CN103954678A - Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead elements in cigarette ashes - Google Patents
Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead elements in cigarette ashes Download PDFInfo
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Abstract
The invention discloses a method for detecting chromium, nickel, arsenic, selenium, cadmium and lead elements in cigarette ashes. The method is characterized in that cigarette ashes are collected by using a cigarette ash plate, a cigarette ash sample is dispelled by adopting a microwave digestion method, and the contents of chromium, nickel, arsenic, selenium, cadmium and lead elements in the cigarette ashes are detected by inductively coupled plasma mass spectrometry. The cigarette ashes are collected by adopting the cigarette ash plate, independent collection of each cigarette ash is achieved on a conventional smoking machine, and loss of cigarette ashes and cross contamination of different cigarette ashes in the smoking process are effectively avoided. The sample is processed by adopting the microwave digestion method, so that the risk caused by use of a perchloric acid in the traditional electric hot plate digestion mode is avoided, the dosage of the acid is reduced, the digestion ability is improved, the method is good in digestion effect, less in element loss, and simple and easy to operate, and the used mixed acid system is applicable to treatment of the cigarette ash sample, and thorough to digest. The interference is effectively corrected by adopting inductively coupled plasma mass spectrum parameters, and the method is high in sensitivity, good in repeatability, high in recovery rate, and accurate in result.
Description
Technical field
The invention belongs to the physical and chemical inspection technical field of cigarette, relating generally to determination of trace element field in cigarette ash, is a kind of method of cigarette ash being collected, processed and adopts chromium, nickel, arsenic, selenium, cadmium, lead in icp ms mensuration cigarette ash specifically.
Background technology
The heavy metal elements such as chromium, nickel, arsenic, selenium, cadmium, lead are the objectionable constituent in cigarette and flue gas.What 46 kinds of objectionable impurities lists of Canadian government in 1998, China in 2006 fulfiled that the scheme of FCTC, FDA in 2011 issue 101 grows tobacco and harmful ingredients in flue gas list all will comprise chromium, nickel, arsenic, selenium, cadmium, plumbously classify as and disclose and regulate content at interior heavy metal element.Heavy metal element aspirates by cigarette burning, or enters human body, or is diffused in environment, or is held back by filter tip, remains in cigarette ash greatly.The research that neutron activation analysis distributes to cigarette element show potassium in cigarette ash be participate in burning cigarette portions 73.6%, zinc is 63.2%, chlorine is 67.3%[Journal of Radioanalytical and Nuclear Chemistry, Vol. 217, No.1 (1997) 77-82].Chromium, nickel, arsenic, selenium, cadmium, plumbous may major part being distributed in the middle of cigarette ash, to environment.Thereby in Accurate Determining cigarette ash after the right solution cigarette burning of the content of heavy metal the distribution of element and the Evaluation of Harmfulness tool of cigarette be of great significance.It is little that neutron activation analysis has matrix effect, highly sensitive, accuracy is good, can carry out the advantages such as multielement, nondestructive analysis, and be applicable to the analysis of all kinds of samples such as liquid, solid, but need to utilize complicated main facilities (as nuclear reactor), analysis cost is high, it is not a kind of very general analysis means.Inductively coupled plasma mass spectrometry is because it can analyze nearly all element on the earth, highly sensitive, detection limit is low, linear detection range wide (can reach 9 orders of magnitude), and can carry out multielement analysis, equipment is general, analysis cost is relatively low and be widely used in ultimate analysis field.
Therefore, in order further to understand the regularity of distribution of element in tobacco, the harm of comprehensive assessment tobacco product to environmental and human health impacts, just need to set up the assay method of the ICP-MS of chromium, nickel, arsenic, selenium, cadmium, plumbous heavy metal element in a kind of highly sensitive, reproducible, simple, efficient cigarette ash.
Summary of the invention
Object of the present invention just based on above-mentioned current condition, be intended to fill up existing detection technique blank, and set up a kind of ICP-MS and measure the method for heavy metal element in cigarette ash.Utilize assay method provided by the invention, can fast, accurately detect the content of heavy metal element in cigarette ash.
