CN102928533A - Element analyzing and detecting method of total sulfur content in tobacco and tobacco products - Google Patents
Element analyzing and detecting method of total sulfur content in tobacco and tobacco products Download PDFInfo
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- CN102928533A CN102928533A CN2012104139620A CN201210413962A CN102928533A CN 102928533 A CN102928533 A CN 102928533A CN 2012104139620 A CN2012104139620 A CN 2012104139620A CN 201210413962 A CN201210413962 A CN 201210413962A CN 102928533 A CN102928533 A CN 102928533A
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Abstract
The invention discloses an element analyzing and detecting method of total sulfur content in tobacco and tobacco products. The element analyzing and detecting method comprises the following steps of: (1) accurately weighing a sample, drying the sample, and grinding and sieving the sample, so as to prepare a test sample; (2) arranging the test sample into an automatic feeding system of an element analyzer; feeding the test sample into an oxidation-reduction system of the element analyzer by the automatic feeding system for an oxidation reaction and a reduction reaction; and then drying obtained matter containing sulfur dioxide; (3) feeding the dried matter containing the sulfur dioxide into an absorption-separation system of the element analyzer, and feeding the separated sulfur dioxide into a detecting system of the element analyzer for detecting an obtained sulfur content curve; and comparing the content curve with a pre-manufactured standard sample curve, so as to obtain the total sulfur content of the sample. With the adoption of the element analyzing and detecting method provided by the invention, the total sulfur content can be conveniently and rapidly detected by only carrying out pretreatment, such as drying and grinding on the tobacco sample and carrying out the follow-up detection by using the element analyzer, so that the detection efficiency can be greatly improved.
Description
Technical field
The present invention relates to the determination techniques field of sulfur content in tobacco and the tobacco product, be specifically one grow tobacco and tobacco product in the determination of elemental analysis method of total sulfur.
Background technology
The content of total sulfur has very important impact to the quality of tobacco and goods thereof in tobacco and the tobacco product, the classic method of measuring total sulfur content in tobacco and the tobacco product mainly contains two kinds, a kind of is to adopt turbidimetry for Determination after adopting digestion, and another is to adopt the chromatography of ions to measure.Two kinds of methods of traditional this all need tobacco sample is digested, this just needs operating personnel to use a large amount of chemical reagent such as organic acid-base pair sample to digest, need a large amount of pre-processing devices such as water cleaning glass vessel, while length consuming time, and use a large amount of chemical reagent easily the healthy of operating personnel to be threatened; In addition, inorganic sulphide is converted into sulfate ion under strong condition, and the compound of the sulfur-bearings such as sulfoxide might transform other component effusion in digestion process, part sulphur can occur losing, causes testing result not accurate enough.Multinomial standard adopts the chromatography of ions to measure in the industry at present, and when adopting this method to measure, single ion chromatograph can't satisfy the enforcement of multinomial standard, so no matter be that purchase cost or operating cost are all larger.In addition, the sense cycle of total sulfur content and batch processing ability are about per 2 days 10 samples in the ion-chromatographic determination tobacco sample of the prior art, a little less than the batch processing ability.
This shows how a kind of assay method of avoiding total sulfur content in tobacco complicated pre-treatment, that accuracy is high and the goods thereof is provided, is the present technical issues that need to address in this area.
Summary of the invention
In view of this, the objective of the invention is, provide one grow tobacco and tobacco product in the determination of elemental analysis method of total sulfur, can avoid complicated pre-treatment, and the accuracy of measuring is high.
For solving the problems of the technologies described above, technical scheme of the present invention is:
One grow tobacco and tobacco product in the determination of elemental analysis method of total sulfur, comprise the steps:
1) accurately take by weighing tobacco to be determined or tobacco product as sample, 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) sample is 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, described oxidation reaction is: obtain oxysulfide adding under the oxygen condition and under 1000 ℃ ~ 1200 ℃ temperature sample and catalyzer reacted, described reduction reaction is: oxysulfide and reductive agent are reacted the material desiccant dryness that contains sulphuric dioxide that then will obtain under 750 ℃ ~ 950 ℃ temperature;
3) the dried material that contains sulphuric dioxide is sent into the absorption-piece-rate system of elemental analyser, with sulphuric dioxide and other separating substances, the sulphuric dioxide that then separation is obtained is sent in the detection system of elemental analyser and is detected, obtain the discharge curve that contains of sulphur, this is contained discharge curve compare with the standard model curve of making in advance, obtain the total sulfur content of sample.
