CN105758929B - The measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of matrix cigarette - Google Patents
The measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of matrix cigarette Download PDFInfo
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- CN105758929B CN105758929B CN201610134527.2A CN201610134527A CN105758929B CN 105758929 B CN105758929 B CN 105758929B CN 201610134527 A CN201610134527 A CN 201610134527A CN 105758929 B CN105758929 B CN 105758929B
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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
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- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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Abstract
The present invention provides the measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of matrix cigarette, includes the following steps：1）Sample pre-treatments：Matrix cigarette sample is weighed, after being cleared up using Microwave Digestion, then cooling, transfer, constant volume are to get sample solution；2）The preparation of standard solution：Prepare germanium72, indium115, bismuth209Inner mark solution and chromium, nickel, arsenic, selenium, cadmium, lead element standard solution；3）Sample solution, standard solution and inner mark solution are subjected to icp ms detection respectively, quantified using internal standard synchronization criterion curve method, the content of chromium, nickel, arsenic, selenium, cadmium, lead element in sample solution is obtained.The measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of matrix cigarette provided by the invention, related coefficient, the rate of recovery with it is reproducible, be conducive to tobacco business related technical personnel and effective quantitative determination control carried out to 6 Heavy Metallic Elements contents in matrix cigarette.
Description
Technical field
The invention belongs to chemical analysis detection technique fields, and in particular to chromium, nickel, arsenic, selenium, cadmium, lead in a kind of matrix cigarette
The measuring method of element.
Background technique
Chromium, nickel, arsenic, selenium, cadmium and lead are common heavy metal elements, are also listed in Hoffmann list in tobacco business
Harmful components have biggish harmfulness to the mankind and environment due to it in recent years, have obtained extensive concern and research.Matrix
Cigarette is a kind of a certain amount of tobacco extract, fragrance and some other edible addition to be added in the colloid for being similar to chewing gum
A kind of novel smokeless gas tobacco product made of agent.When chew take matrix cigarette when, matrix cigarette, which is put directly into oral cavity, to be chewed, wherein
Chromium, nickel, arsenic, selenium, cadmium, lead element can be absorbed by the body, to be caused to human body potentially hazardous.Therefore, it measures and grasps
The content of these heavy metal elements has great importance for the quality and safety metrics evaluation of matrix smoke product in matrix cigarette.
Chromium, nickel, arsenic, selenium, the cadmium, lead element being concentrated mainly in traditional tobacco and tobacco product are largely studied at present
Content analysis.Such as tobacco business standard YC/T380-2010《Tobacco and tobacco product chromium, nickel, arsenic, selenium, cadmium, lead measurement electricity
Feel coupled plasma mass》In define the measurement of chromium, nickel, arsenic, selenium, cadmium, lead content in traditional tobacco and tobacco product
Method.But matrix cigarette is as a kind of new tobacco products, because wherein containing special gum components, YC/T380-2010《Tobacco
And the measurement inductively coupled plasma mass spectrometry of tobacco product chromium, nickel, arsenic, selenium, cadmium, lead》In pre-treating method cannot will
Matrix cigarette resolution completely, for such sample analysis test have biggish limitation, therefore be not applied for chromium in matrix cigarette,
The measurement of nickel, arsenic, selenium, cadmium, lead element content.And standard GB/T/T5009.123-2014《The measurement of chromium in food》,GB/
T5009.138-2003《Nickel-silicon nitride in food》,GB/T5009.11-2003《The measurement of total Arsenic in Food and inorganic arsenic》,GB/
T5009.93-2010《The measurement of selenium in food》,GB/T5009.15-2014《The measurement of cadmium in foods》,GB/T5009.12-
2010《The measurement of Pb in food》The middle detection method for having respectively provided chromium in food, nickel, arsenic, selenium, cadmium, lead.But these standards
In detection method mainly have graphite furnace atomic absorption spectrometry, Hydride generation fluorescence spectrometry, colorimetric method, Singe-sweep polarography
Method, these method pre-treatments operation is relatively complicated, cannot realize the measurement of nickel in sample, arsenic, selenium, cadmium, lead content simultaneously, and extremely
The present without correlation test prove these methods whether suitable for matrix cigarette chromium, nickel, arsenic, selenium, cadmium, lead measurement.Therefore, one is established
Chromium in detection matrix cigarette while kind accurate and reliable, nickel, arsenic, selenium, cadmium, lead element content method have for tobacco business
It is significant.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide chromium in a kind of matrix cigarette, nickel, arsenic,
The measuring method of selenium, cadmium, lead element, for solve lack in the prior art accurately and reliably while detecting chromium in matrix cigarette, nickel,
Arsenic, selenium, cadmium, lead element content method the problem of.
In order to achieve the above objects and other related objects, the present invention provides chromium, nickel, arsenic, selenium, cadmium, lead in a kind of matrix cigarette
The measuring method of element, includes the following steps：
1) sample pre-treatments：Matrix cigarette sample is weighed, after being cleared up using Microwave Digestion, then cools down, transfer, determine
Hold to get sample solution；
Preferably, the sample pre-treatments also need to carry out blank assay.
