CN113655154B - In-situ extraction instrument and test method suitable for measuring moisture in flue gas - Google Patents
In-situ extraction instrument and test method suitable for measuring moisture in flue gas Download PDFInfo
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- CN113655154B CN113655154B CN202010396537.XA CN202010396537A CN113655154B CN 113655154 B CN113655154 B CN 113655154B CN 202010396537 A CN202010396537 A CN 202010396537A CN 113655154 B CN113655154 B CN 113655154B
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Abstract
An in-situ extraction instrument and a testing method suitable for measuring moisture in flue gas comprise an extraction unit and a bracket (12), wherein the extraction unit is arranged on the bracket (12). The invention adopts the trapping of the condensate of the main stream smoke of the cigarettes, the in-situ extraction treatment of the moisture in the smoke, the gas chromatography is used for measuring the moisture content, the trapping device is used for trapping the particulate matters of the cigarettes in the smoke by adopting a trapping device provided with a Cambridge filter, the trapping device is arranged on a pipeline module of the in-situ extraction system on the premise of not opening the trapping device after the trapping is finished, the isopropanol containing a certain concentration of internal standard (ethanol or methanol) is used as an extractant for extraction, and then the gas chromatography is used for realizing the accurate measurement of the moisture in the smoke condensate.
Description
Technical Field
The invention relates to the field of tobacco detection, in particular to an in-situ extraction instrument and a testing method suitable for measuring moisture in smoke.
Background
The heating cigarette is a novel tobacco product which utilizes a special heat source to heat the core base material (the temperature is lower than 300 ℃ or even lower), and the core base material is only heated but not burnt. The tobacco material (core base material) used for heating the cigarettes has obvious differences from the physical and chemical properties of tobacco leaves and traditional reconstituted tobacco leaves, and particularly, the tobacco material uses a higher proportion of alcohol smoke agents, and the smoke agents have high hygroscopicity, so that the moisture content in the main stream smoke of the heated cigarettes is obviously higher than that of the traditional cigarettes. When the heated non-combustible cigarettes are smoked, condensate is arranged on the front cover and the rear cover of the catcher, and the traditional main stream smoke particle phase object catching and extraction treatment mode is not suitable for catching and extraction treatment of high-moisture-content smoke such as the heated cigarettes, so that the measurement result is influenced.
At present, when the moisture analysis and measurement of main stream smoke are carried out, moisture in cigarette smoke is generally trapped by adopting a Cambridge filter, then the Cambridge filter is subjected to extraction treatment by adopting an extracting agent containing an internal standard and is analyzed and tested by a gas chromatography, but when the analysis of novel tobacco products such as heated cigarettes and electronic cigarettes is carried out, a large amount of condensate is found to be generated on the rear cover of the catcher, so that the problem to be solved is how to completely trap and extract the moisture in the main stream smoke of the novel tobacco products such as the heated cigarettes. The calculation of the tar level of the cigarettes relates to the moisture content in the total particulate matters, and the accurate value of the tar amount in the total particulate matters can be obtained only after the moisture content and the nicotine content in the total particulate matters are accurately measured.
Disclosure of Invention
In order to overcome the existing defects, the invention provides an in-situ extraction instrument suitable for measuring the moisture in the flue gas.
An in-situ extraction instrument suitable for measuring moisture in flue gas comprises an extraction unit and a bracket, wherein the extraction unit is arranged on the bracket.
The extraction unit comprises an upper linear slide rail, an upper linear motor, a cylinder, an upper piston, an upper extraction cavity, a catcher, a pipeline module, a lower extraction cavity, a lower piston, a lower linear motor and a lower linear slide rail, wherein the upper linear motor, the upper piston and the upper extraction cavity are arranged on the cylinder and move along with the cylinder; the upper piston is arranged on a motor shaft of the upper linear motor, and is driven by the motor shaft to reciprocate in the upper extraction cavity, and the upper end of the motor shaft is fixed on the upper linear slide rail and the upper limit upper piston performs linear motion; the pipeline module is arranged on the lower extraction cavity, three pipelines are arranged in the pipeline module, namely a suction pipeline, an extraction pipeline and a release pipeline, a motor shaft of the lower linear motor pushes a lower piston to reciprocate in the lower extraction cavity, the lower end of the motor shaft is fixed on a lower linear slide rail, and the lower piston is limited to do linear motion; the lower extraction cavity is fixed on the bracket, and the catcher is arranged between the pipeline module and the upper extraction cavity.
