CN112525889A - CFA-FP method for determining content of calcium carbonate in cigarette paper - Google Patents

CFA-FP method for determining content of calcium carbonate in cigarette paper Download PDF

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CN112525889A
CN112525889A CN202011305724.9A CN202011305724A CN112525889A CN 112525889 A CN112525889 A CN 112525889A CN 202011305724 A CN202011305724 A CN 202011305724A CN 112525889 A CN112525889 A CN 112525889A
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solution
cigarette paper
calcium carbonate
content
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彭丽娟
李苓
李雪梅
王春琼
李郸
陈丹
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Yunnan tobacco quality supervision and inspection station
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Abstract

The invention discloses a CFA-FP method for measuring the content of calcium carbonate in cigarette paper. Fully reacting a cigarette paper sample with 1mol/L hydrochloric acid solution, fixing the volume with water, filtering by qualitative filter paper to obtain a sample solution, continuously feeding sample by using 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 calcium carbonate content in the cigarette paper. The method is simple and convenient to operate, fast, high in accuracy and very suitable for measuring a large number of samples.

Description

CFA-FP method for determining content of calcium carbonate in cigarette paper
Technical Field
The invention belongs to the technical field of detection of physical and chemical indexes of cigarette paper, and particularly relates to a method for rapidly and accurately measuring the content of calcium carbonate in the cigarette paper by using a continuous flow-flame photometric analyzer (CFA-FP).
Background
The calcium carbonate is an important filler in the production of the cigarette paper, and has the effects of improving the physical properties of the cigarette paper, the whiteness of the cigarette ash after combustion, adjusting the combustion performance of the cigarette paper, improving the internal quality and the like. However, the calcium carbonate as the filler has extremely small particle size and cannot be completely retained in the pulp fibers, and the lost fine filler enters a sewage system along with the thick white water, so that the environment is polluted and great waste is caused. In order to improve the problem of calcium carbonate retention rate in the cigarette paper production process, the calcium carbonate content in the cigarette paper needs to be quickly and accurately measured. At present, according to the GB/T742-2008 'determination (900 ℃) of paper, paperboard and pulp residues (ash content)' requirements in the industry, an ash content index is used for evaluation, and because the index contains two parts of ash content brought in by tobacco raw materials and added calcium carbonate, the evaluation of the actually added calcium carbonate content has no practical significance, and the method is complicated and time-consuming, and cannot meet the requirement of monitoring the calcium carbonate retention rate in the production process.
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 of measuring the content of calcium carbonate in the cigarette paper 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 cigarette paper 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 cigarette paper comprises the following steps:
(1) drawing a standard working curve: prepared at a concentration of 10gTransferring 10.0 mL, 8.0 mL, 6.0 mL, 4.0 mL, 2.0 mL and 0.0mL of Ca standard solution into a 100mL volumetric flask by using a pipette, diluting with water to a constant volume to obtain 1.0 g/L, 0.8 g/L, 0.6 g/L, 0.4 g/L, 0.2 g/L and 0.0g/L of 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 (y) 43159x +3301, correlation coefficient r2＝0.9992；
(2) Sample solution preparation: cutting the cigarette paper to be tested into strips, drying the strips at 105 ℃ for 2 hours, weighing 0.5g of dried cigarette paper 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, fixing the volume with water, and then filtering the samples with qualitative filter paper to obtain 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 calcium carbonate content in the cigarette paper sample according to the formula (1)
Figure BDA0002788272900000021
In the formula (I), the compound is shown in the specification,
x represents the content of calcium carbonate in the cigarette paper, 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%.
In the step (2), when the sample to be detected is non-white cigarette paper, activated carbon particles are added into a sample solution for oscillation and decoloration before the sample solution is filtered by qualitative filter paper.
Compared with the prior art, the invention has the following advantages:
the invention firstly utilizes the continuous flow-flame photometric combined analyzer to realize the rapid and accurate determination of the calcium carbonate content in the cigarette paper. Continuous sample introduction by using a continuous flow analyzer, and Ca measurement by using a flame photometer2+The content is that the cigarette paper 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 electrons which are unstable in the excited state and are transited back to the ground state is detected by a photoelectric system, and the energy is detected with 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 0.0090g/L and the quantification limit is 0.0209g/L according to 3 times and 10 times of standard deviation of blank solution measured repeatedly for 10 times. The measurement was repeated 6 times for 2 samples, and the Relative Standard Deviation (RSD) was 0.30% and 0.53%, respectively; the recovery range for 2 addition levels of 2 samples ranged from 95.00% to 101.50%. 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 cigarette paper sample with excessive hydrochloric acid (HCl), adding activated carbon particles, oscillating, filtering, continuously feeding sample with continuous flow analyzer, and measuring Ca with 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+The contents are in proportion 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).
Cigarette paper samples were collected from Yunnan Hongta blue eagle paper industry Co.
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 cigarette paper baked for 2 hours at 105 ℃, putting the 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, and then fixing the volume with water (non-white cigarette paper needs to be added with activated carbon particles for oscillation and decoloration), and then filtering with qualitative filter paper, wherein the filtrate is used as a sample solution for standby.
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 calcium carbonate content in the cigarette paper sample according to the formula (1).
Figure BDA0002788272900000051
In the formula:
x represents the content of calcium carbonate in the cigarette paper, 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 A was treated according to 1.3.2, only the amount of hydrochloric acid concentration was changed, and the influence of the change on the response value of the sample solution was examined. 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
Figure BDA0002788272900000052
Figure BDA0002788272900000061
2.2 Standard operating Curve
Respectively transferring 10.0, 8.0, 6.0, 4.0, 2.0 and 0.0g/L Ca standard solution toDiluting with water to constant volume to scale in a 100mL volumetric flask, sequentially obtaining 1.0, 0.8, 0.6, 0.4, 0.2 and 0.0g/L series of standard working solutions, 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 43159x +3301, correlation coefficient r20.9992, 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 is 0.0090g/L, and the quantification limit is 0.0209 g/L.
TABLE 2 detection limit and quantitation limit calculation procedure
Figure BDA0002788272900000062
2.4 repeatability and stability
The results of the measurement of 2 samples are shown in Table 3 after 6 times of simultaneous measurement and 3 days of different time measurement, and the RSD is respectively 0.30 percent and 0.53 percent, and both are less than 5 percent, which shows that the method has good repeatability and stability.
TABLE 3 repeatability and stability
Figure BDA0002788272900000063
Figure BDA0002788272900000071
2.5 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 were 97.94% and 98.61%, respectively, and the recovery rates ranged from 95.00% to 101.50%, indicating that the method was accurate and reliable in detection results.
TABLE 4 recovery
Figure BDA0002788272900000072
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 (2)

