CN113203818B - Method for measuring calcium carbonate in reconstituted tobacco by high-pressure closed reaction system - Google Patents
Method for measuring calcium carbonate in reconstituted tobacco by high-pressure closed reaction system Download PDFInfo
- Publication number
- CN113203818B CN113203818B CN202110558412.7A CN202110558412A CN113203818B CN 113203818 B CN113203818 B CN 113203818B CN 202110558412 A CN202110558412 A CN 202110558412A CN 113203818 B CN113203818 B CN 113203818B
- Authority
- CN
- China
- Prior art keywords
- solution
- calcium carbonate
- tobacco
- reconstituted tobacco
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring calcium carbonate in reconstituted tobacco by using a high-pressure closed reaction system, which comprises the following steps: s1, beating the reconstituted tobacco into tobacco powder, uniformly mixing, and drying to constant weight for later use; s2, weighing the tobacco powder prepared in the step S1, placing the tobacco powder in a high-pressure reactor, adding a sodium nitrate aqueous solution, adding ethanol for extraction, adding dry ice particles, quickly sealing the reactor, and filtering to obtain a sample solution after the reaction is finished; s3, diluting the sample solution obtained in the step S2 with water, and filtering the diluted sample solution with a water-based filter membrane to obtain a solution to be detected; s4, measuring Ca of the solution to be measured obtained in the step S3 by adopting an inductively coupled plasma mass spectrometer (ICP-MS) 2+ The response signal intensity is then brought into a standard working curve to obtain Ca in the liquid to be detected 2+ And finally, calculating the content of calcium carbonate in the reconstituted tobacco according to a formula. The high-pressure reaction system provided by the method can change the target calcium carbonate into calcium bicarbonate to be extracted, and can avoid the dissolution of other calcium salts in the reconstituted tobacco.
Description
Technical Field
The invention relates to the technical field of analysis of calcium carbonate content in reconstituted tobacco, in particular to a method for determining calcium carbonate in reconstituted tobacco by using a high-pressure closed reaction system.
Background
Calcium carbonate is an inorganic compound of the formula CaCO 3 Commonly known as limestone, stone powder, marble, etc. Calcium carbonate is neutral, substantially insoluble in water, and soluble in hydrochloric acid. White solid, tasteless, odorless. There are amorphous and crystalline forms. The crystal form can be further divided into orthorhombic and hexagonal crystal forms, and is either columnar or rhombic. The relative density was 2.71. Decomposing at 825-896.6 deg.C, and decomposing into calcium oxide and carbon dioxide at about 825 deg.C. Melting point 1339 deg.C, melting point 1289 deg.C at 10.7 MPa. Is insoluble in water and alcohol, reacts with dilute acid, and releases carbon dioxide to form exothermic reaction. Also dissolved in ammonium chloride solution. It is one of the common substances on earth, exists in aragonite, calcite, chalk, limestone, marble, travertine and other rocks, and is also the main component of animal bones or shells. The calcium carbonate is an important additive in the production process of the reconstituted tobacco by the paper-making method, has the functions of reducing the hydrogen bond effect between slurry fibers, is beneficial to improving the bulk of a substrate and the penetration of coating liquid, and reduces the release amount of substances such as tar, CO and the like of the reconstituted tobacco. From the physical index, along with the increase of the mesh number of the calcium carbonate filler, the tensile strength, the burst strength, the filling value and the equilibrium moisture content of the film base and the finished product are increased on the whole, and the bulk is decreased, but the influence of the mesh number of the calcium carbonate on the physical index of the finished product on the whole has no obvious influence on the film base.
