CN102539222A - Determination of total nitrogen of tobacco and tobacco products through element analysis method - Google Patents
Determination of total nitrogen of tobacco and tobacco products through element analysis method Download PDFInfo
- Publication number
- CN102539222A CN102539222A CN2011104604986A CN201110460498A CN102539222A CN 102539222 A CN102539222 A CN 102539222A CN 2011104604986 A CN2011104604986 A CN 2011104604986A CN 201110460498 A CN201110460498 A CN 201110460498A CN 102539222 A CN102539222 A CN 102539222A
- Authority
- CN
- China
- Prior art keywords
- tobacco
- sample
- nitrogen
- total nitrogen
- mensuration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses determination of total nitrogen of tobacco and tobacco products through an element analysis method. The determination comprises the following steps of: (1) accurately weighing a tobacco sample, drying the tobacco sample at the temperature of not greater than 40 DEG C, then grinding and sieving; and sealing sieved powder and uniformly shaking to obtain a prepared sample; (2) placing the sample in an element analyzer to perform oxidation reduction on the sample by using the element analyzer to obtain nitrogen-containing substance; and (3) feeding the substance produced by the reduction reaction into an adsorption-separation system of the element analyzer to separate the nitrogen from other substances, then feeding the separated nitrogen into a detection system of the element analyzer for detection to obtain a nitrogen content curve, and comparing the content curve with a previously drawn standard sample curve to obtain total nitrogen content of the tobacco sample. According to the determination, only the tobacco sample is subjected to pretreatment such as drying and grinding before detection, the total nitrogen content can be conveniently and quickly detected by using the element analyzer in the subsequent detection, and the detection accuracy is greatly increased.
Description
Technical field
The present invention relates to the determination techniques field of nitrogen content in tobacco and the tobacco product, is a kind of through the mensuration of elemental microanalysis method to tobacco and tobacco product total nitrogen specifically.
Background technology
Have comparatively complicated numerous components in the tobacco, the Han Linghui influence of these components in tobacco even the quality of decision tobacco.Contain protein in the tobacco, protein can make the flue gas bitter taste increase after burning, produces acid and excitement; Therefore protein is too much, can be to the trickle generation harmful effect of cigarette, if but protein content is low excessively; Then flue gas will seem flat, and jealous and fragrance also can variation.So each stage in the tobacco production run that is necessary grasps protein content in the tobacco, measure Protein content in the tobacco, so that quality of tobacco is understood.In the prior art, tobacco business can carry out with reference to the tobacco business standard YC/T166-2003 of the People's Republic of China (PRC) the detection method of protein, and the measuring principle of this kind method is; With the protein nitrogen in acid such as the acetate deposition tobacco sample,, then protein is disappeared together with other sediments and boil through with the nitrogenous thing of nonprotein nitrogen and Separation of Proteins, wash-out; Protein nitrogen is converted into ammonium sulfate under the concentrated sulphuric acid and catalyst action, the highly basic distillation discharges ammonia, receives with the standard acid solution; Back titration; Through calculating Protein content in the tobacco, this shows that at last the time that the method pre-treatment process is comparatively complicated, institute spends processing is longer; The reagent that needs is many, and the used time is longer so that whole measuring is decided method in institute.
Summary of the invention
In view of this, the objective of the invention is, provide a kind of, improve detection efficiency through the assay method of elemental microanalysis method to tobacco and tobacco product total nitrogen.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of through the mensuration of elemental microanalysis method to tobacco and tobacco product total nitrogen, comprise the steps:
1) accurately take by weighing tobacco sample, tobacco sample is dried not being higher than under 40 ℃ the temperature, then grind, sieve, the powder-tight that will sieve shakes up, the sample that obtains preparing;
2) utilize elemental analyser sample to be inserted the automatic sample handling system of elemental analyser; The oxidation-reduction system that then sends into elemental analyser by automatic sample handling system carries out oxidation reaction and reduction reaction; Said oxidation reaction is carried out under 900 ℃～1000 ℃ temperature adding under the oxygen condition; Sample and oxygenant reacted obtains oxides of nitrogen, and said reduction reaction is reacted oxides of nitrogen and reductive agent under 450 ℃～550 ℃ temperature;
3) material that reduction reaction is produced is sent into the absorption-piece-rate system of elemental analyser; With nitrogen and other separating substances; The nitrogen that then separation is obtained is sent in the detection system of elemental analyser and is detected the discharge curve that contains that obtains nitrogen; This is contained discharge curve and the standard model curve ratio of making in advance, obtain the total nitrogen content of tobacco sample.