1. A CFA-FP method for measuring the content of calcium carbonate in cigarette paper comprises 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 (y) 43159x +3301, correlation coefficient r2＝0.9992；
(2) Sample solution preparation: cutting the cigarette paper to be tested into strips, drying the strips at 105 ℃ for 2 hours, weighing 0.5g of dried cigarette paper 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, fixing the volume with water, and then filtering the samples with qualitative filter paper to obtain 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 calcium carbonate content in the cigarette paper sample according to the formula (1)
Figure FDA0002788272890000011
In the formula (I), the compound is shown in the specification,
x represents the content of calcium carbonate in the cigarette paper, 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. The method for measuring according to claim 1, wherein: in the step (2), when the sample to be detected is non-white cigarette paper, activated carbon particles are added into a sample solution for oscillation and decoloration before the sample solution is filtered by qualitative filter paper.
CN202011305724.9A 2020-11-20 2020-11-20 CFA-FP method for determining content of calcium carbonate in cigarette paper Withdrawn CN112525889A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113624698A (en) * 2021-07-20 2021-11-09 昆明理工大学 Method for rapidly determining content of calcium carbonate and fibers in white water of cigarette paper

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113624698A (en) * 2021-07-20 2021-11-09 昆明理工大学 Method for rapidly determining content of calcium carbonate and fibers in white water of cigarette paper
CN113624698B (en) * 2021-07-20 2023-12-15 昆明理工大学 Method for rapidly determining content of calcium carbonate and fiber in white water of cigarette paper

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Application publication date: 20210319