CN102507483B - Method for determining content of calcium carbonate in cigarette paper - Google Patents
Method for determining content of calcium carbonate in cigarette paper Download PDFInfo
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Abstract
The invention discloses a method for determining the content of calcium carbonate in cigarette paper, which comprises the steps of: treating the cigarette paper to be determined with hydrochloric acid and distilled water and filtering, adding a potassium iodate aqueous solution and a potassium iodide aqueous solution into the filtrate for reaction; diluting with distilled water without carbon dioxide and analyzing with a spectrophotometer at wavelength of 352nm; and then drawing a standard curve and calculating to obtain the result. In the invention, the spectrophotometer is applied to determining calcium carbonate in cigarette paper for the first time. The recovery rate is 98.2-100.8% and variation coefficient range of continuous five-time determining results is 0.0031-0.40%. The inter-day variation coefficient range is 1.34%. There is no significant difference when comparing the determining result by national standard method with the result by the method of the invention. The method is simple and convenient to operate, fast to analyze, and has high accuracy and precision, strong stability and good application prospect.
Description
Technical field
The invention belongs to cigarette material physical and chemical inspection technical field, be specifically related to a kind of method that can the Accurate Determining content of calcium carbonate in cigarette paper.
Background technology
Calcium carbonate not only affects the exterior quality of cigarette paper, such as whiteness, opacity etc., also affect the gas penetration potential, flammability, bag ash performance of cigarette etc., fall Jiao for Harm reduction techniques to play an important role, so, be an important indicator of cigarette paper quality control always.Because the product after its burning does not hinder health, for many years, or even unique filler of cigarette paper.In the prior art, the report of measuring based on potentiometric titration, thermogravimetric mass spectroscopy etc. is arranged.But all there is the comparatively loaded down with trivial details problem of operation in these methods.
Spectrophotometric method is a kind of common analytical approach, and it absorbs to measure content of material based on material to the selectivity of light, has that analysis speed is fast, accuracy and advantages such as precision is high, easy and simple to handle, highly versatile.If the method is applied to the detection of cigarette paper, should be able to overcomes well the deficiency that existing detection method exists, but successful report is not yet arranged in the prior art.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of method of measuring content of calcium carbonate in cigarette paper is provided, use spectrophotometric method, under the prerequisite that guarantees accuracy in detection, precision and stability, simplify the process of measuring.
Purpose of the present invention is achieved by the following technical programs.
Except as otherwise noted, percentage of the present invention is percent by weight.
A kind of method of measuring content of calcium carbonate in cigarette paper may further comprise the steps:
1, cigarette paper to be measured is shredded and dry to constant weight, take by weighing the 0.50g paper scrap, place the 150mL beaker, adding concentration is the aqueous hydrochloric acid solution 35.0mL of 0.1mol/L, after being stirred well to fiber dispersion, overflowing without bubble, the distilled water of adding 65.0mL removing carbon dioxide filters with qualitative filter paper after fully mixing, and collection filtrate is stand-by;
2, get 2.0mL filtrate in the 50mL volumetric flask, adding concentration is the Potassiumiodate aqueous solution 2.0mL of 5g/L, and concentration is the potassium iodide aqueous solution 3.0mL of 50g/L, react after 5 minutes, to scale, mixing is analyzed in the 352nm wavelength with spectrophotometer with the distilled water diluting of removing carbon dioxide;
3, drawing standard curve: the hydrochloric acid solution 1.0,2.0,3.0,4.0, the 5.0mL that pipette respectively proven 0.1mol/L with transfer pipet, be settled to 100mL, after step (2) colour developing and measuring, take absorbance as horizontal ordinate, calcium carbonate content is ordinate drawing standard working curve; Calcium carbonate content by formula (1) calculates:
In the formula:
CaO%-content of calcium carbonate in cigarette paper, unit are mass percent (%);
C
HClThe accurate concentration of-0.1mol/L HCl standard solution, unit is every liter (mol/L) of mole;
V
HCl-adding the volume of 0.1mol/L HCl standard solution, unit is milliliter (mL);
V
Std-0.1mol/L HCl standard solution the volume of taking when painting typical curve, unit are milliliter (mL);
The calcium oxide quality that the every mole hydrochloride reaction of 28-consumes, unit is every mole (g/mol) of gram;
The 1000-volume conversion factor will be transformed into liter (L) with milliliter volume of the standard solution of (mL) expression;
The G-sample quality, unit is gram (g).
