CN103954678B - The detection method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of cigarette ash - Google Patents
The detection method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of cigarette ash Download PDFInfo
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Abstract
Chromium in a kind of cigarette ash, nickel, arsenic, selenium, cadmium, lead content assay method it is characterised in that：Collect cigarette ash using flue dust plate, flue dust sample is cleared up using Microwave Digestion, detect the content of chromium, nickel, arsenic, selenium, cadmium, lead element in flue dust by inductivity coupled plasma mass spectrometry.The present invention adopts flue dust plate to collect flue dust, achieves being collected separately of every cigarette ash on conventional smoking machine, is prevented effectively from the cross-contamination of the loss of flue dust and different cigarette flue dust in aspiration procedure.Sample is processed using micro-wave digestion mode, it is to avoid the danger that traditional electric hot plate digestion method is brought using perchloric acid, reduce the consumption of acid, improve the ability of clearing up, clear up that effect is good, element loss is few, simple to operation.Used mixing acid system it is adaptable to the process of cigarette ash sample, cleared up thoroughly.This method adopted inductivity coupled plasma mass spectrometry parameter, is corrected to interference, sensitivity is high, reproducible effectively, and the response rate is high, and result is accurate.
Description
Technical field
The invention belongs to the physical and chemical inspection technical field of Medicated cigarette, relate generally to trace elements determination field in cigarette ash,
Specifically a kind of cigarette ash is collected, processes and adopts icp mses measure cigarette ash
Middle chromium, nickel, arsenic, selenium, cadmium, the method for lead.
Background technology
The heavy metal elements such as chromium, nickel, arsenic, selenium, cadmium, lead are the harmful components in Medicated cigarette and flue gas.Canadian political affairs in 1998
46 kinds of mansion harmful substance list, China in 2006 fulfil the scheme of FCTC, FDA in 2011 issues 101 grow tobacco and flue gas has
Evil composition list all by comprise chromium, nickel, arsenic, selenium, cadmium, lead heavy metal element be classified as disclosure and control content.Heavy metal
Element is aspirated by cigarette burning, or enters human body, or is diffused in environment, or is retained by filter tip, greatly then remains
In flue dust.Neutron activation analysis shows that to the research of Medicated cigarette Elemental redistribution in flue dust, potassium is the cigarette portions participating in burning
73.6%, zinc be 63.2%, chlorine be 67.3% [Journal of Radioanalytical and Nuclear Chemistry,
Vol. 217, No.1 (1997) 77-82].Chromium, nickel, arsenic, selenium, cadmium, lead may major part be distributed in the middle of flue dust, to environment
Pollute.Thus the distribution of element and the harm of Medicated cigarette after the content of heavy metal right solution cigarette burning in Accurate Determining flue dust
Property evaluation tool be of great significance.It is little that neutron activation analysis has a matrix effect, and sensitivity is high, and accuracy is good, can carry out
The advantages of multielement, nondestructive analysis, and it is applied to the analysis of all kinds of sample such as liquid, solid, however it is necessary that using complexity
Main facilities（As nuclear reactor）, analysis cost height, is not a kind of very universal analysis means.Inductively coupled plasma
Mass spectrography can analyze nearly all element on the earth due to it, and sensitivity is high, detection limit is low, linear detection range width（Up to 9
The order of magnitude）, and multielement analysises can be carried out, equipment is universal, analysis cost is relatively low and be widely used in elementary analysiss neck
Domain.
Therefore, in order to further appreciate that the regularity of distribution of element in Nicotiana tabacum L., comprehensive assessment tobacco product is to environment and human body
The harm of health it is necessary to set up that a kind of sensitivity is high, reproducible, simple, chromium, nickel, arsenic, selenium, cadmium, lead in efficient flue dust
The assay method of the ICP-MS of heavy metal element.
Content of the invention
The purpose of the present invention is based on above-mentioned current condition, is intended to fill up existing detection technique blank, and sets up one kind
The method that ICP-MS measures heavy metal element in cigarette ash.The assay method being provided using the present invention, can be quick, accurately detects
The content of heavy metal element in cigarette ash.
