CN107677721A - A kind of assay method for heating chromium in non-combustion-type tobacco product main flume, nickel, arsenic, selenium, cadmium and lead element - Google Patents
A kind of assay method for heating chromium in non-combustion-type tobacco product main flume, nickel, arsenic, selenium, cadmium and lead element Download PDFInfo
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- CN107677721A CN107677721A CN201710930795.XA CN201710930795A CN107677721A CN 107677721 A CN107677721 A CN 107677721A CN 201710930795 A CN201710930795 A CN 201710930795A CN 107677721 A CN107677721 A CN 107677721A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The present invention provides a kind of assay method for heating chromium in non-combustion-type tobacco product main flume, nickel, arsenic, selenium, cadmium and lead element, comprises the following steps：Tobacco product is aspirated using smoking machine, and the main flume of tobacco product is taken using the trapping of Electrostatic device, the total particulate matter in mainstream smoke in Electrostatic device is extracted with ethanol, then cleans Electrostatic device with aqueous solution of nitric acid, obtain sample solution；Then icp mses detection is carried out.The present invention heats the main flume of non-combustion-type tobacco product using the trapping of smoking machine Electrostatic device, then using chromium, nickel, arsenic, selenium, cadmium and the lead element in ethanol and aqueous solution of nitric acid extraction heating non-combustion-type tobacco product main flume, and be measured with reference to icp mses, the reappearance, the rate of recovery of the inventive method are very excellent.
Description
Technical field
The present invention relates to chemical analysis detection technique field, and non-combustion-type tobacco product main flow is heated more particularly to one kind
Chromium in flue gas, nickel, arsenic, selenium, the assay method of cadmium and lead element.
Background technology
Chromium, nickel, arsenic, selenium, cadmium and lead are common heavy metal elements, in recent years due to its have to the mankind and environment it is larger
Harmfulness, extensive concern and research are obtained.Chromium, nickel, arsenic, selenium, cadmium, lead in tobacco are having in Hoffmann lists
Evil composition.Heating non-combustion-type tobacco product (also known as low temperature cigarette) is a kind of pipe tobacco to be heated by special heating source
The novel tobacco product sucked, it is mainly by tobacco material, acidity regulator, leavening agent, humectant, stabilizer/coagulator, increasing
Thick dose and natural essence mixing composition；Heating source is divided into " electric heating type ", " fuel hot type " and " physical and chemical reaction hot type ".
When sucking heating non-combustion-type tobacco product, nicotine and fragrance matter volatilization in tobacco product produce flue gas, pass through people
Body oral cavity enters human lung, consumer is obtained the similar satisfaction for sucking traditional cigarette, but heavy metal member therein simultaneously
Element be able to may also be absorbed by the body, so as to do harm to huamn body.Therefore, in order to comprehensively, objectively carry out heating non-combustion-type
The quality and safety appraisal of tobacco product product, it would be desirable to chromium, nickel, arsenic, selenium, cadmium and lead element in its main flume
Content carry out deep analysis and research.
At present, correlative study work both domestic and external is also concentrated mainly on the analysis of traditional cigarette flue gas heavy metal content with cuing open
Analysis.Domestic tobacco business standard YC/T 379-2010《The measure inductance coupling of chromium, nickel, arsenic, selenium, cadmium, lead in cigarette mainstream flue gas
Close ICP-MS》Define the assay method of chromium, nickel, arsenic, selenium, cadmium, lead content in traditional cigarette main flume.Heating
Non-combustion-type tobacco product is complete as a kind of novel tobacco product, its tobacco material procedure and heating source and traditional cigarette
Difference, and the pipe tobacco when aspirating interval is in non-burning state, side-stream smoke and environment flue gas are also greatly lowered, therefore its cigarette
Main component and traditional cigarette difference in gas is more obvious, and the pre-treating method in YC/T 379-2010 will can not add
Chromium, nickel, arsenic, selenium, cadmium, lead element in hot non-combustion-type tobacco product main flume extract completely, so it can not be fitted
For heating the detection of chromium, nickel, arsenic, selenium, cadmium, lead element content in non-combustion-type tobacco product main flume.And in Novel tobacco
In terms of straw-made articles, research work few in number is also concentrated mainly on the content analysis of heavy metal element in electronic cigarette flue gas.According to
Report, Monique Williams et al. are ground with ICP-OES methods to 22 kinds of constituent contents in certain brand electronic cigarette flue gas
Study carefully；The apparatus and method that Tian Yongfeng et al. has invented heavy metal in a kind of on-line analysis electronic cigarette smog, but on heating
The research of content of beary metal is but rarely reported in non-combustion-type tobacco product main flume.Therefore, one kind is established accurately and reliably
Heat non-combustion-type tobacco product main flume in chromium, nickel, arsenic, selenium, cadmium, lead element detection method of content for tobacco business and
Speech has important practical significance.