The shredded tobacco leaves, the tobacco stems, the tobacco powder and the like are main raw materials of the reconstituted tobacco leaves. Reconstituted Tobacco (Reconstituted tobaccos) is a sheet-shaped or filiform regenerated product prepared from Tobacco materials such as Tobacco powder, Tobacco stems, Tobacco shreds and the like serving as raw materials and used as a cigarette filler. The paper-making process reconstituted tobacco is added into the cigarettes, so that the tobacco resources can be fully utilized, the production cost is reduced, the tar content of the cigarettes can be effectively reduced, and the method is an effective way for improving the safety of the cigarettes. The production process of the paper-making reconstituted tobacco mainly comprises main processes of extraction, concentration, pulping, papermaking, coating, drying and the like, and a certain amount of calcium carbonate is usually added in the production process to improve the ash content so as to improve the physical properties, such as liquid absorption performance, appearance performance and the like. The calcium carbonate is a filler which is often added in the production process of the reconstituted tobacco, the smoking quality of the reconstituted tobacco can be improved, and the content of the calcium carbonate directly influences the characteristics of ash content, filling property, porosity, liquid absorption performance, appearance and the like of the reconstituted tobacco. Therefore, the content of calcium carbonate in the reconstituted tobacco is accurately and quickly determined, and the product appearance, the smoke condition and the like are conveniently evaluated. The main methods for measuring calcium carbonate at present are complexation titration, potentiometric titration, continuous flow method and ion chromatography. The measuring process of the complexometric titration method and the potentiometric titration method is complicated, and human errors are easily introduced; the ion chromatography and the continuous flow method are both used for measuring the mass fraction of acid-soluble total calcium, and calcium element in the reconstituted tobacco coexists in various forms (water-soluble inorganic calcium, organic calcium, calcium phosphate, calcium oxalate and calcium carbonate), and calcium in different forms sometimes dissolves out together in an acid solution, so that the two methods cannot accurately reflect the mass fraction of calcium carbonate in a sample.
Chinese patent No. CN102901791A discloses a method for measuring the content of calcium carbonate in reconstituted tobacco, which comprises the steps of firstly extracting the reconstituted tobacco by using excessive acetic acid solution, measuring the total calcium ion content by using a modern analysis method, then analyzing the content of free calcium ions in the reconstituted tobacco extracted by deionized water under the same condition, and calculating the content of calcium carbonate in the reconstituted tobacco by using the difference of the two contents. However, the method has the obvious defect that the reconstituted tobacco contains a large amount of calcium pectate which is insoluble in water and soluble in acetic acid, and the calcium in the calcium pectate is calculated as calcium carbonate according to the measurement result, so that the measurement result is higher.
Chinese patent (CN 201910897278.6) discloses a method for determining the content of calcium carbonate in paper-making reconstituted tobacco. The method is characterized by firstly applying a carbon-nitrogen analyzer to the determination of the content of calcium carbonate in the paper-making reconstituted tobacco, respectively determining total carbon and organic carbon in the paper-making reconstituted tobacco by different pretreatment methods, calculating inorganic carbon by a difference method, and then calculating the content of calcium carbonate in the reconstituted tobacco according to the conversion of the molecular weights of carbon and calcium carbonate. However, this method has significant disadvantages in that the data obtained by the conversion of the molecular weights of carbon and calcium carbonate is large in error, and the influence of other carbon contained in the tobacco itself is not taken into consideration.
Disclosure of Invention
In order to solve the problems, the invention provides a method for measuring calcium carbonate in reconstituted tobacco by using a high-pressure closed reaction system, which comprises the steps of extracting reconstituted tobacco by using sodium nitrate aqueous solution and ethanol, adding dry ice particles for reaction under high pressure, converting water-insoluble calcium carbonate into soluble calcium bicarbonate, filtering and diluting, and measuring Ca by using an inductively coupled plasma mass spectrometer (ICP-MS) 2+ The response signal intensity of (2) is substituted into the standard working curve to obtain Ca 2+ The concentration of (C) is finally calculated by a formula to obtain Ca 2+ The content of (a). CO produced by dry ice gasification 2 Selectively reacting with calcium carbonate (without reacting with other calcium-containing substances in the tobacco leaves) to generate soluble calcium bicarbonate, and calculating the difference between the solution to be detected and the blank solution to be detected to accurately obtain the content of the calcium carbonate in the reconstituted tobacco.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a method for measuring calcium carbonate in reconstituted tobacco by using a high-pressure closed reaction system is characterized by comprising the following steps:
