CN102636448A - Method for determination of montmorillonite content - Google Patents
Method for determination of montmorillonite content Download PDFInfo
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- CN102636448A CN102636448A CN2012101458003A CN201210145800A CN102636448A CN 102636448 A CN102636448 A CN 102636448A CN 2012101458003 A CN2012101458003 A CN 2012101458003A CN 201210145800 A CN201210145800 A CN 201210145800A CN 102636448 A CN102636448 A CN 102636448A
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Abstract
The invention provides a method for determination of montmorillonite content, comprising the steps of taking a montmorillonite sample, preparing pure montmorillonite, measuring the absorbance of montmorillonite and pure montmorillonite prepared wherefrom using UV-visible spectrophotometry, and calculating the adsorption force of the montmorillonite and the pure montmorillonite prepared wherefrom. The montmorillonite content is calculated by the following formula: montmorillonite % = adsorption force of the montmorillonite sample/ adsorption force of pure montmorillonite* 100%. The method eliminates the impact of different adsorption forces of montmorillonite from the bentonite sources in various mining areas or with different properties and different types, and can accurately detect the content of montmorillonite.
Description
Technical field
The present invention relates to a kind of detection method of content of drug, be specifically related to a kind of assay method of smectite content, 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.In the application of smectite, the height of smectite content has crucial influence to its curative effect.
Judge that at present smectite content mainly contains the blue amount of suction and two kinds of methods of X-ray diffraction quantitative test.
With inhaling the content that blue amount method is measured smectite, be a kind of simple universal method.But, measure and inhale also difference of the used method of blue amount owing to confirm to inhale the method difference of blue quantitative response terminal point.See from the article of having reported, mainly contain halo method (Zhang Naixian etc., clay mineral science study method, Science Press, 1990,183); Oscilloscopic polarography (Ye Huali etc., analytical chemistry, 1986,14 (12): 928); AAS (L. ScderLing, et al.AFS Transactions, 1983,91: 77).The halo method is easy to operate, instrument is simple; Use the most generally,, will observe the terminal point of confirming of blue color circle simultaneously with eyes because repeatedly get drop on test paper; The size of blue color circle is bigger because of people's judgement difference; Terminal point determining is to get liquid to observe simultaneously, causes resultant error bigger, and the accuracy of method and precision all are restricted.The terminal point that oscillopolarographic detection is inhaled blue quantitative response is more accurate, but the instrument more complicated because of using is restricted the widespread use of this method.AAS is, sample added distilled water shake, and sample is fully scattered in water; Adding 1% sodium pyrophosphate solution again shakes up; The conical flask that fills mixed solution is placed little the boiling 5 minutes of heating on the electric furnace, make ca-montmorillonite change sodium base shape into, and make it high degree of dispersion.Let excessive methylene blue fully adsorbed by sample; Survey the absorbance that the remaining methylene blue of solution is produced again, and then check in the content of smectite, little the boiling of heating arranged in the step from the typical curve of being done by standard smectite sample; Water evaporates is arranged in the heating process, make the result inaccurate.Inhale blue amount method inspection smectite content, essence is to utilize the absorption affinity of smectite to calculate the content of smectite.Even pure smectite, because the place of production is different, minerogentic condition is different, ore attribute, genotype difference, it inhales blue amount also can not be constant.So, measure and inhale the actual content that blue amount back conversion smectite content can not accurately reflect smectite.
Smectite content control in the current national drug standards smectite quality standard; It is the relative content that detects smectite with X-ray diffracting spectrum; " 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 smectite, but very inaccurate, 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, detect the content of uncontrollable smectite with X-ray diffracting spectrum.
Stipulate that " contain silicon dioxide (SiO2) and should be 55.0%～65.0% of smectite labelled amount, trioxygen-containingization two aluminium (Al2O3) should be 12.0%～25.0% of smectite labelled amount in the existing medicinal smectite quality standard." 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 not accurately be controlled the content of smectite, and complex operation, causes unnecessary a large amount of manpower and materials wastes.
Patent of invention (2012100566354) discloses the detection method of a kind of smectite impurity content and kind, and this method can be used for the assay of smectite, but smectite is fully separated with impurity, and complex operation, is difficult for grasping.
Summary of the invention
The assay method that the purpose of this invention is to provide a kind of smectite content is to guarantee its curative effect and security.
The objective of the invention is to realize so a kind of assay method of smectite content: get the smectite sample, prepare pure smectite; According to " UV-VIS spectrophotometry of Chinese pharmacopoeia record is measured the smectite sample respectively and with the absorbance log of the pure smectite of its preparation, is calculated the absorption affinity of smectite sample and pure smectite, is calculated as follows smectite content:
Smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%.
