CN102607926A - Method for detecting content and categories of montmorillonite impurities - Google Patents
Method for detecting content and categories of montmorillonite impurities Download PDFInfo
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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
The present invention relates to the detection method of impurity content and kind in a kind of medicinal smectite, belong to medical technical field.
Background technology
Smectite is used for treatment diarrhoea at field of medicaments, also is used for other medicine as pharmaceutic adjuvant.
Smectite forms by bentonitic clay is refining; Various dissimilar bentonitic clay mineral deposits are because the origin cause of formation is different; Have significant difference at aspects such as becoming the ore deposit parent rock, become the ore deposit environment, the transformation effect is given birth in the back, this must cause the difference of cationic kind and quantity and associated mineral impurity between smectite content, montmorillonite layer.Use the bentonitic clay in different mineral deposits, the medicinal smectite that adopts different processes to prepare; The kind of impurities; Chemical constitution, crystal chemistry characteristic etc. certainly exist certain difference; This species diversity can cause the variation of their some physicochemical property, and this variation can directly have influence on the security and the effective performance of medicine.Smectite must detect the kind and the content thereof of its contained dirt, to guarantee its curative effect and security as medicine.
The detection method of impurity in the existing medicinal smectite quality standard; It is relative content with the X-ray diffracting spectrum checked for impurities; " characteristic spectral line of smectite is in about 1.5nm and 0.45nm wavelength, and other impurity absorption peak strength must not be higher than second characteristic peak (about 0.45nm) of smectite in the collection of illustrative plates in standard code." this standard can control the relative content of impurity, but the kind of contained mineral not controlled.
The peak intensity of X-ray diffracting spectrum is relevant with the structure of the content of crystalline solid and crystal: same species crystal structure is complete, crystalline form is better, and diffracted intensity is strong more; Crystal structure is incomplete, crystalline form is relatively poor, and diffracted intensity is low more; The high more diffracted intensity of the content of crystalline solid is also just strong more.The height of impurity peaks and smectite 0.45nm place characteristic peak relative intensity is except relevant with content, the crystal habit of impurity, and is also closely related with the crystal habit of smectite self.This area professional and technical personnel is known; Different thing phase X-gamma ray absorption coefficients are very different; Certain thing is mixed in the very little matrix of absorption coefficient more obvious mutually, if when containing the big mineral of the absorption coefficient of more amount in the smectite, on diffractogram, is difficult for discovering; And when containing the little mineral of a small amount of absorption coefficient in the sample, still can produce the obvious diffraction peak.When the big mineral of the absorption coefficient that contains more amount in the smectite, use the X-ray diffracting spectrum detection method, still can't control the kind of contained mineral.
Stipulate in the existing medicinal smectite quality standard, " contain silicon dioxide (SiO
2) should be 55.0%～65.0% of smectite labelled amount, trioxygen-containingization two aluminium (Al
2O
3) should be 12.0%～25.0% of smectite labelled amount." smectite maybe with become ore deposit parent rock and the association of transition type mineral, their silicon dioxide, alundum (Al content maybe be identical with smectite.The parent rock condition that forms bentonite ore is not strict, and the various rocks of being made up of aluminium silicate mineral all can be converted into smectite (bentonitic clay) under suitable geologic agent condition, and existing a host of facts prove, under advantageous conditions, all can be converted into smectite.So, smectite maybe with become ore deposit parent rock and the association of transition type mineral, their silicon dioxide, alundum (Al content maybe be identical.The mineral of smectite and association all contain silicon dioxide, alundum (Al, and comprehensive silicon dioxide, the alundum (Al content of multiple associated mineral impurity maybe be identical with smectite.So the content of chemical examination silicon dioxide, alundum (Al can have the kind of controlling impurity, and complex operation, cause unnecessary a large amount of manpower and materials wastes.
In the existing medicinal smectite quality standard with the absorption affinity of sulfuric acid strychnine mensuration smectite; Existing public reported; The water-insoluble magnesium class mineral of association in the smectite can obviously influence the mensuration of smectite absorption affinity, and absorption affinity is closely related with the curative effect of smectite again; So the kind that detects its contained mineral is very necessary.
Prior art judges that smectite content mainly is the blue amount method of inhaling, and adopts profit around-France usually owing to inhale the test of blue amount, judges titration end-point through naked eyes, causes error easily; Inhaling blue amount method is the ion-exchange absorption that utilizes smectite; Measure the blue amount of methylene first of exchangeable ion exchange; No matter the smectite ion exchange capacity that is different regions or areal all has than big-difference, so, very inaccurate with the impurity content of inhaling blue amount method judgement smectite.
The method of prior art purifying montmorillonite is a lot; What purifying montmorillonite was paid close attention to is the purity of smectite; The inspection method of the kind of contained mineral and content thereof is made and being described and test in the residue of Shang Weiyou after to purifying montmorillonite; It can not make summary targetedly to the kind and the content thereof of contained mineral in the smectite, and the residue behind the purifying montmorillonite also contains smectite, can not be used for the assay of smectite impurity.
Patent of invention (2012100166760) discloses the detection method of asbestos in the smectite; But the kind of contained mineral in the smectite and the inspection method of content thereof are not made description and test; Detect the method for asbestos; The purpose that reaches enrichment impurity is just passable, and smectite is fully separated with impurity, can not be used for assay.The impurity of enrichment also contains smectite, and the discriminating that is used for dopant species also has interference.
Prior art does not have accurately to detect the method for smectite impurity content, can't confirm the purity of purifying montmorillonite yet.
Summary of the invention
The objective of the invention is, the detection method of a kind of medicinal smectite impurity content and kind thereof is provided, maintain strict control over the drug quality pass, to guarantee its curative effect and security.
The objective of the invention is to realize like this detection method of a kind of medicinal smectite impurity content and/or kind: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed the content of calculating impurity with smectite after the drying; Get impurity make the powder crystal X ray diffracting spectrum, according to the characteristic peak of X-ray diffraction, judge the mineral species that exists in the sample; A kind of method in polarized light microscopic method, phase microscope method, ESEM method or the transmission electron microscope method is confirmed the crystal habit of impurity.
A kind of medicinal smectite impurity content that the present invention is above-mentioned and/or the detection method of kind: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity make the powder crystal X ray diffracting spectrum, according to the characteristic peak of X-ray diffraction, judge the mineral species that exists in the sample.
A kind of medicinal smectite impurity content that the present invention is above-mentioned and/or the detection method of kind: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity, drying is with the crystal habit of a kind of method affirmation impurity in polarized light microscopic method, phase microscope method, ESEM method or the transmission electron microscope method.
A kind of medicinal smectite impurity content that the present invention is above-mentioned and/or the detection method of kind: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity, 450 ℃ of dryings 1 hour are confirmed the crystal habit of impurity with a kind of method in polarized light microscopic method, phase microscope method, ESEM method or the transmission electron microscope method.
A kind of medicinal smectite impurity content that the present invention is above-mentioned and/or the detection method of kind: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity.