Preferably, described catalyzer is included as tungstic acid.
Preferably, described reductive agent is wire copper or silver-plated copper or the potpourri of the two.
Preferably, the standard model curve of making in advance adopts the compound of sulfur-bearing to be made as standard model.
Preferably, the standard model curve of making in advance adopts sulphadiazine to be made as standard model.
Preferably, the purity of described sulphadiazine is greater than 99.5%.
Preferably, described detection system is thermal conductivity cell detector.
Preferably, sample is dried in baking oven.
Preferably, described oxidation reaction is carried out under 1150 ℃ temperature.
Preferably, described reduction reaction is carried out under 850 ℃ temperature.
Compared with prior art, the determination of elemental analysis method of total sulfur in tobacco of the present invention and the tobacco product is owing to adopt the method for ultimate analysis, thereby only need before detecting tobacco sample is carried out simple pre-treatment such as oven dry, grinding etc., the following adopted elemental analyser can conveniently detect total sulfur content, greatly improves detection efficiency; Particularly, the present invention has following advantage:
1, the present invention adopts the method for ultimate analysis to measure sulfur content in tobacco, the tobacco product, the elemental analyser that adopts, the expense of buying at hardware resource is that the ion chromatograph than available technology adopting more has superiority, adopt elemental analyser that sulphur is detected, can alleviate to a certain extent the operation burden of ion chromatograph.
2, the assay method of the present invention's employing, the particle powder that only needs tobacco and tobacco product to be ground to form certain order number can directly carry out analyzing and testing, need not the technician uses a large amount of chemical reagent that sample is digested, do not exist with a large amount of pre-treatments such as water cleaning glass vessel and prepare, on reagent, time, human resources, all greatly saved cost.
3, the ability of method mensuration total sulfur of the present invention is about 20-40 of every day, has improved the batch processing ability to sample.
4, method of the present invention is owing to be organic and inorganic sulfur all to be converted into sulfide (partly may be SO
2SO
3), then be converted into SO through reduction
2, namely organic and inorganic sulfur all are converted into sulphuric dioxide and measure, so do not need to digest pre-service and sample transfer, can reduce the loss to a certain extent.
5, method of the present invention need not soda acid or other organic reagent, does not need to digest pre-service, has relatively reduced the harmful effect healthy to the testing staff.
Embodiment
Basic conception of the present invention is: utilize elemental analyser that the tobacco sample organic matter is produced sulfide under the condition of high temperature and high purity oxygen, then by reduction reaction sulfide is reduced to stable sulphuric dioxide, through entering the content that detection system is measured total sulfur after absorption-separation.
In order to make those skilled in the art understand better technical scheme of the present invention, the present invention is described in further detail below by a preferred embodiment.
One, the instrument and equipment of using in the present embodiment:
1. elemental analyser
Comprise automatic sample handling system, oxidation-reduction system, absorption-piece-rate system and detection system (thermal conductivity cell detector) etc.;
2. balance
3. baking oven
4. tinfoil paper boat
More than be the conventional instrument of selecting from prior art, these select should not consist of the restriction 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 0.16MPa, 0.2Mpa, and helium gas flow is 600mL/min; This only is a certain condition selected in the present embodiment, also can select other any suitable conditions in specific implementation process;
2. furnace temperature: 1150 ℃; In other embodiments, also can select at 1000 ℃ ~ 1200 ℃, such as 1000 ℃, 1100 ℃, 1120 ℃, 1180 ℃, 1200 ℃ etc.
3. reduction furnace temperature: 850 ℃.In other embodiments, also can select at 750 ℃ ~ 950 ℃, such as 750 ℃, 780 ℃, 800 ℃, 880 ℃, 890 ℃, 920 ℃, 950 ℃ etc.