The assay method of a kind of smectite content that the present invention is above-mentioned: get the smectite sample respectively and, put in the tool plug conical flask the accurate phosphate buffer 1 0ml that adds pH value 6.8 with the about 0.20g of pure smectite of its preparation; Shake up, the sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths again; Jolting 1 hour filters, and precision is measured subsequent filtrate 10ml; Put in the 250ml measuring bottle, be diluted to scale, shake up with the phosphate buffer of pH value 6.8; Precision is measured 5ml, puts in the 50ml measuring bottle, is diluted to scale with the phosphate buffer of pH value 6.8; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance in the wavelength of 254nm; Other gets above-mentioned sulfuric acid strychnine solution and processes the solution that contains 20 μ g among every 1ml with the phosphate buffer dilution of pH value 6.8 in right amount, measures absorbance with method, calculates the absorption affinity of smectite sample and pure smectite, is calculated as follows smectite content:
Smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%.
The assay method of a kind of smectite content that the present invention is above-mentioned: get the about 0.20g of pure smectite of smectite sample and its preparation respectively, put in the tool plug conical flask, the accurate phosphate buffer 1 0ml that adds pH value 6.8, jolting 1 hour; Place more than 8 hours, the sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths; Jolting 1 hour filters, and precision is measured subsequent filtrate 10ml; Put in the 250ml measuring bottle, the phosphate buffer that adds pH value 6.8 is diluted to scale, shakes up; Precision is measured 5ml, puts in the 50ml measuring bottle, and the phosphate that adds pH value 6.8 is diluted to scale towards liquid; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance log in the wavelength of 254nm; Other gets above-mentioned sulfuric acid strychnine solution and processes the phosphate-buffered liquor that every 1ml contains the sulfuric acid strychnine pH value 6.8 of 20 μ g in right amount, measures absorbance log with method, calculates the absorption affinity of smectite sample and pure smectite, is calculated as follows smectite content:
Smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%.
The assay method of a kind of smectite content that the present invention is above-mentioned: the content that it is characterized in that calculating smectite with smectite sample absorption affinity with the ratio of the pure smectite absorption affinity of its preparation.
The absorption affinity of smectite derives from the imbalance of its internal charge.In smectite Si-O tetrahedral sheet, the Si of tetravalence is sometimes by the Al of trivalent replacement, in Al-O octahedral sheet; The Al of trivalent is sometimes by the Mg of divalence replacement, and this just causes positive charge not enough, and negative charge is superfluous; The negative charge of this surplus is compensated by the kation of absorption on the crystal layer surface; When having water to exist, the compensating cation on crystal layer surface is called exchange absorption easily by other cation exchange.The smectite cation exch ange adsorption has following characteristics: (1) jack per line ion exchanges each other, and kation in smectite unit's crystal layer and the exchange interaction between the kation in the solution are stoichiometric reactions, meet the mass action law; (2) etc. electric weight (or equivalent) is intercoursed, the kation that the smectite surface exchange is come out with equated by the cationic electric weight (or equivalent) of smectite absorption, intercourse like 1 Ca2+ and 2 Na+; (3) cationic exchange and absorption are reversible.According to the ion-exchange absorption characteristics of smectite, the above-mentioned sulfuric acid strychnine of the present invention replaces with the compound that in water, can dissociate positive ion, has same effect.These compounds that in water, can dissociate positive ion include but not limited to ammonium acetate, ammonium chloride, methylene blue, quinine sulfate, berberine, betaine, barium chloride etc.When above-mentioned sulfuric acid strychnine replaces with the compound that in water, can dissociate positive ion; Its absorption affinity assay method also can be made corresponding change, like titrimetry, and high performance liquid chromatography; But ultimate principle all is to let the excessive agent that is adsorbed fully adsorbed by smectite; Survey again and remainingly in the solution be adsorbed agent, calculate absorption affinity, with smectite sample absorption affinity with the content of the ratio calculating smectite of the pure smectite absorption affinity of its preparation.
Ion-exchange absorption characteristics according to smectite; The present invention calculates the content of smectite with the ratio of the pure smectite absorption affinity of smectite sample absorption affinity and its preparation, and the pure smectite cation exchange capacity of cation exchange capacity and its preparation that also can replace with the smectite sample is than the content that calculates smectite; Computing formula is: smectite %=smectite sample cation exchange capacity/pure smectite cation exchange capacity * 100%.
The assay method of a kind of smectite content that the present invention is above-mentioned is to get the smectite preparation, and first water flush away auxiliary material detects smectite content again; Or get the smectite preparation, directly detect smectite content.
The calculating smectite sample that the present invention is above-mentioned and the absorption affinity of pure smectite are calculated as follows:
Absorption affinity (g/g)=(2A1-A2) * M1 * D2/ (M2 * A1 * D1)
A1: sulfuric acid strychnine contrast solution absorbance log
A2: sample solution absorbance log
M1: sulfuric acid strychnine weight
M2: sampling weight
D1: sulfuric acid strychnine contrast solution extension rate
D2: sample solution extension rate.
The smectite of the smectite % that the present invention is above-mentioned is meant pure smectite, and smectite % is the percentage composition of pure smectite; Pure smectite is not to be chemical pure, also possibly contain the non-smectite impurity of minute quantity, and the non-smectite impurity of minute quantity is ignored to the influence of smectite absorption affinity.
