CN102116767A - Method for simultaneously measuring K, Ca and Mg in tobacco - Google Patents
Method for simultaneously measuring K, Ca and Mg in tobacco Download PDFInfo
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Abstract
The invention relates to a method for simultaneously measuring K, Ca and Mg in tobacco, comprising the following steps of: ashing a tobacco sample; after ash residues are dissolved and subjected to constant volume, and analyzing by combining an ion chromatography and an electrical conductivity detector to realize one sample injection; and simultaneously measuring K, Ca and Mg in the tobacco. With the method disclosed by the invention, a tobacco sample is ashed in a muffle furnace until the tobacco sample is grey white; the ash residues are transferred into a volumetric flask with dilute acid; before the sample is fed, the sample is filtered by a filter membrane with the size of 0.45mum; a DIONEXICS 3000 reagent-free ion chromatograph and the electrical conductivity detector are adopted for measuring; K, Ca and Mg in the tobacco are measured by the ion chromatograph; when a CS12A column is adopted for analyzing, the tobacco sample is ashed with the method, no digestion agent or strong-acid substance needs to be added in the ashing process; and after ash residues are dissolved and subjected to constant volume, the influence of utensil does not need to be considered in the pretreatment process, and the ash residues can be directly measured by the ion chromatograph and the electrical conductivity detector, thereby realizing one sample injection, and simultaneously measuring K, Ca and Mg in the tobacco.
Description
Technical field
The present invention relates to a kind of method of measuring K-Mg-Ca in the tobacco, relate in particular to a kind of method of measuring K-Mg-Ca in the tobacco simultaneously, belong to tobacco components detection technique field.
Background technology
Tobacco is in growth course, for normal nutritional need, except constantly absorb CO from surrounding environment
2And water, obtain beyond the hydrocarbon oxygen, also to from soil, absorb another group important element---mineral element, to keep normal vital movement.K, Ca, Mg be the tobacco requirement big, to tobacco production and the comparatively significant mineral element of quality influence.
K is the element relevant with result of combustion of tobacco with Mg, in certain concentration range, and the flammability of the content of K and tobacco and hold firepower and be proportionate in the tobacco.The moderate cigarette ash that can keep of the content of Mg is complete, is difficult for being scattered, and result of combustion of tobacco reduction when Mg content is high, the cigarette ash darker in color, it is inhomogeneous to burn.Ca is the necessary nutrient of tobacco leaf, helps the normal development of tobacco leaf, and the filling power of tobacco is had good effect.Mensuration for K, Ca, Mg in the tobacco is the project that often will survey in the routine check.Measure about K, Ca, Mg in the tobacco, except traditional manual method, comparatively classical and ripe now method is an atomic absorption method, and this kind method is to measure the prefered method of most of metallic element.Also there is relevant standard to issue in tobacco business inside, is respectively the mensuration atomic absorption method of mensuration atomic absorption method, YC/T175-2003 tobacco and tobacco product magnesium of mensuration flame photometry, YC/T174-2003 tobacco and the tobacco product calcium of YC/T173-2003 tobacco and tobacco product potassium.Wherein the mensuration of potassium also has the mensuration continuous flow method of YC/T217-2007 tobacco and tobacco product potassium.The instrument that above-mentioned several method mainly adopts is Atomic Absorption Spectrometer (joining flame), and the pre-treatment process need uses concentrated hydrochloric acid (concentration is 6mol/L); In test process, disturb in order to eliminate matrix, in standard and sample, also need to add matrix modifier---lanthanum chloride; The range of linearity of Atomic Absorption Spectrometer is narrower, for tobacco sample, even sample weighting amount is low to about 0.1g, still needs to dilute more than 50 times before sample introduction; And for different elements, Atomic Absorption Spectrometer need be changed different light sources, therefore, analyzes when can't realize K, Ca, three kinds of components of Mg.
