CN101294896A - Method for measuring cadmium content in smoke tipping paper - Google Patents
Method for measuring cadmium content in smoke tipping paper Download PDFInfo
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- CN101294896A CN101294896A CNA2008100501033A CN200810050103A CN101294896A CN 101294896 A CN101294896 A CN 101294896A CN A2008100501033 A CNA2008100501033 A CN A2008100501033A CN 200810050103 A CN200810050103 A CN 200810050103A CN 101294896 A CN101294896 A CN 101294896A
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Abstract
A method for detecting cadmium content in cigarette used tipping paper is characterized in that the method can quickly and accurately detect the cadmium content in the cigarette used tipping paper by the following steps: adopting mixed acid to carry out microwave digestion for a sample, removing the acid and fixing volume, conducting detection with a graphite furnace atomic absorption spectrophotometer, etc. The method overcomes the shortcoming of the prior art in processing the sample. Compared with the traditional electric heating plate digestion manner, the microwave digestion manner can reduce the usage of samples and strong acid, improve digestion ability, cause less loss to elements to be detected in the sample and less damage to an operator, and facilitate operation. The digestion system of compound acid is completely applicable to the special material of the cigarette used tipping paper. The acid removing process is quick and easy, and a matrix modifier is adopted to eliminate interference. After being detected by optimal heating programs, ashing temperature and atomization temperature related to atomic absorption spectrometry, the special material of the cigarette used tipping paper is recovered with high rate, and detected with accurate result. The working efficiency and the economic benefits are significantly improved.
Description
Technical field:
The invention belongs to the physical and chemical inspection technical field of cigarette tipping paper, relate generally to the determination of trace element technical field of cigarette tipping paper, is a kind of method that adopts graphite furnace atomic absorption spectrophotometer directly to measure cadmium content in the cigarette tipping paper specifically.
Background technology:
According to the requirement of China's health legislation, all should carry out the safety and sanitation inspection for the various products of direct contact human oral cavity.Along with the concern of people to smoking and health problem, the safety of smoking material, health, environmental issue more and more obtain the attention of each side.Wherein, content of beary metal more and more causes now both at home and abroad and pays close attention to widely as one of safety indexes.But, still find no at present and close the bibliographical information that detects the quantivative approach of heavy metal cadmium content in the cigarette tipping paper.
China is to the national proposed standard of the content of cadmium general employing to be detected: the mensuration of cadmium in GB/T 5009.15 food.Select certain several brand cigarette tipping paper, utilize said method, the data after measuring are as shown in table 1 below:
The content of cadmium in certain several brand cigarette tipping paper of table 1
Annotate: the content of cadmium adopts national proposed standard: GB/T 5009.15 to measure in the cigarette tipping paper.
From The above results, adopt the cadmium result error of national proposed standard test bigger for same sample, parallel result is undesirable.Its reason: the one, the composition more complicated of cigarette tipping paper sample, contain a large amount of silicon magnesium oxides, ferriferous oxide, titanium oxide or the like, be difficult to clear up composition, when therefore detecting according to proposed standard, the cigarette tipping paper sample can not be cleared up fully, solution is muddy also to have a large amount of sediments, and color is arranged, and the mensuration of cadmium content has been formed more interference; The 2nd, catch up with sour condition, condition determination inapplicable after clearing up, need be to the relevant heating schedule of atomization process, ashing temperature, conditions such as atomization temperature are optimized again to be determined.Therefore, if adopt the content of cadmium in national proposed standard: the GB/T 5009.15 mensuration cigarette tipping paper samples, just can not truly reflect the content of cadmium in the cigarette tipping paper sample, therefore above-mentioned national standard can not be suitable for.
Summary of the invention:
Purpose of the present invention is intended to overcome the prior art defective, a kind of method that adopts graphite furnace atomic absorption spectrophotometer to measure cadmium content in the cigarette tipping paper is provided, this method can fast, accurately detect the content of cadmium in the cigarette tipping paper, and measurement result is accurate, mensuration is disturbed few.
