CN111077103A - A kind of triacetin content determination method - Google Patents
A kind of triacetin content determination method Download PDFInfo
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Abstract
According to the method for measuring the content of the glyceryl triacetate, provided by the invention, by accurately detecting and controlling the application amount of the glyceryl triacetate in the filter stick, the hardness of the filter stick can be stabilized, the smoking quality of cigarettes is improved, the release amount of phenol in smoke can be indirectly monitored, and the release amount of harmful components in cigarette products is reduced.
Description
Technical Field
The invention relates to a method for quickly measuring the content of glyceryl triacetate in a cigarette filter stick.
Background
Glyceryl triacetate is often used as a plasticizer and a curing agent in the processing and production process of the acetate fiber filter stick, and the content of the glyceryl triacetate can influence the hardness, the suction resistance and the filtering effect of the filter stick. In addition, research in recent years finds that: the glycerol triacetate is added into the filter stick, so that the release amount of phenol in smoke can be reduced. Therefore, the application amount of the glyceryl triacetate in the filter stick is detected and controlled, so that the hardness of the filter stick can be stabilized, the smoking quality of the cigarette can be improved, the release amount of phenol in smoke can be indirectly monitored, and accurate scientific data can be provided for reducing the release amount of harmful components of cigarette products.
At present, a filter stick production workshop mostly adopts a gravimetric method to measure the content of glyceryl triacetate in a filter stick, but the gravimetric method has insufficient detection accuracy and larger detection result error; the industrial standard YC/T331-I2010 adopts gas chromatography to measure the content of the triacetin in the filter stick, the separation effect is good, the detection accuracy is high, but the pretreatment process is complicated, the detection is time-consuming and labor-consuming, an organic reagent is required, and the method is difficult to be used for workshop field measurement. The near infrared spectrum analysis technology is a rapid, simple and easy-to-operate detection method. The method has the advantages that the content of the glyceryl triacetate in the filter stick can be detected in a filter stick workshop by using a near infrared spectrum analysis technology, the sample of the filter stick does not need to be damaged, the operation is simple, the detection speed is high, and the result accuracy is high.
The standard detection method for the phenol content in the mainstream smoke of the cigarettes has the disadvantages of complicated pretreatment steps, long detection time and poor repeatability of analysis results. The important special item for cigarette harm reduction technology, namely the phenol reduction technology system research report shows that: the addition of the glycerol can reduce the release amount of phenol in the smoke and has good effect of reducing the selectivity of the phenol.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for measuring the content of triacetin.
The invention is realized by the following technical scheme.
The invention provides a method for measuring the content of glyceryl triacetate; the method comprises the following steps:
1, establishing a near-infrared quantitative analysis model of the content of the glyceryl triacetate in the filter stick sample and storing the model into a cloud database;
2, acquiring a near infrared spectrum of the content of the glyceryl triacetate in the actual filter stick;
3, searching out the most applicable near-infrared quantitative analysis model and analysis algorithm in a cloud database according to the near-infrared spectrum of the glyceryl triacetate content in the actual filter stick;
and 4, analyzing and predicting the content of the glyceryl triacetate in the actual filter stick.
The method for establishing the near-infrared quantitative analysis model comprises the following steps:
1.1, collecting sample spectrum, and preparing a sample filter stick with the content of the glyceryl triacetate of 0-14 percent;
1.2, measuring the content of the sample glyceryl triacetate, and detecting by adopting an industry standard YC/T331-2010 gas chromatography for measuring the glyceryl triacetate in the acetate fiber filter stick to obtain the accurate content of the glyceryl triacetate in the sample filter stick;
1.3, collecting sample spectra, bundling a plurality of sample filter rods into a cylinder with a certain diameter, putting the cylinder into a sampling cup with a diameter corresponding to the diameter of the cylinder, and performing spectral scanning by using a near-infrared spectrometer to obtain a near-infrared spectrogram of a sample;
1.4, processing the near-infrared spectrogram of the sample filter stick to improve the signal-to-noise ratio;
and 1.5, combining the near infrared spectrum of the filter stick sample and the accurate content of the triacetin in the corresponding filter stick sample, and establishing a near infrared quantitative analysis model of the triacetin content in the filter stick sample by adopting a partial least square method.
