阅读说明：本技术 一种滤片自动涂液装置测定卷烟主流烟气中氨含量的方法 (Method for measuring ammonia content in main stream smoke of cigarette by automatic filter disc liquid coating device ) 是由 李翔宇 常诚 罗彦波 林玉红 张洪非 朱风鹏 姜兴益 庞永强 慎龙舞 吕晓亮 胡 于 2020-05-12 设计创作，主要内容包括：本发明提供一种滤片自动涂液装置测定卷烟主流烟气中氨含量的方法,自动涂液装置包括机体(15),其特征在于,所述机体(15)中,旋转定位盘(9)安装在大齿轮(11)上,小齿轮(10)安装在定位盘旋转电机(12)上,大齿轮(11)和小齿轮(10)相互齿合,通过定位盘旋转电机(12)的转动带动旋转定位盘(9)旋转定位。通过本发明的一种滤片自动涂液装置,其方法具有很好的准确性。此外,在采用该技术测试卷烟烟气氨含量时,其测试结果相对现行标准有些许提高,数据平行性更好,实验时间能够减少10到15分钟。有效解决了手动涂液造成现行技术无法对卷烟主流烟气中氨进行完全捕集和有效萃取的问题。(The invention provides a method for measuring the ammonia content in mainstream smoke of a cigarette by using a filter disc automatic liquid coating device, which comprises a machine body (15), and is characterized in that in the machine body (15), a rotary positioning disc (9) is arranged on a large gear (11), a small gear (10) is arranged on a positioning disc rotary motor (12), the large gear (11) and the small gear (10) are meshed with each other, and the rotary positioning disc (9) is driven to rotate and position by the rotation of the positioning disc rotary motor (12). The automatic liquid coating device for the filter disc has the advantage that the method has high accuracy. In addition, when the technology is used for testing the ammonia content of cigarette smoke, the test result is slightly improved compared with the current standard, the data parallelism is better, and the experiment time can be reduced by 10 to 15 minutes. The problem that the prior art cannot completely trap and effectively extract ammonia in the main stream smoke of the cigarettes due to manual liquid coating is effectively solved.)

1. The utility model provides an automatic liquid device of scribbling of filter element, includes organism (15), its characterized in that, in organism (15), rotational positioning dish (9) are installed on gear wheel (11), pinion (10) are installed on positioning disk rotating electrical machines (12), and gear wheel (11) and pinion (10) are meshing each other, and rotation through positioning disk rotating electrical machines (12) drives rotational positioning dish (9) rotational positioning.

2. The automatic filter element liquid coating device according to claim 1, wherein in the machine body (15), the filter element rotating motor (3) is installed at a position below the filter element placing disc (8) through the rotating bracket (7), the filter element rotating motor (3) is fixedly installed on a lifting rod of the lifting motor (2), when the lifting rod is lifted, the filter element rotating motor (3) is driven to lift upwards to jack the filter element placing disc (8), and then the filter element rotating motor (3) rotates and drives the filter element placing disc (8) to rotate.

3. The automatic filter element liquid coating device according to claim 1 or 2, characterized in that, in the machine body (15), one end of the liquid coating hose (4) is fixed on the transverse overflow slide block (6) and is arranged above the filter element placing disc (8), the other end is arranged on the peristaltic pump (1), the peristaltic pump (1) conveys the experimental liquid to the filter element through the liquid coating hose (4), when the filter element placing disc (8) rotates, the dipping solution in the liquid coating hose (4) flows out and is coated on the filter element placing disc (8), and the support frame (13) and the adjustable foot margin (14) are used for supporting the moving structure and the machine body (15).

4. The automatic filter spreading device according to claim 1, wherein the traverse slider (6) is connected to a traverse motor (5) for pushing the spreading hose forward and backward.

5. The automatic filter disc liquid coating device according to claim 1, wherein a plurality of filter disc placing discs (8) are uniformly placed on the rotary positioning disc (9), and the filter disc placing discs (8) are used for placing filter discs and are arranged on the rotary positioning disc (9).

6. The method for measuring the ammonia content in the mainstream smoke of the cigarette by using the automatic filter liquid coating device according to claim 1, is characterized by comprising the following steps of:

1. coating liquid on a Cambridge filter and collecting smoke;

2. extracting a flue gas sample;

3. carrying out chromatographic analysis;

4. calculating and expressing fruits;

5. detection limit, quantitation limit, precision and recovery rate;

6. repeatability and reproducibility.

