CN103471879A - Smoke gas collecting device and method for quickly and accurately determining seven heavy metals in smoke gas - Google Patents
Smoke gas collecting device and method for quickly and accurately determining seven heavy metals in smoke gas Download PDFInfo
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- CN103471879A CN103471879A CN201310432271XA CN201310432271A CN103471879A CN 103471879 A CN103471879 A CN 103471879A CN 201310432271X A CN201310432271X A CN 201310432271XA CN 201310432271 A CN201310432271 A CN 201310432271A CN 103471879 A CN103471879 A CN 103471879A
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Abstract
The invention discloses a smoke gas collecting device and a method for quickly and accurately determining seven heavy metals in smoke gas. The smoke gas collecting device comprises a suction-filtration flask and a suction-filtration pump, wherein the suction-filtration flask is communicated with the suction-filtration pump through a suction-filtration tube; an opening is formed in the upper part of the side wall of the suction-filtration flask; a glass tube is hermetically arranged at the opening; a layer of cotton is laid at a flask neck of the suction-filtration flask. The method for quickly and accurately determining the seven heavy metals in the smoke gas comprises the following steps: accurately measuring 50ml of sample solution of absorption liquid containing the smoke gas; guiding the sample solution into an inductively coupled plasma emission spectrum mass spectrometer for detection; reading the content of the heavy metals in the sample solution to be detected; performing technical analysis to obtain the content of the heavy metals in the smoke gas of cigarette. The method has the advantages of accuracy in test, simplicity in operation, high sensitivity and high repeatability, is applicable to quantitative determination of the heavy metals in the smoke gas of the cigarette in the tobacco industry, and fills in the blank of the technical field.
Description
Technical field
The invention belongs to cigarette detection technique field, be specifically related to a kind of smoke gathering device of manual imitation smoking cigarette.The invention still further relates to simultaneously and utilize ICP-MS(inductively coupled plasma emission spectrum mass spectrometer) method of 7 heavy metal species in the rapid and accurate determination flue gas.
Background technology
In the cigarette composition, except tar, beyond the common objectionable impurities such as nicotine, lead, cadmium, arsenic, the heavy metals such as chromium also can work the mischief to health.Heavy metal after cigarette burning in flue gas exists with aerocolloidal form, and enters human body in aspiration procedure.During cigarette burning, temperature reaches 300 ℃, forms and compares the flue gas more easily absorbed with common food, in the situation that equal size can produce larger harm to human body.Because the mobility of flue gas is extremely strong, the harm that second-hand-cigarette causes is also quite serious simultaneously.Just comprise As, Cd, Cr, Pb, the 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 by As, Cd, and Cr, Pb, Ni, Se and Hg etc. classifies 44 kinds of objectionable constituent of tobacco as.
In smoking process, the heavy metal in ash content can enter human body hardly, and health hazard is less.But the heavy metal in flue gas can enter the human lung with aspiration procedure, have a strong impact on healthy.At present, the method that detects or measure content of beary metal in pipe tobacco and cigarette ash is more, but to the rarely seen play-by-play of the detection method of heavy metal in flue gas content.
In prior art, the method that in tobacco, the detection of trace element and heavy metal adopts usually has atomic absorption spectrography (AAS) (AAS) (TORRENCE, 2002), ICP-AES (ICP-AES) (Zhang Chengcong, 2000) and UV-VIS spectrophotometry (Shi Honglin, 2002).AAS and UV-VIS spectrophotometry can not detect multiple element simultaneously, and ICP-AES method spectrum is disturbed seriously, should not measure the 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 does not use the accuracy of standard substance verification method.Yin Xiaoling (2010) has studied with heavy metal element in the nitric acid trapping cigarette smoke of concentration 5%, then use the method for aas determination lead, arsenic, chromium, cadmium, mercury, obtain 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 rapidly and accurately the heavy metal element in cigarette, in conjunction with microwave digestion technology, set up DRC-ICP/MS and measured the Cr in cigarette shreds simultaneously, Ni, As, Se, Cd, Cs, the method for Hg and Pb, but flue gas trapping equipment (Electrostatic device) is the accessory that cost is higher, most of laboratory does not have this instrument accessory, and adopts cambridge filter to collect heavy metal element in granule phase substance mensuration cigarette smoke, and filter disc adopts the method for nitrate leaching, the method can only trap the heavy metal in Smoke Particulate, can not measure whole content of beary metal in flue gas.