The method for improving the signal-to-noise ratio of the near infrared spectrum comprises one or more of smoothing treatment, derivative treatment, standard normal transformation and multivariate scattering correction.
The spectrum acquisition parameters of the near infrared instrument in the step 1.3 are as follows: the wave number range is 4000 and 10000cm < -1 >, the scanning times are 64 times, and the resolution is 8cm < -1 >.
The method for measuring the content of the sample glyceryl triacetate in the step 1.2 comprises the following steps:
1.2.1 preparing an anethole absolute ethyl alcohol solution with the purity of not less than 99 percent and the concentration of 1.0mg/mL-1.5mg/mL as an extracting agent;
1.2.2 by mass and volume ratio 1: 20 dissolving triacetin with purity not lower than 99% into the extractant as standard stock solution;
1.2.3 diluting the standard stock solution with an extractant, and preparing n working solutions with different concentrations, wherein the concentration range of the triacetin is 0.5mg/mL-5.0 mg/mL;
1.2.4 taking n sample filter rods containing forming paper, and weighing the sample filter rods by weight K;
1.2.5 longitudinally tearing each sample filter stick, cutting into short filter sticks with the length of 10mm-20mm, putting the short filter sticks into conical bottles with plugs of 250mL respectively, adding 100mL of working solutions with different concentrations Q respectively, and covering with bottle caps;
1.2.6 placing the conical flask with the plug on a rotary oscillator for oscillation extraction for 3h, and taking supernatant for gas chromatography analysis;
1.2.7 measuring the working solution, calculating the peak area ratio of the glyceryl triacetate to the anethole in each working solution, making a linear regression equation of the concentration of the glyceryl triacetate and the peak area ratio, wherein the correlation coefficient r is not less than 0.998;
1.2.8 measuring the supernatant, calculating the peak area ratio of glyceryl triacetate to anethole, and calculating by linear regression equation to obtain the concentration of glyceryl triacetate in the extraction solution.
The expression of the linear regression equation is:
p is the content of the glyceryl triacetate in the sample filter stick; q is the concentration of the working solution;
v volume of working solution;
k/n is the mass of each filter stick.
The content analysis process of the glyceryl triacetate in the filter stick in the step 4 is as follows:
4.1, collecting the spectrum of the filter stick sample to be detected;
4.2, searching out the most applicable near-infrared quantitative analysis model in a cloud database according to the actual near-infrared spectrum of the filter stick sample to be detected;
4.3, analyzing and predicting the content of the glyceryl triacetate in the filter stick to be detected through a near-infrared quantitative analysis model of the content of the glyceryl triacetate in the filter stick sample.
The invention has the beneficial effects that: by accurately detecting and controlling the application amount of triacetin in the filter stick, the hardness of the filter stick can be stabilized, the smoking quality of the cigarette can be improved, the release amount of phenol in smoke can be indirectly monitored, and the release amount of harmful components in the cigarette product can be reduced.
Drawings
FIG. 1 is a flow chart of the detection of the present invention;
FIG. 2 is a flow chart of the near infrared spectroscopy analysis technique
Detailed Description
The technical solutions of the present invention are further described below, but the scope of the claims is not limited thereto.
A method for quickly measuring the content of glyceryl triacetate in a filter stick; the method comprises the following steps:
1, establishing a near-infrared quantitative analysis model of the content of the glyceryl triacetate in the filter stick sample and storing the model into a cloud database;
2, acquiring a near infrared spectrum of the content of the glyceryl triacetate in the actual filter stick;
3, searching out the most applicable near-infrared quantitative analysis model and analysis algorithm in a cloud database according to the near-infrared spectrum of the glyceryl triacetate content in the actual filter stick;
and 4, analyzing and predicting the content of the glyceryl triacetate in the actual filter stick.
