CN103558115A - Method for measuring content of free water in tobacco and tobacco product - Google Patents
Method for measuring content of free water in tobacco and tobacco product Download PDFInfo
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- CN103558115A CN103558115A CN201310535351.8A CN201310535351A CN103558115A CN 103558115 A CN103558115 A CN 103558115A CN 201310535351 A CN201310535351 A CN 201310535351A CN 103558115 A CN103558115 A CN 103558115A
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Abstract
The invention discloses a method for measuring the content of free water in a tobacco and a tobacco product. According to the method, a constant-temperature drying environment with absolute humidity of zero is established by applying an SPSx water analyzer so that the free water in the tobacco is continuously exchanged until the weight of the tobacco is constant, and the weight loss of the tobacco shows the content of the free water in the tobacco. According to the method, the volatilization process of the free water can be considered, the free water extraction efficiency is increased, experiment errors are reduced, and the accuracy and the reliability of detection results are improved.
Description
Technical field
The present invention relates to technical field of tobacco, particularly a kind of method of measuring tobacco and tobacco product free water content.
Background technology
The water percentage of tobacco and tobacco product is one of important physical and chemical index of tobacco, and the water percentage of tobacco directly affects mechanical property, combustion rate, smoke chemistry composition and the organoleptic quality thereof of tobacco leaf.Moisture in tobacco exists with two kinds of forms of Free water and fetter waetr.Free water claims again bulk water, and retained water is not adsorbed by colloidal solid in vegetable cell or large molecule, can move freely, and play solvent action.Free water is from irreducible water because existence is different, and its characteristic is also different, and therefore in cell, role is different.Both ratios are different, can have influence on plasmic physical property, and then affect the intensity of metabolism.The ratio that free water accounts for total moisture content is larger, makes plasmic viscosity less, and is collosol state, and metabolism is also more vigorous.Biological metabolism is vigorous, in conjunction with water, can be converted into free water, makes to reduce in conjunction with the ratio of water and free water.Slow when biological metabolism, free water can be exchanged in conjunction with water, makes to rise in conjunction with water and free water ratio.Free water is more, and metabolism is more vigorous.Stronger in conjunction with the many drought resistances of water.
In tobacco cell, the water of the overwhelming majority exists and can flow freely with the free water form of dissociating, and is therefore necessary to measure the free water content in tobacco.Yet the assay method of at present relevant content of free water in tobaccos is also fewer, is mainly that some are about the assay method of total moisture content.The assay method of total moisture content mainly contains direct method and indirect method, and direct method comprises: heated drying method, the way of distillation, karl Fischer method, microwave method, vapor-phase chromatography and boulton process, indirect method comprises differential calorimetry and near infrared determination method etc.Heated drying method mainly refers to oven method, under more than 100 ℃ high temperature, dries pipe tobacco, represents the content of moisture in pipe tobacco with the variation of tobacco quality.The way of distillation heats by water-fast organic solvent and sample are put into distillation type moisture content determining device, and the condensation in condenser pipe of the moisture in sample is obtained the moisture of sample by the capacity of moisture.Karl Fischer method utilizes water and karl Fischer reagent to produce the content of moisture in redox reaction working sample.Microwave method measure moisture be utilize microwave in transmission during the material by containing moisture part electromagnetic energy just by hydrone, absorbed microwave intensity decayed to some extent.
Boulton process utilizes lower temperature, is under reduced pressure dried and removes moisture, and the amount of moisture of minimizing is the water cut of sample.Moisture in gas chromatography applications organic solvent extracting sample thief is through packed column separation and quantitative.Differential calorimetry is working sample and the energy difference of reference substance and a kind of technology of temperature relation under program temperature is controlled, thereby while containing moisture in sample, there will be the content of endothermic peak analysis moisture.It is by setting up the moisture in the model analysis sample of moisture under near infrared that Near-Infrared Absorption Method is measured moisture.In said method, vapor-phase chromatography, microwave method, NIR method, differential calorimetry and karl Fischer method utilize the physics and chemistry character of water to carry out quantitatively.Other several assay methods, first carry out moisture and testing sample separatedly, then by weighing the quality of moisture or butt matter, obtain the content of moisture.
