography of ions of ammonia of main stream smoke of cigarette content has been detected, method provided by the invention has been avoided environmental background, especially the interference of environment temperature to electric conductivity detector, under varying environment background, for different cigarette samples, adopt same typical curve just can quantitatively obtain the ammonia content in cigarette mainstream flue gas, and testing result have higher accuracy and repeatability.
The present invention gathers the main flume of cigarette sample to be measured, obtains main flume solution.The present invention does not have special restriction to the method for described collection cigarette sample main flume, adopts the technical scheme of collection cigarette sample main flume well known to those skilled in the art.The present invention preferably adopts following steps, obtains the main flume solution of cigarette sample:
A1) by cigarette sample to be measured balance in constant-temperature constant-humidity environment;
A2) cigarette sample after described balance is aspirated, adopt the granule phase substance of cambridge filter trapping main flume;
Adopt the gas gas-phase objects in extractant trapping main flume, obtain gas gas-phase objects solution;
A3) absorption there is is the cambridge filter of total particulate matter in mainstream smoke adopt extractant to extract, obtain granule phase substance solution;
A4) described gas gas-phase objects solution and described granule phase substance solution are mixed, obtain main flume solution.
The present invention is preferably by cigarette sample to be measured balance in constant-temperature constant-humidity environment, and then carries out the collection of main flume.The present invention does not have special restriction to the generator of described constant-temperature constant-humidity environment, adopts climatic chamber well known to those skilled in the art.In the present invention, the temperature of described constant-temperature constant-humidity environment be preferably 22 ℃ ± (1～5) ℃, more preferably 22 ℃ ± (1～3) ℃, most preferably be 22 ℃ ± 1 ℃; The relative humidity of described constant-temperature constant-humidity environment is preferably 60% ± (1%～5%), and more preferably 60% ± (1%～3%), most preferably is 60% ± 2%.In the present invention, the time of described balance is preferably 40h～60h, and more preferably 42h～55h, most preferably is 45h～50h.The present invention does not have special restriction to the type of described cigarette sample, adopts cigarette type well known to those skilled in the art, as being fire-cured tobacco type, can be mixed type yet.
Complete after the balance of described cigarette sample to be measured, the present invention extracts the cigarette sample to be measured after balance, adopts the granule phase substance in cambridge filter trapping main flume; Adopt the gas gas-phase objects in extractant trapping main flume, obtain gas gas-phase objects solution.The present invention does not have special restriction to the parameter of described extraction, adopts the regulation in GB/T19609 national standard well known to those skilled in the art, and the cigarette sample to be measured after balance is aspirated.In the present invention, in described aspiration procedure, the cigarette quantity of each duct suction is preferably 4～6, and in an embodiment of the present invention, the cigarette quantity of each duct suction can be specially 4,5 or 6.Adopt cambridge filter to trap the granule phase substance in the main flume of suction generation, the cigarette smoke that each filter disc trapping is 4～6.The present invention does not have special restriction to the specifications parameter of described cambridge filter, adopts cambridge filter well known to those skilled in the art, and the present invention preferably adopts the cambridge filter of 44mm to trap the granule phase substance in main flume.
In the process that cigarette sample to be measured is aspirated, the present invention adopts the gas gas-phase objects in extractant trapping main flume, obtains gas gas-phase objects solution.In an embodiment of the present invention, concrete, between each drip catcher and suction engine, the container of extractant is equipped with in access, for trapping the gas gas-phase objects of main flume, obtains gas gas-phase objects solution.In the present invention, described extractant is preferably hydrochloric acid solution; The volumetric molar concentration of described hydrochloric acid solution is preferably 5mmol/L～15mmol/L, 8mmo/L～12mmoil/L more preferably, in an embodiment of the present invention, the volumetric molar concentration of described hydrochloric acid solution can be specially 5mmol/L, 8mmol/L, 10mmo/L, 12mmol/L or 15mmol/L.Those skilled in the art can select according to the quantity of smoking cigarette sample the consumption of suitable extractant, and the present invention does not do special restriction to this.In the present invention, when the quantity of described cigarette sample to be measured is 4～6, the consumption of described extractant is preferably 10mL～30mL, more preferably 15mL～25mL.