The object of the invention is to be achieved through the following technical solutions:
In cigarette ash, chromium, nickel, arsenic, selenium, cadmium, plumbous assay method comprise the following steps:
1), the collection of cigarette ash, collect separately every cigarette ash, detailed process is:
Cleaning of a, cigarette ash plate, cigarette ash plate is selected teflon cigarette ash plate, first uses nitric acid dousing teflon cigarette ash plate, uses successively ultrapure water and washed with methanol cigarette ash plate before use, dries, and preserves;
B, cigarette are prepared, and extract cigarette sample according to GB/T 5606.1, and balance 48h under 22 ± 1 DEG C of temperature and relative humidity 60 ± 3% conditions, selects the cigarette that weight is qualified (weight: mean value ± 20mg);
The collection of c, cigarette ash, is placed in clean dry teflon cigarette ash plate on ashtray, adjusts and checks smoking machine suction parameter, smoking cigarette according to GB/T16450 " smoking machine definition and standard conditions for conventional analysis ".After suction finishes, carefully take off cigarette ash plate, collect the cigarette ash of whole cigarette on pan paper, then cigarette ash is transferred in counteracting tank;
2), micro-wave digestion, in micro-wave diminishing pot, add successively nitric acid, hydrochloric acid and hydrogen peroxide solution, put into microwave dissolver and carry out micro-wave digestion, detailed process is:
A, be that massfraction is 65% nitric acid, 37% hydrochloric acid and 30% hydrogen peroxide solution to the acid adding in micro-wave diminishing pot successively, nitric acid, hydrochloric acid, hydrogen peroxide volume are respectively 6mL, 2mL, 1mL.
B, micro-wave digestion program are 5min to 100 DEG C of intensification, keep 5min, and 5min to 160 DEG C of intensification keeps 5min, and 5min to 190 DEG C of intensification keeps 30min.
3), catch up with acid cut to hold, counteracting tank is put into the temperature control electric heater of the dustproof exhaust hood of band, under 130 DEG C of conditions, heating 2～3h, treats that in counteracting tank, remaining liq volume, at 0.5～1mL, takes out counteracting tank, is cooled to room temperature.Sample solution is transferred in 250 mL plastics volumetric flasks, cleans counteracting tank 3～4 times with ultrapure water, cleaning fluid is also transferred in 250 mL volumetric flasks, uses ultrapure water constant volume, shakes up, and obtains sample liquid to be measured;
The effect of dustproof exhaust hood is to prevent from heating process that the heavy metal in environment dust fall and atmosphere enters in digestion solution sample is brought to pollution.
4), the preparation of standard operation solution, standard blank solution: 5% nitric acid, chromium, nickel, arsenic, selenium, cadmium, the plumbous hybrid standard working solution of preparation variable concentrations; Its concentration is respectively 1 μ g/L, 2 μ g/L, 5 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ g/L, 60 μ g/L, 100 μ g/L.
5), inductivity coupled plasma mass spectrometry is measured, draw the standard blank solution of certain volume and the chromium of variable concentrations, nickel, arsenic, selenium, cadmium, plumbous hybrid standard working solution, inject inductivity coupled plasma mass spectrometry, add online interior mark, under selected instrument parameter, with elemental chromium to be measured, nickel, arsenic, selenium, cadmium, lead content is horizontal ordinate with the ratio of corresponding internal standard element content, elemental chromium to be measured, nickel, arsenic, selenium, cadmium, plumbous mass-to-charge ratio intensity is ordinate with the ratio of corresponding internal standard element mass-to-charge ratio intensity, set up chromium, nickel, arsenic, selenium, cadmium, plumbous standard working curve, try to achieve chromium, nickel, arsenic, selenium, cadmium, the one-variable linear regression equation of lead concentration relation, R
2be greater than 0.999, add online interior mark to measure sample solution, bring chromium, nickel, arsenic, selenium, cadmium, plumbous mass-to-charge ratio intensity in sample into regression equation with the ratio of corresponding internal standard element mass-to-charge ratio intensity, calculate chromium, nickel, arsenic, selenium, cadmium, lead content in cigarette ash sample to be measured.
The calculating of chromium, nickel, arsenic, selenium, cadmium, lead content in cigarette ash, draws respectively chromium, nickel, arsenic, selenium, cadmium, plumbous working curve, and testing sample solution is measured, and calculates chromium in every cigarette, nickel, arsenic, selenium, cadmium, plumbous content.
Result is calculated, and in cigarette ash, the computing formula of the content of chromium, nickel, arsenic, selenium, cadmium, lead is:
In formula:
The content of chromium, nickel, arsenic, selenium, cadmium, lead in m-every cigarette ash, unit is every of nanogram (ng/cig);
The concentration of chromium, nickel, arsenic, selenium, cadmium, lead element in A-sample solution to be measured, unit is every liter of microgram (μ g/L);
The volume of 250-sample solution to be measured, unit is milliliter (mL);
N-at every turn the test number (cig) of smoking cigarette.