The chromatography of ions is a new liquid-phase chromatographic analysis technology of 20th century the mid-1970s birth, nowadays be the prefered method of analyzing inorganic yin, yang ion, it has (detect lower limit and can reach the ppt level) easy and simple to handle, highly sensitive, sample pre-treatments is simple, analysis speed is fast, can carry out the advantage that different kinds of ions is analyzed simultaneously.If the K in the tobacco, Ca, Mg can be converted into ionic condition, adopt the chromatography of ions just can analyze simultaneously, analysis efficiency is improved.
Have report to use chromatography of ions that K, Ca, Mg in the tobacco are measured at present: the pre-treating method that is adopted in the report has ultrasonic extraction, the extraction of homogenate method, wet method digestion etc.K in the tobacco is water-soluble or sour, Ca and Mg only have the part form to be dissolved in acid, adopt the method for acid extraction can not make the complete stripping of Ca, Mg in the tobacco, and the increase of acid concentration in the extract, the post of employed cation analysis post CS12A in the ion chromatography is imitated considerable influence; When the concentration of acid reached 100mmol/L, the Mg peak had begun distortion, and the degree of separation of Mg and Ca also reduces.The sample solution acidity that wet method digestion obtains is also stronger, even carried out catching up with acid treatment after the digestion, pH value of solution is still below 1, need in the galvanochemistry and etc. the method adjustment make its pH 2, can sample introduction.
Summary of the invention
The object of the present invention is to provide a kind of method of measuring K-Mg-Ca in the tobacco simultaneously.
To achieve these goals, technical scheme of the present invention has adopted a kind of method of measuring K-Mg-Ca in the tobacco simultaneously, tobacco sample is carried out ashing treatment, lime-ash is behind diluted acid dissolving constant volume, use chromatography of ions to analyze in conjunction with electric conductivity detector, realize single injected sampling, measure the K-Mg-Ca in the tobacco simultaneously.
Method concrete steps of the present invention are as follows:
(1) sample is placed porcelain crucible, sample is carried out ashing;
(2) treat that lime-ash cools to room temperature, use diluted acid that it is transferred to and carry out constant volume in the volumetric flask;
(3) use the diluted acid of same concentration to prepare K, Ca, Mg standard solution;
(4) sample uses chromatography of ions to analyze behind 0.45 μ m membrane filtration.
(5) data processing.
Described step (1) is specially: the flue-cured tobacco sample is placed porcelain crucible, muffle furnace is warming up to 500～550 ℃, sample is positioned over ashing in the muffle furnace, and the ashing time is 4h.
Described step (2) is specially: take out crucible, place exsiccator, be cooled to room temperature, working concentration is that the HCL of 25mmol/L transfers to lime-ash in the glass volumetric flask constant volume.
Step (3) standard solution, the mark liquid concentration of K is 1000mg/L, and the mark liquid concentration of Ca is 1000mg/L, and the mark liquid concentration of Mg is 100mg/L.
The dissolve medium of described K mark liquid is a water, and the dissolve medium of Ca and Mg mark liquid is 1% HCL.
Described water is secondary deionized water.
Employed chromatography of ions model is joined the leacheate generator for DIONEX ICS3000(among the present invention); the cation analysis post that uses is the cation exchange column of Dionex IonPac CS12A(4 * 250mm); the kation guard column of Dionex IonPac CG12A(4 * 50mm); leacheate is MSA; concentration is 20mmol, and flow velocity is 1.2mL/min, sample size 25 μ L; acquisition time is 30min, and type of elution is the degree such as grade.Detecting device is an electric conductivity detector.Rejector adopts CSRS-II, and electric current is 71mA.
Adopt method of the present invention, in muffle furnace with the tobacco sample ashing to canescence, with diluted acid lime-ash is transferred in the volumetric flask, through 0.45 μ m membrane filtration, adopt the DIONEX ICS3000 formulation chromatography of ions distribution of being excused from an examination to lead detecting device and measure before the sample introduction.Use chromatography of ions that K, Ca, Mg in the tobacco are measured, when adopting the CS12A post to analyze, this method is carried out ashing treatment to tobacco sample, podzolic process need not to add any agent or strong acid class material cleared up, lime-ash is behind diluted acid dissolving constant volume, and the pre-treatment process does not need to consider the influence of vessel, can directly use chromatography of ions to analyze in conjunction with electric conductivity detector, thereby the realization single injected sampling is measured K-Mg-Ca the time in the tobacco.