The objective of the invention is to be achieved through the following technical solutions: the assay method of cadmium content in the cigarette tipping paper is characterized in that comprising following processing step:
A, micro-wave digestion place the micro-wave digestion jar with the cigarette tipping paper sample, add nitric acid, hydrofluorite, hydrochloric acid and superoxol successively, put into microwave dissolver then and carry out micro-wave digestion;
B, catch up with acid cut to hold, counteracting tank is heated, catch up with acid treatment, after finishing sample solution is moved in the container,, be sample liquid to be measured with 1% nitric acid constant volume;
C, preparation standard blank solution: 1% nitric acid, the cadmium standard operation solution of preparation variable concentrations;
D, graphite furnace atomic absorption spectrophotometer are measured, the cadmium standard operation solution of absorption standard blank solution and the variable concentrations for preparing, with ammonium dihydrogen phosphate and magnesium nitrate solution is that matrix modifier injects graphite furnace, record its absorbance peak area and try to achieve the absorbance peak area and the one-variable linear regression equation of cadmium concentration relation, related coefficient is more than or equal to 0.99, sample liquid to be measured after clearing up is measured, record the absorbance peak area of cadmium, substitution one-variable linear regression equation is tried to achieve the cadmium content in the sample liquid to be measured.
In the present invention, the nitric acid of Jia Ruing, hydrofluorite, hydrochloric acid and superoxol amount volume ratio are nitric acid successively: hydrofluorite: hydrochloric acid: hydrogen peroxide=5: 1: 1: 1, and wherein concentration of nitric acid 65%, hydrofluoric acid concentration 40%, concentration of hydrochloric acid 37%, concentration of hydrogen peroxide 30%.
Micro-wave digestion heating schedule described in the present invention is: 5min to 120 ℃ of intensification, keep 5min, and 5min to 160 ℃ of intensification keeps 5min, and 5min to 200 ℃ of intensification keeps 25min.
The heating-up temperature of catching up with sour process among the present invention is 150 ℃.
The used atomic absorption spectrometry condition of the present invention is: wavelength 228.8nm; The wide 0.7nm of slit, 550 ℃ of ashing temperature, 1500 ℃ of atomization temperatures.
The concentration of the ammonium dihydrogen phosphate that is added in the steps d is 10g/L, addition 5 μ L, and magnesium nitrate solution concentration is 1g/L, addition 3 μ L.
Why select ammonium dihydrogen phosphate (ADP) and magnesium nitrate as matrix modifier, be because magnesium nitrate generates magnesium oxide at a certain temperature and tested element forms chelate, thereby improved the ashing temperature.Ammonium root in the ammonium dihydrogen phosphate (ADP) exists, and can generate ammonium chloride and can spend decomposition 380, disturbs thereby reduce various muriatic matrixes; The existence of the phosphate radical in the ammonium dihydrogen phosphate (ADP) makes element to be measured at intensification initial stage and its generation phosphate, and the back of heating up generates and contains oxygen phosphoric acid complex compound, be bonded on the graphite-pipe surface, thereby reduce the volatile grade of element to be measured, improved the ashing temperature, help the volatilization of matrix.
The concrete technological process of the present invention is described in further detail as follows:
1 micro-wave digestion sample
Accurately take by weighing (0.2～0.5) g sample, be accurate to 0.0001g, place the micro-wave digestion jar, in the micro-wave digestion jar, add successively an amount of acid mixture (nitric acid: hydrofluorite: hydrochloric acid: hydrogen peroxide=5: 1: 1: the 1) microwave dissolver of packing into after the sealing, carry out micro-wave digestion by the program of clearing up shown in the table 2.
Table 2 micro-wave digestion heating schedule
Clear up and finish, treat that the microwave dissolver temperature reduces to back below 40 ℃ and take out counteracting tank.
Annotate: blank sample, be and do not add sample, add the solution that acid mixture is cleared up the back gained.
2 catch up with acid cut to hold
Counteracting tank is put into the temperature control electric heater, under 150 ℃ of conditions, catch up with acid 2～3 hours, be evaporated near doing.Catch up with acid to finish, sample solution is transferred in the 50mL plastics volumetric flask, wash counteracting tank 3～4 times with 1% nitric acid, cleaning fluid is transferred in the 50mL volumetric flask equally, uses 1% nitric acid constant volume then, and it is to be measured to shake up the back.
3 graphite furnace atomic absorption spectrophotometers are measured
(1) graphite furnace atomic absorption spectrophotometer parameter
Atomic Absorption Spectrometer is then adopted mensuration absorption value and background absorption value under different ashing and atomization temperature, and optimized conditions is final experiment condition, as table 3.
Table 3 atomic absorption spectrometry condition
(2) preparation of cadmium standard operation solution:
The standard blank solution is 1% used nitric acid of constant volume cadmium standard operation solution.
The cadmium standard reserving solution 10.0mg/L that accurately pipettes different volumes is to different plastics volumetric flasks, and the nitric acid with 1% dilutes constant volume, obtains the cadmium standard operation solution of variable concentrations, and its concentration range should cover expectation detected cadmium content in sample.
