CN102590383A - Method for determining content of potassium, sodium, calcium and magnesium in cigarette paper simultaneously - Google Patents
Method for determining content of potassium, sodium, calcium and magnesium in cigarette paper simultaneously Download PDFInfo
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Abstract
The invention discloses a method for determining content of potassium, sodium, calcium and magnesium in cigarette paper simultaneously, which includes the following steps: cutting 100+/-0.1 mg of a cigarette paper sample, using 100mL of 0.02mol/L hydrochloric acid as an extracting agent, ultrasonic-extracting for 18-22min to obtain extract liquor, selecting 5.0mL of the extract liquor to a 25mL volumetric flask, bringing to the volume with 0.02mol/L hydrochloric acid to obtain diluent, and filtering the diluent through a 0.45 mu m filtering film to obtain sample liquid to be detected; selecting sodium chloride, potassium chloride, hexahydrate magnesium chloride and anhydrous calcium chloride, using pure water as solvent, preparing mixed standard solution through gradual diluting, and adding 0.02mol/L hydrochloric acid to prepare series standard working solution; detecting and analyzing the series working solution and the sample liquid to be detected respectively through an ion chromatographic instrument; and drawing a standard curve and calculating results. The method is fast and simple to operate, high in sensitivity, low in detection limit, good in recovery rate, and suitable for batch analyzing of important inorganic elements in the cigarette paper.
Description
Technical field
The present invention relates to a kind of method of measuring potassium in the cigarette paper, sodium, calcium, content of magnesium, a kind of specifically method of measuring potassium in the cigarette paper, sodium, calcium, content of magnesium simultaneously.
Background technology
Cigarette paper is the main auxiliary material of cigarette, and the flue gas composition that cigarette is propped up overall physical properties and cigarette all has material impact.Especially the content of the potassium in the cigarette paper, sodium, calcium, magnesium is the important parameter of evaluating cigarette paper, directly influences the presentation quality and the flammability of cigarette paper.Cigarette paper adds precipitated calcium carbonate not only can improve the outward appearance and the feel of paper, and can also improve air permeability, regulates cigarette burning speed.Discover the flue gas emission of harmful substances when magnesium salts can reduce the cigarette paper burning, add the maximum pyrolysis temperature that magnesium oxide and magnesium hydroxide can reduce cigarette paper, change the fired state of cigarette, thereby reduce the objectionable impurities in the flue gas.Sodium citrate and potassium citrate also are combustion adjuvants commonly used in the cigarette paper, within the specific limits, and along with the increase of addition can significantly reduce tar, nicotine and carbon monoxide content in the main flume.Therefore, accurately measure potassium, sodium, calcium and content of magnesium in the cigarette paper,, further research and develop safety type cigarette and have realistic meaning for evaluating cigarette paper performance and stable cigarette quality.
At present, the assay method of potassium, sodium, calcium, magnesium mainly contains atomic absorption spectrography (AAS), flame photometry etc. in the cigarette paper.Though these methods can solve each compound mensuration problem in the cigarette paper preferably, atomic absorption spectrum and flame photometry all can not realize measuring simultaneously to four kinds of inorganic elements, and the mensuration process is loaded down with trivial details, and precision and sensitivity are relatively poor.
Summary of the invention
The technical issues that need to address of the present invention provide a kind of method of utilizing the chromatography of ions to measure potassium in the cigarette paper, sodium, calcium, content of magnesium simultaneously.
For solving the problems of the technologies described above, the technical scheme that the present invention adopted is:
Measure the method for potassium in the cigarette paper, sodium, calcium, content of magnesium simultaneously, may further comprise the steps,
A. be that the cigarette paper sample of 100 ± 0.1mg shreds with quality; With the hydrochloric acid of 100mL 0.02mol/L as extractant; Ultrasonic extraction 18～22min obtains extract, gets the 5.0mL extract and moves to the 25mL volumetric flask; Carry out constant volume with the hydrochloric acid of 0.02mol/L and obtain dilution, obtain treating sample measuring liquid with the membrane filtration dilution of 0.45 μ m;
B. get sodium chloride, potassium chloride, Magnesium dichloride hexahydrate, anhydrous calcium chloride, use ultrapure water to be solvent,, add the hydrochloric acid preparation series standard working solution of 0.02mol/L then through stepwise dilution preparation mixed standard solution;
C. utilize ion chromatograph respectively to the series standard working solution with treat that sample measuring liquid carries out check and analysis;
D. typical curve is drawn and result's calculating.
Further improvement of the present invention is: the process for preparation of said series standard working solution comprises the steps:
B1, preparation one-level hybrid standard storing solution take by weighing a certain amount of sodium chloride, potassium chloride, Magnesium dichloride hexahydrate and anhydrous calcium chloride respectively and place a volumetric flask, are settled to 100mL with ultrapure water, are mixed with Na
+, K
+, Mg
2+, Ca
2+Concentration is respectively the one-level hybrid standard storing solution of 0.1mg/mL, 0.5mg/mL, 0.1mg/mL, 4mg/mL;
B2, preparation secondary mixed standard solution pipette 10mL one-level hybrid standard storing solution to the 100mL volumetric flask, are settled to scale with ultrapure water, as the secondary mixed standard solution;
B3, be made into the series standard working solution, accurately pipette 0.0mL, 1.0mL, 2.0mL, 3.0mL, 5.0mL, 10.0mL secondary standard solution respectively to 100 mL volumetric flasks, be settled to scale with the HCL of 0.02mol/L, as the series standard working solution.
Further improvement of the present invention is: the chromatographic condition of working among the said step C is the Ionpac CG12A cation exchange column of 4 * 250mm, and guard column is the CG12A of 4 * 50mm, is detecting device with the electric conductivity detector; CSRS kation rejector with 4mm is a rejector; Eluent adopts the Loprazolam of 0.015mol/L, and flow velocity is 1.2mL/min, and the rejector electric current is 53mA; Sample size is 25 μ L, and column temperature is 35 ℃.
Because the technical progress of having adopted technique scheme, the present invention to obtain is:
The present invention adopts ultrasonic extraction coupled ion chromatography, operate fast and convenient, highly sensitive, detection limit is low, the recovery good, is applicable to the batch quantity analysis of important inorganic elements in the cigarette paper, can measure the content of potassium in the cigarette paper, sodium, calcium, magnesium simultaneously.
Wherein,, consider that the content difference of potassium in the cigarette paper, sodium, calcium, four kinds of ions of magnesium is bigger, Ca in the general sample about the selection of cigarette paper amount of samples
2+Content is about Mg
2+100 times, in order to realize determination and analysis simultaneously, consider the chromatogram response of its four kinds of ions and the consumption of extraction solution, with 0.1g as final sampling amount.
For the selection of extract and acidity, two kinds of elements of potassium sodium are easy to extract in the cigarette paper, adopt water seaoning to carry the district and can extract basically in 10 minutes fully.Because calcium and magnesium in the cigarette paper mainly exist with the form of lime carbonate, magnesium carbonate and magnesium hydroxide, and is not soluble in water, therefore select watery hydrochloric acid as extraction solution.Acidity has certain influence to chromatographic column and abundance in addition, and is better for guaranteeing each ion peak shape, and the mensuration result all reaches maximum.Potassium, sodium, calcium and magnesium in the hydrochloric acid extraction cigarette paper of selection 0.02mol/L.
For extracting mode, vibration is extracted lower to the extraction efficiency of four kinds of ions, and 1h still can not be complete with every kind of The ion extraction; Homogenate method 3 minutes can be complete with four kinds of The ion extraction basically, but repeatability is relatively poor, and once can only handle a sample, needs to clean rotary head, and is loaded down with trivial details time-consuming to the batch sample; The cigarette paper sample that ultrasonic extraction is handled is loose floccus, and extraction efficiency reaches about 90% during ultrasonic 10min, and it is maximum that each ion detection value of ultrasonic 18～22min all reaches.
The methyl sulfonic acid of selecting 0.015mol/L is as moving phase, and the response of four kinds of ions is suitable, and retention time is longer, and the ion peak shape is also better.
Description of drawings
Fig. 1 is the chromatography of ions figure of standard model;
Fig. 2 is the chromatography of ions figure of actual sample.
Embodiment
Below in conjunction with embodiment the present invention is explained further details:
Measure the method for potassium in the cigarette paper, sodium, calcium, content of magnesium simultaneously, used instrument, reagent and material are mainly:
ICS3000 ion chromatograph (U.S. DIONEX company); KQ-500 type ultrasonic washing instrument (Kunshan Ultrasonic Instruments Co., Ltd.); HY-5 Clothoid type oscillator (Changzhou Australia China Instr Ltd.); LG16-W type hydro-extractor (BEIJINGJINGLI); IKA T10 type high-speed homogenization machine (Germany); AB204-S type electronic balance (METTLER TOLEDO); Elix Milli-Q ultrapure water machine (MILLIPORE SAS).
Hydrochloric acid, Loprazolam, sodium chloride, potassium chloride, Magnesium dichloride hexahydrate and two hydration lime chloride (analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group).
Cigarette paper is taken from each manufacturer.
Measure the method for potassium in the cigarette paper, sodium, calcium, content of magnesium simultaneously, may further comprise the steps:
A. be that the cigarette paper sample of 0.1g ± 0.1mg shreds with quality, the hydrochloric ultrasonic wave extraction 18～22min with 100mL 0.02mol/L obtains extract, accurately pipettes the 5.0mL extract to the 25mL volumetric flask, obtains dilution with the hydrochloric acid constant volume of 0.02mol/L.Get an amount of dilution after shaking up, obtain treating sample measuring liquid, treat ion chromatography through 0.45 μ m membrane filtration.
B. take by weighing a certain amount of sodium chloride, potassium chloride, Magnesium dichloride hexahydrate and anhydrous calcium chloride respectively, they are placed the volumetric flask of a 100mL, be settled to the scale of 100mL, be mixed with Na with ultrapure water
+, K
+, Mg
2+, Ca
2+Concentration is respectively the one-level hybrid standard storing solution of 0.1mg/mL, 0.5mg/mL, 0.1mg/mL, 4mg/mL; Pipette 10mL one-level hybrid standard storing solution to the 100mL volumetric flask, be settled to the scale of 100mL with ultrapure water, as the secondary mixed standard solution; Accurately pipette 0.0mL, 1.0mL, 2.0mL, 3.0mL, 5.0mL, 10.0mL secondary standard solution respectively to 100 mL volumetric flasks, be settled to the scale of 100mL with the hydrochloric acid of 0.02M, as the series standard working solution.
C. utilize ion chromatograph respectively to the series standard working solution with treat that sample measuring liquid carries out check and analysis; Chromatographic condition is the Ionpac CG12A cation exchange column of 4 * 250mm, and guard column is the CG12A of 4 * 50mm, is detecting device with the electric conductivity detector; CSRS kation rejector with 4mm is a rejector; Eluent adopts the 0.015mol/L Loprazolam, and flow velocity is 1.2mL/min, and the rejector electric current is 53mA; Sample size is 25 μ L, and column temperature is 35 ℃.
D. typical curve is drawn and result's calculating.
The chromatography of ions figure of the chromatography of ions of experiment acquisition Fig. 1 standard model and the actual sample of Fig. 2.
Result and discussion
1. the selection of sample pre-treatments condition
(1) selection of sample size
The content difference of potassium, sodium, calcium, four kinds of ions of magnesium is bigger in the cigarette paper, Ca in the general sample
2+Content is about Mg
2+100 times, in order to realize determination and analysis simultaneously, consider the chromatogram response of its four kinds of ions and the consumption of extraction solution, with 0.1g as final sampling amount.
(2) selection of extract and acidity
Two kinds of elements of potassium sodium are easy to extract in the cigarette paper; Adopt water seaoning to extract and to extract basically in 10 minutes fully; Because calcium and magnesium in the cigarette paper mainly exist with the form of lime carbonate, magnesium carbonate and magnesium hydroxide, and is not soluble in water, therefore select watery hydrochloric acid as extraction solution.Analyze and the hydrochloric acid extraction cigarette paper of experimental selection 0.02mol/L in potassium, sodium, calcium and magnesium, guaranteeing quantitative accuracy, and each ion peak shape is better, measures the result and all reaches maximum.
(3) selection of extracting mode and time
For selecting suitable extracting mode, the present invention compares ultrasonic, vibration and three kinds of modes of homogenate.Obtain of the influence of table 1 extracting mode to four kinds of ion measurement results.Experimental result shows: it is lower to the extraction efficiency of four kinds of ions to vibrate, and 1h still can not be complete with every kind of The ion extraction; Homogenate method 3 minutes can be complete with four kinds of The ion extraction basically, but repeatability is relatively poor, and once can only handle a sample, needs to clean rotary head, and is loaded down with trivial details time-consuming to the batch sample; The cigarette paper sample of ultrasonic Treatment is loose floccus.Through excusing from death 10min, 20min, 30min, 40min comparative measurements result; Extraction efficiency reaches about 90% when finding excusing from death 10min; It is maximum that each ion detection value of ultrasonic 20min all reaches; Along with the prolongation of excusing from death time, it is on a declining curve to measure the result, concrete like the influence of table 2 ultrasonic time to four kinds of ion measurement results.In sum, adopt Extraction by Ultrasound cigarette paper sample, extraction time 18～22min, preferred 20min.
Table 1
| Extracting mode | Na +(mg/g) | K +(mg/g) | Mg 2+(mg/g) | Ca 2+(mg/g) |
| Homogenate | 3.53 | 8.94 | 1.58 | 130.98 |
| Vibration | 2.43 | 7.89 | 1.25 | 123.00 |
| Ultrasonic | 3.81 | 8.95 | 1.39 | 133.52 |
Table 2
| Ultrasonic time | Na +(mg/g) | K +(mg/g) | Mg 2+(mg/g) | Ca 2+(mg/g) |
| 10min | 1.86 | 7.07 | 0.58 | 117.67 |
| 20min | 1.97 | 7.93 | 0.80 | 141.20 |
| 30min | 1.98 | 7.08 | 0.78 | 138.05 |
| 40min | 2.04 | 7.72 | 0.79 | 142.73 |
2. the optimization of chromatography of ions condition
The methyl sulfonic acid of selecting 0.015mol/L is as moving phase, and the response of four kinds of ions is suitable, and retention time is longer, and the ion peak shape is also better.
3. the detection limit of method, linearity, precision and recovery test
Calculate detection limit of the present invention, linearity, precision and recovery test shown in linearity, detection limit and the precision of the recovery of standard addition test findings of 3 four kinds of ions of following table and table 4 method: wherein, RSD is a relative standard deviation, R
2Be related coefficient.
Table 3
The linearity of table 4 method, detection limit and precision
| Project | 1 | 2 | 3 | 4 | 5 | RSD（%） | R 2（%） | Detection limit (mg/g) |
| Na + (mg/g) | 2.05 | 2.18 | 2.14 | 2.03 | 2.25 | 4.26 | 0.976 | 0.05 |
| K + (mg/g) | 7.69 | 7.97 | 8.45 | 8.69 | 8.43 | 4.91 | 0.999 | 0.09 |
| Mg 2+ (mg/g) | 1.20 | 1.29 | 1.32 | 1.29 | 1.33 | 3.96 | 0.998 | 0.02 |
| Ca 2+ (mg/g) | 122.26 | 126.75 | 133.67 | 137.63 | 130.72 | 4.58 | 0.999 | 0.69 |
4. the mensuration of actual sample
Choosing the white cigarette paper of 10 trades mark tests with this method; The result sees the content (mg/g) of sodium, potassium, magnesium and calcium in the different trade mark cigarette paper of table 5; The result shows: calcium content is the highest in 4 kinds of ions of cigarette paper; Average out to 129.2 mg/g, and difference is less between kinds of cigarettes paper, and the coefficient of variation is 5.2%; Next is a potassium, mean value 6.77 mg/g, and the content of sodium and magnesium is minimum, on average is respectively 2.82 mg/g, 1.17 mg/g, and sodium element difference in kinds of cigarettes paper is maximum, and the coefficient of variation reaches 56.9%.
Table 5
| Numbering | Na + | K + | Mg 2+ | Ca 2+ |
| A | 1.29 | 7.08 | 0.88 | 125.7 |
| B | 2.14 | 8.45 | 1.32 | 133.7 |
| C | 2.39 | 5.35 | 0.85 | 134.8 |
| D | 4.46 | 8.34 | 1.19 | 125.8 |
| E | 2.25 | 3.33 | 1.10 | 130.9 |
| F | 1.75 | 5.00 | 1.01 | 134.8 |
| G | 3.56 | 5.22 | 1.72 | 127.1 |
| H | 2.19 | 8.16 | 1.36 | 116.9 |
| I | 1.65 | 8.24 | 1.24 | 123.0 |
| J | 6.53 | 8.54 | 1.02 | 139.5 |
Claims (3)
1. measure the method for potassium in the cigarette paper, sodium, calcium, content of magnesium simultaneously, it is characterized in that: may further comprise the steps,
A. be that the cigarette paper sample of 100 ± 0.1mg shreds with quality; With the hydrochloric acid of 100mL 0.02mol/L as extractant; Ultrasonic extraction 18～22min obtains extract, gets the 5.0mL extract and moves to the 25mL volumetric flask; Carry out constant volume with the hydrochloric acid of 0.02mol/L and obtain dilution, obtain treating sample measuring liquid with the membrane filtration dilution of 0.45 μ m;
B. get sodium chloride, potassium chloride, Magnesium dichloride hexahydrate, anhydrous calcium chloride, use ultrapure water to be solvent,, add the hydrochloric acid preparation series standard working solution of 0.02mol/L then through stepwise dilution preparation mixed standard solution;
C. utilize ion chromatograph respectively to the series standard working solution with treat that sample measuring liquid carries out check and analysis;
D. typical curve is drawn and result's calculating.
2. the method for measuring potassium in the cigarette paper, sodium, calcium, content of magnesium simultaneously according to claim 1 is characterized in that the process for preparation of said series standard working solution comprises the steps:
B1, preparation one-level hybrid standard storing solution take by weighing a certain amount of sodium chloride, potassium chloride, Magnesium dichloride hexahydrate and anhydrous calcium chloride respectively and place a volumetric flask, are settled to 100mL with ultrapure water, are mixed with Na
+, K
+, Mg
2+, Ca
2+Concentration is respectively the one-level hybrid standard storing solution of 0.1mg/mL, 0.5mg/mL, 0.1mg/mL, 4mg/mL;
B2, preparation secondary mixed standard solution pipette 10mL one-level hybrid standard storing solution to the 100mL volumetric flask, are settled to scale with ultrapure water, as the secondary mixed standard solution;
B3, be made into the series standard working solution, accurately pipette 0.0mL, 1.0mL, 2.0mL, 3.0mL, 5.0mL, 10.0mL secondary standard solution respectively to 100 mL volumetric flasks, be settled to scale with the HCL of 0.02mol/L, as the series standard working solution.
3. the method for measuring potassium in the cigarette paper, sodium, calcium, content of magnesium simultaneously according to claim 1; It is characterized in that: the chromatographic condition of working among the said step C is the Ionpac CG12A cation exchange column of 4 * 250mm, and guard column is the CG12A of 4 * 50mm, is detecting device with the electric conductivity detector; CSRS kation rejector with 4mm is a rejector; Eluent adopts the Loprazolam of 0.015mol/L, and flow velocity is 1.2mL/min, and the rejector electric current is 53mA; Sample size is 25 μ L, and column temperature is 35 ℃.
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| CN103969378A (en) * | 2014-04-14 | 2014-08-06 | 北京工业大学 | Ion chromatography method for detecting conventional ions |
| 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 |
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