4, the result calculates: the absorbance of solution per sample, reading result from the typical curve obtains the calcium carbonate content of sample after the deduction blank, take the mean value of twice replicate determination as final measurement result, the difference of absolute value should be above 0.4% as a result to be accurate to 0.1%, twice replicate determination.
With respect to prior art, the present invention has the following advantages: the present invention is applied to spectrophotometric method the mensuration of calcium carbonate in the cigarette paper initiatively.Its recovery scope is 98.2～100.8%, and the coefficient of variation scope of continuous 5 measurement results is: 0.0031～0.40%, and coefficient of variation scope is in the daytime: 1.34%, compare no significant difference with the testing result of national standard method.The method is easy and simple to handle, analysis speed is fast, and accuracy and precision are high, stability is strong, have a good application prospect.
Description of drawings
Fig. 1 potassium iodate solution addition is on the impact of sample solution absorbance;
Fig. 2 liquor kalii iodide addition is on the impact of sample solution absorbance;
Fig. 3 reaction time is on the impact of sample solution absorbance;
Fig. 4 sample standing time is on the impact of sample solution absorbance;
Fig. 5 standard working curve.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples, but drawings and Examples are not limited to the technical solution, and all should belong to protection scope of the present invention based on the variation that training centre of the present invention is done.
1. experimental principle, material and method
1.1 experimental principle
The excessive HCl solution reaction of cigarette paper sample and known accurate amount is by using the remaining H+ of spectrophotometry.The content of acid is directly proportional with the colour developing production concentration, can measure in the 352nm place.Can extrapolate cigarette paper calcium carbonate content (in CaO) by acid content.
1.2 material and instrument
Potassiumiodate (AR, prompt chemical reagent company limited is moistened in Shanghai); Potassium iodide (AR, Solution on Chemical Reagents in Shanghai company limited), hydrochloric acid (AR, chemical plant, Gansu Province, west, Shantou, Guangdong city); Calcium carbonate (working standard reagent (capacity), analysis on trace institute of Tongji University); The distilled water of removing carbon dioxide (self-control); 4 cigarette paper samples are Yunnan Hongta Lanying Paper Industry Co., Ltd.'s product.
JA5002 balance (sensibility reciprocal 0.01g, Shanghai balance equipment factory); METLER AE200 analytical balance (sensibility reciprocal: 0.0001g, Switzerland METLER TOLEDO company); HP5873 ultraviolet-visible pectrophotometer (U.S. Hewlett-Packard Corporation); 101A-2 drying box (Shanghai City experimental apparatus head factory).
1.3 sample preparation and analysis
1.3.1 acid reaction
Take by weighing the dry to constant weight paper scrap (0.5cm * 2.5cm) of (being accurate to 0.01g) of 0.5g, put into the 150mL beaker, add 0.1mol/L hydrochloric acid solution 35.0mL with transfer pipet, after being stirred well to fiber dispersion, overflowing without bubble with glass rod, add the 65.0mL deionized water with transfer pipet, filter with qualitative filter paper after fully mixing, collection filtrate is stand-by.
1.3.2 colour developing and mensuration
Get 2.0mL filtrate in the 50mL volumetric flask, add 5g/L Potassiumiodate aqueous solution 2.0mL, 50g/L potassium iodide aqueous solution 3.0mL reacted after 5 minutes, used the distilled water diluting of removing carbon dioxide to scale, and mixing is analyzed in the 352nm wavelength with spectrophotometer.