Complete after the trapping of described main flume, the present invention has the cambridge filter of total particulate matter in mainstream smoke to adopt extractant to extract absorption, obtains granule phase substance solution.Each cambridge filter that the present invention completes suction is placed in the container that is contained with extractant, and the granule phase substance in extraction cambridge filter, obtains granule phase substance solution.In the present invention, described extractant is preferably the volumetric molar concentration of hydrochloric acid solution described in hydrochloric acid solution and is preferably 5mmol/L～15mmol/L, 8mmo/L～12mmoil/L more preferably, in an embodiment of the present invention, the volumetric molar concentration of described hydrochloric acid solution can be specially 5mmol/L, 8mmol/L, 10mmo/L, 12mmol/L or 15mmol/L.Those skilled in the art can select according to the quantity of smoking cigarette sample the consumption of suitable extractant, and the present invention does not do special restriction to this.In the present invention, when the quantity of described cigarette sample to be measured is 4～6, the consumption of described extractant is preferably 10mL～30mL, more preferably 15mL～25mL.The present invention does not have special restriction to described extraction container, can adopt the tool plug conical flask of 50mL well known to those skilled in the art.
Obtain after gas gas-phase objects solution and granule phase substance solution, the present invention mixes described gas gas-phase objects solution and granule phase substance solution, obtains main flume solution.The present invention does not have special restriction to the method for described mixing, adopts the technical scheme of mixing well known to those skilled in the art.The present invention, in order to be applicable to chromatography of ions detection and the quantitative test to testing result of subsequent step, in an embodiment of the present invention, to pipette respectively the granule phase substance solution of 5mL and the gas gas-phase objects solution of 5mL and mixes, and obtains main flume solution.
Obtain after main flume solution, the present invention mixes described main flume solution with internal standard compound, obtain solution to be measured, and described internal standard compound comprises Li
+.The present invention preferably adds internal standard substance solution in described main flume solution, obtains solution to be measured.In order to realize the quantitative test to measurement result, the present invention preferably adds internal standard substance solution in described main flume solution, after constant volume, obtains solution to be measured.In the present invention, the mass concentration of described internal standard substance solution is preferably 0.1 μ g/mL～3 μ g/mL, more preferably 0.5 μ g/mL～2 μ g/mL.In an embodiment of the present invention, the mass concentration of described internal standard substance solution can be specially 1 μ g/mL.In the present invention, the quantity of described cigarette sample to be measured and the mass ratio of described internal standard compound are preferably (4～6): (0.25 μ g～7.5 μ g), more preferably (4～6): (1.25 μ g～5 μ g).In the present invention, the mass concentration of described internal standard compound in described solution to be measured is preferably 0.05 μ g/mL～0.5 μ g/mL, more preferably 0.1 μ g/mL～0.3 μ g/mL.
Obtain after solution to be measured, the present invention carries out chromatography of ions detection by described solution to be measured, obtains the chromatography of ions figure of described solution to be measured.The present invention preferably crosses described solution to be measured after water filter membrane, then carries out chromatography of ions detection, obtains chromatography of ions figure.In the present invention, the aperture of described water filter membrane is preferably 0.2 μ m～0.6 μ m, more preferably 0.45 μ m.In the present invention, the sample size that described chromatography of ions detects is preferably 0.5mL～2mL, more preferably 1mL.The present invention does not have special restriction to the mode of described sample introduction, the input mode that adopts chromatography of ions well known to those skilled in the art to detect.The present invention is preferably and adopts disposable syringe to extract solution to be measured, between syringe and chromatography of ions injection port, uses water filter membrane to be connected, and filtration is sample introduction afterwards, carries out chromatography of ions detection.
In the present invention, the mobile phase that described chromatography of ions detects is preferably methanesulfonic acid solution, the volumetric molar concentration of described methanesulfonic acid solution is preferably 10mmol/L～25mmol/L, 15mmol/L～20mmol/L more preferably, in an embodiment of the present invention, the volumetric molar concentration of described methane-sulforic acid can be specially 15mmol/L or 16mmol/L.In the present invention, the flow velocity of described mobile phase is preferably 0.5mL/min～5mL/min, 1mL/min～3mL/min more preferably, and in an embodiment of the present invention, the flow velocity of described mobile phase can be specially 1mL/min, 2mL/min or 3mL/min.In the present invention, the inhibition electric current that described chromatography of ions detects is preferably 40mA～55mA, 45mA～50mA more preferably, and in an embodiment of the present invention, described inhibition electric current can be specially 45mA, 48mA or 50mA.In the present invention, the quantitative ring volume that described chromatography of ions detects is preferably 50 μ L～200 μ L, and more preferably 80 μ L～150 μ L, most preferably are 90 μ L～110 μ L, in an embodiment of the present invention, described quantitative ring volume can be specially 90 μ L, 100 μ L or 110 μ L.In the present invention, the chromatographic column that described chromatography of ions detects is preferably CS18 and CG18; The detecting device that described chromatography of ions detects can be specially electric conductivity detector.
