CN102175753B - Method for measuring transfer rate of solid filter tip additive of cigarette in main stream smoke - Google Patents
Method for measuring transfer rate of solid filter tip additive of cigarette in main stream smoke Download PDFInfo
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- CN102175753B CN102175753B CN 201110006960 CN201110006960A CN102175753B CN 102175753 B CN102175753 B CN 102175753B CN 201110006960 CN201110006960 CN 201110006960 CN 201110006960 A CN201110006960 A CN 201110006960A CN 102175753 B CN102175753 B CN 102175753B
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Abstract
The invention discloses a method for measuring the transfer rate of a solid filter tip additive of a cigarette in main stream smoke, and the method comprises the following steps: selecting a component element in the solid filter tip additive of the cigarette as a target element; collecting particle-phase substances in the main stream smoke of the cigarette by utilizing an electrostatic catcher; and measuring the content of the target element in the collected particle-phase substances by adopting an inductive coupling plasma mass spectrometry, thereby realizing the quantitative detection of the transfer rate of the solid filter tip additive of the cigarette in the main stream smoke and further judging the possibility that the solid filter tip additive of the cigarette escapes along with air current and is sucked into a human body. The method disclosed by the invention is accurate, reliable, simple and convenient and has important guide values in the development of the solid filter tip additive of the cigarette.
Description
Technical field
The present invention relates to the assay method that cigarette filter-tip additive agent is overflowed with flue gas and sucked human body; Be specifically related to the assay method of the solid-state additives of filter tip of a kind of cigarette rate of transform in main flume, can judge according to this that the solid-state additives of filter tip of cigarette overflows with air-flow and suck the possibility into human body.
Background technology
Smoking has become society and the medical problem that people generally pay attention to, and the research that reduces objectionable impurities in the tobacco is all being actively developed in countries in the world.The improvement filter tip that employing contains adjuvant is a kind of important cigarette harm reduction means.By the difference of additive types, the improvement filter tip mainly can be divided into several kinds of active carbon filter, aluminosilicate filter tip, bio-additive filter tip and catalyzer filter tips etc.At present, the improvement filter tip accounts for about 10% of the cigarette market share.Above-mentioned employed different additives of filter tip, what have is harmless, have get into oral cavity or respiratory tract with main flume after human body is had toxic action, the effect to human body that has it be unclear that.After human body had toxic action and at present the unknown additives of filter tip of human body effect is applied to production of cigarettes, should investigate its rate of transform in cigarette mainstream flue gas, promptly investigate it and overflow with air-flow and suck possibility into human body from filter tip.Research for the solid-state additives of filter tip of cigarette at present mainly concentrates on preparation method and harm reduction effect aspect, how to measure additives of filter tip and does not appear in the newspapers as yet from the analytical approach that filter tip shifts in cigarette mainstream flue gas.
Summary of the invention
The objective of the invention is to the prior art situation, specialized designs a kind of simple and convenient, assay method of the solid-state additives of filter tip of cigarette rate of transform in main flume accurately and reliably.