The present invention is above-mentioned gets the pure smectite of smectite specimen preparation, and method is to get smectite water partition method or heavy-fluid method or electrophoresis to prepare pure smectite.
The above-mentioned absorption affinity of the present invention is meant the weight of the adsorbed material of per 1 gram smectite sample or the absorption of pure smectite.
2% the sulfuric acid strychnine solution that the present invention is above-mentioned, compound method is to get sulfuric acid strychnine 2.00g, puts in the 100ml measuring bottle, and it is an amount of to add water, and heating makes dissolving in the water-bath, puts coldly, is diluted with water to scale, shakes up, and promptly gets.
The phosphate buffer of the pH value 6.8 that the present invention is above-mentioned can be prepared with the method that pharmacopeia is recorded.
Substantive progressive being of the present invention; Though for the smectite that the bentonitic clay of each mining area, each attribute, genotype is originated; Ion exchange capacity is different, and the varying in size of its absorption affinity is no matter but whether to contain impurity absorption power for same smectite sample be identical.So; Calculate the content of smectite through the smectite sample with the ratio of the pure smectite absorption affinity of its preparation; Eliminate the different influence of absorption affinity of smectite in the bentonitic clay source of different mining areas, different attribute, different genotypes, can check smectite content more accurately; The present invention uses UV-VIS spectrophotometry to measure absorption affinity, has improved accuracy and precision than the halo method; The present invention detects the relative content of smectite than X-ray diffracting spectrum, disappears except when when containing the big or non-absorbent mineral of the absorption coefficient of more amount in the smectite, detect the deficiency of uncontrollable smectite content with X-ray diffracting spectrum.
Further specify of the present invention substantive progressive below through Test Example.
1, the medicinal smectite sample 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." the medicinal smectite sample of two producers of first, second all meets medicinal standard.
2, it is an amount of to get medicinal smectite first, the medicinal smectite second of two producers of first, second respectively, adds 1% aqueous dispersant of 30 times of weight, and ultrasonic dispersing 30 minutes left standstill 8 hours; Get top 3/4 suspending liquid, centrifugal, remove supernatant; Add water, stir, centrifugal; Remove supernatant, sediment is drying to obtain pure smectite first, pure smectite second.
3, get it filled respectively with smectite first, medicinal smectite second, pure smectite first, the about 0.20g of pure smectite second, put in the tool plug conical flask, the accurate phosphate buffer 1 0ml that adds pH value 6.8; Shake up, the sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths again; Jolting 1 hour filters, and precision is measured subsequent filtrate 10ml; Put in the 250ml measuring bottle, be diluted to scale, shake up with the phosphate buffer of pH value 6.8; Precision is measured 5ml, puts in the 50ml measuring bottle, is diluted to scale with the phosphate buffer of pH value 6.8; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance in the wavelength of 254nm; Other gets above-mentioned sulfuric acid strychnine solution and processes the solution that contains 20 μ g among every 1ml with the phosphate buffer dilution of pH value 6.8 in right amount, measures absorbance with method, calculates absorption affinity, calculates smectite content;
Medicinal smectite first smectite content is 82.6%, and medicinal smectite second smectite content is 94.3%.
Two X-ray diffracting spectrums meet the smectite of medicinal standard, and the smectite content difference is so big, explain that the content with X-ray diffracting spectrum control smectite needs to improve.The present invention can control the content of smectite more accurately.
4, get the deposition of this experimental example 2, drying and crushing is made the powder crystal X ray diffracting spectrum, according to the characteristic peak analysis of X-ray diffraction, and the medicinal smectite impurity of first producer mainly contains smalite, and the medicinal smectite impurity of second producer mainly contains quartz.
Embodiment
The objective of the invention is to realize so a kind of assay method of smectite content: get the smectite sample, prepare pure smectite; According to " UV-VIS spectrophotometry of Chinese pharmacopoeia record is measured the absorbance log of smectite sample and pure smectite respectively, calculates the absorption affinity of smectite sample and pure smectite, is calculated as follows smectite content;
Smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%.
The assay method of a kind of smectite content that the present invention is above-mentioned: get the smectite sample, prepare pure smectite; Get smectite sample and the about 0.20g of pure smectite respectively, put in the tool plug conical flask, the accurate phosphate buffer 1 0ml that adds pH value 6.8 shakes up; The sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths again, and jolting 1 hour filters; Precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, is diluted to scale with the phosphate buffer of pH value 6.8, shakes up; Precision is measured 5ml, puts in the 50ml measuring bottle, is diluted to scale with the phosphate buffer of pH value 6.8; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance in the wavelength of 254nm; Other gets above-mentioned sulfuric acid strychnine solution and processes the solution that contains 20 μ g among every 1ml with the phosphate buffer dilution of pH value 6.8 in right amount, measures absorbance with method, calculates the absorption affinity of smectite sample and pure smectite, is calculated as follows smectite content;
Smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%.