Obtain after the chromatography of ions figure of solution to be measured, the present invention, according to the chromatography of ions figure of described solution to be measured and predetermined typical curve, obtains the ammonia content in solution to be measured.In the present invention, described typical curve preferably obtains in accordance with the following methods:
Serial NH4 is provided
+the standard solution of concentration, described standard solution comprises NH4
+and Li
+;
Described standard solution is carried out to chromatography of ions detection, obtain the chromatography of ions figure of standard solution;
According to described standard solution chromatography of ions figure, obtain NH4
+the peak area of chromatographic peak;
According to described NH4
+the concentration of the standard solution that the peak area of chromatographic peak is corresponding with it, obtains typical curve.
The invention provides the standard solution of series concentration, described standard solution comprises NH4
+and Li
+.The mother liquor of preferred disposition standard solution of the present invention, as required, by described mother liquor dilution series multiple, obtains the standard solution of series concentration.In the present invention, NH4 in described standard solution
+mass concentration be preferably 0.1 μ g/mL～1.0 μ g/mL, internal standard compound Li in described standard solution
+mass concentration be preferably 0.05 μ g/mL～0.3 μ g/mL; In an embodiment, NH4 in described standard solution
+mass concentration can be specially 0.1 μ g/mL, 0.3 μ g/mL, 0.5 μ g/mL, 0.7 μ g/mL or 1.0 μ g/mL, the mass concentration of internal standard compound can be specially 0.1 μ g/mL, obtains the standard solution of series concentration.
Obtain after standard solution, the present invention carries out chromatography of ions detection by described standard solution, obtains respectively the chromatography of ions figure of the standard solution of series concentration.The present invention preferably adopts the technical scheme that chromatography of ions detects described in technique scheme to detect the standard solution of described series concentration, does not repeat them here.
Obtain after the chromatography of ions figure of series concentration standard solution, the present invention calculates wherein NH4 according to described chromatography of ions figure
+the peak area of chromatographic peak.The present invention does not have special restriction to the computing method of chromatography of ions peak-to-peak area, adopts the computing method of chromatographic peak well known to those skilled in the art.
Obtain NH4
+after the peak area of chromatographic peak, the present invention is according to described NH4
+the concentration of its corresponding standard solution of peak area of chromatographic peak, obtains typical curve.The present invention is preferably with NH4
+with Li
+mass concentration ratio be horizontal ordinate, with NH4
+chromatographic peak and Li
+the peak area ratio of chromatographic peak is ordinate, and linear fit obtains typical curve.
Obtain after typical curve, the chromatography of ions figure of the solution to be measured that the present invention obtains according to technique scheme and described typical curve, obtain the ammonia content of solution to be measured.The present invention calculates NH4 according to the chromatography of ions figure of the solution to be measured obtaining
+chromatographic peak and Li
+the peak area ratio of chromatographic peak, according to described NH4
+chromatographic peak and Li
+the peak area ratio of chromatographic peak and described typical curve, obtain NH4
+with Li
+mass concentration ratio; According to described NH4
+with Li
+mass concentration ratio and known solution to be measured in Li
+mass concentration, obtain the ammonia content in solution to be measured.
Obtain after the ammonia content in described solution to be measured, the present invention, according to the quantity of the ammonia content of described solution to be measured and described solution to be measured, obtains the ammonia content in cigarette mainstream flue gas.The present invention, according to the ammonia content of described solution to be measured, calculates the quality of ammonia in described solution to be measured, thereby obtains ammonia content total in the main flume of cigarette sample to be measured; According to ammonia content total in described cigarette sample main flume to be measured and the quantity of cigarette sample to be measured, thereby obtain the ammonia content in cigarette mainstream flue gas.
The invention provides a kind of method of measuring ammonia of main stream smoke of cigarette content, comprise the following steps: a) gather the main flume of cigarette sample to be measured, obtain main flume solution; C) described main flume solution is mixed with internal standard compound, obtain solution to be measured, described internal standard compound comprises Li
+; D) described solution to be measured is carried out to chromatography of ions detection, obtain the chromatography of ions figure of described solution to be measured; E), according to the chromatography of ions figure of described solution to be measured and predetermined typical curve, obtain the ammonia content of solution to be measured; F), according to the quantity of the ammonia content of described solution to be measured and described cigarette to be measured, obtain the ammonia content in cigarette mainstream flue gas.Assay method provided by the invention is with Li
+as internal standard compound, realized the chromatography of ions of ammonia of main stream smoke of cigarette content has been detected, method provided by the invention has been avoided the interference of environmental background to electric conductivity detector, under varying environment background, for different cigarette samples, adopt same typical curve just can quantitatively obtain the ammonia content in cigarette mainstream flue gas, and testing result have higher accuracy and repeatability.Experimental result shows, method provided by the invention is under different environment temperatures, and the testing result obtaining has higher repeatability, improved the stability and the accuracy that detect.