The purpose of the present invention is achieved through the following technical solutions：
In cigarette ash, chromium, nickel, arsenic, selenium, cadmium, the assay method of lead comprise the following steps：
1）, the collection of flue dust, be collected separately every cigarette ash, detailed process is：
A, the cleaning of flue dust plate, politef flue dust plate selected by flue dust plate, first uses nitric acid dousing politef flue dust
Plate, uses ultra-pure water and methanol to rinse flue dust plate successively using front, dries, preserve；
B, Medicated cigarette prepare, and extract cigarette sample according to GB/T 5606.1, in 22 ± 1 DEG C of temperature and relative humidity 60 ± 3%
Under the conditions of balance 48h, select the qualified cigarette of weight（Weight：Meansigma methodss ± 20mg）；
C, the collection of flue dust, the dry politef flue dust plate of cleaning are placed on ashtray, according to GB/T16450
《Conventional analyses smoking machine definition and standard conditions》Adjustment checks smoking machine smoking parameters, smoking cigarette.After suction terminates, little
The heart takes off flue dust plate, and the flue dust collecting whole cigarette, on pan paper, then flue dust is transferred in counteracting tank；
2）, micro-wave digestion, in micro-wave diminishing pot, sequentially add nitric acid, hydrochloric acid and hydrogen peroxide solution, put into micro-wave digestion
Carry out micro-wave digestion, detailed process is in instrument：
A, the acid adding in micro-wave diminishing pot successively are that 65% nitric acid, 37% hydrochloric acid and 30% dioxygen are water-soluble for mass fraction
Liquid, nitric acid, hydrochloric acid, hydrogen peroxide volume are respectively 6mL, 2mL, 1mL.
B, micro-wave digestion program are intensification 5min to 100 DEG C, keep 5min, intensification 5min to 160 DEG C, keep 5min, rise
Warm 5min to 190 DEG C, keep 30min.
3）, catch up with acid cut hold, counteracting tank is put in the temperature control electric heater with dust-proof exhaust hood, under the conditions of 130 DEG C,
Heating 2～3h, treats that in counteracting tank, remaining liq volume is in 0.5～1mL, takes out counteracting tank, be cooled to room temperature.Sample solution is turned
Move in 250 mL plastics volumetric flasks, clean counteracting tank 3～4 times with ultra-pure water, cleanout fluid is also transferred in 250 mL volumetric flasks,
Use ultra-pure water constant volume, shake up, obtain final product sample prepare liquid；
The effect of dust-proof exhaust hood is to prevent the heavy metal in environment dust fall and air in heating process from entering in digestion solution
Pollution is brought to sample.
4）, the preparation of standard working solution, standard blank solution：5% nitric acid, prepare the chromium of variable concentrations, nickel, arsenic, selenium,
Cadmium, lead hybrid standard working solution；Its concentration be respectively 1 g/L, 2 g/L, 5 g/L, 10 g/L, 20 g/L, 40 g/L, 60
g/L、100µg/L.
5）, inductivity coupled plasma mass spectrometry measure, draw the standard blank solution of certain volume and variable concentrations chromium,
Nickel, arsenic, selenium, cadmium, lead hybrid standard working solution, in injection inductivity coupled plasma mass spectrometry, add internal standard online, are selecting
Instrument parameter under, with elemental chromium to be measured, nickel, arsenic, selenium, cadmium, lead content and corresponding internal standard element content ratio as abscissa,
Elemental chromium to be measured, nickel, arsenic, selenium, cadmium, lead mass-to-charge ratio intensity are vertical coordinate with the ratio of corresponding internal standard element mass-to-charge ratio intensity, build
Vertical chromium, nickel, arsenic, selenium, cadmium, the standard working curve of lead, try to achieve chromium, nickel, arsenic, selenium, cadmium, the one-variable linear regression of lead concentration relation
Equation, R2More than 0.999, online addition internal standard is measured to sample solution, by chromium, nickel, arsenic, selenium, cadmium, lead matter lotus in sample
Specific strength brings regression equation into the ratio of corresponding internal standard element mass-to-charge ratio intensity, calculate chromium in flue dust sample to be measured, nickel,
Arsenic, selenium, cadmium, lead content.