The assay method of a kind of smectite content that the present invention is above-mentioned: get the smectite sample, prepare pure smectite; Get smectite sample and the about 0.20g of pure smectite respectively, put in the tool plug conical flask, the accurate phosphate buffer 1 0ml that adds pH value 6.8, jolting 1 hour; Place more than 8 hours, the sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths jolting 1 hour; Filter, precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, and the phosphate buffer that adds pH value 6.8 is diluted to scale; Shake up, precision is measured 5ml, puts in the 50ml measuring bottle, and the phosphate that adds pH value 6.8 is diluted to scale towards liquid; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance log in the wavelength of 254nm; Other gets above-mentioned sulfuric acid strychnine solution and processes the phosphate-buffered liquor that every 1ml contains the sulfuric acid strychnine pH value 6.8 of 20 μ g in right amount, measures absorbance log with method, calculates the absorption affinity of smectite sample and pure smectite, is calculated as follows smectite content;
Smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%.
The assay method of a kind of smectite content that the present invention is above-mentioned: it is characterized in that the ratio with the pure smectite absorption affinity of smectite sample absorption affinity and its preparation calculates the content of smectite.
The calculating smectite sample that the present invention is above-mentioned and the absorption affinity of pure smectite are calculated as follows:
Absorption affinity (g/g)=(2A1-A2) * M1 * D2/ (M2 * A1 * D1)
A1: sulfuric acid strychnine contrast solution absorbance log
A2: sample solution absorbance log
M1: sulfuric acid strychnine weight
M2: sampling weight
D1: sulfuric acid strychnine contrast solution extension rate
D2: sample solution extension rate.
The assay method of a kind of smectite content that the present invention is above-mentioned: get the smectite sample, prepare pure smectite, method is to get smectite samples with water partition method or heavy-fluid method or electrophoresis to prepare pure smectite.
Water partition method of the present invention prepares pure smectite, and method is to include but not limited to following method:
Get the smectite sample and put in the container, add the water of 10-50 times of weight, fully mixing after the dispersion, leaves standstill more than 8 hours, gets top suspending liquid, is drying to obtain.
Get the smectite sample and put in the container, add the water of 10-50 times of weight, fully mixing after the dispersion, leaves standstill more than 8 hours, gets 4/5 top suspending liquid, is drying to obtain.
Get the smectite sample and put in the container, add the water of 10-50 times of weight, fully mixing after the dispersion, leaves standstill more than 8 hours, gets 4/5 top suspending liquid, and is centrifugal, removes supernatant, and drying precipitate promptly gets.
Get the smectite sample and put in the container, add the phosphate buffer of the pH value 6.8 of 10-50 times of weight, placed 24 hours, get 3/5 top suspending liquid, be drying to obtain.
Get the smectite sample and 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, get the suspending liquid on top 1/2, centrifugal, remove supernatant, add water; Stir, centrifugal, remove supernatant, drying precipitate promptly gets.
Get the aqueous dispersant that the smectite sample adds the 0.3%-1% of 10-50 times of weight, ultrasonic dispersing 10-30 minute, leave standstill more than 8 hours, get top 3/4 suspending liquid, centrifugal, remove supernatant, add water, stir, centrifugal, remove supernatant, drying precipitate promptly gets.
Get the smectite sample and 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 is to 0.8% one 1% of liquid weight; Ultrasonic dispersing 10-30 minute, leave standstill more than 8 hours, get top 3/4 suspending liquid, centrifugal; Remove supernatant, add water, stir; Centrifugal, remove supernatant, drying precipitate promptly gets.
Get the smectite sample and add water and shake up, add the alkalescent spreading agent, ultrasonic dispersing, centrifugal with hydro-extractor, get top suspending liquid, centrifugal, remove supernatant, add water, stir, centrifugal, the removal supernatant, drying precipitate promptly gets.
Get the water that the smectite sample adds 4-8 times of weight, jolting disperses it, adds the alkaline dispersing agent WS of 20-100 times of weight; Sonicated 5-20 minute, be transferred in the centrifuge tube, centrifugal 5-20 minute (1000 rev/mins) are got top suspending liquid; Centrifugal (3000 rev/mins) are removed supernatant, add water, stir; Centrifugal, remove supernatant, sediment is drying to obtain.
The above-mentioned alkalescent spreading agent of the present invention comprise be not limited to soda mint, sodium carbonate, sodium pyrophosphate, sodium hexametaphosphate, sodium borate, sodium acetate, sodium sulphate, (ammonium salt comprises ammonium chloride, ammonium nitrate to ammonium salt; Ammonium sulfate, ammonium oxalate) etc.; When wherein using sodium sulphate, ammonium salt, transfer solution to alkalescent with basic species.Can be made into the WS that weight percent concentration is 0.1%-2% to alkaline dispersing agent earlier, the WS of preferred 0.2%-1% also can directly add alkaline dispersing agent, and alkaline dispersing agent amount contained in the addition and the use alkaline dispersing agent WS is suitable.