Preferably, said oxygenant comprises plumbous chromate, cerium oxide, cupric oxide.
Preferably, said reductive agent comprises wire copper, silver-plated copper.
Preferably, in the step 1), grinding the time that continues is below 2min minute.
Preferably, the standard model curve of making in advance adopts antifebrin to be made as standard model.
Preferably, said detection system is a thermal conductivity cell detector.
Preferably, tobacco sample is dried in baking oven.
Compared with prior art; Of the present invention through elemental microanalysis method to the assay method of tobacco and tobacco product total nitrogen owing to adopt the method for ultimate analysis; Thereby only need before detecting tobacco sample is carried out simple pre-treatment like oven dry, grinding etc.; The following adopted elemental analyser can detect total nitrogen content quickly and easily, improves detection efficiency greatly.
Embodiment
Of the present inventionly be contemplated that basically; Utilize elemental analyser that the nitrogen in the tobacco sample organic matter is oxidized to oxides of nitrogen under high temperature, catalyzer, excess of oxygen; Oxides of nitrogen is reduced into nitrogen through going back native copper, detects with thermal conductivity detector (TCD) at last and obtains total nitrogen content.
In order to make those skilled in the art understand technical scheme of the present invention better, through a preferred embodiment the present invention is done further detailed description below.
One, the instrument and equipment of using in the present embodiment:
1. the German Elementar Vario EL of company elemental analyser,
Comprise automatic sample handling system, oxidation-reduction system, absorption-piece-rate system and detection system (thermal conductivity cell detector) etc.;
2. 1,000,000/balance, model: Sartorius M2P;
3. baking oven
4. tinfoil paper boat (the Shanxi Qia Nuosi 4*4*11mm of Science and Technology Ltd.);
More than be the conventional instrument of from prior art, selecting, these selections should not constitute the qualification to protection domain of the present invention, in the implementation process, can select also that other can realize the instrument of said function in the prior art.
Two, instrument condition:
1. helium and oxygen pressure are 0.2MPa, 0.2Mpa, and helium gas flow is 200ml/min;
2. furnace temperature: 950 ℃; In other embodiments, also can select, as 900 ℃, 1000 ℃, 920 ℃, 970 ℃, 980 ℃, 940 ℃ at 900 ℃～1000 ℃.
3. reduction furnace temperature: 500 ℃.In other embodiments, also can select, as 450 ℃, 550 ℃, 460 ℃, 470 ℃, 480 ℃, 510 ℃, 520 ℃, 530 ℃, 545 ℃ at 450 ℃～550 ℃.
4. burning condition: 90 seconds oxygenation time;
5. oxidation tube-oxygenant
5.1 plumbous chromate, the ultimate analysis special agent;
5.2 cerium oxide, the ultimate analysis special agent;
5.3 cupric oxide, the ultimate analysis special agent;
6. reduction tube-reductive agent
6.1 wire copper, purity (massfraction) is not less than 99%;
6.2 silver-plated copper, purity (massfraction) is not less than 99%;
7. standard model:
Select for use the approaching material of nitrogen content and tobacco sample as standard model, present embodiment selects for use antifebrin as the organic element analysis standard substance, and its purity is greater than 99.5%;
8. gas
8.1 helium: purity is not less than 99.995%;
8.2 oxygen: purity is not less than 99.995%.
Three, the assay method of present embodiment comprises the steps:
1, tobacco sample pre-treatment
Tobacco sample-tobacco leaf is put into baking oven, in not being higher than 40 ℃ baking oven, dry, twist into pieces until available finger.The good tobacco leaf of taking-up baking grinds at once from baking oven, and it is 0.45mm (40 order) sieve that lasting milling time should not crossed the aperture above 2min.It is airtight in the wide-necked bottle of clean dried that the powder that sieves is packed into immediately.Fully shake mixing.This is the sample for preparing.
2, the preparation of instrument
Start instrument, the gas circuit of inspection apparatus total system;
Set analytical parameters, regulate instrument by operating conditions;
After treating that furnace temperature reaches, do repeatedly blank analysis value and sample condition operation (measure number of times should reach stability till), how much regulate the oxygenation time according to sample size with instrument system.
The correction of instrument (proofreading and correct) with the organic element analysis standard substance:
Calibration curve (20-30 point): this curve generally is to do once a period of time, is kept in the workstation;
Day correction coefficient: on the basis of calibration curve, record, must take multiple measurements on the same day of specimen.Accurately take by weighing 1-3mg standard substance (survey the CHN element and can do standard with antifebrin) and measure a day correction coefficient, general continuous is measured 5-7 time, and the capable coefficient of making even is as day correction coefficient mean value.Whenever advance sample 8-10 time, be standard specimen 2-3 time, with the stability of detection system, and the day correction coefficient of adjustment in time.