The content of the invention
In view of the above the shortcomings that prior art, it is an object of the invention to provide one kind to heat non-combustion-type tobacco system
Chromium in product main flume, nickel, arsenic, selenium, the assay method of cadmium and lead element, the assay method is with inductivity coupled plasma mass spectrometry
Instrument heats chromium, nickel, arsenic, selenium, cadmium and lead element content in non-combustion-type tobacco product main flume as determining instrument, measure,
So that tobacco business person skilled is to chromium, nickel, arsenic, selenium, cadmium and lead member in heating non-combustion-type tobacco product main flume
Cellulose content carries out quantitative determination control, and the quality and safety evaluation work of non-combustion-type tobacco product is heated for tobacco business
Make to provide strong technical support.
In order to achieve the above objects and other related objects, the present invention provides a kind of heating non-combustion-type tobacco product mainstream smoke
Chromium in gas, nickel, arsenic, selenium, the assay method of cadmium and lead element, comprise the following steps：
1) sample pre-treatments：The tobacco product is aspirated using smoking machine, and using the trapping of Electrostatic device
The main flume of the tobacco product is taken, the total particulate matter in mainstream smoke in Electrostatic device, Ran Houyong are extracted with organic solvent
Aqueous solution of nitric acid cleans Electrostatic device, retransfers, constant volume, produces sample solution；
2) preparation of standard liquid：Prepare germanium72, indium115, bismuth209Internal standard standard liquid and chromium, nickel, arsenic, selenium, cadmium, lead element
Working Standard Solution；
3) determine：The internal standard standard liquid and Working Standard Solution for respectively preparing sample solution in step 1), step 2)
Icp mses detection is carried out, is quantified using internal standard synchronization criterion curve method, is obtained in sample solution
Chromium, nickel, arsenic, selenium, cadmium, the content of lead element.
It is preferred that the sample pre-treatments also need to carry out blank assay.
Preferably, the blank assay is not place tobacco product, extracted using organic solvent, aqueous solution of nitric acid several times
After cleaning Electrostatic pipe, retransfer, constant volume, produce blank solution.
Preferably, in step 1), the sparking mode of the smoking machine Electrostatic device is manual ignition.
Preferably, in step 1), the pumping volume of the smoking machine is 35.0 ± 0.3mL, to tobacco system every described
Product aspirate 14-16 mouths, and every mouthful of time aspirated to the tobacco product is 2-4s, and tobacco product every described is taken out
Inhale bell-like puffing profile.
Preferably, the Electrostatic device contains one or more Electrostatic pipe, the every Electrostatic Guan Jun
Collect the main flume of 4-6 branch tobacco products.
Preferably, in step 1), the solid-to-liquid ratio of the tobacco product and the organic solvent is (0.6-5.4) g/
(0.8-1.2)ml。
Preferably, the organic solvent in ethanol, methanol and acetone any one or more.
It is highly preferred that the organic solvent is ethanol.It is because ethanol is nontoxic from ethanol, does not pollute the environment,
Experimenter's health is not influenceed, is on the other hand that ethanol cost is relatively low and be easy to get.
Preferably, in step 1), the concentration of volume percent of the aqueous solution of nitric acid is 0.5-2%.
Preferably, in step 2), the preparation of the Working Standard Solution, comprise the following steps：
A chromium, nickel, arsenic, selenium, cadmium, lead element) are pipetted respectively, with aqueous solution of nitric acid dilution and constant volume, prepare chromium, nickel, arsenic,
Selenium, cadmium, lead element Standard Stock solutions.
It is preferred that the chromium, nickel, arsenic, selenium, cadmium, lead element Standard Stock solutions be chromium, nickel, arsenic, selenium, cadmium, lead mixing or
Single-element Standard Stock solutions.
