CN102901791A - Method for determining content of calcium carbonate in reconstituted tobacco - Google Patents
Method for determining content of calcium carbonate in reconstituted tobacco Download PDFInfo
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- CN102901791A CN102901791A CN2012103927068A CN201210392706A CN102901791A CN 102901791 A CN102901791 A CN 102901791A CN 2012103927068 A CN2012103927068 A CN 2012103927068A CN 201210392706 A CN201210392706 A CN 201210392706A CN 102901791 A CN102901791 A CN 102901791A
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Abstract
The invention relates to a method for determining the content of calcium carbonate in reconstituted tobacco, which belongs to the technical field of the reconstituted tobacco. The method is characterized in that an excessive acetic acid solution is used for extracting the reconstituted tobacco, a modern analytical method is utilized to determine the content of total calcium ions in the reconstituted tobacco, then the content of free calcium ions in the reconstituted tobacco extracted by deionized water is analyzed, and the difference between the content of the total calcium ions and the content of the free calcium ions is utilized to calculate the content of the calcium carbonate in the reconstituted tobacco. The method has the characteristics of easiness and convenience in operation, high analysis speed, high sensitivity and good accuracy and stability, and is especially suitable for determining the content of the calcium carbonate in a large number of reconstituted tobacco samples.
Description
Technical field:
The invention belongs to the reconstituted tobacco technical field, be specifically related to the assay method of calcium carbonate content in a kind of reconstituted tobacco.
Background technology:
Reconstituted tobacco (Reconstituted Tobacco) is to utilize the tobacco materials such as offal, offal, tobacco cut to make sheet or thread reconstituted product for raw material, as cigarette filler.Adding papermaking-method reconstituted tobaccos in cigarette, not only can take full advantage of the tobacco leaf resource, reduce production costs, can also effectively reduce tar content in cigarette, is the effective way that improves safety cigarette.The main technique such as the papermaking-method reconstituted tobaccos production run mainly comprises extraction, concentrated, slurrying, manufactures paper with pulp and be coated with, dry are added a certain amount of calcium carbonate to improve ash content, usually to improve its physical property, such as absorbent, appearance property etc. in the production.The content of calcium carbonate is convenient to estimate its product appearance, smoke condition etc. in the therefore accurate Fast Measurement reconstituted tobacco.At present, the method of domestic mensuration calcium ion mainly contains ultraviolet-visible photometry, atomic absorption spectrography (AAS), potentiometric titration, inductive coupling ICP-MS, the chromatography of ions etc., the sample pre-treatments of aforementioned several method is complicated, complex operation, minute is longer, and use the ion-chromatographic determination calcium ion, its analysis speed is fast, operating process simple, accuracy and precision is high, favorable reproducibility, has a good application prospect.2011, land house inscription improves the tobacco business standard, and " YC/T 314-2009 content of calcium carbonate in cigarette paper is measured, potentiometric titration ", the content of calcium carbonate in cigarette paper that utilized ion chromatography, have the characteristics such as detectability is low, accuracy is high, good reproducibility (Yunnan chemical, 38(5): 29-30).
Have no at present calcium carbonate content mensuration research in the report reconstituted tobacco, in the prior art, also do not utilize the report of calcium carbonate content in the ion chromatography analysis reconstituted tobacco so far.
Summary of the invention:
For the problems referred to above, the purpose of this invention is to provide the assay method of calcium carbonate content in a kind of reconstituted tobacco, the method is easy and simple to handle, highly sensitive, quick and precisely.
For achieving the above object, the present invention takes following technical scheme:
The assay method of calcium carbonate content in a kind of reconstituted tobacco, it is characterized in that containing following steps: first with excessive acetic acid solution extraction reconstituted tobacco, utilize Modern Methods to measure its total calcium ion content, then under similarity condition, analyze the reconstituted tobacco Free Calcium ion concentration of deionized water extraction, utilize both differences to calculate calcium carbonate content in the reconstituted tobacco.
Described Modern Methods is one or more in the chromatography of ions, inductive coupling plasma spectroscopy, inductive coupling ICP-MS or the atomic absorption method, is preferably the chromatography of ions.
The chromatography of ions of the described chromatography of ions need be equipped with pump module, electric conductivity detector/chromatogram module, injector module, leacheate generator and chromatographic work station routinely.
