CN103063489B - Extraction method of nicotine with diffusion cell - Google Patents
Extraction method of nicotine with diffusion cell Download PDFInfo
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- CN103063489B CN103063489B CN201210567338.6A CN201210567338A CN103063489B CN 103063489 B CN103063489 B CN 103063489B CN 201210567338 A CN201210567338 A CN 201210567338A CN 103063489 B CN103063489 B CN 103063489B
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- nicotine
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Abstract
The invention discloses an extraction method of nicotine with a diffusion cell, the method includes the following steps: A1, weighing a sample; A2, injecting absorption liquid; A3, sealing in advance; A4, injecting alkaline liquor; A5, heating for diffusing; A6, collecting extracting solution; and A7, calculating nicotine content. The extraction method of the nicotine is simple in terms of used analytical equipment, used analytical instrument and operation, moreover capable of saving chemical reagent and energy greatly, and suitable for nicotine analysis work in common chemical analysis laboratory.
Description
Technical field
The present invention relates to chemical analysis technology field, in particular a kind of method of diffusion boat extraction nicotine, be applicable to the mensuration of nicotine content.
Background technology
Pure nicotine is at room temperature colourless oil liquid, and boiling point 246.1 DEG C, has levorotation; Have strong impulse, taste is pungent; Nicotine is soluble in water, and can with water with arbitrary proportion phase mixing; Nicotine also can be dissolved in the organic solvents such as ethanol, ether and low-density oil; The short wavelength light (i.e. ultraviolet light) of nicotine to a certain wave band has maximum absorbance capacity, and its absorbance is directly proportional to the content of nicotine.
Nicotine is alkali compounds, can generate salt with multiple mineral acid and organic acid reaction, this in conjunction with state nicotine soluble in water and organic solvent mostly, can decompose in the basic conditions and produce free state nicotine.
The alkalescence of free state nicotine is greater than in conjunction with state nicotine, and volatile.Nicotine is very stable when steam distillation, namely has the special nature be not decomposed with water vapor volatilization.
Separating and extracting process research at present for nicotine is more, and often kind of method is not identical with the purity of separating-purifying to the extraction efficiency of nicotine, can select suitable method in concrete test and production run in conjunction with actual needs.Wherein, the solvent extraction of the way of distillation, ion-exchange-resin process and routine achieves suitability for industrialized production.
The way of distillation wants the energy of at substantial and alkali-treated tobacco leaf to be difficult to process, does not generally advocate extensive use.This method is comparatively conventional in nicotine conventional chemical analysis, but Gao Lianzhen etc.
[1]think that macroprocedure steam distillation device is more complicated in general teaching material, and drug dosage is large, length consuming time, is generally difficult to complete within two class hours of experiment outline arrangement.They adopt Miniature water steam distillation to extract experimental provision to nicotine and improve, result not only simplify apparatus after showing improvement, decrease thermal source, and reduce the consumption of medicine, phenomenon is obvious, is convenient to observe, and shortens experimental period, student is interior when normal laboratory just can complete, respond well.
Ion-exchange-resin process shortcoming is the pre-service of ion exchange resin and regenerates comparatively loaded down with trivial details.Be not suitable for chemical analysis in nicotine Routine Test Lab.
Solvent extraction shortcoming is that NaOH relates to instrument corrosion comparatively greatly to experiment, in general should not be used as fertilizer in addition, be difficult to process with the scarp of NaOH process.Be not suitable for chemical analysis in nicotine Routine Test Lab.
Summary of the invention
Technical matters to be solved by this invention is a kind of method providing diffusion boat extraction nicotine for the deficiencies in the prior art, is applicable to the mensuration of nicotine content.
Technical scheme of the present invention is as follows:
A method for diffusion boat extraction nicotine, comprises the following steps: A1, takes sample: take 0.08-0.1g cigarette sample with thousand points of balances, is evenly dispersed in diffusion boat mistress (3);
A2, injects absorbing liquid: the sulfuric acid of 5mL 4mol/L to be injected in diffusion boat room (4) as absorbing liquid with syringe;
A3, pre-closed: on diffusion boat outer wall, evenly to coat glycerine along on frosted mouth, cover ground glass cover plate (2), light pressure left rotation and right rotation, the glycerine of outer ring is uniformly distributed, to improve sealing effectiveness, pricks on diffusion boat with bungee, with fixing ground glass cover plate (2), enhanced leaktightness effect;
A4, injects alkali lye: draw 10 mL 4mol/L NaOH solution with another one syringe, then slip off ground glass cover plate (2), injects alkali lye from liquid injection hole to diffusion boat mistress (3), and sliding glass cover plate of hastening afterwards seals;
A5, adds thermal diffusion: diffusion boat is held level with both hands and puts into baking oven and heat, keep 8h at 80 DEG C;
A6. extract is collected: pipette the nicotine absorption liquid in room in diffusion boat (4) after heating terminates, be settled to 250mL.
A7, nicotine content is calculated: calculate nicotine content in extract with ultraviolet spectrophotometer method.