The objective of the invention is to realize like this: the assay method of the solid-state additives of filter tip of a kind of cigarette rate of transform in main flume; This method is chosen a certain component in the cigarette filter-tip additive agent of solid granular or solid powdery as object element; This object element should be content in the cigarette smoke lower, simultaneously can be by the element that inductively coupled plasma mass spectrometry detected, object element is mainly: Mg, Al, Mn, Fe, Co, Ni, Zn or Pd; Utilize the static drip catcher to collect the granule phase substance matter in the main flume; Adopt inductively coupled plasma mass spectrometry to measure the content of object element in the collected granule phase substance matter then; Thereby realize detection by quantitative, judge that according to this solid-state additives of filter tip of cigarette overflows with air-flow and suck the possibility into human body the solid-state additives of filter tip of cigarette rate of transform in main flume;
Concrete steps are following:
1) cigarette props up preparation:
Used cigarette sample adds the cigarette Zhi Zuowei lab rolls cigarette sample of 1-60mg/ cigarette solid additives through weight and resistance to suction sorting in filter tip, the cigarette that does not add solid additives in the filter tip props up and is the contrast cigarette sample;
2) granule phase substance matter is collected in the flue gas:
Cigarette props up by the GB/T19609-2004 standard and after smoking machine burns and sucks, utilizes the static drip catcher to collect the granule phase substance matter in the main flume, and static drip catcher WV is 10-25kV;
3) sample pretreatment:
The granule phase substance matter of collecting in the static drip catcher with 20～80mL methanol solution wash-out, is transferred to eluent in the counteracting tank; Counteracting tank is placed 80～120 ℃ of heating down, make solvent evaporates to 1～2mL; Add 3～5mL 65%HNO
3, react 20～40min down at 90 ℃; Add 1～3mL 65%HNO
3, 1～2mL30%H
2O
2, 0.2mL 40%HF, clear up by the program of setting of clearing up, clearing up program is that room temperature is warming up to 110 ℃ through 5min, insulation 5min is warming up to 160 ℃ through 5min then, insulation 5min is warming up to 190 ℃ through 10min then, insulation 25min; Clear up after the end sample transfer to the 50mL volumetric flask, add 2mL 2% boric acid,, be settled to 50mL with ultrapure water then, promptly obtain testing sample solution at 85～100 ℃ of insulation 5～15min down; Simultaneously, adopt above-mentioned same fully method that the cigarette Zhi Jinhang that does not add adjuvant in the filter tip is handled, preparation contrast cigarette sample solution;
4) drafting of typical curve:
The series standard solution of preparation object element detects each standard liquid with inductively coupled plasma mass spectrometry, and draws the calibration curve of this object element based on testing result;
5) object element detects:
Testing sample solution and control sample solution are detected with inductively coupled plasma mass spectrometry successively, according to the concentration of object element in the typical curve calculation sample of object element;
6) rate of transform is calculated: be calculated as follows the rate of transform of the solid-state additives of filter tip of cigarette in main flume:
Wherein: TP%: the rate of transform of the solid-state additives of filter tip of cigarette in main flume, percentage by weight;
C
1: the object element detectable concentration of contrast cigarette sample, mg/L;
C
2: the object element detectable concentration of experiment cigarette sample, mg/L;
N: suction cigarette number;
M: the solid additives weight that adds in every cigarette, mg;
C
M: the content of object element in the solid-state additives of filter tip, percentage by weight.
The present invention be directed to the situation of above-mentioned prior art; And it is at present domestic as yet not to the report of the solid-state additives of filter tip of cigarette rate of transform in main flume; Specialized designs the assay method of the solid-state additives of filter tip of a kind of cigarette rate of transform in main flume; The component that this method is passed through to select the suitable solid-state additives of filter tip of cigarette is as object element; Utilize the static drip catcher to collect the granule phase substance matter in the cigarette mainstream flue gas, realize quantitative measurement the rate of transform of the solid-state additives of filter tip of cigarette in main flume through inductivity coupled plasma mass spectrometry (ICP-MS) method.
The present invention chooses a certain component in the cigarette filter-tip additive agent of solid granular or solid powdery as object element; This object element should be the element lower, that can be detected by the ICP-MS method simultaneously of content in the cigarette smoke, and object element mainly comprises Mg, Al, Mn, Fe, Co, Ni, Zn, Pd.Utilize the static drip catcher to collect the granule phase substance matter in the main flume; Adopt the ICP-MS method to measure the content of object element in the collected granule phase substance matter then; Thereby realize detection by quantitative, judge that according to this solid-state additives of filter tip of cigarette overflows with air-flow and suck the possibility into human body the solid-state additives of filter tip of cigarette rate of transform in main flume.
The invention has the beneficial effects as follows: utilize the static drip catcher to collect the granule phase substance matter in the main flume, reduce the pollution of object element in the flue gas granule phase substance matter collection process as far as possible and disturb; Select content in the cigarette smoke lower, simultaneously can be by the component of inductivity coupled plasma mass spectrometry (ICP-MS) the solid-state additives of filter tip of cigarette that method detected as object element, can the rate of transform of the solid-state additives of filter tip of quantitative response cigarette in main flume; Analytical approach accurately and reliably, simple and convenient, can judge according to this that the solid-state additives of filter tip of cigarette overflows with air-flow and suck the possibility into human body, result of study has important guiding value to the exploitation of the solid-state additives of filter tip of cigarette.
Embodiment
Make further detailed description in the face of the present invention down, but following examples are illustrative, are not determinate, can not limit protection scope of the present invention with this.