In order to further illustrate the present invention, below in conjunction with embodiment, the method for mensuration ammonia of main stream smoke of cigarette content provided by the invention is described in detail, but they can not be interpreted as to limiting the scope of the present invention.
With 1000 μ g/mL NH
4 +standard solution, the hydrochloric acid solution that the volumetric molar concentration of take is 10mmol/L is solvent, is mixed with the NH that concentration is 100 μ g/mL
4 +storing solution;
Pipette the NH that 1mL mass concentration is 100 μ g/mL
4 +storing solution is to 100mL volumetric flask, and constant volume, is mixed with the NH that mass concentration is 1 μ g/mL
4 +solution;
In kind, with 1000 μ g/mL Li
+storing solution is mixed with the Li that mass concentration is 1 μ g/mL
+solution;
Pipette the NH that mass concentration is 1 μ g/mL
4 +solution 1mL, is placed in the volumetric flask that volume is 10mL, then in volumetric flask, adds the Li that 1mL mass concentration is 1 μ g/mL
+solution, constant volume, is mixed with thus and take the Li that interior mark concentration is 0.1 μ g/mL
+, NH
4 +concentration is the standard solution of 0.1 μ g/mL;
By Virginian-type cigarette sample a, in temperature, be balance 48h in 22 ± 1 ℃ and the relative humidity climatic chamber that is 60 ± 2%.According to GB/T19609 regulation, carry out cigarette smoking, adopt 44mm cambridge filter, 4 cigarette smokes of each filter disc trapping, are used for trapping total particulate matter in mainstream smoke; Between each drip catcher and suction engine, the hydrochloric acid solution 20mL that volumetric molar concentration is 10mmol/L is equipped with in access, is used for trapping main flume gas gas-phase objects;
Each filter disc that suction is completed, putting into respectively volume is the tool plug conical flask of 50mL, adding wherein respectively volumetric molar concentration is the hydrochloric acid solution 20mL of 10mmol/L, concussion 40min, extraction grain phase constituent;
From the mutually gentle phase solution of grain, get 5mL respectively, move in the volumetric flask of 25mL, constant volume, obtains the solution to be measured of sample a.
According to cigarette sample b main flume employing method is carried out to main flume collection to Virginian-type cigarette sample b and sample c, a kind of blended type cigarette sample d and a kind of outer odor type cigarette sample e, obtain the solution to be measured of sample b, sample c, sample d and sample e;
Use the disposable syringe 1mL solution to be measured of bleeding, filter 0.45 μ m water filter membrane and inject ion chromatograph, carry out ion chromatography, obtain the chromatography of ions figure of solution to be measured, the condition of ion chromatography is:
Chromatographic column is CS18+CG18; Mobile phase is that volumetric molar concentration is the methanesulfonic acid solution of 16mmol/L; Flow velocity is 1mL/min; Rejector electric current is 48mA; Sample size is 50 μ L; Quantitatively ring is 100 μ L; Detecting device is electric conductivity detector, and environment temperature is room temperature.
Testing result as shown in Figure 1, Fig. 1 is the standard substance that obtains of the embodiment of the present invention 1 and the chromatography of ions figure of cigarette sample, the chromatography of ions curve that wherein curve 1 is standard substance, curve 2 is the chromatography of ions curve of Virginian-type cigarette sample a, curve 3 is the chromatography of ions curve of Virginian-type cigarette sample b, curve 4 is the chromatography of ions curve of Virginian-type cigarette sample c, curve 5 is the chromatography of ions curve of blended type cigarette sample d, curve 6 is the chromatography of ions curve of outer odor type cigarette sample e, as seen from Figure 1, in the main flume of the cigarette of different-style, do not contain Li
+, and Li
+and NH
4 +between also have obvious Na
+, Li
+and NH4
+chromatographic peak between have good degree of separation, therefore, the present invention adopts Li
+as internal standard compound.