The calculating of chromium, nickel, arsenic, selenium, cadmium, lead content in cigarette ash, draws chromium, nickel, arsenic, selenium, cadmium, the work of lead respectively
Curve, is measured to testing sample solution, calculates the content of chromium, nickel, arsenic, selenium, cadmium, lead in every Medicated cigarette.
Result calculates, and in cigarette ash, the computing formula of the content of chromium, nickel, arsenic, selenium, cadmium, lead is：
In formula：
Chromium, nickel, arsenic, selenium, cadmium, the content of lead in every flue dust of m, unit is nanogram every（ng/cig）；
Chromium, nickel, arsenic, selenium, cadmium, the concentration of lead element in A sample solution to be measured, unit is micro- gram per liter（µg/L）；
The volume of 250 samples solution to be measured, unit is milliliter（mL）；
N tests the number of smoking cigarette every time（cig）.
The specific method of the present invention is described in further detail as follows：
1st, the cleaning of flue dust plate, uses 20%HNO3（Volume fraction）Soak more than politef flue dust plate 48h, take out cigarette
Hawk, with ultrapure water 3～4 times, removes the nitric acid on surface, then uses methanol（Top pure grade）Rinse flue dust plate surface, 100
Dry in ten thousand grades of cleaning cabinets, dust-proof, antifouling preservation.
2nd, micro-wave digestion sample, sequentially adding mass fraction in micro-wave diminishing pot is 65% nitric acid, 37% hydrochloric acid and 30% pair
Oxygen aqueous solution, wherein nitric acid:Hydrochloric acid:Hydrogen peroxide=6mL: 2mL:1mL.Program of clearing up as shown in table 1 carries out microwave and disappears
Solution.
Table 1 micro-wave digestion heating schedule
Clear up and finish, treat that microwave dissolver temperature is down to less than 40 DEG C, take out counteracting tank.
Clearing up of sample blank, is not added with sample in counteracting tank, only adds ibid mix acid liquor, with same micro-wave digestion program
Sample blank is cleared up.
3rd, the preparation of standard working solution, standard blank solution：5% salpeter solution（Volume fraction）, pipette 50mL65% nitre
Acid solution, in 1000mL plastics volumetric flask, is diluted with ultra-pure water, constant volume.
Chromium, nickel, arsenic, selenium, cadmium, lead one-level hybrid standard storing solution：Concentration 10mg/L.（Preserve in the environment of 4 DEG C, effectively
1 year phase）.
Chromium, nickel, arsenic, selenium, cadmium, two grades of hybrid standard storing solutions of lead：Accurately pipette 0.5mL chromium, nickel, arsenic, selenium, cadmium, lead one
Level hybrid standard storing solution is settled to 50 mL with 5% salpeter solution dilution to 50mL plastics volumetric flask.（Protect in the environment of 4 DEG C
Deposit, 1 month effect duration）.
Chromium, nickel, arsenic, selenium, cadmium, lead hybrid standard working solution：Accurately pipette respectively 0.5mL, 1mL, 2.5mL, 5mL,
10mL, 20mL, 30mL chromium, nickel, arsenic, selenium, cadmium, two grades of hybrid standard storing solution 50mL plastics volumetric flasks of lead, the nitric acid with 5% is dilute
Release constant volume, shake up, prepare 7 grades of chromium, nickel, arsenic, selenium, cadmium, lead standard working solution.Take two grades of hybrid standard storing solutions as the 8th
Level standard working solution.Prepare example such as table 2, that is, join and use.