Preferably, the blank assay is not place matrix cigarette sample, after being cleared up using Microwave Digestion, then it is cold
But, transfer, constant volume are to get blank solution.
Preferably, the Microwave Digestion is the method cleared up using microwave dissolver to matrix cigarette sample.It is described
Microwave dissolver is conventional use of micro-wave digestion equipment, and the microwave dissolver is furnished with micro-wave diminishing pot.
Preferably, the digestion agent that uses of the Microwave Digestion for nitric acid, hydrogen peroxide, hydrofluoric acid mixed aqueous solution.
Preferably, the digestion agent be 60-65% (percent by volume v/v) nitric acid, 20-30% (v/v) hydrogen peroxide,
The mixed aqueous solution of 30-40% (v/v) hydrofluoric acid.
It is highly preferred that 60-65% (v/v) nitric acid, 20-30% (v/v) hydrogen peroxide, 30-40% (v/ in the digestion agent
V) the ratio between addition volume of hydrofluoric acid is 5-12：2-6：1.
It is highly preferred that the digestion agent is 65% (v/v) nitric acid, 30% (v/v) hydrogen peroxide, 40% (v/v) hydrofluoric acid
Mixed aqueous solution.
It is further preferred that (v/v) nitric acid, 30% (v/v) hydrogen peroxide, 40% (v/v) hydrogen 65% in the digestion agent
The ratio between addition volume of fluoric acid is 5-10：2-4：1.
Most preferably, 65% (v/v) nitric acid, 30% (v/v) hydrogen peroxide, 40% (v/v) hydrofluoric acid in the digestion agent
The ratio between addition volume be 10：4：1.
Preferably, the solid-to-liquid ratio for the volume that the addition weight of the matrix cigarette sample is added with digestion agent is：0.03-
0.10：1(g/ml).
Preferably, the solid-to-liquid ratio for the volume that the addition weight of the matrix cigarette sample is added with digestion agent is：0.03-
0.05：1(g/ml).
Preferably, the temperature program of the Microwave Digestion is：Initial temperature is room temperature (20-25 DEG C), with 4-6min's
Heating-up time rises to 110-130 DEG C, keeps 4-6min；160-170 DEG C is risen to the heating-up time of 4-6min again, keeps 4-
6min；180-200 DEG C is risen to the heating-up time of 4-6min again, keeps 15-25min.
Preferably, the temperature program of the Microwave Digestion is：Initial temperature is room temperature (20-25 DEG C), with the liter of 5min
The warm time rises to 120 DEG C, keeps 5min；170 DEG C are risen to the heating-up time of 5min again, keeps 5min；Again with the heating of 5min
Time rises to 190 DEG C, keeps 20min.
Preferably, described be cooled to room temperature (20-25 DEG C).
Preferably, the transfer is that solution by sample after clearing up is transferred in dosing container.The dosing container is
Volumetric flask.
Preferably, when the transfer, digestion container is cleaned multiple times on a small quantity with cleaning solution, the cleaning solution is together
It is transferred in dosing container.
It is highly preferred that the cleaning solution is water.
Preferably, the constant volume is that constant volume is diluted with water in dosing container.
Above-mentioned with water is ultrapure water.
2) preparation of standard solution：Prepare germanium72, indium115, bismuth209Inner mark solution and chromium, nickel, arsenic, selenium, cadmium, lead element standard
Solution；
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；
Preferably, 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, germanium is weighed respectively72, indium115, bismuth209Standard substance solution prepares germanium with aqueous solution of nitric acid dilution and constant volume72、
Indium115, bismuth209Inner mark solution；
Preferably, the germanium72, indium115, bismuth209Inner mark solution is germanium72, indium115, bismuth209Mixing or single-element internal standard are molten
Liquid.
Preferably, the germanium72, indium115, bismuth209The concentration of mixing or single-element inner mark solution is 100-10000 μ g/
L。
It is highly preferred that the germanium72, indium115, bismuth209The concentration of mixing or single-element inner mark solution is 1000 μ g/L.
Preferably, the germanium72, indium115, bismuth209It mixes or the condition of storage of single-element inner mark solution is：Storage temperature：
0-4℃；Storage time：1 month.
C, 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 standard solution of a series of various concentrations.
Preferably, the chromium, nickel, arsenic, selenium, cadmium, lead element standard solution are chromium, nickel, arsenic, selenium, cadmium, lead mixing or single
Elemental standard solution.
Preferably, the concentration of volume percent of the aqueous solution of nitric acid is 1-10% (v/v).
Preferably, the concentration of volume percent of the aqueous solution of nitric acid is 5% (v/v).
The standard solution should cover sample concentration range, can be i.e. with i.e. use.
3) it measures：Sample solution, step 2) are prepared in step 1) standard solution and inner mark solution are subjected to inductance respectively
Couple plasma mass spectrometer (ICP-MS) detection, is quantified using internal standard synchronization criterion curve method, is obtained in sample solution
The content of chromium, nickel, arsenic, selenium, cadmium, lead element.
