CN110658236A - Heishun tablet processing process Ca2+Content monitoring method and rinsing end point judging method - Google Patents
Heishun tablet processing process Ca2+Content monitoring method and rinsing end point judging method Download PDFInfo
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- CN110658236A CN110658236A CN201911014873.7A CN201911014873A CN110658236A CN 110658236 A CN110658236 A CN 110658236A CN 201911014873 A CN201911014873 A CN 201911014873A CN 110658236 A CN110658236 A CN 110658236A
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- conductivity
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- water bleaching
- bleaching liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/06—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a liquid
Abstract
The invention discloses a processing process Ca of Heishun tablets2+A content monitoring method and a rinsing end point judging method, which solve the problem that the calcium ion content is not monitored in the black strip processing process in the prior art. The invention relates to a processing process Ca of Heishun tablets2+The content monitoring method is used for judging Ca of the black flake by measuring the conductivity of the water bleaching liquid2+And (4) content. And finishing the water bleaching step when the conductivity of the water bleaching liquid is less than or equal to 10000 mus/cm. The invention has scientific design, simple method and simple and convenient operation. The invention creatively can judge Ca of the black flake by measuring the conductivity of the water bleaching liquid2+Content, the rinsing process is monitored.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine processing, and particularly relates to a processing process Ca of Heishun tablets2+A content monitoring method and a rinsing end point judging method.
Background
The HEISHUANG tablet is soaked in gallbladder-containing calcium ion. In the prior art, the processing technology of the Heishun tablet comprises a water rinsing step after the Heishun tablet is soaked in the bile, and the bile ingredients including calcium ions in the Heishun tablet can be dissolved out to a certain degree through the water rinsing. In addition, in the prior art, the research on the calcium ions of the black cis-tablets mainly focuses on the research on the calcium ion detection method of finished product decoction pieces, including atomic absorption and titration method determination; the water bleaching process directly related to the content of calcium ions in the finished product decoction pieces is rarely researched. In the prior art, the judgment of the end point of the water rinsing process is always empirical, the content of calcium ions in the black cis-tablets is not monitored, and the situation that the content of calcium ions in the processed black cis-tablets is higher (more than 400 mu mol/g) is often caused.
Therefore, providing a method for monitoring the calcium ion content in the black strip processing process, which can effectively judge the calcium ion content in the black strip rinsing process and judge the rinsing endpoint, becomes a problem to be solved by those skilled in the art.
Disclosure of Invention
The technical problem solved by the invention is as follows: provides a Heishun tablet processing process Ca2+The content monitoring method solves the problem that the calcium ion content is not monitored in the processing process of the black tablets in the prior art.
The invention also provides a method for judging the rinsing endpoint in the processing process of the Heishun tablet.
The technical scheme adopted by the invention is as follows:
according to the inventionA method for monitoring calcium ion content in processing process of HEISHUN tablet comprises determining the electrical conductivity of water bleaching solution to determine Ca content of HEISHUN tablet2+And (4) content.
Specifically, the conductivity of the water bleaching liquid is directly measured by a conductivity meter.
Further, when the conductivity of the water bleaching liquid is 2800-2+The content is 97-358. mu. mol/g.
Further, when the conductivity of the water bleaching liquid is 3000-10000 mu s/cm, Ca in the black strip is2+The content is 100-350 mu mol/g.
Further, the method for directly measuring the conductivity of the water bleaching liquid by using the conductivity meter comprises the following steps: taking the water bleaching liquid to be measured, measuring the temperature, and then setting the temperature of the conductivity meter to be consistent with the temperature of the water bleaching liquid to be measured; and (4) inserting the electrode of the conductivity meter into the water bleaching liquid to be measured, and reading.
Furthermore, if the number is read, no numerical value is displayed on a display screen of the conductivity meter, which indicates that the conductivity value of the water bleaching liquid exceeds the measurement range of the conductivity meter, the water bleaching liquid needs to be diluted by times by distilled water and then the measurement is carried out.
The invention relates to a rinsing endpoint judgment method in a black sheet processing process, which adopts the monitoring method to measure the conductivity of a water bleaching solution, and can finish the water bleaching step when the conductivity of the water bleaching solution is less than or equal to 10000 mus/cm.
Preferably, the water bleaching step can be completed when the conductivity of the water bleaching liquid is 3000-10000 mu s/cm.