The serial chromium of table 2, nickel, arsenic, selenium, cadmium, lead hybrid standard working solution are prepared
| Series standard working solution | Chromium（µg/L） | Nickel（µg/L） | Arsenic（µg/L） | Selenium（µg/L） | Cadmium（µg/L） | Lead（µg/L） |
| 1 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 |
| 2 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 |
| 3 | 5.00 | 5.00 | 5.00 | 5.00 | 5.00 | 5.00 |
| 4 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 |
| 5 | 20.00 | 20.00 | 20.00 | 20.00 | 20.00 | 20.00 |
| 6 | 40.00 | 40.00 | 40.00 | 40.00 | 40.00 | 40.00 |
| 7 | 60.00 | 60.00 | 60.00 | 60.00 | 60.00 | 60.00 |
| 8 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 | 100.00 |
4th, sample determination
（1）Inductivity coupled plasma mass spectrometry（ICP-MS）Parameter
The running parameter of ICP-MS is optimized, makes the sensitivity of instrument, oxide, double charge, quality axle all just
Often in working range.The Instrument working parameter such as table 3 optimizing.
Table 3 ICP-MS running parameter
| Project | Working condition | Project | Working condition |
| Radio-frequency power（W） | 1330 | Peristaltic pump gathers rotating speed（rps） | 0.1 |
| Flow rate of carrier gas（L/min） | 1.18 | Peristaltic pump lifts rotating speed（rps） | 0.3 |
| Sampling depth（mm） | 7.2 | Peristaltic pump lifts the time（s） | 30 |
| Nebulizer | Babington | Peristaltic pump stabilization time（s） | 45 |
| Atomization room temperature（℃） | 2 | Repeated acquisition number of times | 3 |
Note：Rps refers to the revolution of peristaltic pump each second.
Choose appropriate measurement isotopic number and internal standard element, for the properities optimization best total of points time of different elements, have
Body parameter such as table 4.
Table 4 measurement isotope, internal standard element and the time of integration
| Element | Measurement isotope | Internal standard element | The time of integration |
| Cr | 53Cr | 115In | 0.3 |
| Ni | 60Ni | 115In | 0.3 |
| As | 75As | 115In | 2.0 |
| Se | 82Se | 115In | 1.0 |
| Cd | 111Cd | 115In | 2.0 |
| Pb | 208Pb | 209Bi | 0.3 |
（2）The mensure of chromium, nickel, arsenic, selenium, cadmium, lead in flue dust testing sample solution
Draw appropriate standard blank solution respectively, the chromium of variable concentrations, nickel, arsenic, selenium, cadmium, lead hybrid standard working solution,
Injection inductivity coupled plasma mass spectrometry in, online add internal standard, under selected instrument parameter, with elemental chromium to be measured, nickel,
Arsenic, selenium, cadmium, lead content are abscissa with the ratio of corresponding internal standard element content, elemental chromium to be measured, nickel, arsenic, selenium, cadmium, lead matter lotus
Specific strength is vertical coordinate with the ratio of corresponding internal standard element mass-to-charge ratio intensity, sets up the standard work of chromium, nickel, arsenic, selenium, cadmium, lead
Curve.Linear regression is carried out to correction data, tries to achieve chromium, nickel, arsenic, selenium, cadmium, the regression equation of lead concentration relation, R2Should not be little
In 0.999.Online add internal standard that sample solution is measured, by chromium in sample, nickel, arsenic, selenium, cadmium, lead mass-to-charge ratio intensity with
The ratio of corresponding internal standard element mass-to-charge ratio intensity brings regression equation into, calculate chromium in flue dust sample to be measured, nickel, arsenic, selenium, cadmium,
The content of lead.
Inner mark solution is 1mg/L In and Bi mixed solution, and substrate is 5% salpeter solution.
The quantitation of element adopts external standard method, the online error and the matrix that add internal standard predominantly to eliminate the unstable introducing of instrument
Effect.
（3）The detection limit of the inventive method
Take the result of 10 replicate samples blank solutions and 3 parallel assay finite concentration each element standard solution
As a result, it is calculated as follows, and calculate the detection limit of every cigarette ash sample, result such as table 5.