Preferably, the internal standard synchronization criterion curve method includes the following steps：
When the internal standard synchronization criterion curve method refers to that ICP-MS is measured, on-line synchronous is measured in standard solution neutralization
Solution is marked, standard working curve, and then on-line synchronous measurement inner mark solution and actual sample solution are obtained, so that it is real to measure acquisition
The method of border sample concentration.Due to ICP-MS instrument trait, inner mark solution and sample solution pass through two peristaltic pump tubes respectively, together
When synchronize online sample introduction, measured after sampling valve mixes, and the mode that is measured after sample is added in unconventional internal standard.
A, respectively by the chromium of various concentrations a series of in the C of step 2), nickel, arsenic, selenium, cadmium, lead element standard solution, step
2) germanium in B72, indium115, bismuth209Inner mark solution is synchronous to carry out ICP-MS detection, obtains respective element/corresponding internal standard element matter
Lotus specific strength than to the linear relationship of respective element/corresponding internal standard element mass concentration ratio, it is bent to draw the work of corresponding standard
The regression equation of respective element standard working curve is calculated in line.
Preferably, in the standard curve, using respective element/corresponding internal standard element mass-to-charge ratio intensity ratio as ordinate (Y
Axis), corresponding respective element/corresponding internal standard element mass concentration ratio is abscissa (X-axis).
Preferably, the respective element and the corresponding relationship 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.Concrete condition is shown in Table 1.
1 respective element quality measurement number of table, internal standard element table
| Element | Mass number | Internal standard element |
| Chromium | 52 | Germanium72 |
| Nickel | 60 | Germanium72 |
| Arsenic | 75 | Germanium72 |
| Selenium | 78 | Germanium72 |
| Cadmium | 111 | Indium115 |
| Lead | 208 | Bismuth209 |
B, by sample solution in step 1) and its blank solution, step 2) B in inner mark solution is synchronous carries out ICP-MS inspection
It surveys, by the respective element of acquisition/corresponding internal standard element mass-to-charge ratio intensity ratio, substitutes into respective element standard work in step a respectively
Make the regression equation of curve, and the known quality concentration of the corresponding inner mark solution according to synchronous detection, sample solution is calculated
The mass concentration of middle respective element.
Preferably, the icp ms (ICP-MS) are octupole bar collision/reaction in step 3)
Pond-icp ms (ORS-ICP-MS).
Preferably, the testing conditions of the ORS-ICP-MS are：Ion source：ICP source；Radio-frequency power (RF power)：1500-
1600W；RF matching voltage：1.7-1.9V；Cooling air：Argon gas, flow velocity：14.0-16.0L/min；Non-user setting；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
Gas, 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；Eight
Pole bar deflection voltage：- 19.0 to -17.0V；Energy is discriminated against：2.5-3.5V；Sample feeding rate：0.05-0.15rps；It repeats secondary
Number：2-5；Scanning mode：Sequence jumps peak.
It is highly preferred that the testing conditions of the ORS-ICP-MS are：Ion source：ICP source；Radio-frequency power (RF power)：
1550W；RF matching voltage：1.8V；Cooling air：Argon gas, flow velocity：15.0L/min；Non-user setting；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：4.3mL/min；
It is atomized room temperature：2.0℃；Atomization gas：Argon gas, flow velocity：1.15L/min；Octupole bar deflection voltage：-18.0V；Energy is discriminated against：
3.0V；Sample feeding rate：0.1rps；Number of repetition：3；Scanning mode：Sequence jumps peak.
As described above, in a kind of matrix cigarette of the invention chromium, nickel, arsenic, selenium, cadmium, lead element measuring method, using microwave
Resolution method to matrix cigarette carry out pre-treatment after, then using inductively coupled plasma mass spectrometry simultaneously measure chromium in matrix cigarette, nickel,
The content of arsenic, selenium, cadmium, lead element.The standard working curve coefficient R of the method for the present invention2>0.999,6 kind of element is averaged
The rate of recovery is between 85.0~116.4%, and for relative standard deviation (RSD) less than 5%, the rate of recovery and repeatability are satisfactory,
It can be effectively applied to chromium in matrix cigarette, nickel, arsenic, selenium, cadmium, lead element quantitative analysis measurement.The method of the present invention is conducive to tobacco row
Industry related technical personnel carry out effective quantitative determination control to 6 Heavy Metallic Elements contents in matrix cigarette, and produce for matrix cigarette
The evaluation of quality safety indexes provides strong technical support.
Detailed description of the invention
The process that Fig. 1 is shown as the measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of matrix cigarette of the invention is shown
It is intended to.
Specific embodiment
The present invention is further explained combined with specific embodiments below, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
The reagent and instrument that following embodiment uses are as follows：
1, reagent
Nitric acid (excellent pure grade, German Merck company)；Hydrogen peroxide (excellent pure grade, Sinopharm Chemical Reagent Co., Ltd.)；
Hydrofluoric acid (excellent pure grade, German Merck company)；Chromium, nickel, arsenic, selenium, cadmium, lead element hybrid standard substance solution (10mg/L, beauty
Agilent Science and Technology Ltd. of state)；Germanium72, indium115, bismuth209Element internal standard hybrid standard substance solution (100mg/L, the U.S.
