Method for detecting content and categories of montmorillonite impurities

A technology of impurity content and detection method, applied in the field of medicine, can solve the problems of inaccurate description and test, inaccurate impurity content, easy to cause errors, etc., and achieve the effect of solving inaccurate inspection methods, improving quality controllability, and simple method

Inactive Publication Date: 2012-07-25
JINAN KANGZHONG PHARMA TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Judging the content of montmorillonite in the prior art is mainly the blue-absorbing method, because the test of blue-absorbing amount usually adopts the moistening ring method, and the titration end point is judged by naked eyes, which is easy to cause errors; the blue-absorbing method is to use the ion-exchange adsorption of montmorillonite , Determining the amount of methylene methylene blue that can be exchanged for ion exchange, there is a large difference in the ion exchange amount of montmorillonite in different regions or in the same region. Inaccurate
[0009] There are many methods for purifying montmorillonite in the prior art. What is concerned about the purification of montmorillonite is the purity of montmorillonite. There is no description and inspection method for the types and contents of minerals contained in the residue after purification of montmorillonite. test, it cannot make a targeted summary of the types and contents of minerals contained in montmorillonite, and the residue after purification of montmorillonite still contains montmorillonite, which cannot be used for the content determination of montmorillonite impurities
[0010] The invention patent (2012100166760) discloses the detection method of asbestos in montmorillonite, but does not describe and test the types of minerals contained in montmorillonite and the inspection method of its content, and the method of detecting asbestos achieves the goal of enriching impurities. The purpose is enough, and it does not need to fully separate the montmorillonite and impurities, so it cannot be used for content determination
[0011] There is no method for accurately detecting the impurity content of montmorillonite in the prior art, nor can it determine the purity of purified montmorillonite

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0107] Take 2 grams of montmorillonite sample, put it in a container, add 10ml of water, stir well, add 0.006mg of sodium hexametaphosphate, shake vigorously for 30 minutes, let it stand for 12 hours, discard the upper suspension, the precipitate , then add 60ml of water, stir well, add 0.01g of water glass, shake vigorously for 20 minutes, let it stand for 8 hours, discard the upper suspension, repeat again, the sediment, dry to constant weight, calculate the weight percentage of impurities 6%.

[0108] Take the impurity and dry it at 450°C for 1 hour, make a powder crystal X-ray diffraction pattern, and analyze according to the characteristic peaks of X-ray diffraction. The impurity in this sample is mainly quartz and contains a small amount of magnesium hydroxide and trace asbestos. Fibrous crystals were found by polarizing microscope observation.

Embodiment 2

[0110] Get 10 grams of montmorillonite samples, put them in a container, add 500 grams of water, fully stir, add 0.03 grams of water glass, stir at 5000 rpm for 10 minutes, let stand for 24 hours, discard the upper suspension, For the precipitate, add 200 grams of water, stir well, add 0.05 water glass, stir at 3000 rpm for 20 minutes, let stand for 8 hours, discard the upper suspension, repeat again, wash 3 times with water, dry and weigh , the weight percentage of calculated impurity is 10%.

[0111] The impurities were taken for powder crystal X-ray diffraction pattern, and according to the characteristic peak analysis of X-ray diffraction, the impurities of the sample were mainly cristobalite, attapulgite and kaolinite. Observation by phase contrast microscopy revealed fibrous and book-like crystals.

Embodiment 3

[0113] Take 5 grams of montmorillonite sample, put it in a container, add 150ml of water, stir well, add 1% sodium pyrophosphate of montmorillonite sample weight, shake vigorously for 40 minutes, let stand for 12 hours, discard the upper part Suspension, sediment, then add 150ml of 0.03% sodium pyrophosphate aqueous solution, shake vigorously for 40 minutes, let stand for 10 hours, discard the upper suspension, repeat again, sediment, dry at 450°C for 1 hour, weigh , The weight percentage of calculated impurity is 15.5%.

[0114] The impurities were taken for powder crystal X-ray diffraction pattern, and according to the characteristic peak analysis of X-ray diffraction, the impurities in the sample were mainly zeolite, illite and trace sepiolite. Scanning electron microscopy revealed rod-like, honeycomb and flaky crystals.

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PUM

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Abstract

The invention relates to a method for detecting content and/or categories of medicinal montmorillonite impurities. The method includes: taking a montmorillonite sample, using water separation method or heavy liquid separation method to completely separate impurities from the montmorillonite, drying, weighing and calculating impurity content; subjecting the impurities to X-ray powder diffraction diagram, and judging categories of minerals in the sample according to the characteristic peak of X-ray diffraction; and using one of the polarizing microscope method, the phase difference microscope method, the scanning electron microscope method or the transmission electron microscope to confirm crystal habits of the impurities. Using the method which is simple can accurately detect content and categories of the impurities in the montmorillonite and solve the technical problem that existing methods for detecting impurity content of montmorillonite are inaccurate.

Description

technical field [0001] The invention relates to a method for detecting the content and type of impurities in medicinal montmorillonite, which belongs to the technical field of medicine. Background technique [0002] Montmorillonite is used in the medical field to treat diarrhea, and is also used as a pharmaceutical excipient in other medicines. [0003] Montmorillonite is refined from bentonite. Different types of bentonite deposits have significant differences in ore-forming parent rock, ore-forming environment, and epigenetic transformation due to their different origins. This will inevitably lead to montmorillonite content, montmorillonite The types and quantities of cations and the differences of associated mineral impurities between stone layers. Bentonite from different mineral deposits and medicinal montmorillonite prepared by different processes must have certain differences in the types of impurities, chemical components, and crystal chemical characteristics. This ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/34G01N23/20G01N23/22G01N5/04
Inventor 张为胜李诗标许翠萍张晶牛凤菊冯立娟周长征
Owner JINAN KANGZHONG PHARMA TECH DEV
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