It is all very simple that the present invention establishes a kind of analytical equipment used, instrument and method of operating, and can save chemical reagent and energy in a large number, is applicable to the Method of Nicotine Extraction of nicotine analysis work in ordinary chemical analysis room.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the inventive method;
1 diffusion boat, 2 ground glass cover plates, 3 diffusion boat mistress, content is: 10mL 4mol/LNaOH+ cigarette sample; Room in 4 diffusion boats, content is: 5mL 4mol/L H
2sO
4
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Instrument and equipment: baking oven, diffusion boat, balance (sensibility reciprocal 0.0001), transfer pipet (syringe);
Reagent: the sulfuric acid of 4moL/L concentration, as the absorbing liquid of volatilization state nicotine; The NaOH solution of 4mol/L concentration, as tobacco leaf;
Operation steps and method:
1. take sample: take 0.08-0.1g cigarette sample with thousand points of balances, be evenly dispersed in diffusion boat mistress 3.
2. inject absorbing liquid: the sulfuric acid of 5mL 4mol/L to be injected in diffusion boat room 4 as absorbing liquid with syringe.
3. close in advance: on diffusion boat outer wall, evenly coat glycerine along on frosted mouth, cover ground glass cover plate 2, light pressure also left rotation and right rotation, the glycerine of outer ring is uniformly distributed, to improve sealing effectiveness, pricks on diffusion boat with bungee, with fixing ground glass cover plate 2, enhanced leaktightness effect.
4. inject alkali lye: draw 10 mL 4mol/L NaOH solution with another one syringe, then slip off ground glass cover plate 2, inject alkali lye from liquid injection hole to diffusion boat mistress 3, sliding glass cover plate of hastening afterwards seals.
5. add thermal diffusion: diffusion boat 1 is held level with both hands and puts into baking oven and heat, placement is spent the night to keep 8h(to advise at 80 DEG C).
6. collect extract: pipette the nicotine absorption liquid (interior room will clean 3 times, washing lotion and absorbing liquid is all incorporated in volumetric flask) in diffusion boat in room 4 after heating terminates, be settled to 250mL.
7. nicotine content measuring and calculating: calculate nicotine content in extract with ultraviolet spectrophotometer method; Analyze Upon Strict Inspection and draw, operate as stated above, the nicotine that diffusion method is extracted accounts for 88.29% of nicotine actual content in tobacco leaf; So, need to be multiplied by correction coefficient 1.1326 when calculating nicotine actual content.
2-3 blank must be set in analysis design mothod.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (1)
1. by a method for diffusion boat extraction nicotine, it is characterized in that, comprise the following steps: A1, take sample: take 0.08-0.1g cigarette sample with thousand points of balances, be evenly dispersed in diffusion boat mistress (3);
A2, injects absorbing liquid: the sulfuric acid of 5mL 4mol/L to be injected in diffusion boat room (4) as nicotine absorption liquid with syringe;
A3, pre-closed: on diffusion boat outer wall, evenly to coat glycerine along on frosted mouth, cover ground glass cover plate (2), light pressure left rotation and right rotation, the glycerine of outer ring is uniformly distributed, to improve sealing effectiveness, pricks on diffusion boat with bungee, with fixing ground glass cover plate (2), enhanced leaktightness effect;
A4, inject alkali lye: draw 10mL 4mol/L NaOH solution with another one syringe, then slip off ground glass cover plate (2), inject alkali lye from liquid injection hole to diffusion boat mistress (3), sliding glass cover plate of hastening afterwards seals;
A5, adds thermal diffusion: diffusion boat is held level with both hands and puts into baking oven and heat, keep 8h at 80 DEG C;
A6. nicotine absorption liquid is collected: pipette the nicotine absorption liquid in room in diffusion boat (4) after heating terminates, be settled to 250mL.
A7, nicotine content is calculated: calculate nicotine content in nicotine absorption liquid with ultraviolet spectrophotometer method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210567338.6A CN103063489B (en) | 2012-12-24 | 2012-12-24 | Extraction method of nicotine with diffusion cell |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210567338.6A CN103063489B (en) | 2012-12-24 | 2012-12-24 | Extraction method of nicotine with diffusion cell |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103063489A CN103063489A (en) | 2013-04-24 |
| CN103063489B true CN103063489B (en) | 2015-04-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201210567338.6A Expired - Fee Related CN103063489B (en) | 2012-12-24 | 2012-12-24 | Extraction method of nicotine with diffusion cell |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064680A (en) * | 1992-03-07 | 1992-09-23 | 吴景峰 | The production technique of nicotine salt and pure nicotine products |
| CN1335315A (en) * | 2000-07-20 | 2002-02-13 | 李森兰 | Nicotine extracting process from tobacco |
| CN102796076A (en) * | 2012-09-03 | 2012-11-28 | 国家烟草质量监督检验中心 | Preparation method for nicotine standard substance |
-
2012
- 2012-12-24 CN CN201210567338.6A patent/CN103063489B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064680A (en) * | 1992-03-07 | 1992-09-23 | 吴景峰 | The production technique of nicotine salt and pure nicotine products |
| CN1335315A (en) * | 2000-07-20 | 2002-02-13 | 李森兰 | Nicotine extracting process from tobacco |
| CN102796076A (en) * | 2012-09-03 | 2012-11-28 | 国家烟草质量监督检验中心 | Preparation method for nicotine standard substance |
Non-Patent Citations (3)
| Title |
|---|
| 从烟叶中提取烟碱方法的改革;张欣;《大庆师范学院学报》;20060430;第26卷(第2期);全文 * |
| 微波和超声波在烟碱提取中的作用;刘雷 等;《烟草化学》;20080520(第5期);全文 * |
| 高纯度烟碱的制备;储志兵 等;《应用化工》;20070131;第36卷(第1期);全文 * |
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| CN103063489A (en) | 2013-04-24 |
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