CN107677842A - A kind of smectite content automatic testing method - Google Patents
A kind of smectite content automatic testing method Download PDFInfo
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- CN107677842A CN107677842A CN201710974382.1A CN201710974382A CN107677842A CN 107677842 A CN107677842 A CN 107677842A CN 201710974382 A CN201710974382 A CN 201710974382A CN 107677842 A CN107677842 A CN 107677842A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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Abstract
The invention discloses a kind of smectite content automatic testing method, using following steps：1）, prepare 0.00500mol/L methylene blue solution；2）, prepare 1% sodium pyrophosphate solution；3）, sample treatment；4）, with graduated cylinder weigh 50ml distilled water in conical flask, then, accurately weigh 0.2000 0.2050g sample powders and be put into the conical flask for claiming have 50ml distilled water and shake up；5）, the sodium pyrophosphate solution 20ml prepared added in conical flask using charger continue to shake up as dispersant；6）, conical flask is placed on electric furnace and boils micro-boiling to 4 5min, remove and be cooled to room temperature, obtain analyte sample fluid；7）, prepare measure；8）, check and correction；9）, automatically determine.The present invention more accurately judges titration end-point, is automatically determined using computer program, as a result more accurate.
Description
Technical field
The present invention relates to the detection method of smectite content, more particularly to a kind of smectite content automatic testing method.
Background technology
In the last few years with montmorillonite development and be widely applied, this requirement for the mass content of montmorillonite is continuous
Improve, judge that smectite content mainly has two methods of Absorbance ratio-derivative method and X x ray diffraction quantitative analysis at present.Its pass of Absorbance ratio-derivative method method
Key is the judgement of titration end-point, judges titration end-point generally use halo method or AAS, halo method is easy to operate, instrument
Device is simple, and application is the most universal, because repeatedly taking drop on test paper, while determines end with eye observation blue color circle
Point, the size of blue color circle is because the judgement difference of people is larger, while terminal point determining is to take liquid to observe, and causes resultant error bigger,
The degree of accuracy and precision for making method are all restricted.AAS is that sample is added into distilled water shakes, and makes sample in water
In fully scatter, add 1% sodium pyrophosphate solution and shake up, the conical flask for filling mixed solution is placed on electric furnace and heated
Micro-boiling 5 minutes, ca-montmorillonite is changed into sodium base shape, and be allowed to high degree of dispersion.Excessive methylene blue is allowed to be filled by sample
Divide absorption, then survey absorbance caused by the remaining methylene blue of solution, then again from the mark made by standard montmorillonite sample
The content of montmorillonite is checked on directrix curve, has heating micro-boiling in step, has moisture evaporation in heating process, makes result inaccurate.
For this, my company puts into the method that substantial amounts of time and efforts sums up in test experiment, and for same sample and X
Diffraction patterns difference is ± 0.5%, and precision is within the scope of 0.2%.
The content of the invention
The defects of it is an object of the invention to overcome prior art, there is provided a kind of smectite content automatic testing method, it
Automatic detection is realized, improves detection efficiency, reduces human error.
