CN103293216A - Method for quickly and accurately determining 4 heavy metals in cigarette smoke - Google Patents
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Abstract
The invention discloses a method for quickly and accurately determining 4 heavy metals in cigarette smoke. The method comprises the following steps of: accurately weighing a cigarette powder sample; placing the cigarette powder sample in a triangular flask with a stopper; adding 5ml of nitric acid and 5ml of 30% of hydrogen peroxide; digesting by heating in medium flame for 5 minutes, cooling for 2 minutes, heating in medium flame for 5 minutes and heating in high flame for 15 minutes; taking out after cooling, discoloring by active carbon, filtering and transferring to a sample flask for measuring; guiding a sample solution to an inductive coupling plasma emission spectrum mass spectrometer for detecting, reading out the content of heavy metals into the to-be-measured sample cut cigarette and cigarette ash; representing the content of the heavy metals in cigarette smoke of the cigarette by using a subtraction method according to the difference value between the cut cigarette and the content of the heavy metals in the cigarette ash. The method for quickly and accurately determining the 4 heavy metals in the cigarette smoke is accurate in test, simple to operate, high in flexibility and good in repeatability. Moreover, the method is suitable for the cigarette industry and carrying out quantitative measurement onto the heavy metals in the cigarette sample, so that the blank in the technical field is filled up.
Description
Technical field
The invention belongs to cigarette detection technique field, specifically relate to a kind of ICP-MS(of utilization inductively coupled plasma emission spectrum mass spectrometer) and subtract the method for 4 heavy metal species content in the poor method rapid and accurate determination cigarette smoke.
Background technology
In the cigarette composition, except tar, beyond the common objectionable impurities such as nicotine, lead, cadmium, arsenic, heavy metals such as chromium also can work the mischief to health.Heavy metal in the flue gas of cigarette burning can exist with aerocolloidal form, enters human body.Temperature can reach 300 ℃ in cigarette burning, forms the flue gas of comparing easier absorption with common food, can produce bigger harm to human body under the situation of equal size.And because flue gas mobile extremely strong, hazards of second-hand smoke is also quite serious.Just comprise As, Cd, Cr, Pb, elements such as Ni and Hg in 107 kinds of cigarette smoke objectionable constituent of U.S.'s report in 1989.Nineteen ninety Hoffmann inventory is also with A s, Cd, and Cr, Pb, Ni, Se and Hg etc. classify 44 kinds of objectionable constituent of tobacco as.
In the prior art, the method that the detection of trace element and heavy metal is adopted usually in the tobacco has atomic absorption spectrography (AAS) (AAS) (TORRENCE, 2002), ICP-AES (ICP-AES) (Zhang Chengcong, 2000) and ultraviolet-visible spectrophotometry (Shi Honglin, 2002).But AAS and ultraviolet-visible spectrophotometry can not detect multiple element simultaneously, and ICP-AES method spectrum serious interference should not measure elements such as arsenic, cadmium, mercury.Suo Weiguo (2008) adopts ICP/MS to measure 7 kinds of trace elements in the finished cut tobacco, but the accuracy of standard substance verification method of no use.Yin Xiaoling (2010) has studied with concentration 5% nitric acid and has captured heavy metal element in the cigarette smoke, uses the method for aas determination lead, arsenic, chromium, cadmium, mercury then, obtains satisfactory result.But the method complicated operation, every kind of element all needs special element lamp, and experimental period is long.Wang Haili (2010) adopts DRC-ICP/MS to eliminate Cr, and the mass spectrum of Ni and Se disturbs.In order to measure the heavy metal element in the cigarette rapidly and accurately, in conjunction with microwave digestion technology, set up DRC-ICP/MS and measured Cr in the cigarette shreds, Ni, As, Se, Cd, Cs, the method for Hg and Pb simultaneously.But flue gas trapping equipment and ICP-MS are the higher instruments of cost, and most of laboratory does not have condition determination.And adopt cambridge filter to collect granule phase substance and measure heavy metal element in the cigarette smoke, filter disc adopts the method for nitrate leaching.This method can only capture the heavy metal in the flue gas granule phase substance, can not measure whole content of beary metal in the flue gas.