Agilent Science and Technology Ltd.)；
2, instrument
The octupole 7700X bar collision/reaction tank-icp ms (the limited public affairs of U.S. Agilent science and technology
Department)；Milli-Q ultrapure water instrument (Millipore company of the U.S.)；MARS microwave dissolver (U.S. CE M company)
Embodiment 1
1, measuring method
1.1 sample pre-treatments
It accurately weighs matrix cigarette sample to be placed in micro-wave diminishing pot, sample weighting amount is accurate to 0.1mg, then to micro-wave diminishing pot
Middle addition digestion agent.Wherein, the solid-to-liquid ratio for the volume that the addition weight of the matrix cigarette sample is added with digestion agent is：0.03-
0.10：1(g/ml).The digestion agent is the mixed aqueous solution of nitric acid, hydrogen peroxide, hydrofluoric acid, specially 5-12ml60-65%
Nitric acid, 2-6ml 20-30% hydrogen peroxide, 1ml 30-40% hydrofluoric acid, preferably 5-10ml65% nitric acid, 2-4ml 30%
Hydrogen peroxide, 40% hydrofluoric acid of 1ml.Sealed digestion tank, is placed in microwave dissolver.
The temperature program of Microwave Digestion is set, specially：Initial temperature is room temperature (20-25 DEG C), with the liter of 4-6min
The warm time rises to 110-130 DEG C, keeps 4-6min；160-170 DEG C is risen to the heating-up time of 4-6min again, keeps 4-6min；
180-200 DEG C is risen to the heating-up time of 4-6min again, keeps 15-25min.
Sample after clearing up is cooled to room temperature (20-25 DEG C), is transferred in volumetric flask, is repeatedly rushed on a small quantity with ultrapure water
Counteracting tank is washed, flushing liquor is transferred in volumetric flask together, then with shaking up after ultrapure water constant volume constant volume, obtains sample solution.Meanwhile
Matrix cigarette sample is not placed, after being cleared up by above-mentioned the same terms progress Microwave Digestion, then cooling, transfer, constant volume, it obtains
Blank solution.
The preparation of 1.2 standard solution
Chromium, nickel, arsenic, selenium, cadmium, lead element standard substance solution are pipetted respectively, are diluted and are determined with 1-10% aqueous solution of nitric acid
Hold, prepares the single-element Standard Stock solutions of chromium, nickel, arsenic, selenium, cadmium, lead respectively.Alternatively, pipetting chromium, nickel, arsenic, selenium, cadmium, lead
Element hybrid standard substance solution prepares the mixing of chromium, nickel, arsenic, selenium, cadmium, lead with the dilution of 1-10% aqueous solution of nitric acid and constant volume
Elemental standards stock solution.The chromium, nickel, arsenic, selenium, cadmium, lead mix or the mass concentration of single-element Standard Stock solutions is equal
For 100-10000 μ g/L.Condition of storage can store 1 month under the conditions of 0-4 DEG C.
Germanium is pipetted respectively72, indium115, bismuth209Standard substance solution is matched respectively with the dilution of 1-10% aqueous solution of nitric acid and constant volume
Germanium processed72, indium115, bismuth209Single-element inner mark solution.Alternatively, pipetting germanium72, indium115, bismuth209Hybrid standard substance solution is used
The dilution of 1-10% aqueous solution of nitric acid and constant volume, prepare germanium72, indium115, bismuth209Complex element inner mark solution.The germanium72, indium115、
Bismuth209The concentration of mixing or single-element inner mark solution is 100-10000 μ g/L.Condition of storage can store up under the conditions of 0-4 DEG C
It deposits 1 month.
The single-element Standard Stock solutions for pipetting the chromium of different volumes, nickel, arsenic, selenium, cadmium, lead respectively, with 1-10% nitre
Aqueous acid dilution and constant volume prepare chromium, nickel, arsenic, selenium, cadmium, lead mixing or single-element standard solution.Alternatively, pipetting difference
The chromium of volume, nickel, arsenic, selenium, cadmium, lead complex element Standard Stock solutions matched with the dilution of 1-10% aqueous solution of nitric acid and constant volume
Chromium processed, nickel, arsenic, selenium, cadmium, lead complex element standard solution.The standard solution should cover sample concentration range, can be i.e. with i.e.
With.
The measurement of 1.3 samples
Sample solution, 1.2 standard solution prepared and inner mark solution in 1.1 are subjected to inductively coupled plasma constitution respectively
Spectrometer (ICP-MS) detection, 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 the chromium of various concentrations a series of in 1.2, nickel, arsenic, selenium, cadmium, lead element standard solution, germanium72、
Indium115, bismuth209Element inner mark solution is synchronous to carry out ICP-MS detection, obtains respective element/corresponding internal standard element mass-to-charge ratio intensity
Than to the linear relationship of respective element/corresponding internal standard element mass concentration ratio, with respective element/corresponding internal standard element matter lotus
Specific strength ratio is ordinate (Y-axis), and corresponding respective element/corresponding internal standard element mass concentration ratio is abscissa (X
Axis) corresponding standard working curve is drawn, the regression equation of respective element standard working curve is calculated.