About the assay method of content of free water in tobaccos mainly contains Abbe refractometer method, weight method and vapor-phase chromatography at present.Abbe refractometer method is the method for free water content in a kind of general mensuration vegetable cell, this method is soaked in tobacco leaf in the sugar juice of high concentration and displaces the free water in tobacco leaf, and application Abbe refractometer is measured the content of sugar juice change detection free water of concentration before and after soaking.Weight method is soaked in tobacco leaf equally in the sugar juice of high concentration and displaces the free water in tobacco leaf, then directly weighs the quality of blade before and after soaking, and represents the content of free water with the difference of quality.Vapor-phase chromatography is by selecting moisture in applicable organic solvent extracting sample thief through packed column separation and quantitative.Although these methods are relatively conventional, also there are some problems, such as mensuration process is relatively complicated, repeatability influence factor slightly poor, free water extraction efficiency is more, experimental error is larger etc.
Application number is that 201110048801.1 patent discloses a kind of method of measuring content of free water in tobaccos, it adopts the simple and quick mensuration of carrying out tobacco sample free water content of method of gas chromatographic analysis, the fully wetting tobacco sample of its choice for use by extractant, the freely free water of activity in tobacco sample is dissolved in extractant, has got rid of the impact of volatile ingredient in tobacco.Application number is that 201010235301.4 patent discloses a kind of method and specific constant temperature and humidity analyzer thereof of measuring cigarette humid keeping performance, this invention is that sample and meausring apparatus are built in constant temperature and humidity casing, by the inner cased type operation gloves operation sample of sealing and the instrument of weighing, obtain the water retention of testing sample under different time sections different condition, and then the humid keeping performance of judgement cigarette.Yet the method is used the inner cased type operation gloves of sealing, inconvenient operation.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method that the SPSx of application water analysis instrument is measured tobacco and tobacco product free water content.
The method is zero freeze-day with constant temperature environment by setting up an absolute humidity, free water in tobacco leaf is constantly swapped out until quality of tobacco is invariable, difference with quality of tobacco represents that tobacco leaf freely contains liquid water content, this method not only can be investigated the volatilization process of free water, and improved free water extraction efficiency, reduce experimental error, improved accuracy and the reliability of testing result.
The present invention adopts following technical proposals:
A method of measuring tobacco and tobacco product free water content, determination step is as follows:
1) regulating SPSx water analysis instrument humidity is 0%, and it is constant that temperature keeps;
2) put into the weighing plate of dress sample, separately put into an identical weighing plate as blank reference dish, then weigh tare weight;
3) take sample and be placed in weighing plate, weigh initial sample quality;
4) at interval of certain hour automatic weighing sample quality, treat the constant balance that reaches of constant mass, finish to measure;
5) changing value of calculated mass, obtains the content of free water in sample.
Further, the temperature range described in step 1) is at 5-60 ℃.
Further, step 2), institute's sample thief quality is 0.10-1.50g.
Further, the time interval scope described in step 4) is 1-10min; The minimum single cycle time used is 120min; The maximum single cycle time used is 100 hours.
SPSx water analysis instrument comprises adjustable climatic chamber, porous specimen holder, weighing plate and sample chamber; Porous specimen holder is located in constant temperature and humidity box body; Weighing plate is placed on porous specimen holder; Sample chamber is provided with temperature controller and humidity controller; Constant temperature and humidity box body cavity of resorption is provided with built-in high accuracy analysis balance, temperature sensor and automatic sampler; High accuracy analysis balance, temperature sensor and automatic sampler are connected with computer and realize monitoring in real time.
Beneficial effect of the present invention:
The present invention can realize the on-line real time monitoring of sample free water content, reflects the change procedure of free water.The method can be used for the mensuration of tobacco and tobacco product free water content, simple to operate, accurately convenient.
Accompanying drawing explanation
Fig. 1 is the SPSx water analysis instrument operation schematic diagram using for the present invention.Wherein, 1 climatic chamber, 2 porous specimen holders, 3 weighing plates, 4 sample chambers, 5 temperature controllers, 6 humidity controllers, 7 high accuracy analysis balances, 8 temperature sensors, 9 automatic samplers and 10 computers.