(3) mensuration of cadmium content
Each 20 μ L of cadmium standard operation solution of absorption standard blank solution and the variable concentrations for preparing, ammonium dihydrogen phosphate 5 μ L and magnesium nitrate solution 3 μ L inject graphite furnace, record its absorbance peak area and try to achieve the absorbance peak area and the one-variable linear regression equation of cadmium concentration relation, related coefficient is more than or equal to 0.99.Sample after clearing up is measured, recorded the absorbance peak area of cadmium, substitution one-variable linear regression equation is tried to achieve the cadmium content in reagent blank liquid and the test liquid.
(4) detection limit of the inventive method:
Clear up 10 blank samples simultaneously, catch up with acid cut to hold after, use these 10 blank sample values of atomic absorption spectrometry then, calculate its deviation, 3 times of detection limits as this element with deviate the results are shown in Table 4.
The detection limit of table 4 heavy metal element cadmium
Annotate: detection limit mg/kg with sample weighing 0.2g, is settled to 50mL and calculates.
(5) repeatability of the inventive method and recovery of standard addition:
To cigarette tipping paper, to measure simultaneously six times, the repeatability of computing method the results are shown in Table 5.Then according to the content of cadmium in the actual sample that has recorded, we adopt equivalent to add the target method tipping pattern product are carried out recovery of standard addition to test, the results are shown in Table 6.
Table 5 sample repeated experiment result (mg/kg of unit)
The recovery of standard addition of cadmium in table 6 sample
Method of the present invention has overcome the deficiency of prior art sample treatment, has optimized the relevant heating schedule of atomic absorption spectrography (AAS), ashing temperature, atomization temperature at the cigarette tipping paper sample.Compared with prior art the inventive method has following excellent results:
1. with traditional electric hot plate digestion method relatively, ability is cleared up in use amount, the raising of adopting the micro-wave digestion mode can reduce sample and strong acid, and sample element loss to be measured few, operating personnel are endangered little, easy operating.To this special material of cigarette tipping paper, the system of clearing up of compound acid is suitable fully.Digestion solution clarification, transparent, precipitation not.
2. few owing to clearing up the sample agents useful for same, catch up with sour process simple fast, the recovery height of determining of catching up with 150 ℃ of sour temperature, the blank value value is low, and measurement result is accurate.
3. adopt matrix modifier to eliminate interference.
4. at this special material of cigarette tipping paper, adopt the relevant heating schedule of the atomic absorption spectrography (AAS) of optimizing, the ashing temperature, after atomization temperature is measured, recovery height, measurement result is accurate.
5. this method has the advantage of easy and simple to handle, quick, accurate, sensitivity and good reproducibility.
Description of drawings
Fig. 1 is assay method process flow diagram of the present invention (this figure is as Figure of abstract).
Fig. 2 catches up with acid in different temperatures, to the influence of sample recovery rate.
Fig. 3 utilizes Atomic Absorption Spectrometer, has optimized the ashing temperature of cadmium, and the ashing temperature of measuring cadmium is 550 ℃.
Fig. 4 utilizes Atomic Absorption Spectrometer, has optimized the atomization temperature of cadmium.The atomization temperature of measuring cadmium is 1500 ℃.
Embodiment
The present invention is described further below in conjunction with example, but is not restriction the present invention.
The assay method of cadmium in a kind of cigarette tipping paper, its test process are the cigarette tipping paper samples that will take by weighing, and after usefulness acid mixture (nitric acid, hydrofluorite, hydrochloric acid and hydrogen peroxide) is cleared up processing, use 1% nitric acid dissolve, and constant volume are to certain volume.Draw an amount of sample liquid and matrix modifier in graphite furnace atomizer, drying, ashing, atomization.Under selected instrument parameter, element cadmium absorbing wavelength to be measured is the resonance line of 228.8nm, and its absorbance is directly proportional with cadmium content, and is more quantitative with standard series.
Example 1:
1. instrument and reagent: plastics volumetric flask, 50mL.Analytical balance, sensibility reciprocal 0.0001g.Polytetrafluoroethylene beaker, 100mL.Closed microwave counteract appearance (joining the micro-wave digestion jar).The temperature control electric heater.Graphite furnace atomic absorption spectrophotometer.Water, the redistilled water of ultrapure water or equal purity.Nitric acid, 65%.Nitric acid, 1%.Hydrogen peroxide, 30%.Hydrochloric acid, 37%.Hydrofluorite, 40%.Ammonium dihydrogen phosphate, 10g/L.Magnesium nitrate solution, 1g/L.The cadmium standard reserving solution, concentration 10.0mg/L.