In sum, set up the method for 7 heavy metal species in a kind of smoke gathering device that can simulate artificial smoking cigarette rapid and accurate determination cigarette smoke, with the content of heavy metal in objective reality ground reaction cigarette smoke, significant to aspects such as cigarette composition design, product maintenance and quality controls.
Summary of the invention
The object of the invention is to for deficiency of the prior art, a kind of smoke gathering device of simple in structure, manual imitation smoking cigarette is provided.
Simultaneously, the present invention also aims to provide a kind of easy and simple to handle, highly sensitive, reproducible, can quick and precisely simulate the method for 7 heavy metal species content in artificial suction mensuration cigarette smoke.
Purpose of the present invention is achieved through the following technical solutions.
Except as otherwise noted, percentage of the present invention is mass percent.
A kind of smoke gathering device of manual imitation smoking cigarette, comprise bottle,suction and suction filter pump, it is characterized in that: described bottle,suction is communicated with by suction filtering tube with described suction filter pump; Be provided with opening on sidewall more than described bottle,suction medium position, at opening part, be sealed and installed with glass tube; The bottle mouth position of described bottle,suction lays one deck cotton.
Wherein, one deck cotton is laid at described suction filtering tube mouth of pipe place.
A kind of method of 7 heavy metal species in rapid and accurate determination flue gas comprises the following steps:
(1) absorption liquid preparation:
1. accurately take sodium chloride 1.0g, potassium chloride 1.0g, magnesium chloride 0.05g, lime chloride 0.8g, sodium hydrogen phosphate 0.8g, sodium carboxymethyl cellulose 10g, glycoprotein 0.1g, ptyalin 0.1g and nipalgin 0.3g, measure distilled water 1L, standby;
2. measure 700mL distilled water, add sodium carboxymethyl cellulose, immersion adds sodium chloride, potassium chloride, magnesium chloride, lime chloride after its swelling again, glycoprotein, ptyalin and nipalgin, add sodium dihydrogen phosphate after stirring and dissolving, and add residue distilled water, stir evenly rear use 0.01% hydrochloric acid or 0.05% NaOH and be adjusted to pH=7, the flowing steam sterilization that is 100 ℃ by temperature after bottling 30 minutes, obtain absorption liquid;
(2) sample solution preparation:
Measuring absorption liquid 100mL is placed in the bottle,suction of smoke gathering device, after taking single cigarette weight, cigarette filter is inserted to glass tube lighting cigarette, open suction filter pump, flue gas enters bottle,suction by glass tube, the cigarette afterburnt is closed suction filter pump, after flue gas is absorbed liquid and absorbs fully, measure the absorption liquid of 50mL containing flue gas, be placed in the 50mL sample bottle to be measured; According to the combustion case of cigarette, regulating the suction filter pump flow is 0.6-1.5L/min, guarantees cigarette after-flame within 5-10 minute;
(3) 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 measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be 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 measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
3. the foundation of copper standard working curve: compound concentration is 10 μ g/g, 20 μ g/g, and 30 μ g/g,, 40 μ g/g, the copper typical curve sample of 50 μ g/g, solvent is deionized water; Copper typical curve sample is measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
4. the foundation of zinc 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; Zinc typical curve sample is measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
5. 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 measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
6. 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 measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
7. the foundation of mercury standard working curve: compound concentration is 1 μ g/g, 2 μ g/g, and 5 μ g/g,, 10 μ g/g, the cadmium typical curve sample of 15 μ g/g, solvent is deionized water; Mercury typical curve sample is measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
(4) detect:
Sample solution is imported in inductively coupled plasma emission spectrum mass spectrometer and detected, read the content of cigarette sample heavy metal in flue gas to be measured, reading is ρ (flue gas), and condition determination is as table 1,
Table 1ICP-MS instrumental analysis condition:
(5) computing method:
The c(flue gas)=ρ (flue gas) * 0.05/m(cigarette), the μ g/g of unit
With respect to prior art, the present invention has the following advantages:
1, trapping flue gas to detect content of beary metal wherein be a key and the technology of difficulty.In international up-to-date detection cigarette smoke, heavy metal adopts Fume collector, and this Fume collector relies on import, 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 flue gas fully.Based on this actual conditions, the present invention imitates water pipe structure among the people, invented easy aspirator, and designed absorption liquid according to the principal ingredient of human saliva, utilize the most effective mode to trap the flue gas heavy metal entered in human body in the manual imitation mode, the harm of having avoided artificial suction to bring.