Preferably, the mass concentration of the chromium, nickel, arsenic, selenium, cadmium, lead mixing or single-element Standard Stock solutions is
100-10000μg/L。
It is highly preferred that the mass concentration of the mixing of the chromium, nickel, arsenic, selenium, cadmium, lead or single-element Standard Stock solutions is equal
For 1000 μ g/L.
Preferably, the condition of storage of the chromium, nickel, arsenic, selenium, cadmium, lead mixing or single-element Standard Stock solutions is：Storage
Deposit temperature：0-4℃；Storage time：1 month.
B chromium, nickel, arsenic, selenium, cadmium, the lead element Standard Stock solutions in the step A of different volumes) are pipetted respectively, use nitric acid
Aqueous solution constant volume is formulated as chromium, nickel, arsenic, selenium, cadmium, the lead element Working Standard Solution of a series of various concentrations.
It is preferred that the chromium, nickel, arsenic, selenium, cadmium, lead element standard liquid are chromium, nickel, arsenic, selenium, cadmium, lead mixing or single
Element Working Standard Solution.
It is preferred that the concentration of volume percent of the aqueous solution of nitric acid is 1-10%.
Preferably, the concentration of volume percent of the aqueous solution of nitric acid is 1%.
The Working Standard Solution should cover sample concentration scope, can be i.e. with i.e. use.
Preferably, in step 2), the preparation of the internal standard standard liquid comprises the following steps：Germanium is weighed respectively72、
Indium115, bismuth209Standard substance solution, with aqueous solution of nitric acid dilution and constant volume, prepare germanium72, indium115, bismuth209Internal standard standard liquid.
It is preferred that the germanium72, indium115, bismuth209Inner mark solution is germanium72, indium115, bismuth209Mixing or single-element internal standard mark
Quasi- solution.
Preferably, the germanium72, indium115, bismuth209The concentration of mixing or single-element internal standard standard liquid is 50-10000 μ
g/L。
It is highly preferred that the germanium72, indium115, bismuth209The concentration of mixing or single-element internal standard standard liquid is 1000 μ g/
L。
Preferably, the germanium72, indium115, bismuth209Mix or the condition of storage of single-element internal standard standard liquid is：Storage temperature
Degree：0-4℃；Storage time：1 month.
Preferably, in step 3), the internal standard synchronization criterion curve method comprises the following steps：
A) respectively by germanium 72 in chromium, nickel, arsenic, selenium, cadmium, lead element Working Standard Solution, step 2) in step 2), indium 115,
The internal standard standard liquid of bismuth 209 synchronously carries out icp mses detection, obtains respective element/corresponding internal standard element
Mass-to-charge ratio intensity than the linear relationship of the mass concentration ratio to respective element/corresponding internal standard element, draw corresponding standard work
Make curve, the regression equation of respective element standard working curve is calculated；
B) internal standard standard liquid in sample solution, step 2) in step 1) is synchronously subjected to inductivity coupled plasma mass spectrometry
Instrument detects, and by the mass-to-charge ratio intensity ratio of the respective element of acquisition/corresponding internal standard element, substitutes into respective element mark in step a) respectively
The regression equation of quasi- working curve, and according to the known quality concentration of the corresponding internal standard standard liquid synchronously detected, be calculated
The mass concentration of respective element in sample solution.
Preferably, the respective element and the corresponding relation of corresponding internal standard element are：Chromium corresponds to germanium72Internal standard element；
Nickel element corresponds to germanium72Internal standard element；Arsenic element corresponds to germanium72Internal standard element；Selenium element corresponds to germanium72Internal standard element；Cadmium element is corresponding
Indium115Internal standard element；Lead element corresponds to bismuth209Internal standard element.
Preferably, in step 3), the icp mses are ends of the earth bar collision/reaction tank-inductance
Couple plasma mass spectrometer.
Preferably, the testing conditions of the icp mses are：Ion gun：ICP source；Radio-frequency power：
1500-1600W；RF matching voltages：1.7-1.9V；Cool down gas：Argon gas, flow velocity：14.0-16.0L/min；Non-user is set；Carry
Gas：Argon gas, flow velocity：0.80-0.90L/min；Carrier gas compensates gas：Argon gas, flow velocity：0.2-0.4L/min；Collision/reaction tank gas
Body：Helium, flow velocity：4.0-4.5mL/min；It is atomized room temperature：1.0-3.0℃；Atomization gas：Argon gas, flow velocity：1.10-1.20L/
min；Ends of the earth bar deflection voltage：- 19.0 to -17.0V；Energy is discriminated against：2.5-3.5V；Sample feeding speed：0.05-0.15rps；
Number of repetition：2-5；Scan mode：Order jumps peak.