2. sample preparation: precision accurately takes by weighing 0.2g tipping paper sample A, place the micro-wave digestion jar, 65% nitric acid that in the micro-wave digestion jar, adds certain volume successively, 40% hydrofluorite, the microwave dissolver of packing into after the sealing of 37% hydrochloric acid and 30% hydrogen peroxide carries out micro-wave digestion by the program of clearing up shown in the table 2.Clear up and finish, treat that the microwave dissolver temperature reduces to back below 40 ℃ and take out counteracting tank.Counteracting tank is put into the temperature control electric heater, under 150 ℃ of conditions, catch up with acid 2～3 hours, be evaporated near doing.Catch up with acid to finish, sample solution is transferred in the 50mL plastics volumetric flask, wash counteracting tank 3～4 times with 1% nitric acid, cleaning fluid is transferred in the 50mL volumetric flask equally, uses 1% nitric acid constant volume then.
3. assay method: draw the standard blank solution, the 0.2 μ g/L for preparing, 0.4 μ g/L, 0.6 μ g/L, 0.8 μ g/L, 1 μ g/L cadmium standard operation solution and clear up after each 20 μ L of sample, ammonium dihydrogen phosphate 5 μ L and magnesium nitrate solution 3 μ L inject graphite furnace and measure, and record cadmium 0.41mg/kg in the sample.
Example 2:
As described in embodiment 1, selecting the trade mark is the tipping paper sample of B, records cadmium 0.21mg/kg in the sample.
Example 3:
As described in embodiment 1, selecting the trade mark is the tipping paper sample of C, records cadmium 0.08mg/kg in the sample.
Example 4:
As described in embodiment 1, the shrub branches and leaves combination sample standard substance sample of selecting China National Measuring Science Research Inst. to provide records cadmium 0.20mg/kg in the sample.
Claims (7)
1, the assay method of cadmium content in a kind of cigarette tipping paper is characterized in that: comprise following processing step:
A, micro-wave digestion place the micro-wave digestion jar with the cigarette tipping paper sample, add nitric acid, hydrofluorite, hydrochloric acid and superoxol successively, put into microwave dissolver then and carry out micro-wave digestion;
B, catch up with acid cut to hold, counteracting tank is heated, catch up with acid treatment, after finishing sample solution is moved in the container,, be sample liquid to be measured with 1% nitric acid constant volume;
C, preparation standard blank solution: 1% nitric acid, the cadmium standard operation solution of preparation variable concentrations;
D, graphite furnace atomic absorption spectrophotometer are measured, the cadmium standard operation solution of absorption standard blank solution and the variable concentrations for preparing, with ammonium dihydrogen phosphate and magnesium nitrate solution is that matrix modifier injects graphite furnace, record its absorbance peak area and try to achieve the absorbance peak area and the one-variable linear regression equation of cadmium concentration relation, related coefficient is more than or equal to 0.99, sample liquid to be measured after clearing up is measured, record the absorbance peak area of cadmium, substitution one-variable linear regression equation is tried to achieve the cadmium content in the sample liquid to be measured.
2, the assay method of cadmium content in the cigarette tipping paper according to claim 1, it is characterized in that: the nitric acid of Jia Ruing, hydrofluorite, hydrochloric acid and superoxol amount volume ratio are nitric acid successively: hydrofluorite: hydrochloric acid: hydrogen peroxide=5: 1: 1: 1, wherein concentration of nitric acid 65%, hydrofluoric acid concentration 40%, concentration of hydrochloric acid 37%, concentration of hydrogen peroxide 30%.
3, the assay method of cadmium content in the cigarette tipping paper according to claim 1, it is characterized in that: the micro-wave digestion heating schedule is: n to 120 ℃ of intensification 5mi keeps 5min, 5min to 160 ℃ of intensification, keep 5min, 5min to 200 ℃ of intensification keeps 25min.
4, the assay method of cadmium content in the cigarette tipping paper according to claim 1, it is characterized in that: the heating-up temperature of catching up with sour process is 150 ℃.
5, the assay method of cadmium content in the cigarette tipping paper according to claim 1, it is characterized in that: the atomic absorption spectrometry condition is: wavelength 228.8nm, the wide 0.7nm of slit, 550 ℃ of ashing temperature, 1500 ℃ of atomization temperatures.
6, the assay method of cadmium content in the cigarette tipping paper according to claim 1, it is characterized in that: the concentration of ammonium dihydrogen phosphate is 10g/L, addition 5 μ L.
7, the assay method of cadmium content in the cigarette tipping paper according to claim 1, it is characterized in that: the concentration of magnesium nitrate solution is 1g/L, addition 3 μ L.
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|---|---|
| CN101294896B (en) | 2010-12-01 |
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