4. burning condition: 120 seconds oxygenation time;
5. oxidation tube-oxygenant
Tungstic acid;
6. reduction tube-reductive agent
Wire copper, purity (massfraction) is not less than 99%;
7. drying agent
Phosphorus pentoxide; This drying agent contains indicator, when the colourless blueness that is changed to is arranged, illustrates that suction is saturated.
8. standard model:
Select the compound of sulfur-bearing as standard model, present embodiment selects sulphadiazine as the organic element analysis standard substance, and its purity also can select other sulfocompounds as standard model greater than 99.5% in other embodiments.
9. gas
9.1 helium: purity is not less than 99.995%;
9.2 oxygen: purity is not less than 99.995%;
Three, the method for 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, until available finger twists into pieces.Take out the good tobacco leaf of baking from baking oven, grind at once, crossing the aperture is the 0.45mm(40 order) sieve.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 whole system;
Set analytical parameters, regulate instrument by operating conditions;
After furnace temperature reaches, do repeatedly the blank analysis value and the correction (proofreading and correct with the organic element analysis standard substance) of sample condition operation instrument:
Calibration curve (20-30 point): this curve generally is to do once a period of time, is kept in the workstation;
Day correction coefficient: the basis at calibration curve records, and must take multiple measurements on the same day of specimen.Accurately take by weighing the 25mg standard substance and measure a day correction coefficient, general METHOD FOR CONTINUOUS DETERMINATION 2 ~ 5 times, the capable coefficient of making even is as day correction coefficient mean value.Whenever advance sample 15 ~ 30 times, be standard specimen 2-3 time, with the stability of detection system, and in time adjust a day correction coefficient.
The preparation of typical curve:
Accurately take by weighing standard model (3.8) 0mg, 0.5mg, 1.0mg, 1.5mg, 2mg, 3mg, 4mg, 5mg, 6mg, 8mg, 10mg, 15mg, 20mg, 25mg, 30mg, 35mg, 40mg, 45mg, 50mg in the tinfoil paper boat, put into the stable sample injection disc of system behind the good seal, newly-built standard model is set up and preserved to operation method according to the data of gained.The same day, correction factor factor exceeded outside 0.9 ~ 1.1 scope, again made curve.
3, the mensuration of tobacco sample total sulfur content
Under the test condition identical with standard model, sample is measured.Accurately take by weighing the 25mg sample, the record sample weighting amount is also in the sample weighting amount input service station, the tinfoil paper boat is put into the stable sample injection disc of elemental analyser, operation method, that is: sample is inserted the automatic sample handling system of elemental analyser, then sent in the oxidation-reduction system of elemental analyser by automatic sample handling system and carry out oxidation reaction and reduction reaction, described oxidation reaction is: obtain oxysulfide adding under the oxygen condition and under 1150 ℃ temperature sample and catalyzer reacted, described reduction reaction is: oxysulfide and reductive agent are reacted the material desiccant dryness that contains sulphuric dioxide that then will obtain under 850 ℃ temperature; The dried material that contains sulphuric dioxide is sent into the absorption-piece-rate system of elemental analyser, with sulphuric dioxide and other separating substances, the sulphuric dioxide that then separation is obtained is sent in the detection system of elemental analyser and is detected, obtain the discharge curve that contains of sulphur, the discharge curve that contains of this sulphur is compared with the standard model curve of making in advance, obtain the total sulfur content of sample.
Adopt method of the present invention to measure to standard tealeaves (containing the sulphur standard value) sample, the results are shown in Table 1 and table 2.
Table 1 analyses result and canonical reference value be (n=3) relatively
Remarks:
(1) total sulfur adopts the TCD detecting device to measure.
(2) standard is shone sample measurement result is higher for the first time, the higher calibration sample of previous sulfur content (sulphadiazine) impact when mainly being put to the test, all the other several times measurement result illustrate that all in the scope of reference content method measurement result of the present invention is accurate.
Table 2 analyses result and canonical reference value be (n=6) relatively
Remarks:
(1) total sulfur adopts the IR detecting device to measure.
(2) it is higher that standard is shone the sample measurement result first time, the higher calibration sample of previous sulfur content (sulphadiazine) impact when mainly being put to the test, and measurement result is most all in the scope of reference content several times for all the other, illustrates that method measurement result of the present invention is accurate.
