CN114002187A - Method for monitoring production quality of glue agent based on turbidity analysis - Google Patents
Method for monitoring production quality of glue agent based on turbidity analysis Download PDFInfo
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- CN114002187A CN114002187A CN202111273859.6A CN202111273859A CN114002187A CN 114002187 A CN114002187 A CN 114002187A CN 202111273859 A CN202111273859 A CN 202111273859A CN 114002187 A CN114002187 A CN 114002187A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/59—Transmissivity
Abstract
The invention relates to the technical field of glue quality analysis, in particular to a glue quality monitoring method based on turbidity analysis. Comprises the following steps: firstly, preparing and diluting the glue or the glue intermediate product into glue solution, representing the concentration of the glue solution by the refractive index (namely Brix) of the glue solution, and measuring the concentration of the glue solution by adopting a refraction method; according to the concentration measured by a refraction method, diluting the glue solution to a specific concentration; measuring the turbidity of the glue solution to be detected with the specific concentration by using a turbidity meter; and judging the quality of the colloid in the production process according to the numerical values of the refractive index and the turbidity. The method has reasonable testing principle, the concentration of the glue solution is measured by a refraction method, and the linear relation is good through gravimetric method verification; according to the optical characteristics of impurities, the turbidity of the glue solution with specific concentration is used for representing water-insoluble impurities in the glue solution, so that the actual situation of water-insoluble substances can be better represented; simple operation and high analysis efficiency, wherein, the refractive method for measuring the concentration of the glue solution has the characteristics of rapidness, convenience and simplicity.
Description
Technical Field
The invention relates to the technical field of animal gum quality analysis, in particular to a gum production quality monitoring method based on turbidity analysis.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The gel is solid block oral preparation prepared by decocting animal skin, bone, nail or horn with water to obtain gel, concentrating, molding, and air drying, such as colla Corii Asini, gelatinum oxhide, colla Cornus Cervi, cornu Cervi, etc. The 'glue' is a semitransparent solid with uniform color and no abnormal odor specified in the general rule of China pharmacopoeia-0184 glue of 2020 edition. No foreign matter should be present after dissolving in hot water. In the case of donkey-hide gelatin, the donkey-hide gelatin is prepared by taking donkey hide as a raw material and decocting and concentrating the raw material. The donkey-hide gelatin is famous for yellow as amber and black as paint, and is well-proportioned in south China and in the period of Liang Tai ceramic carry landscape in the 'herbal Jing Ji Zhu' course: the glue has three types of clear and turbid: for thin and clear people, it is used for painting and calligraphy; thick and clear, called the basin-coating glue, … … used as a medicine, which is turbid and black, can be used as a glue without being added with medicine. Therefore, the turbidity of the glue agent is an important index for evaluating the quality of the glue agent.
The production process of the glue agent comprises the working procedures of decocting, extracting glue juice, filtering, primarily concentrating, foaming and concentrating, statically precipitating, modulating and concentrating, boxing, cooling, slicing, airing and the like, wherein the working procedures of filtering, concentrating, foaming, statically precipitating and the like of the glue juice are key factors influencing the quality of the glue agent. In these steps, the active substances are concentrated, the nonvolatile impurities (water-insoluble substances) are removed, the water and the odorous substances are evaporated, and the high molecular substances are degraded. Wherein the filtration, foam beating and static precipitation mainly remove water insoluble substances; the condensation, foam beating and static sedimentation processes are all accompanied with the evaporation of water and the improvement of the transparency of glue solution. The phenomena of the processes are reflected in the production that the glue solution becomes thick and clear gradually, the fishy smell is reduced, the gum fragrance is increased, and the quality indexes related to the final product are the light transmittance of the gum block, the water insoluble substances and the appearance characteristics of the gum block.
The water-insoluble substances are water-insoluble substances as the name suggests, and the amount of the water-insoluble substances is closely related to the turbidity degree of the gum. During the gum production process, the initial extract is heterogeneous in liquid phase and contains many insoluble impurities. The filtering, foam beating, static settling and other steps in the subsequent process are mainly used for removing glue solution impurities, and the water-insoluble substances are main components forming the impurities. The generalized water-insoluble substances comprise impurities which affect the permeability of glue solution and glue blocks, such as animal fat, fatty protein, dander, insoluble keratin and the like, and the impurities are thoroughly removed, so that the clarity of the glue solution is high, the glue blocks are bright, smooth and high in transmittance, and otherwise, the glue solution is turbid, and the glue blocks are dull, rough and poor in transmittance.
For the identification of the permeability of the glue solution, GB 6783-2013 national food safety standard-food additive-gelatin provides a method for measuring the transmittance of a gelatin solution (6.67%) at the wavelengths of 450nm and 620nm by a spectrophotometry at 45 ℃, the method can also be used for the production analysis of the glue solutions such as donkey-hide gelatin and the like theoretically, but for the rapid measuring method lacking the concentration of the glue solution, the concentration of the prepared accurate glue solution becomes a limiting factor; and the light transmittance and the glue solution property of the glue agent are different from those of gelatin, so that the method is not suitable for the rapid detection of the glue agent production.
The quality control of the existing glue production process relates to the concentration of glue and the removal condition of glue impurities, and is basically controlled by the empirical judgment of a glue cooker. Due to the difference of human factors and the lack of effective technical monitoring means, the blindness of the production process is large, the quality fluctuation of the glue solution is serious, and the quality (such as light transmission and smooth finish) of the glue blocks is uneven. These situations indicate that there is a great need for a characterization method and a test method capable of monitoring and analyzing the concentration and impurities of the intermediate product in the existing gum production.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a glue production quality monitoring method based on turbidity analysis, which can truly represent the actual conditions of glue solution concentration change and impurity content in the glue solution production process, has the advantages of simple and rapid operation, truly reflects the change condition of the glue solution, and has feasible monitoring effect on glue solution production.