Assay method of the present invention has accurately, characteristics fast and efficiently.Also have the following advantages in addition: the method for ashing is selected in pre-treatment for use, and podzolic process does not need to use other reagent; The dissolving lime-ash uses rarer HCl, and environmental pollution is little; K, Ca, three kinds of elements of Mg are analyzed simultaneously, and are more efficient, easier; Use general glass apparatus to get final product in pre-treatment and the mensuration process.
Adopt assay method used in the present invention that flue-cured tobacco, burley tobaccos, Turkish tobaccos, Virginian-type cigarette, blended type cigarette, six kinds of samples of thin slice are analyzed, analysis result and aas determination result fit like a glove.Specifically see Table 1.
With the flue-cured tobacco sample is example, the recovery of standard addition that assay method used in the present invention is measured K, Ca, Mg in the tobacco is respectively 98.0～105.0%, 98.6～102.8%, 97.0～104.9%, precision is respectively 2.29%, 2.36%, 4.96%, and concrete outcome sees Table 2 and table 3.
Adopt assay method used in the present invention, measure minimum cup standard solution 10 times, with 3 times of standard deviations of measurement result detection limit as method, then the detectability of K, Ca, three kinds of elements of Mg is respectively 35ng/mL, 49ng/mL, 16ng/mL.
Data computation formula of the present invention is as follows:
In the formula, X: the Instrument observation value of sample, every milliliter of unit microgram (μ g/mL);
V: the constant volume of sample, unit are milliliter (being 100mL herein);
M: sample quality, unit is gram (g);
W: the percent water content of sample, %(massfraction).
Description of drawings
Fig. 1 is the chromatography of ions figure of flue-cured tobacco sample among the present invention;
Fig. 2 is the chromatography of ions figure of burley tobaccos sample among the present invention.
Embodiment
Embodiment 1: the mensuration of K, Ca, Mg in the flue-cured tobacco
1) sample pre-treatments
Accurately take by weighing 0.1g flue-cured tobacco sample to the 20mL porcelain crucible, be accurate to 0.1mg.Muffle furnace is warming up to 500～550 ℃, and sample is positioned over ashing in the stove, and the ashing time is 4h; Take out crucible, place exsiccator, be cooled to room temperature, use the HCL of 25mmol/L lime-ash to be transferred in the 100mL glass volumetric flask constant volume;
2) preparation of standard solution
K mark liquid pipettes 2.5mL, 2mL, 1.5mL, 1mL, 0.5mL respectively; Ca mark liquid pipettes 2.5 mL, 2mL, 1.5mL, 1mL, 0.5mL respectively; Mg mark liquid pipettes 7.5mL respectively, 4mL, 1.5mL, 0.75mL, 0.15mL to the 50mL volumetric flask, with the hydrochloric acid constant volume of 25mmol/L, the concentration K that obtains work mark liquid is 50,40,30,20,10 μ g/mL, Ca is 50,40,30,20,10 μ g/mL, and Mg concentration is 15,8,3,1.5,0.3 μ g/mL;
3) with sample solution behind 0.45 μ m membrane filtration, use chromatography of ions to analyze:
The chromatography of ions model is joined the leacheate generator for DIONEX ICS3000(); the cation analysis post that uses is the cation exchange column of Dionex IonPac CS12A(4 * 250mm); the kation guard column of Dionex IonPac CG12A(4 * 50mm); leacheate is MSA; concentration is 20mmol/L, and flow velocity is 1.2mL/min, sample size 25 μ L; acquisition time is 30min, and type of elution is the degree such as grade.Detecting device is an electric conductivity detector.Rejector adopts CSRS-II, and electric current is 71mA;
4) after sequence has been moved, integral condition is set, adopts retention time qualitative, peak area quantification, from peak valley to the peak valley integration.Typical curve adopts a curve;
5) the sample collection of illustrative plates is seen Fig. 1;
6) data computation
The peak area at K, Ca, Mg peak carries out regretional analysis to its respective concentration, obtains typical curve.Peak area by test sample then obtains the concentration of sample correspondence, i.e. Instrument observation value by typical curve.