s1, beating the reconstituted tobacco into tobacco powder, uniformly mixing, and drying to constant weight for later use;
s2, weighing the tobacco powder prepared in the step S1, placing the tobacco powder into a high-pressure reactor, adding a sodium nitrate water solution and ethanol as extraction liquid for extraction, then adding dry ice particles, sealing the reactor, and filtering to obtain a sample solution after the reaction is finished;
s3, diluting the sample solution obtained in the step S2 with water, and filtering the diluted sample solution with a water-based filter membrane to obtain a solution to be detected;
s4, measuring Ca of the solution to be measured obtained in the step S3 by adopting ICP-MS 2+ The Ca of the response signal of (2) is calculated from the standard curve 2+ The concentration of (3) C; measuring Ca of the blank solution to be measured by ICP-MS 2+ The Ca of the response signal of (2) was calculated from the standard curve 2+ Concentration C of 0 ；
The blank liquid to be detected is different from the liquid to be detected in that no dry ice particles are added;
the manufacturing method of the standard working curve comprises the following steps: preparing Ca with different concentrations 2+ Standard solution, measuring Ca with different concentrations by ICP-MS 2+ Signal intensity of (2), then with Ca 2+ Intensity of signal of (2) to Ca in standard solution 2+ Linear regression is carried out on the corresponding concentration, an instrument automatically establishes a standard curve, and Ca in the detected liquid is calculated according to the standard curve 2+ The concentration of (c);
s5, calculating the content of calcium carbonate in the reconstituted tobacco:
in the above formula:
x represents the content of calcium carbonate in the reconstituted tobacco, and the unit is microgram per gram (mu g/g);
c-concentration of target in micrograms per milliliter (. mu.g/mL) from the standard working curve;
C 0 -target concentration in micrograms per milliliter (μ g/mL) in a blank sample from a standard working curve;
v-volume of extract in milliliters (mL);
f is dilution multiple;
m-sample mass in grams (g);
100——CaCO 3 the formula (2);
40——Ca 2+ the formula (2).
Further, the mass ratio of the tobacco powder, the sodium nitrate aqueous solution, the ethanol and the dry ice in the step S2 is (0.1-0.2): (50-100): 3.945: (2-5).
Further, after the dry ice particles are added in the step S2, the pressure in the high pressure reactor is 15 to 30 Psi.
Further, the sample solution in the step S3 is diluted by 90 to 110 times with water.
Further, the water-based filter membrane in the step S3 is a 0.45 μm water-based filter membrane.
Further, in the step S2, the extraction time of the sodium nitrate aqueous solution and the ethanol is 20-60 min.
Na in aqueous sodium nitrate solution + And NO 3- The calcium ion generator is completely ionized, hydrolysis does not occur, and other precipitates cannot be generated by reaction with calcium ions when water is used for dilution in the later period, so that errors in experimental results are avoided, and the accuracy of experiments is further improved.
Dry Ice (Dry Ice) is solid carbon dioxide, which is liquefied to a colorless liquid at 6250.5498 kpa and rapidly solidified at low pressure. And the carbon dioxide absorbs a large amount of heat when changing from a solid to a gas, so that the temperature of the surrounding air is rapidly reduced.
Dry ice is added into a high-pressure reactor, and the dry ice can be rapidly gasified to generate a large amount of CO 2 Gas, greatly improves the pressure of the system, and can increase CO 2 Solubility in water, such that CO 2 In addition, the gasification of the dry ice can also absorb the ambient heat and reduce the temperature of the reaction system, so that the temperature of the reaction system is maintained at low temperature, the stability of the calcium bicarbonate in the solution is improved, and the increase of the internal energy of the solution and the temperature rise caused by high pressure can be effectively avoided. Meanwhile, sodium nitrate and ethanol are added into the extraction liquid to reduce the freezing point of the extraction liquid, so that the temperature of the reaction system is prevented from being reduced after the dry ice is added, and the extraction liquid is solidified.
The invention has the beneficial effects that:
1. according to the method for determining calcium carbonate in the reconstituted tobacco by using the high-pressure closed reaction system, provided by the invention, the reconstituted tobacco is extracted by using a sodium nitrate aqueous solution and ethanol, then dry ice particles are added into the reconstituted tobacco, after the dry ice particles are sublimated, the water-insoluble calcium carbonate is converted into soluble calcium bicarbonate under a high-pressure condition, meanwhile, the dissolution of other calcium salts (calcium phosphate, calcium oxalate and calcium sulfate) in the reconstituted tobacco can be avoided, the extraction accuracy is high, and the reliability is strong. The method has the characteristics of small interference, high sensitivity, no reagent pollution and the like, and can be applied to the determination of the content of calcium carbonate in various calcium salt mixed systems.