Element determination parameter is set by table 1.Specifically, the corresponding relationship of the respective element and 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.
ICP-MS detection is carried out by inner mark solution in sample solution in 1.1 and its blank solution, 1.2 is synchronous again, will be obtained
Respective element/corresponding internal standard element mass-to-charge ratio intensity ratio, substitute into the regression equation of respective element standard working curve respectively,
And the known quality concentration of the corresponding inner mark solution according to synchronous detection, the quality that respective element in sample solution is calculated are dense
Degree, i.e., the content of chromium, nickel, arsenic, selenium, cadmium, lead element in acquisition sample solution.
Wherein, the icp ms (ICP-MS) are octupole bar collision/reaction tank-inductive coupling etc.
Gas ions mass spectrograph (ORS-ICP-MS).
The testing conditions of ORS-ICP-MS described in the ORS-ICP-MS are：Ion source：ICP source；Radio-frequency power (RF function
Rate)：1500-1600W；RF matching voltage：1.7-1.9V；Cooling air：Argon gas, flow velocity：14.0-16.0L/min；Non-user is set
It is fixed；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
Pond 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；Octupole bar deflection voltage：- 19.0 to -17.0V；Energy is discriminated against：2.5-3.5V；Sample feeding rate：0.05-
0.15rps；Number of repetition：2-5；Scanning mode：Sequence jumps peak.
Embodiment 2
1, measuring method
1.1 sample pre-treatments
It accurately weighs matrix cigarette sample to be placed in micro-wave diminishing pot, sample weighting amount is accurate to 0.1mg, then to micro-wave diminishing pot
Middle addition digestion agent.Wherein, the solid-to-liquid ratio for the volume that the addition weight of the matrix cigarette sample is added with digestion agent is：0.03-
0.05：1(g/ml).The digestion agent be nitric acid, hydrogen peroxide, hydrofluoric acid mixed aqueous solution, specially 5ml65% nitric acid,
30% hydrogen peroxide of 2ml, 0.5ml40% hydrofluoric acid, are placed in microwave dissolver.
The temperature program of Microwave Digestion is set, specially：Initial temperature is room temperature (20-25 DEG C), with the heating of 5min
Time rises to 120 DEG C, keeps 5min；170 DEG C are risen to the heating-up time of 5min again, keeps 5min；When again with the heating of 5min
Between rise to 190 DEG C, keep 20min.Specifically it is shown in Table 2.
2 micro-wave digestion temperature program of table
Sample after clearing up is cooled to room temperature (20-25 DEG C), is transferred in 50mL polypropylene volumetric flask, uses ultrapure water
A small amount of repeatedly to rinse counteracting tank, flushing liquor is transferred to together in 50mL polypropylene volumetric flask, then with ultrapure water constant volume constant volume 50mL
After shake up, obtain sample solution.Meanwhile matrix cigarette sample is not placed, Microwave Digestion, which is carried out, by above-mentioned the same terms disappears
Xie Hou, then cooling, transfer, constant volume, obtain blank solution.
The preparation of 1.2 standard solution
Chromium, nickel, arsenic, selenium, cadmium, lead element hybrid standard substance solution are pipetted, dilutes simultaneously constant volume with 5% aqueous solution of nitric acid,
Prepare the complex element Standard Stock solutions of chromium, nickel, arsenic, selenium, cadmium, lead.The chromium, nickel, arsenic, selenium, cadmium, lead complex element mark
The mass concentration of quasi- stock solution is 1000 μ g/L.Condition of storage can store 1 month under the conditions of 0-4 DEG C.
Pipette germanium72, indium115, bismuth209Hybrid standard substance solution prepares germanium with the dilution of 5% aqueous solution of nitric acid and constant volume72、
Indium115, bismuth209Complex element inner mark solution.The germanium72, indium115, bismuth209The concentration of complex element inner mark solution is 1000 μ g/
L.Condition of storage can store 1 month under the conditions of 0-4 DEG C.
The complex element Standard Stock solutions for pipetting the chromium of different volumes, nickel, arsenic, selenium, cadmium, lead, with 5% aqueous solution of nitric acid
Simultaneously constant volume is diluted, the complex element standard solution of chromium, nickel, arsenic, selenium, cadmium, lead is prepared.The standard solution should cover sample concentration
Range, can be i.e. with i.e. use.Specific concentration range is shown in Table 3.