Installing the balanced Cambridge filter disc in a smoke catcher of an in-situ extractor and connecting the balanced Cambridge filter disc with a smoking machine suction channel;
the catcher is arranged on the pipeline module, the cylinder is lowered after the catcher is arranged, the upper extraction cavity, the catcher, the management module and the lower extraction cavity are connected together to form a pipeline passage, and the pipeline is switched through an electromagnetic valve in the pipeline module to select a suction pipeline;
the upper piston moves upwards to suck the extracting agent into the upper extracting cavity, the upper piston rises to the highest position at the moment, after the completion, the pipeline inside the pipeline module is switched to an extracting pipeline,
the upper extraction cavity and the lower extraction cavity are connected into a passage, and the upper piston and the lower piston reciprocate up and down at the same time to push the extractant to flow back and forth between the upper extraction cavity and the lower extraction cavity in a circulating way so as to enable the extractant to flow back and forth through the catcher in a circulating way.
After the test times, the upper piston and the lower piston are moved to the highest positions, the pipeline module switches the pipeline to a release pipeline, the upper piston moves downwards to release the extraction liquid in the upper extraction cavity, and the rear cylinder is lifted to separate the catcher from the upper extraction cavity and take down the catcher;
and (5) completing extraction.
And the moisture content was determined by gas chromatography.
Detection limit and quantification limit; and (3) carrying out gas chromatographic analysis by adopting a standard working solution sample with the lowest concentration, repeatedly sampling for 10 times, measuring the moisture content, calculating the standard deviation, taking 3 times of the standard deviation as the moisture content detection limit of the method, and taking 10 times of the standard deviation as the moisture content quantitative lower limit of the method.
Recovery rate and repeatability, the average value of five parallel measurement of the heated non-burning cigarette sample is used as the basis for calculating the initial content. Standard substances with high, medium and low concentration levels are respectively added to carry out recovery rate tests.
The invention adopts an in-situ extraction device to trap particulate matters of cigarettes in smoke by adopting a trap with a Cambridge filter disc, the trap is arranged on a pipeline module of an in-situ extraction system on the premise of not opening the trap after the trapping is completed, isopropanol containing a certain concentration of internal standard (ethanol or methanol) is used as an extractant for extraction, and then gas chromatography is adopted to realize accurate determination of moisture in smoke condensate.
Aiming at the problems of trapping and testing the condensate of the smoke with high moisture content of the prior heating cigarette, the invention realizes the purpose of accurately trapping and testing the moisture content of the smoke by the design and the transformation of a sample trapping device and the optimization and the adjustment of the sample pretreatment process.
Drawings
FIG. 1 is a schematic diagram of an in situ extractor suitable for use in the determination of moisture in flue gas.
Figure 2 is a graph of puff flow rate of a smoking machine measured using a puff profiler.
FIG. 3 is a gas chromatogram.
Detailed Description
The invention provides an in-situ extraction instrument suitable for measuring moisture in flue gas, which is described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 shows an in situ extractor suitable for the determination of moisture in flue gas, comprising an extraction unit and a holder 12, the extraction unit being mounted on the holder 12.
The extraction unit comprises an upper linear slide rail 1, an upper linear motor 2, a cylinder 3, an upper piston 4, an upper extraction cavity 5, a catcher 6, a pipeline module 7, a lower extraction cavity 8, a lower piston 9, a lower linear motor 10 and a lower linear slide rail 11, wherein the upper linear motor 2, the upper piston 4 and the upper extraction cavity 5 are arranged on the cylinder 3 and move along with the cylinder 3; the upper piston 4 is arranged on a motor shaft of the upper linear motor 2, and is driven by the motor shaft to reciprocate in the upper extraction cavity 5, and the upper end of the motor shaft is fixed on the upper linear slide rail 1 and the upper limit upper piston 4 performs linear motion; the pipeline module 7 is arranged on the lower extraction cavity 8, three pipelines which are respectively a suction pipeline, an extraction pipeline and a release pipeline are arranged in the pipeline module 7, a motor shaft of the lower linear motor 10 pushes the lower piston 9 to reciprocate in the lower extraction cavity 8, the lower end of the motor shaft is fixed on the lower linear slide rail 11, and the lower piston 4 is limited to do linear motion; the lower extraction chamber 8 is fixed on a support 12, and the catcher 6 is mounted between the pipeline module 7 and the upper extraction chamber 5.