It is highly preferred that the testing conditions of the icp mses are：Ion gun：ICP source；Radio frequency work(
Rate：1550W；RF matching voltages：1.8V；Cool down gas：Argon gas, flow velocity：15.0L/min；Non-user is set；Carrier gas：Argon gas, stream
Speed：0.85L/min；Carrier gas compensates gas：Argon gas, flow velocity：0.3L/min；Collision/reaction tank gas：Helium, flow velocity：4.5mL/
min；It is atomized room temperature：2.0℃；Atomization gas：Argon gas, flow velocity：1.15L/min；Ends of the earth bar deflection voltage：-18.0V；Energy discrimination
Depending on：3.0V；Sample feeding speed：0.1rps；Number of repetition：3；Scan mode：Order jumps peak.
As described above, the present invention provide chromium in a kind of heating non-combustion-type tobacco product main flume, nickel, arsenic, selenium, cadmium and
The assay method of lead element, has the advantages that：
Then the present invention is made using the main flume of smoking machine Electrostatic device trapping heating non-combustion-type tobacco product
Chromium, nickel, arsenic, selenium, cadmium and the lead element in non-combustion-type tobacco product main flume are heated with ethanol and aqueous solution of nitric acid extraction,
And be measured with reference to icp mses, establish chromium in heating non-combustion-type tobacco product main flume,
Nickel, arsenic, selenium, cadmium and lead element content assaying method, the reappearance, the rate of recovery of the inventive method are satisfactory, can be effective
Determined in the quantitative analysis for heating chromium in non-combustion-type tobacco product main flume, nickel, arsenic, selenium, cadmium and lead element.
Brief description of the drawings
Fig. 1 is shown as heating chromium, nickel, arsenic, selenium, cadmium and lead element in non-combustion-type tobacco product main flume in the present invention
Assay method schematic flow sheet.
Embodiment
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
The reagent and instrument that following examples use are as follows：
1st, reagent：65% concentrated nitric acid (top pure grade, German Merck companies)；(analysis is pure, Shanghai Ling Feng chemistry for absolute ethyl alcohol
Reagent Co., Ltd)；Chromium, nickel, arsenic, selenium, cadmium, lead element mixed standard solution (Agilent Science and Technology Ltd.s of the U.S.)；Germanium
72nd, indium 115, the element internal standard standard liquid of bismuth 209 (Agilent Science and Technology Ltd.s of the U.S.).
2nd, instrument：7700X icp mses (Agilent Science and Technology Ltd.s of the U.S.)；RM20H rotating disks
Formula smoking machine (German Borgwaldt companies)；Milli-Q ultra-pure waters instrument (Millipore companies of the U.S.).
Embodiment 1
1.1 sample pre-treatments
A, flue gas is trapped：Heating non-combustion-type tobacco product is pumped in the temperature and relative humidity difference of experiment test environment
To be carried out under conditions of (22.0 ± 2.0) DEG C and (60.0 ± 5.0) %.Manual ignition, pumping volume is set as (35.0 ± 0.3)
ML, bell-like puffing profile are carried out, and 15 mouthfuls are aspirated to every tobacco product to ensure complete tobacco product of suction, every mouthful of suction
Time is 3s, and every Electrostatic pipe collects the mainstream smoke total particulate matter of 5 identical heating non-combustion-type tobacco products, often
The weight of Zhi Jiare non-combustion-type tobacco products is 0.45g.
B, solvent extraction：After suction, the total particulate matter in mainstream smoke in Electrostatic pipe is extracted with 5ml ethanol, then use
1% (v/v) nitric acid cleans Electrostatic pipe several times.
C, constant volume is shifted：Extract and cleaning fluid are transferred in 50mL polypropylene volumetric flasks in the lump, using volume basis
The aqueous solution constant volume of the nitric acid of specific concentration 1%, obtain testing sample solution after shaking up.