The present invention is equipped with pure smectite with the electrophoresis legal system, and method is to include but not limited to following method:
Get the smectite sample, put in the container, add the water of 10-50 times of weight, jolting 1 hour is put into electricity ice groove again and carries out electrophoresis, and the smectite that has negative charge is flocked on the anode, and taking-up is drying to obtain.
Get the smectite sample, 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 negative charge is flocked on the anode, taking-up is drying to obtain.
The present invention prepares pure smectite with the heavy-fluid method, and method is to include but not limited to following method:
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, slowly 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, gets top suspending liquid, drying, and many sodium tungstates are removed in washing, are drying to obtain.
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, slowly 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, gets top suspending liquid, drying, many sodium tungstates are removed in washing, are drying to obtain.
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, and powerful jolting is centrifugal, gets top suspending liquid, and drying is washed 3 times, is drying to obtain.
Get the smectite sample, 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, and powerful jolting is centrifugal; Get top suspending liquid, drying is washed 3 times, is drying to obtain.
2% the sulfuric acid strychnine solution that the present invention is above-mentioned, compound method is to get sulfuric acid strychnine 2.00g, puts in the 100ml measuring bottle, and it is an amount of to add water, and heating makes dissolving in the water-bath, puts coldly, is diluted with water to scale, shakes up, and promptly gets.
The phosphate buffer of the pH value 6.8 that the present invention is above-mentioned can be prepared with the method that pharmacopeia is recorded.
The absorption affinity of smectite derives from the imbalance of its internal charge.In smectite Si-O tetrahedral sheet, the Si of tetravalence is sometimes by the Al of trivalent replacement, in Al-O octahedral sheet; The Al of trivalent is sometimes by the Mg of divalence replacement, and this just causes positive charge not enough, and negative charge is superfluous; The negative charge of this surplus is compensated by the kation of absorption on the crystal layer surface; When having water to exist, the compensating cation on crystal layer surface is called exchange absorption easily by other cation exchange.The smectite cation exch ange adsorption has following characteristics: (1) jack per line ion exchanges each other, and kation in smectite unit's crystal layer and the exchange interaction between the kation in the solution are stoichiometric reactions, meet the mass action law; (2) etc. electric weight (or equivalent) is intercoursed, the kation that the smectite surface exchange is come out with equated by the cationic electric weight (or equivalent) of smectite absorption, intercourse like 1 Ca2+ and 2 Na+; (3) cationic exchange and absorption are reversible.According to the ion-exchange absorption characteristics of smectite, the above-mentioned sulfuric acid strychnine of the present invention replaces with the compound that in water, can dissociate positive ion, has same effect.These compounds that in water or ethanolic solution, can dissociate positive ion include but not limited to ammonium acetate, ammonium chloride, methylene blue, quinine sulfate, berberine, betaine, barium chloride etc.
The assay method of a kind of smectite content that the present invention is above-mentioned is to get the smectite preparation, first water or 50% ethanol flush away auxiliary material, the assay method checked for impurities content and the kind thereof of pressing smectite content again.
The assay method of a kind of smectite content that the present invention is above-mentioned is to get the smectite preparation, presses the direct checked for impurities content of assay method and the kind thereof of smectite content.
For example, further specify the present invention below.
Embodiment 1
Get smectite sample 3g and put in the container, add the water of 50 times of weight, fully mixing after the dispersion, leaves standstill more than 8 hours, gets 1/2 top suspending liquid, and is centrifugal, removes supernatant, and drying precipitate makes pure smectite.
Take by weighing smectite sample 0.20g, pure smectite 0.20g, put respectively in the tool plug conical flask, the accurate phosphate buffer 1 0ml that adds pH value 6.8 shakes up; The sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths again, and jolting 1 hour filters; Precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, is diluted to scale with the phosphate buffer of pH value 6.8, shakes up; Precision is measured 5ml, puts in the 50ml measuring bottle, is diluted to scale with the phosphate buffer of pH value 6.8; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance in the wavelength of 254nm; Other gets above-mentioned sulfuric acid strychnine solution and processes the solution that contains 20 μ g among every 1ml with the phosphate buffer dilution of pH value 6.8 in right amount, measures absorbance with method, is calculated as follows the absorption affinity of smectite sample and pure smectite.
Absorption affinity (g/g)=(2A1-A2) * M1 * D2/ (M2 * A1 * D1);
A1: sulfuric acid strychnine contrast solution absorbance log;
A2: sample solution absorbance log;
M1: sulfuric acid strychnine weight;
M2: smectite sample or pure smectite weight;
D1: sulfuric acid strychnine contrast solution extension rate;
D2: sample solution extension rate.
Every 1g smectite absorption sulfuric acid strychnine 0.46g, the pure smectite absorption of every 1g sulfuric acid strychnine 0.51g.
Calculate smectite content;
Smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%=0.46/0.51 * 100%=90.2%
Embodiment 2
Get smectite sample 5g and put in the container, add the phosphate buffer of the pH value 6.8 of 50 times of weight, placed 24 hours, get 3/4 top suspending liquid, centrifugal, remove supernatant, add water, stir, centrifugal, remove supernatant, drying precipitate makes pure smectite.