3 standard solution of table is with tabulation (unit：μg/L)
| Serial number | Chromium | Nickel | Arsenic | Selenium | Cadmium | Lead |
| Lv1 | 0 (reagent blank) | 0 (reagent blank) | 0 (reagent blank) | 0 (reagent blank) | 0 (reagent blank) | 0 (reagent blank) |
| Lv2 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Lv3 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| Lv4 | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 |
| Lv5 | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 | 3.0 |
| Lv6 | 5.0 | 5.0 | 5.0 | 5.0 | 5.0 | 5.0 |
| Lv7 | 10.0 | 10.0 | 10.0 | 10.0 | 10.0 | 10.0 |
| Lv8 | 15.0 | 15.0 | 15.0 | 15.0 | 15.0 | 15.0 |
The measurement of 1.3 samples
Sample solution, 1.2 standard solution prepared and inner mark solution in 1.1 are subjected to inductively coupled plasma constitution respectively
Spectrometer (ICP-MS) detection, 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 the chromium of various concentrations a series of in 1.2, nickel, arsenic, selenium, cadmium, lead element standard solution, germanium72、
Indium115, bismuth209Element inner mark solution is synchronous to carry out ICP-MS detection, obtains respective element/corresponding internal standard element mass-to-charge ratio intensity
Than to the linear relationship of respective element/corresponding internal standard element mass concentration ratio, with respective element/corresponding internal standard element matter lotus
Specific strength ratio is ordinate (Y-axis), and corresponding respective element/corresponding internal standard element mass concentration ratio is abscissa (X
Axis) corresponding standard working curve is drawn, the regression equation of respective element standard working curve is calculated.
Element determination parameter is set by table 1.Specifically, the corresponding relationship of the respective element and 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.
ICP-MS detection is carried out by inner mark solution in sample solution in 1.1 and its blank solution, 1.2 is synchronous again, will be obtained
Respective element/corresponding internal standard element mass-to-charge ratio intensity ratio, substitute into the regression equation of respective element standard working curve respectively,
And the known quality concentration of the corresponding inner mark solution according to synchronous detection, the quality that respective element in sample solution is calculated are dense
Degree, i.e., the content of chromium, nickel, arsenic, selenium, cadmium, lead element in acquisition sample solution.
Wherein, the icp ms (ICP-MS) are octupole bar collision/reaction tank-inductive coupling etc.
Gas ions mass spectrograph (ORS-ICP-MS).
The testing conditions of the ORS-ICP-MS are：Ion source：ICP source；Radio-frequency power (RF power)：1550W；RF matching
Voltage：1.8V；Cooling air：Argon gas, flow velocity：15.0L/min；Non-user setting；Carrier gas：Argon gas, flow velocity：0.85L/min；Carrier gas
Compensate gas：Argon gas, flow velocity：0.3L/min；Collision/reaction tank gas：Helium, flow velocity：4.3mL/min；It is atomized room temperature：2.0
℃；Atomization gas：Argon gas, flow velocity：1.15L/min；Octupole bar deflection voltage：-18.0V；Energy is discriminated against：3.0V；Sample feeding speed
Rate：0.1rps；Number of repetition：3；Scanning mode：Sequence jumps peak.
Embodiment 3
1, results and discussion
The selection of 1.1 digestion solutions
Matrix cigarette sample is added in blank solution, selects digestion agent 1 respectively：65% nitric acid, 30% hydrogen peroxide, 40%
(the ratio between volume is 10 to hydrofluoric acid：4：1)；Digestion agent 2：65% nitric acid, 30% hydrogen peroxide (the ratio between volume 5：2)；Digestion agent 3：
65% nitric acid, 30% hydrogen peroxide, 35% hydrochloric acid (the ratio between volume 5:2:1).Microwave is carried out by 1.1 rated conditions in embodiment 2
Resolution, and cooling, transfer, constant volume, obtain sample solution.Blank assay is carried out by 1.1 rated conditions in embodiment 2 simultaneously, is obtained
Obtain blank solution.Further according in embodiment 2 1.2 standard solution and inner mark solution, finally detected respectively with ICP-MS,
ICP-MS testing conditions are shown in that 1.3 in embodiment 2, specific testing result is shown in Table 4.It is compared by table 4 it is found that when selecting digestion agent 1,
Testing result value of 6 kinds of elements after ICP-MS is detected is optimal in matrix cigarette sample, can clear up completely matrix cigarette sample.
The testing result of the different digestion agents of table 4 compares
| Detection elements | Digestion agent 1 (mg/kg) | Digestion agent 2 (mg/kg) | Digestion agent 3 (mg/kg) |
| Chromium | 0.66 | 0.52 | 0.56 |
| Nickel | 0.58 | 0.44 | 0.51 |
| Arsenic | 0.11 | 0.08 | 0.07 |
| Selenium | 0.09 | 0.07 | 0.08 |
| Cadmium | 0.23 | 0.14 | 0.16 |
| Lead | 0.29 | 0.23 | 0.23 |
The selection of 1.2 micro-wave digestion temperature programs
Matrix cigarette sample is added in blank solution, selection digestion agent is：65% nitric acid, 30% hydrogen peroxide, 40% hydrogen
(the ratio between volume is 10 to fluoric acid：4：1) different micro-wave digestion temperature programs, is selected to be cleared up respectively.