The method for establishing the near-infrared quantitative analysis model comprises the following steps:
1.1, collecting sample spectrum, and preparing a sample filter stick with the content of the glyceryl triacetate of 0-14 percent;
1.2, measuring the content of the sample glyceryl triacetate, and detecting by adopting an industry standard YC/T331-2010 gas chromatography for measuring the glyceryl triacetate in the acetate fiber filter stick to obtain the accurate content of the glyceryl triacetate in the sample filter stick;
1.3, collecting sample spectra, bundling a plurality of sample filter rods into a cylinder with a certain diameter, putting the cylinder into a sampling cup with a diameter corresponding to the diameter of the cylinder, and performing spectral scanning by using a near-infrared spectrometer to obtain a near-infrared spectrogram of a sample;
1.4, processing the near-infrared spectrogram of the sample filter stick to improve the signal-to-noise ratio;
and 1.5, combining the near infrared spectrum of the filter stick sample and the accurate content of the triacetin in the corresponding filter stick sample, and establishing a near infrared quantitative analysis model of the triacetin content in the filter stick sample by adopting a Partial Least Squares (PLS) method and a partial least square method.
The method for improving the signal-to-noise ratio of the near infrared spectrum is one or more of the combination of smoothing Savitzkyt-Golay, Karl Norris, derivative processing of a first derivative, a second derivative, standard normal transformation (SNV), standard normal variational transformation (Standard), Multiple Scattering Correction (MSC) and multiple positive scatter correction (multiple scatter correction).
The spectrum acquisition parameters of the near infrared instrument in the step 1.3 are as follows: the wave number range is 4000 and 10000cm < -1 >, the scanning times are 64 times, and the resolution is 8cm < -1 >.
The method for measuring the content of the sample glyceryl triacetate in the step 1.2 comprises the following steps:
1.2.1 preparing an anethole absolute ethyl alcohol solution with the purity of not less than 99 percent and the concentration of 1.0mg/mL-1.5mg/mL as an extracting agent;
1.2.2 by mass and volume ratio 1: 20 dissolving triacetin with purity not lower than 99% into the extractant as standard stock solution;
1.2.3 diluting the standard stock solution with an extractant, and preparing n working solutions with different concentrations, wherein the concentration range of the triacetin is 0.5mg/mL-5.0 mg/mL;
1.2.4 taking n sample filter rods containing forming paper, and weighing the sample filter rods by weight K;
1.2.5 longitudinally tearing each sample filter stick, cutting into short filter sticks with the length of 10mm-20mm, putting the short filter sticks into conical bottles with plugs of 250mL respectively, adding 100mL of working solutions with different concentrations Q respectively, and covering with bottle caps;
1.2.6 placing the conical flask with the plug on a rotary oscillator for oscillation extraction for 3h, and taking supernatant for gas chromatography analysis;
1.2.7 measuring the working solution, calculating the peak area ratio of the glyceryl triacetate to the anethole in each working solution, making a linear regression equation of the concentration of the glyceryl triacetate and the peak area ratio, wherein the correlation coefficient r is not less than 0.998;
1.2.8 measuring the supernatant, calculating the peak area ratio of glyceryl triacetate to anethole, and calculating by linear regression equation to obtain the concentration of glyceryl triacetate in the extraction solution.
The expression of the linear regression equation is:
p is the content of the glyceryl triacetate in each sample filter stick and is expressed as mg/rod;
q is the concentration mg/mL of the working solution;
v volume mL of working solution;
k/n is the mass mg of each filter stick.
The content analysis process of the glyceryl triacetate in the filter stick in the step 4 is as follows:
4.1, collecting the spectrum of the filter stick sample to be detected;
4.2, searching out the most applicable near-infrared quantitative analysis model in a cloud database according to the actual near-infrared spectrum of the filter stick sample to be detected;
4.3, analyzing and predicting the content of the glyceryl triacetate in the filter stick to be detected through a near-infrared quantitative analysis model of the content of the glyceryl triacetate in the filter stick sample.
As shown in fig. 1, the central cloud server group of the present invention, which uses a WEB interaction server, a spectral analysis server, a filter information retrieval server, and an analysis result server, implements an interactive application between the central cloud server and a terminal user through a cloud and a client system. The cloud system comprises a data management system, a near-infrared cloud analysis system, an inquiry management system, a WEB interaction system and a data transmission system. The client system uploads instrument information, spectrum information and filter rod information to the cloud end by driving the spectrum instrument to scan a spectrum, and returns a glyceryl triacetate detection result to the terminal after model analysis.