In order to achieve the above object, the technical solution of the present invention is as follows:
in a first aspect of the invention, there is provided a method for monitoring gum production based on turbidity analysis, comprising the steps of:
firstly, preparing and diluting the glue or the glue intermediate product into glue solution, representing the concentration of the glue solution by the refractive index (namely Brix) of the glue solution, and measuring the concentration of the glue solution by adopting a refraction method; according to the concentration measured by a refraction method, diluting the glue solution to a specific concentration; measuring the turbidity of the glue solution to be detected with the specific concentration by using a turbidity meter; and judging the quality of the colloid in the production process according to the numerical values of the refractive index and the turbidity.
The characterization of the glue solution concentration is obtained by measuring the refractive index of the glue solution, specifically, the glue solution concentration is obtained by measuring the refractive index (namely, Brix) of the glue solution and calculating by a formula; the characterization of the impurities in the glue solution is the turbidity characterization of the glue solution with a specific concentration, specifically, the glue solution to be tested with a certain concentration is prepared, the turbidity of the glue solution is tested, and the content condition of the impurities in the glue solution is judged according to the turbidity value.
In one or more embodiments, the gel or gel intermediate comprises a solid skin gel (such as colla Corii Asini), bone gel, nail gel and horn gel prepared from animal skin, bone, nail or horn, or an intermediate gel solution of the gel production process.
In one or more embodiments, the refractive index of the glue solution is used to represent the concentration of the glue solution, and the specific steps of measuring the concentration of the glue solution by adopting a refraction method are as follows:
(1) taking a specific glue solution, and measuring the mass fraction concentration of the glue solution by a gravimetric method;
(2) preparing a series of glue solutions with known concentrations by taking the glue solutions with known concentrations as mother solutions;
(3) measuring the refractive index of the series of glue solutions;
(4) performing linear regression on the mass fraction-the Brix of the glue solution to obtain a Brix-mass fraction equation of the glue solution;
(5) and testing the brix of the glue solution to be detected, and calculating the concentration of the glue solution to be detected through a linear equation.
In one or more embodiments, the method for preparing the glue solution to be detected with a specific concentration comprises the following steps:
(1) taking a glue solution, dripping the glue solution under a cover plate of a refractometer, testing the Brix of the glue solution, and recording the Brix value as B1；
(2) Taking the glue solution, accurately weighing the glue solution, wherein the weight of the glue solution is M1According to the Brix B of the gum solution1And a predetermined concentration B2Calculating the weight M of the prepared glue solution2Adding water until the total weight of the solution is calculated weight, and uniformly mixing to obtain a to-be-detected glue solution with a specific concentration as a test solution 2; wherein the content of the first and second substances,
in one or more embodiments, the turbidity test method is: adding the sample solution 2 into a turbidimeter, measuring the turbidity of the sample solution 2 with purified water as blank control, and recording the turbidity value as B2Turbidity at concentration.
In one or more embodiments, when the intermediate product of the glue agent is a viscous intermediate glue solution in the production process of hide glue, bone glue, nail glue and gutta percha, the viscous intermediate glue solution is diluted first, and then the refractive index is measured;
in the production process of the glue agent, after primary concentration, the concentration of the glue solution is more than 20%, in the subsequent concentration, foam forming, static precipitation and modulation processes, the concentration of the glue solution is higher (30-70%), the temperature of the field solution is close to 100 ℃, the glue solution is in a liquid state at high temperature, and is in a gel state when cooled to room temperature or the temperature is slightly reduced, so that the glue solution is not convenient for direct test by a refractometer. Therefore, the invention designs the field dilution method for measuring the brix of the glue solution, and calculates the content of the effective components of the glue solution through the conversion relation; because the field glue solution is a high-temperature solution, the sampling process is usually accompanied with the volatilization and cooling gelation of the water content of the glue solution, and errors are brought to the measurement, so that the volatilization of the water content is required to be reduced as much as possible in the field sampling process, and the operation requirement is fast and accurate.
In one or more embodiments, when the glue is a solid skin glue (such as colla Corii Asini), bone glue, nail glue, or horn glue, the solid glue is prepared into glue solution and then detected;
preferably, the step of preparing the solid glue into the glue solution comprises the following steps: weighing the solid gum accurately to 0.001g, adding an appropriate amount of water, heating and melting until the solid gum is completely dispersed, cooling to room temperature, and adding water until the concentration of the solution is 5-10%.
In a second aspect of the invention, there is provided the use of the method for monitoring the quality of gum production based on turbidity analysis of the first aspect in the quality control of a gum production process.
In a third aspect of the present invention, a quality control method in a glue production process is provided, the method comprises: representing the concentration of the glue solution by the refractive index (namely the Brix) of the glue solution, and measuring the concentration of the glue solution by adopting a refraction method; according to the concentration measured by a refraction method, diluting the glue solution to a specific concentration by a dilution ratio; measuring the turbidity of the glue solution to be detected with the specific concentration by using a turbidity meter; and controlling the quality of the glue in the production process according to the refractive index and turbidity values.
