CN101980010A - Method for measuring chlorine and sulphur in tobaccos and tobacco products - Google Patents
Method for measuring chlorine and sulphur in tobaccos and tobacco products Download PDFInfo
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- CN101980010A CN101980010A CN2010101822999A CN201010182299A CN101980010A CN 101980010 A CN101980010 A CN 101980010A CN 2010101822999 A CN2010101822999 A CN 2010101822999A CN 201010182299 A CN201010182299 A CN 201010182299A CN 101980010 A CN101980010 A CN 101980010A
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Abstract
The invention relates to a method for measuring chlorine and sulphur in tobaccos and tobacco products. The method comprises the following steps of: (1) carbonizing the tobaccos or the tobacco products in a processed crucible; (2) moving the crucible into a muffle furnace to perform ashing; (3) extracting chlorine and sulphur in the ashed substance to obtain a sample to be analyzed; and (4) performing ion chromatography on the sample to be analyzed and quantifying by an external standard method. The method has the advantage that: the chlorine and sulphur in the tobaccos and the tobacco products can be effectively transformed into an ionized state by extracting the tobaccos and the tobacco products through alkali fusion; and the chlorine and sulphur in the tobaccos and the tobacco products are precisely and quantificationally analyzed through complete extraction.
Description
Technical field
The present invention relates to the tobacco assay method, relate in particular to the assay method of chlorine and sulphur in tobacco and the tobacco product.
Background technology
Chlorine in the tobacco and sulphur play a very important role to the quality tool of tobacco product, and its content is to influence cigarette to prop up combustible key factor.The existing flow analysis of analytical approach, the chromatography of ions of present tobacco chlorine, the analytical approach of sulphur has barium sulfate turbidimetry, gravimetric method and precipitation titration, the chromatography of ions.Because flow analysis, barium sulfate turbidimetry, gravimetric method and precipitation titration complicated operation, process is tediously long, and the not high accurate quantification that causes of automaticity is very difficult.For the chromatography of ions, if because the chlorine in the tobacco leaf, sulphur are not converted into ionic forms during ion chromatography, then can not realize accurately quantitatively, when carrying out pre-treatment, can cause accurate quantification to be difficult to realize again to the grasp yardstick of ashing condition.
Summary of the invention
Purpose of the present invention is just at existing weak point in the prior art, and the method for measuring chlorine and sulphur in tobacco and the tobacco product is provided.This method can at first be converted into ionic condition with chlorine in the tobacco and sulphur effectively, extracts fully again, thus the chlorine in the realization tobacco and the accurate quantification analysis of sulphur.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of measuring chlorine and sulphur in tobacco and the tobacco product may further comprise the steps successively:
(1) tobacco or tobacco product carbonization treatment: take by weighing tobacco or tobacco product 0.2g-0.5g muffle furnace after pure water is cleaned and be incubated in the crucible that cools off behind the 3h for 800 ℃, the concentration that adds 1mL-3mL is the 1%-5% alkaline solution, leave standstill after the concussion evenly, place carbonization 15min-30min on the electric furnace afterwards;
(2) crucible moved into rise to 450 ℃-650 ℃ in the muffle furnace, keep 1h-3h, calcination;
(3) extraction of chlorine and sulphur in tobacco or the tobacco product: after the crucible cooling wherein calcination be transferred to and use the pure water extraction in the beaker, extract is filtered in the 100mL volumetric flask, is settled to the volumetric flask scale with pure water, obtains sample to be analyzed after shaking up filtration;
(4) the income analysis sample is carried out ion chromatography, adopt external standard method quantitative.
Chromatographic condition is: chromatographic column: IonPac AS11-HC (4 * 250mm) anion-exchange columns; Guard column: IonPac AG11-HC (4 * 50mm); Leacheate: 20mmol/L KOH solution, flow velocity 1.00mL/min; Rejector ASRS300 4mm; Electric current: 75mA; Column temperature: 30 ℃; Sample size: 25 μ L.
In the present invention, described tobacco or tobacco product can be the broken end of tobacco, cured tobacco leaf or Turkish tobaccos tobacco leaf.
Described alkaline solution can be NaOH or sodium carbonate liquor.