Embodiment
Use instrument: SPSx water analysis instrument comprises adjustable climatic chamber 1, porous specimen holder 2, weighing plate 3 and sample chamber 4; Porous specimen holder 2 is located in climatic chamber 1 casing; Weighing plate 3 is placed on porous specimen holder 2; Sample chamber is provided with temperature controller 5 and humidity controller 6; Climatic chamber 1 casing cavity of resorption is provided with built-in high accuracy analysis balance 7, temperature sensor 8 and automatic sampler 9; High accuracy analysis balance 7, temperature sensor 8 and automatic sampler 9 are connected with computer 10 and realize monitoring in real time.
Get 0.40 gram of C
3f tobacco sample, is placed in the SPSx water analysis instrument aluminium matter weighing plate of having surveyed tare weight, and when instrument temperature is set to 20 ℃, relative humidity is 0%, at interval of 5 minutes mensuration one inferior qualities, treats that its mass change is less than 0.01% in 2 hours, finishes to measure.Initial mass per sample and final mass, the free water content that calculates sample is 8.026%.
In formula: W free water water percentage, %
G adds weighing plate quality (g) after sample;
G
0weighing plate quality (g);
G
nfinal sample and weighing plate quality (g);
For verifying the precision of this new method, replicate determination 5 times, result is as table 1, and in his-and-hers watches 1, data are carried out precision analysis and are obtained table 2, and result shows that the precision of the inventive method is better.
Table 15 time replicate determination result
N(number) | 1 | 2 | 3 | 4 | 5 |
Free water content (%) | 8.026 | 8.031 | 8.013 | 8.021 | 8.018 |
Table 25 time replicate determination precision analysis result
Mean value (%) | 8.022 |
Standard deviation (%) | 0.007 |
Coefficient of variation C.V.% | 0.087 |
Variance | 0.0000487 |
Get 0.50 gram of C
3f tobacco sample, is placed in the SPSx water analysis instrument aluminium matter weighing plate of having surveyed tare weight, and when instrument temperature is set to 20 ℃, relative humidity is 0%, at interval of 3 minutes mensuration one inferior qualities, treats that its mass change is less than 0.01% in 2 hours, finishes to measure.Initial mass per sample and final mass, the free water content that can calculate sample is 8.017%.
Get 1.00 grams of C
3f tobacco sample, is placed in the SPSx water analysis instrument weighing plate of having surveyed tare weight, and when instrument temperature is set to 20 ℃, relative humidity is 0%, at interval of 10 minutes mensuration one inferior qualities, treats that its mass change is less than 0.01% in 4 hours, finishes to measure.Initial mass per sample and final mass, the free water content that can calculate sample is 8.020%.
Get 0.80 gram of B
3f tobacco sample, is placed in the SPSx water analysis instrument aluminium matter weighing plate of having surveyed tare weight, and when instrument temperature is set to 10 ℃, relative humidity is 0%, at interval of 3 minutes mensuration one inferior qualities, treats that its mass change is less than 0.01% in 3 hours, finishes to measure.Initial mass per sample and final mass, the free water content that can calculate sample is 8.160%.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here cannot give all embodiments exhaustive.Every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention extends out or change that belong to.
Claims (4)
1. a method of measuring tobacco and tobacco product free water content, is characterized in that, determination step is as follows:
1) regulating SPSx water analysis instrument humidity is 0%, and it is constant that temperature keeps;
2) put into the weighing plate of dress sample, separately put into an identical weighing plate as blank reference dish, then weigh tare weight;
3) take sample and be placed in weighing plate, weigh initial sample quality;
4) at interval of certain hour automatic weighing sample quality, treat the constant balance that reaches of constant mass, finish to measure;
5) changing value of calculated mass, obtains the content of free water in sample.
2. a kind of method of measuring tobacco and tobacco product free water content according to claim 1, is characterized in that: the temperature range described in step 1) is at 5-60 ℃.
3. a kind of method of measuring tobacco and tobacco product free water content according to claim 1, is characterized in that: step 2) in institute sample thief quality be 0.10-1.50g.