Taking a conventional donkey-hide gelatin production process as an example, the quality control of the gelatin and the intermediate product gelatin liquid in the production process according to the refractive index and turbidity values comprises the following control indexes: the concentration of the third extract of the extraction stage glue solution is less than 5.8 percent of brix (corresponding to about 5.0 percent by mass), otherwise, the fourth extract is added; the brix concentration of the glue solution at the initial concentration section reaches 25-35%, so that the next working procedure is conveniently carried out; when the concentration of the liquid cement in the foam beating stage is controlled to be 40-50%, foam is conveniently extracted, and the foam extraction quality is controlled to be 1%, and the turbidity value of the whiteness is less than 450 NTU; controlling the turbidity value of 1% of the whiteness of the glue solution to be less than 380NTU in the static settling section; the turbidity value of 1% Brix gelatin solution is controlled to be less than 500 NTU. The conventional colla Corii Asini is colla Corii Asini produced by modern process such as extracting gelatin juice with high pressure rotary spherical digester; the same applies below.
The specific embodiment of the invention has the following beneficial effects:
(1) the method has reasonable testing principle, the concentration of the glue solution is measured by a refraction method, and the linear relation is good through gravimetric method verification; according to the optical characteristics of impurities, the turbidity of the glue solution with specific concentration is used for representing water-insoluble impurities in the glue solution, so that the actual situation of water-insoluble substances can be better represented;
(2) the method is simple to operate and high in analysis efficiency, and the method for determining the concentration of the glue solution by the refraction method has the characteristics of rapidness, convenience and simplicity;
(3) the concentration of the glue solution is measured by adopting a dilution method, so that the technical difficulty that the measurement by adopting a refraction method is not adopted due to gelation of the high-concentration glue solution after cooling and high-temperature solution is easy to volatilize is avoided;
(4) the test solution is prepared by adopting a quantitative dilution method, so that the problem of large error of low reading of the refractometer is solved;
(5) the turbidity is used as a quality index influencing the permeability of the gel block, and can reflect the quality difference of the gel; the turbidity of the glue solution is closely related to suspended matters in the glue solution, the suspended matters are composed of greasy foreign protein, keratin, mechanical impurities and the like, and belong to glue agent impurities, and the impurities bring serious influence on the permeability of a glue block; the result of the invention is closely related to the quality of the glue solution, so that the quality change and the control index of the glue solution production process are judged according to the result, the product quality of the glue solution can be better improved, and the standardized development of the glue solution industry is guided.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic flow chart of the method for monitoring the quality of a colloid based on turbidity analysis according to the present invention;
FIG. 2 is a linear relationship graph of Brix-concentration of the donkey hide extract in the conventional process of manufacturing donkey-hide gelatin according to example 1 of the present invention;
FIG. 3 is a linear relationship graph of initial concentration band Brix-concentration in example 2 of the present invention;
FIG. 4 is a linear relationship graph of Brix-concentration of deer bone glue extract in example 5 of the present invention;
FIG. 5 is a graph showing the turbidity change of the dope in the frothing process in example 9;
FIG. 6 is a graph showing the transmittance of a dope in the foam forming process in example 9.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The invention will be further explained and illustrated with reference to specific examples.
Example 1 concentration analysis of conventional donkey-hide gelatin donkey skin extract
Experimental materials: the gelatin juice is extracted by melting skin in the conventional donkey-hide gelatin production process.
Linear relationship analysis method:
(1) determining the concentration of the glue solution by a gravimetric method:
uniformly mixing and sampling the glue solution in the extraction section, placing the glue solution in a bottle with a plug, and cooling the glue solution to room temperature to be used as working solution for later use;
taking about 10g of glue solution working solution, placing the glue solution working solution into a numbered and constant-weight weighing bottle, precisely weighing, drying the glue solution in a 105 ℃ oven to constant weight, precisely weighing, and calculating the mass percentage concentration of the glue solution;
(2) preparing a series of standard solution concentrations:
working solution is used as mother solution, and a series of glue solution with standard concentration (the concentration is expressed by omega) is prepared by a gravimetric method;
(3) the brix of the standard solution is measured:
adding 1-2 drops of standard liquid under a refractometer cover plate, and testing the whiteness (B) of the test liquid;
(4) and drawing a standard curve of the Brix (B) -mass percent concentration (omega) of the standard solution by taking the Brix (B) as an abscissa and the mass percent concentration (omega) as an ordinate, and calculating a linear relation equation to obtain K values of the glue solution at different sections.
TABLE 1 measurement of Brix-concentration Linear relationship of donkey hide extract in conventional donkey-hide gelatin production process
And (3) actually measuring results: the linear relation is that Y is equal to 0.858X-0.0004, and the measured value K is equal to 0.858
The method for analyzing the concentration of the extracting solution comprises the following steps:
collecting two batches of extractive solutions 20210607 (first juice, second juice, and third juice) No. 1, 2, 3, 20210609 (first juice, second juice, and third juice) No. 4, 5, and 6, placing in triangular flask with plug, and cooling to room temperature. (the concentration of the extracting solution is dilute, and the extracting solution can not be diluted.)
Taking several drops under a cover plate of a refractometer, testing the Brix of the glue solution, and recording the Brix value as B1。
The glue solution concentration can be calculated according to the following formula:
ω1＝KB1×100％………………………………(1)
in the formula of omega1As the concentration of the gum solution, B1In order to actually measure the whiteness, K is the whiteness of the gum solution-gum solution conversion coefficient, and is obtained by measuring the linear relation of the prior gum solution, wherein K is 0.858.
And (5) result verification: and (3) sampling the glue solution into a constant-weight weighing bottle, drying at 105 ℃ to constant weight, and calculating the mass percentage of the solid glue solution.
The experimental results are as follows:
table 2 example of analysis of concentration of extract juice
The experimental result shows that the linear relation of the glue solution is good. The absolute error is found to be less than 0.2%.