2, inductivity coupled plasma mass spectrometry ICP/MS method (inductively coupled plasma mass spectrometry) is to take the mass spectrometry that inductively coupled plasma (ICP) is ionization source.This technology has overcome AAS and UV-VIS spectrophotometry can not detect multiple element simultaneously, and ICP-AES method spectrum serious interference, should not measure the shortcoming of the elements such as arsenic, cadmium, mercury, can carry out the analysis of most heavy metal elements simultaneously, there is the advantages such as detection sensitivity is high, detection limit is low, linear detection range is wide.The present invention adopts the ICP-MS method to measure the Pb in the flue gas, Cd, Cu, Zn, As simultaneously, As, and the content of Cr, at Accurate Determining, reduce costs and be widely used three aspects and found the most reasonably configuration.
The accompanying drawing explanation
The structural representation that Fig. 1 is smoke gathering device of the present invention.
In figure: 1-bottle,suction, 2-suction filter pump, 3-suction filtering tube, 4-glass tube, 5-cotton.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.Should be appreciated that specific embodiment described herein, only in order to explain analysis condition technical essential of the present invention, is not intended to limit the present invention.
The main agents of using and instrument:
(top grade is pure for sodium chloride, Guangdong chemical reagent two factories), (top grade is pure for potassium chloride, Guangdong chemical reagent two factories), (top grade is pure for magnesium chloride, Guangdong chemical reagent two factories), (top grade is pure for lime chloride, Guangdong chemical reagent two factories), (top grade is pure for sodium hydrogen phosphate, Guangdong chemical reagent two factories), (top grade is pure for sodium carboxymethyl cellulose, Guangdong chemical reagent two factories), (top grade is pure for sodium carboxymethyl cellulose, Guangdong chemical reagent two factories), (top grade is pure for glycoprotein, Guangdong chemical reagent two factories), (top grade is pure for ptyalin, Guangdong chemical reagent two factories), nipalgin (Chemical Industry in Guangzhou import and export corporation) ultrapure water (18.2M Ω/cm, Beijing UPW-20N of company's epoch type Superpure water machine self-control), plumbous, cadmium, copper, zinc, arsenic, chromium, mercury standard solution (national standardization material research centre, 1000 μ g/g), high-purity Ar 2, ELAN9000 inductivity coupled plasma mass spectrometry (ICP-MS) instrument (U.S. Perkin Elmer SCIEX company), vacuum filtration pump (Shanghai Ling De Instrument Ltd.), analytical balance (sensibility reciprocal 0.1mg).
The glassware used all soaks and goes metal to process through 10%HNO3; 10 kinds of common cigarette samples.
As shown in Figure 1, the smoke gathering device of manual imitation smoking cigarette used in the present embodiment, comprise bottle,suction 1 and suction filter pump 2, and described bottle,suction 1 is communicated with by suction filtering tube 3 with described suction filter pump 2, and the position of suction filtering tube 3 is more than described bottle,suction 1 centre position; Be provided with opening on sidewall more than described bottle,suction 1 medium position, at opening part, be sealed and installed with glass tube 4, for cigarette 6 is installed; The bottle mouth position of described bottle,suction 1 lays one deck cotton 5; One deck cotton 5 is laid at described suction filtering tube 3 mouth of pipe places, and the effect of laying cotton 5 can seal flue gas after being to soak with absorption liquid.