Technical scheme is as follows：
A kind of smectite content automatic testing method, using following steps：
1st, 0.00500mol/L methylene blue solution is prepared：Weigh the reagent methylene of purity >=99.9% without the crystallization water
Blue 1.5995g, it is dissolved in 1000 milliliters of water, constant volume；
2nd, 1% sodium pyrophosphate solution is prepared：The analytically pure sodium pyrophosphates of 10g, in the volumetric flask of constant volume to 1000ml, shake up, treat
After being completely dissolved, static 24h is used；
3rd, sample treatment：The drying of montmorillonite sample is levigate, dried again after crossing 200 mesh sieves, obtain sample powder；
4th, 50ml distilled water is weighed in conical flask with graduated cylinder, then, accurately weigh 0.2000-0.2050g sample powders, accurately
To 0.0000g, it is put into the conical flask for claiming have 50ml distilled water and shakes up；
5th, the sodium pyrophosphate solution 20ml prepared is added in conical flask using charger to continue to shake up as dispersant, if having
Untill bulk is not easy to disperse to continue to be stirred with glass bar；
6th, conical flask is placed on electric furnace and boils micro-boiling to 4-5min, removed and be cooled to room temperature, obtain analyte sample fluid；
7th, measure is prepared：The methylene blue solution prepared is added into analyte sample fluid with buret, instills 10ml scheduled volumes
2/3 or so, with hand rolling 30s, methylene blue is fully absorbed by montmorillonite, then with glass bar be stained with a drop test solution drop in it is fixed
Measure on Medium speed filter paper, liquid-drop diameter is preferably 10-15mm on filter paper, obtains spot image；Observe the week in navy blue spot
Enclose and nattier blue point-like or halo whether occur, be colourless wetting circle outside point-like or halo, can by magnifying glass or
Micro- sem observation, or by mobile phone camera function take pictures and amplification picture observe, determine whether to reach titration end-point；If not
Titration end-point, continue that methylene blue solution is added dropwise, until obtaining satisfactory spot image, judgement reaches titration end-point, and
The volume of record consumption methylene blue；
8th, proofread：Contrasted, prepare liquid is filtered with qualitative filter paper, filtrate is put into diameter 1cm using ultraviolet spectrophotometer
Cuvette in distilled water make reference subject, with determining absorbance at wavelength 666nm, absorbance scope 0.01 ~
It is judgement terminal between 0.10, and gathers the spot image and be designated as standard endpoint spot image；
9th, automatically determine：Repeat the above steps after 1-6, automatically determined with full-automatic smectite content measuring instrument and other treat test sample
Product, full-automatic smectite content measuring instrument include memory, processor and storage on a memory and can transported on a processor
Capable computer program,
Memory, for storing computer program and standard endpoint spot image；
Processor, for performing the computer program, the computer program further comprises：
Titration procedure, it is configured as that methylene blue solution gradually is added dropwise to a small amount of by volume toward analyte sample fluid is interior；
Spot image obtain program, its be configured as with take drop pipe constantly dip drop drip to filter paper formed spot image；
Spot image alignment programs, it is configured as the spot image of acquisition being compared with standard endpoint spot image, from
It is dynamic to judge titration end-point；
Calculation procedure, it is configured as recording methylene blue consumption, calculates Absorbance ratio-derivative method and be converted into smectite content and export
Display.
The advantage of the invention is that：1st, the present invention more accurately sentences by magnifying glass, microscope or enlarging function of taking pictures
Determine titration end-point, and contrast to obtain standard endpoint spot image with ultraviolet spectrophotometer；2nd, using computer program certainly
Dynamic measure, it is as a result more accurate.
The invention will be further described below embodiment.