Compared with the prior art, the invention has the following beneficial effects:
the invention has scientific design, simple method and simple and convenient operation. The invention creatively can judge Ca of the black flake by measuring the conductivity of the water bleaching liquid2+Content, the rinsing process is monitored. The research of the invention shows that the conductivity range of the water bleaching liquid is controlled to be 3000-10000 mu s/cm, so that Ca in the black cis-butenedioic piece2+The content is in the range of 100-350 mu mol/g, which meets the raw material quality requirement of the black flake.
Drawings
FIG. 1 is a graph showing the relationship between the conductivity of the water bleaching liquid and the content of calcium ions in the black flakes.
Detailed Description
The present invention will be further described with reference to the following description and examples, which include but are not limited to the following examples.
The conductivity meter used in the embodiment of the present invention: thunder magnet, DDS-307; and a conductive electrode DJS-10C.
Example 1
The embodiment discloses a method for directly measuring the conductivity of water bleaching liquid by using a conductivity meter, which specifically comprises the following steps:
taking the water bleaching liquid to be measured, measuring the temperature, and then setting the temperature of the conductivity meter to be consistent with the temperature of the water bleaching liquid to be measured; taking out the conductive electrode of the conductivity meter, washing with distilled water for several times, and slightly wiping with filter paper after washing; inserting the conductive electrode into the water bleaching liquid to be measured, and reading after the numerical value on the display screen is stable to obtain the conductivity value of the water bleaching liquid; if no value is displayed on the display screen, the conductivity value of the water bleaching liquid (with large concentration) exceeds the measurement range of the conductivity meter, and the rinsing liquid needs to be diluted by times by using distilled water and then measured.
Example 2
This example discloses the relationship between the conductivity of different aqueous bleaching solutions and the calcium ion content in corresponding black flakes.
Conductivity is the ability of a material to carry current, as opposed to resistance, in units of Siemens/cm (S/cm), which is 10-6Expressed in μ s/cm, 10-3Expressed in ms/cm. Since radix Aconiti lateralis Preparata should be soaked in the gallbladder liquid during processing of HEISHUAN tablet, which mainly contains calcium chloride (CaCl)2·2H2O), so that CaCl is formed after monkshood is soaked in the bile-bar liquid2High content, and rinsing liquid contains a large amount of CaCl in the water rinsing process after boiling and slicing2Exists in an ionic form and has conductivity.
The black cis-butenedioic tablets need to be repeatedly rinsed by changing water for several times in the rinsing process, the rinsing time is about 12 hours each time, and the soaked black cis-butenedioic tablets need to be stirred for 1-2 times in the process, so that calcium ions and diester alkaloids with high toxicity in the black cis-butenedioic tablets can be dissolved out conveniently. Because the soaking time before water change is longer, the calcium ions in the black strip and the calcium ions in the rinsing liquid reach dynamic balance, the content of the calcium ions in the black strip can be reflected to a greater extent by the amount of the calcium ions in the rinsing liquid, namely, the content of the calcium ions in the black strip is reflected on the side surface by detecting the conductivity of the water bleaching liquid before water change.
In the embodiment, different water bleaching liquids are collected, the conductivity of the water bleaching liquids is measured, the black cis-strips in the water bleaching liquids are fished out, the black cis-strips are dried, the calcium ion content is measured by a titration method, and the conductivity results in the different water bleaching liquids and the calcium ion content in the corresponding black cis-strips are shown in figure 1.
The specific operation of the titration method for determining the content of calcium ions in the embodiment is as follows: precisely weighing 0.5g of black flake powder (screened by a third sieve), adding 10mL of mixed solution of nitric acid and perchloric acid (4: 1), slowly heating and digesting until the mixture is slightly boiled, emitting thick white smoke, continuously digesting until the white smoke is completely dispersed, volatilizing (if the mixture is not completely digested, continuously adding acid for digestion), adding 3mL of 5% hydrochloric acid solution for dissolving, adding 25mL of water, adding 10mL of sodium hydroxide test solution, adding 1mL of 30% triethanolamine, shaking up, adding a proper amount of calcium purpurin indicator, and titrating by using EDTA titration solution (0.01mol/L) until the solution is changed from purple red to pure blue, wherein each 1mLEDTA (0.01mol/L) is equivalent to 10 mu mol of Ca.
As can be seen from the attached FIG. 1, the fluctuation curve of the conductivity value is consistent with the trend of the fluctuation curve chart of the calcium ion content of the black cis-tablets measured correspondingly. According to the 9 groups of rinsing liquid conductivity and black strip calcium ion content data, a correlation function correl (the first array is the rinsing liquid conductivity, and the second array is the black strip calcium ion content of corresponding rinsing) is drawn up to obtain that the correlation coefficient of the rinsing liquid conductivity and the corresponding black strip calcium ion rate is 0.996, the correlation is high, and the situation of the black strip calcium ion content can be judged by measuring the conductivity.