Blank assay should be done simultaneously, is specially：Do not place tobacco product, extracted using ethanol, aqueous solution of nitric acid several times
After cleaning Electrostatic pipe, retransfer, constant volume, produce blank solution.
The preparation of 1.2 standard liquids
A, chromium, nickel, arsenic, selenium, cadmium, lead element standard substance solution are pipetted respectively, with the nitre that concentration of volume percent is 1%
Aqueous acid dilution and constant volume, prepare chromium, nickel, arsenic, selenium, cadmium, the single-element Standard Stock solutions of lead respectively.Or pipette
Chromium, nickel, arsenic, selenium, cadmium, lead element hybrid standard substance solution, with the aqueous solution of nitric acid dilution that concentration of volume percent is 1% simultaneously
Constant volume, prepare chromium, nickel, arsenic, selenium, cadmium, the complex element Standard Stock solutions of lead.The chromium, nickel, arsenic, selenium, cadmium, lead mixing or
The mass concentration of single-element Standard Stock solutions is 100-10000 μ g/L, it is preferable that the chromium, nickel, arsenic, selenium, cadmium, lead
The mass concentration of mixing or single-element Standard Stock solutions is 1000.0ug/L.Condition of storage can store under the conditions of 0-4 DEG C
1 month.
B, chromium, nickel, arsenic, selenium, cadmium, the single-element Standard Stock solutions of lead of different volumes are pipetted respectively, with volume hundred
Divide the aqueous solution of nitric acid dilution that specific concentration is 1% and constant volume, preparation chromium, nickel, arsenic, selenium, cadmium, lead mix or single-element work mark
Quasi- solution.Or chromium, nickel, arsenic, selenium, cadmium, the complex element Standard Stock solutions of lead of different volumes are pipetted, use volume basis
The aqueous solution of nitric acid dilution and constant volume, preparation chromium, nickel, arsenic, selenium, cadmium, the complex element working stamndard of lead that specific concentration is 1% are molten
Liquid.The Working Standard Solution should cover sample concentration scope, can be i.e. with i.e. use.Specific concentration range is shown in Table 1.
C, germanium is pipetted respectively72, indium115, bismuth209Standard substance solution, with the aqueous solution of nitric acid that concentration of volume percent is 1%
Simultaneously constant volume is diluted, prepares germanium respectively72, indium115, bismuth209Single-element internal standard standard liquid.Or pipette germanium72, indium115、
Bismuth209Hybrid standard substance solution, with the aqueous solution of nitric acid dilution and constant volume that concentration of volume percent is 1%, prepare germanium72、
Indium115, bismuth209Complex element internal standard standard liquid.The germanium72, indium115, bismuth209Mixing or single-element internal standard standard liquid
Concentration is 100-10000 μ g/L.Condition of storage can store 1 month under the conditions of 0-4 DEG C.
The Working Standard Solution of table 1 is with tabulation (unit：ug/L)
The detection of 1.3 samples
Sample solution, 1.2 Working Standard Solutions prepared and internal standard standard liquid in 1.1 are subjected to inductive etc. respectively
Gas ions mass spectrograph (ICP-MS) detect, quantify using internal standard synchronization criterion curve method, acquisition sample solution in chromium, nickel,
Arsenic, selenium, cadmium, the content of lead element.
Specifically, first by a series of chromium of various concentrations in 1.2, nickel, arsenic, selenium, cadmium, lead element Working Standard Solution,
Germanium72, indium115, bismuth209Element inner mark solution synchronously carries out ICP-MS detections, obtains the mass-to-charge ratio of respective element/corresponding internal standard element
Intensity than the mass concentration ratio to respective element/corresponding internal standard element linear relationship, with respective element/corresponding internal standard element
Mass-to-charge ratio intensity ratio is ordinate (Y-axis), and the mass concentration ratio of its corresponding respective element/corresponding internal standard element is abscissa
(X-axis) draws corresponding standard working curve, and the regression equation of respective element standard working curve is calculated.Working stamndard is bent
Line linearly dependent coefficient R2>0.999。
Element determination parameter is set by table 2.Specifically, the respective element and the corresponding relation of corresponding internal standard element
For：Chromium corresponds to germanium72Internal standard element；Nickel element corresponds to germanium72Internal standard element；Arsenic element corresponds to germanium72Internal standard element；Selenium element
Corresponding germanium72Internal standard element；Cadmium element corresponds to indium115Internal standard element；Lead element corresponds to bismuth209Internal standard element.