K, Ca, Mg content in butt are drawn by following formula:
In the formula, X: the Instrument observation value of sample, every milliliter of unit microgram (μ g/mL);
V: the constant volume of sample, unit are milliliter (being 100mL herein);
M: sample quality, unit is gram (g);
W: the percent water content of sample, %(massfraction);
The content of being calculated K in the flue-cured tobacco by above formula is 2～3%, and the content of Ca is 2～5%, and the content of Mg is within 0.1～1% scope.
Embodiment 2: the mensuration of K, Ca, Mg in the burley tobaccos
1) sample pre-treatments
Accurately take by weighing 0.1g burley tobaccos sample to the 20mL porcelain crucible, be accurate to 0.1mg, muffle furnace is warming up to 500～550 ℃, sample is positioned over ashing in the stove, and the ashing time is 4h, takes out crucible, place exsiccator, be cooled to room temperature, use the HCl of 25mmol/L lime-ash to be transferred in the 100mL glass volumetric flask constant volume;
2) preparation of standard solution
K mark liquid pipettes 2.5mL, 2mL, 1.5mL, 1mL, 0.5mL respectively; Ca mark liquid pipettes 2.5 mL, 2mL, 1.5mL, 1mL, 0.5mL respectively; Mg mark liquid pipettes 7.5mL respectively, 4mL, and 1.5mL, 0.75mL is in 0.15mL to the 50mL volumetric flask, with the hydrochloric acid constant volume of 25mmol/L.The concentration K that obtains work mark liquid is 50,40,30,20,10 μ g/mL, and Ca is 50,40,30,20,10 μ g/mL, and Mg concentration is 15,8,3,1.5,0.3 μ g/mL;
3) with sample solution behind 0.45 μ m membrane filtration, use chromatography of ions to analyze
The chromatography of ions model is joined the leacheate generator for DIONEX ICS3000(); the cation analysis post that uses is the cation exchange column of Dionex IonPac CS12A(4 * 250mm); the kation guard column of Dionex IonPac CG12A(4 * 50mm); leacheate is MSA; concentration is 20mmol/L, and flow velocity is 1.2mL/min, sample size 25 μ L; acquisition time is 30min, and type of elution is the degree such as grade.Detecting device is an electric conductivity detector.Rejector adopts CSRS-II, and electric current is 71mA;
4) after sequence has been moved, integral condition is set, adopts retention time qualitative, peak area quantification, to the peak valley integration, typical curve adopts a curve from peak valley;
5) the sample collection of illustrative plates is seen Fig. 2;
6) data computation
The peak area at K, Ca, Mg peak carries out regretional analysis to its respective concentration, obtains typical curve.Peak area by test sample then obtains the concentration of sample correspondence, i.e. Instrument observation value by typical curve.
K, Ca, Mg content in butt are drawn by following formula:
In the formula, X: the Instrument observation value of sample, every milliliter of unit microgram (μ g/mL);
V: the constant volume of sample, unit are milliliter (being 100mL herein);
M: sample quality, unit is gram (g);
W: the percent water content of sample, %(massfraction);
The content of being calculated K in the burley tobaccos by above formula is 2～3%, and the content of Ca is 2～5%, and the content of Mg is within 0.1～1% scope.
Claims (7)
1. method of measuring K-Mg-Ca in the tobacco simultaneously, it is characterized in that: tobacco sample is carried out ashing treatment, and lime-ash uses chromatography of ions to analyze in conjunction with electric conductivity detector behind diluted acid dissolving constant volume, realize single injected sampling, measure the K-Mg-Ca in the tobacco simultaneously.