Wherein, it is room temperature (20-25 DEG C) that temperature program 1, which is initial temperature, and initial temperature is room temperature (20-25 DEG C), with
The heating-up time of 5min rises to 120 DEG C, keeps 5min；170 DEG C are risen to the heating-up time of 5min again, keeps 5min；Again with
The heating-up time of 5min rises to 190 DEG C, keeps 20min.
Temperature program 2：Initial temperature is room temperature (20-25 DEG C), rises to 120 DEG C with the heating-up time of 5min, keeps 5min；
170 DEG C are risen to the heating-up time of 5min again, keeps 20min.
Temperature program 3：Initial temperature is room temperature (20-25 DEG C), rises to 120 DEG C with the heating-up time of 5min, keeps 5min；
170 DEG C are risen to the heating-up time of 5min again, keeps 5min；210 DEG C are risen to the heating-up time of 5min again, keeps 20min.
Cooling after resolution, transfer, constant volume, obtain sample solution.Blank is carried out by 1.1 rated conditions in embodiment 2 simultaneously
Experiment obtains blank solution.Further according in embodiment 2 1.2 standard solution and inner mark solution, finally carried out respectively with ICP-MS
Detection, ICP-MS testing conditions are shown in that 1.3 in embodiment 2, specific testing result is shown in Table 5.It is compared by table 5 it is found that when selecting heating
When program 1, the digestion condition of selection is best, and testing result value of 6 kinds of elements after ICP-MS is detected be most in matrix cigarette sample
It is excellent, matrix cigarette sample can be cleared up completely.
The testing result of the different micro-wave digestion temperature programs of table 5 compares
| Detection elements | Temperature program 1 (mg/kg) | Temperature program 2 (mg/kg) | Temperature program 3 (mg/kg) |
| Chromium | 0.69 | 0.56 | 0.68 |
| Nickel | 0.55 | 0.50 | 0.53 |
| Arsenic | 0.13 | 0.12 | 0.13 |
| Selenium | 0.14 | 0.13 | 0.13 |
| Cadmium | 0.27 | 0.28 | 0.27 |
| Lead | 0.32 | 0.29 | 0.30 |
Embodiment 4
1, standard working curve, detection limit and quantitative limit
It is molten by a series of in embodiment 2 1.2 chromium that are formulated as various concentrations, nickel, arsenic, selenium, cadmium, the complex element standard of lead
Liquid, specific concentration range are shown in Table 3.Meanwhile germanium is prepared by embodiment 2 1.272, indium115, bismuth209Complex element inner mark solution.
A series of standard solution of above-mentioned prepared various concentrations and inner mark solution are pressed respectively 1.3 in embodiment 2
Regulation, it is synchronous to carry out ORS-ICP-MS detection, using respective element/corresponding internal standard element mass-to-charge ratio intensity ratio as ordinate (Y
Axis), corresponding respective element/corresponding internal standard element mass concentration ratio is abscissa (X-axis), carries out regression analysis, obtains
To regression equation and its related coefficient, as shown in table 6.
As shown in Table 6, the linear relationship of regression equation is good, coefficient R2>0.999.To the target in standard solution
Object response signal is repeated sample introduction 10 times using minimum concentration standard specimen, carries out ORS-ICP-MS analysis, is inspection with its 3 times of standard deviations
Rising limit (LOD), 10 times of standard deviations are quantitative limit (LOQ), be scaled after sample size obtain object detection be limited to 0.004~
0.015mg/kg, quantitative limit is in 0.014~0.048mg/kg, sensitivity with higher.
6 working curve of table and detection limit
| Element | Standard curve | Related coefficient (R2) | Detection limit (mg/kg) | Quantitative limit (mg/kg) |
| Chromium | Y=0.0618x+0.0059 | >0.999 | 0.008 | 0.028 |
| Nickel | Y=0.0297x+0.0036 | >0.999 | 0.008 | 0.026 |
| Arsenic | Y=0.0056x+3.9017 × 10-5 | >0.999 | 0.010 | 0.034 |
| Selenium | Y=4.6904*10-4x+9.4775×10-5 | >0.999 | 0.015 | 0.048 |
| Cadmium | Y=0.0016x+2.9040 × 10-6 | >0.999 | 0.004 | 0.014 |
| Lead | Y=0.0078x+4.5318 × 10-4 | >0.999 | 0.005 | 0.016 |
y：Mass-to-charge ratio intensity ratio；x：Concentration ratio
2, the rate of recovery and precision
Respectively in the matrix cigarette sample of known concentration, chromium, nickel, arsenic, selenium, the cadmium, lead element standard of known concentration is added
Solution carries out sample pre-treatments and ORS-ICP-MS is analyzed, and according to scalar quantity and measured value by testing conditions in embodiment 2
Its rate of recovery is calculated, while 6 times (n=6) is measured in parallel to same sample solution, precision determination data is obtained, the results are shown in Table
7.As can be seen from Table 7, between 85.0~116.4%, relative standard deviation (RSD) is less than the average recovery rate of object
5%, illustrate that the rate of recovery of the method for the present invention and repeatability are satisfactory, is able to satisfy detection needs completely.