Internal standard standard liquid in sample solution in 1.1 and its blank solution, 1.2 is synchronously subjected to ICP-MS detections again, will
The mass-to-charge ratio intensity ratio of the respective element of acquisition/corresponding internal standard element, substitutes into the recurrence of respective element standard working curve respectively
Equation, and according to the known quality concentration of the corresponding inner mark solution synchronously detected, respective element in sample solution is calculated
Mass concentration, that is, obtain chromium, nickel, arsenic, selenium, cadmium, the content of lead element in sample solution.
The respective element quality measurement number of table 2, internal standard element
Wherein, the icp mses (ICP-MS) are ends of the earth bar collision/reaction tank-inductive etc.
Gas ions mass spectrograph (ORS-ICP-MS).
The testing conditions of the ORS-ICP-MS are：Ion gun：ICP source；Radio-frequency power：1550W；RF matching voltages：
1.8V；Cool down gas：Argon gas, flow velocity：15.0L/min；Non-user is set；Carrier gas：Argon gas, flow velocity：0.85L/min；Carrier gas compensates
Gas：Argon gas, flow velocity：0.3L/min；Collision/reaction tank gas：Helium, flow velocity：4.5mL/min；It is atomized room temperature：2.0℃；Mist
Change gas：Argon gas, flow velocity：1.15L/min；Ends of the earth bar deflection voltage：-18.0V；Energy is discriminated against：3.0V；Sample feeding speed：
0.1rps；Number of repetition：3；Scan mode：Order jumps peak.
Embodiment 2
As a result with discussion
1st, standard working curve, detection limit and quantitative limit
Marked by a series of complex element work of in embodiment 1 1.2 chromium, nickel, arsenic, selenium, cadmium, lead for being formulated as various concentrations
Quasi- solution, specific concentration range are shown in Table 1.Meanwhile prepare germanium by embodiment 1 1.272, indium115, bismuth209Complex element internal standard standard
Solution.
By a series of Working Standard Solution of the above-mentioned various concentrations prepared and internal standard standard liquid respectively by embodiment 1
In 1.3 regulation, synchronous to carry out ORS-ICP-MS detections, the mass-to-charge ratio intensity ratio using respective element/corresponding internal standard element is vertical
Coordinate (Y-axis), the mass concentration ratio of its corresponding respective element/corresponding internal standard element is abscissa (X-axis), return and divides
Analysis, obtains regression equation and its coefficient correlation, as shown in table 3.
As shown in Table 3, the linear relationship of regression equation is good, coefficient R2>0.999.To the target in standard liquid
Thing response signal, sample introduction is repeated 10 times using least concentration standard specimen, carries out ORS-ICP-MS analyses, using its 3 times of standard deviations as inspection
Rising limit (LOD), 10 times of standard deviations are quantitative limit (LOQ), be scaled after sample size draw object detection be limited to 0.065~
0.301ng/cig, quantitative limit have higher sensitivity in 0.217~1.003ng/cig.
The working curve and detection limit of the present invention of table 3
2nd, repeatability and recovery of standard addition
The chromium of addition concentration known, nickel, arsenic, selenium, cadmium, lead element working stamndard in the sample solution of concentration known respectively
Solution, by testing conditions in embodiment 1, carry out sample pre-treatments and analyzed with ORS-ICP-MS, and according to adding scalar sum measured value
Its rate of recovery is calculated, while to the parallel determination of same sample solution 6 times (n=6), obtains precision determination data, the results are shown in Table.
As can be seen from Table 4, between 91.3~112.1%, relative standard deviation (RSD) is less than the average recovery rate of object
8.7%, illustrate that the rate of recovery of the inventive method and repeatability are satisfactory, be entirely capable of meeting detection needs.
The repeatability and the rate of recovery of the present invention of table 4
Embodiment 3
Using the testing conditions of embodiment in the inventive method 1, to two kinds of different heating non-combustion-type tobacco systems of reality
Chromium, nickel, arsenic, selenium, cadmium, the content of lead element are measured in the main flume of product, are specifically shown in Table 5.As shown in Table 5, for adding
Hot non-combustion-type tobacco product, this method can effectively determine the content of its chromium, nickel, arsenic, selenium, cadmium, lead element, method operation letter
Just, applicability is good, as a result accurately, reliably.