Measure the method for 7 heavy metal species in the flue gas trapped by above-mentioned smoke gathering device in the present embodiment, comprise the following steps:
1. absorption liquid preparation
Absorption liquid is for simulated saliva, and concrete compound method is:
1.1 accurately take sodium chloride 1.0g, potassium chloride 1.0g, magnesium chloride 0.05g, lime chloride 0.8g, sodium hydrogen phosphate 0.8g, sodium carboxymethyl cellulose 10g, glycoprotein 0.1g, ptyalin 0.1g and nipalgin 0.3g, measure distilled water 1L, standby.
1.2 measure 700mL distilled water, add sodium carboxymethyl cellulose, immersion adds sodium chloride, potassium chloride, magnesium chloride, lime chloride after its swelling again, glycoprotein, ptyalin and nipalgin, add sodium dihydrogen phosphate after stirring and dissolving, and add residue distilled water, stir evenly rear use 0.01% hydrochloric acid or 0.05% NaOH and be adjusted to pH=7, the flowing steam sterilization that is 100 ℃ by temperature after bottling 30 minutes, obtain absorption liquid.
2. sample solution preparation
Be placed in the bottle,suction of smoke gathering device 2.1 measure absorption liquid 100mL, guarantee that the surface level of absorption liquid is lower than glass tube and suction filtering tube nozzle position.
2.2 will be laid in the cotton of bottle,suction 1 bottleneck, suction filtering tube 3 mouths of pipe, with absorption liquid, infiltrate, to seal flue gas.
2.3 after taking single cigarette weight (m), cigarette filter is inserted to glass tube 4 lighting cigarette, open suction filter pump 2, flue gas enters bottle,suction 1 by glass tube 4, the cigarette afterburnt is closed suction filter pump 2, after flue gas is absorbed liquid and absorbs fully, measure the absorption liquid of 50mL containing flue gas, be placed in the 50mL sample bottle to be measured; According to the combustion case of cigarette, the flow of regulating suction filter pump is 0.6-1.5L/min, guarantees cigarette after-flame within 5-10 minute.
3. the foundation of standard working curve
3.1 the foundation of plumbous standard working curve
3.1.1 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.
3.1.2 get respectively the plumbous standard solution 10ml of 100 μ g/g, 20ml, 30ml, 40ml, 50ml is in the 100ml volumetric flask, and it is 10 μ g/g that constant volume obtains concentration, 20 μ g/g, 30 μ g/g, 40 μ g/g, the plumbous typical curve sample of 50 μ g/g.
3.1.3 plumbous typical curve sample is measured in ICP-MS is upper, obtain standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999.
3.2 the foundation of cadmium standard working curve
3.2.1 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.
3.2.2 get respectively the cadmium standard solution 10ml of 100 μ g/g, 20ml, 30ml, 40ml, 50ml is in the 100ml volumetric flask, and it is 10 μ g/g that constant volume obtains concentration, 20 μ g/g, 30 μ g/g, 40 μ g/g, the cadmium typical curve sample of 50 μ g/g.
3.2.3 cadmium typical curve sample is measured in ICP-MS is upper, obtain standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999.
3.3 the foundation of copper standard working curve
3.3.1 get 1000 μ g/g copper standard solution 20ml, distilled water is settled to 200ml, makes the copper standard solution of 100 μ g/g.
3.3.2 get respectively the copper standard solution 10ml of 100 μ g/g, 20ml, 30ml, 40ml, 50ml is in the 100ml volumetric flask, and it is 10 μ g/g that constant volume obtains concentration, 20 μ g/g, 30 μ g/g, 40 μ g/g, the copper typical curve sample of 50 μ g/g.
3.3.3 copper typical curve sample is measured in ICP-MS is upper, obtain standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999.
3.4 the foundation of zinc standard working curve
3.4.1 get 1000 μ g/g Zinc standard solution 20ml, distilled water is settled to 200ml, makes the Zinc standard solution of 100 μ g/g.
3.4.2 get respectively the Zinc standard solution 10ml of 100 μ g/g, 20ml, 30ml, 40ml, 50ml is in the 100ml volumetric flask, and it is 10 μ g/g that constant volume obtains concentration, 20 μ g/g, 30 μ g/g, 40 μ g/g, the zinc typical curve sample of 50 μ g/g.