The extraction units are multiple and are fixed in parallel.
The aim of the invention is realized by the following technical scheme:
1. capturing condensate of main stream smoke of cigarettes:
and installing the balanced Cambridge filter disc in a self-designed cigarette smoke catcher and connecting the balanced Cambridge filter disc with a smoking machine suction channel. Before aspiration, the aspiration volume and aspiration profile should be checked and modified accordingly without aspiration. The suction capacity of the machine was calibrated to 35mL using a soap film flow meter according to standard suction conditions specified in GB/T19609-2004, i.e. with a 1KPa pressure drop device attached.
Figure 2 is a graph of the puff flow rate of a smoking machine measured using a puff profiler, and it can be seen that under standard conditions the puff flow rate graph is bell-shaped, the puff volume, maximum airflow value, maximum time of occurrence, etc. all meet the requirements of GB/T16450-2004 for puff flow rate graph (see table 1). It is explained that when the trapping device is connected with a smoking machine, the smoking channel of the smoking machine meets the related standard requirements.
And on the premise of ensuring that the requirements of related standards are met, sucking the heated cigarettes and capturing particulate matters, wherein each catcher (44 mm Cambridge filter) captures 5 heated cigarettes.
Table 1 parameters of the suction curve measured by the 1KPa pressure drop device under standard conditions
2. In-situ extraction treatment of moisture in flue gas
The catcher 6 is arranged on the pipeline module 7, the cylinder 3 is lowered after the catcher 6 is arranged, the upper extraction cavity 5, the catcher 6, the management module 7 and the lower extraction cavity 8 are connected together to form a pipeline passage, and the pipeline is switched through an electromagnetic valve in the pipeline module 7 to select a suction pipeline;
the upper piston 4 moves upwards to suck the extracting agent into the upper extracting chamber 5, the upper piston 4 rises to the highest position at the moment, after the completion, the pipeline inside the pipeline module 7 is switched to the extracting pipeline,
the upper extraction cavity 5 and the lower extraction cavity 8 are connected into a passage, the upper piston 4 and the lower piston 8 reciprocate up and down at the same time, and the extractant is pushed to flow between the upper extraction cavity 5 and the lower extraction cavity 8 in a circulating and reciprocating way, so that the extractant flows through the catcher 6 in a circulating and reciprocating way.
After the test times, the upper piston 4 and the lower piston 8 are moved to the highest positions, the pipeline module 7 switches the pipeline to a release pipeline, the upper piston 4 moves downwards to release the extraction liquid in the upper extraction cavity 5, the rear cylinder 3 is lifted after completion, the catcher 6 is separated from the upper extraction cavity 5, and the catcher 6 is taken down;
and (5) completing extraction.
3. The moisture content was measured by gas chromatography and FIG. 3 is a chromatogram.
Chromatographic conditions:
packing chromatographic column recommended operating conditions:
-column box temperature: 170 ℃ (isotherm);
sample inlet temperature: 250 ℃;
detector temperature: 250 ℃;
-carrier gas: helium with a flow rate of 30mL/min;
sample injection volume: 2. Mu.L.
Operating conditions recommended for capillary chromatography columns:
-column box temperature: 170 ℃ (isotherm);
sample inlet temperature: 250 ℃;
detector temperature: 250 ℃;
-carrier gas: helium with a flow rate of 3mL/min;
sample injection volume: 2 mu L, split ratio 5:1, no split state sample volume: 0.5. Mu.L.
4. Detection limit and quantification limit:
the gas chromatographic analysis is carried out by adopting a standard working solution sample with the lowest concentration, the sample injection is repeated for 10 times, the moisture content is measured (the measurement result is shown in Table 2), the standard deviation is calculated, the 3-time standard deviation is taken as the moisture content detection limit of the method, the 10-time standard deviation is taken as the moisture content quantitative lower limit of the method, and the detection limit of the method is 0.0026 mg/count and the quantitative limit is 0.0086 mg/count.