Example 2 analysis of the concentration of the dope in the concentration stage
Experimental materials: concentrating the glue solution: filtering the (conventional colla Corii Asini) gelatin juice, and concentrating to obtain gelatin solution.
Linear relationship analysis method:
(1) determining the concentration of the glue solution by a gravimetric method:
uniformly mixing and sampling the glue solution in the concentration section, placing the mixture in a bottle with a plug, and cooling the mixture to room temperature for later use;
taking a glue solution sample, placing the glue solution sample in a numbered and constant-weight weighing bottle, precisely weighing, drying the glue solution sample in a 105 ℃ oven until the weight of the glue solution sample is constant, precisely weighing, and calculating the mass percentage concentration of the glue solution;
(2) preparing a series of standard solution concentrations:
the glue solution sample is prepared into working solution with a certain concentration, the working solution is used as mother solution, and a series of glue solutions with standard concentrations (the concentration is expressed by omega) are prepared by a gravimetric method.
(3) The brix of the standard solution is measured:
adding 1-2 drops of standard liquid under a refractometer cover plate, and testing the whiteness (B) of the test liquid;
(4) and drawing a standard curve of the Brix (B) -mass percent concentration (omega) of the standard solution by taking the Brix (B) as an abscissa and the mass percent concentration (omega) as an ordinate, and calculating a linear relation equation.
The test results are shown in tables 4 and 5, and a linear relation graph is drawn according to the test results, which are shown in figures 3 and 4.
TABLE 3 Brix-concentration measurement of the dope in the concentration stage
And (3) actually measuring results: the linear relation is that Y is equal to 0.858X-0.0004, and the measured value K is equal to 0.860
Concentration analysis method of the concentration section:
(1) taking glue solution
Sample and dilution method:
preparing a triangular bottle with a plug, adding magnetons, numbering, and accurately weighing and peeling. Sampling at sampling port of colla Corii Asini concentrating section for 2, 4, 6, 8, 10 hr after concentrating, adding into triangular flask with plug, and accurately weighing the added glue solution amount M1Accurately to 0.01g, adding a proper amount of purified water, and uniformly stirring. Cooling to room temperature, weighing the total weight of the gum solution (M)2) To the nearest 0.01 g. As sample solution 1.
(2) The method for testing the Brix comprises the following steps:
adding 1 drop of test solution under the cover plate of refractometer, testing the Brix of the test solution, and recording the Brix value B1。
(3) Calculating the concentration of the glue solution:
the glue solution concentration is estimated according to the following formula:
ω＝KB×M2/M1×100％………………………………(1)
wherein B is the actually measured Brix value, omega is the concentration of the primary rubber solution,
M1in terms of the weight of the extracted gum solution, M2Is the weight of the diluted glue solution.
K is the gel liquid Brix-gel liquid conversion coefficient and is calculated by the gel liquid of the same type with known concentration and the Brix value, wherein K is 0.860.
Table 4 concentration analysis example of concentration section
Example 3 analysis of the concentration of the gum solution during frothing
Experimental materials: on-line sampling of glue solution and purified water in the foam beating process in the production process of conventional donkey-hide gelatin (20210422).
The analysis method comprises the following steps:
(1) the solution dilution method comprises the following steps:
adding magneton into triangular flask with plug, peeling, adding about 10g of glue solution into the triangular flask, and accurately weighing the added glue solution1Accurately to 0.01g, about 10g of purified water is added and stirred uniformly. Cooling to room temperature, weighing the total weight of the gum solution (M)2) To the nearest 0.01 g. As sample solution 1.
(2) The method for testing the Brix comprises the following steps:
adding 1 drop of test solution under the cover plate of refractometer, testing the Brix of the test solution, and recording the Brix value B1。
(3) Calculating the concentration of the glue solution:
the glue solution concentration is estimated according to the following formula:
ω＝KB1×M2/M1×100％………………………………(1)
in the formula B1Is the actually measured Brix value, omega is the concentration of the primary rubber solution,
M1in terms of the weight of the extracted gum solution, M2Is the weight of the diluted glue solution.
K is the gel liquid Brix-gel liquid conversion coefficient and is calculated by the similar gel liquid with known concentration and the Brix value, and is 0.881 here.
TABLE 5 example of concentration test of glue solution in frothing procedure
Example 4 analysis of the concentration of the dope in the static precipitation stage
Experimental materials: the gel liquid is sampled on line and purified water is obtained in the static precipitation process in the conventional donkey-hide gelatin (20210521120) production.
The analysis method comprises the following steps:
(1) sampling and solution dilution:
preparing a triangular bottle with a plug, adding magnetons, peeling and numbering; collecting the gel solution of conventional colla Corii Asini (20210521120) at the position 5CM below the liquid surface after static precipitation for 0, 5, 10, and 15 hr, respectively (sample numbers are 1, 2, 3, and 4), adding 10g into a triangular flask, and accurately weighing the gel solution1Accurately to 0.01g, about 10g of purified water is added and stirred uniformly. Cooling to room temperature, weighing the total weight of the gum solution (M)2) To the nearest 0.01g, as sample solution 1.
(3) The method for testing the Brix comprises the following steps:
adding 1 drop of test solution under the cover plate of refractometer, testing the Brix of the test solution, and recording the Brix value B1。
(4) Calculating the concentration of the glue solution:
the glue solution concentration is estimated according to the following formula:
ω＝KB1×M2/M1×100％………………………………(1)
in the formula B1Is the actually measured Brix value, omega is the concentration of the primary rubber solution,
M1in terms of the weight of the extracted gum solution, M2Is the weight of the diluted glue solution.