The separated form water method that the present invention is above-mentioned is to be that fully to separate smectite be that medium is aided with other physics, chemical method and fully separates smectite and impurity with impurity or with water to medium with water.
The heavy liquid separation method that the present invention is above-mentioned is to get the smectite sample, puts in the container, adds the light liquid of preparation heavy-fluid, after the placement; Centrifugal, abandoning supernatant moves in the heavy-fluid, fully disperses, and is centrifugal; Wash repeatedly with heavy-fluid, wash repeatedly with the light liquid of preparation heavy-fluid, wash repeatedly, drying promptly gets impurity.
The heavy liquid separation method that the present invention is above-mentioned is to get the smectite sample, puts in the container, adds the light liquid of preparation heavy-fluid; After fully disperseing, centrifugal, abandoning supernatant moves in the heavy-fluid of proportion between smectite and impurity; Fully stir, centrifugal, wash impurity with heavy-fluid, wash impurity with the light liquid of preparation heavy-fluid again; Wash impurity again, drying promptly gets impurity.
A kind of medicinal smectite impurity content that the present invention is above-mentioned and/or the detection method of kind are to get the smectite preparation, first water flush away auxiliary material, checked for impurities content and/or kind again.
A kind of medicinal smectite impurity content that the present invention is above-mentioned and/or the detection method of kind are to get the smectite preparation, directly checked for impurities content and/or kind.
The above-mentioned separated form water method of the present invention includes but not limited to following method:
Take by weighing smectite, put in the container, add the water of 10-50 times of weight, fully mixing; After the dispersion, leave standstill more than 8 hours, discard top suspending liquid, sediment; The water that adds 10-50 times of weight again, fully mixing after the dispersion, leaves standstill more than 8 hours; Discard top suspending liquid, repeated multiple times, until the upper liquid clarification, sediment promptly is an impurity.
Take by weighing smectite, put in the container, add the water of 10-50 times of weight, fully mixing adds spreading agent; After fully disperseing, leave standstill more than 8 hours, discard top suspending liquid, sediment adds the water of 10-50 times of weight again; Fully mixing adds spreading agent, after fully disperseing, leaves standstill more than 8 hours; Discard top suspending liquid, repeated multiple times, until the upper liquid clarification, sediment promptly is an impurity.
Take by weighing smectite, put in the container, add the water of 10-50 times of weight, abundant mixing, the spreading agent of the 0.3%-1.5% of adding smectite sample weight; Fully mixing left standstill more than 8 hours, discarded top suspending liquid, and sediment adds smectite sample weight 10-30 water doubly again; The spreading agent that adds the 0.3%-1.5% of smectite sample weight after fully disperseing, leaves standstill more than 8 hours, discards top suspending liquid; Repeated multiple times, until the upper liquid clarification, sediment is dry below 450 ℃, promptly gets impurity.
Take by weighing smectite, put in the container, add the aqueous dispersant of 10-50 times of weight, fully mixing; Leave standstill more than 8 hours, discard top suspending liquid, sediment adds the aqueous dispersant of 10-50 times of weight again; Fully mixing left standstill more than 8 hours, discarded top suspending liquid; Repeated multiple times, until the upper liquid clarification, sediment promptly is an impurity.
Take by weighing the smectite of 105 ℃ of dry constant weights, put in the container, add the aqueous dispersant of the 0.3%-1% of 10-50 times of weight, ultrasonic dispersing 10-30 minute; Leave standstill more than 8 hours, discard top suspending liquid, sediment adds 0.3% aqueous dispersant of 10-30 times of weight again; Ultrasonic dispersing 10-30 minute, leave standstill more than 8 hours, discard top suspending liquid; Repeat once, sediment i.e. 105 ℃ of dry constant weights, promptly get impurity again.
Take by weighing the smectite of 105 ℃ of dry constant weights, add 10-50 0.5%-3% magnesium salt solution doubly, ultrasonic dispersing 10-30 minute, leave standstill more than 8 hours; Discard top suspending liquid, sediment adds the 10-30 0.5%-3% WS doubly again; Ultrasonic dispersing 10-30 minute, leave standstill more than 8 hours, discard top suspending liquid; Repeat once, 105 ℃ of dry constant weights of sediment promptly get impurity again.
Take by weighing the smectite of 105 ℃ of dry constant weights, add 10-50 times of water, add sodium carbonate and magnesium oxide again, make sodium carbonate to 1% one 2% of liquid weight; Magnesium oxide left standstill more than 8 hours by 0.8% 1 1%, ultrasonic dispersing 10-30 minute of liquid weight, discarded top suspending liquid; Add sodium carbonate and magnesium oxide again, make the 1%-2% of sodium carbonate to liquid weight, magnesium oxide is to the 0.8%-1% of liquid weight, ultrasonic dispersing 10-30 minute; Leave standstill more than 8 hours, discard top suspending liquid, repeated multiple times; Until the upper liquid clarification, 105 ℃ of dry constant weights of sediment promptly get impurity.
Take by weighing the smectite of 105 ℃ of dry constant weights; Put in the container, add the aqueous dispersant of the 0.3%-1% of 10-50 times of weight, ultrasonic dispersing 10-30 minute; Be put into electricity ice groove again and carry out electrophoresis; The smectite that has load is flocked on the anode separates with other impurity, 105 ℃ of dry constant weights of impurity promptly get impurity.
Take by weighing smectite, dry constant weight is soaked in water, and is centrifugal, and abandoning supernatant gets the water logging smectite; With the WS of highdensity cadmium iodide and barium iodide, put in the container, add water and also stir, the water logging smectite can keep the state that freely suspends when static to liquid, must cadmium iodide and barium iodide heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes repeatedly with cadmium iodide and barium iodide heavy-fluid, washes repeatedly again, and dry constant weight promptly gets impurity.
Take by weighing the smectite of 105 ℃ of dry constant weights, be soaked in water, centrifugal, abandoning supernatant gets the water logging smectite; With the WS of highdensity cadmium iodide and barium iodide, put in the container, add water and also stir, the water logging smectite can keep the state that freely suspends when static to liquid, must cadmium iodide and barium iodide heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, and with washing repeatedly, 105 ℃ of dry constant weights promptly get impurity.
With the WS of highdensity cadmium iodide and barium iodide, to put in the container, interpolation water also stirs; Smectite can keep the state that freely suspends when static to liquid, adds the smectite sample, fully mixing; Put into Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment promptly is an impurity; With washing repeatedly, be dried to constant weight, promptly get impurity.
Take by weighing smectite, add water and stir, process suspended matter, ultrasonic dispersing 10-30 minute; Adding density is the cadmium iodide of 3.10 g/ml and the WS of barium iodide, and the limit edged stirs, and smectite can keep the state that freely suspends when static to liquid, in the immigration Centrifuge Cup; 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid; Wash 3 times, dry 105 ℃ are dried to constant weight, promptly get impurity again.