By using a proper model transfer algorithm (for example, a Spectrum Space Transformation (SST) method, see table 1), a host machine model loaded by a near-infrared cloud analysis system can be converted into a sub-machine model suitable for each near-infrared detection terminal, so that detection and analysis of filter rod samples of each terminal are realized, and the data quality of a detection result is ensured. And adjusting the application amount of the glyceryl triacetate in the filter stick on the production line in time according to the detection result, so as to ensure the quality of the filter stick product.
Example (b):
establishing an analysis model of the sample filter stick,
1. collecting filter stick sample spectrum
(1) For a sampling cup with the diameter of 5cm, after the filter stick samples (50 conventional filter stick samples and 85 fine filter stick samples) are tied by two rubber bands, inserting the sampling cup into the rotary table, and placing the sampling cup on the rotary table;
(2) setting the spectrum acquisition parameters of a near infrared instrument as follows: the wave number range is 4000 and 10000cm < -1 >, the scanning times are 64 times, and the resolution is 8cm < -1 >.
2. Measuring the content of glyceryl triacetate in a filter stick sample
And detecting by using an industry standard YC/T331-2010 (gas chromatography for measuring the glyceryl triacetate in the acetate fiber filter stick) to obtain the accurate content of the glyceryl triacetate in the filter stick.
3. Establishing filter stick glyceryl triacetate quantitative analysis model
(1) The content distribution of the triacetin of the filter stick in the modeling sample is 0-14% (including but not limited to a common filter stick, a high-transparency filter stick, a fine filter stick, a bead blasting filter stick, a groove filter stick and the like);
(2) a spectrum pretreatment mode is adopted to improve the near infrared spectrum signal to noise ratio of a filter stick sample, and the common near infrared spectrum pretreatment mode comprises the following steps: smoothing (Savitzkyt-Golay, Karl Norris), derivative processing (first derivative, second derivative), standard normal transformation (SNV), Multiple Scattering Correction (MSC), etc., without being limited to one or a combination of several of them;
(3) and (3) establishing a near infrared quantitative analysis model of the content of the glyceryl triacetate in the filter stick sample by adopting a Partial Least Squares (PLS) method in combination with the near infrared spectrum of the filter stick sample and the gas phase detection data corresponding to the content of the glyceryl triacetate in the filter stick sample.
4. Rapid detection of glyceryl triacetate content in filter stick by near infrared spectrum analysis technology
(1) Collecting a near infrared spectrum (same as 1) of a filter stick sample with unknown glyceryl triacetate content;
(2) and calling an established applicable filter stick glyceryl triacetate quantitative analysis model according to the filter stick near infrared spectrum information, and predicting the content of glyceryl triacetate in the filter stick.
Near-infrared quantitative analysis model performance of triacetin content of filter stick near-infrared quantitative analysis model performance of triacetin content of conventional filter sticks (common filter sticks and high-transmittance filter sticks):
TABLE 1
Near-infrared model prediction conventional filter stick
Near-infrared model prediction conventional bead blasting filter stick
Note: the conventional bead blasting filter stick is a high-transparency forming paper, a common circumference bead adding filter stick.
The method for calculating the weight of the glyceryl triacetate in the filter rod on the machine table of the filter rod forming machine comprises the following steps:
(1) when the forming machine set operates, cutting a certain number of filter rods added with the glyceryl triacetate, and measuring the weight W;
(2) pressing down a button for stopping spraying glyceryl triacetate on the operation control panel, producing the same number of filter sticks without adding glyceryl triacetate according to the same conditions (the tows are the same, the production speed is the same, and the speed ratio of each roller is the same), and measuring the weight of the filter sticks to be W1;
(3) measuring and calculating the weight T of the forming paper, the hot melt adhesive and the inner bonding line adhesive used by the same number of filter rods;
(4) calculating the content of the glyceryl triacetate:
the method comprises the following steps of (1) expressing the content of triacetin in a filter stick triacetin near-infrared quantitative analysis model:
the calculation method comprises the following steps:
(1) according to a determination method of industry standard YC/T331-2010 'gas chromatography for determining triacetin in a cellulose acetate filter rod', obtaining the content of the triacetin in the filter rod (mode one), and obtaining the percentage content of the triacetin in the filter rod (mode two) according to the ratio of the content of the triacetin in the filter rod to the quality of the filter rod;
(2) taking 5 filter rods containing forming paper, hot melt adhesive and inner bonding line adhesive, respectively weighing the weight of the sampling filter rod, the weight of the sampling filter rod paper and the weight of the adhesive, and accurately weighing the weight to 0.0001 g;
(3) respectively calculating the average mass of each extracted filter stick and the weight of single filter stick paper and glue according to the weighed weight in the step (2);
(4) according to (1), (2) and (3), the dry filament percentage (%) and the tow percentage (%) of the triacetin content in the filter rod can be calculated.