Detection limit（µg/L）
In formula：
σ：The standard deviation of blank reagent solution；
S：The CPS of certain standard solution each element standard solution（Signal intensity）；
B：The CPS of blank reagent solution；
C：The concentration of each element standard solution.
Chromium, nickel, arsenic, selenium, cadmium, the detection limit of lead in table 5 flue dust
| Element | Regression equation | The range of linearity (g/L) | Correlation coefficient | Detection limit（ng/cig） |
| Cr | Y=1.991E-3X+3.525E-4 | 0.00～100.00 | 0.9998 | 1.1 |
| Ni | Y=2.391E-2X+2.407E-3 | 0.00～100.00 | 0.9996 | 1.2 |
| As | Y=9.418E-3X+2.319E-3 | 0.00～100.00 | 1.0000 | 0.7 |
| Se | Y=6.892E-4X+7.175E-4 | 0.00～100.00 | 0.9997 | 1.4 |
| Cd | Y=1.127E-3X+3.924E-4 | 0.00～100.00 | 1.0000 | 0.4 |
| Pb | Y=2.086E-2X+2.281E-3 | 0.00～100.00 | 0.9999 | 0.8 |
Note：Detection limit ng/ cig, to be settled to 250 mL, one Medicated cigarette of suction calculates.
(4) repeatability of the inventive method and the response rate
To flue dust sample parallel assay 6 times, repeatability is represented with relative standard deviation RSD% of measurement result.Result such as table
6.
Table 6 repeated experiment result（ng/cig）
| Numbering | 1 | 2 | 3 | 4 | 5 | 6 | RSD % |
| Cr | 712.2 | 698.5 | 701.1 | 660.0 | 643.6 | 732.1 | 4.8 |
| Ni | 533.2 | 512.7 | 489.4 | 531.0 | 497.0 | 463.8 | 5.3 |
| As | 155.3 | 132.2 | 120.1 | 109.8 | 135.0 | 114.6 | 13.0 |
| Se | 139.0 | 142.9 | 133.8 | 141.5 | 135.7 | 129.5 | 3.7 |
| Cd | 599.1 | 616.0 | 576.2 | 631.0 | 551.1 | 620.2 | 5.1 |
| Pb | 1185.0 | 1109.0 | 1096.8 | 1024.5 | 1100.0 | 1177.4 | 5.3 |
Add a certain amount of standard solution in flue dust solution to be measured, the solution to be measured after former solution to be measured and mark-on is entered
Row measures, and investigates the response rate of method.As table 7.
Chromium, nickel, arsenic, selenium, cadmium, the response rate of lead in table 7 flue dust
The present invention overcomes the deficiency of prior art sample collection and sample-pretreating method, improve conventional smoking
The collection method of machine flue dust and digestion procedure, optimize the testing conditions of ICP-MS, compared with prior art the present invention have with
Lower excellent results.
Flue dust is collected using flue dust plate, being collected separately of every cigarette ash is achieved on conventional smoking machine, effectively keeps away
Exempt from the cross-contamination of the loss of flue dust and different cigarette flue dust in aspiration procedure.
Compare with traditional electric hot plate digestion method, sample is processed using micro-wave digestion mode, it is to avoid the acid such as perchloric acid
Property strong, the use of dangerous high reagent, and decrease the consumption of acid, reduce the harm to operator.Clear up effect
Good, element loss is few, simple to operate.Present invention mixing acid system for flue dust Specimen eliminating thoroughly, clarify, transparent by digestion solution.
Optimize ICP-MS sampling parameter, add internal standard online, take appropriate internal standard element that interference is corrected, measure
The high result of flue dust sample recovery rate is accurate.
The present invention also has the advantages of quick, accurate, easy and simple to handle, sensitivity is high, reproducible, and the response rate is high.
Brief description
Fig. 1 is the flow chart of assay method of the present invention.