Get the smectite sample, add water and smectite is fully expanded and disperse, centrifugal, abandoning supernatant, the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and many sodium tungstates are dissolved fully, add to liquid when static the water logging smectite can keep the state that freely suspends, must heavy-fluid; The water logging smectite is put into heavy-fluid, fully stir, move in the Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment is washed 3 times with heavy-fluid, washes 3 times again, and drying promptly gets impurity.
Get the smectite sample, add water and stir, add spreading agent, process suspended matter, ultrasonic dispersing 10-30 minute, centrifugal, abandoning supernatant got the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and many sodium tungstates are dissolved fully, add to liquid when static the water logging smectite can keep the state that freely suspends, must heavy-fluid; The water logging smectite is put into heavy-fluid, fully stir, move in the Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid, washes 3 times again, and drying promptly gets impurity.
Get the smectite sample, add water and stir, process suspended matter, placed 10-30 minute, centrifugal, abandoning supernatant gets the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and the water logging smectite can keep the state that freely suspends when many sodium tungstates being dissolved fully add to liquid static, must heavy-fluid; The water logging smectite is put into heavy-fluid, ultrasonic dispersing 10-30 minute, move in the Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid, and with washing 3 times, drying promptly gets impurity again.
Get the smectite sample, add the aqueous dispersant of the 0.3%-1% of 10-50 times of weight, process suspended matter, ultrasonic dispersing 10-30 minute, centrifugal, abandoning supernatant got the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and the water logging smectite begins come-up when many sodium tungstates being dissolved fully add to liquid static, heavy-fluid; The water logging smectite is put into heavy-fluid, ultrasonic dispersing 10-30 minute, move in the Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid, and with washing 3 times, drying promptly gets impurity again.
Get the smectite sample, add water and stir, ultrasonic dispersing 10-30 minute, bit by bit add many sodium tungstates again; The limit edged stirs, and smectite begins come-up when many sodium tungstates being dissolved fully add to liquid static, moves in the Centrifuge Cup; 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid; With washing 3 times, drying promptly gets impurity again.
The above-mentioned spreading agent of the present invention has sodium hexametaphosphate, water glass, sodium pyrophosphate, sodium phosphate, soda mint, sodium carbonate, ammonium hydroxide, acrylic acid etc. multiple.Magnesium salts, magnesium oxide, sodium carbonate
The above-mentioned heavy liquid separation method of the present invention includes but not limited to following method:
Take by weighing smectite, put in the container, add the light liquid of preparation heavy-fluid, after fully disperseing, centrifugal; Abandoning supernatant moves in the heavy-fluid, fully stirs, and centrifugal, sediment is washed 3 times with heavy-fluid; Wash 3 times with the light liquid of preparation heavy-fluid, wash 3 times again, dry constant weight below 450 ℃ promptly gets impurity.
Get the smectite sample, put in the airtight container, add absolute ethyl alcohol, placed 30 minutes; Centrifugal, abandoning supernatant moves in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.85-1.95 powerful jolting; Centrifugal, sediment promptly is an impurity, with absolute ethanol washing 3 times; 105 ℃ of dry constant weights, drying promptly gets impurity.
Take by weighing smectite, add in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.85-1.95, powerful jolting, centrifugal, sediment promptly is an impurity, with bromine virtue absolute ethyl alcohol heavy-fluid washing 3 times, uses absolute ethanol washing again 3 times, 105 ℃ of dry constant weights promptly get impurity.
Take by weighing smectite, put in the airtight container, add absolute ethyl alcohol, ultrasonic dispersing 10-30 minute; Placed 30 minutes, centrifugal, abandoning supernatant moves in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.85-1.95; Powerful jolting, centrifugal, sediment promptly is an impurity, washes 3 times with bromine virtue absolute ethyl alcohol heavy-fluid; Use absolute ethanol washing again 3 times, wash 3 times again, 105 ℃ of dry constant weights promptly get impurity.
Take by weighing smectite, add absolute ethyl alcohol, ultrasonic dispersing 10-30 minute, add the bromine virtue while stirring, smectite begins come-up when static to liquid, abundant mixing, centrifugal, sediment promptly is an impurity, washes 3 times with absolute ethyl alcohol, 105 ℃ of dry constant weights promptly get impurity.
Take by weighing smectite, put in the airtight container, add absolute ethyl alcohol, ultrasonic dispersing 10-30 minute while stirring; Centrifugal, abandoning supernatant moves in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.85-1.95 ultrasonic dispersing 10-30 minute while stirring; Centrifugal, sediment promptly is an impurity, washes 3 times with bromine virtue absolute ethyl alcohol heavy-fluid, uses absolute ethanol washing again 3 times; Wash 3 times, 105 ℃ of dry constant weights promptly get impurity again.
Take by weighing smectite, placing percentage by weight is the n-octyl amine WS of 10-30%, fully stirs, and places 0.5 hour; Centrifugal, abandoning supernatant adds phenixin, fully disperses; 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes repeatedly with phenixin; Wash repeatedly with absolute ethyl alcohol, 105 ℃ of dry constant weights promptly get impurity again.
Take by weighing smectite, placing percentage by weight is 20% the n-octyl amine WS, fully stirs ultrasonic dispersing 10-30 minute; Centrifugal, abandoning supernatant adds phenixin, fully disperses; 3000-5000 r/min is centrifugal, and sediment is with promptly being impurity, and phenixin is washed 3 times; Wash 3 times with absolute ethyl alcohol, 105 ℃ of dry constant weights promptly get impurity again.
Take by weighing smectite, placing percentage by weight is 20% the n-octyl amine WS, fully stirs; Centrifugal, abandoning supernatant adds phenixin; Ultrasonic dispersing 10-30 minute, 3000-5000 r/min was centrifugal, and sediment is washed 3 times with phenixin; Wash 3 times with absolute ethyl alcohol, 105 ℃ of dry constant weights promptly get impurity again.
Take by weighing smectite, placing percentage by weight is 20% the n-octyl amine WS, ultrasonic dispersing 10-30 minute, centrifugal; Abandoning supernatant adds phenixin, ultrasonic dispersing 10-30 minute; 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with phenixin; Wash 3 times with absolute ethyl alcohol, 105 ℃ of dry constant weights promptly get impurity again.
Pour bromoform stoste into container, put the smectite sample into, slowly drip the dimethyl formamide thinning agent; Fully stir, stop ultrasonic dispersing 10-30 minute when the part mineral begin to sink when liquid is static immediately; Sediment promptly is an impurity; Wash 3 times with ethanol, be dried to constant weight, promptly get impurity.
The present invention confirms dopant species with the powder crystal X-ray diffraction method, must understand the standard x-ray diffraction data of mineral, and the X-ray diffraction characteristic of relevant mineral can be from international powder crystal X-ray diffraction card retrieval.
Smectite under the present invention fully separates with impurity, is through X-x ray diffraction atlas analysis, does not contain the smectite characteristic peak in the impurity, peak free from foreign meter in the smectite.