The content of the triacetin in the filter stick can be expressed in the five ways, wherein the way is expressed in absolute value, and the other four ways are expressed in relative value (percentage). The method is expressed in an absolute value form, the influence of the type of the filter stick and the quality of the filter stick on the result needs to be considered, and different types of filter sticks require different triacetin quality, so that the comparison between data and actual control operation are inconvenient.
In the relative value form representation: when the method II is used for calculation, the denominator is the weight of the filter stick, the weights of the paper and the glue are not deducted, and the calculation result is lower; when the method is calculated in the fourth mode, the denominator not only deducts the weight of paper and glue, but also subtracts the content of the glyceryl triacetate in the filter stick, and the calculation result is higher (see the following table); in the calculation methods of the third mode and the fifth mode, the denominators are obtained by deducting the weight of the removed paper and the removed glue, and the calculation results are relatively consistent. However, the third method is a simpler and coarser weight calculation method, and is influenced by more factors (such as accuracy of filter rod weighing, machine station triacetin residual quantity, accuracy of measurement and calculation results of paper and glue, and the like), and the deviation between the calculation result and the true value is larger.
Different representation modes of glyceryl triacetate content in filter stick
| Serial number | Filename | Mode one (mg/rod) | Mode two (%) | Manner four (%) | Mode five (%) |
| 1 | lb 001 | 48.337 | 7.80 | 9.83 | 9.12 |
| 2 | lb 002 | 49.153 | 8.03 | 10.18 | 9.41 |
| 3 | lb 003 | 50.177 | 8.16 | 10.35 | 9.56 |
| 4 | lb 004 | 50.253 | 8.19 | 10.39 | 9.59 |
| 5 | lb 005 | 52.426 | 8.45 | 10.74 | 9.88 |
| 6 | lb 006 | 53.272 | 8.61 | 10.97 | 10.08 |
| 7 | lb 007 | 54.779 | 8.80 | 11.24 | 10.29 |
| 8 | lb 008 | 55.309 | 8.86 | 11.31 | 10.35 |
| 9 | lb 009 | 55.726 | 8.93 | 11.41 | 10.43 |
| 10 | lb 010 | 55.849 | 9.05 | 11.60 | 10.59 |
| 11 | lb 011 | 56.196 | 9.17 | 11.79 | 10.75 |
| 12 | lb 012 | 58.310 | 9.32 | 11.97 | 10.89 |
Therefore, in the filter stick glyceryl triacetate near-infrared quantitative analysis model, the glyceryl triacetate calculation result is expressed in a five-way mode, so that the data accuracy is ensured, the application amount of the glyceryl triacetate in the filter stick is conveniently monitored and adjusted on a filter stick forming machine table, and the actual production operation is facilitated.
Claims (7)
1. A method for measuring the content of glyceryl triacetate comprises the following steps:
1) establishing a near-infrared quantitative analysis model of the content of the glyceryl triacetate in the filter stick sample and storing the model into a cloud database;
2) collecting a near infrared spectrum of the glyceryl triacetate content in the actual filter stick;
3) searching out the most applicable near-infrared quantitative analysis model and analysis algorithm in a cloud database according to the near-infrared spectrum of the glyceryl triacetate content in the actual filter stick;
4) analyzing and predicting the content of the glyceryl triacetate in the actual filter stick.
