CN101187629B - Tobacco and tobacco product arsenic content determination method - Google Patents
Tobacco and tobacco product arsenic content determination method Download PDFInfo
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- CN101187629B CN101187629B CN2007100325075A CN200710032507A CN101187629B CN 101187629 B CN101187629 B CN 101187629B CN 2007100325075 A CN2007100325075 A CN 2007100325075A CN 200710032507 A CN200710032507 A CN 200710032507A CN 101187629 B CN101187629 B CN 101187629B
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Abstract
The invention discloses a method for testing arsenic content in tobaccos and tobacco products, which comprises following steps: adopting nitric acid-hydrogen peroxide to digest through microwaves, then taking chlorine lawrencium acid ammonium and citric acid as chemical promoting agents, using Zeeman to deduct backgrounds automatically, and adopting a graphite furnace atomic absorption method to test the arsenic content in tobacco samples. Results show that the detecting limit of the arsenic content is 0.28 um g/L, recovery ratio is between 92.0%-102.0%, and RSD is<3.0%. Agent species and quantity which are used for digesting are decreased greatly, analyzing time is shortened greatly, the invention is simple, rapid, and applicable to the rapid arsenic content tests of tobacco samples in batches, and the invention has good technique extension value.
Description
Technical field
The invention belongs to the physical and chemical inspection technical field, be specifically related to micro-arsenic Determination on content method in tobacco and the tobacco product.
Background technology
Arsenic is a harmful heavy metal species, and matter containing arsenic is commonly used for pesticide, germifuge, herbicide, defoliant etc. and is used in soil, makes soil be subjected to arsenic contamination, the energetic supersession of the arsenic meeting interference cell of high dose, thus cause the death of biosome.
Trace element in the soil and heavy metal can be absorbed by the cigarette strain in cigarette strain growth course, and can enter human body by smoking, also comprise arsenic.
Therefore, the arsenic of measuring rapidly and accurately in the cigarette product is very necessary.The mensuration of arsenic adopts atomic fluorescence method and ICP-MS method more in the domestic tobacco, the former sample pre-treatments complexity, and latter's instrument costliness is difficult to promote.
Canada is existing at present does the relevant criterion that the chemical modification agent sampling Graphite Furnace Atomic Absorption is measured arsenic in the tobacco with nickel nitrate, compare with classic method, this method is many fast and accurately, but employedly clears up reagent type and consumption is all many, is not suitable for the mensuration of arsenic in the tobacco batch sample.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, and arsenic Determination on content method in a kind of new tobacco and the tobacco product is provided, and is suitable for the mensuration of micro amount of arsenic in tobacco batch and the goods thereof.
Technical scheme of the present invention provide one grow tobacco and tobacco product in arsenic Determination on content method, may further comprise the steps:
(1) tobacco sample prepares liquid to be measured through pre-treatment and nitric acid-hydrogen peroxide system micro-wave digestion;
(2) make chemical modification agent with chlorine rhodium acid ammonium and citric acid, adopt graphite oven atomic absorption, utilize the automatic background correction of Zeeman, calculate the arsenic content of liquid to be measured according to calibration curve.
The pre-treatment of the described tobacco sample of step (1) comprises the dry of tobacco sample and pulverizes.
The pulverizing of described sample is for being crushed to 40 orders.
Described nitric acid-hydrogen peroxide system micro-wave digestion is to get the 0.2g sample to place 50mL micro-wave digestion jar, adds 3mL 68% nitric acid, leaves standstill 15min under the room temperature, adds 1mL 30% hydrogen peroxide, carries out micro-wave digestion after covering the teflon inner cap.
The described program of clearing up is: 140 ℃ of intensification 2min keep 10min; 170 ℃ of intensification 1min keep 10min; 200 ℃ of intensification 1min keep 10min; 100 ℃ of cooling 3min keep 7min.
The described chemical modification agent of step (2) is the citric acid solution of 1 μ L 0.01g/mL chlorine rhodium acid ammonium solution and 2 μ L0.005g/mL.
The described atomic absorption analysis condition of step (2) is: detect wavelength 193.7nm; Slit 0.7nm; Lamp current 380mA; Carrier gas flux 250mL/min, atomized stage is stopped the supple of gas or steam; Sample size 20 μ L; Peak area integral measurement mode.
The invention has the beneficial effects as follows:
After the present invention has selected the mixing improver of chlorine rhodium acid ammonium+citric acid, can improve the ashing temperature, and there is not the volatilization loss of arsenic, because citric acid decomposes the formation that the reductibility environment that discharges active gases and carbon generation helps Rh-As alloy or intermetallic compound, detect sharply symmetry of peak shape.
The present invention adopts nitric acid-hydrogen peroxide system micro-wave digestion, make chemical modification agent with chlorine rhodium acid ammonium and citric acid, utilize the automatic background correction of Zeeman, adopt the arsenic content of graphite furnace atomic absorption spectrometry tobacco sample, compared with prior art, the present invention is guaranteeing that Specimen eliminating is completely under the prerequisite, clearing up reagent type and consumption all greatly reduces, and shortened analysis time greatly, reduced the detection cost, easyly fast be applicable to the fast measuring of arsenic in the tobacco batch sample, have good technology popularization and be worth.