The invention provides the method for a kind of abundant separation smectite and impurity, can accurately record the content of impurity in the smectite, solved the technical matters that impurity content in the present medicinal smectite does not have assay method.Improved the quality controllability of medicinal smectite.
The present invention fully separates smectite with impurity, weighs after the drying, calculates the content of impurity, and method is simple, can accurately record the content of impurity in the smectite, has solved the inaccurate technical matters of impurity content inspection method in the present smectite.Improved the quality controllability of medicinal smectite.
Further specify of the present invention substantive progressive below through Test Example.
1, the medicinal smectite of getting two producers of first, second is made X-ray diffracting spectrum; " characteristic spectral line of smectite is in about 1.5nm and 0.45nm wavelength, and other impurity absorption peak strength all are not higher than second characteristic peak (about 0.45nm) of smectite in the collection of illustrative plates for the result." meet medicinal standard.
2, get the medicinal smectite of two producers of first, second respectively, 105 ℃ are dried to constant weight, get the sample 10g after the dry constant weight respectively, put in the container; The water that adds 300ml, abundant mixing, the sodium pyrophosphate of adding 0.03g, fully mixing; Leave standstill more than 8 hours, discard top suspending liquid, sediment adds the water of smectite 100ml again; The sodium pyrophosphate that adds 0.03g, ultrasonic dispersing 10 minutes, placement is spent the night, and discards top suspending liquid; Repeated multiple times, until the upper liquid clarification, sediment moves in the evaporating dish of 105 ℃ of dry constant weights, after 80 ℃ of dryings; 105 ℃ are dried to constant weight, and the medicinal smectite impurity content that calculates first producer is 25.3%, and the medicinal smectite impurity content of second producer is 4.5%.
3, take the impurity and the smectite of the medicinal smectite separation of two producers of first, second respectively, make X-ray diffracting spectrum, the impurity that the medicinal smectite of two producers of result separates does not all show the characteristic spectral line of smectite; The smectite X-ray diffracting spectrum that the medicinal smectite of two producers separates does not have other impurity peaks except that the characteristic spectral line of smectite.Explain that this method can make smectite fully separate with impurity, this method can be used for the dirt content test of smectite.
Through international powder crystal X-ray diffraction card retrieval, the medicinal smectite impurity of first producer mainly contains smalite, and the medicinal smectite impurity of second producer mainly contains quartz.
Embodiment
Get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity make the powder crystal X ray diffracting spectrum, according to the characteristic peak of X-ray diffraction, judge the mineral species that exists in the sample; A kind of method in polarized light microscopic method, phase microscope method, ESEM method or the transmission electron microscope method is confirmed the crystal habit of impurity.
Get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity make the powder crystal X ray diffracting spectrum, according to the characteristic peak of X-ray diffraction, judge the mineral species that exists in the sample.
Get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity, drying is with the crystal habit of a kind of method affirmation impurity in polarized light microscopic method, phase microscope method, ESEM method or the transmission electron microscope method.
Get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity, 450 ℃ of dryings 1 hour are confirmed the crystal habit of impurity with a kind of method in polarized light microscopic method, phase microscope method, ESEM method or the transmission electron microscope method.
Get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity.
The separated form water method is to be that medium is aided with other physics, chemical method and fully separates smectite and impurity with water.
Heavy liquid separation method is to get the smectite sample, puts in the container, adds the light liquid of preparation heavy-fluid, after the placement; Centrifugal, abandoning supernatant moves in the heavy-fluid, fully disperses, and is centrifugal; Wash repeatedly with heavy-fluid, wash repeatedly with the light liquid of preparation heavy-fluid, wash repeatedly, drying promptly gets impurity.
Heavy liquid separation method is to get the smectite sample, puts in the container, adds the light liquid of preparation heavy-fluid, after fully disperseing; Centrifugal, abandoning supernatant moves in the heavy-fluid, fully stirs, and is centrifugal; Wash 3 times with heavy-fluid, wash 3 times with the light liquid of preparation heavy-fluid, wash 3 times again, 450 ℃ of dryings 1 hour promptly get impurity.
Get the smectite preparation, first water flush away auxiliary material, checked for impurities content and kind thereof again.
Get the smectite preparation, directly checked for impurities content and kind thereof.
Take by weighing smectite, put in the container, add the water of 10-50 times of weight, fully mixing; After the dispersion, leave standstill more than 8 hours, discard top suspending liquid, sediment; The water that adds 10-50 times of weight again, fully mixing after the dispersion, leaves standstill more than 8 hours; Discard top suspending liquid, repeated multiple times, until the upper liquid clarification, sediment promptly is an impurity.
Take by weighing smectite, put in the container, add the water of 10-50 times of weight, fully mixing adds spreading agent; After fully disperseing, leave standstill more than 8 hours, discard top suspending liquid, sediment adds the water of 10-50 times of weight again; Fully mixing adds spreading agent, after fully disperseing, leaves standstill more than 8 hours; Discard top suspending liquid, repeated multiple times, until the upper liquid clarification, sediment promptly is an impurity.
Take by weighing smectite, put in the container, add the water of 10-50 times of weight, abundant mixing, the spreading agent of the 0.3%-1.5% of adding smectite sample weight; Fully mixing left standstill more than 8 hours, discarded top suspending liquid, and sediment adds smectite sample weight 10-30 water doubly again; The spreading agent that adds the 0.3%-1.5% of smectite sample weight after fully disperseing, leaves standstill more than 8 hours, discards top suspending liquid; Repeated multiple times, until the upper liquid clarification, sediment is dry below 450 ℃, promptly gets impurity.
Take by weighing smectite, put in the container, add the aqueous dispersant of 10-50 times of weight, fully mixing; Leave standstill more than 8 hours, discard top suspending liquid, sediment adds the aqueous dispersant of 10-50 times of weight again; Fully mixing left standstill more than 8 hours, discarded top suspending liquid; Repeated multiple times, until the upper liquid clarification, sediment promptly is an impurity.
Take by weighing the smectite of 105 ℃ of dry constant weights, put in the container, add the aqueous dispersant of the 0.3%-1% of 10-50 times of weight, ultrasonic dispersing 10-30 minute; Leave standstill more than 8 hours, discard top suspending liquid, sediment adds 0.3% aqueous dispersant of 10-30 times of weight again; Ultrasonic dispersing 10-30 minute, leave standstill more than 8 hours, discard top suspending liquid; Repeat once, sediment i.e. 105 ℃ of dry constant weights, promptly get impurity again.
Take by weighing the smectite of 105 ℃ of dry constant weights, add 10-50 0.5%-3% magnesium salt solution doubly, ultrasonic dispersing 10-30 minute, leave standstill more than 8 hours; Discard top suspending liquid, sediment adds the 10-30 0.5%-3% WS doubly again; Ultrasonic dispersing 10-30 minute, leave standstill more than 8 hours, discard top suspending liquid; Repeat once, 105 ℃ of dry constant weights of sediment promptly get impurity again.