2. According to the method for determining calcium carbonate in reconstituted tobacco by using high-pressure closed reaction system, provided by the invention, after the added dry ice particles are sublimated, the pressure in the reaction system can be increased, the temperature is reduced, and CO can be increased 2 The solubility in water promotes the calcium carbonate in the reconstituted tobacco to be converted into calcium bicarbonate, and the temperature of a reaction system can be kept at a low temperature, so that the stability of the calcium bicarbonate is improved.
3. According to the method for determining calcium carbonate in reconstituted tobacco by using the high-pressure closed reaction system, provided by the invention, sodium nitrate and ethanol are added into the extraction liquid, so that the freezing point of the extraction liquid can be reduced, and the phenomenon that the temperature of the reaction system is reduced after dry ice is added to the extraction liquid, so that the extraction liquid is solidified is prevented.
Drawings
FIG. 1 is a flow chart of a method for determining calcium carbonate in reconstituted tobacco by using a high-pressure closed reaction system in the embodiment of the invention.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the following will describe the specific embodiments of the present invention with reference to the accompanying drawings.
It is obvious that the drawings in the following description are only some examples of the invention, and it is obvious to a person skilled in the art that other drawings and other embodiments can be obtained from these drawings without inventive effort, and the invention is not limited to this example.
The specific embodiment of the invention is as follows:
ICP-MS instrument analysis conditions: the measurement mode is He collision mode; the radio frequency power is 1550W; sampling depth: 7.5 mm; the flow rate of plasma gas is 15.0L/min; the carrier gas flow is 1.0L/min; the auxiliary gas flow is 1.0L/min; the temperature of the atomization chamber is 2 ℃; the acquisition mode is full quantitative analysis; the number of repetitions was 3.
Example 1
Preparation of a standard curve:
six gradients of calcium ion standard solutions were prepared at concentrations of 0.2mg/L, 0.5 mg/L, 1.0 mg/L, 1.5 mg/L, 2.0 mg/L, and 2.5mg/L, and Ca was measured using ICP-MS for these six standard solutions 2+ In response to signal intensity of (2), then with Ca 2+ The concentration is an abscissa and the corresponding response signal intensity is an ordinate, the instrument automatically establishes a standard curve to obtain a linear equation Y =0.2063X +0.0126, wherein Y is the response signal intensity and X is Ca 2+ And the correlation coefficient of the concentration is 0.9998, the correlation coefficient is close to 1, and the explanation error is small, which shows that the working curve has a good linear fitting relation in the range of 0.2-2.5 mg/L. At the later stage, the response signal intensity is brought in through a linear equation, and Ca in the liquid to be detected can be directly obtained 2+ And (4) concentration.
Relative Standard Deviation (SD)
The Relative Standard Deviation (RSD) is also called standard deviation coefficient, variation coefficient, etc. the precision of the result can be analyzed in the inspection and detection work by dividing the standard deviation by the corresponding average value and multiplying by 100%.
Grinding the reconstituted tobacco into tobacco powder samples, drying to constant weight for later use, weighing 0.2036g of the samples with the sample numbers of 1-5 in five times by using an electronic scale, placing the samples into respective corresponding high-pressure reactors, accurately adding 50mL of sodium nitrate aqueous solution, then adding 5mL of ethanol, finally adding 2g of dry ice particles, and rapidly sealing the reactors, wherein the pressure in the high-pressure reactors is 15 Psi. After the reaction is finished, filtering to obtain a sample solution; accurately transferring appropriate amount of sample solution, diluting with water by 100 times, filtering with 0.45 μm water system filter membrane (discarding the first few drops) to obtain solution to be tested, rapidly detecting the solution to be tested on the machine, measuring by ICP-MS, measuring each group of samples for 5 times, averaging, and substituting into standard curve to obtain corresponding Ca 2+ The concentrations and the measurement results are shown in the following table 1.
TABLE 1 method repeatability results
As can be seen from table 1, the relative standard deviation of five measurements is between 3.74%. The accuracy of the standard curve in calculating the concentration is higher.
Method recovery
Grinding the reconstituted tobacco into a tobacco powder sample, drying to constant weight for later use, weighing 0.2036g of the sample by using an electronic scale, placing the sample in a high-pressure reactor, accurately adding 50mL of sodium nitrate aqueous solution, then adding 5mL of ethanol, adding a certain amount of light calcium carbonate into the high-pressure reactor in the extraction process, subsequently calculating the recovery rate of the calcium carbonate, carrying out three tests, adding different amounts of light calcium carbonate each time, measuring 5 times in each group, and taking an average value, wherein the results are shown in Table 2.
