CN106950143A - A kind of measuring method of content of calcium carbonate in cigarette paper - Google Patents
A kind of measuring method of content of calcium carbonate in cigarette paper Download PDFInfo
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- CN106950143A CN106950143A CN201710202905.0A CN201710202905A CN106950143A CN 106950143 A CN106950143 A CN 106950143A CN 201710202905 A CN201710202905 A CN 201710202905A CN 106950143 A CN106950143 A CN 106950143A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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Abstract
The invention discloses a kind of measuring method of content of calcium carbonate in cigarette paper, it is related to cigarette material physical and chemical inspection technical field, is to utilize thermogravimetry, the content of calcium carbonate in cigarette paper is accurately measured by TG curves.Sample size is small, analysis time is short, low cost, simple to operate needed for present invention detection, and experimental result is accurate.
Description
Technical field
The present invention relates to a kind of measuring method of content of calcium carbonate in cigarette paper, belong to cigarette material physical and chemical inspection technology neck
Domain.
Background technology
CaCO3Influence as the important filler of cigarette paper to cigarette has：(1) whiteness of cigarette paper is increased；(2) paper is improved
Index of refraction is opened, so as to improve the opacity of cigarette paper, makes the not show-through color of pipe tobacco；(3) Smoldering rate of cigarette paper is adjusted, is allowed to
It is consistent with the Smoldering rate of pipe tobacco, it is to avoid pipe tobacco seam broken or cigarette extinguish；(4) air permeability of cigarette paper is adjusted, is ensureing cigarette
Tar content in reduction flue gas on the basis of suction taste；(5) the grey performance of bag of cigarette paper is improved.Therefore, calcium carbonate is to improving cigarette
Quality, lowering harm and decreasing coking are played an important role, and the quality for monitoring cigarette paper is used for frequently as a key index.
The method of existing detection content of calcium carbonate in cigarette paper has potentiometric titration, AAS, but these methods are deposited
Operating the problems such as relatively complicated, agents useful for same is numerous and diverse.
Thermogravimetry be usually used in study biomass pyrolytic characteristic, can with tracking display biomass in pyrolytic process in real time
Physical characteristic (quality etc.) change, there is quick, easy, accurate and METHOD FOR CONTINUOUS DETERMINATION.Research shows, in cigarette pattern
On the thermogravimetric curve of product, the catabolic phase of calcium carbonate and other courses of reaction are relatively independent, therefore can based on thermogravimetric curve
So that the content of calcium carbonate in cigarette paper is precisely calculated.
The content of the invention
To overcome the defect of prior art, the invention provides a kind of measuring method of content of calcium carbonate in cigarette paper, purport
Thermogravimetry is being used, the content of calcium carbonate in cigarette paper is accurately obtained by TG curves.
The present invention solves technical problem and adopted the following technical scheme that：
The measuring method of content of calcium carbonate in cigarette paper of the present invention, comprises the following steps：
Step 1, pretreatment
Cigarette paper is cut into fragment, then dries to constant weight, places into standby in drying basin；
Step 2, thermogravimetric analysis
Set the heating rate of thermogravimetric analyzer for 20 DEG C/min, work climate be air atmosphere, operating temperature be 50~
900 DEG C, measure the thermogravimetric curve of cigarette paper after being pre-processed；The thermogravimetric curve is using temperature as abscissa, with weightlessness
Percentage is ordinate；
Step 3, calculating calcium carbonate content
According to the thermogravimetric curve obtained, the mass percent shared by obtaining calcium carbonate in cigarette paper is calculated as formula (1)
In formula：For the mass percent shared by calcium carbonate in cigarette paper, unit %；
w1For in thermogravimetric curve, 560 DEG C of corresponding percent weight loss, unit %；
w2For in thermogravimetric curve, 800 DEG C of corresponding percent weight loss, unit %；
For the molal weight of carbon dioxide, it is worth for 44g/mol；
For the molal weight of calcium carbonate, it is worth for 100g/mol.
In the thermal weight loss TG curves of cigarette paper, horizontal linear is presented in 560 ± 20 DEG C of temperature ranges, this stage is calcium carbonate
Stable state before decomposition；To 800 ± 20 DEG C, Decomposition of Calcium Carbonate terminates, and horizontal linear is presented in TG curves again.In this two horizontal linear
Between curve corresponding to temperature range be Decomposition of Calcium Carbonate temperature range.Therefore, it is used as volume using 560 DEG C and 800 DEG C
The measurement standard of calcium carbonate content in cigarette paper.
Decomposition equation of the calcium carbonate in the case of heated be：CaCO3=CaO+CO2↑.Therefore, the temperature of Decomposition of Calcium Carbonate
Mass loss in interval should be attributed to calcium carbonate and be discharged CO by thermal decomposition2It is caused, therefore obtain the computing formula of formula (1).