Take by weighing the smectite of 105 ℃ of dry constant weights, add 10-50 times of water, add sodium carbonate and magnesium oxide again, make sodium carbonate to 1% one 2% of liquid weight; Magnesium oxide left standstill more than 8 hours by 0.8% 1 1%, ultrasonic dispersing 10-30 minute of liquid weight, discarded top suspending liquid; Add sodium carbonate and magnesium oxide again, make the 1%-2% of sodium carbonate to liquid weight, magnesium oxide is to the 0.8%-1% of liquid weight, ultrasonic dispersing 10-30 minute; Leave standstill more than 8 hours, discard top suspending liquid, repeated multiple times; Until the upper liquid clarification, 105 ℃ of dry constant weights of sediment promptly get impurity.
Take by weighing the smectite of 105 ℃ of dry constant weights; Put in the container, add the aqueous dispersant of the 0.3%-1% of 10-50 times of weight, ultrasonic dispersing 10-30 minute; Be put into electricity ice groove again and carry out electrophoresis; The smectite that has load is flocked on the anode separates with other impurity, 105 ℃ of dry constant weights of impurity promptly get impurity.
Take by weighing smectite, dry constant weight is soaked in water, and is centrifugal, and abandoning supernatant gets the water logging smectite; With the WS of highdensity cadmium iodide and barium iodide, put in the container, add water and also stir, the water logging smectite can keep the state that freely suspends when static to liquid, must cadmium iodide and barium iodide heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes repeatedly with cadmium iodide and barium iodide heavy-fluid, washes repeatedly again, and dry constant weight promptly gets impurity.
Take by weighing the smectite of 105 ℃ of dry constant weights, be soaked in water, centrifugal, abandoning supernatant gets the water logging smectite; With the WS of highdensity cadmium iodide and barium iodide, put in the container, add water and also stir, the water logging smectite can keep the state that freely suspends when static to liquid, must cadmium iodide and barium iodide heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, and with washing repeatedly, 105 ℃ of dry constant weights promptly get impurity.
With the WS of highdensity cadmium iodide and barium iodide, to put in the container, interpolation water also stirs; Smectite can keep the state that freely suspends when static to liquid, adds the smectite sample, fully mixing; Put into Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment promptly is an impurity; With washing repeatedly, be dried to constant weight, promptly get impurity.
Take by weighing smectite, add water and stir, process suspended matter, ultrasonic dispersing 10-30 minute; Adding density is the cadmium iodide of 3.10 g/ml and the WS of barium iodide, and the limit edged stirs, and smectite can keep the state that freely suspends when static to liquid, in the immigration Centrifuge Cup; 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid; Wash 3 times, dry 105 ℃ are dried to constant weight, promptly get impurity again.
Get the smectite sample, add water and smectite is fully expanded and disperse, centrifugal, abandoning supernatant, the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and many sodium tungstates are dissolved fully, add to liquid when static the water logging smectite can keep the state that freely suspends, must heavy-fluid; The water logging smectite is put into heavy-fluid, fully stir, move in the Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment is washed 3 times with heavy-fluid, washes 3 times again, and drying promptly gets impurity.
Get the smectite sample, add water and stir, process suspended matter, ultrasonic dispersing 10-30 minute, centrifugal, abandoning supernatant got the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and many sodium tungstates are dissolved fully, add to liquid when static the water logging smectite can keep the state that freely suspends, must heavy-fluid; The water logging smectite is put into heavy-fluid, fully stir, move in the Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid, washes 3 times again, and drying promptly gets impurity.
Get the smectite sample, add water and stir, process suspended matter, placed 10-30 minute, centrifugal, abandoning supernatant gets the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and the water logging smectite can keep the state that freely suspends when many sodium tungstates being dissolved fully add to liquid static, must heavy-fluid; The water logging smectite is put into heavy-fluid, ultrasonic dispersing 10-30 minute, move in the Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid, and with washing 3 times, drying promptly gets impurity again.
Get the smectite sample, add the aqueous dispersant of the 0.3%-1% of 10-50 times of weight, process suspended matter, ultrasonic dispersing 10-30 minute, centrifugal, abandoning supernatant got the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and the water logging smectite begins come-up when many sodium tungstates being dissolved fully add to liquid static, heavy-fluid; The water logging smectite is put into heavy-fluid, ultrasonic dispersing 10-30 minute, move in the Centrifuge Cup, 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid, and with washing 3 times, drying promptly gets impurity again.
Get the smectite sample, add water and stir, ultrasonic dispersing 10-30 minute, bit by bit add many sodium tungstates again; The limit edged stirs, and smectite begins come-up when many sodium tungstates being dissolved fully add to liquid static, moves in the Centrifuge Cup; 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with heavy-fluid; With washing 3 times, drying promptly gets impurity again.
The above-mentioned spreading agent of the present invention has sodium hexametaphosphate, water glass, sodium pyrophosphate, sodium phosphate, soda mint, sodium carbonate, ammonium hydroxide, acrylic acid etc. multiple.Magnesium salts, magnesium oxide, sodium carbonate
Take by weighing smectite, put in the container, add the light liquid of preparation heavy-fluid, after fully disperseing, centrifugal; Abandoning supernatant moves in the heavy-fluid, fully stirs, and centrifugal, sediment is washed 3 times with heavy-fluid; Wash 3 times with the light liquid of preparation heavy-fluid, wash 3 times again, dry constant weight below 450 ℃ promptly gets impurity.
Get the smectite sample of 105 ℃ of dry constant weights, put in the airtight container, add absolute ethyl alcohol, placed 30 minutes; Centrifugal, abandoning supernatant moves in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.85-1.95 powerful jolting; Centrifugal, sediment promptly is an impurity, with absolute ethanol washing 3 times; 105 ℃ of dry constant weights, drying promptly gets impurity.
Take by weighing smectite, add in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.85-1.95, powerful jolting, centrifugal, sediment promptly is an impurity, with bromine virtue absolute ethyl alcohol heavy-fluid washing 3 times, uses absolute ethanol washing again 3 times, 105 ℃ of dry constant weights promptly get impurity.
Take by weighing smectite, put in the airtight container, add absolute ethyl alcohol, ultrasonic dispersing 10-30 minute; Placed 30 minutes, centrifugal, abandoning supernatant moves in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.85-1.95; Powerful jolting, centrifugal, sediment promptly is an impurity, washes 3 times with bromine virtue absolute ethyl alcohol heavy-fluid; Use absolute ethanol washing again 3 times, wash 3 times again, 105 ℃ of dry constant weights promptly get impurity.
Take by weighing smectite, add absolute ethyl alcohol, ultrasonic dispersing 10-30 minute, add the bromine virtue while stirring, smectite begins come-up when static to liquid, abundant mixing, centrifugal, sediment promptly is an impurity, washes 3 times with absolute ethyl alcohol, 105 ℃ of dry constant weights promptly get impurity.