K is a conversion coefficient of the gel liquid Brix and the gel liquid, and is calculated by the similar gel liquid with known concentration and the Brix value, and is 0.8803 here.
The experimental results are as follows:
TABLE 6 example of the analysis of the concentration of the cement in the settling stage
Example 5 analysis of the concentration of the glue solution in the deer bone glue production process:
experimental materials: the deer bone glue is extracted to obtain the glue juice in the production process.
Linear relationship analysis method:
(1) determining the concentration of the glue solution by a gravimetric method:
uniformly mixing and sampling the glue solution in the extraction section, placing the glue solution in a bottle with a plug, and cooling the glue solution to room temperature to be used as working solution for later use;
taking about 10g of glue solution working solution, placing the glue solution working solution into a numbered and constant-weight weighing bottle, precisely weighing, drying the glue solution in a 105 ℃ oven to constant weight, precisely weighing, and calculating the mass percentage concentration of the glue solution;
(2) preparing a series of standard solution concentrations:
working solution is used as mother solution, and a series of glue solution with standard concentration (the concentration is expressed by omega) is prepared by a gravimetric method;
(3) the brix of the standard solution is measured:
adding 1-2 drops of standard liquid under a refractometer cover plate, and testing the whiteness (B) of the test liquid;
(4) and drawing a standard curve of the Brix (B) -mass percent concentration (omega) of the standard solution by taking the Brix (B) as an abscissa and the mass percent concentration (omega) as an ordinate, and calculating a linear relation equation to obtain K values of the glue solution at different sections.
TABLE 7 determination of the Brix-concentration Linear relationship of deer bone glue extract
And (3) actually measuring results: the linear relation is that Y is 0.8455X-0.0001, and the measured value K is 0.8455
The method for analyzing the concentration of the extracting solution comprises the following steps:
taking three batches of extract 072301 (first juice, second juice and third juice), numbers 1, 2, 3, 072302 (first juice, second juice and third juice), numbers 4, 5, 6, 072303 (first juice, second juice and third juice), numbers 7, 8 and 9, placing in a triangular flask with a plug, and cooling to room temperature.
Taking several drops under the cover plate of refractometer, testing glueThe Brix value is recorded as B1。
The glue solution concentration can be calculated according to the following formula:
ω1＝KB1×100％………………………………(1)
in the formula of omega1As the concentration of the gum solution, B1K is the Brix of the glue solution to the conversion coefficient of the glue solution, and is obtained by measuring the linear relation of the previous glue solution, wherein K is 0.8455.
And (5) result verification: and (3) putting the glue solution into a constant-weight weighing bottle, drying the glue solution in a 105 ℃ oven to constant weight, and calculating the solid mass percentage content of the glue solution.
TABLE 8 analysis example of the concentration of deer bone glue extract gel juice
The experimental result shows that the linear relation of the glue solution is good. The absolute error is found to be less than 0.3%.
Example 6 turbidity analysis of donkey hide extract in conventional donkey-hide gelatin production Process
Experimental materials: the traditional colla Corii Asini (214015) production process comprises dissolving colla Corii Asini juice (primary juice, secondary juice, tertiary juice, and quaternary juice), and purified water.
(Note: the traditional donkey-hide gelatin refers to the donkey-hide gelatin produced by classical technology- -such as extracting gelatin juice in open pot- -the same applies below)
The analysis method comprises the following steps:
(1) sampling:
respectively taking 200ml of first to fourth juice extracting solutions of the glue solution in the traditional donkey-hide gelatin (214015) skin melting and extracting stage, placing in a triangular flask with a plug, and cooling to room temperature to serve as a test solution 1 for later use.
(2) And (3) measuring the concentration of the glue solution:
respectively shaking the test solution 1 cooled to room temperature, adding several drops of the solution under a cover plate of a refractometer, testing the Brix of the solution, and recording the Brix value B1。
(3) Preparing a 1% Brix solution:
shaking of test solution 1Homogenizing, peeling off dried Erlenmeyer flask on a balance with index value of 0.01g, adding 10g of test solution 1, and precisely weighing (M)1) Then, the weight M of the solution with the whiteness of 1 percent is prepared according to the whiteness calculation of the glue solution2Adding water to the total weight of the solution M2And mixing to obtain 1% Brix solution as sample solution 2. The calculation formula is as follows:
in the formula, B1The Brix of test solution 1, M1For sample volume of test solution 1, B2The Brix of the solution to be prepared (test solution 2) was 1% here.
(3) Turbidity test
And adding the test solution 2 into a turbidity meter, measuring turbidity and recording a turbidity value.
The experimental results are as follows:
TABLE 9 turbidity analysis results of skin segment gel juice in the conventional colla Corii Asini production process
The experimental result shows that the concentration of the glue juice extracted for four times is gradually reduced in the donkey skin extraction process; in the aspect of turbidity change, the turbidity of 1% glue solution is not changed greatly in the first two times, and the turbidity of the second two times (three juice and four juice) is gradually increased, which indicates that the amount of collagen in the later glue solution is gradually reduced and the impurity components are gradually increased; this is because, as the extraction intensity increases, part of the horny layer is dispersed and eluted, and as a result, impurities in the dope increase, and the transmittance of the dope decreases.
Example 7Glue solution turbidity analysis of filtration and concentration section in traditional donkey-hide gelatin production process
Experimental materials: the traditional colla Corii Asini (214015) production process comprises dissolving colla Corii Asini juice (first juice, second juice, and third juice), filtering, concentrating to obtain concentrated colla Corii Asini juice (sample numbers 1, 2, and 3 respectively), and purifying with purified water.