Compared with prior art, beneficial effects of the present invention are embodied in：
The present invention utilizes thermogravimetry, by the thermal weight loss TG curves of cigarette paper sample can it is easy, accurately measure
The content of calcium carbonate in cigarette paper, not only highly shortened analysis total time on test, measurement efficiency is improved, while subtracting significantly
Sample size needed for few detection (milligram level), in addition invention also avoids numerous and diverse operating process involved in the prior art and
Reagent is consumed.
Brief description of the drawings
Fig. 1 is that content of calcium carbonate in cigarette paper test repeatability tests TG curves；
Fig. 2 is content of calcium carbonate in cigarette paper test rate of recovery experiment TG curves.
Embodiment
Below by way of embodiment, and with reference to accompanying drawing, the invention will be further described.
Embodiment 1
The present embodiment is with identical three (A of cigarette paper sample retest1、A2、A3), to verify the precision of the inventive method
Degree.Concrete operations are comprised the steps of：
Step 1, pretreatment
Cigarette paper is cut into 1mm2The fragment of size, is placed in 50 DEG C of baking ovens 48 hours, is then placed in standby in drying basin.
Step 2, thermogravimetric analysis
Empty crucible is placed on thermogravimetric analyzer test balance, treats that in-furnace temperature stably reaches thermogravimetric program initial temperature 50
DEG C when, reset balance mass number.Weigh 10 ± 1mg samples to be placed in crucible, be put into stove, treat that in-furnace temperature stably reaches thermogravimetric
During 50 DEG C of program initial temperature, cigarette paper chip samples quality is accurately weighed.
With 20 DEG C/min heating rate under air atmosphere (20mL/min), from 50 DEG C of temperature programmings to 900 DEG C, obtain
Thermal weight loss TG curve of the cigarette paper sample under air atmosphere.
Step 3, calculating calcium carbonate content
According to the thermogravimetric curve obtained, the mass percent shared by obtaining calcium carbonate in cigarette paper is calculated as formula (1)
In formula：For the mass percent shared by calcium carbonate in cigarette paper, unit %；
w1For in thermogravimetric curve, 560 DEG C of corresponding percent weight loss, unit %；
w2For in thermogravimetric curve, 800 DEG C of corresponding percent weight loss, unit %；
For the molal weight of carbon dioxide, it is worth for 44g/mol；
For the molal weight of calcium carbonate, it is worth for 100g/mol.
Repeat step 1-3 is tested 3 times, and Fig. 1 is the TG curve maps of cigarette paper sample retest three times, and table 1 is calcium carbonate
Content reperformance test result, the relative deviation and the coefficient of variation of test result are respectively less than 1%, illustrate the precision of the inventive method
Degree is high.
The reperformance test result of table 1
Embodiment 2
The present embodiment cigarette after non-mark-on calcium carbonate cigarette paper sample A (known calcium carbonate content is 29.3%) and mark-on
Pattern product A+1, A+2 (calcium carbonate content is respectively 32.1%, 35.3% after mark-on) make rate of recovery test.
Fig. 2 is the TG curves of sample test before and after calcium carbonate mark-on, and table 2 is rate of recovery test result, is surveyed twice after mark-on
The rate of recovery for trying calcium carbonate is respectively 100.6% and 100.8%, illustrates that the accuracy of the inventive method is good, test result can
Lean on.
The rate of recovery test result of table 2
| Sample | Calcium carbonate original content/% | Test value/% | The rate of recovery/% |
| A | 29.3 | - | - |
| A+1 | 32.1 | 32.3 | 100.6 |
| A+2 | 35.3 | 35.6 | 100.8 |
Embodiment 3
10 kinds of cigarette paper samples are randomly selected in the present embodiment, calcium carbonate content test is carried out according to the inventive method, and
Contrasted with the potentiometric titration testing result of 10 cigarette paper samples, to verify the accuracy of the inventive method.
Experiment parameter is set and experimentation is same as Example 1, and comparing result is shown in Table 3.The inventive method and current potential
The result of titration test calcium carbonate content is compared, and difference is smaller, and relative deviation is respectively less than 2%, illustrates two methods detection knot
Fruit is consistent.