TABLE 2 detection limit and quantitative limit measurement results Table (mg/count)
5. Recovery and repeatability:
for a certain heating non-burning cigarette sample, the average value of five parallel measurement is taken as the basis for calculating the initial content. Standard substances with high, medium and low concentration levels are respectively added to carry out recovery rate tests. As can be seen from the table, the recovery rate is between 96% and 103% in samples with different contents, and the result meets the method requirements.
Table 3 shows recovery and reproducibility of the process of the invention
In one embodiment, the balanced and screened heated cigarettes are smoked by a linear smoking machine according to the standard conditions stipulated by ISO, 5 heated cigarettes are smoked in each experiment, a catcher with a Cambridge filter disc is adopted to catch the particulate matters of the cigarettes, the catcher is arranged on a pipeline module of an in-situ extraction system on the premise that the catcher is not opened after the catching is finished, isopropanol (20 mL) with a certain concentration of internal standard (3 mg/mL ethanol) is used as an extractant for extraction, and then the moisture content of the flue gas condensate is measured by adopting a gas chromatography.
TABLE 4 comparison of the invention with the results of the current standard method test (ISO suction mode)
In another embodiment, the balanced and screened heated cigarettes are smoked by a linear type smoking machine according to standard conditions specified by a depth smoking mode, 3 cigarettes are smoked in each experiment, a catcher with a Cambridge filter disc is adopted to catch the particulate matters of the cigarettes, the catcher is arranged on a pipeline module of an in-situ extraction system on the premise that the catcher is not opened after the catching is finished, isopropanol (20 mL) with a certain concentration of internal standard (3 mg/mL ethanol) is used as an extractant for extraction, and then the moisture content of the smoke condensate is measured by adopting a gas chromatography.
TABLE 5 comparison of the invention with the results of the current standard method test (deep pumping mode)
As can be seen from the data in tables 4 and 5, the method provided by the invention can obtain the effect consistent with the current standard by testing the moisture of the traditional cigarette smoke, and has good accuracy. In addition, when the technology is adopted to test the moisture content of the smoke of the heating cigarettes, the test result is improved by about 20 percent compared with the current standard, and the problems that the current technology cannot completely capture and effectively extract the moisture in the main stream smoke of the novel tobacco products such as the heating cigarettes and the electronic cigarettes due to the fact that a large amount of condensate is formed on the rear cover of the catcher during the analysis of the novel tobacco products such as the heating cigarettes and the electronic cigarettes are effectively solved.
Finally, it should be noted that the above embodiments are only intended to describe the technical solution of the present invention and not to limit the technical method, the present invention extends to other modifications, variations, applications and embodiments in application, and therefore all such modifications, variations, applications, embodiments are considered to be within the spirit and scope of the teachings of the present invention.
Claims (3)
1. An in-situ extraction instrument suitable for measuring moisture in flue gas comprises an extraction unit and a bracket (12), and is characterized in that the extraction unit is arranged on the bracket (12),
the extraction unit comprises an upper linear slide rail (1), an upper linear motor (2), a cylinder (3), an upper piston (4), an upper extraction cavity (5), a catcher (6), a pipeline module (7), a lower extraction cavity (8), a lower piston (9), a lower linear motor (10) and a lower linear slide rail (11), wherein the upper linear motor (2), the upper piston (4) and the upper extraction cavity (5) are arranged on the cylinder (3) and move along with the cylinder (3); the upper piston (4) is arranged on a motor shaft of the upper linear motor (2), and is driven by the motor shaft to reciprocate in the upper extraction cavity (5), and the upper end of the motor shaft is fixed on the upper linear slide rail (1) and is used for limiting the upper piston (4) to do linear motion; the pipeline module (7) is arranged on the lower extraction cavity (8), three pipelines which are respectively a suction pipeline, an extraction pipeline and a release pipeline are arranged in the pipeline module (7), a motor shaft of the lower linear motor (10) pushes the lower piston (9) to reciprocate in the lower extraction cavity (8), the lower end of the motor shaft is fixed on the lower linear slide rail (11), and the lower piston (9) is limited to do linear motion; the lower extraction cavity (8) is fixed on the support (12), the catcher (6) is arranged between the pipeline module (7) and the upper extraction cavity (5), and the upper extraction cavity (5) and the lower extraction cavity (8) are connected into a passage.