3.4.3 zinc typical curve sample is measured in ICP-MS is upper, obtain standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999.
3.5 the foundation of arsenic standard working curve
3.5.1 get 1000 μ g/g arsenic standard solution 20ml, distilled water is settled to 200ml, makes the arsenic standard solution of 100 μ g/g.
3.5.2 get respectively the arsenic standard solution 10ml of 100 μ g/g, 20ml, 30ml, 40ml, 50ml is in the 100ml volumetric flask, and it is 10 μ g/g that constant volume obtains concentration, 20 μ g/g, 30 μ g/g, 40 μ g/g, the arsenic typical curve sample of 50 μ g/g.
3.5.3 arsenic typical curve sample is measured in ICP-MS is upper, obtain standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999.
3.6 the foundation of chromium standard working curve
3.6.1 get 1000 μ g/g chromium standard solution 20ml, distilled water is settled to 200ml, makes the chromium standard solution of 100 μ g/g.
3.6.2 get respectively the chromium standard solution 10ml of 100 μ g/g, 20ml, 30ml, 40ml, 50ml is in the 100ml volumetric flask, and it is 10 μ g/g that constant volume obtains concentration, 20 μ g/g, 30 μ g/g, 40 μ g/g, the chromium typical curve sample of 50 μ g/g.
3.6.3 chromium typical curve sample is measured in ICP-MS is upper, obtain standard working curve, curve is strong
System makes zero, linearly dependent coefficient R
2need be greater than 0.999.
3.7 the foundation of mercury standard working curve
3.7.1 get 1000 μ g/g mercury standard solution 20ml, distilled water is settled to 200ml, makes the mercury standard solution of 100 μ g/g.
3.7.2 get respectively the mercury standard solution 10ml of 100 μ g/g, 20ml, 30ml, 40ml, 50ml is in the 100ml volumetric flask, and it is 10 μ g/g that constant volume obtains concentration, 20 μ g/g, 30 μ g/g, 40 μ g/g, the mercury typical curve sample of 50 μ g/g.
3.7.3 mercury typical curve sample is measured in ICP-MS is upper, obtain standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999.
4. detect
Sample solution is imported in inductively coupled plasma emission spectrum mass spectrometer and detected, read the content of cigarette sample heavy metal in flue gas to be measured, reading is ρ (flue gas), and condition determination is as table 1,
Table 1ICP-MS instrumental analysis condition:
5. computing method
The c(flue gas)=ρ (flue gas) * 0.05/m(cigarette), the μ g/g of unit
6. method evaluation
Do contrast 6.1 utilize import Fume collector-ICP-MS method to measure to relevant producer the flue gas content of absorption liquid (artificial saliva) absorption measurement, result is as follows:
Table 2.2 kind of method is measured the Pb in flue gas
6.2 as can be seen from Table 2, with flue gas trapping equipment, compare, the present invention can absorb in flue gas 87.9% lead content, and the correlation ratio of most of sample is all between 80%-90%, the coefficient of variation is low, and the present invention is for be absorbed by the body content with a high credibility of Pb of flue gas.
Table 32 kind of method is measured the Cd in flue gas
6.3 as can be seen from Table 3, with flue gas trapping equipment, compare, the present invention can absorb in flue gas 80.7% cadmium content, and wherein the correlation ratio of 6 kinds of samples has all surpassed 80%, the coefficient of variation is extremely low, and the present invention is for measuring be absorbed by the body content with a high credibility of Cd of flue gas.
Table 42 kind of method is measured the Cu in flue gas
6.4 as can be seen from Table 4, with flue gas trapping equipment, compare, the present invention can absorb in flue gas 80.5% copper content, and wherein the correlation ratio of 7 kinds of samples has all surpassed 80%, the coefficient of variation is extremely low, and the present invention is for measuring be absorbed by the body content with a high credibility of Cu of flue gas.