Take by weighing the smectite of 105 ℃ of dry constant weights, put in the airtight container, add absolute ethyl alcohol, ultrasonic dispersing 10-30 minute while stirring; Centrifugal, abandoning supernatant moves in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.85-1.95 ultrasonic dispersing 10-30 minute while stirring; Centrifugal, sediment promptly is an impurity, washes 3 times with bromine virtue absolute ethyl alcohol heavy-fluid, uses absolute ethanol washing again 3 times; Wash 3 times, 105 ℃ of dry constant weights promptly get impurity again.
Take by weighing the smectite of 105 ℃ of dry constant weights, placing percentage by weight is the n-octyl amine WS of 10-30%, fully stirs, and places 0.5 hour; Centrifugal, abandoning supernatant adds phenixin, fully disperses; 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes repeatedly with phenixin; Wash repeatedly with absolute ethyl alcohol, 105 ℃ of dry constant weights promptly get impurity again.
Take by weighing the smectite of 105 ℃ of dry constant weights, placing percentage by weight is 20% the n-octyl amine WS, fully stirs ultrasonic dispersing 10-30 minute; Centrifugal, abandoning supernatant adds phenixin, fully disperses; 3000-5000 r/min is centrifugal, and sediment is with promptly being impurity, and phenixin is washed 3 times; Wash 3 times with absolute ethyl alcohol, 105 ℃ of dry constant weights promptly get impurity again.
Take by weighing smectite, placing percentage by weight is 20% the n-octyl amine WS, fully stirs; Centrifugal, abandoning supernatant adds phenixin; Ultrasonic dispersing 10-30 minute, 3000-5000 r/min was centrifugal, and sediment is washed 3 times with phenixin; Wash 3 times with absolute ethyl alcohol, drying promptly gets impurity again.
Take by weighing smectite, placing percentage by weight is 20% the n-octyl amine WS, ultrasonic dispersing 10-30 minute, centrifugal; Abandoning supernatant adds phenixin, ultrasonic dispersing 10-30 minute; 3000-5000 r/min is centrifugal, and sediment promptly is an impurity, washes 3 times with phenixin; Wash 3 times with absolute ethyl alcohol, drying promptly gets impurity again.
Pour bromoform stoste into container, put the smectite sample into, slowly drip the dimethyl formamide thinning agent; Fully stir, stop ultrasonic dispersing 10-30 minute when the part mineral begin to sink when liquid is static immediately; Sediment promptly is an impurity; Wash 3 times with ethanol, be dried to constant weight, promptly get impurity.
The present invention confirms dopant species with the powder crystal X-ray diffraction method, must understand the standard x-ray diffraction data of mineral, and the X-ray diffraction characteristic of relevant mineral can be from international powder crystal X-ray diffraction card retrieval.
The invention provides the method for a kind of abundant separation smectite and impurity, can accurately record the content of impurity in the smectite, solved the technical matters that impurity content in the present medicinal smectite does not have assay method.Improved the quality controllability of medicinal smectite
The present invention fully separates smectite with impurity, weighs after the drying, calculates the content of impurity, can accurately record the content of impurity in the smectite, has solved the inaccurate technical matters of impurity content inspection method in the present smectite.Improved the quality controllability of medicinal smectite.
Further specify the present invention below by way of example.
Embodiment 1
Be to get smectite sample 2 grams, put in the container, add the water of 10ml, fully stir, add the sodium hexametaphosphate of 0.006mg; Powerful jolting 30 minutes was left standstill 12 hours, discarded top suspending liquid, and sediment adds the water of 60ml again; Fully stir, add the water glass of 0.01g, powerful jolting 20 minutes was left standstill 8 hours, discarded top suspending liquid; Repeat again once, sediment, dry constant weight, the percentage by weight that calculates impurity is 6%.
Got 450 ℃ of dryings of impurity 1 hour, and made the powder crystal X ray diffracting spectrum, according to the characteristic peak analysis of X-ray diffraction, this sample impurity mainly is quartzy and contains little hydrogen magnesium oxide and micro-asbestos.Polarized light microscopic method is observed and is found to have fibrous crystal.
Embodiment 2
Be to get smectite sample 10 grams, put in the container, add the water of 500 gram weight, fully stir, add the water glass of 0.03 gram; 5000 rev/mins were stirred 10 minutes, left standstill 24 hours, discarded top suspending liquid, and sediment adds the water of 200 grams again; Fully stir, add 0.05 water glass, 3000 rev/mins were stirred 20 minutes, left standstill 8 hours, discarded top suspending liquid; Repeat once again, wash 3 times, drying is weighed, and the percentage by weight that calculates impurity is 10%.
Get impurity make the powder crystal X ray diffracting spectrum, according to the characteristic peak analysis of X-ray diffraction, this sample impurity mainly is cristobalite, attapulgite and smalite.The phase microscope method is observed and is found have fibrous and the crystallization of books shape.
Embodiment 3
Get smectite sample 5 gram, put in the container, add the water of 150ml, fully stir, add 1% sodium pyrophosphate of smectite sample weight; Powerful jolting 40 minutes was left standstill 12 hours, discarded top suspending liquid, and sediment adds the sodium pyrophosphate WS of 150ml0.03% again; Powerful jolting 40 minutes was left standstill 10 hours, discarded top suspending liquid, repeated once again; Sediment, 450 ℃ of dryings 1 hour are weighed, and the percentage by weight that calculates impurity is 15.5%.
Get impurity make the powder crystal X ray diffracting spectrum, according to the characteristic peak analysis of X-ray diffraction, this sample impurity mainly is zeolite, illite and and micro-sepiolite.The ESEM method is observed and is found to have bar-shaped, cellular and flaky crystal.
Embodiment 4
Get smectite sample 0.5 gram, put in the container, add the water of 40 times of weight, fully stir, add 1.5% sodium phosphate of smectite sample weight; Ultrasonic dispersing 15 minutes left standstill 1 day, discarded top suspending liquid, sediment; 0.1% the sodium phosphate aqueous solution that adds 25 times of weight of smectite sample weight again, 5000 rev/mins were stirred 10 minutes, left standstill 1 day, discarded top suspending liquid; Repeat again once, sediment, 105 ℃ are dried to constant weight, and the percentage by weight that calculates impurity is 10.3%.
Get impurity and make to show in powder crystal X ray diffracting spectrum, the collection of illustrative plates kaolinic characteristic peak.
Embodiment 5
Get smectite and be dried to constant weight for 105 ℃, take by weighing 0.2 gram, put in the airtight container, add absolute ethyl alcohol; Ultrasonic dispersing 20 minutes was placed 30 minutes, and is centrifugal, abandoning supernatant; Move in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.85, fully stir, centrifugal, sediment is with absolute ethanol washing 3 times; Wash again 3 times, 105 ℃ of dry constant weights, the percentage by weight that calculates impurity is 5.5%.
Get impurity and make to show in powder crystal X ray diffracting spectrum, the collection of illustrative plates characteristic peak of chlorite.