In sum, set up a kind of can the rapid and accurate determination cigarette smoke in the method for 4 heavy metal species, with the content of heavy metal in the objective reality ground reaction cigarette smoke, significant to aspects such as cigarette composition design, product maintenance and quality controls.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of easy and simple to handle, highly sensitive, good reproducibility be provided, can the rapid and accurate determination cigarette smoke in the method for 4 heavy metal species content.
Purpose of the present invention is achieved through the following technical solutions.
Except as otherwise noted, percentage of the present invention is mass percent.
The method of 4 heavy metal species in a kind of rapid and accurate determination cigarette smoke may further comprise the steps:
(1) foundation of standard working curve:
1. the foundation of plumbous standard working curve: compound concentration is 10 μ g/g, 20 μ g/g, and 30 μ g/g, 40 μ g/g, the plumbous typical curve sample of 50 μ g/g, solvent is deionized water; Plumbous typical curve sample is gone up mensuration in ICP-MS, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2Need greater than 0.999;
2. the foundation of cadmium standard working curve: compound concentration is 10 μ g/g, 20 μ g/g, and 30 μ g/g,, 40 μ g/g, the cadmium typical curve sample of 50 μ g/g, solvent is deionized water; Cadmium money typical curve sample is gone up in ICP-MS and is measured, and obtains standard working curve, and curve is forced to make zero linearly dependent coefficient R
2Need greater than 0.999;
3. the foundation of arsenic standard working curve: compound concentration is 1 μ g/g, 3 μ g/g, and 5 μ g/g,, 7 μ g/g, the arsenic typical curve sample of 10 μ g/g, solvent is deionized water; Arsenic typical curve sample is gone up mensuration in ICP-MS, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2Need greater than 0.999;
4. the foundation of chromium standard working curve: compound concentration is 1 μ g/g, 2 μ g/g, and 5 μ g/g,, 10 μ g/g, the chromium typical curve sample of 15 μ g/g, solvent is deionized water; Chromium typical curve sample is gone up mensuration in ICP-MS, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2Need greater than 0.999;
(2) sample solution preparation:
1. from cigarette, separate pipe tobacco, tobacco sample is pulverized, cross 40 mesh sieves; Take by weighing 0.2000g tobacco powder sample, place in the tool plug triangular flask, cover tightly stopper, add 5ml nitric acid, the 5ml30% hydrogen peroxide was cleared up according to 5 minutes-Gao of 5 minutes-2 minutes-moderate heat of cooling of moderate heat fire in 15 minutes; Take out the cooling back, and activated carbon decolorizing filters, and is transferred in the sample bottle to be measured;
2. will collect cigarette ash after the cigarette spontaneous firing, take by weighing 0.2000g cigarette ash sample, place in the tool plug triangular flask, cover tightly stopper, add 5ml nitric acid, the 5ml30% hydrogen peroxide was cleared up according to 5 minutes-Gao of 5 minutes-2 minutes-moderate heat of cooling of moderate heat fire in 15 minutes; Take out the cooling back, and activated carbon decolorizing filters, and is transferred in the sample bottle to be measured;
(3) detect: sample solution is imported in the inductively coupled plasma emission spectrum mass spectrometer detect, read the content of heavy metal in cigarette sample pipe tobacco to be measured and the cigarette ash, reading is ρ (pipe tobacco) and ρ (cigarette ash), condition determination such as table 1,
Table 1ICP-MS instrumental analysis condition:
Calculate with minusing then:
The c(pipe tobacco)=and ρ (pipe tobacco) * 0.05/0.2, the μ g/g of unit
C(cigarette ash)=and ρ (cigarette ash) * 0.05/0.2, the μ g/g of unit
The c(flue gas)=the c(pipe tobacco)-c(cigarette ash), the μ g/g of unit represents content of beary metal in the cigarette smoke according to the difference of content of beary metal in pipe tobacco and the cigarette ash.
The present invention has the following advantages with respect to prior art:
1, capturing flue gas detection content of beary metal wherein is the difficult technologies of a key.Heavy metal adopts Fume collector in the international up-to-date detection cigarette smoke, and this Fume collector relies on import, and is with high costs, and can only collect the heavy metal in the gas grain, can not measure the content that especially enters the heavy metal of human body in the flue gas fully.Based on this actual conditions, our indexing utilizes minusing to measure heavy metal in the flue gas, and this is a kind of thinking design of shifting fully.