The analysis method comprises the following steps:
(1) sampling and solution dilution:
adding magneton into triangular flask with plug, peeling, respectively adding 10g of the concentrated filtrate (sample numbers 1, 2, and 3) of the first juice, the second juice and the third juice of conventional colla Corii Asini (214015) into the triangular flask, accurately weighing the added glue solution M1Adding about 10g of purified water into the mixture until the weight is accurate to 0.01g, and uniformly stirring the mixture; cooling to room temperature, weighing the total weight of the gum solution (M)2) To the nearest 0.01g, as sample solution 1.
(3) The method for testing the Brix comprises the following steps:
adding 1 drop of test solution under the cover plate of refractometer, testing the Brix of the test solution, and recording the Brix value B1；
(4) Preparing a 1% Brix solution:
cooling the sample solution 1 to room temperature, shaking, peeling with a dry conical flask on a balance with a division value of 0.01g, adding 10g of the sample solution 1, and accurately weighing (M)3) According to the Brix B of the test solution 11Calculating the weight of the prepared solution, adding water until the total weight of the solution is the calculated weight M4And uniformly mixing to obtain a 1% Brix glue solution serving as a test solution 2, wherein the calculation formula is as follows:
in the formula, B1The Brix of test solution 1, M3For sample volume of test solution 1, B2The Brix of the solution to be prepared (test solution 2) was 1% here.
(5) Turbidity test
And adding the test solution 2 into a turbidity meter, taking purified water as a blank, measuring turbidity, and recording a turbidity value.
The experimental results are as follows:
TABLE 10 turbidity analysis of the filtrate in the concentration stage of conventional colla Corii Asini production
Compared with the example, the turbidity of the glue solution after filtration and concentration is obviously reduced, which shows that the impurity removal effect is obvious.
Example 8The conventional donkey-hide gelatin extracting solution impurity removing process contrast experiment analysis:
experimental materials: the conventional colla Corii Asini (202102015) production process comprises dissolving colla Corii Asini juice (primary juice, secondary juice, and tertiary juice) and purified water.
The analysis method comprises the following steps:
(1) treating a rubber sample and sampling:
respectively taking 5 parts of first juice glue solution of a conventional donkey-hide gelatin (202102015) in a skin melting and extracting stage, respectively centrifuging for 5min at 80 ℃ and 2000 rpm, 10min at 80 ℃ and 4000 rpm, filtering by filter cotton, respectively taking 100ml of the processed glue solution in a triangular flask with a plug, cooling to room temperature, and taking the treated glue solution as test solution 1 for later use, wherein the serial numbers are 1, 2, 3, 4 and 5 respectively.
(2) And (3) measuring the concentration of the glue solution:
mixing the test solution 1 cooled to room temperature, adding several drops of the test solution under a cover plate of a refractometer, testing the Brix of the test solution, and recording the Brix value B1。
(3) Preparing a 0.3% Brix solution:
shaking the sample solution 1, peeling with a dry conical flask on a balance with a division value of 0.01g, adding 10g of the sample solution 1, and precisely weighing (M)1) Then, the weight M of the solution with the Brix of 0.3 percent is prepared according to the Brix of the glue solution2Adding water to the total weight of the solution M2Mixing to obtain 0.3% Brix solution as sample solution 2. The calculation formula is as follows:
in the formula, B1The Brix of test solution 1, M1For sample volume of test solution 1, B2To prepare a solutionThe Brix of (sample 2) was 0.3% in this case.
(4) Turbidity test
And adding the test solution 2 into a turbidity meter, measuring turbidity and recording a turbidity value.
The experimental results are as follows:
TABLE 11 turbidity contrast experiment for impurity removal process of extractive solution in conventional colla Corii Asini production process
Compared with a sample which is not processed, the impurity removal effect of the glue solution is obvious, and the processing effects of different processes can be seen.
Example 9 analysis of turbidity Change of gum solution during foam beating
Experimental materials: on-line sampling of glue solution and purified water in the foam beating process in the production process of conventional donkey-hide gelatin (20210422).
The analysis method comprises the following steps:
(1) the solution dilution method comprises the following steps:
adding magneton into triangular flask with plug, peeling, adding about 10g of glue solution into the triangular flask, and accurately weighing the added glue solution1Adding about 10g of purified water into the mixture until the weight is accurate to 0.01g, and uniformly stirring the mixture; cooling to room temperature, weighing the total weight of the gum solution (M)2) To the nearest 0.01g, as sample solution 1.
(2) The method for testing the Brix comprises the following steps:
adding 1 drop of test solution under the cover plate of refractometer, testing the Brix of the test solution, and recording the Brix value B1。
(3) Preparing a 1% Brix solution:
cooling the sample solution 1 to room temperature, shaking, peeling with a dry conical flask on a balance with a division value of 0.01g, adding about 10g of the sample solution 1, and accurately weighing (M)3) According to the Brix B of the test solution 11Calculating the weight of the prepared solutionAdding water to the total weight of the solution to calculate the weight M4And uniformly mixing to obtain a 1% Brix glue solution serving as a test solution 2, wherein the calculation formula is as follows:
in the formula, B1The Brix of test solution 1, M3For sample volume of test solution 1, B2The Brix of the solution to be prepared (test solution 2) was 1% here.
(4) Turbidity test
And adding the test solution 2 into a turbidity meter, taking purified water as a blank, measuring turbidity, and recording a turbidity value.