Embodiment:
Select Si-Al molecular sieve certain trade mark cigarette as cigarette filter-tip additive agent, wherein the content of aluminium element in the Si-Al molecular sieve sample is 3.76%, and present embodiment selects Al as object element.
1. cigarette props up preparation: used cigarette sample adds the cigarette Zhi Zuowei lab rolls cigarette sample of 5mg/ cigarette solid additives through weight and resistance to suction sorting in filter tip, and the cigarette that does not add solid additives in the filter tip props up and is the contrast cigarette sample.
2. granule phase substance matter is collected in the flue gas: cigarette props up by the GB/T19609-2004 standard and after smoking machine burns and sucks, utilizes the static drip catcher to collect the granule phase substance matter in the main flume, and static drip catcher WV is 17kV.
3. sample pretreatment: the granule phase substance matter of collecting in the static drip catcher with 40mL methanol solution wash-out, is transferred to eluent in the counteracting tank; Counteracting tank is placed 90 ℃ of heating down, make solvent evaporates to 1mL; Add 4mL 65%HNO
3, react 30min down at 90 ℃; Add 2mL 65%HNO
3, 1.5mL 30%H
2O
2, 0.2mL 40%HF, clear up by the program of setting of clearing up, clearing up program is that room temperature is warming up to 110 ℃ through 5min, insulation 5min is warming up to 160 ℃ through 5min then, insulation 5min is warming up to 190 ℃ through 10min then, insulation 25min; Clear up after the end sample transfer to the 50mL volumetric flask, add 2mL 2% boric acid,, be settled to 50mL with ultrapure water then, be mixed with testing sample solution at 95 ℃ of insulation 10min down; Preparation control sample solution uses the same method.
4. standard solution configuration: precision is measured 0.1mL, 0.3mL, 0.5mL, 0.7mL, and the 10mg/L aluminum standard solution places the 50mL volumetric flask that has been added with 2mL 2% boric acid respectively, uses 5%HNO then
3Constant volume shakes up to 50mL, processes concentration and is respectively 0.02mg/L, 0.06mg/L, 0.10mg/L, 0.14mg/L standard solution.
5. object element detects: each concentration standard solution and testing sample solution are detected with ICP-MS successively, according to the concentration of object element in the typical curve calculation sample solution of object element.
Testing result is as shown in the table:
6. the rate of transform is calculated: be calculated as follows the rate of transform of the solid-state additives of filter tip of cigarette in main flume:
＝{(0.0662-0.0652)*0.05}/{20*5*0.0376}
＝0.0013%
Wherein: TP%: the rate of transform of the solid-state additives of filter tip of cigarette in main flume, percentage by weight;
C
1: the object element detectable concentration of contrast cigarette sample, mg/L;
C
2: the object element detectable concentration of experiment cigarette sample, mg/L;
N: suction cigarette number;
M: the solid additives weight that adds in every cigarette, mg;
C
M: the content of object element in the solid-state additives of filter tip, percentage by weight.