Take by weighing smectite sample 0.20g, pure smectite 0.20g, put respectively in the tool plug conical flask, the accurate phosphate buffer 1 0ml that adds pH value 6.8, jolting 1 hour; Placed 24 hours, the sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths jolting 1 hour; Filter, precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, and the phosphate buffer that adds pH value 6.8 is diluted to scale; Shake up, precision is measured 5ml, puts in the 50ml measuring bottle, and the phosphate that adds pH value 6.8 is diluted to scale towards liquid; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance log in the wavelength of 254nm; Other gets above-mentioned sulfuric acid strychnine solution and processes the phosphate-buffered liquor that every 1ml contains the sulfuric acid strychnine pH value 6.8 of 20 μ g in right amount, measures absorbance log with method, calculates the absorption affinity of smectite sample and pure smectite.
Smectite sample absorption affinity 0.38g, pure smectite absorption affinity 0.49g.
Calculate smectite content:
Smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%=0.38/0.49 * 100%=77.6%.
Embodiment 3
1, it is an amount of to get smectite, adds 1% pyrophosphoric acid WS 100g again, and ultrasonic dispersion 10 minutes is put in the SB-120DTN type ultrasonic cleaning machine that NingBo XinZhi Biology Science Co., Ltd produces in jolting; Use the XCYZ-13 electric centrifuge, 1000 rev/mins of rotor speeds centrifugal 5 minutes, are got 4/5 top suspending liquid; Centrifugal, remove supernatant, add water, stir; Centrifugal, remove supernatant, drying precipitate makes pure smectite.
2, the preparation massfraction is 0.2% methylene blue solution: be taken at the solution transfer of 93 ℃ ± 2 ℃ oven dry 4h methylene blue 2.0611g waters to the brown volumetric flask of 1000ml, thin up shakes up to scale, places 8h.Precision is measured this liquid 50ml, puts in the water-bath and heats 75 ℃, and precision adds potassium dichromate (0.01667mol/L) 25ml, shakes up; 75 ℃ of insulations 20 minutes, put coldly, filter with sintered glass funnel, beaker and funnel are with water washing 4 times; Each 2.5ml filters, and merging filtrate and washing lotion are in the dislocation tool plug conical flask; Add water 250ml, sulfuric acid solution (1 → 5) 25ml and potassium iodide test solution 10ml shake up, with sodium thiosulfate vs (0.1mol/L) titration; During to nearly terminal point, add starch indicator solution 2ml, continue titration and disappear to blue.And the result of titration proofreaied and correct with blank test.Every 1ml potassium dichromate (0.01667mol/L) is equivalent to the C16H18ClN3S of 10.66mg.The concentration that calculates methylene blue solution is: 0.201%.
3, preparation phosphate buffer (pH6.8): get the 0.1mol/L hydrochloric acid solution and the 0.2mol/L sodium radio-phosphate,P-32 solution mixes by 3:1, get pH value 6.83 with the Ph instrumentation.
4, take by weighing smectite sample 0.19961g, pure smectite 0.2016g, put respectively in the tool plug conical flask, accurate adding phosphate buffer 1 0ml, jolting 1 hour; Placed 24 hours, the accurate methylene blue mark solution 50ml that adds puts in 37 ℃ of water-baths jolting 1 hour; Filter with dry middling speed filter paper, precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, adds phosphate buffer (pH6.8) and is diluted to scale; Shake up, precision is measured 5ml, puts in the 50ml measuring bottle; Add phosphate and be diluted to scale, shake up, according to the Chinese Pharmacopoeia AAS towards liquid (pH6.8); Measure absorbance log in the 665nm wavelength: other gets 0.2% methylene blue titer and adds phosphate buffer (pH6.8) in right amount and process the solution that contains 2ug among every ml, measures absorbance log with method, calculates absorption affinity.
Smectite sample absorption affinity 0.333g, pure smectite absorption affinity 0.3845g.
Smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%=0.333/0.3845 * 100%=86.6%.
Embodiment 4
Get the diffusing 5g of smectite and add 40 times of water, add sodium carbonate and magnesium oxide again, make the 1%-2% of sodium carbonate to liquid weight, magnesium oxide is to 0.8%% of liquid weight; Ultrasonic dispersing 20 minutes left standstill 8 hours, got 2/3 top suspending liquid, and is centrifugal; Remove supernatant, add water, stir, centrifugal; Remove supernatant, drying precipitate promptly gets pure smectite.