7. The method for measuring the ammonia content in the mainstream smoke of the cigarette by using the automatic liquid coating device for the filter disc as claimed in claim 6, wherein the cambridge filter disc is subjected to liquid coating and smoke trapping;

before the liquid coating starts, a power supply is turned on, the device is electrified, a plurality of filter discs are uniformly placed on a filter disc placing disc (8), and parameters of the peristaltic pump (1) are set;

during the preparation of coating liquid, a positioning disc rotating motor (12) rotates to drive a rotating positioning disc (9) to rotate, a first filter disc placing disc (8) is rotated to a position above the rotating motor (3), a lifting motor (2) is lifted to drive the rotating motor (3) to lift, the filter disc placing disc (8) is jacked up and separated from the rotating positioning disc (9), a transverse moving motor (5) is placed to drive a transverse moving slide block (6) to perform transverse moving motion, and a coating liquid hose (4) is driven to move to a specified position above the filter disc placing disc (8);

when the coating liquid starts, the peristaltic pump (1) starts to work, the hydrochloric acid-ethanol aqueous solution is conveyed upwards through the coating liquid hose (4), the rotating motor (3) starts to rotate and drives the filter disc placing disc (8) to rotate along with the rotation, the filter disc also rotates on the filter disc placing disc (8), and the hydrochloric acid-ethanol aqueous solution is coated on the filter disc at a constant speed through the coating liquid hose (4);

when the first filter disc is coated with liquid, the peristaltic pump (1) stops working, the lifting motor (2) descends to drive the rotating motor (3) to descend, the filter disc placing disc (8) falls down and is placed on the rotary positioning disc (9), the positioning disc rotating motor (12) rotates to drive the rotary positioning disc (9) to rotate, the second filter disc placing disc (8) rotates to a position above the rotating motor (3), and liquid coating action is repeated;

according to the steps, after the liquid coating of all the filter discs is finished, the liquid coating work of the group is finished.

8. The method for determining the ammonia content in the mainstream smoke of the cigarette by using the automatic filter element liquid coating device according to claim 6, wherein the smoke sample is subjected to extraction treatment;

after the cigarette is smoked, folding 2 Cambridge filter discs trapping the mainstream smoke and putting the Cambridge filter discs into a 100mL conical flask, and accurately adding 40mL of extract liquor; placing the conical flask on an oscillator, and performing oscillation extraction for 40min, wherein the oscillation frequency is set based on the maximum speed of the filter disc without oscillation, to obtain main stream smoke trapping extract liquid; transferring about 10mL of the main stream smoke trapping extract liquid, passing through a 0.45-micron water-phase filter membrane, discarding the first 5mL of filtrate, and placing the residual filtrate in a chromatographic bottle to be tested; the sample to be tested should complete the ion chromatography within 12 h.

9. The method for determining the ammonia content in the mainstream smoke of the cigarette by using the automatic filter liquid coating device according to claim 6, wherein the result is calculated and expressed by the following steps:

carrying out chromatographic determination on the series of standard working solutions, and using retention time for qualitative determination and an external standard method for quantitative determination; establishing a quadratic fit standard working curve of NH4+ according to the concentration of the prepared standard solution and the response peak area thereof;

calculating the ammonia release amount of the main stream smoke of the cigarette according to a formulaCalculating to obtain:

in the formula:

m-released amount of ammonia in mainstream smoke of the sample in micrograms per cigarette (μ g/cig);

c-measured concentration of ammonium ions in the sample treatment solution in micrograms per milliliter (. mu.g/mL);

c0 — measured concentration of ammonium ions in micrograms per milliliter (μ g/mL) in blank sample treatment solution;

v-volume of extract in milliliters (mL);

n is the number of cigarettes to be smoked, and the unit is a cigarette (cig);

17.03-formula weight of NH 3;

18.04-formula weight of NH4 +;

the arithmetic mean of two parallel samples was taken as the test result, with the accuracy of 0.01. mu.g/cig.

Technical Field

The invention relates to the field of tobacco detection, in particular to a method for measuring the ammonia content in main stream smoke of a cigarette by using an automatic filter element liquid coating device.

Background

In recent years, as people pay more and more attention to harmful ingredients in cigarette smoke, the evaluation standard of cigarette harmfulness is gradually shifted to various trace chemical ingredients from conventional indexes (tar, nicotine and CO). The ammonia is one of the accepted harmful trace components in the smoke, and the accurate and rapid determination of the content of the ammonia in the mainstream smoke of the cigarettes has great significance in controlling or reducing the release amount of the ammonia in the mainstream smoke.

Currently, when mainstream smoke ammonia is analyzed and measured, a Cambridge filter is generally adopted to capture ammonia in cigarette smoke, and then a dilute hydrochloric acid extraction agent is adopted to extract the Cambridge filter and the Cambridge filter is analyzed and measured through an ion chromatography. However, in the existing method, hydrochloric acid-ethanol aqueous solution is manually coated when the hydrochloric acid-ethanol aqueous solution is added in the Cambridge filter sheet trapping and ion chromatography for measuring ammonia in main stream smoke of cigarettes. The problems of time and labor waste, uneven liquid coating, reagent waste and the like exist in manual liquid coating, and the time for testing the ammonia in the mainstream smoke by experimenters is prolonged.

Disclosure of Invention

In order to overcome the existing defects, the invention provides a method for measuring the ammonia content in main stream smoke of a cigarette by using an automatic filter disc liquid coating device.

The utility model provides an automatic liquid device of scribbling of filter element, includes the organism, in the organism, the rotational positioning dish is installed on the gear wheel, and the pinion is installed on positioning disk rotating electrical machines, and gear wheel and pinion intermeshing drive rotational positioning dish rotational positioning through positioning disk rotating electrical machines's rotation.

Wherein, in the organism, filter element rotating electrical machines passes through runing rest to be installed in the position of filter element placing plate below, and filter element rotating electrical machines fixed mounting drives filter element rotating electrical machines and upwards rises when the lifter rises on lifter's lifter, places the dish jack-up with the filter element, then filter element rotating electrical machines) rotation to it rotates to drive the filter element and place the dish.

In the machine body, one end of a liquid coating hose is fixed on a transverse overflow sliding block and is arranged above a filter disc placing disc, the other end of the liquid coating hose is arranged on a peristaltic pump, experimental liquid is conveyed onto the filter disc by the peristaltic pump through the liquid coating hose, when the filter disc placing disc rotates, dipping solution in the liquid coating hose flows out and is coated on the filter disc placing disc, and a support frame and an adjustable foot margin are used for supporting the moving structure and the machine body.

Wherein, the traversing slide block is connected with a traversing motor and used for pushing the liquid coating hose to move forwards and backwards.

Wherein, a plurality of filter discs of placing are evenly placed to the rotational positioning dish, and the filter disc is placed the dish and is used for placing the filter disc, installs on the rotational positioning dish.

A method for measuring the ammonia content in main stream smoke of a cigarette by a filter disc automatic liquid coating device comprises the following steps:

1. coating liquid on a Cambridge filter and collecting smoke;

2. extracting a flue gas sample;

3. carrying out chromatographic analysis;

4. calculating and expressing fruits;

5. detection limit, quantitation limit, precision and recovery rate;

6. repeatability and reproducibility.

According to the automatic filter disc liquid coating device, a sword bridge filter disc catcher filled with a dipping hydrochloric acid-ethanol aqueous solution is used for catching particulate matters of cigarette smoke, dilute hydrochloric acid is used as an extracting agent for extraction after catching is finished, and then accurate determination of ammonia in a smoke condensate is realized by adopting an ion chromatography. And the aim of accurately and quickly capturing and testing the ammonia content in the smoke is fulfilled by optimizing and adjusting the design and modification of the filter disc brake coating liquid.

Drawings

FIG. 1 is a schematic view of an automatic liquid-applying device for filter discs.

Fig. 2 is a schematic view of an automatic filter liquid applying device 2.

Detailed Description

The automatic filter liquid applying device provided by the invention is described in detail below with reference to the accompanying drawings and specific embodiments.

Fig. 1 and 2 show an automatic liquid coating device for a filter disc, which comprises a machine body 15, wherein in the machine body 15, a rotary positioning disc 9 is arranged on a large gear 11, a small gear 10 is arranged on a positioning disc rotating motor 12, the large gear 11 and the small gear 10 are meshed with each other, and the rotary positioning disc 9 is driven to rotate and position through the rotation of the positioning disc rotating motor 12.

In the organism 15, filter element rotating electrical machines 3 installs the position in filter element placing disc 8 below through runing rest 7, and filter element rotating electrical machines 3 fixed mounting drives filter element rotating electrical machines 3 and upwards rises on the lifter of elevator motor 2 when the lifter rises, places the dish 8 jack-up with the filter element, then filter element rotating electrical machines 3 is rotatory to drive filter element placing disc 8 and rotate.

In the machine body 15, one end of a liquid coating hose 4 is fixed on a transverse overflow sliding block 6 and is arranged above a filter disc placing disc 8, the other end of the liquid coating hose is arranged on a peristaltic pump 1, the peristaltic pump 1 conveys test liquid onto the filter disc through the liquid coating hose 4, when the filter disc placing disc 8 rotates, immersion liquid in the liquid coating hose 4 flows out and is coated on the filter disc placing disc 8, and a support frame 13 and an adjustable foot margin 14 are used for supporting a moving structure and the machine body 15.

The traversing slide block 6 is connected with a traversing motor 5 and is used for pushing the coating liquid hose to move forward and backward.

A plurality of filter disc placing discs 8 are evenly placed on the rotary positioning disc 9, and the filter disc placing discs 8 are used for placing filter discs and are installed on the rotary positioning disc 9.

A method for measuring the ammonia content in main stream smoke of a cigarette by using an automatic filter liquid coating device is characterized by comprising the following steps:

1. cambridge filter coating liquid and smoke trapping

A plurality of filter discs 8 are placed to rotary positioning disc 9 and have evenly been placed, rotary positioning disc 9 is installed on gear wheel 11, pinion 10 is installed on positioning disc rotating electrical machines 12, gear wheel 11 and pinion 10 mesh each other, rotation through positioning disc rotating electrical machines 12 drives rotary positioning disc 9 rotational positioning, filter disc rotating electrical machines 3 are installed in the position that filter discs 8 below were placed, 3 fixed mounting of filter disc rotating electrical machines are on elevator rod of elevator motor 2, drive filter disc rotating electrical machines 3 and upwards rise when the elevator rod rises, place filter discs 8 jack-up, then filter disc rotating electrical machines 3 are rotatory, and drive filter discs and place 8 rotations of disc. One end of a liquid coating hose 4 is fixed on the transverse overflow slide block 6 and is arranged above the filter disc placing disc 8, the other end of the liquid coating hose is arranged on the peristaltic pump 1, the peristaltic pump 1 conveys experimental liquid onto the filter disc through the liquid coating hose 4, when the filter disc placing disc 8 rotates, hydrochloric acid-ethanol water solution in the liquid coating hose 4 flows out and is coated on the filter disc placing disc 8, and the support frame 13 and the adjustable feet 14 are used for supporting a moving structure and the machine body 15.

The working process is described in the following with the attached drawings:

before the coating liquid begins, the power supply is turned on, the device is powered on, a plurality of filter discs are uniformly placed on the filter disc placing disc 8, and parameters of the peristaltic pump 1 are set.

During the preparation period of coating liquid, the positioning disc rotating motor 12 rotates to drive the rotary positioning disc 9 to rotate, the first filter disc placing disc 8 is rotated to the position above the rotating motor 3, the lifting motor 2 ascends to drive the rotating motor 3 to ascend, the filter disc placing disc 8 is jacked up and separated from the rotary positioning disc 9, the transverse moving motor 5 is placed to drive the transverse moving slide block 6 to perform transverse moving motion, and the coating liquid hose 4 is driven to move to the specified position above the filter disc placing disc 8.

When the coating liquid starts, the peristaltic pump 1 starts to work, the hydrochloric acid-ethanol aqueous solution is conveyed upwards through the coating liquid hose 4, the rotating motor 3 starts to rotate and drives the filter disc placing disc 8 to rotate along with the rotation, the filter disc also rotates on the filter disc placing disc 8, the hydrochloric acid-ethanol aqueous solution is coated on the filter disc at a constant speed through the coating liquid hose 4, the matching of the rotating motor 3 and the transverse moving motor 5 is controlled, the coating liquid with various curves such as a circular curve, a square curve, a spiral curve and the like can be realized, and the requirements of different experiments are met.

When the first filter disc is coated with liquid, the peristaltic pump 1 stops working temporarily, the lifting motor 2 descends to drive the rotating motor 3 to descend, the filter disc placing disc 8 falls down and is placed on the rotary positioning disc 9, the positioning disc rotating motor 12 rotates to drive the rotary positioning disc 9 to rotate, the second filter disc placing disc 8 rotates to a position above the rotating motor 3, and liquid coating action is repeated. According to the steps, after the liquid coating of all the filter discs is finished, the liquid coating work of the group is finished.

And then the cambridge filter disc coated with the solution is put into a constant temperature and humidity box with the temperature of 22 +/-1 ℃ and the relative humidity of 60 +/-3 percent to be balanced for 2 to 8 hours, so as to obtain the filter disc pretreated by the immersion solution. 2 sheets of 44mm Cambridge filter (1 sheet is pretreated by the impregnation liquid, and 1 sheet is untreated) are placed in a cigarette holder, wherein the filter sheet pretreated by the impregnation liquid is placed at the front end of the cigarette holder, and both the two filter sheets are rough and face towards the direction of a filter tip. Suction was performed according to the regulations GB/T16450 and GB/T19609. The linear type smoking machine sucks 4 cigarettes in the same pore channel of each sample.