7 the method for the present invention rate of recovery of table and precision
Embodiment 5
1, the measurement of actual sample
Using the testing conditions of embodiment 2 in the method for the present invention, to chromium, nickel, arsenic, selenium, cadmium, lead in practical matrix cigarette sample
The content of element is measured, and is specifically shown in Table 8.As shown in Table 8, for matrix cigarette sample, this method can effectively measure its chromium,
The content of nickel, arsenic, selenium, cadmium, lead element, method is easy to operate, applicability is good, as a result accurately, reliably.
8 actual sample testing result (unit of table：mg/kg)
| Serial number | Chromium | Nickel | Arsenic | Selenium | Cadmium | Lead |
| 1 | 0.54 | 0.50 | 0.04 | 0.05 | 0.04 | 0.08 |
| 2 | 0.33 | 0.46 | 0.09 | 0.06 | 0.13 | 0.21 |
| 3 | 0.62 | 0.55 | 0.12 | 0.10 | 0.21 | 0.31 |
So the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (6)
1. the measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element, includes the following steps in a kind of matrix cigarette：
1) sample pre-treatments：Matrix cigarette sample is weighed, after being cleared up using Microwave Digestion, then cooling, transfer, constant volume, i.e.,
Obtain sample solution；
2) preparation of standard solution：Prepare germanium72, indium115, bismuth209Inner mark solution and chromium, nickel, arsenic, selenium, cadmium, lead element standard are molten
Liquid；
3) it measures：Sample solution, step 2) are prepared in step 1) standard solution and inner mark solution are subjected to inductive coupling respectively
Plasma mass spectrograph detection, quantify using internal standard synchronization criterion curve method, acquisition sample solution in chromium, nickel, arsenic, selenium,
The content of cadmium, lead element；
In step 1), the digestion agent that the Microwave Digestion uses is 60-65% nitric acid, 20-30% hydrogen peroxide, 30-40%
The mixed aqueous solution of hydrofluoric acid；
The ratio between addition volume of 60-65% nitric acid, 20-30% hydrogen peroxide, 30-40% hydrofluoric acid is 5- in the digestion agent
12：2-6：1；
In step 1), the solid-to-liquid ratio for the volume that the addition weight of the matrix cigarette sample is added with digestion agent is：0.03-0.10：
1；
In step 1), the temperature program of the Microwave Digestion is：Initial temperature is room temperature, is risen to the heating-up time of 4-6min
110-130 DEG C, keep 4-6min；160-170 DEG C is risen to the heating-up time of 4-6min again, keeps 4-6min；Again with 4-6min
Heating-up time rise to 180-200 DEG C, keep 15-25min.
2. the measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in matrix cigarette according to claim 1, which is characterized in that
In step 2), the preparation of the standard solution includes 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 germanium) is weighed respectively72, indium115, bismuth209Standard substance solution prepares germanium with aqueous solution of nitric acid dilution and constant volume72, indium115、
Bismuth209Inner mark solution；
C 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 solution of a series of various concentrations.
3. the measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in matrix cigarette according to claim 1, which is characterized in that
In step 3), the internal standard synchronization criterion curve method includes the following steps：
A) respectively by chromium, nickel, arsenic, selenium, cadmium, lead element standard solution, the germanium 72, indium in step 2) in step 2)115, bismuth209It is interior
The synchronous progress ICP-MS detection of solution is marked, respective element/corresponding internal standard element mass-to-charge ratio intensity ratio and respective element/phase are obtained
The linear relationship for answering the mass concentration ratio of internal standard element draws corresponding standard working curve, and respective element standard is calculated
The regression equation of working curve；
B) carry out ICP-MS detection for inner mark solution in sample solution in step 1), step 2) is synchronous, by the respective element of acquisition/
The mass-to-charge ratio intensity ratio of corresponding internal standard element substitutes into the regression equation of respective element standard working curve in step a) respectively, and
According to the known quality concentration of the corresponding inner mark solution of synchronous detection, the quality that respective element in sample solution is calculated is dense
Degree.
4. the measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in matrix cigarette according to claim 3, which is characterized in that
The respective element and the corresponding relationship of corresponding internal standard element are：Chromium corresponds to germanium72Internal standard element；Nickel element corresponds to germanium72It is interior
Mark 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.
5. the measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in matrix cigarette according to claim 1, which is characterized in that
In step 3), the icp ms are octupole bar collision/reaction tank-inductivity coupled plasma mass spectrometry
Instrument.
6. the measuring method of chromium, nickel, arsenic, selenium, cadmium, lead element in matrix cigarette according to claim 5, which is characterized in that
The testing conditions of the ORS-ICP-MS are：Ion source：ICP source；Radio-frequency power：1500-1600W；RF matching voltage：1.7-
1.9V；Cooling air：Argon gas, flow velocity：14.0-16.0L/min；Non-user setting；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；Octupole bar deflection voltage：-19.0
To -17.0V；Energy is discriminated against：2.5-3.5V；Sample feeding rate：0.05-0.15rps；Number of repetition：2-5；Scanning mode：It is suitable
Sequence jumps peak.
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