Calculate the content of smectite with the pure smectite cation exchange capacity ratio of cation exchange capacity and its preparation.Take by weighing the about 1.000g of sample respectively, put in the centrifuge tube, add 20mL50% ethanol, on magnetic stirring apparatus, stir 5min, make the soluble salt dissolving.Take off, centrifuging, inclining clear liquid and discards.Add 50mL0.5mol/L ammonium chloride 50% ethanol exchange liquid, on magnetic stirring apparatus, stir 30min again.Take off, centrifuging, inclining clear liquid and discards.With 95% washing with alcohol residue and centrifuge tube inwall twice, about at every turn 25mL.Residue after the washing is moved in the 100mL conical flask; Add lime chloride-formaldehyde mixed solution 25mL, add 4 phenolphthalein indicators, bottle stoppers beyond the Great Wall again; Fierce vibration 1min, continuation does not disappear to stable pink 3min with the titration of 0.1mol/L standard solution of sodium hydroxide and is terminal point.Be calculated as follows cation exchange capacity: CEC=C * V * 100.In the formula: CEC is cation exchange capacity (mmol/100g); C is standard solution of sodium hydroxide concentration (mol/L); V is for consuming the volume (mL) of standard solution of sodium hydroxide.
Record: the cation exchange capacity that smectite looses is 47.32 mmol/100g, and the cation exchange capacity of pure smectite is 69.46mmol/100g.
The smectite %=smectite cation exchange capacity/pure smectite cation exchange capacity * 100%=47.32 ÷ 69.46 * 100%=68.1% that looses.
Embodiment 5
Get smectite sample 10g, put in the container, add the water of 20 times of weight, ultrasonic dispersing 30 minutes is put into electricity ice groove again and carries out electrophoresis, and the smectite that has negative charge is flocked on the anode, takes out and is drying to obtain pure smectite.
Edit with Zheng Xiuhua; " mensuration of bentonitic clay cation exchange capacity " method that publishing house of China University of Geosciences 09 month calendar year 2001 the 1st edition " bentonitic clay application technology " records is measured; Measure for being adsorbed agent with ammonium acetate; The cation exchange capacity of smectite sample is 70.12mmol/100g, and the cation exchange capacity of pure smectite is 81.46mmol/100g.Smectite content is 86.1%.
Embodiment 6
1, get the diffusing 10g of smectite, add 50% ethanol 300ml, behind the shake well, centrifugal (3000 rev/mins) 15 minutes; Abandoning supernatant repeats 2 times, content is transferred in the evaporating dish of constant weight; Evaporate to dryness, 105 ℃ are dried to constant weight, and (this kind smectite also contains impurity to get the weight that contains smectite in the test product; The smectite content that can not loose as smectite) 9.8g, this kind smectite content is 98% in the test product.
2, get the smectite 6g of 1 preparation, add 1% sodium hexametaphosphate solution 150ml, jolting, 1000 rev/mins of ultrasonic dispersions 10 minutes are centrifugal 5 minutes; Get 4/5 top suspending liquid, 3000 rev/mins centrifugal 15 minutes, remove supernatant, add water; Stir, 3000 rev/mins centrifugal 15 minutes, remove supernatant; Repeat 2 times, drying precipitate makes pure smectite.
Take by weighing smectite 0.20g, the pure smectite 0.20g of 1 preparation, put respectively in the tool plug conical flask, the accurate phosphate buffer 1 0ml that adds pH value 6.8, jolting 1 hour; Placed 24 hours, the sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths jolting 1 hour; Filter, precision is measured subsequent filtrate 10ml, puts in the 250ml measuring bottle, and the phosphate buffer that adds pH value 6.8 is diluted to scale; Shake up, precision is measured 5ml, puts in the 50ml measuring bottle, and the phosphate that adds pH value 6.8 is diluted to scale towards liquid; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance log in the wavelength of 254nm; Other gets above-mentioned sulfuric acid strychnine solution and processes the phosphate-buffered liquor that every 1ml contains the sulfuric acid strychnine pH value 6.8 of 20 μ g in right amount, measures absorbance log with method, calculates the absorption affinity of smectite and pure smectite.
Smectite absorption affinity 0.41g, pure smectite absorption affinity 0.50g.
Calculate the pure smectite content that smectite looses:
Smectite %=smectite absorption affinity/pure smectite absorption affinity * 98%=0.41/0.50 * 98%=80.36%.
Embodiment 7
The smectite of getting 1 preparation looses 2 bags, adds 1.5% aqueous sodium carbonate 150ml, jolting, and 1000 rev/mins of ultrasonic dispersions 10 minutes are centrifugal 5 minutes; Get 4/5 top suspending liquid, 3000 rev/mins centrifugal 15 minutes, remove supernatant, add water; Stir, 3000 rev/mins centrifugal 15 minutes, remove supernatant; Repeat 2 times, drying precipitate makes pure smectite.
Take by weighing the diffusing 0.25g (containing smectite 0.20 approximately) of smectite of 1 preparation, pure smectite 0.20g, put respectively in the tool plug conical flask, the accurate phosphate buffer 1 0ml that adds pH value 6.8, jolting 1 hour; Placed 24 hours, the sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths; Jolting 1 hour filters, and precision is measured subsequent filtrate 10ml; Put in the 250ml measuring bottle, the phosphate buffer that adds pH value 6.8 is diluted to scale, shakes up; Precision is measured 5ml, puts in the 50ml measuring bottle, and the phosphate that adds pH value 6.8 is diluted to scale towards liquid; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance log in the wavelength of 254nm; Other gets above-mentioned sulfuric acid strychnine solution and processes the phosphate-buffered liquor that every 1ml contains the sulfuric acid strychnine pH value 6.8 of 20 μ g in right amount, measures absorbance log with method, calculates the smectite absorption affinity with pure smectite of loosing.