Specific embodiment
The present invention is described further with reference to embodiments：
Example 1：
1. reagent and instrument：
Cr, Ni, As, Se, Cd, Pb mixed standard solution (10mg/L, Agilent company of the U.S.)；In, Bi mix internal standard
Solution（1mg/L, Agilent company of the U.S.）；Ce, Co, Li, Tl, Y tune liquid（10 μ g/L, Agilent company of the U.S.）；Methanol
(top pure grade, German Merck company)；HNO3(top pure grade, 65%, mass fraction, German Merck company)；HCL（Top pure grade,
37%, mass fraction, German Merck company）；H2O2(top pure grade, 30%, mass fraction, German Merck company)；Ultra-pure water
(resistivity >=18.2 M Ω cm).
RM 20H rotating disk smoking machine（German Borgwaldt-KC company）；Agilent 7500a inductively coupled plasma
Mass spectrograph（ICP-MS, Agilent company of the U.S.）；CEM Mars6 microwave dissolver（U.S. CE M company）；Milli-Q50 surpasses
Pure water meter（Millipore company of the U.S.）；Temperature control electric heater（BHW-09C, Shanghai company of Botong）, dust-proof exhaust hood;PET holds
Measuring bottle 50mL, PET volumetric flask 250 mL, PET volumetric flask 1000 mL.
2. sample treatment：
Extract cigarette sample A (Virginian-type cigarette) according to GB/T 5606.1, balance 48h（22 ± 1 DEG C of temperature, relative humidity
60 ± 3%）, select qualified cigarette（Weight：Meansigma methodss ± 20mg）.Place the dry politef flue dust plate of cleaning in suction
On cigarette machine ashtray, according to GB/T16450《Conventional analyses smoking machine definition and standard conditions》Adjustment smoking machine smoking parameters.
Smoking cigarette on Borgwaldt-KCRM 20H smoking machine.After suction terminates, carefully take off flue dust plate, collect the cigarette of whole cigarette
Ash, on pan paper, is then poured flue dust in counteracting tank into.Sequentially add in counteracting tank 65% nitric acid 6mL, 37% hydrochloric acid 2mL and
30% hydrogen peroxide 1mL.Program of clearing up as shown in table 1 carries out micro-wave digestion.After microwave dissolver temperature is down to below 40 DEG C
Take out counteracting tank.Counteracting tank is put into temperature control electric heater, under the conditions of 130 DEG C, catches up with acid 2～3 hours, remaining liq volume
Take out counteracting tank during 0.5～1mL, be cooled to room temperature.Sample solution is transferred in 250 mL volumetric flasks, is cleaned with ultra-pure water and disappear
Solution tank 3～4 times, cleanout fluid is all transferred in 250 mL volumetric flasks, uses ultra-pure water constant volume, shakes up.
3. sample determination：
Open ICP-MS, after instrument stabilizer, draw Ce, Co, Li, Tl, Y tuning liquid adjustment instrument parameter, make sensitivity
With the level of chaff interference in the reasonable scope.Absorption standard blank solution, 1 g/L preparing, 2 g/L, 5 g/L, 10 g/L,
20 g/L, 40 g/L, 60 g/L, 100 g/L chromium, nickel, arsenic, selenium, cadmium, lead hybrid standard working solution, add internal standard online, enter
Row ICP-MS measures.With the ratio of constituent content to be measured and corresponding internal standard element content as abscissa, element mass-to-charge ratio to be measured is strong
Degree is vertical coordinate with the ratio of corresponding internal standard element mass-to-charge ratio intensity, sets up elemental standards working curve to be measured.To correction data
Carry out regression analyses, obtain chromium, nickel, arsenic, selenium, cadmium, the regression equation of lead concentration relation.Sample solution and inner mark solution are entered simultaneously
Row measures, and is brought into the ratio of corresponding internal standard element mass-to-charge ratio intensity with chromium, nickel, arsenic, selenium, cadmium, lead mass-to-charge ratio intensity in sample
Regression equation, through calculating, obtains final product chromium, nickel, arsenic, selenium, cadmium, the content of lead in flue dust sample to be measured, the results are shown in Table 8.