2, inductivity coupled plasma mass spectrometry ICP/MS method (inductively coupled plasma mass spectrometry) is to be the mass spectrometry of ionization source with inductively coupled plasma (ICP).This technology has overcome AAS and ultraviolet one visible spectrophotometry can not detect multiple element simultaneously, and ICP-AES method spectrum serious interference, should not measure the shortcoming of elements such as arsenic, cadmium, mercury, can carry out most Analytical Chemistry of Heavy Metals simultaneously, have advantages such as detection sensitivity height, detection limit is low, linear detection range is wide.The present invention adopts ICP-MS method to measure the Pb in pipe tobacco and the cigarette ash simultaneously, Cd, and As, As, the content of Cr in accurate mensuration, reduces cost and is extensive use of three aspects and found reasonable configuration the most.
Embodiment
The present invention is described in further detail below by embodiment.Should be appreciated that specific embodiment described herein only in order to explaining analysis condition technical essential of the present invention, and be not used in restriction the present invention.
Embodiment 1
Employed main agents and instrument:
30% hydrogen peroxide, (top grade is pure, Guangdong chemical reagent two factories), (top grade is pure for 63% red fuming nitric acid (RFNA), Guangdong chemical reagent two factories), ultrapure water (18.2M Ω/cm, the self-control of Beijing UPW-20N of company's epoch type Superpure water machine), plumbous, cadmium, arsenic, chromium standard solution (national standardization material research centre, 1000 μ g/g), high-purity Ar
2, ELAN9000 inductivity coupled plasma mass spectrometry (instrument (U.S. Perkin Elmer SCIEX company) of ICP-MS), Multiwave microwave dissolver (Austrian Anton Paar company), analytical balance (sensibility reciprocal 0.1mg), constant temperature oven (German BINDER).
The glassware that uses is all through 10%HNO
3Immersion goes metal to handle; 10 kinds of common cigarette samples.
1. the foundation of standard working curve
1.1 the foundation of plumbous standard working curve
1.1.1 get the plumbous standard solution 20ml of 1000 μ g/g, distilled water is settled to 200ml, makes the plumbous standard solution of 100 μ g/g.
1.1.2 get the plumbous standard solution 10ml of 100 μ g/g respectively, 20ml, 30ml, 40ml, 50ml are in the 100ml volumetric flask, it is 10 μ g/g that constant volume obtains concentration, 20 μ g/g, and 30 μ g/g,, 40 μ g/g, the plumbous typical curve sample of 50 μ g/g.
1.1.3 plumbous typical curve sample and ICP-MS are gone up mensuration, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2=0.9999.
1.2 the foundation of cadmium standard working curve
1.2.1 get 1000 μ g/g cadmium standard solution 20ml, distilled water is settled to 200ml, makes the cadmium standard solution of 100 μ g/g.
1.2.2 get the cadmium standard solution 10ml of 100 μ g/g respectively, 20ml, 30ml, 40ml, 50ml are in the 100ml volumetric flask, it is 10 μ g/g that constant volume obtains concentration, 20 μ g/g, and 30 μ g/g,, 40 μ g/g, the cadmium typical curve sample of 50 μ g/g.
Measure 1.2.3 cadmium money typical curve sample and ICP-MS go up, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2=0.9999.
1.3 the foundation of arsenic standard working curve
1.3.1 get 1000 μ g/g arsenic standard solution 10ml, distilled water is settled to 100ml, makes the arsenic standard solution of 100 μ g/g.
1.3.2 get the arsenic standard solution 1ml of 100 μ g/g respectively, 3ml, 5ml, 7ml, 10ml are in the 100ml volumetric flask, it is 1 μ g/g that constant volume obtains concentration, 3 μ g/g, and 5 μ g/g,, 7 μ g/g, the arsenic typical curve sample of 10 μ g/g.
1.3.3 arsenic typical curve sample and ICP-MS are gone up mensuration, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2=0.9999.
1.4 the foundation of chromium standard working curve
1.4.1 get 1000 μ g/g chromium standard solution 10ml, distilled water is settled to 100ml, makes the chromium standard solution of 100 μ g/g.