2. Flue gas sample extraction treatment

After the cigarette is smoked, 2 Cambridge filter discs trapping the mainstream smoke are folded and placed into a 100mL conical flask, and 40mL of extract liquid is accurately added. Placing the conical flask on an oscillator, and performing oscillation extraction for 40min, wherein the oscillation frequency is set based on the maximum speed of the filter disc without oscillation (reference value is 160r/min), to obtain the main stream smoke trapping extract. About 10mL of the mainstream smoke trap extract was removed, passed through a 0.45 μm aqueous membrane filter, the first 5mL of filtrate was discarded, and the remaining filtrate was placed in a chromatography flask for assay. The sample to be tested should complete the ion chromatography within 12 h.

3. Chromatographic analysis conditions

-mobile phase a: 0.1mol/L methanesulfonic acid (4.6);

-mobile phase B: water;

-flow rate: 1.0 mL/min;

-mobile phase gradient: see table 2;

-sample size: 25 mu L of the solution;

-column temperature: 30 ℃;

-the suppressor current: 132 mA;

-injector temperature: 4 ℃ is prepared.

If no low-temperature sample injection equipment is available, the sample can be stored in a refrigerator at 4 ℃, and sample injection is completed within 1 hour after the sample is taken out. The mobile phase elution procedure is shown in table 1.

Table 1 mobile phase elution procedure

4. And calculating and expressing the result:

1) the standard working curve is made up by using standard working curve,

and carrying out chromatographic determination on the series of standard working solutions, and using retention time for qualitative determination and an external standard method for quantitative determination. And establishing a quadratic fit standard working curve of NH4+ according to the concentration of the prepared standard solution and the response peak area thereof.

2) The amount of ammonia released is calculated,

the release amount of ammonia in the main stream smoke of the cigarette is according to a formulaCalculating to obtain:

in the formula:

m-released amount of ammonia in mainstream smoke of the sample in micrograms per cigarette (μ g/cig);

c-measured concentration of ammonium ions in the sample treatment solution in micrograms per milliliter (. mu.g/mL);

c0 — measured concentration of ammonium ions in micrograms per milliliter (μ g/mL) in blank sample treatment solution;

v-volume of extract in milliliters (mL);

n is the number of cigarettes to be smoked, and the unit is a cigarette (cig);

17.03-formula weight of NH 3;

18.04-formula weight of NH4 +.

The arithmetic mean of two parallel samples was taken as the test result, with the accuracy of 0.01. mu.g/cig. The relative mean deviation between the results of the replicates was no more than 10%.

5. Detection limit, quantitation limit, precision and recovery

The results of detection limit, quantitation limit, precision and recovery rate of spiking of the present method are shown in Table 2.

TABLE 2 detection limits, quantitation limits, precision and recovery of the methods

6. Repeatability and reproducibility

The repeatability and reproducibility results of the method are shown in table 3.

TABLE 3 repeatability and reproducibility of the method

In one embodiment, the cigarettes after balancing and screening are smoked by a linear smoking machine according to the standard conditions specified by ISO, 4 cigarettes are smoked in each experiment, a catcher provided with a manual liquid-coated Cambridge filter disc and an automatic liquid-coated Cambridge filter disc is used for catching particulate matters in the smoke of the cigarettes, 0.01mol/L dilute hydrochloric acid extractant is used for extraction after catching is completed, and then the ammonia content in the smoke condensate is determined by ion chromatography.

TABLE 4 comparison of test results for manual and automatic application methods

As can be seen from the data in Table 4, the results consistent with the current standard can be obtained by testing the ammonia in the traditional cigarette smoke by adopting the method, and the method has good accuracy. In addition, when the technology is used for testing the ammonia content of cigarette smoke, the test result is slightly improved compared with the current standard, the data parallelism is better, and the experiment time can be reduced by 10 to 15 minutes. Effectively solves the problem that the prior art can not completely capture and effectively extract ammonia in the main stream smoke of the cigarettes due to manual liquid coating.

Finally, it should be noted that the above examples are only intended to describe the technical solutions of the present invention and not to limit the technical methods, the present invention can be extended in application to other modifications, variations, applications and embodiments, and therefore all such modifications, variations, applications, embodiments are considered to be within the spirit and teaching scope of the present invention.