Table 52 kind of method is measured the Zn in flue gas
6.5 as can be seen from Table 5, with flue gas trapping equipment, compare, the present invention can absorb in flue gas 77.0% zinc content, and wherein the correlation ratio of all samples has all surpassed 70%, the coefficient of variation is extremely low, and the present invention is high for measuring the be absorbed by the body confidence level of content of Zn of flue gas.
Table 62 kind of method is measured the As in flue gas
6.6 as can be seen from Table 6, with flue gas trapping equipment, compare, the present invention can absorb in flue gas 84.8% arsenic content, and wherein the correlation ratio of 8 samples has all surpassed 80%, the coefficient of variation is extremely low, and the present invention is high for measuring the be absorbed by the body confidence level of content of As of flue gas.
Table 72 kind of method is measured the Cr in flue gas
6.7 as can be seen from Table 7, with flue gas trapping equipment, compare, the present invention can absorb in flue gas 85.3% chromium content, and wherein the correlation ratio of 8 samples has all surpassed 80%, the coefficient of variation is low, and the present invention is for measuring be absorbed by the body content with a high credibility of Cr of flue gas.
Table 82 kind of method is measured the Hg in flue gas
6.8 as can be seen from Table 8, with flue gas trapping equipment, compare, the present invention can absorb in flue gas 83.8% mercury content, and wherein the correlation ratio of 6 samples has all surpassed 80%, the coefficient of variation is low, and the present invention is for measuring be absorbed by the body content with a high credibility of Hg of flue gas.
Result shows: artificial suction method can't complete this test.
Result shows: partial detection is extremely low, and part can't detect, and illustrates that the effect of heavy metal in distilled water trapping cigarette smoke is bad.
Result shows: the 50ml absorption liquid absorbs with the 100ml absorption liquid and absorbs and compare, and detection level is on the low side, and the 50ml absorption liquid fails more fully to absorb the heavy metal in cigarette smoke.
Result shows: the 200ml absorption liquid is consistent with 100ml absorption liquid content of beary metal, and 100ml is optimal absorption liquid consumption.
Result shows: testing result is consistent, but people's saliva is difficult to obtain, and apt to deteriorate, poor practicability.
Claims (3)
1. the smoke gathering device of a manual imitation smoking cigarette, comprise bottle,suction and suction filter pump, it is characterized in that: described bottle,suction is communicated with by suction filtering tube with described suction filter pump; Be provided with opening on sidewall more than described bottle,suction medium position, at opening part, be sealed and installed with glass tube; The bottle mouth position of described bottle,suction lays one deck cotton.
2. smoke gathering device according to claim 1, it is characterized in that: one deck cotton is laid at described suction filtering tube mouth of pipe place.
3. the method for 7 heavy metal species in a rapid and accurate determination flue gas comprises the following steps:
(1) absorption liquid preparation:
1. accurately take sodium chloride 1.0g, potassium chloride 1.0g, magnesium chloride 0.05g, lime chloride 0.8g, sodium hydrogen phosphate 0.8g, sodium carboxymethyl cellulose 10g, glycoprotein 0.1g, ptyalin 0.1g and nipalgin 0.3g, measure distilled water 1L, standby;
2. measure 700mL distilled water, add sodium carboxymethyl cellulose, immersion adds sodium chloride, potassium chloride, magnesium chloride, lime chloride after its swelling again, glycoprotein, ptyalin and nipalgin, add sodium dihydrogen phosphate after stirring and dissolving, and add residue distilled water, stir evenly rear use 0.01% hydrochloric acid or 0.05% NaOH and be adjusted to pH=7, the flowing steam sterilization that is 100 ℃ by temperature after bottling 30 minutes, obtain absorption liquid;
(2) sample solution preparation:
Measuring absorption liquid 100mL is placed in the bottle,suction of smoke gathering device claimed in claim 2, after taking single cigarette weight, cigarette filter is inserted to glass tube lighting cigarette, open suction filter pump, the flow of regulating suction filter pump is 0.6-1.5L/min, flue gas enters bottle,suction by glass tube, and the cigarette afterburnt is closed suction filter pump, after flue gas is absorbed liquid and absorbs fully, measure the absorption liquid of 50mL containing flue gas, be placed in the 50mL sample bottle to be measured;
(3) 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 measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be 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 measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
3. the foundation of copper standard working curve: compound concentration is 10 μ g/g, 20 μ g/g, and 30 μ g/g,, 40 μ g/g, the copper typical curve sample of 50 μ g/g, solvent is deionized water; Copper typical curve sample is measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
4. the foundation of zinc 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; Zinc typical curve sample is measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
5. 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 measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
6. 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 measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
7. the foundation of mercury standard working curve: compound concentration is 1 μ g/g, 2 μ g/g, and 5 μ g/g,, 10 μ g/g, the cadmium typical curve sample of 15 μ g/g, solvent is deionized water; Mercury typical curve sample is measured in ICP-MS is upper, obtained standard working curve, curve is forced to make zero, linearly dependent coefficient R
2need be greater than 0.999;
(4) detect:
Sample solution is imported in inductively coupled plasma emission spectrum mass spectrometer and detected, read the content of cigarette sample heavy metal in flue gas to be measured, reading is ρ (flue gas), and condition determination is as table 1,
Table 1ICP-MS instrumental analysis condition:
(5) computing method:
The c(flue gas)=ρ (flue gas) * 0.05/m(cigarette), the μ g/g of unit.