Claims (2)
1. the assay method of the solid-state additives of filter tip of cigarette rate of transform in main flume; It is characterized in that; This method is chosen a certain component in the cigarette filter-tip additive agent of solid granular or solid powdery as object element; This object element should be content in the cigarette smoke lower, simultaneously can be by the element that inductively coupled plasma mass spectrometry detected, object element is: Mg, Al, Mn, Fe, Co, Ni, Zn or Pd; Utilize the static drip catcher to collect the granule phase substance matter in the main flume; Adopt inductively coupled plasma mass spectrometry to measure the content of object element in the collected granule phase substance matter then; Thereby realize detection by quantitative, judge that according to this solid-state additives of filter tip of cigarette overflows with air-flow and suck the possibility into human body the solid-state additives of filter tip of cigarette rate of transform in main flume;
Concrete steps are following:
1) cigarette props up preparation:
Used cigarette sample adds the cigarette Zhi Zuowei lab rolls cigarette sample of 1-60 mg/ cigarette solid additives through weight and resistance to suction sorting in filter tip, the cigarette that does not add solid additives in the filter tip props up and is the contrast cigarette sample;
2) granule phase substance matter is collected in the flue gas:
Cigarette props up by the GB/T19609-2004 standard and after smoking machine burns and sucks, utilizes the static drip catcher to collect the granule phase substance matter in the main flume, and static drip catcher WV is 10-25 kV;
3) sample pretreatment:
The granule phase substance matter of collecting in the static drip catcher with 20～80 mL methanol solution wash-outs, is transferred to eluent in the counteracting tank; Counteracting tank is placed 80～120 ℃ of heating down, make solvent evaporates to 1～2 mL; Add 3～5 mL, 65% HNO
3, react 20～40 min down at 90 ℃; Add 1～3 mL, 65% HNO
3, 1～2 mL, 30% H
2O
2, 0.2 mL, 40% HF, clear up by the program of setting of clearing up, clearing up program is that room temperature is warming up to 110 ℃ through 5 min; Be incubated 5 min, be warming up to 160 ℃ through 5 min then, be incubated 5 min; Be warming up to 190 ℃ through 10 min then, be incubated 25 min; Clear up after the end in sample transfer to the 50 mL volumetric flask, add 2 mL, 2% boric acid,, be settled to 50 mL with ultrapure water then, promptly obtain testing sample solution at 85～100 ℃ of insulation 5～15 min down; Simultaneously, adopt above-mentioned same fully method that the cigarette Zhi Jinhang that does not add adjuvant in the filter tip is handled, preparation contrast cigarette sample solution;
4) drafting of typical curve:
The series standard solution of preparation object element detects each standard liquid with inductively coupled plasma mass spectrometry, and draws the calibration curve of this object element based on testing result;
5) object element detects:
Testing sample solution and control sample solution are detected with inductively coupled plasma mass spectrometry successively, according to the concentration of object element in the typical curve calculation sample of object element;
6) rate of transform is calculated: be calculated as follows the rate of transform of the solid-state additives of filter tip of cigarette in main flume:
TP%?＝
Wherein: TP%: the rate of transform of the solid-state additives of filter tip of cigarette in main flume, percentage by weight;
C
1: the object element detectable concentration of contrast cigarette sample, mg/L;
C
2: the object element detectable concentration of experiment cigarette sample, mg/L;
N: suction cigarette number;
M: the solid additives weight that adds in every cigarette, mg;
C
M: the content of object element in the solid-state additives of filter tip, percentage by weight.
2. the assay method of the solid-state additives of filter tip of cigarette according to claim 1 rate of transform in main flume is characterized in that the solid-state additives of filter tip of said cigarette is a Si-Al molecular sieve, and its component Al is as object element; Concrete steps are following:
1) cigarette props up preparation:
Used cigarette sample adds the cigarette Zhi Zuowei testing sample of 1 –, 50 mg/ cigarette Si-Al molecular sieves through weight and resistance to suction sorting in filter tip, the cigarette that does not add solid additives in the filter tip props up and is control sample;
2) granule phase substance matter is collected in the flue gas:
Cigarette props up and after smoking machine burns and sucks, is utilizing the static drip catcher to collect the granule phase substance matter in the main flume under the GB/T19609-2004 standard aspiration condition, and static drip catcher WV is 17 kV;
3) sample pretreatment:
The granule phase substance matter of collecting in the static drip catcher with 40 mL methanol solution wash-outs, is transferred to eluent in the counteracting tank; Counteracting tank is placed 90 ℃ of heating down, make solvent evaporates to 1 mL; Add 4 mL, 65% HNO
3, react 30 min down at 90 ℃; Add 2 mL, 65% HNO
3, 1.5 mL, 30% H
2O
2, 0.2 mL, 40% HF, clear up by the program of setting of clearing up, clearing up program is that room temperature is warming up to 110 ℃ through 5 min; Be incubated 5 min, be warming up to 160 ℃ through 5 min then, be incubated 5 min; Be warming up to 190 ℃ through 10 min then, be incubated 25 min; Clear up after the end in sample transfer to the 50 mL volumetric flask; Add 2 mL, 2% boric acid; Be incubated 10 min down at 95 ℃, be settled to 50 mL and be formulated as testing sample solution with ultrapure water then, simultaneously; Adopt above-mentioned identical method that the cigarette Zhi Jinhang that does not add adjuvant in the filter tip is handled, preparation control sample solution;
4) typical curve is drawn: precision is measured 0.1 mL, 0.3 mL, 0.5 mL, 0.7 mL, and 10 mg/L aluminum standard solutions place the 50 mL volumetric flasks that have been added with 2 mL, 2% boric acid respectively, use 5% HNO then
3Constant volume is to 50 mL; Shake up; Process concentration and be respectively 0.02 mg/L, 0.06 mg/L, 0.10 mg/L, 0.14 mg/L standard solution, each standard solution is detected with inductively coupled plasma mass spectrometry, and according to the typical curve of testing result render target element al;
5) object element detects: testing sample solution and control sample solution are detected with inductively coupled plasma mass spectrometry successively, according to the concentration of object element in the typical curve calculation sample solution of object element;
6) rate of transform is calculated: be calculated as follows the rate of transform of the solid-state additives of filter tip of cigarette in main flume:
TP%?＝?