2. The in situ extractor suitable for measuring moisture in flue gas according to claim 1, wherein the plurality of extraction units are arranged in a plurality of groups and are fixed side by side.
3. The method for testing an in-situ extractor suitable for measuring moisture in flue gas according to any of the claims 1-2, wherein,
1) Capturing condensate of main stream smoke of cigarettes:
installing the balanced Cambridge filter disc in a catcher (6) of the in-situ extraction instrument and connecting the balanced Cambridge filter disc with a smoking machine suction channel;
2) In-situ extraction treatment of moisture in flue gas:
the catcher (6) is arranged on the pipeline module (7), the cylinder (3) is lowered after the catcher is arranged, the upper extraction cavity (5), the catcher (6), the pipeline module (7) and the lower extraction cavity (8) are connected together to form a pipeline passage, and the pipeline is switched through an electromagnetic valve in the pipeline module (7) to select a suction pipeline;
the upper piston (4) moves upwards to suck the extracting agent into the upper extracting cavity (5), the upper piston (4) rises to the highest position at the moment, after the completion, the pipeline inside the pipeline module (7) is switched to an extracting pipeline,
the upper extraction cavity (5) and the lower extraction cavity (8) are connected into a passage, the upper piston (4) and the lower piston (9) reciprocate up and down at the same time, and the extractant is pushed to flow back and forth between the upper extraction cavity (5) and the lower extraction cavity (8) in a circulating way, so that the extractant flows back and forth through the catcher (6);
after the test times are up, the upper piston (4) and the lower piston (9) are moved to the highest positions, the pipeline module (7) switches the pipeline to a release pipeline, the upper piston (4) moves downwards to release the extraction liquid in the upper extraction cavity (5), the rear cylinder (3) is lifted after completion, the catcher (6) is separated from the upper extraction cavity (5), and the catcher (6) is taken down;
completing extraction;
3) Measuring the moisture content by gas chromatography;
4) Detection limit and quantification limit:
carrying out gas chromatographic analysis by adopting a standard working solution sample with the lowest concentration, repeatedly sampling for 10 times, measuring the moisture content, calculating the standard deviation of the sample, taking 3 times of the standard deviation as the moisture content detection limit of the method, and taking 10 times of the standard deviation as the moisture content quantitative lower limit of the method;
5) Recovery and repeatability:
taking the average value of five parallel measurement of the heated non-combustible cigarette sample as the basis for calculating the initial content; standard substances with high, medium and low concentration levels are respectively added to carry out recovery rate tests.
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| CN104634914A (en) * | 2015-02-16 | 2015-05-20 | 国家烟草质量监督检验中心 | Method for determining content of 1,2-propanediol, propanetriol and triethylene glycol in suction aerosol of electronic cigarette |
| EP2893855A1 (en) * | 2014-01-14 | 2015-07-15 | bendis SWISS GmbH | Extractor |
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| CN110895231A (en) * | 2019-12-26 | 2020-03-20 | 贵州中烟工业有限责任公司 | Method for measuring moisture in aerosol of heated non-combustible cigarette |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5242787B2 (en) * | 2009-06-25 | 2013-07-24 | 株式会社日立ハイテクノロジーズ | Pretreatment device and mass spectrometer equipped with the same |
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- 2020-05-12 CN CN202010396537.XA patent/CN113655154B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2893855A1 (en) * | 2014-01-14 | 2015-07-15 | bendis SWISS GmbH | Extractor |
| CN104634914A (en) * | 2015-02-16 | 2015-05-20 | 国家烟草质量监督检验中心 | Method for determining content of 1,2-propanediol, propanetriol and triethylene glycol in suction aerosol of electronic cigarette |
| CN108051524A (en) * | 2018-01-05 | 2018-05-18 | 国家烟草质量监督检验中心 | A kind of cigarette, the assay method for heating Related Component in do not burn cigarette, electronic cigarette main flume |
| CN110895231A (en) * | 2019-12-26 | 2020-03-20 | 贵州中烟工业有限责任公司 | Method for measuring moisture in aerosol of heated non-combustible cigarette |
Non-Patent Citations (1)
| Title |
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| 卷烟烟气在模拟口腔环境中pH值的测定;李怀奇 等;《食品与机械》;20190228;第35卷(第4期);第60-63+162页 * |
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