2. result and discussion
2.1 choice of experimental conditions
2.1.1 wavelength is selected
Take 1nm as the interval, light absorption to standard specimen from 200nm to 700nm scans, and the gained absorption curve shows two absorption peaks, is respectively 280nm and 352nm, consider that the 280nm chaff interference is more, therefore select to have more distinctive 352nm as the optimal wavelength of analyzing.
2.1.2 the potassium iodate solution consumption is on the impact of sample solution absorbance
Keep other condition constant, add the 5g/L Potassiumiodate aqueous solution of different amounts, the absorbance log of sample solution changes such as Fig. 1.The result shows that the Potassiumiodate amount of aqueous solution used is on the not obviously impact of sample solution absorbance.This experimental selection 2.0mL.
2.1.3 the liquor kalii iodide consumption is on the impact of sample solution absorbance
Other condition is constant, adds respectively 50g/L liquor kalii iodide 0.4ml, 0.8ml, 1.2mL, 1.6mL, 2.0mL, 3.0mL, 5.0mL, 8.0mL, surveys absorbance, as shown in Figure 2, the addition of liquor kalii iodide during greater than 3mL absorbance change less.So selecting 3.0mL is the addition of liquor kalii iodide.
2.1.4 the reaction time is on the impact of sample solution absorbance
After three kinds of reagent mix, reaction occurs immediately, and it is faint yellow that solution is, and different reaction durations produces different absorbances.Keep other condition constant, the absorbance variation of reacting respectively after 0,1,2,5,15 minute sees that Fig. 3, result show, chemical reaction is very fast, and afterreaction reached stable in 5 minutes, therefore selected 5 minutes reaction time.
2.1.5 sample solution test stabilization time
Sample solution was placed 2,5,10,20,30,60,180,300 minutes respectively at room temperature, measured its stability.Test findings is seen Fig. 4.As seen sample was stable in 3 hours.
2.2 typical curve
Preparation and demarcation concentration are the hydrochloric acid solution of 0.1074mol/L, pipette respectively this solution 1.0,2.0,3.0,4.0,5.0mL with transfer pipet, be settled to 100mL, after the 1.3.2 colour developing and measuring, calculate corresponding calcium carbonate content (in CaO) according to formula (1), obtain the standard working curve such as Fig. 5, the x axle is the absorbance of solution, the y axle is calcium carbonate content (in CaO)), equation of linear regression is y=-0.6014x+21.65, coefficient R 2=1.
2.3 the recovery
In the pattern of known content (mean values of 3 mensuration), add calcium carbonate a certain amount of, that behind 110～120 ℃ of baking 1.5～2h, in sulphuric acid desiccator, cool off, measure its calcium carbonate, the recovery is respectively 98.2%, 100.8% (seeing Table 1), the accuracy of illustration method is good, and testing result is reliable.
Table 1 recovery
2.4 repeatability
A, B, C, a D4 sample are distinguished continuous detecting 5 times, the results are shown in Table 2.The coefficient of variation is 0.40% to the maximum, illustrates that the precision of the method is high.
The reperformance test result of table 2 spectrophotometric method
2.5 stability test
The C sample is detected 3 times at different time, and each sample continuous detecting 5 times the results are shown in Table 3.The coefficient of variation is 1.34%, illustrates that this method has good stability.
The stability test result of table 3 spectrophotometric method
Annotate: 1. each data is the mean value of continuous 5 measurement results
2.6 the comparison with other method
Detect respectively 4 samples with spectrophotometric method and potentiometric titration, the results are shown in Table 4.Spectrophotometric method is compared with potentiometric titration, and detected value is on the low side, but difference is less, and maximum difference is 0.3%, illustrates that spectrophotometric method is consistent with the potentiometric titration testing result.