Embodiment 2
With 1000 μ g/mL NH
4 +standard solution, the hydrochloric acid solution that the volumetric molar concentration of take is 10mmol/L is solvent, is mixed with the NH that concentration is 100 μ g/mL
4 +storing solution;
Pipette the NH that 1mL mass concentration is 100 μ g/mL
4 +storing solution is to 100mL volumetric flask, and constant volume, is mixed with the NH that mass concentration is 1 μ g/mL
4 +solution;
In kind, with 1000 μ g/mL Li
+storing solution is mixed with the Li that mass concentration is 1 μ g/mL
+solution;
Pipette respectively the NH that mass concentration is 1 μ g/mL
4 +solution 1mL, 3mL, 5mL, 7mL and 9mL, be placed in respectively the volumetric flask that 5 volumes are 10mL, then in each volumetric flask, adds respectively the Li that 1mL mass concentration is 1 μ g/mL
+solution, constant volume, is mixed with thus and take the Li that interior mark concentration is 0.1 μ g/mL
+, NH
4 +concentration is respectively the series concentration standard solution of 0.1 μ g/mL, 0.3 μ g/mL, 0.5 μ g/mL, 0.7 μ g/mL and 0.9 μ g/mL;
The standard solution of described series concentration is carried out respectively to chromatography of ions detection, and chromatographic column is CS18+CG18, mobile phase is that volumetric molar concentration is the methanesulfonic acid solution of 16mmol/L, flow velocity is 1mL/min, rejector electric current is 48mA, sample size is 50 μ L, quantitatively ring is 100 μ L, detecting device is electric conductivity detector, environment temperature is room temperature, obtain the chromatography of ions figure of standard solution, result as shown in Figure 2, Fig. 2 is the chromatography of ions figure of the standard solution of the series concentration that obtains of the embodiment of the present invention 2, wherein curve 1 for mass concentration be the chromatography of ions figure of the standard solution of 0.1 μ g/mL, curve 2 for mass concentration be the chromatography of ions figure of the standard solution of 0.3 μ g/mL, curve 3 for mass concentration be the chromatography of ions figure of the standard solution of 0.5 μ g/mL, curve 4 for mass concentration be the chromatography of ions figure of the standard solution of 0.7 μ g/mL, curve 5 for mass concentration be the chromatography of ions figure of the standard solution of 1.0 μ g/mL.As seen from Figure 2, under the same terms, Li
+and NH
4 +concentration change more consistent
With NH
4 +with Li
+concentration ratio be horizontal ordinate, with NH
4 +with Li
+peak area ratio is ordinate, and linear fit obtains typical curve.
As shown in Figure 3, Fig. 3 is the canonical plotting that the embodiment of the present invention 2 obtains to result, and typical curve related coefficient is 0.9993; 3 times of least concentration standard solution standard deviation of take are method detection limit, and result is 0.0030 μ g/mL.
Embodiment 3
By cigarette sample a, in temperature, be balance 48h in 22 ± 1 ℃ and the relative humidity climatic chamber that is 60 ± 2%, sample a is Virginian-type cigarette sample.According to GB/T19609 regulation, carry out cigarette smoking, adopt 44mm cambridge filter, 4 cigarette smokes of each filter disc trapping, are used for trapping total particulate matter in mainstream smoke; Between each drip catcher and suction engine, the hydrochloric acid solution 20mL that volumetric molar concentration is 10mmol/L is equipped with in access, is used for trapping main flume gas gas-phase objects;
Each filter disc that suction is completed, putting into respectively volume is the tool plug conical flask of 50mL, adding wherein respectively volumetric molar concentration is the hydrochloric acid solution 20mL of 10mmol/L, concussion 40min, extraction grain phase constituent;
From the mutually gentle phase solution of grain, get 5mL respectively, move in the volumetric flask of 25mL, finally adding wherein mass concentration is the Li of 1 μ g/mL
+inner mark solution 2.5mL, constant volume, obtains solution to be measured.
Use the disposable syringe 1mL solution to be measured of bleeding, filter 0.45 μ m water filter membrane and inject ion chromatograph, carry out ion chromatography, obtain the chromatography of ions figure of solution to be measured, the condition of ion chromatography is:
Chromatographic column is CS18+CG18; Mobile phase is that volumetric molar concentration is the methanesulfonic acid solution of 16mmol/L; Flow velocity is 1mL/min; Rejector electric current is 48mA; Sample size is 50 μ L; Quantitatively ring is 100 μ L; Detecting device is electric conductivity detector, and environment temperature is room temperature.
Obtain after the chromatography of ions figure of solution to be measured, the chromatography of ions figure of the solution to be measured that the typical curve obtaining according to embodiment 21 and the present embodiment obtain, calculate the content (unit is μ g/mL) of ammonia in the sample a of the present embodiment, result is as shown in table 2, table 2 for the embodiment of the present invention 2～6 obtain the testing result of ammonia content.
Embodiment 2～6
According to the technical scheme of embodiment 1, respectively the ammonia content in sample b, sample c, sample d and sample e main flume is detected, sample b and sample c are Virginian-type cigarette, sample d is blended type cigarette, sample e is outer odor type cigarette, testing result is as shown in table 2, table 2 for the embodiment of the present invention 2～6 obtain the testing result of ammonia content.
The actual value of ammonia content (unit: μ g/mL) in sample main flume in table 1 embodiment of the present invention 2～6
| Sample | Sample a | Sample b | Sample c | Sample d | Sample e |
| Actual value | 0.1960 | 0.1978 | 0.2649 | 0.3133 | 0.2217 |
Table 2 embodiment of the present invention 2～6 obtain the testing result (unit: μ g/mL) of ammonia content
| Test environment | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Room temperature | 0.1968 | 0.1981 | 0.2648 | 0.3103 | 0.2217 |
| Room temperature | 0.1984 | 0.1965 | 0.2622 | 0.3127 | 0.2216 |
| Room temperature | 0.1970 | 0.1960 | 0.2623 | 0.3131 | 0.2221 |
| Room temperature | 0.1955 | 0.1954 | 0.2651 | 0.3136 | 0.2247 |
| Room temperature | 0.1962 | 0.1991 | 0.2624 | 0.3147 | 0.2232 |
Contrast table 1 and table 2 can be found out, detection for ammonia content in five kinds of samples of a～e, the testing result Data duplication that method provided by the invention at room temperature obtains is fine, compared with prior art, without adopting temperature-controlling system to control, temperature is carried out to accuracy controlling, at room temperature also can greatly strengthen detecting stability and the accuracy of data.
Comparative example 1
With 1000 μ g/mL NH
4 +standard solution, the hydrochloric acid solution that the volumetric molar concentration of take is 10mmol/L is solvent, is mixed with the NH that concentration is 100 μ g/mL
4 +storing solution;
Pipette the NH that 1mL mass concentration is 100 μ g/mL
4 +storing solution is to 100mL volumetric flask, and constant volume, is mixed with the NH that mass concentration is 1 μ g/mL
4 +solution;
Pipette respectively the NH that mass concentration is 1 μ g/mL
4 +solution 1mL, 3mL, 5mL, 7mL and 9mL, be placed in respectively the volumetric flask that 5 volumes are 10mL, and constant volume is mixed with NH thus
4 +concentration is respectively the series concentration standard solution of 0.1 μ g/mL, 0.3 μ g/mL, 0.5 μ g/mL, 0.7 μ g/mL and 0.9 μ g/mL;
The standard solution of described series concentration is carried out respectively to chromatography of ions detection, obtain the chromatography of ions figure of standard solution.
With NH
4 +mass concentration be horizontal ordinate, with NH
4 +chromatography of ions peak area be ordinate, linear fit obtains typical curve.
Comparative example 2
By cigarette sample a, in temperature, be balance 48h in 22 ± 1 ℃ and the relative humidity climatic chamber that is 60 ± 2%, sample a is Virginian-type cigarette sample.According to GB/T19609 regulation, carry out cigarette smoking, adopt 44mm cambridge filter, 4 cigarette smokes of each filter disc trapping, are used for trapping total particulate matter in mainstream smoke; Between each drip catcher and suction engine, the hydrochloric acid solution 20mL that volumetric molar concentration is 10mmol/L is equipped with in access, is used for trapping main flume gas gas-phase objects;
Each filter disc that suction is completed, putting into respectively volume is the tool plug conical flask of 50mL, adding wherein respectively volumetric molar concentration is the hydrochloric acid solution 20mL of 10mmol/L, concussion 40min, extraction grain phase constituent;
From the mutually gentle phase solution of grain, get 5mL respectively, move in the volumetric flask of 25mL, finally adding wherein mass concentration is the Li of 1 μ g/mL
+inner mark solution 2.5mL, constant volume;
Absorption liquid after constant volume is shaken up, use 0.45um water membrane filtration, filtrate is placed in chromatogram bottle, obtains liquid to be measured;
The liquid to be measured obtaining is carried out to chromatography of ions detection, chromatography of ions instrument parameter is set:
Mobile phase is that volumetric molar concentration is the Loprazolam of 0.016mol/L, and rejector electric current is 48mA, and sample size is 50 μ L, and environment temperature is room temperature, detects the chromatography of ions figure that obtains liquid to be measured;
The chromatography of ions figure that the typical curve obtaining according to comparative example 1 and the present embodiment obtain, calculates ammonia content in liquid to be measured, and result is as shown in table 3, the testing result of the ammonia content that table 3 obtains for comparative example 2～6 of the present invention.
Comparative example 2～6
Adopt the technical scheme of comparative example 2 respectively the ammonia content in sample b, sample c, sample d and sample e main flume to be detected, sample b and sample c are Virginian-type cigarette, sample d is blended type cigarette, sample e is outer odor type cigarette, testing result is as shown in table 3, the testing result of the ammonia content that table 3 obtains for comparative example 2～6 of the present invention.