TABLE 2 Process recovery results
As can be seen from Table 2, the recovery rate of the method is between 99% and 108%, and the recovery rate is good. The stability and reliability of the standard curve for calculating the concentration is demonstrated.
Example 2
Ca in blank sample 2+ Concentration C 0 The calculation of (2):
s1, grinding the reconstituted tobacco A into tobacco powder, and drying to constant weight for later use;
s2, weighing 0.2036g of the tobacco powder prepared in the step S1, placing the tobacco powder in a high-pressure reactor, adding 50mL of sodium nitrate aqueous solution, adding 5mL of ethanol, extracting for 60min, rapidly sealing the reactor, and filtering to obtain a blank sample solution after the reaction is finished;
s3, diluting the blank sample solution obtained in the step S2 by 100 times with water, and filtering the diluted solution through a 0.45-micron water system filter membrane to obtain a blank solution to be detected;
s4, measuring Ca of the blank solution to be measured obtained in the step S3 by adopting ICP-MS 2+ Then, the absorbance of the solution is substituted into a standard working curve to obtainCa in the effluent to be tested 2+ Concentration C of 0 ；
The reconstituted tobacco A in the example 2 is divided into 6 parts for calcium carbonate content test, and the specific test process is as shown in the examples 3 to 8.
Example 3
S1, grinding the reconstituted tobacco A into tobacco powder, and drying to constant weight for later use;
s2, weighing 0.1g of the tobacco powder prepared in the step S1, placing the tobacco powder in a high-pressure reactor, adding 50mL of sodium nitrate aqueous solution, adding 5mL of ethanol, adding 2g of dry ice particles, extracting for 20min, quickly sealing the reactor, controlling the pressure in the high-pressure reactor to be 15Psi, and filtering to obtain a sample solution after the reaction is finished;
s3, diluting the sample solution obtained in the step S2 by 100 times with water, and filtering the sample solution through a 0.45-micron water system filter membrane to obtain a solution to be detected;
s4, measuring Ca of the solution to be measured obtained in the step S3 by adopting ICP-MS 2+ Then the absorbance is brought into a standard working curve to obtain Ca in the solution to be detected 2+ Concentration C of 1 ；
S5, calculating the content of calcium carbonate in the reconstituted tobacco:
example 4
S1, grinding the reconstituted tobacco A into tobacco powder, and drying to constant weight for later use;
s2, weighing 0.12 g of the tobacco powder prepared in the step S1, placing the tobacco powder in a high-pressure reactor, adding 60mL of sodium nitrate aqueous solution, adding 5mL of ethanol, adding 2g of dry ice particles, extracting for 30min, quickly sealing the reactor, controlling the pressure in the high-pressure reactor to be 15Psi, and filtering to obtain a sample solution after the reaction is finished;
s3, diluting the sample solution obtained in the step S2 by 100 times with water, and filtering the sample solution through a 0.45-micron water system filter membrane to obtain a solution to be detected;
s4, measuring Ca of the solution to be measured obtained in the step S3 by adopting ICP-MS 2+ Then the absorbance is brought into a standard working curve to obtain Ca in the solution to be detected 2+ Concentration C of 2 ；
S5, calculating the content of calcium carbonate in the reconstituted tobacco:
example 5
S1, grinding the reconstituted tobacco A into tobacco powder, and drying to constant weight for later use;
s2, weighing 0.14 g of the tobacco powder prepared in the step S1, placing the tobacco powder in a high-pressure reactor, adding 70mL of sodium nitrate aqueous solution, adding 5mL of ethanol, adding 2g of dry ice particles, extracting for 40min, quickly sealing the reactor, controlling the pressure in the high-pressure reactor to be 15Psi, and filtering to obtain a sample solution after the reaction is finished;