Chromium, nickel, arsenic, selenium, cadmium, lead content testing result in table 8 cigarette sample A flue dust
| Element | Cr | Ni | As | Se | Cd | Pb |
| Content ng/cig） | 307.9 | 665.6 | 124.1 | 50.8 | 454.8 | 1189.4 |
Example 2：
Concrete steps as described in Example 1, cigarette sample B（Bai Leyan）, record chromium in cigarette ash, nickel, arsenic, selenium, cadmium,
The content of lead is shown in Table 9.
Chromium, nickel, arsenic, selenium, cadmium, lead content testing result in table 9 cigarette sample B flue dust
| Element | Cr | Ni | As | Se | Cd | Pb |
| Content（ng/cig） | 434.4 | 821.3 | 135.3 | 26.0 | 769.4 | 1337.0 |
Example 3：
Concrete steps as described in Example 1, cigarette sample C（Turkish tobaccos）, record chromium in cigarette ash, nickel, arsenic, selenium, cadmium,
The content of lead is shown in Table 10.
Chromium, nickel, arsenic, selenium, cadmium, lead content testing result in table 10 cigarette sample C flue dust
| Element | Cr | Ni | As | Se | Cd | Pb |
| Content（ng/cig） | 656.4 | 869.2 | 181.1 | 42.5 | 310.9 | 661.9 |
Example 4：
Concrete steps as described in Example 1, cigarette sample D（Blended type cigarette）, record chromium in cigarette ash, nickel, arsenic,
Selenium, cadmium, the content of lead are shown in Table 11.
Chromium, nickel, arsenic, selenium, cadmium, lead content testing result in table 11 cigarette sample D flue dust
| Element | Cr | Ni | As | Se | Cd | Pb |
| Content（ng/cig） | 353.6 | 485.1 | 297.1 | 207.9 | 238.6 | 1374.0 |
Claims (6)
1. in a kind of cigarette ash, chromium, nickel, arsenic, selenium, cadmium, the detection method of lead element walk it is characterised in that including following technique
Suddenly：
1) collection of flue dust, is collected separately every cigarette ash with politef flue dust plate；
2）Micro-wave digestion, flue dust is placed in micro-wave diminishing pot, adds nitric acid, hydrochloric acid and hydrogen peroxide solution successively, put into tank
Enter and in microwave dissolver, carry out micro-wave digestion；
3）Catch up with acid cut to hold, heating carried out to Specimen eliminating liquid and catches up with acid treatment, be then transferred in volumetric flask, use ultra-pure water constant volume,
Obtain sample prepare liquid, catch up with the temperature control electric heater used by acid need to join air draft dust cover, catch up with 130 DEG C of sour temperature highest；
4）The preparation of standard working solution, standard blank solution is volume fraction 5% nitric acid, is prepared with the nitric acid of volume fraction 5%
The chromium of variable concentrations, nickel, arsenic, selenium, cadmium, lead hybrid standard working solution；
5）Inductivity coupled plasma mass spectrometry measures, draw the chromium of the standard blank solution of certain volume and variable concentrations, nickel,
Arsenic, selenium, cadmium, lead hybrid standard working solution, in injection icp mses, add internal standard online, are selecting
Instrument parameter under, with elemental chromium to be measured, nickel, arsenic, selenium, cadmium, lead content and corresponding internal standard element content ratio as abscissa,
Elemental chromium to be measured, nickel, arsenic, selenium, cadmium, lead mass-to-charge ratio intensity are vertical coordinate with the ratio of corresponding internal standard element mass-to-charge ratio intensity, build
Vertical chromium, nickel, arsenic, selenium, cadmium, the standard working curve of lead, try to achieve chromium, nickel, arsenic, selenium, cadmium, the one-variable linear regression of lead concentration relation
Equation, R2More than 0.999, online addition internal standard is measured to sample solution, by chromium, nickel, arsenic, selenium, cadmium, lead matter lotus in sample
Specific strength brings regression equation into the ratio of corresponding internal standard element mass-to-charge ratio intensity, calculate chromium in flue dust sample to be measured, nickel,
Arsenic, selenium, cadmium, lead content.