Embodiment
Further describe the present invention below in conjunction with specific embodiment.
Determining of embodiment 1 working curve and detection limit
1, key instrument and reagent
AAS800 type atomic absorption spectrophotometer (AAS) (U.S. PERKIN-ELMER company) is equipped with the THGA graphite-pipe, the electrodeless discharge lamp of arsenic; MWS-3+ microwave digestion system (German BERGHOF company); H110 type electronic balance (sensibility reciprocal 0.0001g, German SARTORIUS company).
1000 μ g/mL arsenic standard solutions (national Iron and Steel Research Geueral Inst provides); Chlorine rhodium acid ammonium (analyze pure, mountain of a specified duration, Shanghai chemical reagent company); Citric acid (analyze pure, Guangzhou Chemical Reagent Factory); 68% (massfraction) nitric acid (top grade is pure, new east station of Guangzhou reddening factory); 30% (massfraction) hydrogen peroxide (top grade is pure, Guangdong brilliance chemical reagent work); Ultrapure water (by the Milli-Q preparation); Tobacco leaf and cigarette sample.
The automatic dilution function of utilizing AAS800 to have, is 5,10,15,20,30,40,50 μ g/L series arsenic standard solution with 0.2% nitric acid with 1000 μ g/mL arsenic standard solution stepwise dilution to concentration, do blank with 0.2% nitric acid, the citric acid solution of 1 μ L 0.01g/mL chlorine rhodium acid ammonium solution and 2 μ L 0.005g/mL is made chemical modification agent, respectively serial arsenic standard solution is carried out atomic absorption analysis, and drafting absorbance-concentration working curve, its regression equation is y=0.00203x-0.00017, related coefficient 0.9998.
In the formula, the y-absorbance; X-arsenic concentration (μ g/L).
According to the spectroscopy detection limit definition of IUPAC (IUPAC), 20 blank values of METHOD FOR CONTINUOUS DETERMINATION, detecting of calculating during by K=3 is limited to 0.30 μ g/L.
Arsenic Determination on content in embodiment 2 tobacco samples
(1) tobacco sample prepares liquid to be measured through pre-treatment and nitric acid-hydrogen peroxide system micro-wave digestion;
Take by weighing the 40 order offal samples that the 0.2g drying is pulverized, place 50mL micro-wave digestion jar, add 3mL 68% nitric acid, leave standstill 15min under the room temperature, add 1mL 30% hydrogen peroxide, carry out micro-wave digestion after covering the teflon inner cap.Clearing up program is: 140 ℃ of intensification 2min keep 10min; 170 ℃ of intensification 1min keep 10min; 200 ℃ of intensification 1min keep 10min; 100 ℃ of cooling 3min keep 7min.After clearing up end, be cooled to room temperature, open jar, digestion solution is transferred in the 25mL volumetric flask, with 0.2% (volume fraction, down together) nitric acid washing counteracting tank, cleansing solution is incorporated in the volumetric flask, and constant volume shakes up, and gets liquid to be measured.
(2) make chemical modification agent with chlorine rhodium acid ammonium and citric acid, adopt graphite oven atomic absorption, utilize the automatic background correction of Zeeman, calculate the arsenic content of liquid to be measured according to calibration curve.
Compare with the treating fluid that does not add the offal sample, title per sample, sample weighting amount and dilution ratio (when concentration surpasses detection limit) editor's sample message table, citric acid solution and the 20 μ L samples liquid to be measured of being drawn chemical modification agent 1 μ L 0.01g/mL chlorine rhodium acid ammonium solution and 2 μ L 0.005g/mL by automatic sampler successively carry out atomic absorption analysis in graphite furnace, heating schedule sees Table 1, adopt the Zeeman automatic background to proofread and correct, according to the arsenic content in the calibration curve calculation sample.The instrument condition of work is:
Detect wavelength: 193.7nm; Slit: 0.7nm; Lamp current: 380mA; Carrier gas (Ar) flow: 250mL/min, atomized stage is stopped the supple of gas or steam; Sample size: 20 μ L; Metering system: peak area integration.
Table 1 graphite furnace heating schedule
Embodiment 3 relative differences, the recovery and repeated experiment
Get 2 parallel sample according to embodiment 2 described methods, adopt the inventive method to measure its arsenic content respectively, the arsenic content that records is respectively 0.44 and 0.46mg/kg, average out to 0.45mg/kg, relative differences is 4.4%, meets the requirement of GB/T5009.12-1996 relative differences≤20%.
Get 3 different samples, all mark-on 5 μ g/L measure its arsenic content respectively, and according to former content, add scalar sum measured quantity calculate recovery rate, the results are shown in Table 2.By table 2 as seen, the recovery of standard addition of this method illustrates that this method has higher accuracy between 92.0%～102.0%.
The recovery of table 2 arsenic
| Sample number into spectrum | Content (μ g/L) | Mark-on measured value (μ g/L) | The recovery (%) |
| 1 | 3.6 | 8.3 | 94.0 |
| 2 | 4.3 | 9.4 | 102.0 |
Annotate: 1. add scalar and be 5.0 μ g/L.
Same sample has been carried out 6 replicate determinations, and RSD＜3.0% sees Table 3 as a result, shows that the repeatability of this law is better.
Table 3 sample segment measured value and detection precision (n=6)
Claims (4)
- One grow tobacco and tobacco product in arsenic Determination on content method, may further comprise the steps:(1) pre-treatment of tobacco sample drying and pulverizing and nitric acid-hydrogen peroxide system micro-wave digestion prepares liquid to be measured; Described nitric acid-hydrogen peroxide system micro-wave digestion is to get the 0.2g sample to place 50mL micro-wave digestion jar, adds 3mL 68% nitric acid, leaves standstill 15min under the room temperature, adds the 1mL30% hydrogen peroxide, carries out micro-wave digestion after covering the teflon inner cap;(2) make chemical modification agent with chlorine rhodium acid ammonium and citric acid, adopt graphite oven atomic absorption, utilize the automatic background correction of Zeeman, calculate the arsenic content of liquid to be measured according to calibration curve;It is characterized in that described chemical modification agent is the citric acid solution of 1 μ L0.01g/mL chlorine rhodium acid ammonium solution and 2 μ L0.005g/mL;The heating schedule of described graphite furnace is:The step temperature/℃ the heating-up time/s retention time/s1 110 1 20 ；2 200 15 30 ；3 1600 10 20 ；4 2300 0 3 ；5 20 8 3 ；6 2450 5 5 。
- 2. according to arsenic Determination on content method in described tobacco of claim 1 and the tobacco product, the pulverizing that it is characterized in that described sample is for being crushed to 40 orders.
- 3. according to arsenic Determination on content method in described tobacco of claim 1 and the tobacco product, it is characterized in that the described micro-wave digestion program of step (1) is: 140 ℃ of intensification 2min keep 10min; 170 ℃ of intensification 1min keep 10min; 200 ℃ of intensification 1min keep 10min; 100 ℃ of cooling 3min keep 7min.
- 4. according to arsenic Determination on content method in described tobacco of claim 1 and the tobacco product, it is characterized in that the described atomic absorption analysis condition of step (2) is: detect wavelength 193.7nm; Slit 0.7nm; Lamp current 380mA; Carrier gas flux 250mL/min, atomized stage is stopped the supple of gas or steam; Sample size 20 μ L; Peak area integral measurement mode.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101294898B (en) * | 2008-06-23 | 2010-04-14 | 中国烟草总公司郑州烟草研究院 | Method for measuring chromium content in smoke tipping paper |
| CN101614657B (en) * | 2008-06-27 | 2012-07-04 | 上海宝钢工业检测公司 | Method for measuring arsenic in gas and dust discharged by roasting and burning furnace |
| CN101738376B (en) * | 2008-11-25 | 2011-08-31 | 中国第一重型机械股份公司 | Method for measuring graphite oven atomic absorption spectrum of arsenic element in steel |
| CN101776607B (en) * | 2009-12-30 | 2014-09-10 | 中国科学院上海硅酸盐研究所 | Method for analyzing total arsenic in glass |
| CN103196851A (en) * | 2013-03-27 | 2013-07-10 | 广西中烟工业有限责任公司 | Measuring method of arsenic content of glyceryl triacetate |
| CN103196853A (en) * | 2013-04-15 | 2013-07-10 | 贵州百灵企业集团制药股份有限公司 | Method for detecting arsenic salt of Huanglian Shangqing tablets |
| CN104215627A (en) * | 2014-05-09 | 2014-12-17 | 武汉红金龙印务股份有限公司 | Method for microwave digestion-inductively coupled plasma mass spectrometer (ICP-MS) determination of metal ions such as lead, arsenic, cadmium and chromium in cigarette case |
| CN105021582B (en) * | 2015-07-16 | 2017-07-18 | 广西大学 | With the method for the trace arsenic in SPE Rice By Atomic Fluorescence Spectrometry |
| CN105241948B (en) * | 2015-11-09 | 2019-01-29 | 中国农业科学院烟草研究所 | A kind of method that ICP-MS measures As and Hg in tobacco simultaneously |
| CN106442363A (en) * | 2016-11-30 | 2017-02-22 | 大工（青岛）新能源材料技术研究院有限公司 | Method for determination of arsenic content in wastewater |
| CN110186909B (en) * | 2019-06-20 | 2022-06-28 | 上海瀚海检测技术股份有限公司 | Microwave digestion and ICP-OES (inductively coupled plasma-optical emission spectrometry) test of heavy metal elements in leather product |
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