s3, diluting the sample solution obtained in the step S2 by 100 times with water, and filtering the sample solution through a 0.45-micron water system filter membrane to obtain a solution to be detected;
s4, measuring Ca of the solution to be measured obtained in the step S3 by adopting ICP-MS 2+ Then the absorbance is brought into a standard working curve to obtain Ca in the solution to be detected 2+ Concentration C of 3 ；
S5, calculating the content of calcium carbonate in the reconstituted tobacco:
example 6
S1, grinding the reconstituted tobacco A into tobacco powder, and drying to constant weight for later use;
s2, weighing 0.16 g of the tobacco powder prepared in the step S1, placing the tobacco powder in a high-pressure reactor, adding 80mL of sodium nitrate aqueous solution, adding 5mL of ethanol, adding 5g of dry ice particles, extracting for 50min, quickly sealing the reactor, controlling the pressure in the high-pressure reactor to be 30Psi, and filtering to obtain a sample solution after the reaction is finished;
s3, diluting the sample solution obtained in the step S2 by 100 times with water, and filtering the sample solution through a 0.45-micron water system filter membrane to obtain a solution to be detected;
s4, measuring Ca of the solution to be measured obtained in the step S3 by adopting ICP-MS 2+ Then the absorbance is brought into a standard working curve to obtain Ca in the solution to be detected 2+ Concentration C of 4 ；
S5, calculating the content of calcium carbonate in the reconstituted tobacco:
example 7
S1, grinding the reconstituted tobacco A into tobacco powder, and drying to constant weight for later use;
s2, weighing 0.18 g of the tobacco powder prepared in the step S1, placing the tobacco powder in a high-pressure reactor, adding 90mL of sodium nitrate aqueous solution, adding 5mL of ethanol, adding 5g of dry ice particles, extracting for 60min, quickly sealing the reactor, controlling the pressure in the high-pressure reactor to be 30Psi, and filtering to obtain a sample solution after the reaction is finished;
s3, diluting the sample solution obtained in the step S2 by 100 times with water, and filtering the sample solution through a 0.45-micron water system filter membrane to obtain a solution to be detected;
s4, measuring Ca of the solution to be measured obtained in the step S3 by adopting ICP-MS 2+ Then the absorbance is brought into a standard working curve to obtain Ca in the solution to be detected 2+ Concentration C of 5 ；
S5, calculating the content of calcium carbonate in the reconstituted tobacco:
example 8
S1, grinding the reconstituted tobacco A into tobacco powder, and drying to constant weight for later use;
s2, weighing 0.20g of the tobacco powder prepared in the step S1, placing the tobacco powder in a high-pressure reactor, adding 100mL of sodium nitrate aqueous solution, adding 5mL of ethanol, adding 5g of dry ice particles, extracting for 60min, quickly sealing the reactor, controlling the pressure in the high-pressure reactor to be 30Psi, and filtering to obtain a sample solution after the reaction is finished;
s3, diluting the sample solution obtained in the step S2 by 100 times with water, and filtering the sample solution through a 0.45-micron water system filter membrane to obtain a solution to be detected;
s4, measuring Ca of the solution to be measured obtained in the step S3 by adopting ICP-MS 2+ Then the absorbance is brought into a standard working curve to obtain Ca in the solution to be detected 2+ Concentration C of 6 ；
S5, calculating the content of calcium carbonate in the reconstituted tobacco:
the results of testing the calcium carbonate content of examples 3-8 are shown in table 3 below.
TABLE 3-determination of calcium carbonate in reconstituted tobacco of examples 3-8
As can be seen from Table 3, the errors in the calcium carbonate contents determined in examples 3 to 8 are small, further illustrating the reliability and accuracy of the method.