More than the present invention is described in detail, use specific case 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 (10)
- One grow tobacco and tobacco product in the determination of elemental analysis method of total sulfur, it is characterized in that, comprise the steps:1) accurately take by weighing tobacco to be determined or tobacco product as sample, 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) sample is 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, described oxidation reaction is: obtain oxysulfide adding under the oxygen condition and under 1000 ℃ ~ 1200 ℃ temperature sample and catalyzer reacted, described reduction reaction is: oxysulfide and reductive agent are reacted the material desiccant dryness that contains sulphuric dioxide that then will obtain under 750 ℃ ~ 950 ℃ temperature;3) the dried material that contains sulphuric dioxide is sent into the absorption-piece-rate system of elemental analyser, with sulphuric dioxide and other separating substances, the sulphuric dioxide that then separation is obtained is sent in the detection system of elemental analyser and is detected, obtain the discharge curve that contains of sulphur, the discharge curve that contains of this sulphur is compared with the standard model curve of making in advance, obtain the total sulfur content of sample.
- 2. the determination of elemental analysis method of total sulfur in tobacco as claimed in claim 1 and the tobacco product is characterized in that described catalyzer is included as tungstic acid.
- 3. the determination of elemental analysis method of total sulfur in tobacco as claimed in claim 1 and the tobacco product is characterized in that, described reductive agent is wire copper or silver-plated copper or the potpourri of the two.
- 4. the determination of elemental analysis method of total sulfur in tobacco as claimed in claim 1 and the tobacco product is characterized in that, the standard model curve of making in advance adopts the compound of sulfur-bearing to be made as standard model.
- 5. the determination of elemental analysis method of total sulfur in tobacco as claimed in claim 1 and the tobacco product is characterized in that, the standard model curve of making in advance adopts sulphadiazine to be made as standard model.
- 6. the determination of elemental analysis method of total sulfur in tobacco as claimed in claim 5 and the tobacco product is characterized in that the purity of described sulphadiazine is greater than 99.5%.
- 7. the determination of elemental analysis method of total sulfur in tobacco as claimed in claim 1 and the tobacco product is characterized in that, described detection system is thermal conductivity cell detector.
- 8. the determination of elemental analysis method of total sulfur in tobacco as claimed in claim 1 and the tobacco product is characterized in that sample is dried in baking oven.
- 9. the determination of elemental analysis method of total sulfur in tobacco as claimed in claim 1 and the tobacco product is characterized in that described oxidation reaction is carried out under 1150 ℃ temperature.
- 10. the determination of elemental analysis method of total sulfur in tobacco as claimed in claim 1 and the tobacco product is characterized in that described reduction reaction is carried out under 850 ℃ temperature.
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| CN2012104139620A CN102928533A (en) | 2012-10-25 | 2012-10-25 | Element analyzing and detecting method of total sulfur content in tobacco and tobacco products |
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| CN2012104139620A CN102928533A (en) | 2012-10-25 | 2012-10-25 | Element analyzing and detecting method of total sulfur content in tobacco and tobacco products |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108196005A (en) * | 2017-12-07 | 2018-06-22 | 中国科学院东北地理与农业生态研究所 | Carbon in a kind of organic liquid sample, nitrogen, hydrogen, sulfur content assay method |
| CN111257502A (en) * | 2020-03-05 | 2020-06-09 | 江苏权正检验检测有限公司 | Method for measuring sulfur dioxide in dried mushrooms |
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| CN101915812A (en) * | 2010-07-20 | 2010-12-15 | 云南出入境检验检疫局检验检疫技术中心 | Method for measuring carbon, hydrogen, nitrogen and sulfur in lavender |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108196005A (en) * | 2017-12-07 | 2018-06-22 | 中国科学院东北地理与农业生态研究所 | Carbon in a kind of organic liquid sample, nitrogen, hydrogen, sulfur content assay method |
| CN111257502A (en) * | 2020-03-05 | 2020-06-09 | 江苏权正检验检测有限公司 | Method for measuring sulfur dioxide in dried mushrooms |
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Application publication date: 20130213 |