The concrete method of the present invention is described in further detail as follows:
1, cigarette ash plate is clean,use 20%HNO
3(volume fraction) takes out cigarette ash plate more than soaking teflon cigarette ash plate 48h, with ultrapure water flushing 3～4 times, removes surperficial nitric acid, then uses methyl alcohol (top grade is pure) to rinse cigarette ash plate surface, in 1,000,000 grades of cleaning cabinets, dries, dustproof, antifouling preservation.
2, micro-wave digestion sample,be 65% nitric acid, 37% hydrochloric acid and 30% hydrogen peroxide solution, wherein nitric acid to adding successively massfraction in micro-wave diminishing pot: hydrochloric acid: hydrogen peroxide=6mL:2mL:1mL.Carry out micro-wave digestion by the program of clearing up shown in table 1.
table 1 micro-wave digestion heating schedule
Clear up completely, treat that microwave dissolver temperature is down to below 40 DEG C, take out counteracting tank.
Clearing up of sample blank, does not add sample in counteracting tank, only add the same mix acid liquor, with same micro-wave digestion program, sample blank is cleared up.
3, the preparation of standard operation solution,standard blank solution: 5% salpeter solution (volume fraction), pipettes 50mL65% salpeter solution in 1000mL plastics volumetric flask, with ultrapure water dilution, constant volume.
Chromium, nickel, arsenic, selenium, cadmium, plumbous one-level hybrid standard storing solution: concentration 10mg/L.(under the environment of 4 DEG C, preserving the term of validity 1 year).
Chromium, nickel, arsenic, selenium, cadmium, plumbous secondary hybrid standard storing solution: accurately pipette 0.5mL chromium, nickel, arsenic, selenium, cadmium, plumbous one-level hybrid standard storing solution to being settled to 50 mL with 5% salpeter solution dilution in 50mL plastics volumetric flask.(under the environment of 4 DEG C, preserving the term of validity 1 month).
Chromium, nickel, arsenic, selenium, cadmium, plumbous hybrid standard working solution: accurately pipette respectively 0.5mL, 1mL, 2.5mL, 5mL, 10mL, 20mL, 30mL chromium, nickel, arsenic, selenium, cadmium, plumbous secondary hybrid standard storing solution 50mL plastics volumetric flask, with 5% nitric acid dilution constant volume, shake up, prepare 7 grades of chromium, nickel, arsenic, selenium, cadmium, plumbous standard operation solution.Get secondary hybrid standard storing solution as the 8th grade standard working solution.Preparation example, as table 2, is joined and is used.
the serial chromium of table 2, nickel, arsenic, selenium, cadmium, the preparation of plumbous hybrid standard working solution
| Series standard working solution | Chromium (μ g/L) | Nickel (μ g/L) | Arsenic (μ g/L) | Selenium (μ g/L) | Cadmium (μ g/L) | Plumbous (μ g/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 |
4, sample determination
(1) inductivity coupled plasma mass spectrometry (ICP-MS) parameter
Running parameter to ICP-MS is optimized, and makes the sensitivity, oxide, double charge, mass axes of instrument all in normal range of operation.The Instrument working parameter of optimizing is as table 3.
table 3 ICP-MS running parameter
| Project | Condition of work | Project | Condition of work |
| Radio-frequency power (W) | 1330 | Peristaltic pump gathers rotating speed (rps) | 0.1 |
| Flow rate of carrier gas (L/min) | 1.18 | Peristaltic pump promotes rotating speed (rps) | 0.3 |
| Sampling depth (mm) | 7.2 | Peristaltic pump promotes the time (s) | 30 |
| Atomizer | Babington | Peristaltic pump stabilization time (s) | 45 |
| Spray chamber temperature (DEG C) | 2 | Repeated acquisition number of times | 3 |
note: rps refers to the peristaltic pump revolution of p.s..