Wherein: TP%: be the rate of transform of the solid-state additives of filter tip Si-Al molecular sieve of cigarette in main flume, percentage by weight;
C
1: the object element Al detectable concentration of contrast cigarette sample, mg/L;
C
2: contain the object element Al detectable concentration of additives of filter tip cigarette sample, mg/L;
N: suction cigarette number;
M: the solid additives Si-Al molecular sieve weight that adds in every cigarette, mg;
C
M: the content of object element Al in the solid-state additives of filter tip, percentage by weight.
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| CN102175753B true CN102175753B (en) | 2012-12-26 |
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| CN103743768B (en) * | 2014-01-10 | 2016-06-15 | 江苏中烟工业有限责任公司 | The evaluation methodology of material transport is there is in a kind of cigarette filter rod in aspiration procedure |
| CN104614436B (en) * | 2015-01-21 | 2018-04-03 | 上海烟草集团有限责任公司 | The detection method of arsenogen cellulose content in a kind of cigarette mainstream flue gas |
| CN113174292A (en) * | 2021-05-07 | 2021-07-27 | 上海烟草集团有限责任公司 | Template essence for researching transfer behavior of flavor components in cigarettes and application of template essence |
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| JP2001242052A (en) * | 2000-02-29 | 2001-09-07 | Sumitomo Metal Ind Ltd | Method for analyzing impurity in semiconductor substrate or chemicals |
| US20070292991A1 (en) * | 2006-06-20 | 2007-12-20 | Lisa Edith Helberg | Method for quantification of analytes in a titanium, tin or silcon tetrachloride sample |
| CN101339103B (en) * | 2008-08-07 | 2011-10-05 | 云南烟草科学研究院 | Flue gas trapping and absorption apparatus and its uses in cigarette flue gas heavy metal element determination |
| CN101551357B (en) * | 2009-02-26 | 2013-02-06 | 中国兵器工业集团第五三研究所 | ICP-MS measuring method of trace metal impurities in high purity lead |
| CN101685081A (en) * | 2009-08-24 | 2010-03-31 | 云南出入境检验检疫局检验检疫技术中心 | Method for measuring various elements in food additive citric acid through ICP-MS |
| CN101846651A (en) * | 2010-04-30 | 2010-09-29 | 浙江出入境检验检疫局检验检疫技术中心 | Method for measuring boric acid and borate in cosmetics by microwave digestion -ICP-MS |
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Address after: 610017 Jackie Chan Road, Chengdu economic and Technological Development Zone, Longquanyi District, Sichuan, China, No. 2, No. Applicant after: China Tobacco Chuanyu Industrial Co., Ltd. Address before: 610017 No. 2 Jackie Chan Road, National Economic Development Zone, Longquanyi District, Sichuan, Chengdu, Chengdu Applicant before: China Tobacco Chuanyu Industrial Corporation |
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Effective date of registration: 20161229 Address after: 610000, Sichuan, Chengdu, Longquanyi economic and Technological Development Zone, Jackie Chan Road, Longquan, No. 2, paragraph Patentee after: CHINA TOBACCO SICHUAN INDUSTRIAL CO., LTD. Patentee after: CHONGQING CHINA TOBACCO INDUSTRIAL CO., LTD. Address before: 610017 Jackie Chan Road, Chengdu economic and Technological Development Zone, Longquanyi District, Sichuan, China, No. 2, No. Patentee before: China Tobacco Chuanyu Industry Co., Ltd. |