(5) And (3) light transmittance measurement:
and (3) adding the test solution 2 into a 1cm glass cuvette, taking purified water as a blank, measuring the light transmittance of the test solution at 500nm and 600nm by using a UV2700 spectrophotometer, and recording the light transmittance value.
The test results were as follows:
TABLE 12 comparison of turbidity and transmittance of foam-beating glue solution in conventional colla Corii Asini production process
Example 10 analysis of turbidity Change of glue solution during settling
Experimental materials: the gel liquid is sampled on line and purified water is obtained in the static precipitation process in the conventional donkey-hide gelatin (20210521120) production.
The analysis method comprises the following steps:
(1) sampling and solution dilution:
preparing a triangular bottle with a plug, adding magnetons, peeling and numbering. Collecting the liquid glue of the static precipitation stage in the production process of colla Corii Asini (20210521120), standing for 0, 5, 10, and 15 hr, sampling at 5CM position below the liquid surface (sample numbers are 1, 2, 3, and 4), adding 10g each into a triangular flask, and accurately weighing the added liquid glue amount M1Accurately to 0.01g, about 10g of purified water is added and stirred uniformly. Cooling to room temperature, weighingWeighing the total weight of glue solution (M)2) To the nearest 0.01g, as sample solution 1.
(3) The method for testing the Brix comprises the following steps:
adding 1 drop of test solution under the cover plate of refractometer, testing the Brix of the test solution, and recording the Brix value B1。
(4) Preparing a 1% Brix solution:
cooling the sample solution 1 to room temperature, shaking, peeling with a dry conical flask on a balance with a division value of 0.01g, adding 10g of the sample solution 1, and accurately weighing (M)3) According to the Brix B of the test solution 11Calculating the weight of the prepared solution, adding water until the total weight of the solution is the calculated weight M4And uniformly mixing to obtain a 1% Brix glue solution serving as a test solution 2, wherein the calculation formula is as follows:
in the formula, B1The Brix of test solution 1, M3For sample volume of test solution 1, B2The Brix of the solution to be prepared (test solution 2) was 1% here.
(5) Turbidity test
And adding the test solution 2 into a turbidity meter, taking purified water as a blank, measuring turbidity, and recording a turbidity value.
The experimental results are as follows:
TABLE 13 turbidity Change analysis of conventional donkey-hide gelatin during static precipitation
The results show that: the turbidity of the glue solution is gradually reduced along with the increase of the static settling time, and the early-stage reduction amplitude is larger.
Example 11 analysis of the light transmittance and turbidity of the donkey-hide gelatin Block
Experimental materials: traditional colla Corii Asini block (specification 95 × 42 × 7mm, selecting blocks with same thickness and different permeability for comparison experiment), and purified water.
The experimental method comprises the following steps:
(1) and (3) light transmittance measurement:
sample treatment: selecting various rubber blocks, selecting the rubber blocks with the same thickness (6.8mm), scraping off the seal marks by using a blade, and wiping off floating dust by using clean gauze. Placing the rubber block on a light path of a diffuse transmission densitometer, and measuring the transmittance at a wavelength of 380-760 nm by taking air as reference contrast and a unthreaded hole with the diameter of 2 mm;
(2) preparing a glue solution A: cutting the gel block by a guillotine, sampling, adding 10 times of water, melting at 40-60 ℃, cooling to room temperature, adding water to a certain weight until the gel content of the solution is about 5%, and uniformly mixing to obtain a test solution 1;
(3) the method for testing the Brix comprises the following steps:
adding 1 drop of test solution under the cover plate of refractometer, testing the Brix of test solution 1, and recording Brix value B1。
(4) Preparing a test solution with the Brix of 1 percent:
shaking the sample solution 1, peeling with a dry conical flask on a balance with a division value of 0.01g, adding the sample solution 1, weighing accurately, wherein the weight of the gel solution is M3According to the Brix of the test solution 1 and the predetermined concentration B2Calculating the weight M of the prepared glue solution4Adding water until the total weight of the solution is calculated weight, uniformly mixing to obtain a glue solution with a specific concentration as a test solution 2, wherein the calculation formula is as follows:
in the formula, B2＝1.0％
Uniformly mixing to obtain a glue solution with the whiteness of 1 percent as a test solution 2;
(5) the turbidity test method comprises the following steps: adding the sample solution 2 into a turbidimeter, measuring the turbidity of the sample solution 2 with purified water as blank control, and recording the turbidity value as B2Turbidity at concentration.
The test results were as follows:
TABLE 14 block transmittance and 1% gum turbidity control
Example 12 analysis of light transmittance and turbidity of the gel masses of antler glue and tortoise-shell glue
Experimental materials: the finished product of colla cornus cervi and colla Plastri Testudinis (specification 35 × 25 × 5mm, selecting colla Corii Asini blocks with same thickness and different permeability for comparison experiment), and purified water.