Table 4 spectrophotometric method and other method testing result are relatively
3, conclusion
Utilize that spectrophotometry cigarette paper calcium carbonate is easy and simple to handle, the result is accurate, precision is high, good stability, with other consistent with methods and results, be a kind ofly can satisfy the method that modernized production of cigarettes detects.
Claims (1)
1. method of measuring content of calcium carbonate in cigarette paper may further comprise the steps:
(1) cigarette paper to be measured is shredded and dry to constant weight, take by weighing the 0.50g paper scrap, place the 150mL beaker, adding concentration is the aqueous hydrochloric acid solution 35.0mL of 0.1mol/L, after being stirred well to fiber dispersion, overflowing without bubble, the distilled water of adding 65.0mL removing carbon dioxide filters with qualitative filter paper after fully mixing, and collection filtrate is stand-by;
(2) get 2.0mL filtrate in the 50mL volumetric flask, adding concentration is the Potassiumiodate aqueous solution 2.0mL of 5g/L, and concentration is the potassium iodide aqueous solution 3.0mL of 50g/L, react after 5 minutes, to scale, mixing is analyzed in the 352nm wavelength with spectrophotometer with the distilled water diluting of removing carbon dioxide;
(3) drawing standard curve: the hydrochloric acid solution 1.0,2.0,3.0,4.0, the 5.0mL that pipette respectively proven 0.1mol/L with transfer pipet, be settled to 100mL, after step (2) colour developing and measuring, take absorbance as horizontal ordinate, calcium carbonate content is ordinate drawing standard working curve; Calcium carbonate content by formula (1) calculates:
In the formula:
CaO(%)-content of calcium carbonate in cigarette paper represents that with CaO number percent unit is mass percent (%);
C
HClThe accurate concentration of-0.1mol/L HCl standard solution, unit is every liter (mol/L) of mole;
V
HCl-adding the volume of 0.1mol/L HCl standard solution, unit is milliliter (mL);
V
Std-0.1mol/L HCl standard solution the volume of taking when painting typical curve, unit are milliliter (mL);
The calcium oxide quality of 28-every mole hydrochloride reaction consumption, unit is every mole (g/mol) of gram;
1000-volume conversion factor will be transformed into liter (L) with milliliter volume of the standard solution of (mL) expression;
G-sample quality, unit is gram (g);
(4) result calculates: the absorbance of solution per sample, reading result from the typical curve obtains the calcium carbonate content of sample after the deduction blank, take the mean value of twice replicate determination as final measurement result, the difference of absolute value should be above 0.4% as a result to be accurate to 0.1%, twice replicate determination.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| JP6826810B2 (en) * | 2015-10-07 | 2021-02-10 | 住友化学株式会社 | Polarizer |
| CN105758813A (en) * | 2016-04-22 | 2016-07-13 | 广西中烟工业有限责任公司 | Method for determining phosphate in cigarette paper |
| CN106370609A (en) * | 2016-08-29 | 2017-02-01 | 云南省烟草质量监督检测站 | Method for measuring acid value of tobacco essence |
| CN106442499A (en) * | 2016-09-26 | 2017-02-22 | 云南省烟草质量监督检测站 | Method for measuring content of calcium carbonate in paper-making reconstituted tobacco |
| CN106950143A (en) * | 2017-03-30 | 2017-07-14 | 安徽中烟工业有限责任公司 | A kind of measuring method of content of calcium carbonate in cigarette paper |
| CN109030274A (en) * | 2018-08-01 | 2018-12-18 | 超威电源有限公司 | The measuring method of carbonic acid lead content in a kind of lead-acid accumulator green plate |
| 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 |
| CN113203614B (en) * | 2021-05-21 | 2022-05-17 | 江苏中烟工业有限责任公司 | Method for determining calcium carbonate in reconstituted tobacco by applying enzymatic reaction |
| 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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