2. The method for measuring the content of triacetin according to claim 1, characterized in that: the method for establishing the near-infrared quantitative analysis model comprises the following steps:
1.1) collecting sample spectrum, and preparing a sample filter stick with the content of the glyceryl triacetate of 0-14%;
1.2) measuring the content of the sample glyceryl triacetate, and detecting by adopting an industry standard YC/T331-2010 gas chromatography for measuring the glyceryl triacetate in the acetate fiber filter stick to obtain the accurate content of the glyceryl triacetate in the sample filter stick;
1.3) collecting sample spectrum, bundling a plurality of sample filter rods into a cylinder with a certain diameter, putting the cylinder into a sampling cup with a diameter corresponding to the diameter of the cylinder, and performing spectrum scanning by using a near-infrared spectrometer to obtain a near-infrared spectrogram of the sample;
1.4) carrying out signal-to-noise ratio improvement treatment on the near-infrared spectrogram of the sample filter stick;
and 1.5) combining the near infrared spectrum of the filter stick sample and the accurate content of the triacetin content in the corresponding filter stick sample, and establishing a near infrared quantitative analysis model of the triacetin content in the filter stick sample by adopting a Partial Least Squares (PLS) method.
3. The method for measuring the glyceryl triacetate content according to claim 2, wherein: the method for improving the signal-to-noise ratio of the near infrared spectrum is one or more of smoothing (Savitzkyt-Golay, Karl Norris), derivative processing (first derivative, second derivative), standard normal transformation (SNV), and Multiple Scattering Correction (MSC).
4. The method for measuring the glyceryl triacetate content according to claim 2, wherein: the spectrum acquisition parameters of the near infrared instrument in the step 1.3) are as follows: the wave number range is 4000 and 10000cm < -1 >, the scanning times are 64 times, and the resolution is 8cm < -1 >.
5. The method for measuring the glyceryl triacetate content according to claim 2, wherein: the method for measuring the content of the sample glyceryl triacetate in the step 1.2) comprises the following steps:
1.2.1) preparing an anethole absolute ethyl alcohol solution with the purity of not less than 99 percent and the concentration of 1.0mg/mL-1.5mg/mL as an extracting agent;
1.2.2) by mass and volume ratio 1: 20 dissolving glyceryl triacetate with the purity not lower than 99% into an extracting agent to be used as a standard stock solution;
1.2.3) diluting the standard stock solution by using an extractant, and preparing n working solutions with different concentrations, wherein the concentration range of the triacetin is 0.5mg/mL-5.0 mg/mL;
1.2.4) taking n sample filter sticks containing forming paper, and weighing the sample filter sticks by weight K;
1.2.5) longitudinally tearing each sample filter stick, cutting into short filter sticks with the length of 10mm-20mm, putting the short filter sticks into conical bottles with plugs of 250mL respectively, adding 100mL of working solutions with different concentrations Q respectively, and covering with bottle caps;
1.2.6) placing the conical flask with the plug on a rotary oscillator for oscillation extraction for 3h, and taking supernatant for gas chromatography analysis;
1.2.7) measuring the working solutions, calculating the peak area ratio of the glyceryl triacetate to the anethole in each working solution, and making a linear regression equation of the concentration of the glyceryl triacetate and the peak area ratio, wherein the correlation coefficient r is not less than 0.998;
1.2.8) measuring the supernatant, calculating the peak area ratio of glyceryl triacetate to anethole, and calculating the concentration of glyceryl triacetate in the extraction solution by a linear regression equation.
6. The method for measuring the glyceryl triacetate content according to claim 5, wherein: the expression of the linear regression equation is:
p is the content of triacetin in the sample filter rod (milligrams per stick, expressed as mg/rod);
q is the concentration of the working solution (mg/mL);
v volume of working solution (mL);
k/n is the mass (mg) of each filter stick.
7. The method for measuring the content of triacetin according to claim 1, characterized in that: the content analysis process of the glyceryl triacetate in the filter stick in the step 4) is as follows:
4.1) collecting the spectrum of the filter stick sample to be tested according to the step 1.3) in the claim 2;
4.2) according to the actual near infrared spectrum of the filter stick sample to be detected, searching the most applicable near infrared quantitative analysis model in the cloud database according to the step 3) in the claim 1;
4.3) analyzing and predicting the content of the glyceryl triacetate in the filter stick to be tested through the near-infrared quantitative analysis model of the content of the glyceryl triacetate in the filter stick sample established according to claim 2.
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