Embodiment 6
Get smectite and be dried to constant weight for 105 ℃, take by weighing 1 gram, put in the airtight container, add absolute ethyl alcohol; Powerful jolting 30 minutes was placed 100 minutes, and is centrifugal, abandoning supernatant; Move in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.95, fully stir, ultrasonic dispersing 20 minutes, centrifugal; Sediment is washed 3 times with absolute ethanol washing 3 times again, and 105 ℃ are dried to constant weight, and the percentage by weight that calculates impurity is 5.5%.
Get impurity do in powder crystal X ray diffracting spectrum, the collection of illustrative plates to show quartzy, cristobalite and malthacite, characteristic peak.
Embodiment 7
Get smectite 3 grams, put in the airtight container, add absolute ethyl alcohol, electromagnetic agitation 30 minutes; Placed 40 minutes, centrifugal, abandoning supernatant moves in the bromine virtue absolute ethyl alcohol heavy-fluid of proportion 1.90; Fully stir, ultrasonic dispersing 20 minutes, centrifugal, sediment is with absolute ethanol washing 3 times; Wash again 3 times, 105 ℃ of dry constant weights, the percentage by weight that calculates impurity is 5.5%.
Transmission electron microscope method is observed and is found to have acicular crystal.
Embodiment 8
Get smectite sample 0.3 gram, be soaked in water 100 minutes, ultrasonic dispersing 30 minutes was placed 60 minutes, and is centrifugal, discards liquid, gets the water logging smectite; With density is the cadmium iodide of 3.10 g/ml and the WS of barium iodide, puts into tool plug triangular flask, adds water, and the water logging smectite can keep the state that freely suspends when static to liquid, must heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 5000 r/min are centrifugal, discard upper liquid, repeat 2 times again; Sediment washing 3 times, 105 ℃ are dried to constant weight, and the percentage by weight that calculates impurity is 9.2%.
Get impurity make the powder crystal X ray diffracting spectrum, according to the characteristic peak analysis of X-ray diffraction, this sample impurity mainly is talcum, smalite, illite and wollastonite.The ESEM method is observed and is found to have bar-shaped, acicular crystal.
Embodiment 9
Get smectite sample 5 grams, be soaked in water 10 minutes, ultrasonic dispersing 10 minutes was placed 10 minutes, and is centrifugal, discards liquid, gets the water logging smectite; With density is the cadmium iodide of 3.10 g/ml and the WS of barium iodide, puts into tool plug triangular flask, adds water, and the water logging smectite can keep the state that freely suspends when static to liquid, must heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 3000r/min is centrifugal, discards upper liquid, repeats 2 times again; Sediment washing 3 times, drying gets impurity, weighs, and the percentage by weight that calculates impurity is 9.2%.
Embodiment 10
Get smectite and be dried to constant weight for 105 ℃, take by weighing 1 gram, be soaked in water 30 minutes, ultrasonic dispersing 20 minutes was placed 30 minutes, and is centrifugal, discards liquid, gets the water logging smectite; With density is the cadmium iodide of 3.10 g/ml and the WS of barium iodide, puts into tool plug triangular flask, adds water, and the water logging smectite can keep the state that freely suspends when static to liquid, must heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 5000 r/min are centrifugal, discard upper liquid, repeat 2 times again; Sediment washing 3 times, 105 ℃ are dried to constant weight, get impurity, and the percentage by weight that calculates impurity is 5%.
Embodiment 11
Get smectite and be dried to constant weight for 105 ℃, take by weighing 0.2 gram, add 0.6 milligram sodium pyrophosphate, add water and soaked 60 minutes for 5 milliliters, ultrasonic dispersing 25 minutes was placed 50 minutes, and is centrifugal, discards liquid, gets the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and many sodium tungstates is dissolved fully add to liquid water logging smectite when static can keep the state that freely suspends, must heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 5000 r/min are centrifugal, discard upper liquid, repeat 2 times again; Sediment washing 3 times, 105 ℃ are dried to constant weight, get 4.0126 milligrams of impurity.
Embodiment 12
Get smectite and be dried to constant weight for 105 ℃, take by weighing 0.5 gram, be soaked in water 45 minutes, ultrasonic dispersing 20 minutes was placed 40 minutes, and is centrifugal, discards liquid, gets the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and many sodium tungstates is dissolved fully add to liquid water logging smectite when static can keep the state that freely suspends, must heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 3000 r/min are centrifugal, discard upper liquid, repeat 2 times again; Sediment is washed 3 times, and 105 ℃ dry permanent in heavy, gets 25 milligrams of impurity.
Embodiment 13
Get the smectite dispersing tablet, be ground into fine powder, get fine powder 1 gram, be soaked in water 25 minutes, ultrasonic dispersing 30 minutes was placed 40 minutes, and is centrifugal, discards liquid, gets the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and many sodium tungstates is dissolved fully add to liquid water logging smectite when static can keep the state that freely suspends, must heavy-fluid; The water logging smectite is put into heavy-fluid, and fully mixing is put into Centrifuge Cup, and 3000 r/min are centrifugal, discard upper liquid, repeat 2 times again; Sediment washing 3 times, 105 ℃ of dry constant weights, the percentage by weight that calculates the used smectite impurity of smectite dispersing tablet is 5.36%.
Embodiment 14
Get diffusing 1 gram of smectite, wash 3 times, add 30 gram water, ultrasonic dispersing 30 minutes adds the soda mint that accounts for smectite sample weight 0.3%; Powerful jolting 30 minutes was left standstill 24 hours, discarded liquid, and sediment adds the water of 30 times of weight again; Fully stir, add the sodium carbonate that accounts for smectite sample weight 1%, powerful jolting 20 minutes was left standstill 8 hours, discarded top suspending liquid; Repeat again once, sediment washing 3 times, 105 ℃ of dry constant weights, the percentage by weight that calculates impurity is 6%.
Embodiment 15
Get smectite turbid liquor 10ml, add the water of 20 times of amounts, add 0.3 gram ammonium hydroxide, jolting 30 minutes; Left standstill 10 hours, and discarded top suspending liquid, sediment adds 30 ml water again; Fully stir, add 0.3 gram acrylic acid, jolting 20 minutes; Left standstill 8 hours, and discarded top suspending liquid, repeat again once; Sediment washing 3 times, 105 ℃ are dried to constant weight, and the percentage by weight that calculates impurity is 5.1%.
Embodiment 16
Get the smectite sample, put in the container, add the aqueous dispersant of the 0.3%-1% of 50 times of weight; Ultrasonic dispersing 10-30 minute, be put in the electrophoresis tank, smectite is flocked on the anode; Take out, remaining solids is washed 3 times; 105 ℃ are dried to constant weight, and the percentage by weight that calculates impurity is 7.32%.