1.4.2 get the chromium standard solution 1ml of 100 μ g/g respectively, 2ml, 5ml, 10ml, 15ml are in the 100ml volumetric flask, it is 1 μ g/g that constant volume obtains concentration, 2 μ g/g, and 5 μ g/g,, 10 μ g/g, the chromium typical curve sample of 15 μ g/g.
1.4.3 chromium typical curve sample and ICP-MS are gone up mensuration, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2=0.9999.
2. testing sample is prepared
2.1 tobacco sample is prepared
2.1.1 from cigarette, separate pipe tobacco, tobacco sample is pulverized, cross 40 mesh sieves.Take by weighing 0.2000g tobacco powder sample, place in the tool plug triangular flask, cover tightly stopper, add 5ml nitric acid, the 5ml30% hydrogen peroxide is cleared up according to following steps.
2.1.2 moderate heat 5 minutes---cooled off---moderate heat 5 minutes---high fire 2 minutes 15 minutes.
2.1.3 take out the cooling back, activated carbon decolorizing filters, and is transferred in the plastic sample bottle to be measured.
2.2 cigarette ash
2.2.1 will collect cigarette ash behind the cigarette auto-ignition combustion.Take by weighing 0.2000g cigarette ash sample, place in the tool plug triangular flask, cover tightly stopper, add 5ml nitric acid, the 5ml30% hydrogen peroxide, clear up according to following steps:
2.2.2 moderate heat 5 minutes---cooled off---moderate heat 5 minutes---high fire 2 minutes 15 minutes.
2.2.3 take out the cooling back, activated carbon decolorizing filters, and is transferred in the plastic sample bottle to be measured.
* contrast is not for adding the space management of pipe tobacco and cigarette ash
3. the flue gas heavy metal minusing calculates: utilize the difference of content of beary metal in pipe tobacco and the cigarette ash to represent flue gas heavy metal in the cigarette: the c(flue gas)=and the c(pipe tobacco)-(cigarette ash)
4. show the 1ICP-MS testing conditions
5. the calculating of analysis result
5.1 read the content of 4 heavy metal species in cigarette sample pipe tobacco to be measured and the cigarette ash, can directly calculate the content of flue gas heavy metal in the cigarette sample.
5.2 can also be according to the total amount of the contained heavy metal of flue gas in every cigarette burning process of mass conversion of cigarette.
6. method evaluation
Utilize import Fume collector-ICP-MS method to measure 6.1 will subtract the flue gas content of poor method mensuration with relevant producer, reach Fume collector-NITRATE BY FLAME ATOMIC absorption measurement flue gas content and do contrast, the result is as follows:
Table 2.3 kind of method is measured the Pb in the flue gas
6.2 as can be seen from Table 2, compare with flue gas trapping equipment, subtract plumbous content in the fine reaction flue gas of poor method energy, Fume collector can absorb 86.0% flue gas, and the correlation ratio of most of sample is all between 80%-90%; Atomic absorption method also can detect the lead in the flue gas, and average correlation ratio is 85.5%, but degree of stability and accuracy are all relatively poor, and the correlation ratio variation range is bigger.
Table 33 kind of method is measured the Cd in the flue gas
6.3 as can be seen from Table 3, Fume collector has reached 93.3% with the correlation ratio that subtracts cadmium in the poor method mensuration flue gas, and wherein the correlation ratio of 9 kinds of samples has all surpassed 90%, two kind of method measurement result unanimity; Aas determination is more much lower than subtracting poor method as a result, and correlation ratio has only 82.6%.
Table 43 kind of method is measured the As in the flue gas
6.4 as can be seen from Table 4, the Fume collector method with subtract poor method and measure the correlation ratio of arsenic content in the flue gas to have reached 94.3% two kind of method measurement result consistent; Atomic absorption method with subtract the difference compare, though also can go out the arsenic content in most of sample flue gas, but being lower than 0.05 μ g/g, content can't detect data, and the correlation ratio that detects data and subtract between the poor method on average has only 70.8%, and the coefficient of variation is very big, so atom absorbs the detection that is not suitable for arsenic content in the flue gas.