This example shows that Ca in a black flake can be made by controlling the conductivity to 3000-10000. mu.s/cm2+The content is controlled at 100-350 mu mol/g, thereby meeting the requirement of the calcium ion of the black flake raw material. If the conductivity of the water bleaching liquid is higher than 10000 mu s/cm, the rinsing is continued until the conductivity of the water bleaching liquid is lower than 10000 mu s/cm, preferably 3000-10000 mu s/cmAnd s/cm, finishing rinsing.
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but all the insubstantial modifications or changes made within the spirit and scope of the main design of the present invention, which still solve the technical problems consistent with the present invention, should be included in the scope of the present invention.
Claims (8)
1. Heishun tablet preparation process Ca2+The content monitoring method is characterized in that Ca of the black flakes is judged by measuring the conductivity of the water bleaching liquid2+And (4) content.
2. The process Ca of claim 1 for processing HEIHUAN tablet2+The content monitoring method is characterized in that the conductivity of the water bleaching liquid is directly measured by a conductivity meter.
3. The process Ca for processing Heishun tablet as claimed in claim 1 or 22+The content monitoring method is characterized in that when the conductivity of the water bleaching liquid is 2800-2+The content is 97-358. mu. mol/g.
4. The method of claim 3, wherein Ca is prepared from HEISAN tablet2+The content monitoring method is characterized in that when the conductivity of the water bleaching liquid is 3000-10000 mu s/cm, Ca in the black strips2+The content is 100-350 mu mol/g.
5. The process Ca of claim 2 for processing HEIHUAN tablet2+The content monitoring method is characterized in that a conductivity meter is adopted to directly measure the conductivity of the water bleaching liquid, and the method comprises the following steps: taking the water bleaching liquid to be measured, measuring the temperature, and then setting the temperature of the conductivity meter to be consistent with the temperature of the water bleaching liquid to be measured; and (4) inserting the electrode of the conductivity meter into the water bleaching liquid to be measured, and reading.
6. A process according to claim 5Heishun tablet processing process Ca2+The content monitoring method is characterized in that if the number is read, no numerical value is displayed on a display screen of the conductivity meter, the conductivity value of the water bleaching liquid is beyond the measurement range of the conductivity meter, and the water bleaching liquid needs to be diluted by times by using distilled water and then is measured.
7. A method for judging rinsing endpoint in black sheet processing process is characterized in that the conductivity of the water bleaching solution is measured by the monitoring method of any one of claims 1 to 6, and the water bleaching step can be completed when the conductivity of the water bleaching solution is less than or equal to 10000 mus/cm.
8. The method as claimed in claim 7, wherein the water rinsing step is completed when the conductivity of the water rinsing solution is 3000-10000 μ s/cm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149248A (en) * | 2013-02-22 | 2013-06-12 | 浙江大学 | Conductivity-based donkey-hide gelatin skin-blanching process terminal judging method |
| CN103463220A (en) * | 2013-09-22 | 2013-12-25 | 江西中医药高等专科学校 | Standardized processing technology of Chinese herbal piece stewed aconite |
| CN103585017A (en) * | 2013-09-22 | 2014-02-19 | 王小平 | Industrialized preparing process for traditional Chinese medicine decoction pieces simmered monkshood and automatic temperature-control simmering furnace |
-
2019
- 2019-10-24 CN CN201911014873.7A patent/CN110658236A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149248A (en) * | 2013-02-22 | 2013-06-12 | 浙江大学 | Conductivity-based donkey-hide gelatin skin-blanching process terminal judging method |
| CN103463220A (en) * | 2013-09-22 | 2013-12-25 | 江西中医药高等专科学校 | Standardized processing technology of Chinese herbal piece stewed aconite |
| CN103585017A (en) * | 2013-09-22 | 2014-02-19 | 王小平 | Industrialized preparing process for traditional Chinese medicine decoction pieces simmered monkshood and automatic temperature-control simmering furnace |
Non-Patent Citations (4)
| Title |
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| 刘忠: "《造纸湿部化学》", 30 September 2010 * |
| 刘红梅 等: "盐附子漂洗过程中钙离子含量的测定方法", 《中国科技论文》 * |
| 姜玉英: "《造水泥工艺实验》", 31 August 1992, 武汉工业大学出版社 * |
| 过震文 等: "《风积沙路基公路建设关键技术与应用》", 30 April 2017, 上海科学技术出版社 * |
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Application publication date: 20200107 |