Described extraction process can be ultrasonic extraction, also can be the concussion extraction, or soaks extraction.
The invention has the beneficial effects as follows: this method is utilized alkali fusion extracted tobacco and tobacco product, at first can effectively chlorine in tobacco and the tobacco product and sulphur be converted into free state, extract fully again, thus the chlorine in realization tobacco and the tobacco product and the accurate quantification analysis of sulphur.Alkali fusion extracting process of the present invention is handled simply, extraction efficiency is high, easy and simple to handle, quick.
Embodiment
The present invention is further described below with reference to embodiment, but does not limit the present invention.
Embodiment 1
1, the tobacco sample 0.2 that took by weighing 40 mesh sieves is in crucible, and the concentration that adds 1mL is 5% sodium carbonate liquor, leaves standstill 5min after the concussion evenly, places carbonization 15min on the electric furnace.
2, crucible is moved into be warming up to 550 ℃ in the muffle furnace, heating 2h, take out cooling, change in the 100mL beaker, with 50mL moisture extracted twice, at normal temperatures, the ultrasonic extraction frequency is each ultrasonic 5min under 40KHz and the ultrasonic power 640w, uses filter paper filtering then in the 100mL volumetric flask, use the deionized water constant volume, get sample to be analyzed.
3, gained sample to be analyzed is carried out ion chromatography.
Embodiment 2
1, the tobacco sample 0.5g that took by weighing 40 mesh sieves is in crucible, and the concentration that adds 3mL is 1% sodium carbonate liquor, leaves standstill 5min after the concussion evenly, places carbonization 20min on the electric furnace.
2, crucible is moved into be warming up to 450 ℃ in the muffle furnace, heating 3h, take out cooling, change in the 100mL beaker, with 50mL moisture extracted twice, at normal temperatures, under rotating speed 150r/min each concussion 30min, use filter paper filtering then in the 100mL volumetric flask, use the deionized water constant volume, get sample to be analyzed.
3, gained sample to be analyzed is carried out ion chromatography.
Embodiment 3
1, the tobacco sample 0.3g that took by weighing 40 mesh sieves adds 3% sodium carbonate liquor of 2mL in crucible, leaves standstill 5min after the concussion evenly, places carbonization 30min on the electric furnace.
2, crucible is moved into be warming up to 650 ℃ in the muffle furnace, heating 1h takes out cooling, change in the 100mL beaker,, soak 1.5h at normal temperatures respectively with 50mL moisture extracted twice, use filter paper filtering then in the 100mL volumetric flask, use the deionized water constant volume, get sample to be analyzed.
3, gained sample to be analyzed is carried out ion chromatography.
Claims (4)
1. method of measuring chlorine and sulphur in tobacco and the tobacco product is characterized in that: may further comprise the steps successively:
(1) tobacco or tobacco product carbonization treatment: take by weighing tobacco or tobacco product 0.2g-0.5g muffle furnace after pure water is cleaned and be incubated in the crucible that cools off behind the 3h for 800 ℃, the concentration that adds 1mL-3mL is the 1%-5% alkaline solution, leave standstill after the concussion evenly, place carbonization 15min-30min on the electric furnace afterwards;
(2) crucible moved into rise to 450 ℃-650 ℃ in the muffle furnace, keep 1h-3h, calcination;
(3) extraction of chlorine and sulphur in tobacco or the tobacco product: after the crucible cooling wherein calcination be transferred to and use the pure water extraction in the beaker, extract is filtered in the 100mL volumetric flask, is settled to the volumetric flask scale with pure water, obtains sample to be analyzed after shaking up filtration;
(4) the income analysis sample is carried out ion chromatography, adopts external standard method quantitative:
Chromatographic condition is: chromatographic column: IonPac AS11-HC anion-exchange column; Guard column: IonPacAG11-HC; Leacheate: 20mmol/L KOH solution, flow velocity 1.00mL/min; Rejector ASRS3004mm; Electric current: 75mA; Column temperature: 30 ℃; Sample size: 25 μ L.
2. a kind of method of measuring chlorine and sulphur in tobacco and the tobacco product according to claim 1, it is characterized in that: described tobacco or tobacco product can be the broken end of tobacco, cured tobacco leaf or Turkish tobaccos tobacco leaf.