Actual sample testing result (the unit of table 5：ng/cig)
In summary, the present invention heats the mainstream smoke of non-combustion-type tobacco product using the trapping of smoking machine Electrostatic device
Gas, then using the chromium in ethanol and aqueous solution of nitric acid extraction heating non-combustion-type tobacco product main flume, nickel, arsenic, selenium, cadmium
And lead element, and be measured with reference to icp mses, establish heating non-combustion-type tobacco product main flow
Chromium, nickel, arsenic, selenium, cadmium and lead element content assaying method in flue gas, the reappearance, the rate of recovery of the inventive method are satisfactory,
It can be effectively used for heating the quantitative analysis measure of chromium in non-combustion-type tobacco product main flume, nickel, arsenic, selenium, cadmium and lead element.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of assay method for heating chromium in non-combustion-type tobacco product main flume, nickel, arsenic, selenium, cadmium and lead element, it is special
Sign is, comprises the following steps：
1) sample pre-treatments：Tobacco product is aspirated using smoking machine, and the cigarette is taken using the trapping of Electrostatic device
The main flume of straw-made articles, the total particulate matter in mainstream smoke in Electrostatic device is extracted with organic solvent, it is then water-soluble with nitric acid
Liquid cleans Electrostatic device, retransfers, constant volume, produces sample solution；
2) preparation of standard liquid：Prepare germanium72, indium115, bismuth209Internal standard standard liquid and chromium, nickel, arsenic, selenium, cadmium, the work of lead element
Make standard liquid；
3) determine：Sample solution, step 2) are prepared in step 1) internal standard standard liquid and Working Standard Solution are carried out respectively
Icp mses detect, quantify using internal standard synchronization criterion curve method, acquisition sample solution in chromium,
Nickel, arsenic, selenium, cadmium, the content of lead element.
2. chromium, nickel, arsenic, selenium, cadmium and lead element in heating non-combustion-type tobacco product main flume according to claim 1
Assay method, it is characterised in that in step 1), the sparking mode of the smoking machine is manual ignition.
3. chromium, nickel, arsenic, selenium, cadmium and lead element in heating non-combustion-type tobacco product main flume according to claim 1
Assay method, it is characterised in that in step 1), the pumping volume of the smoking machine is 35.0 ± 0.3mL, to described in every
Tobacco product aspirates 14-16 mouths, and every mouthful of time aspirated to the tobacco product is 2-4s, to tobacco product every described
Aspirated bell-like puffing profile；
And/or the Electrostatic device contains one or more Electrostatic pipe, the every Electrostatic pipe collects 4-
The main flume of 6 tobacco products.
4. chromium, nickel, arsenic, selenium, cadmium and lead element in heating non-combustion-type tobacco product main flume according to claim 1
Assay method, it is characterised in that in step 1), the solid-to-liquid ratio of the tobacco product and the organic solvent is (0.6-
5.4)g/(0.8-1.2)ml；
And/or in step 1), any one or more of the organic solvent in ethanol, methanol and acetone；
And/or in step 1), the concentration of volume percent of the aqueous solution of nitric acid is 0.5-2%.
5. chromium, nickel, arsenic, selenium, cadmium and lead element in heating non-combustion-type tobacco product main flume according to claim 1
Assay method, it is characterised in that in step 2), the preparation of the Working Standard Solution, comprise the following steps：
A chromium, nickel, arsenic, selenium, cadmium, lead element) are pipetted respectively, with aqueous solution of nitric acid dilution and constant volume, prepare chromium, nickel, arsenic, selenium,
Cadmium, lead element Standard Stock solutions；
B chromium, nickel, arsenic, selenium, cadmium, the lead element Standard Stock solutions in the step A of different volumes) are pipetted respectively, it is water-soluble with nitric acid
Liquid constant volume is formulated as chromium, nickel, arsenic, selenium, cadmium, the lead element standard liquid of a series of various concentrations.
6. chromium, nickel, arsenic, selenium, cadmium and lead element in heating non-combustion-type tobacco product main flume according to claim 1
Assay method, it is characterised in that in step 2), the preparation of the internal standard standard liquid comprises the following steps：Weigh respectively
Germanium72, indium115, bismuth209Standard substance solution, with aqueous solution of nitric acid dilution and constant volume, prepare germanium72, indium115, bismuth209Internal standard standard is molten
Liquid.