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| CN104215486A (en) * | 2014-09-12 | 2014-12-17 | 云南中烟工业有限责任公司 | Cigarette paper combustion product capturing method for biological detection |
| 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 |
| 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 |
| CN104634707A (en) * | 2015-02-13 | 2015-05-20 | 湖南中烟工业有限责任公司 | Method for detecting forms of trace metal particles in smoke based on plasma inductively-coupled atomic absorption spectrum |
| CN104713752A (en) * | 2015-03-31 | 2015-06-17 | 云南中烟工业有限责任公司 | Smoke collecting device and smoke collecting method for evaluating biological effects of electronic cigarette smoke |
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| CN105866232A (en) * | 2015-01-19 | 2016-08-17 | 上海市食品药品检验所 | Methods for determining total amount mercury and valence mercury content in biological tissues and organs |
| CN106198708A (en) * | 2016-08-11 | 2016-12-07 | 深圳瀚星翔科技有限公司 | The detection method of the content of heavy metal in electronic cigarette atomizing vapour |
| CN108226136A (en) * | 2018-01-26 | 2018-06-29 | 福州大学 | A kind of device and its application method of quick detection Nicotine in Tobacco content |
| CN108982691A (en) * | 2018-07-25 | 2018-12-11 | 舟山市食品药品检验检测研究院 | Arsenic mercury shape simultaneous quantitative determination in aquatic products |
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| CN104215486A (en) * | 2014-09-12 | 2014-12-17 | 云南中烟工业有限责任公司 | Cigarette paper combustion product capturing method for biological detection |
| 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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| CN104764791A (en) * | 2015-03-27 | 2015-07-08 | 云南中烟工业有限责任公司 | Device and method for realtime on-line analysis of heavy metal in electronic cigarette smoke |
| CN104713752B (en) * | 2015-03-31 | 2017-09-22 | 云南中烟工业有限责任公司 | A kind of smoke gathering device evaluated for electronic cigarette flue gas biological effect and method |
| CN104713752A (en) * | 2015-03-31 | 2015-06-17 | 云南中烟工业有限责任公司 | Smoke collecting device and smoke collecting method for evaluating biological effects of electronic cigarette smoke |
| CN106198708A (en) * | 2016-08-11 | 2016-12-07 | 深圳瀚星翔科技有限公司 | The detection method of the content of heavy metal in electronic cigarette atomizing vapour |
| CN108226136A (en) * | 2018-01-26 | 2018-06-29 | 福州大学 | A kind of device and its application method of quick detection Nicotine in Tobacco content |
| CN108982691A (en) * | 2018-07-25 | 2018-12-11 | 舟山市食品药品检验检测研究院 | Arsenic mercury shape simultaneous quantitative determination in aquatic products |
| CN111964985A (en) * | 2019-05-20 | 2020-11-20 | 湖南中烟工业有限责任公司 | Device and method for trapping fresh smoke of cigarettes |
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