Testing result (the unit: μ g/mL) of the ammonia content that table 3 comparative example 2～6 of the present invention obtains
| Testing environment | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 |
| Room temperature | 0.1868 | 0.1891 | 0.2498 | 0.3103 | 0.2117 |
| Room temperature | 0.2484 | 0.2515 | 0.3322 | 0.4127 | 0.2816 |
| Room temperature | 0.1490 | 0.1530 | 0.2023 | 0.2531 | 0.1721 |
| Room temperature | 0.1825 | 0.1854 | 0.2451 | 0.3036 | 0.2067 |
| Room temperature | 0.1962 | 0.1991 | 0.2624 | 0.3247 | 0.2232 |
Contrast table 1 and table 3 can be found out, for the detection of ammonia content in five kinds of samples of a～e, at room temperature, use the repeatability of prior art detection the data obtained poor, and the accuracy of testing result is lower.
Embodiment 7
According to the scheme described in embodiment 2, prepare the Li that interior mark concentration is 0.1 μ g/mL
+, NH
4 +concentration is the standard solution of 0.1 μ g/mL, and the detection method described in this standard solution employing embodiment 3 is carried out to chromatography of ions detection, and different, in the present embodiment, quantitatively ring solvent is respectively 25 μ L and 100 μ L.
Result as shown in Figure 4, Fig. 4 is that the standard solution that the embodiment of the present invention 7 obtains is changing the chromatogram contrast quantitatively encircling after solvent, wherein curve 1 is the chromatography of ions figure that 25 μ L obtain for quantitatively encircling volume, curve 2 is the chromatography of ions figure that 100 μ L obtain for quantitatively encircling volume, as seen from Figure 4, quantitatively ring volume is that peak shape in the chromatogram that obtains of 100 μ L is better, peak height is larger, therefore, to select quantitative ring volume be that 100 μ L carry out chromatography of ions detection to solution to be measured and standard solution in the present invention.
Embodiment 7
According to the technical scheme of embodiment 3 to Virginian-type cigarette sample a, blended type cigarette sample d and outer odor type cigarette sample e duplicate detection 5 times, recording detection data, calculate respectively standard deviation, result is as shown in table 4, the repeated testing result that table 4 obtains for the embodiment of the present invention 7.
The repeated testing result that table 4 embodiment of the present invention 7 obtains
As can be seen from Table 4, the RSD of method provided by the invention is 1.59～4.42, has good repeatability.
Embodiment 8
Get concentration known sample solution, add respectively 3 kinds of concentration standard solution, according to the technical scheme described in embodiment 3, carry out ion chromatography, record content, calculate recovery rate, result is as shown in table 5, the testing result of the recovery that table 5 obtains for the embodiment of the present invention 8.
The testing result of the recovery that table 5 embodiment of the present invention 8 obtains
| Sample | Add scalar/(ug/ml) | Detected value/(ug/ml) | Recovery/℅ |
| Raw sample | 0 | 0.1439 | ? |
| Mark-on 1 | 0.25 | 0.3848 | 96.3 |
| ? | 0.25 | 0.3926 | 99.5 |
| Mark-on 2 | 0.50 | 0.6189 | 95.0 |
| ? | 0.50 | 0.6528 | 101.8 |
| Mark-on 3 | 0.70 | 0.8812 | 105.3 |
| ? | 0.70 | 0.8647 | 103.0 |
As can be seen from Table 5, method provided by the invention is measured the recovery of cigarette mainstream flue gas between 96.3%～103.0%, and this illustrates that detection method accuracy provided by the invention is higher, can quantitatively detect.
As seen from the above embodiment, the invention provides a kind of method of measuring ammonia of main stream smoke of cigarette content, comprise the following steps: a) gather the main flume of cigarette sample to be measured, obtain main flume solution; C) described main flume solution is mixed with internal standard compound, obtain solution to be measured, described internal standard compound comprises Li
+; D) described solution to be measured is carried out to chromatography of ions detection, obtain the chromatography of ions figure of described solution to be measured; E), according to the chromatography of ions figure of described solution to be measured and predetermined typical curve, obtain the ammonia content of solution to be measured; F), according to the quantity of the ammonia content of described solution to be measured and described cigarette to be measured, obtain the ammonia content in cigarette mainstream flue gas.Assay method provided by the invention is with Li
+as internal standard compound, realized the chromatography of ions of ammonia of main stream smoke of cigarette content has been detected, method provided by the invention has been avoided the interference of environmental background to electric conductivity detector, under varying environment background, for different cigarette samples, adopt same typical curve just can quantitatively obtain the ammonia content in cigarette mainstream flue gas, and testing result have higher accuracy and repeatability.Experimental result shows, method provided by the invention is under different environment temperatures, and the testing result obtaining has higher repeatability, improved the stability and the accuracy that detect.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a method of measuring ammonia of main stream smoke of cigarette content, comprises the following steps:
A) gather the main flume of cigarette sample to be measured, obtain main flume solution;
C) described main flume solution is mixed with internal standard compound, obtain solution to be measured, described internal standard compound comprises Li
+;
D) described solution to be measured is carried out to chromatography of ions detection, obtain the chromatography of ions figure of described solution to be measured;
E), according to the chromatography of ions figure of described solution to be measured and predetermined typical curve, obtain the ammonia content of solution to be measured;
F), according to the quantity of the ammonia content of described solution to be measured and described cigarette to be measured, obtain the ammonia content in cigarette mainstream flue gas.