3, the mensuration of tobacco sample total nitrogen content
Under the test condition identical, tobacco and tobacco product sample are measured with standard model.Accurately take by weighing 1-5mg sample (constituent content is just controlled sample size per sample, makes each element produced in the sample signal and the standard model approaching), solid sample is with Xi Zhou or tin can parcel and flattening, and making does not wherein have air.
Tobacco sample sent in the elemental analyser detect, obtain the total nitrogen content in the tobacco sample.
More than the present invention has been carried out detailed introduction, use concrete example in the literary composition principle of the present invention and embodiment set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (7)
1. a mensuration of passing through elemental microanalysis method to tobacco and tobacco product total nitrogen is characterized in that, comprises the steps:
1) accurate rare tobacco sample of getting is dried tobacco sample not being higher than under 40 ℃ the temperature, then grinds, sieves, and the powder-tight that will sieve, shakes up the sample that obtains preparing;
2) utilize elemental analyser sample to be inserted the automatic sample handling system of elemental analyser; The oxidation-reduction system that then sends into elemental analyser by automatic sample handling system carries out oxidation reaction and reduction reaction; Said oxidation reaction is carried out under 900 ℃～1000 ℃ temperature adding under the oxygen condition; Sample and oxygenant reacted obtains oxides of nitrogen, and said reduction reaction is reacted oxides of nitrogen and reductive agent under 450 ℃～550 ℃ temperature;
3) material that reduction reaction is produced is sent into the absorption-piece-rate system of elemental analyser; With nitrogen and other separating substances; The nitrogen that then separation is obtained is sent in the detection system of elemental analyser and is detected; Obtain the discharge curve that contains of nitrogen, this is contained discharge curve and the standard model curve ratio of making in advance, obtain the total nitrogen content of tobacco sample.
2. as claimed in claim 1 through the mensuration of elemental microanalysis method to tobacco and tobacco product total nitrogen, it is characterized in that said oxygenant comprises plumbous chromate, cerium oxide, cupric oxide.
3. as claimed in claim 1 through the mensuration of elemental microanalysis method to tobacco and tobacco product total nitrogen, it is characterized in that said reductive agent comprises wire copper, silver-plated copper.
4. the mensuration of passing through elemental microanalysis method to tobacco and tobacco product total nitrogen as claimed in claim 1 is characterized in that in the step 1), grinding the time that continues is below 2min minute.
5. the mensuration of passing through elemental microanalysis method to tobacco and tobacco product total nitrogen as claimed in claim 1 is characterized in that the standard model curve of making in advance adopts antifebrin to be made as standard model.
6. as claimed in claim 1 through the mensuration of elemental microanalysis method to tobacco and tobacco product total nitrogen, it is characterized in that said detection system is a thermal conductivity cell detector.
7. as claimed in claim 1 through the mensuration of elemental microanalysis method to tobacco and tobacco product total nitrogen, it is characterized in that tobacco sample is dried in baking oven.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104604986A CN102539222A (en) | 2011-12-31 | 2011-12-31 | Determination of total nitrogen of tobacco and tobacco products through element analysis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104604986A CN102539222A (en) | 2011-12-31 | 2011-12-31 | Determination of total nitrogen of tobacco and tobacco products through element analysis method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102539222A true CN102539222A (en) | 2012-07-04 |
Family
ID=46346660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104604986A Pending CN102539222A (en) | 2011-12-31 | 2011-12-31 | Determination of total nitrogen of tobacco and tobacco products through element analysis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102539222A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105842370A (en) * | 2016-05-27 | 2016-08-10 | 鼎泰（湖北）生化科技设备制造有限公司 | Fixed-nitrogen analysis equipment with series and parallel connection water removal mechanisms |
| CN108918452A (en) * | 2018-06-13 | 2018-11-30 | 国网上海市电力公司 | The measuring method of nitrogen content in a kind of insulating paper |