4. a kind of method of measuring tobacco and tobacco product free water content according to claim 1, is characterized in that: the time interval scope described in step 4) is 1-10min; The minimum single cycle time used is 120min; The maximum single cycle time used is 100 hours.
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CN104020073A (en) * | 2014-05-30 | 2014-09-03 | 江苏中烟工业有限责任公司 | Method of detecting the total amount of petroleum ether extracts in tobacco and tobacco products |
CN104062203A (en) * | 2014-07-15 | 2014-09-24 | 安徽中烟再造烟叶科技有限责任公司 | Method for measuring content of sand of papermaking process reconstituted tobacco raw material and process product |
WO2015043332A1 (en) * | 2013-09-25 | 2015-04-02 | 上海烟草集团有限责任公司 | Full-automatic dynamic tobacco moisture analysis climate box |
CN104655519A (en) * | 2015-02-12 | 2015-05-27 | 北京市农林科学院 | Method for measuring content of free water |
CN104913999A (en) * | 2015-06-15 | 2015-09-16 | 三峡大学 | Interference-free weighing device applied to specific temperature and humidity environment |
CN105699239A (en) * | 2016-02-23 | 2016-06-22 | 江苏中烟工业有限责任公司 | Method for analyzing moisture retention ability of tobaccos and tobacco products by aid of near-infrared spectral models |
CN106124444A (en) * | 2016-06-14 | 2016-11-16 | 安徽省农业科学院园艺研究所 | A kind of method using near infrared device to measure open country Fructus Fragariae Ananssae sleeping process |
CN108760927A (en) * | 2018-06-08 | 2018-11-06 | 云南中烟工业有限责任公司 | Electrical heating based on stove volatile matter is not burnt cigarette presentation quality analysis method |
CN113966855A (en) * | 2021-11-24 | 2022-01-25 | 河南中烟工业有限责任公司 | Co-heating type tobacco sample preparation device with fixed moisture content and preparation method |
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Cited By (14)
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WO2015043332A1 (en) * | 2013-09-25 | 2015-04-02 | 上海烟草集团有限责任公司 | Full-automatic dynamic tobacco moisture analysis climate box |
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CN104020073A (en) * | 2014-05-30 | 2014-09-03 | 江苏中烟工业有限责任公司 | Method of detecting the total amount of petroleum ether extracts in tobacco and tobacco products |
CN104062203A (en) * | 2014-07-15 | 2014-09-24 | 安徽中烟再造烟叶科技有限责任公司 | Method for measuring content of sand of papermaking process reconstituted tobacco raw material and process product |
CN104655519B (en) * | 2015-02-12 | 2017-08-25 | 北京市农林科学院 | A kind of free water content assay method |
CN104655519A (en) * | 2015-02-12 | 2015-05-27 | 北京市农林科学院 | Method for measuring content of free water |
CN104913999A (en) * | 2015-06-15 | 2015-09-16 | 三峡大学 | Interference-free weighing device applied to specific temperature and humidity environment |
CN105699239A (en) * | 2016-02-23 | 2016-06-22 | 江苏中烟工业有限责任公司 | Method for analyzing moisture retention ability of tobaccos and tobacco products by aid of near-infrared spectral models |
CN106124444A (en) * | 2016-06-14 | 2016-11-16 | 安徽省农业科学院园艺研究所 | A kind of method using near infrared device to measure open country Fructus Fragariae Ananssae sleeping process |
CN106124444B (en) * | 2016-06-14 | 2018-08-28 | 安徽省农业科学院园艺研究所 | A method of open country strawberry sleeping process is measured using near infrared device |
CN108362605B (en) * | 2018-04-28 | 2024-02-02 | 华中科技大学 | Automatic change integrated form air humidity measuring device |
CN108760927A (en) * | 2018-06-08 | 2018-11-06 | 云南中烟工业有限责任公司 | Electrical heating based on stove volatile matter is not burnt cigarette presentation quality analysis method |
CN108760927B (en) * | 2018-06-08 | 2020-10-27 | 云南中烟工业有限责任公司 | Electric heating non-combustible cigarette appearance quality analysis method based on furnace volatile matter |
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