Table 53 kind of method is measured the Cr in the flue gas
6.5 as can be seen from Table 5, Fume collector and the correlation ratio that subtracts between the poor method have reached 88.5%, and the coefficient of variation is low, therefore subtract the content that poor method can accurately detect chromium in the flue gas; Atomic absorption method can not accurately be measured the content of chromium in the flue gas, and the sample that content is lower than 0.05 μ g/g can't detect, and content is that the value of detecting of the sample of 0.05-0.10 μ g/g all is 0.05 μ g/g, and correlation ratio has only 65.1%, and the coefficient of variation reaches 40.7%.
Embodiment 2
Repeat embodiment 1, following difference is arranged: use special-purpose teflon digester to substitute tool plug triangular flask and clear up.
The result shows: the result who obtains after special-purpose teflon digester and tool plug triangular flask are cleared up is basic identical, but cost exceeds more than 10 times.
Embodiment 3
Repeat embodiment 1, following difference is arranged: in digestion process, do not cool off.The result shows: continuous high temperature is cleared up and can be made pipe tobacco and cigarette ash form pastel, is bonded on the triangular flask wall, causes and clears up not exclusively.
Embodiment 4
Repeat embodiment 1, following difference arranged: replace microwave dissolver with common microwave stove, clear up according to following steps: 500w(5 minute)-cooling (2 minutes)-500w(5 minute)-800w(15 minute).
Take out the cooling back, is transferred in the plastic sample bottle, and constant volume 50ml is to be measured.The result shows: replace microwave dissolver can obtain the product of 70%-80% with common microwave stove, can do interim replacement and use when experiment condition does not possess.
Embodiment 5
Repeat embodiment 1, following difference is arranged: utilize artificial the smoking to replace cigarette spontaneous firing, produce cigarette ash then.The result shows: the content basically identical of 4 heavy metal species in artificial smoking and the spontaneous firing cigarette ash should be test method with spontaneous firing in the experiment, the human health damage of avoiding smoking and bringing.
Embodiment 6
Repeat embodiment 1, following difference is arranged: adopt different temperature of combustion, to investigate different temperatures to the influence of cigarette flue gas heavy metal measurement result.The result shows: temperature of combustion is more high.The content of contained heavy metal is more high in the cigarette ash, and this completeness with burning is relevant, but difference is all in 5%, and suitable temperature of combustion should be selected according to self-condition in the laboratory.
Embodiment 7～16
Repeat embodiment 1, following difference is arranged: tobacco leaf was not ground 40 mesh sieves.The result shows: pipe tobacco is difficult for clearing up or clears up not exclusively, and the amount of digestion solution reduces, so must grind and cross 40 mesh sieves to tobacco leaf in the test
Embodiment 17～26
Repeat embodiment 1, following difference is arranged: do not carry out activated carbon decolorizing after Specimen eliminating is finished.
The result shows: sample segment is cleared up back pipe tobacco pigment and is separated out, and it is yellow, yellowish-brown that Specimen eliminating liquid is, or brown, do not meet the mensuration requirement of ICP-MS, can't measure or the measurement result error big.So must carry out activated carbon decolorizing in the test.
Embodiment 27～36
Repeat embodiment 1, following difference is arranged: do not filter after Specimen eliminating is finished.
The result shows: sample mixes not filter and is mixed with impurity, does not meet the mensuration requirement of ICP-MS, can't measure, so must filter in the test.
Claims (1)
1. the method for 4 heavy metal species in the rapid and accurate determination cigarette smoke may further comprise the steps:
(1) foundation of standard working curve
1. the foundation of plumbous standard working curve: compound concentration is 10 μ g/g, 20 μ g/g, and 30 μ g/g, 40 μ g/g, the plumbous typical curve sample of 50 μ g/g, solvent is deionized water; Plumbous typical curve sample is gone up mensuration in ICP-MS, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2Need greater than 0.999;
2. the foundation of cadmium standard working curve: compound concentration is 10 μ g/g, 20 μ g/g, and 30 μ g/g, 40 μ g/g, the cadmium typical curve sample of 50 μ g/g, solvent is deionized water; Cadmium typical curve sample is gone up mensuration in ICP-MS, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2Need greater than 0.999;
3. the foundation of arsenic standard working curve: compound concentration is 1 μ g/g, 3 μ g/g, and 5 μ g/g, 7 μ g/g, the arsenic typical curve sample of 10 μ g/g, solvent is deionized water; Arsenic typical curve sample is gone up mensuration in ICP-MS, obtain standard working curve, curve is forced to make zero, and linearly dependent coefficient R2 needs greater than 0.999;
4. the foundation of chromium standard working curve: compound concentration is 1 μ g/g, 2 μ g/g, and 5 μ g/g,, 10 μ g/g, the chromium typical curve sample of 15 μ g/g, solvent is deionized water; Chromium typical curve sample is gone up mensuration in ICP-MS, obtain standard working curve, curve is forced to make zero linearly dependent coefficient R
2Need greater than 0.999;
(2) specimen preparation
1. from cigarette, separate pipe tobacco, tobacco sample is pulverized, cross 40 mesh sieves; Take by weighing 0.2000g tobacco powder sample, place in the tool plug triangular flask, cover tightly stopper, add 5ml nitric acid, the 5ml30% hydrogen peroxide was cleared up according to 5 minutes-Gao of 5 minutes-2 minutes-moderate heat of cooling of moderate heat fire in 15 minutes; Take out the cooling back, and activated carbon decolorizing filters, and is transferred in the sample bottle to be measured;
2. will collect cigarette ash after the cigarette spontaneous firing, take by weighing 0.2000g cigarette ash sample, place in the tool plug triangular flask, cover tightly stopper, add 5ml nitric acid, the 5ml30% hydrogen peroxide was cleared up according to 5 minutes-Gao of 5 minutes-2 minutes-moderate heat of cooling of moderate heat fire in 15 minutes; Take out the cooling back, and activated carbon decolorizing filters, and is transferred in the sample bottle to be measured;
(3) detect: sample solution is imported in the inductively coupled plasma emission spectrum mass spectrometer detect, read the content of heavy metal in cigarette sample pipe tobacco to be measured and the cigarette ash, reading is ρ (pipe tobacco) and ρ (cigarette ash), condition determination such as table 1:
Table 1ICP-MS instrumental analysis condition:
Calculate with minusing then:
The c(pipe tobacco)=and ρ (pipe tobacco) * 0.05/0.2, the μ g/g of unit
C(cigarette ash)=and ρ (cigarette ash) * 0.05/0.2, the μ g/g of unit
The c(flue gas)=the c(pipe tobacco)-c(cigarette ash), the μ g/g of unit represents content of beary metal in the cigarette smoke according to the difference of content of beary metal in pipe tobacco and the cigarette ash.
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| CN103471879A (en) * | 2013-09-22 | 2013-12-25 | 红云红河烟草(集团)有限责任公司 | Smoke gas collecting device and method for quickly and accurately determining seven heavy metals in smoke gas |
| CN104568531A (en) * | 2013-10-22 | 2015-04-29 | 南京工程学院 | Method for preparing standard substance for LA-ICP-MS |
| 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 |
| CN103954678A (en) * | 2014-05-26 | 2014-07-30 | 国家烟草质量监督检验中心 | Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead elements in cigarette ashes |
| CN103969324A (en) * | 2014-05-26 | 2014-08-06 | 国家烟草质量监督检验中心 | Method for detecting chromium, nickel, arsenic, selenium, cadmium and lead in cigarette side-stream smoke |
| CN103954678B (en) * | 2014-05-26 | 2017-03-08 | 国家烟草质量监督检验中心 | The detection method of chromium, nickel, arsenic, selenium, cadmium, lead element in a kind of cigarette ash |
| CN104237369A (en) * | 2014-09-25 | 2014-12-24 | 上海烟草集团有限责任公司 | Method for separation and determination of arsenic elements in different forms in tobacco and tobacco products |
| CN104266889A (en) * | 2014-09-25 | 2015-01-07 | 上海烟草集团有限责任公司 | Separation determination method for different forms of cadmium elements in tobaccos and tobacco products |
| CN104266888A (en) * | 2014-09-25 | 2015-01-07 | 上海烟草集团有限责任公司 | Method for separating and measuring arsenic elements with different forms in main stream smoke of cigarettes |
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