The above-described aspects may be implemented individually or in various combinations, and such variations are within the scope of the present invention.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the specific embodiments of the invention be limited to these descriptions. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (4)
1. A method for measuring calcium carbonate in reconstituted tobacco by using a high-pressure closed reaction system is characterized by comprising the following steps:
s1, beating the reconstituted tobacco into tobacco powder, mixing uniformly, and drying to constant weight for later use;
s2, weighing the tobacco powder prepared in the step S1, placing the tobacco powder into a high-pressure reactor, adding a sodium nitrate water solution and ethanol as extraction liquid for extraction, then adding dry ice particles, sealing the reactor, and filtering to obtain a sample solution after the reaction is finished;
s3, diluting the sample solution obtained in the step S2 with water, and filtering the diluted sample solution with a water system filter membrane to obtain a solution to be detected;
s4, measuring Ca of the solution to be measured obtained in the step S3 by adopting ICP-MS 2+ The Ca of the response signal is calculated according to the standard working curve 2+ The concentration of (3) C; measuring Ca of the blank solution by ICP-MS 2+ The Ca of the response signal is calculated according to the standard working curve 2+ Concentration C of 0 ；
The preparation of the blank solution to be tested comprises the following steps: weighing the tobacco powder prepared in the step S1, placing the tobacco powder in a high-pressure reactor, adding a sodium nitrate aqueous solution, adding ethanol for extraction, sealing the reactor, filtering to obtain a blank sample solution after the reaction is finished, diluting the blank sample solution with water, and then passing through a water system filter membrane to obtain a blank liquid to be tested, wherein the mass ratio of the tobacco powder, the sodium nitrate aqueous solution and the ethanol is the same as that of the tobacco powder, the sodium nitrate aqueous solution and the ethanol in the step S2;
the manufacturing method of the standard working curve comprises the following steps: preparing Ca with different concentrations 2+ Standard solution, measuring Ca with different concentrations by ICP-MS 2+ Signal intensity of (2), then with Ca 2+ Intensity of signal of (2) to Ca in standard solution 2+ Linear regression is carried out on the corresponding concentration, and the instrument automatically establishes a standard working curve for calculating Ca in the measured liquid according to the standard working curve 2+ The concentration of (c);
s5, calculating the content of calcium carbonate in the reconstituted tobacco:
in the above formula:
x represents the content of calcium carbonate in the reconstituted tobacco, and the unit is microgram per gram (mu g/g);
c-concentration of target in micrograms per milliliter (. mu.g/mL) from the standard working curve;
C 0 -target concentration in micrograms per milliliter (μ g/mL) in a blank sample from a standard working curve;
v-volume of extract in milliliters (mL);
f is dilution multiple;
m-sample mass in grams (g);
100——CaCO 3 the formula (2);
40——Ca 2+ the formula (2);
the mass ratio of the tobacco powder, the sodium nitrate aqueous solution, the ethanol and the dry ice in the step S2 is (0.1-0.2): (50-100): 3.945: (2-5);
after the dry ice particles are added in the step S2, the pressure in the high-pressure reactor is 15-30 Psi.
2. The method for determining calcium carbonate in reconstituted tobacco according to claim 1, wherein the sample solution in the step S3 is diluted by 90-110 times with water.
3. The method for determining calcium carbonate in reconstituted tobacco according to claim 1, wherein the water-based filter membrane in the step S3 is a 0.45 μm water-based filter membrane.
4. The method for determining calcium carbonate in reconstituted tobacco according to claim 1, wherein the extraction time of the sodium nitrate aqueous solution and the ethanol in the step S2 is 20-60 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110558412.7A CN113203818B (en) | 2021-05-21 | 2021-05-21 | Method for measuring calcium carbonate in reconstituted tobacco by high-pressure closed reaction system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110558412.7A CN113203818B (en) | 2021-05-21 | 2021-05-21 | Method for measuring calcium carbonate in reconstituted tobacco by high-pressure closed reaction system |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113203818A CN113203818A (en) | 2021-08-03 |
| CN113203818B true CN113203818B (en) | 2022-08-26 |
Family
ID=77022899
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110558412.7A Active CN113203818B (en) | 2021-05-21 | 2021-05-21 | Method for measuring calcium carbonate in reconstituted tobacco by high-pressure closed reaction system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113203818B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2565165A1 (en) * | 2011-08-31 | 2013-03-06 | Omya Development AG | Remineralization of desalinated and of fresh water by dosing of a calcium carbonate solution in soft water |