7. chromium, nickel, arsenic, selenium, cadmium and lead element in heating non-combustion-type tobacco product main flume according to claim 1
Assay method, it is characterised in that in step 3), the internal standard synchronization criterion curve method comprises the following steps：
A) respectively by germanium in chromium, nickel, arsenic, selenium, cadmium, lead element Working Standard Solution, step 2) in step 2)72, indium115, bismuth209It is interior
Mark standard liquid and synchronously carry out icp mses detection, obtain the matter lotus of respective element/corresponding internal standard element
Specific strength draws corresponding standard working curve than the linear relationship of the mass concentration ratio to respective element/corresponding internal standard element,
The regression equation of respective element standard working curve is calculated；
B) internal standard standard liquid in sample solution, step 2) in step 1) is synchronously subjected to icp mses inspection
Survey, by the mass-to-charge ratio intensity ratio of the respective element of acquisition/corresponding internal standard element, substitute into respective element standard work in step a) respectively
Make the regression equation of curve, and according to the known quality concentration of the corresponding internal standard standard liquid synchronously detected, sample is calculated
The mass concentration of respective element in solution.
8. chromium, nickel, arsenic, selenium, cadmium and lead element in heating non-combustion-type tobacco product main flume according to claim 7
Assay method, it is characterised in that the respective element and the corresponding relation of corresponding internal standard element are：Chromium corresponds to germanium72It is interior
Mark element；Nickel element corresponds to germanium72Internal standard element；Arsenic element corresponds to germanium72Internal standard element；Selenium element corresponds to germanium72Internal standard element；Cadmium
Element corresponds to indium115Internal standard element；Lead element corresponds to bismuth209Internal standard element.
9. chromium, nickel, arsenic, selenium, cadmium and lead element in heating non-combustion-type tobacco product main flume according to claim 1
Assay method, it is characterised in that in step 3), the icp mses are ends of the earth bar collision/reaction
Pond-icp mses.
10. chromium, nickel, arsenic, selenium, cadmium and lead member in heating non-combustion-type tobacco product main flume according to claim 1
The assay method of element, it is characterised in that the testing conditions of the icp mses are：Ion gun：ICP source；
Radio-frequency power：1500-1600W；RF matching voltages：1.7-1.9V；Cool down gas：Argon gas, flow velocity：14.0-16.0L/min；Non- use
Family is set；Carrier gas：Argon gas, flow velocity：0.80-0.90L/min；Carrier gas compensates gas：Argon gas, flow velocity：0.2-0.4L/min；Collision/
Reaction tank gas：Helium, flow velocity：4.0-4.5mL/min；It is atomized room temperature：1.0-3.0℃；Atomization gas：Argon gas, flow velocity：
1.10-1.20L/min；Ends of the earth bar deflection voltage：- 19.0 to -17.0V；Energy is discriminated against：2.5-3.5V；Sample feeding speed：
0.05-0.15rps；Number of repetition：2-5；Scan mode：Order jumps peak.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112114023A (en) * | 2019-06-19 | 2020-12-22 | 湖北中烟工业有限责任公司 | Method for detecting aluminum release amount in smoke of cigarette heated without burning |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103969324A (en) * | 2014-05-26 | 2014-08-06 | 国家烟草质量监督检验中心 | Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead in cigarette side-stream smoke |
| CN104597109A (en) * | 2015-01-21 | 2015-05-06 | 上海烟草集团有限责任公司 | Method for detecting content of selenium in cigarette mainstream smoke |
-
2017
- 2017-10-09 CN CN201710930795.XA patent/CN107677721A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103969324A (en) * | 2014-05-26 | 2014-08-06 | 国家烟草质量监督检验中心 | Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead in cigarette side-stream smoke |
| CN104597109A (en) * | 2015-01-21 | 2015-05-06 | 上海烟草集团有限责任公司 | Method for detecting content of selenium in cigarette mainstream smoke |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112114023A (en) * | 2019-06-19 | 2020-12-22 | 湖北中烟工业有限责任公司 | Method for detecting aluminum release amount in smoke of cigarette heated without burning |
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