Choose appropriate measurement isotopic number and internal standard element, optimize the best total of points time for the character of different elements, design parameter is as table 4.
table 4 is measured isotope, internal standard element and integral time
| Element | Measure isotope | Internal standard element | Integral time |
| Cr | 53 Cr | 115In | 0.3 |
| Ni | 60 Ni | 115In | 0.3 |
| As | 75 As | 115In | 2.0 |
| Se | 82 Se | 115In | 1.0 |
| Cd | 111 Cd | 115In | 2.0 |
| Pb | 208Pb | 209Bi | 0.3 |
(2) mensuration of chromium, nickel, arsenic, selenium, cadmium, lead in cigarette ash testing sample solution
Draw respectively appropriate standard blank solution, the chromium of variable concentrations, nickel, arsenic, selenium, cadmium, plumbous hybrid standard working solution, inject inductivity coupled plasma mass spectrometry, add online interior mark, under selected instrument parameter, taking elemental chromium to be measured, nickel, arsenic, selenium, cadmium, lead content with the ratio of corresponding internal standard element content as horizontal ordinate, elemental chromium to be measured, nickel, arsenic, selenium, cadmium, plumbous mass-to-charge ratio intensity are ordinate with the ratio of corresponding internal standard element mass-to-charge ratio intensity, set up the standard working curve of chromium, nickel, arsenic, selenium, cadmium, lead.Correction data is carried out to linear regression, try to achieve the regression equation of chromium, nickel, arsenic, selenium, cadmium, lead concentration relation, R
2should not be less than 0.999.Add online interior mark to measure sample solution, bring chromium, nickel, arsenic, selenium, cadmium, plumbous mass-to-charge ratio intensity in sample into regression equation with the ratio of corresponding internal standard element mass-to-charge ratio intensity, calculate the content of chromium in cigarette ash sample to be measured, nickel, arsenic, selenium, cadmium, lead.
Inner mark solution is 1mg/L In and Bi mixed solution, and matrix is 5% salpeter solution.
The quantitative employing external standard method of element, adds interior mark to be mainly error and the matrix effect of eliminating the unstable introducing of instrument online.
(3) detection limit of the inventive method
Get the result of 10 replicate determination sample blank solution and the result of 3 each element standard solution of replicate determination finite concentration, be calculated as follows, and calculate the detection limit of every cigarette ash sample, result is as table 5.
Detection limit (μ g/L)
In formula:
σ: the standard deviation of blank reagent solution;
S: the CPS(signal intensity of the each element standard solution of certain standard solution);
B: the CPS of blank reagent solution;
C: the concentration of each element standard solution.
the detection limit of chromium, nickel, arsenic, selenium, cadmium, lead in table 5 cigarette ash
| Element | Regression equation | The range of linearity (μ g/L) | Related 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, aspirates a cigarette and calculates.
(4) repeatability of the inventive method and the recovery
To cigarette ash sample replicate determination 6 times, represent repeatability with the relative standard deviation RSD% of measurement result.Result is 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 |
In cigarette ash solution to be measured, add a certain amount of standard solution, the solution to be measured after former solution to be measured and mark-on is measured to the recovery of investigation method.As table 7.
the recovery of chromium, nickel, arsenic, selenium, cadmium, lead in table 7 cigarette ash
The inventive method has overcome the deficiency of prior art sample collection and sample-pretreating method, has improved collection method and the digestion procedure of conventional smoking machine cigarette ash, has optimized the testing conditions of ICP-MS, and compared with prior art the present invention has following excellent results.
Adopt cigarette ash plate to collect cigarette ash, on conventional smoking machine, realized the independent collection of every cigarette ash, effectively avoided the loss of cigarette ash and the cross pollution of different cigarette cigarette ashes in aspiration procedure.
With traditional electric hot plate digestion method comparison, adopt micro-wave digestion mode processing sample, avoid the acidity such as perchloric acid strong, the use of dangerous high reagent, and reduced sour consumption, reduce the harm to operating personnel.Clear up effectively, element loss is few, simple to operate.Acid mixture system of the present invention is thorough for cigarette ash Specimen eliminating, and digestion solution clarification is transparent.
Optimize ICP-MS sampling parameter, add online interior mark, take appropriate internal standard element to proofread and correct disturbing, measure the high result of cigarette ash sample recovery rate accurate.
The present invention also has quick, accurate, easy and simple to handle, highly sensitive, reproducible, recovery advantages of higher.
Brief description of the drawings
Fig. 1 is the process flow diagram of assay method of the present invention.
Embodiment
The present invention is described further below in conjunction with embodiment:
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 mixing inner mark solution (1mg/L, Agilent company of the U.S.); Ce, Co, Li, Tl, the tuning liquid of Y (10 μ g/L, Agilent company of the U.S.); Methyl alcohol (top grade is pure, German Merck company); HNO
3(top grade is pure, and 65%, massfraction, German Merck company); HCL(top grade is pure, and 37%, massfraction, German Merck company); H
2o
2(top grade is pure, and 30%, massfraction, German Merck company); Ultrapure water (resistivity>=18.2 M Ω cm).