The inventive method of table 3 is contrasted with potentiometric titration testing result
| Sample number into spectrum | The inventive method/% | Potentiometric titration/% | Relative deviation/% |
| 1 | 29.3 | 29.4 | -0.34 |
| 2 | 28.4 | 28.7 | -1.05 |
| 3 | 31.7 | 32.1 | -1.25 |
| 4 | 31.3 | 31.8 | -1.57 |
| 5 | 29.8 | 30.1 | -1.00 |
| 6 | 32.1 | 32.0 | 0.31 |
| 7 | 32.6 | 32.0 | 1.88 |
| 8 | 27.6 | 27.1 | 1.85 |
| 9 | 31.5 | 31.9 | -1.25 |
| 10 | 31.3 | 31.8 | -1.57 |
To sum up, using thermogravimetry measure content of calcium carbonate in cigarette paper is simple to operate, required sample size is few, detection is tied
Fruit is accurate, precision is high, with other consistent with methods and resultses.
The exemplary embodiment of the present invention is the foregoing is only, is not intended to limit the invention, it is all the present invention's
Any modification, equivalent and improvement made within spirit and principle etc., should be included within the scope of the present invention.
Claims (2)
1. a kind of measuring method of content of calcium carbonate in cigarette paper, it is characterised in that comprise the following steps：
Step 1, pretreatment
Cigarette paper is cut into fragment, then dries to constant weight, places into standby in drying basin；
Step 2, thermogravimetric analysis
It is that air atmosphere, operating temperature are 50~900 for 20 DEG C/min, work climate to set the heating rate of thermogravimetric analyzer
DEG C, measure the thermogravimetric curve of cigarette paper after being pre-processed；The thermogravimetric curve is using temperature as abscissa, with weightless percentage
Than for ordinate；
Step 3, calculating calcium carbonate content
According to the thermogravimetric curve obtained, the mass percent shared by obtaining calcium carbonate in cigarette paper is calculated as formula (1)：
In formula：For the mass percent shared by calcium carbonate in cigarette paper, unit %；
w1For in thermogravimetric curve, 560 DEG C of corresponding percent weight loss, unit %；
w2For in thermogravimetric curve, 800 DEG C of corresponding percent weight loss, unit %；
For the molal weight of carbon dioxide, it is worth for 44g/mol；
For the molal weight of calcium carbonate, it is worth for 100g/mol.
2. the measuring method of content of calcium carbonate in cigarette paper according to claim 1, it is characterised in that：Dried in step 1
Method to constant weight is dried 48 hours to be placed in 50 DEG C of baking ovens.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108680454A (en) * | 2018-05-23 | 2018-10-19 | 福建中烟工业有限责任公司 | A kind of method and device of evaluation calcium carbonate quality stability |
| CN108827819A (en) * | 2018-04-09 | 2018-11-16 | 广东电网有限责任公司 | Regression analysis-based silicone rubber content determination method |
| 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 |
| CN109540728A (en) * | 2018-10-23 | 2019-03-29 | 福建中烟工业有限责任公司 | Predict the method for releasing content of coke tar and/or carbon monoxide release amount in cigarette |
| 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 |
| CN111579422A (en) * | 2020-06-17 | 2020-08-25 | 福建中烟工业有限责任公司 | Method for determining calcium carbonate in reconstituted tobacco |
| CN111595721A (en) * | 2020-06-24 | 2020-08-28 | 广东联塑科技实业有限公司 | Method for measuring PVC (polyvinyl chloride) content and calcium content in polyvinyl chloride product |
| CN112798732A (en) * | 2020-12-29 | 2021-05-14 | 国高材高分子材料产业创新中心有限公司 | Method for detecting content of calcium carbonate in polyolefin material |
| 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 (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108827819A (en) * | 2018-04-09 | 2018-11-16 | 广东电网有限责任公司 | Regression analysis-based silicone rubber content determination method |
| CN108680454A (en) * | 2018-05-23 | 2018-10-19 | 福建中烟工业有限责任公司 | A kind of method and device of evaluation calcium carbonate quality stability |
| 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 |
| CN109540728A (en) * | 2018-10-23 | 2019-03-29 | 福建中烟工业有限责任公司 | Predict the method for releasing content of coke tar and/or carbon monoxide release amount in cigarette |
| CN109540728B (en) * | 2018-10-23 | 2021-08-06 | 福建中烟工业有限责任公司 | Method for predicting tar release amount and/or carbon monoxide release amount in cigarette |
| 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 |
| CN111579422A (en) * | 2020-06-17 | 2020-08-25 | 福建中烟工业有限责任公司 | Method for determining calcium carbonate in reconstituted tobacco |
| CN111595721A (en) * | 2020-06-24 | 2020-08-28 | 广东联塑科技实业有限公司 | Method for measuring PVC (polyvinyl chloride) content and calcium content in polyvinyl chloride product |
| CN112798732A (en) * | 2020-12-29 | 2021-05-14 | 国高材高分子材料产业创新中心有限公司 | Method for detecting content of calcium carbonate in polyolefin material |
| 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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