A kind of smectite content automatic testing method, using following steps,
1st, 0.00500mol/L methylene blue solution is prepared：Weigh the reagent methylene of purity >=99.9% without the crystallization water
Blue 1.5995g, it is dissolved in 1000 milliliters of water, constant volume；
2nd, 1% sodium pyrophosphate solution is prepared：The analytically pure sodium pyrophosphates of 10g, in the volumetric flask of constant volume to 1000ml, shake up, treat
After being completely dissolved, static 24h is used；
3rd, sample treatment：The drying of montmorillonite sample is levigate, dried again after crossing 200 mesh sieves, obtain sample powder；
4th, 50ml distilled water is weighed in conical flask with graduated cylinder, then, accurately weigh 0.2000-0.2050g sample powders, accurately
To 0.0000g, it is put into the conical flask for claiming have 50ml distilled water and shakes up；
5th, the sodium pyrophosphate solution 20ml prepared is added in conical flask using charger to continue to shake up as dispersant, if having
Untill bulk is not easy to disperse to continue to be stirred with glass bar；
6th, conical flask is placed on electric furnace and boils micro-boiling to 4-5min, removed and be cooled to room temperature, obtain analyte sample fluid；
7th, measure is prepared：The methylene blue solution prepared is added into analyte sample fluid with buret, instills 10ml scheduled volumes
2/3 or so, with hand rolling 30s, methylene blue is fully absorbed by montmorillonite, then with glass bar be stained with a drop test solution drop in it is fixed
Measure on Medium speed filter paper, liquid-drop diameter is preferably 10-15mm on filter paper, obtains spot image；Observe the week in navy blue spot
Enclose and nattier blue point-like or halo whether occur, be colourless wetting circle outside point-like or halo, can by magnifying glass or
Micro- sem observation, or by mobile phone camera function take pictures and amplification picture observe, determine whether to reach titration end-point；If not
Titration end-point, continue that methylene blue solution is added dropwise, until obtaining satisfactory spot image, judgement reaches titration end-point, and
The volume of record consumption methylene blue；
8th, proofread：Contrasted, prepare liquid is filtered with qualitative filter paper, filtrate is put into diameter 1cm using ultraviolet spectrophotometer
Cuvette in distilled water make reference subject, with determining absorbance at wavelength 666nm, absorbance scope 0.01 ~
It is judgement terminal between 0.10, and gathers the spot image and be designated as standard endpoint spot image；
9th, automatically determine：Repeat the above steps after 1-6, automatically determined with full-automatic smectite content measuring instrument and other treat test sample
Product, full-automatic smectite content measuring instrument include memory, processor and storage on a memory and can transported on a processor
Capable computer program,
Memory, for storing computer program and standard endpoint spot image；
Processor, for performing the computer program, the computer program further comprises：
Titration procedure, it is configured as that methylene blue solution gradually is added dropwise to a small amount of by volume toward analyte sample fluid is interior；
Spot image obtain program, its be configured as with take drop pipe constantly dip drop drip to filter paper formed spot image；
Spot image alignment programs, it is configured as the spot image of acquisition being compared with standard endpoint spot image, from
It is dynamic to judge titration end-point；
Calculation procedure, it is configured as recording methylene blue consumption, calculates Absorbance ratio-derivative method and be converted into smectite content and export
Display.
Standard endpoint spot image of the present invention, i.e., the standard endpoint spot figure gathered by above-mentioned steps 1-8
Picture, substantial amounts of standard endpoint spot image storage is in processes.
The computational methods used in calculation procedure for：
MBI---- Absorbance ratio-derivative methods（g/100g）
C ----methylene blue concentration（mol/L）
V --- the volume of-consumption methylene blue（ml）
M ----weigh the quality of sample（g）；
The cubage formula of Absorbance ratio-derivative method conversion bentonite montmorillonite
M=MBI/0.442
The content of montmorillonite in M---- samples（%）
MBI--- Absorbance ratio-derivative methods（g/100g）
0.442 montmorillonite conversion coefficient.
The present invention principle be：Methylene blue is dissolved in water and monovalence weak cation is presented, and montmorillonite has quantitative to methylene blue
Absorption relation, using TLC, the montmorillonite of methylene blue is adsorbed with diffusion velocity of the methylene blue on filter paper not
The spot of visible terminal is presented together, is compared with standard drawing, you can determine terminal, montmorillonite is calculated automatically with computer program
Content.
10 groups of contrast and experiments of experimental example, it is as shown in the table,
Sample size is mass fraction in table, and X diffraction analysis method operates as standard value, GB/T20973-2007 according to national standard
Method is examined, and research and development method is to be detected using the inventive method, it can be seen that the inventive method detection is closest with standard value.