| CN103134849A (en) * | 2013-01-30 | 2013-06-05 | 福建中烟工业有限责任公司 | Quick method for simultaneously measuring potassium content and sodium content and calcium content and magnesium content in cigarette paper |
| CN103616447A (en) * | 2013-11-25 | 2014-03-05 | 福建农林大学 | Method for quickly measuring content of calcium carbonate in paper through headspace gas chromatography |
| CN112525979A (en) * | 2020-11-20 | 2021-03-19 | 云南省烟草质量监督检测站 | ICP-MS method for determining content of calcium carbonate in paper-making reconstituted tobacco |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103837530B (en) * | 2014-03-17 | 2016-04-06 | 四川大学 | On-line analysis and sample processing device thereof while water sample nitrite and nitrate |
-
2021
- 2021-05-21 CN CN202110558412.7A patent/CN113203818B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2565165A1 (en) * | 2011-08-31 | 2013-03-06 | Omya Development AG | Remineralization of desalinated and of fresh water by dosing of a calcium carbonate solution in soft water |
| CN103134849A (en) * | 2013-01-30 | 2013-06-05 | 福建中烟工业有限责任公司 | Quick method for simultaneously measuring potassium content and sodium content and calcium content and magnesium content in cigarette paper |
| CN103616447A (en) * | 2013-11-25 | 2014-03-05 | 福建农林大学 | Method for quickly measuring content of calcium carbonate in paper through headspace gas chromatography |
| CN112525979A (en) * | 2020-11-20 | 2021-03-19 | 云南省烟草质量监督检测站 | ICP-MS method for determining content of calcium carbonate in paper-making reconstituted tobacco |
Non-Patent Citations (5)
| Title |
|---|
| ICP-MS法同时测试卷烟纸中锌、硒、锂、镁;蒋衍钜等;《黑龙江造纸》;20160315(第01期);全文 * |
| 应用高压美拉德反应改性烟梗提取液;尤晓娟等;《食品工业》;20181020(第10期);全文 * |
| 碳酸钙加入量对造纸法再造烟叶的影响;王相凡;《安徽农学通报(下半月刊)》;20121225(第24期);全文 * |
| 银负载氧化钛包覆碳酸钙的复合纳米催化剂的制备及性能研究;王驰等;《化工新型材料》;20180615(第06期);全文 * |
| 预处理方法对再造烟叶中烟梗品质的影响;赵春雷等;《食品与机械》;20170528(第05期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113203818A (en) | 2021-08-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| de Kanel et al. | The chemistry of orthophosphate uptake from seawater on to calcite and aragonite | |
| Fisher et al. | Colorimetric determination of cyanide in stack gas and waste water | |
| Taylor et al. | The determination of anionic detergents with iron (II) chelates: application to sewage and sewage effluents | |
| Kagaya et al. | Flame atomic absorption spectrometric determination of lead in waste water and effluent after preconcentration using a rapid coprecipitation technique with gallium phosphate | |
| Gao et al. | Determination of antimony in waste water with chromazurol S by beta-correction spectrophotometry | |
| CN113203818B (en) | Method for measuring calcium carbonate in reconstituted tobacco by high-pressure closed reaction system | |
| Bartlett et al. | Simple kinetic fractionation of reactive aluminum in soil “solutions” | |
| CN113030071A (en) | Method for determining cyanide easily released in thiocyanate-containing water | |
| Suarez et al. | Reevaluation of calcite supersaturation in soils | |
| CN108802234B (en) | Method for measuring content of ammonium ions in fly ash | |
| Chen et al. | Organic solvent-soluble membrane filters for the preconcentration and spectrophotometric determination of iron (II) traces in water with Ferrozine | |
| CN113203614B (en) | Method for determining calcium carbonate in reconstituted tobacco by applying enzymatic reaction | |
| Tokahoglu et al. | Determination of trace metals in waters by FAAS after enrichment as metal-HMDTC complexes using solid phase extraction | |
| Martin et al. | Dicyanatodipyridine copper (II) complex for colorimetric determination of cyanate | |
| CN113203826B (en) | CO (carbon monoxide) 2 Method for measuring calcium carbonate in reconstituted tobacco by continuous flow system | |
| Amrhein et al. | Calcite supersaturation in soil suspensions | |
| Saracoglu et al. | The enrichment/separation of Fe, Co, Pb, Cd, and Cr on Ambersorb 563 prior to their flame atomic absorption spectrometric determinations | |
| Pal et al. | Determination of cyanide based upon its reaction with colloidal silver in the presence of oxygen | |
| Hibbard | Micromethods for determination of zinc | |
| Ensafi et al. | Determination of thiocyanate at the nanogram level by a kinetic method | |
| Guo et al. | A simple new method for the determination of ammonium isotopes by gas chromatography-mass spectrometry | |
| Jenkins | Analysis of estuarine waters | |
| Fernandez-de Cordova et al. | Determination of Trace Amounts of Cobalt at sub-μg 1− 1Level by Solid Phase Spectrophotometry | |
| CN111707776A (en) | Accurate detection method for citrate content in cigarette paper | |
| Parmar et al. | An improved colorimetric determination of micro amounts of chromium (VI) and chromium (III) using p-aminoacetophenone and phloroglucinol in different samples |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |