CN112525890A - CFA-FP method for determining content of calcium carbonate in paper-making reconstituted tobacco - Google Patents
CFA-FP method for determining content of calcium carbonate in paper-making reconstituted tobacco Download PDFInfo
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Abstract
The invention discloses a CFA-FP method for measuring the content of calcium carbonate in paper-making reconstituted tobacco. Fully reacting a reconstituted tobacco sample with an excessive hydrochloric acid solution, adding activated carbon particles, oscillating, decoloring, filtering to obtain a sample solution, continuously feeding the sample solution through a continuous flow analyzer, and measuring Ca of a standard working solution and the sample solution by using a flame photometer2+And finally, calculating to determine the calcium carbonate content in the sample. The invention firstly utilizes the continuous flow-flame photometric combined analyzer to realize the rapid and accurate determination of the content of calcium carbonate in the reconstituted tobacco. The method is simple and convenient to operate, fast, high in accuracy and very suitable for measuring a large number of samples.
Description
Technical Field
The invention belongs to the technical field of cigarette physicochemical index detection, and particularly relates to a method for rapidly and accurately determining the content of calcium carbonate in paper-making reconstituted tobacco by using a continuous flow-flame photometric combined analyzer (CFA-FP).
Background
The calcium carbonate is an important filler of the paper-making reconstituted tobacco, the content of the calcium carbonate affects the physical indexes of the reconstituted tobacco sheet base and the product, such as ash content, quantification, filling value, balanced water content, tensile strength, bulk and the like, and the smoking quality of tar, CO release amount, total particulate matters, smoke, nicotine and the like, and the calcium carbonate plays a role in reducing the cost. Reports of measuring the content of calcium carbonate in cigarette paper by a potentiometric titration method, a burning method and the like are available in the industry, but the methods are all tedious and time-consuming and cannot meet the requirement of monitoring the retention rate of calcium carbonate in the production process of reconstituted tobacco.
The Flame Photometric (FP) method utilizes the emission spectrum characteristics of metal atoms, and the content of metal elements is calculated by a mathematical model of the relation between the intensity of an emission spectrum line and the concentration of an object to be measured, so that the method has the advantages of short test time, simple sample pretreatment, time saving, labor saving and the like. The Continuous Flow (CFA) method has the advantages of continuous sample introduction, instant data processing and the like due to online mixing and dilution, and can realize continuous detection of samples by being combined with the FP meter, thereby greatly improving the detection working efficiency. However, no report for measuring the content of calcium carbonate in the paper-making reconstituted tobacco by a CFA-FP method is found in the prior art.
Disclosure of Invention
The invention aims to provide a method for simply, conveniently, quickly and accurately measuring the content of calcium carbonate in paper-making reconstituted tobacco, aiming at the defects of the prior art.
The purpose of the invention is realized by the following technical scheme.
All percentages used in the present invention are mass percentages unless otherwise indicated.
A CFA-FP method for measuring the content of calcium carbonate in paper-making reconstituted tobacco adopts the following steps:
(1) drawing a standard working curve: preparing 10g/L Ca standard solution, respectively transferring 10.0, 8.0, 6.0, 4.0, 2.0 and 0.0mL Ca standard solution into a 100mL volumetric flask by using a pipette, diluting with water to a constant volume to scale, and respectively obtaining 1.0, 0.8, 0.6, 0.4, 0.2 and 0.0g/L standard working solution; using continuous flow analyser for continuous sample introduction and flame photometer for measuring standard working liquidCa2+Content, using concentration of calcium solution as abscissa and response value of calcium instrument as ordinate to draw standard working curve, linear regression equation (42412 x + 3730.7) and correlation coefficient r2＝0.9997；
(2) Sample solution preparation: cutting reconstituted tobacco to be tested into strips, drying the strips at 105 ℃ for 2 hours, weighing 0.5g of dried reconstituted tobacco strips as samples, putting the samples into a 100mL volumetric flask, adding 4.5mL of hydrochloric acid solution with the concentration of 1mol/L, shaking the volumetric flask until fibers are dispersed and no bubbles overflow, then fixing the volume with water, adding activated carbon particles, oscillating and decoloring, and filtering with qualitative filter paper to obtain a sample solution;
(3) measuring by an instrument:
the continuous flow-flame photometric combined analyzer comprises the following flow paths: a black/black pump pipe for air with the flow rate of 0.32 mL/min; the sample solution is pumped by a red/red pump tube at the flow rate of 0.80 mL/min; the waste liquid is pumped by a white/white pump pipe, and the flow rate is 0.60 mL/min; using a yellow/yellow pump tube for the hydrochloric acid solution, wherein the flow rate is 1.20 mL/min;
the measurement conditions were: detecting speed: 45 samples/h; sample introduction/cleaning time ratio: 1.7; baseline correction: opening;
(4) and (4) calculating a result: calculating the content of calcium carbonate in the reconstituted tobacco sample according to the formula (1)
In the formula (I), the compound is shown in the specification,
x represents the content of calcium carbonate in the reconstituted tobacco, and the unit is mass percent (%);
0.4004-conversion coefficient of calcium ion into calcium carbonate;
c-an instrumental measurement of the calcium ion concentration in the sample solution in grams per liter (g/L);
m is sample weighing, and the unit is gram (g);
the average value of two parallel measurements is used as the final measurement result, the accuracy is 0.1%, and the difference between the absolute values of the two parallel measurements should not exceed 0.4%.
Compared with the prior art, the invention has the following advantages:
the invention firstly utilizes a continuous flow-flame photometric combined analyzer to realize the rapid and accurate determination of the calcium carbonate content in the paper-making reconstituted tobacco. Continuous sample introduction by using a continuous flow analyzer, and Ca measurement by using a flame photometer2+The content, the reconstituted tobacco sample reacts with excessive hydrochloric acid solution, the outer layer electrons of calcium atoms are transited from a ground state to an excited state, the energy released by the transition from the excited state to the ground state after the excited state is unstable is detected by a photoelectric system, and the energy is detected by Ca in the sample solution2+The contents are in proportion relation, so that CaCO in the sample can be calculated3And (4) content. The detection limit of the method is respectively calculated to be 0.10g/L and the quantification limit is 0.26g/L according to 3 times and 10 times of standard deviation of blank solution measured repeatedly for 10 times. The 3 samples are respectively determined repeatedly for 6 times, and the Relative Standard Deviation (RSD) range is 1.29-2.85%; the recovery rate range of 3 addition levels of 2 samples is 95.19% -98.88%; the method is simple, convenient, rapid and accurate, and is very suitable for measuring mass samples.
Drawings
FIG. 1 is a schematic view of a flow path setup for a continuous flow-flame photometric co-analyzer;
figure 2 is a standard operating curve.
Detailed Description
The present invention is further described in detail with reference to the drawings and examples, which are not intended to limit the technical scope of the present invention, and all changes and equivalents which come within the spirit of the teachings of the present invention shall fall within the scope of the present invention.
Example 1
1 materials and methods
1.1 principle of the method
Reacting the paper-making reconstituted tobacco sample with excessive hydrochloric acid (HCl) solution, adding activated carbon particles, vibrating, filtering, continuously feeding sample by using a continuous flow analyzer, and measuring Ca by using a flame photometer2+The content of Ca in the sample solution is determined by the energy released by the transition of the outer electrons of calcium atoms from ground state to excited state, the energy released by the transition of the excited state to ground state and the energy released by Ca2+In an amount ofProportional relation, so that CaCO in the sample can be calculated3And (4) content.
1.2 materials, reagents and instruments
BRAN LUEBBE AA3 continuous flow analyzer (BRAN LUEBBE, Germany); flame Photometer 410(Sherwood), METLER AE200 analytical balance (sensitivity: 0.0001g, METLER TOLEDO, Switzerland).
Hydrochloric acid (AR, west longridge chemical plant, guangdong Shantou city); calcium carbonate (working standard reagent, peer trace element institute); activated carbon granules (Shanghai chemical Co., Ltd., China medicine).
The paper-making method reconstituted tobacco samples are collected from the tobacco reconstituted tobacco limited responsibility company in Yunnan.
1.3 sample calcium carbonate content determination
1.3.1 preparation of Standard working solutions
Respectively transferring 10.0, 8.0, 6.0, 4.0, 2.0 and 0.0mL of Ca standard solution (10g/L) into a 100mL volumetric flask, diluting with water to a constant volume to obtain a series of standard working solutions of 1.0, 0.8, 0.6, 0.4, 0.2 and 0.0g/L in sequence, and storing in a refrigerator at 4 ℃.
1.3.2 sample treatment
Weighing 0.5g (accurate to 0.01g) of thin strips (0.5cm multiplied by 2.5cm) of the reconstituted tobacco leaves by the paper-making method, drying for 2 hours at 105 ℃, putting the thin strips into a 100mL volumetric flask, adding 4.5mL of 1mol/L hydrochloric acid solution, shaking the volumetric flask until fibers are dispersed and no bubbles overflow, then fixing the volume with water, adding activated carbon particles, oscillating and decoloring, then filtering with qualitative filter paper, and taking the filtrate as a sample solution for later use.
1.3.3 instrumental measurements
The analysis was carried out with a continuous flow-flame photometric analyzer, the flow path setup is shown in FIG. 1, and the analysis conditions were: detecting speed: 45 samples/h; sample introduction/cleaning time ratio: 1.7; baseline correction: and (4) opening.
1.3.4 results calculation
And (3) calculating the content of calcium carbonate in the reconstituted tobacco sample according to the formula (1).
In the formula:
x represents the content of calcium carbonate in the reconstituted tobacco, and the unit is mass percent (%);
0.4004-conversion coefficient of calcium ion into calcium carbonate;
c-an instrumental measurement of the calcium ion concentration in the sample solution in grams per liter (g/L);
m is sample weighing, and the unit is gram (g);
the average value of two parallel measurements is used as the final measurement result, the accuracy is 0.1%, and the difference between the absolute values of the two parallel measurements should not exceed 0.4%.
2 results and discussion
2.1 pretreatment condition optimization: influence of the hydrochloric acid concentration
Sample 1a was subjected to sample treatment in accordance with 1.3.2, and only the amount of hydrochloric acid concentration was changed to examine the influence thereof on the response value of the sample solution. When the hydrochloric acid concentration is 1mol/L, the measured value is the largest, so that the hydrochloric acid concentration is 1 mol/L.
TABLE 1 influence of hydrochloric acid concentration on the measurement results
2.2 Standard operating Curve
Respectively transferring 10.0, 8.0, 6.0, 4.0, 2.0 and 0.0mL of Ca standard solution (10g/L) into a 100mL volumetric flask, diluting with water to a constant volume to obtain a series of standard working solutions of 1.0, 0.8, 0.6, 0.4, 0.2 and 0.0g/L in sequence, and storing in a refrigerator at 4 ℃. Continuous sample introduction by a continuous flow analyzer, and Ca determination of standard working solution by a flame photometer2+Content, using concentration of calcium solution as abscissa and response value of calcium instrument as ordinate to draw standard working curve, linear regression equation is that y is 42412x +3730.7, correlation coefficient r20.9997, as shown in fig. 2.
2.3 detection and quantitation limits
The determination is repeated for 10 times by using blank solution according to GB/T27417-. The detection limit was 0.10g/L and the quantification limit was 0.26 g/L.
TABLE 2 detection limit and quantitation limit calculation procedure
2.4 repeatability and stability
The results of the 3 samples are respectively measured for 6 times at the same time and for 3 days at different time are shown in the table 3, the RSD ranges are 1.29-2.85%, and are all less than 5%, which shows that the method has good repeatability and stability.
TABLE 3 repeatability and stability
2.4 recovery
Adding a certain amount of calcium carbonate into a sample with a known content, drying the calcium carbonate for 1.5 to 2 hours at the temperature of 110 to 120 ℃, and cooling the calcium carbonate in a sulfuric acid dryer to determine the content of the calcium carbonate. As shown in Table 4, the average recovery rates of the 2 samples are 97.00% and 97.65%, respectively, and the recovery rates range from 95.19% to 98.88%, indicating that the method has good accuracy and reliable detection results.
TABLE 4 recovery
Each data is the average of 3 consecutive determinations
3 conclusion
The method is simple, convenient, rapid and accurate, and is very suitable for measuring mass samples.
Claims (1)
1. A CFA-FP method for measuring the content of calcium carbonate in paper-making reconstituted tobacco adopts the following steps:
(1) drawing a standard working curve: preparing 10g/L Ca standard solution, respectively transferring 10.0, 8.0, 6.0, 4.0, 2.0 and 0.0mL Ca standard solution into a 100mL volumetric flask by using a pipette, diluting with water to a constant volume to scale, and respectively obtaining 1.0, 0.8, 0.6, 0.4, 0.2 and 0.0g/L standard working solution; continuous sample introduction is carried out by adopting a continuous flow analyzer, and Ca of the standard working solution is measured by a flame photometer2+Content, using concentration of calcium solution as abscissa and response value of calcium instrument as ordinate to draw standard working curve, linear regression equation (42412 x + 3730.7) and correlation coefficient r2＝0.9997；
(2) Sample solution preparation: cutting reconstituted tobacco to be tested into strips, drying the strips at 105 ℃ for 2 hours, weighing 0.5g of dried reconstituted tobacco strips as samples, putting the samples into a 100mL volumetric flask, adding 4.5mL of hydrochloric acid solution with the concentration of 1mol/L, shaking the volumetric flask until fibers are dispersed and no bubbles overflow, then fixing the volume with water, adding activated carbon particles, oscillating and decoloring, and filtering with qualitative filter paper to obtain a sample solution;
(3) measuring by an instrument:
the continuous flow-flame photometric combined analyzer comprises the following flow paths: a black/black pump pipe for air with the flow rate of 0.32 mL/min; the sample solution is pumped by a red/red pump tube at the flow rate of 0.80 mL/min; the waste liquid is pumped by a white/white pump pipe, and the flow rate is 0.60 mL/min; using a yellow/yellow pump tube for the hydrochloric acid solution, wherein the flow rate is 1.20 mL/min;
the measurement conditions were: detecting speed: 45 samples/h; sample introduction/cleaning time ratio: 1.7; baseline correction: opening;
(4) and (4) calculating a result: calculating the content of calcium carbonate in the reconstituted tobacco sample according to the formula (1)
In the formula (I), the compound is shown in the specification,
x represents the content of calcium carbonate in the reconstituted tobacco, and the unit is mass percent (%);
0.4004-conversion coefficient of calcium ion into calcium carbonate;
c-an instrumental measurement of the calcium ion concentration in the sample solution in grams per liter (g/L);
m is sample weighing, and the unit is gram (g);
the average value of two parallel measurements is used as the final measurement result, the accuracy is 0.1%, and the difference between the absolute values of the two parallel measurements should not exceed 0.4%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113203826A (en) * | 2021-05-21 | 2021-08-03 | 江苏中烟工业有限责任公司 | CO (carbon monoxide)2Method for measuring calcium carbonate in reconstituted tobacco by continuous flow system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113203826A (en) * | 2021-05-21 | 2021-08-03 | 江苏中烟工业有限责任公司 | CO (carbon monoxide)2Method for measuring calcium carbonate in reconstituted tobacco by continuous flow system |
| CN113203826B (en) * | 2021-05-21 | 2022-08-26 | 江苏中烟工业有限责任公司 | CO (carbon monoxide) 2 Method for measuring calcium carbonate in reconstituted tobacco by continuous flow system |
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