Embodiment 17
Get the smectite sample, put in the container, add the water of 30 times of weight, fully stir, add 0.3% sodium phosphate of smectite sample weight; Fully stir, leave standstill 10h then, discard top suspending liquid, remaining suspending liquid and sediment; The water that adds 15 times of weight more fully stirs, and adds 0.3% sodium phosphate of smectite sample weight, fully stirs; Be put in the electrophoresis tank, smectite is flocked on the anode, takes out remaining solids; Washing is not to there being phosphate radical, and drying gets impurity, and the percentage by weight that calculates impurity is 6.26%.
Embodiment 18
Get the smectite sample, put in the container, add the water of 25 times of weight, fully stir; Add 1% soda mint of smectite sample weight, fully stir, be put in the electrophoresis tank, smectite is flocked on the anode; Take out, remaining solids is washed 2 times; Drying gets impurity, and the percentage by weight that calculates impurity is 6.26%.
Embodiment 19
Get the smectite sample, add water and stir, ultrasonic dispersing 10-30 minute, centrifugal, abandoning supernatant got the water logging smectite; Water is put into container, bit by bit add many sodium tungstates again, the limit edged stirs, and many sodium tungstates are dissolved fully, add to liquid when static the water logging smectite can keep the state that freely suspends; Put into the water logging smectite, fully stir, be put in the electrophoresis tank, smectite is flocked on the anode, takes out, and remaining liq is centrifugal, solids, wash dry back drying one hour in 450 ℃ of high temperature furnaces 3 times.Get impurity, the percentage by weight that calculates impurity is 4.66%.The ESEM sem observation has fibrous material.
Embodiment 20
Get the smectite sample, put in the container, add the water of 25 times of weight, fully stir, put in the ultrasonic disperser; Ultrasonic dispersing 10-30 minute, be put in the electrophoresis tank, smectite is flocked on the anode, takes out; Remaining solids, drying gets impurity, and the percentage by weight that calculates impurity is 9.1%.
Embodiment 21
Get the smectite sample, add 3% magnesium chloride brine of 50 times of weight, ultrasonic dispersing 30 minutes left standstill more than 8 hours; Discard top suspending liquid, sediment adds 10-30 0.5% magnesium sulfate solution doubly, ultrasonic dispersing 10 minutes again; Be put in the electrophoresis tank, smectite is flocked on the anode, takes out remaining solids; Drying gets impurity, and the percentage by weight that calculates impurity is 7.2%.
Claims (9)
1. the detection method of medicinal smectite impurity content and/or kind: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity make the powder crystal X ray diffracting spectrum, according to the characteristic peak of X-ray diffraction, judge the mineral species that exists in the sample; A kind of method in polarized light microscopic method, phase microscope method, ESEM method or the transmission electron microscope method is confirmed the crystal habit of impurity.
2. according to a kind of medicinal smectite impurity content of claim 1 and/or the detection method of kind, it is characterized in that: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity make the powder crystal X ray diffracting spectrum, according to the characteristic peak of X-ray diffraction, judge the mineral species that exists in the sample.
3. according to a kind of medicinal smectite impurity content of claim 1 and/or the detection method of kind, it is characterized in that: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity, drying is with the crystal habit of a kind of method affirmation impurity in polarized light microscopic method, phase microscope method, ESEM method or the transmission electron microscope method.
4. according to a kind of medicinal smectite impurity content of claim 1 and/or the detection method of kind, it is characterized in that: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity; Get impurity, 450 ℃ of dryings 1 hour are confirmed the crystal habit of impurity with a kind of method in polarized light microscopic method, phase microscope method, ESEM method or the transmission electron microscope method.
5. according to a kind of medicinal smectite impurity content of claim 1 and/or the detection method of kind, it is characterized in that: get the smectite sample, water partition method or heavy liquid separation method with after impurity fully separates, are weighed smectite after the drying, calculate the content of impurity.
6. according to claim 1 or a kind of medicinal smectite impurity content of claim 2 or claim 3 or claim 4 or claim 5 and/or the detection method of kind; It is characterized in that: the separated form water method is to be that fully to separate smectite be that medium is aided with other physics, chemical method and fully separates smectite and impurity with impurity or with water to medium with water.
7. according to claim 1 or a kind of medicinal smectite impurity content of claim 2 or claim 3 or claim 4 or claim 5 and/or the detection method of kind, it is characterized in that: heavy liquid separation method is to get the smectite sample, puts in the container; Add the light liquid of preparation heavy-fluid, centrifugal after the placement, abandoning supernatant; Move in the heavy-fluid, fully disperse, centrifugal, wash repeatedly with heavy-fluid; Wash repeatedly with the light liquid of preparation heavy-fluid, wash repeatedly, drying promptly gets impurity.
8. according to claim 1 or a kind of medicinal smectite impurity content of claim 2 or claim 3 or claim 4 or claim 5 and/or the detection method of kind, it is characterized in that: heavy liquid separation method is to get the smectite sample, puts in the container; The light liquid that adds preparation heavy-fluid, after fully disperseing, centrifugal; Abandoning supernatant moves in the heavy-fluid of proportion between smectite and impurity, fully stirs; Centrifugal, wash impurity with heavy-fluid, wash impurity with the light liquid of preparation heavy-fluid again; Wash impurity again, drying promptly gets impurity.
9. according to claim 1 or a kind of medicinal smectite impurity content of claim 2 or claim 3 or claim 4 or claim 5 and/or the detection method of kind; It is characterized in that: get the smectite preparation; Elder generation's water flush away auxiliary material, checked for impurities content and kind thereof again; Perhaps get the smectite preparation, directly checked for impurities content and kind thereof.
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| CN112730147A (en) * | 2020-12-16 | 2021-04-30 | 浙江工业大学 | Method for analyzing content of nonferrous metals in waste incineration slag according to different particle size grading |
| CN113358680A (en) * | 2021-06-01 | 2021-09-07 | 中国科学院地质与地球物理研究所 | Method for distinguishing and semi-quantitatively analyzing different types of montmorillonite in geological sample and application |
| CN113916713A (en) * | 2021-09-28 | 2022-01-11 | 苏州中材非金属矿工业设计研究院有限公司 | Separation and determination method of graphite impurities |
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| CN101504379A (en) * | 2009-01-14 | 2009-08-12 | 济南康众医药科技开发有限公司 | Medicinal smectite X-ray diffraction map identification standard |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112730147A (en) * | 2020-12-16 | 2021-04-30 | 浙江工业大学 | Method for analyzing content of nonferrous metals in waste incineration slag according to different particle size grading |
| CN113358680A (en) * | 2021-06-01 | 2021-09-07 | 中国科学院地质与地球物理研究所 | Method for distinguishing and semi-quantitatively analyzing different types of montmorillonite in geological sample and application |
| CN113916713A (en) * | 2021-09-28 | 2022-01-11 | 苏州中材非金属矿工业设计研究院有限公司 | Separation and determination method of graphite impurities |
| CN113916713B (en) * | 2021-09-28 | 2024-07-16 | 苏州中材非金属矿工业设计研究院有限公司 | Separation and determination method of graphite impurities |
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