2. method according to claim 1, is characterized in that, the mass concentration of described internal standard compound in solution to be measured is 0.05 μ g/mL～0.5 μ g/mL.
3. method according to claim 1, is characterized in that, the flow velocity of the mobile phase that described chromatography of ions detects is 0.5mL/min～5mL/min.
4. method according to claim 3, is characterized in that, described mobile phase is methanesulfonic acid solution, and the volumetric molar concentration of described methanesulfonic acid solution is 10mmol/L～25mmol/L.
5. method according to claim 1, is characterized in that, the rejector electric current that described chromatography of ions detects is 40mA～55mA.
6. method according to claim 1, is characterized in that, the quantitative ring volume that described chromatography of ions detects is 50 μ L～200 μ L.
7. method according to claim 1, is characterized in that, described step a) is specially:
A1) by cigarette sample to be measured balance in constant-temperature constant-humidity environment;
A2) cigarette sample after described balance is aspirated, adopt the granule phase substance of cambridge filter trapping main flume;
Adopt the gas gas-phase objects in extractant trapping main flume, obtain gas gas-phase objects solution;
A3) absorption there is is the cambridge filter of total particulate matter in mainstream smoke adopt extractant to extract, obtain granule phase substance solution;
A4) described gas gas-phase objects solution and described granule phase substance solution are mixed, obtain main flume solution.
8. method according to claim 5, is characterized in that, described extractant is hydrochloric acid solution.
9. method according to claim 5, is characterized in that, the volumetric molar concentration of described hydrochloric acid solution is 5mmol/L～15mmol/L.
10. method according to claim 5, is characterized in that, the temperature of described constant-temperature constant-humidity environment is 22 ℃ ± 5 ℃;
The relative humidity of described constant-temperature constant-humidity environment is 60% ± 5%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104820035A (en) * | 2015-05-12 | 2015-08-05 | 川渝中烟工业有限责任公司 | Method for determining ammonia content in cigarette main stream smoke by ion chromatography |
| 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 |
| 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 |
| CN107907617A (en) * | 2017-06-15 | 2018-04-13 | 中国烟草总公司贵州省公司 | It is a kind of to trap the method for phenolic compound and ammonia in cigarette mainstream flue gas at the same time using liquid feeding filter disc is in situ |
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| 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 |
| 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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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102012418A (en) * | 2010-11-04 | 2011-04-13 | 中国烟草总公司郑州烟草研究院 | Method for measuring ammonia of main stream smoke of cigarette |
| CN102841158A (en) * | 2012-09-26 | 2012-12-26 | 贵州省烟草科学研究所 | Method for measuring main stream smoke of cigarettes by using amino acid analyzer |
-
2013
- 2013-12-06 CN CN201310655480.0A patent/CN103616453A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102012418A (en) * | 2010-11-04 | 2011-04-13 | 中国烟草总公司郑州烟草研究院 | Method for measuring ammonia of main stream smoke of cigarette |
| CN102841158A (en) * | 2012-09-26 | 2012-12-26 | 贵州省烟草科学研究所 | Method for measuring main stream smoke of cigarettes by using amino acid analyzer |
Non-Patent Citations (6)
| Title |
|---|
| DIONEX CORPORATION: "《IonPac CS18 and IonPac CG18 Product Manual》", 28 February 2006, article "IonPac CS18 and IonPac CG18 Product Manual" * |
| 中国烟草标准化研究室: "《中华人民共和国国家标准 GB/T 16447-1996》", 1 January 1997, article "烟草和烟草制品 调节和测试的大气环境" * |
| 史中华 等: "成品卷烟抽吸过程中氨的转移", 《轻工科技》, no. 9, 30 September 2013 (2013-09-30) * |
| 国家烟草专卖局: "《中华人民共和国烟草行业标准 YC/T 377-2010 卷烟 主流烟气中氨的测定离子色谱法》", 30 April 2011, article "卷烟 主流烟气中氨的测定离子色谱法" * |
| 王希琴 等: "卷烟主流烟气中氨的捕集及其离子色谱法测定", 《分析测试学报》, vol. 24, no. 6, 30 November 2005 (2005-11-30) * |
| 马雁军 等: "改进的离子色谱法用于卷烟主流烟气中氨的测定", 《中国烟草学报》, vol. 18, no. 4, 31 August 2012 (2012-08-31) * |
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