The experimental method comprises the following steps:
(1) and (3) light transmittance measurement:
sample treatment: selecting various rubber blocks, selecting the rubber blocks with the same thickness (5.3mm), scraping off the seal marks by a blade, and wiping off floating dust by clean gauze. Placing the rubber block on a light path of a diffuse transmission densitometer, and measuring the transmittance at a wavelength of 380-760 nm by taking air as reference contrast and a unthreaded hole with the diameter of 2 mm;
(2) preparing a glue solution A: cutting the gel block by a guillotine, sampling, adding 10 times of water, melting at 40-60 ℃, cooling to room temperature, adding water to a certain weight until the gel content of the solution is about 6%, and uniformly mixing to obtain a test solution 1;
(3) the method for testing the Brix comprises the following steps:
adding 1 drop of test solution under the cover plate of refractometer, testing the Brix of test solution 1, and recording Brix value B1。
(4) Preparing a test solution with the Brix of 1 percent:
shaking the sample solution 1, peeling with a dry conical flask on a balance with a division value of 0.01g, adding the sample solution 1, weighing accurately, wherein the weight of the gel solution is M3According to the Brix of the test solution 1 and the predetermined concentration B2Calculating the weight M of the prepared glue solution4Adding water until the total weight of the solution is calculated weight, uniformly mixing to obtain a glue solution with a specific concentration as a test solution 2, wherein the calculation formula is as follows:
in the formula, B2＝1.0％
Uniformly mixing to obtain a glue solution with the whiteness of 1 percent as a test solution 2;
(5) turbid urineThe degree testing method comprises the following steps: adding the sample solution 2 into a turbidimeter, measuring the turbidity of the sample solution 2 with purified water as blank control, and recording the turbidity value as B2Turbidity of the gum solution at concentration.
The test results were as follows:
TABLE 15 contrast of transmittance of antler glue, tortoise-shell glue and turbidity of 1% glue
As can be seen from the results of examples 11-12, the light transmittance of the cement with different permeabilities and the turbidity of the cement solution are essentially inversely related, indicating that the cement turbidity is correlated with the light transmittance of the cement.
The above examples show that the turbidity in the glue solution is closely related to the suspended matter in the glue solution, and it is feasible to monitor the suspended matter in the glue solution by a turbidity method during the glue production process, and further control the light transmittance of the glue solution and the glue block.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A glue quality monitoring method based on turbidity analysis is characterized by comprising the following steps:
firstly, preparing and diluting the glue or the glue intermediate product into glue solution, representing the concentration of the glue solution by the refractive index of the glue solution, and measuring the concentration of the glue solution by adopting a refractive method; according to the concentration measured by a refraction method, diluting the glue solution to a specific concentration; measuring the turbidity of the glue solution to be detected with the specific concentration by using a turbidity meter; and judging the quality of the colloid in the production process according to the numerical values of the refractive index and the turbidity.
2. The method for monitoring the production quality of glue based on turbidity analysis as claimed in claim 1, wherein said glue or intermediate product of glue comprises solid glue of hide, bone glue, nail glue and horn glue prepared from animal skin, bone, nail or horn, or intermediate glue solution in the glue production process.
3. The method for monitoring the production quality of the glue based on turbidity analysis as claimed in claim 1, wherein the refractive index of the glue is used for representing the concentration of the glue, and the specific steps for measuring the concentration of the glue by adopting the refraction method are as follows:
(1) taking a specific glue solution, and measuring the mass fraction concentration of the glue solution by a gravimetric method;
(2) preparing a series of glue solutions with known concentrations by taking the glue solutions with known concentrations as mother solutions;
(3) measuring the refractive index of the series of glue solutions;
(4) performing linear regression on the mass fraction-the Brix of the glue solution to obtain a Brix-mass fraction equation of the glue solution;
(5) and testing the brix of the glue solution to be detected, and calculating the concentration of the glue solution to be detected through a linear equation.
4. The method for monitoring the production quality of glues based on turbidity analysis according to claim 1, characterized in that, the method for preparing the glue to be tested at a specific concentration is:
(1) taking a glue solution, dripping the glue solution under a cover plate of a refractometer, testing the Brix of the glue solution, and recording the Brix value as B1；
(2) Taking the glue solution, accurately weighing the glue solution, wherein the weight of the glue solution is M1According to the Brix B of the glue solution1And a predetermined concentration B2Calculating the weight M of the prepared glue solution2Adding water until the total weight of the solution is calculated weight, and uniformly mixing to obtain a to-be-detected glue solution with a specific concentration as a test solution 2; wherein the content of the first and second substances,
5. the turbidity analysis-based gum production quality monitoring method of claim 1, wherein the turbidity testing method is: adding the glue solution to be detected with a specific concentration into a turbidity meter, taking purified water as a blank control, measuring the turbidity of the glue solution to be detected with the specific concentration, and recording the turbidity value as the turbidity under the specific concentration.
6. The method for monitoring the production quality of the glue agent based on the turbidity analysis as claimed in claim 1, wherein when the glue solution is a viscous intermediate glue solution in the production process of hide glue, bone glue, nail glue and horn glue, the viscous intermediate glue solution is diluted first, and then the refractive index is measured.
7. The method for monitoring the quality of the glue based on the turbidity analysis as claimed in claim 1, wherein when the glue is solid skin glue, bone glue, nail glue and horn glue, the solid glue is prepared into glue solution and then detected.
8. The method for monitoring the quality of a gel based on turbidity analysis as claimed in claim 7, wherein the step of formulating the solid gel into a gel comprises: weighing the solid gum accurately to 0.001g, adding an appropriate amount of water, heating and melting until the solid gum is completely dispersed, cooling to room temperature, and adding water until the concentration of the solution is 5-10%.
9. Use of a method for monitoring the quality of a gum production process based on turbidity analysis according to any one of claims 1-8 in the quality control of a gum production process.
10. A quality control method in the production process of a glue agent is characterized by comprising the following steps: representing the concentration of the glue solution by using the refractive index of the glue solution, and measuring the concentration of the glue solution by adopting a refraction method; according to the concentration measured by a refraction method, diluting the glue solution to a certain concentration; measuring the turbidity of the glue solution to be detected with the specific concentration by using a turbidity meter; and controlling the quality of the glue solution in the production process according to the numerical values of the refractive index and the turbidity.
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