The smectite absorption affinity 0.30g that looses, pure smectite absorption affinity 0.48g.
Calculate the pure smectite content that smectite looses:
The smectite %=smectite absorption affinity/pure smectite absorption affinity * 100%=0.30/0.48 * 100%=62.5% that looses.
Claims (10)
1. the assay method of a smectite content is characterized in that: get the smectite sample, prepare pure smectite; According to " UV-VIS spectrophotometry of Chinese pharmacopoeia record is measured the smectite sample respectively and with the absorbance log of the pure smectite of its preparation; Calculate the absorption affinity of the pure smectite of smectite sample and its preparation, be calculated as follows smectite content: smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%.
2. according to the assay method of a kind of smectite content of claim 1, it is characterized in that: get the smectite sample respectively and, put in the tool plug conical flask the accurate phosphate buffer 1 0ml that adds pH value 6.8 with the about 0.20g of pure smectite of its preparation; Shake up, the sulfuric acid strychnine solution 10ml of accurate adding 2% puts in 37 ℃ of water-baths jolting 1 hour again; Do not place or place more than 8 hours, filter, precision is measured subsequent filtrate 10ml; Put in the 250ml measuring bottle, be diluted to scale, shake up with the phosphate buffer of pH value 6.8; Precision is measured 5ml, puts in the 50ml measuring bottle, is diluted to scale with the phosphate buffer of pH value 6.8; Shake up, according to " UV-VIS spectrophotometry of two appendix IV of Chinese pharmacopoeia version in 2010 A record is measured absorbance in the wavelength of 254nm; It is an amount of that other gets above-mentioned sulfuric acid strychnine solution; The sulfuric acid strychnine solution that contains 20 μ g among every 1ml is processed in phosphate buffer dilution with pH value 6.8; Measure absorbance with method; Calculate the absorption affinity of smectite sample and pure smectite, be calculated as follows smectite content: smectite %=smectite sample absorption affinity/pure smectite absorption affinity * 100%.
3. according to the assay method of a kind of smectite content of claim 1 or claim 2, it is characterized in that: the content that calculates smectite with smectite sample absorption affinity with the ratio of the pure smectite absorption affinity of its preparation.
4. according to the assay method of a kind of smectite content of claim 1 or claim 2; It is characterized in that: when the sulfuric acid strychnine replaces with the compound that in water, can dissociate positive ion; Its absorption affinity assay method is made corresponding change, calculates the content of smectite with smectite sample absorption affinity with the ratio of the pure smectite absorption affinity of its preparation.
5. according to the assay method of a kind of smectite content of claim 1 or claim 2 or claim 4; It is characterized in that: the sulfuric acid strychnine replaces with ammonium acetate or ammonium chloride or methylene blue or quinine sulfate or berberine or betaine or barium chloride; Its absorption affinity assay method is made corresponding change, calculates the content of smectite with smectite sample absorption affinity with the ratio of the pure smectite absorption affinity of its preparation.
6. according to the assay method of a kind of smectite content of claim 1; It is characterized in that: calculate the content of smectite with smectite sample absorption affinity with the ratio of the pure smectite absorption affinity of its preparation, replace with the cation exchange capacity of smectite with the content of the ratio calculating smectite of the pure smectite cation exchange capacity of its preparation; Computing formula is: smectite %=smectite sample cation exchange capacity/pure smectite cation exchange capacity * 100%.
7. according to the assay method of a kind of smectite content of claim 1 or claim 2 or claim 3 or claim 4 or claim 5 or claim 6; It is characterized in that: get the smectite preparation; Elder generation's water flush away auxiliary material; Detect smectite content again, or get the smectite preparation and directly detect smectite content.
8. according to the assay method of a kind of smectite content of claim 1 or claim 2 or claim 3 or claim 4 or claim 5 or claim 6 or claim 7; It is characterized in that: get the pure smectite of smectite specimen preparation, method is to get smectite water partition method or heavy-fluid method or electrophoresis to prepare pure smectite.
9. according to the assay method of a kind of smectite content of claim 1 or claim 9, it is characterized in that: preparing pure smectite, is to get the smectite sample to put in the container; The water that adds 10-50 times of weight, abundant mixing is after the dispersion; Leave standstill more than 8 hours, get top suspending liquid, centrifugal; Remove supernatant, drying precipitate promptly gets.
10. according to the assay method of a kind of smectite content of claim 1 or claim 9, it is characterized in that: preparing pure smectite, is to get the smectite sample to add water and shake up, and adds spreading agent; Ultrasonic dispersing, centrifugal with hydro-extractor, get top suspending liquid, centrifugal; Remove supernatant, add water, stir; Centrifugal, remove supernatant, drying precipitate promptly gets.
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