RM 20H rotating disk smoking machine (German Borgwaldt-KC company); Agilent 7500a icp ms (ICP-MS, Agilent company of the U.S.); CEM Mars6 microwave dissolver (U.S. CE M company); Milli-Q50 ultrapure water instrument (Millipore company of the U.S.); Temperature control electric heater (BHW-09C, Shanghai company of Botong), dustproof exhaust hood; PET volumetric flask 50mL, PET volumetric flask 250 mL, PET volumetric flask 1000 mL.
2. sample preparation:
Extract cigarette sample A (Virginian-type cigarette) according to GB/T 5606.1,22 ± 1 DEG C of balance 48h(temperature, relative humidity 60 ± 3%), select qualified cigarette (weight: mean value ± 20mg).Place clean dry teflon cigarette ash plate on smoking machine ashtray, adjust smoking machine suction parameter according to GB/T16450 " smoking machine definition and standard conditions for conventional analysis ".Smoking cigarette on Borgwaldt-KCRM 20H smoking machine.After suction finishes, carefully take off cigarette ash plate, collect the cigarette ash of whole cigarette on pan paper, then cigarette ash is poured in counteracting tank.In counteracting tank, add successively 65% nitric acid 6mL, 37% hydrochloric acid 2mL and 30% hydrogen peroxide 1mL.Carry out micro-wave digestion by the program of clearing up shown in table 1.After being down to below 40 DEG C, microwave dissolver temperature takes out counteracting tank.Counteracting tank is put into temperature control electric heater, under 130 DEG C of conditions, catch up with acid 2～3 hours, when remaining liq volume 0.5～1mL, take out counteracting tank, be cooled to room temperature.Sample solution is transferred in 250 mL volumetric flasks, cleans counteracting tank 3～4 times with ultrapure water, cleaning fluid is all transferred in 250 mL volumetric flasks, uses ultrapure water constant volume, shakes up.
3. sample determination:
Open ICP-MS, after instrument stabilizer, draw Ce, Co, Li, Tl, the tuning liquid adjustment of Y instrument parameter, make the level of sensitivity and chaff interference in the reasonable scope.Absorption standard blank solution, 1 μ g/L, the 2 μ g/L, 5 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ g/L, 60 μ g/L, 100 μ g/L chromium, nickel, arsenic, selenium, cadmium, the plumbous hybrid standard working solution that prepare, add online interior mark, carry out ICP-MS mensuration.Taking constituent content to be measured with the ratio of corresponding internal standard element content as horizontal ordinate, element mass-to-charge ratio intensity to be measured is ordinate with the ratio of corresponding internal standard element mass-to-charge ratio intensity, sets up element standard working curve to be measured.Correction data is carried out to regretional analysis, obtain the regression equation of chromium, nickel, arsenic, selenium, cadmium, lead concentration relation.Sample solution and inner mark solution are measured simultaneously, bring regression equation with chromium, nickel, arsenic, selenium, cadmium, plumbous mass-to-charge ratio intensity in sample into the ratio of corresponding internal standard element mass-to-charge ratio intensity, through calculating, the content that obtains chromium in cigarette ash sample to be measured, nickel, arsenic, selenium, cadmium, lead, the results are shown in Table 8.
chromium, nickel, arsenic, selenium, cadmium, lead content testing result in table 8 cigarette sample A cigarette ash
| Element | Cr | Ni | As | Se | Cd | Pb |
| Content ng/cig) | 307.9 | 665.6 | 124.1 | 50.8 | 454.8 | 1189.4 |
Example 2:
As described in Example 1, cigarette sample B(strangles cigarette to concrete steps in vain), record the content of chromium in cigarette ash, nickel, arsenic, selenium, cadmium, lead in table 9.
chromium, nickel, arsenic, selenium, cadmium, lead content testing result in table 9 cigarette sample B cigarette ash
| 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, plumbous content in table 10.
chromium, nickel, arsenic, selenium, cadmium, lead content testing result in table 10 cigarette sample C cigarette ash
| 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, plumbous content in table 11.