The analysis condition of the described chromatography of ions is: cation exchange column DIONEX Ion Pac CS12 (4 mm i.d * 50 mm); Kation guard column Ion Pac CG12 (4mm i.d * 50 mm), leacheate is the degree drip washing such as pyrovinic acid (MSA), and drip washing concentration is 20 mmol/L, and flow velocity is 1.0mL/min, rejector DIONEX CSRS 300 4 mm, suppressing electric current is 59 mA; Column temperature: 30 ℃; Sample size is 50 μ L.
The present invention mainly adopts the chromatography of ions to measure respectively the reconstituted tobacco Free Calcium ion concentration of total calcium ion content, deionized water extraction in the reconstituted tobacco of excessive acetic acid solution extraction, utilize both difference to calculate the content of calcium carbonate in the reconstituted tobacco, effectively like this got rid of the impact of the calcium ion of sample on measurement result own.
The present invention is owing to take above technical scheme to have the following advantages: the present invention is applied to the chromatography of ions mensuration of calcium carbonate in the reconstituted tobacco initiatively, and its detection is limited to 0.0136 mg/L, and recovery of standard addition is 94.08%-99.30%, and precision is 0.27%.The method is easy and simple to handle, highly sensitive, quick and precisely, the characteristics such as good reproducibility, have a good application prospect.
Description of drawings
Fig. 1 is calcium ion standard operation liquid chromatography of ions figure of the present invention.
Embodiment
Following embodiment is described in detail of the present invention.
(1) the reconstituted tobacco sample mill is powdered and mistake 40 mesh sieves, accurately take by weighing 0.1g (being accurate to 0.0001 g) sample, place the 250mL conical flask, accurately add the deionized water of 100mL1% acetic acid aqueous solution or 100mL, shaking table vibration 30min(rotating speed is 120 to turn under room temperature);
(2) get supernatant liquor, extract (10 times of the need dilutions of acid solution extraction) is moved into the 2mL sample bottle behind 0.22 μ m membrane filtration, stand-by;
(3) drawing standard curve: acetic acid aqueous solution 0.5 mL, 1.5 mL, 2.5 mL, 3.5 mL, 4.5 mL, 5 mL that pipette respectively proven 100 ug/mL with transfer pipet, be settled to 50 mL, obtain the standard operation liquid of 6 variable concentrations (1ppm, 3 ppm, 5 ppm, 7 ppm, 9 ppm, 10 ppm), standard solution is carried out analyzing and testing, obtain the measurement result of standard operation liquid, horizontal ordinate is retention time (min), ordinate is conductivity (μ S), the drawing standard working curve; Calcium carbonate content by formula (1) calculates:
M=100 * (M1-M2)/40 formula (1)
In the formula:
M(ω, CaCO
3)---calcium carbonate content in the thin slice, unit are milligram/every gram (mg/g);
M1(ω
1)---the calcium ion content that the acetic acid solution extraction obtains, unit is milligram/every gram (mg/g);
M2(ω
2)---the calcium ion content that the deionized water extraction obtains, unit is milligram/every gram (mg/g).
(4) result calculates: the peak area of solution calcium ion per sample, reading result from the typical curve, calculate the calcium carbonate content of thin slice sample, take the mean value of twice replicate determination as final measurement result, be accurate to 0.001 mg/g, the twice replicate determination as a result difference of absolute value should not surpass 1%.
Embodiment
1, sample pre-treatments
Powdered and mistake 40 mesh sieves with the reconstituted tobacco sample mill, accurately take by weighing 0.1g (being accurate to 0.0001 g) sample, place the 250mL conical flask, accurately add 100mL, the deionized water of 1% acetic acid aqueous solution or 100mL, shaking table vibration 30min(rotating speed is 120 to turn under room temperature).Extract (10 times of the need dilutions of acid solution extraction) is moved into the 2mL sample bottle behind 0.22 μ m membrane filtration, carry out the calcium ion analysis.
2, chromatographiccondition
Cation exchange column DIONEX Ion Pac CS12 (4 mm i.d * 50 mm); Kation guard column Ion Pac CG12 (4mm i.d * 50 mm).Leacheate is the degree drip washing such as pyrovinic acid (MSA), and drip washing concentration is 20 mmol/L, and flow velocity is 1.0mL/min.Rejector DIONEX CSRS 300 4 mm, suppressing electric current is 59 mA; Column temperature: 30 ℃; Sample size is 50 μ L.