2. the method for measuring K-Mg-Ca in the tobacco simultaneously according to claim 1 is characterized in that: specifically may further comprise the steps:
(1) sample is placed porcelain crucible, sample is carried out ashing;
(2) treat that lime-ash cools to room temperature, use diluted acid that it is transferred to and carry out constant volume in the volumetric flask;
(3) use the diluted acid of same concentration to prepare K, Ca, Mg standard solution;
(4) behind the sample filtering, use chromatography of ions to analyze.
3. the method for measuring K-Mg-Ca in the tobacco simultaneously according to claim 1, it is characterized in that: described step (1) is specially: the flue-cured tobacco sample is placed porcelain crucible, muffle furnace is warming up to 500～550 ℃, and sample is positioned over ashing in the muffle furnace, and the ashing time is 4h.
4. the method for measuring K-Mg-Ca in the tobacco simultaneously according to claim 1, it is characterized in that: described step (2) is specially: take out crucible, place exsiccator, be cooled to room temperature, working concentration is that the HCL of 25mmol/L transfers to lime-ash in the glass volumetric flask constant volume.
5. the method for measuring K-Mg-Ca in the tobacco simultaneously according to claim 1 is characterized in that: step (3) standard solution, and the mark liquid concentration of K is 1000mg/L, and the mark liquid concentration of Ca is 1000mg/L, and the mark liquid concentration of Mg is 100mg/L.
6. the method for measuring K-Mg-Ca in the tobacco simultaneously according to claim 5 is characterized in that: the dissolve medium of described K mark liquid is a water, and the dissolve medium of Ca and Mg mark liquid is 1% HCL.
7. according to arbitrary described method of measuring K-Mg-Ca in the tobacco simultaneously in the claim 1-6, it is characterized in that: described water is secondary deionized water.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102901791A (en) * | 2012-10-16 | 2013-01-30 | 红塔烟草(集团)有限责任公司 | Method for determining content of calcium carbonate in reconstituted tobacco |
| CN105699503A (en) * | 2016-01-14 | 2016-06-22 | 广西中烟工业有限责任公司 | Method for simultaneously determining content of sodium, potassium, magnesium and calcium in tobaccos |
| CN106226455A (en) * | 2016-08-17 | 2016-12-14 | 广西中烟工业有限责任公司 | Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously |
| CN106645503A (en) * | 2017-02-28 | 2017-05-10 | 云南省烟草质量监督检测站 | Measuring method of contents of Li<+>, Na<+>, NH4<+>, K<+>, Mg<2+> and Ca<2+> ions in smoke-laden packaging bag |
| CN108279274A (en) * | 2017-12-28 | 2018-07-13 | 科之杰新材料集团有限公司 | The detection method of calcium oxide and content of magnesia in a kind of portland cement |
| US10073019B2 (en) | 2014-11-06 | 2018-09-11 | Cem Corporation | Rapid quantitative element testing |
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2010
- 2010-11-17 CN CN 201010547686 patent/CN102116767B/en active Active
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102901791A (en) * | 2012-10-16 | 2013-01-30 | 红塔烟草(集团)有限责任公司 | Method for determining content of calcium carbonate in reconstituted tobacco |
| US10073019B2 (en) | 2014-11-06 | 2018-09-11 | Cem Corporation | Rapid quantitative element testing |
| CN105699503A (en) * | 2016-01-14 | 2016-06-22 | 广西中烟工业有限责任公司 | Method for simultaneously determining content of sodium, potassium, magnesium and calcium in tobaccos |
| CN106226455A (en) * | 2016-08-17 | 2016-12-14 | 广西中烟工业有限责任公司 | Ammonium, potassium, calcium and the analysis method of magnesium in a kind of Nicotiana tabacum L. of mensuration simultaneously |
| CN106645503A (en) * | 2017-02-28 | 2017-05-10 | 云南省烟草质量监督检测站 | Measuring method of contents of Li<+>, Na<+>, NH4<+>, K<+>, Mg<2+> and Ca<2+> ions in smoke-laden packaging bag |
| CN108279274A (en) * | 2017-12-28 | 2018-07-13 | 科之杰新材料集团有限公司 | The detection method of calcium oxide and content of magnesia in a kind of portland cement |
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