chromium, nickel, arsenic, selenium, cadmium, lead content testing result in table 11 cigarette sample D cigarette ash
| Element | Cr | Ni | As | Se | Cd | Pb |
| Content (ng/cig) | 353.6 | 485.1 | 297.1 | 207.9 | 238.6 | 1374.0 |
Claims (7)
1. a detection method for chromium, nickel, arsenic, selenium, cadmium, lead element in cigarette ash, is characterized in that, comprises following processing step:
1) collection of cigarette ash, collects separately every cigarette ash;
2) micro-wave digestion, is placed in micro-wave diminishing pot by cigarette ash, adds nitric acid, hydrochloric acid and hydrogen peroxide solution successively in tank, puts into microwave dissolver and carries out micro-wave digestion;
3) catch up with acid cut to hold, Specimen eliminating liquid is heated and catches up with acid treatment, be then transferred in volumetric flask, use ultrapure water constant volume, obtain sample liquid to be measured;
4) preparation of standard operation solution, standard blank solution is 5% nitric acid, chromium, nickel, arsenic, selenium, cadmium, the plumbous hybrid standard working solution of the nitric acid preparation variable concentrations with 5%;
5) inductivity coupled plasma mass spectrometry is measured, draw the standard blank solution of certain volume and the chromium of variable concentrations, nickel, arsenic, selenium, cadmium, plumbous hybrid standard working solution, inject inductivity coupled plasma mass spectrometry, add online interior mark, under selected instrument parameter, with elemental chromium to be measured, nickel, arsenic, selenium, cadmium, lead content is horizontal ordinate with the ratio of corresponding internal standard element content, elemental chromium to be measured, nickel, arsenic, selenium, cadmium, plumbous mass-to-charge ratio intensity is ordinate with the ratio of corresponding internal standard element mass-to-charge ratio intensity, set up chromium, nickel, arsenic, selenium, cadmium, plumbous standard working curve, try to achieve chromium, nickel, arsenic, selenium, cadmium, the one-variable linear regression equation of lead concentration relation, R
2be greater than 0.999, add online interior mark to measure sample solution, bring chromium, nickel, arsenic, selenium, cadmium, plumbous mass-to-charge ratio intensity in sample into regression equation with the ratio of corresponding internal standard element mass-to-charge ratio intensity, calculate chromium, nickel, arsenic, selenium, cadmium, lead content in cigarette ash sample to be measured.
2. according to the assay method of chromium, nickel, arsenic, selenium, cadmium, lead content in the cigarette ash described in claims 1, it is characterized in that: in step 1), with every cigarette ash of teflon cigarette ash plate collection, the clean 20%HNO that passes through of cigarette ash plate
3more than soaking 48h, after ultrapure water rinses, use washed with methanol surface, dry.
3. according to the assay method of chromium, nickel, arsenic, selenium, cadmium, lead content in the cigarette ash described in claims 1, it is characterized in that: be that massfraction is 65% nitric acid, 37% hydrochloric acid and 30% hydrogen peroxide solution to the acid adding in micro-wave diminishing pot successively, nitric acid, hydrochloric acid, hydrogen peroxide volume are respectively 6mL, 2mL, 1mL.
4. according to the assay method of chromium, nickel, arsenic, selenium, cadmium, lead content in the cigarette ash described in claims 1, it is characterized in that: micro-wave digestion program is 5min to 100 DEG C of intensification, keep 5min, 5min to 160 DEG C of intensification, keep 5min, 5min to 190 DEG C of intensification, keeps 30min.
5. according to the assay method of chromium, nickel, arsenic, selenium, cadmium, lead content in the cigarette ash described in claims 1, it is characterized in that: catch up with acid temperature control electric heater used need join air draft dust cover, catch up with sour temperature the highest 130 DEG C.
6. according to the assay method of chromium, nickel, arsenic, selenium, cadmium, lead content in the cigarette ash described in claims 1, it is characterized in that: in adopting, mark is proofreaied and correct ICP-MS measuring process.
7. according to the assay method of chromium, nickel, arsenic, selenium, cadmium, lead content in the cigarette ash described in claims 1, it is characterized in that: the concentration of the chromium of described variable concentrations, nickel, arsenic, selenium, cadmium, plumbous hybrid standard working solution is respectively 1 μ g/L, 2 μ g/L, 5 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ g/L, 60 μ g/L, 100 μ g/L.
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| CN105823536A (en) * | 2016-04-15 | 2016-08-03 | 河南中烟工业有限责任公司 | Method for measuring adhesive consumption of cigarette lap adhesive by marker method |
| 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 |
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| CN105823536A (en) * | 2016-04-15 | 2016-08-03 | 河南中烟工业有限责任公司 | Method for measuring adhesive consumption of cigarette lap adhesive by marker method |
| 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 |
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| 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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