Under above-mentioned chromatographic condition, standard specimen and the sample of calcium ion carried out analyzing and testing, adopt retention time qualitative, external standard method is quantitative.
3, working curve and detectability, quantitative limit
3.1 working curve is made
With national standard sample calcium Ca as Ca
2+Reference material, with the acetic acid aqueous solution of 1% (volume fraction) as solvent, preparation calcium ion standard reserving solution.It is the standard operation liquid of 6 variable concentrations (1 mg/L, 3 mg/L, 5 mg/L, 7 mg/L, 9 mg/L, 10 mg/L) that standard reserving solution is diluted, standard solution is carried out analyzing and testing, obtain the measurement result of standard operation liquid, horizontal ordinate is retention time (min), and ordinate is conductivity (μ S) (seeing Fig. 1).Concentration by measurement result and standard operation liquid can obtain standard working curve equation and related coefficient (seeing Table 1).
The range of linearity of table 1 calcium ion, linear equation, related coefficient, detectability and quantitative limit
3.2 detectability and quantitative limit
Get the low concentration standard operation liquid 2mL of calcium ion in sample injection bottle, replicate determination 11 times is calculated standard deviation and is obtained detectability and the quantitative limit (seeing Table 1) of calcium ion according to measurement result.
4, reappearance and the recovery
4.1 reappearance
Accurately take by weighing 5 parts of reconstituted tobacco samples, every part of 0.1 g (accurate 0.0001 g) carries out replicate determination under above-mentioned extraction and analysis condition, calcium ion relative standard deviation (RSD) is 0.74%, the analytical approach precision that calcium ion is described is good, has preferably reappearance.
4.2 the recovery
Accurately take by weighing the reconstituted tobacco sample, every part of 0.1 g (accurate 0.0001 g), the standard model that adds respectively three variable concentrations extracts and measures with identical condition, by add scalar, measured quantity is not calculated its recovery (seeing Table 2) behind mark-on measured quantity and the mark-on.The calcium ion recovery illustrates that the analytical approach accuracy of calcium ion is good between 94.08% ~ 99.30%, calcium ion has the preferably recovery (the mark-on measured quantity is not the mean value of 5 replicate determinations, and measured quantity is the mean value of 2 replicate determinations behind the mark-on).
The recovery of table 2 calcium ion
5, the mensuration of actual sample
Accurately take by weighing 18 kinds of reconstituted tobacco sample 0.1g (accurately 0.0001g) and under above-mentioned calcium ion acetic acid solution extraction, deionized water extraction and analysis condition, carry out two parts of replicate determinations respectively, and by calculating CaCO in the reconstituted tobacco
3Content, measurement result sees Table 3, measurement result and theoretical addition are basically identical.
18 kinds of reconstituted tobacco sample tests of table 3 result
Claims (5)
1. the assay method of calcium carbonate content in the reconstituted tobacco, it is characterized in that containing following steps: first with excessive acetic acid solution extraction reconstituted tobacco, utilize Modern Methods to measure its total calcium ion content, then under similarity condition, analyze the reconstituted tobacco Free Calcium ion concentration of deionized water extraction, utilize both differences to calculate calcium carbonate content in the reconstituted tobacco.
2. the assay method of calcium carbonate content in a kind of reconstituted tobacco according to claim 1, it is characterized in that: described Modern Methods is one or more in the chromatography of ions, inductive coupling plasma spectroscopy, inductive coupling ICP-MS or the atomic absorption method, is preferably the chromatography of ions.
3. the assay method of calcium carbonate content in a kind of reconstituted tobacco according to claim 1 and 2, it is characterized in that: the chromatography of ions of the described chromatography of ions need be equipped with pump module, electric conductivity detector/chromatogram module, injector module, leacheate generator and chromatographic work station.
4. the assay method of calcium carbonate content in a kind of reconstituted tobacco according to claim 1 and 2, it is characterized in that: the analysis condition of the described chromatography of ions is: cation exchange column DIONEX Ion Pac CS12 (4 mm i.d * 50 mm); Kation guard column Ion Pac CG12 (4mm i.d * 50 mm), leacheate is the degree drip washing such as pyrovinic acid (MSA), and drip washing concentration is 20 mmol/L, and flow velocity is 1.0mL/min, rejector DIONEX CSRS 300 4 mm, suppressing electric current is 59 mA; Column temperature: 30 ℃; Sample size is 50 μ L.