2. chromium, nickel, arsenic, selenium, cadmium, the detection method of lead element in cigarette ash according to claim 1, its feature exists
In：In step 1）In, the cleaning of flue dust plate passes through volume fraction 20%HNO3Soak more than 48h, after ultrapure water, use first
Alcohol rinses surface, dries.
3. chromium, nickel, arsenic, selenium, cadmium, the detection method of lead element in cigarette ash according to claim 1, its feature exists
In：Successively in micro-wave diminishing pot add acid be mass fraction be 65% nitric acid, mass fraction be 37% hydrochloric acid and mass fraction
For 30% hydrogen peroxide solution, nitric acid, hydrochloric acid, hydrogen peroxide volume are respectively 6mL, 2mL, 1mL.
4. chromium, nickel, arsenic, selenium, cadmium, the detection method of lead element in cigarette ash according to claim 1, its feature exists
In：Micro-wave digestion program is intensification 5min to 100 DEG C, keeps 5min, intensification 5min to 160 DEG C, keeps 5min, intensification 5min is extremely
190 DEG C, keep 30min.
5. chromium, nickel, arsenic, selenium, cadmium, the detection method of lead element in cigarette ash according to claim 1, its feature exists
In：Using internal standard, ICP-MS measurement process is corrected.
6. chromium, nickel, arsenic, selenium, cadmium, the detection method of lead element in cigarette ash according to claim 1, its feature exists
In：The chromium of described variable concentrations, nickel, arsenic, selenium, cadmium, lead hybrid standard working solution concentration be respectively 1 g/L, 2 g/L, 5
g/L、10µg/L、20µg/L、40µg/L、60µg/L、100µg/L.
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| CN105021692A (en) * | 2015-08-06 | 2015-11-04 | 云南同创检测技术股份有限公司 | Method for simultaneously determining multiple inorganic elements in cigarette liquid of electronic cigarette |
| CN106841366A (en) * | 2015-12-07 | 2017-06-13 | 中国科学院大连化学物理研究所 | A kind of method for recognizing cigarette ash and other ashes |
| CN105823536B (en) * | 2016-04-15 | 2018-06-26 | 河南中烟工业有限责任公司 | The method that marker method measures cigarette overlapping glue resin added |
| CN106198708A (en) * | 2016-08-11 | 2016-12-07 | 深圳瀚星翔科技有限公司 | The detection method of the content of heavy metal in electronic cigarette atomizing vapour |
| CN106404515A (en) * | 2016-11-08 | 2017-02-15 | 苏州恒润商品检验有限公司 | Detection method for determining multiple elements in solid cosmetic powder |
| CN106840838A (en) * | 2016-12-19 | 2017-06-13 | 湖南省农业生物技术研究中心 | A kind of digestion procedure of paddy rice sample determination cadmium isotope content |
| CN107271534A (en) * | 2017-08-23 | 2017-10-20 | 国家烟草质量监督检验中心 | The method that a kind of micro-wave digestion-inductively coupled plasma mass spectrometry determines electronic cigarette heater strip Contents of Main Components |
| CN107462626A (en) * | 2017-08-23 | 2017-12-12 | 国家烟草质量监督检验中心 | A kind of method of micro-wave digestion-inductively coupled plasma mass spectrometry measure tobacco juice for electronic smoke contacting metal utensil main component |
| CN110110343A (en) * | 2018-12-19 | 2019-08-09 | 中国科学院广州地球化学研究所 | Mass spectrometric data processing method, system, terminal and computer readable storage medium |
| CN110057791A (en) * | 2019-02-25 | 2019-07-26 | 滕亚君 | The measuring method of arsenic, mercury, bismuth, lead, cadmium content in a kind of eucalyptus oil |
| CN112051129A (en) * | 2020-08-17 | 2020-12-08 | 上海烟草集团有限责任公司 | Digestion method of tobacco essence and heavy metal determination method |
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