| CN110208319A (en) * | 2019-06-05 | 2019-09-06 | 北京诺德泰科仪器仪表有限公司 | A kind of Dumars azotometer reaction tube |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE29703604U1 (en) * | 1997-02-28 | 1997-04-30 | Elementar Analysensysteme Gmbh | Reduction tube for nitrogen determination in elemental analysis |
-
2011
- 2011-12-31 CN CN2011104604986A patent/CN102539222A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE29703604U1 (en) * | 1997-02-28 | 1997-04-30 | Elementar Analysensysteme Gmbh | Reduction tube for nitrogen determination in elemental analysis |
Non-Patent Citations (2)
| Title |
|---|
| 郭晓旭等: "饲料中硝态氮对燃烧法与凯氏法总氮含量测定结果的影响", 《动物生产》, vol. 44, no. 21, 31 December 2008 (2008-12-31), pages 49 - 50 * |
| 陈剑: "元素分析仪测定磷酸一铵、磷酸二铵中总氮含量", 《贵州化工》, vol. 34, no. 4, 31 August 2009 (2009-08-31), pages 28 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105842370A (en) * | 2016-05-27 | 2016-08-10 | 鼎泰（湖北）生化科技设备制造有限公司 | Fixed-nitrogen analysis equipment with series and parallel connection water removal mechanisms |
| CN108918452A (en) * | 2018-06-13 | 2018-11-30 | 国网上海市电力公司 | The measuring method of nitrogen content in a kind of insulating paper |
| CN110208319A (en) * | 2019-06-05 | 2019-09-06 | 北京诺德泰科仪器仪表有限公司 | A kind of Dumars azotometer reaction tube |
| CN110208319B (en) * | 2019-06-05 | 2022-03-04 | 北京诺德泰科仪器仪表有限公司 | Dumas azotometer reaction tube |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Koziet | Isotope ratio mass spectrometric method for the on‐line determination of oxygen‐18 in organic matter | |
| CN102213714A (en) | Detection method for identifying natural taurine and synthesized taurine | |
| CN106053674B (en) | Chromatographic detection method that is a kind of while analyzing ammonium ion in tobacco leaf, amino acid and biogenic amine | |
| US10656130B2 (en) | Elemental analysis system and method with a reactor having two metal zeolite nitrogen oxides reduction reaction zones | |
| Minguillón et al. | Secondary organic aerosol origin in an urban environment: influence of biogenic and fuel combustion precursors | |
| CN106556665B (en) | The method for measuring 14 kinds of acid flavor component separatelies in cigarette mainstream flue gas simultaneously | |
| CN112782291A (en) | Method for identifying donkey-derived components in donkey-hide gelatin and preparation thereof | |
| CN102539222A (en) | Determination of total nitrogen of tobacco and tobacco products through element analysis method | |
| CN106124641B (en) | A kind of synchronous method for detecting carboxymethyl-lysine and lysopine in green tea | |
| CN110687189A (en) | Method for distinguishing milk producing area tracing and identifying based on multiple elements and multiple indexes | |
| CN110243952A (en) | A method of using each component content of AGEs in HPLC-MS/MS standard measure measurement milk powder | |
| Pozhidaev et al. | Determination of noble metals in rocks and ores using adsorbent PSTM-3T | |
| CN114674958B (en) | Method for measuring content of active ingredients in fructus gleditsiae | |
| Busigny et al. | Quantification and isotopic analysis of nitrogen in rocks at the ppm level using sealed tube combustion technique: A prelude to the study of altered oceanic crust | |
| US20190025266A1 (en) | Method for Elemental Analysis | |
| TW569007B (en) | A method for measuring the total concentration of carbon monoxide and hydrocarbons in oxygen by means of ion mobility spectrometry | |
| CN103115977B (en) | Method for rapidly detecting phosphorus hydride residue in tobaccos and tobacco products | |
| CN105866313A (en) | Method for rapidly determining nitrogen isotope ratio in nitrogen-containing sample | |
| López-García et al. | Liquid chromatography–electrothermal atomic absorption spectrometry for the separation and preconcentration of molybdenum in milk and infant formulas | |
| CN102565425B (en) | Method for measuring protein nitrogen content in tobaccos | |
| CN102928533A (en) | Element analyzing and detecting method of total sulfur content in tobacco and tobacco products | |
| CN115047126A (en) | Method for simultaneously and rapidly measuring nitrogen and sulfur contents in aquatic products | |
| CN103728358A (en) | Zirconia-base NOx sensor and manufacturing method thereof | |
| CN106066368A (en) | Quickly measure the method for carbon isotope ratio in organic matter samples | |
| CN110749691A (en) | HPLC-MS/MS method for determining aflatoxin and homologue thereof in infant auxiliary food |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Kong Haohui Inventor after: Chen Cuiling Inventor after: Cheng Zhiying Inventor before: Kong Haohui Inventor before: Zhou Rong Inventor before: Cheng Zhiying |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: KONG HAOHUI ZHOU RONG CHENG ZHIYING TO: KONG HAOHUI CHEN CUILING CHENG ZHIYING |
|
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120704 |