5. the assay method of calcium carbonate content in a kind of reconstituted tobacco according to claim 3, it is characterized in that: the analysis condition of the described chromatography of ions is: cation exchange column DIONEX Ion Pac CS12 (4 mm i.d * 50 mm); Kation guard column Ion Pac CG12 (4mm i.d * 50 mm), leacheate is the degree drip washing such as pyrovinic acid (MSA), and drip washing concentration is 20 mmol/L, and flow velocity is 1.0mL/min, rejector DIONEX CSRS 300 4 mm, suppressing electric current is 59 mA; Column temperature: 30 ℃; Sample size is 50 μ L.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675143A (en) * | 2013-12-17 | 2014-03-26 | 红塔烟草(集团)有限责任公司 | Method for determining content of calcium carbonate in reconstituted tobacco |
| CN103675186A (en) * | 2013-12-17 | 2014-03-26 | 红塔烟草(集团)有限责任公司 | Method for determining content of calcium oxalate in tobacco |
| CN103743803A (en) * | 2013-12-13 | 2014-04-23 | 云南中烟昆船瑞升科技有限公司 | Method for measuring calcium carbonate retention rate of papermaking method reconstituted tobacco |
| CN104483230A (en) * | 2014-12-17 | 2015-04-01 | 云南瑞升烟草技术（集团）有限公司 | Method for testing content of calcium carbonate in paper-making process regenerated tobacco leaf |
| CN104886756A (en) * | 2015-05-13 | 2015-09-09 | 湖北中烟工业有限责任公司 | Method for detecting padding calcium carbonate content in paper-making process sheet tobacco basic sheet |
| CN109142450A (en) * | 2018-07-17 | 2019-01-04 | 青岛大学 | Method based on electrical conductivity method measurement sugar alcohol fertilizer of chelated calcium chelation percent |
| CN110631947A (en) * | 2019-09-23 | 2019-12-31 | 云南省烟草质量监督检测站 | Method for determining content of calcium carbonate in paper-making reconstituted tobacco |
| CN112525979A (en) * | 2020-11-20 | 2021-03-19 | 云南省烟草质量监督检测站 | ICP-MS method for determining content of calcium carbonate in paper-making reconstituted tobacco |
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Cited By (9)
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|---|---|---|---|---|
| CN103743803A (en) * | 2013-12-13 | 2014-04-23 | 云南中烟昆船瑞升科技有限公司 | Method for measuring calcium carbonate retention rate of papermaking method reconstituted tobacco |
| CN103743803B (en) * | 2013-12-13 | 2015-09-09 | 云南中烟再造烟叶有限责任公司 | A kind of method measuring papermaking-method reconstituted tobaccos calcium carbonate retention rate |
| CN103675143A (en) * | 2013-12-17 | 2014-03-26 | 红塔烟草(集团)有限责任公司 | Method for determining content of calcium carbonate in reconstituted tobacco |
| CN103675186A (en) * | 2013-12-17 | 2014-03-26 | 红塔烟草(集团)有限责任公司 | Method for determining content of calcium oxalate in tobacco |
| CN104483230A (en) * | 2014-12-17 | 2015-04-01 | 云南瑞升烟草技术（集团）有限公司 | Method for testing content of calcium carbonate in paper-making process regenerated tobacco leaf |
| CN104886756A (en) * | 2015-05-13 | 2015-09-09 | 湖北中烟工业有限责任公司 | Method for detecting padding calcium carbonate content in paper-making process sheet tobacco basic sheet |
| CN109142450A (en) * | 2018-07-17 | 2019-01-04 | 青岛大学 | Method based on electrical conductivity method measurement sugar alcohol fertilizer of chelated calcium chelation percent |
| CN110631947A (en) * | 2019-09-23 | 2019-12-31 | 云南省烟草质量监督检测站 | Method for determining content of calcium carbonate in paper-making reconstituted tobacco |
| CN112525979A (en) * | 2020-11-20 | 2021-03-19 | 云南省烟草质量监督检测站 | ICP-MS method for determining content of calcium carbonate in paper-making reconstituted tobacco |
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