3. a kind of method of measuring chlorine and sulphur in tobacco and the tobacco product according to claim 1, it is characterized in that: described alkaline solution can be NaOH or sodium carbonate liquor.
4. a kind of method of measuring chlorine and sulphur in tobacco and the tobacco product according to claim 1, it is characterized in that: described extraction process can be ultrasonic extraction, also can be the concussion extraction, or soaks extraction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2010101822999A CN101980010A (en) | 2010-05-25 | 2010-05-25 | Method for measuring chlorine and sulphur in tobaccos and tobacco products |
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| CN2010101822999A CN101980010A (en) | 2010-05-25 | 2010-05-25 | Method for measuring chlorine and sulphur in tobaccos and tobacco products |
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| CN101980010A true CN101980010A (en) | 2011-02-23 |
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| CN2010101822999A Pending CN101980010A (en) | 2010-05-25 | 2010-05-25 | Method for measuring chlorine and sulphur in tobaccos and tobacco products |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590375A (en) * | 2012-01-30 | 2012-07-18 | 云南民族大学 | Method for extracting anions from plant medicine by alkali fusion method performing ion chromatographic detection |
| CN102879501A (en) * | 2012-10-11 | 2013-01-16 | 中国建材检验认证集团股份有限公司 | Measuring method for simple substance sulfur content in building material |
| CN103454356A (en) * | 2013-09-11 | 2013-12-18 | 神华集团有限责任公司 | Method for determining total chlorine content in direct coal liquefaction product |
| CN106290632A (en) * | 2016-08-06 | 2017-01-04 | 青岛农业大学 | The detection method of chloride ion content in paper pulp |
| CN111380820A (en) * | 2018-12-29 | 2020-07-07 | 贵州中烟工业有限责任公司 | Method for measuring sulfide in tobacco and tobacco products |
| CN112083102A (en) * | 2020-09-15 | 2020-12-15 | 安徽皖维高新材料股份有限公司 | Method for measuring sulfate ion content in PVA |
| CN112229941A (en) * | 2020-09-29 | 2021-01-15 | 中国科学院地球化学研究所 | Halogen detection method in geological sample |
| CN114487225A (en) * | 2022-01-20 | 2022-05-13 | 东莞理工学院 | Method for measuring sulfur and chlorine content in fly ash |
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| CN101587093A (en) * | 2008-05-23 | 2009-11-25 | 上海宝钢工业检测公司 | Method for measuring content of chloridion in wet flat liquid |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102590375A (en) * | 2012-01-30 | 2012-07-18 | 云南民族大学 | Method for extracting anions from plant medicine by alkali fusion method performing ion chromatographic detection |
| CN102879501A (en) * | 2012-10-11 | 2013-01-16 | 中国建材检验认证集团股份有限公司 | Measuring method for simple substance sulfur content in building material |
| CN102879501B (en) * | 2012-10-11 | 2014-01-08 | 中国建材检验认证集团股份有限公司 | Measuring method for simple substance sulfur content in building material |
| CN103454356A (en) * | 2013-09-11 | 2013-12-18 | 神华集团有限责任公司 | Method for determining total chlorine content in direct coal liquefaction product |
| CN106290632A (en) * | 2016-08-06 | 2017-01-04 | 青岛农业大学 | The detection method of chloride ion content in paper pulp |
| CN106290632B (en) * | 2016-08-06 | 2020-10-23 | 青岛农业大学 | Method for detecting content of chloride ions in paper pulp |
| CN111380820A (en) * | 2018-12-29 | 2020-07-07 | 贵州中烟工业有限责任公司 | Method for measuring sulfide in tobacco and tobacco products |
| CN112083102A (en) * | 2020-09-15 | 2020-12-15 | 安徽皖维高新材料股份有限公司 | Method for measuring sulfate ion content in PVA |
| CN112229941A (en) * | 2020-09-29 | 2021-01-15 | 中国科学院地球化学研究所 | Halogen detection method in geological sample |
| CN114487225A (en) * | 2022-01-20 | 2022-05-13 | 东莞理工学院 | Method for measuring sulfur and chlorine content in fly ash |
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Application publication date: 20110223 |