Claims (1)
1. a kind of smectite content automatic testing method, it is characterised in that using following steps：
1）, prepare 0.00500mol/L methylene blue solution：Weigh the reagent methylene of purity >=99.9% without the crystallization water
Blue 1.5995g, it is dissolved in 1000 milliliters of water, constant volume；
2）, prepare 1% sodium pyrophosphate solution：The analytically pure sodium pyrophosphates of 10g, in the volumetric flask of constant volume to 1000ml, shake up,
Until completely dissolved, static 24h is used；
3）, sample treatment：The drying of montmorillonite sample is levigate, dried again after crossing 200 mesh sieves, obtain sample powder；
4）, with graduated cylinder weigh 50ml distilled water in conical flask, then, accurately weigh 0.2000-0.2050g sample powders, essence
0.0000g really is arrived, is put into the conical flask for claiming have 50ml distilled water and shakes up；
5）, the sodium pyrophosphate solution 20ml prepared added in conical flask using charger continue to shake up as dispersant, if
Have bulk be not easy it is scattered continue to be stirred with glass bar untill；
6）, conical flask is placed on electric furnace and boils micro-boiling to 4-5min, remove and be cooled to room temperature, obtain analyte sample fluid；
7）, prepare measure：The methylene blue solution prepared is added into analyte sample fluid with buret, instills 10ml scheduled volumes
2/3 or so, with hand rolling 30s, methylene blue is fully absorbed by montmorillonite, then with glass bar be stained with a drop test solution drop in it is fixed
Measure on Medium speed filter paper, a diameter of 10-15mm of drop, obtains spot image on filter paper；Observe is around navy blue spot
It is no nattier blue point-like or halo occur, it is colourless wetting circle outside point-like or halo, can be by magnifying glass or micro-
Sem observation, or by mobile phone camera function take pictures and amplification picture observe, determine whether to reach titration end-point；If not titration
Terminal, continue that methylene blue solution is added dropwise, until obtaining satisfactory spot image, judgement reaches titration end-point, and records
Consume the volume of methylene blue；
8）, check and correction：Contrasted, prepare liquid is filtered with qualitative filter paper, filtrate is put into diameter 1cm using ultraviolet spectrophotometer
Cuvette in distilled water make reference subject, with determining absorbance at wavelength 666nm, absorbance scope 0.01 ~
It is judgement terminal between 0.10, and gathers the spot image and be designated as standard endpoint spot image；
9）, automatically determine：Repeat the above steps after 1-6, automatically determined with full-automatic smectite content measuring instrument and other treat test sample
Product, full-automatic smectite content measuring instrument include memory, processor and storage on a memory and can transported on a processor
Capable computer program,
Memory, for storing computer program and standard endpoint spot image；
Processor, for performing the computer program, the computer program further comprises：
Titration procedure, it is configured as that methylene blue solution gradually is added dropwise to a small amount of by volume toward analyte sample fluid is interior；
Spot image obtain program, its be configured as with take drop pipe constantly dip drop drip to filter paper formed spot image；
Spot image alignment programs, it is configured as the spot image of acquisition being compared with standard endpoint spot image, from
It is dynamic to judge titration end-point；
Calculation procedure, it is configured as recording methylene blue consumption, calculates Absorbance ratio-derivative method and be converted into smectite content and export
Display.
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| CN201710974382.1A CN107677842A (en) | 2017-10-19 | 2017-10-19 | A kind of smectite content automatic testing method |
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| CN201710974382.1A CN107677842A (en) | 2017-10-19 | 2017-10-19 | A kind of smectite content automatic testing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112595709A (en) * | 2020-10-27 | 2021-04-02 | 重庆建工建材物流有限公司 | Automatic device and method for machine-made sand methylene blue test |
| CN113960244A (en) * | 2021-10-09 | 2022-01-21 | 武汉科技大学 | Method for measuring content of montmorillonite in metallurgical pellets |
Citations (3)
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|---|---|---|---|---|
| CN101493451A (en) * | 2008-09-27 | 2009-07-29 | 辽宁工程技术大学 | Automatic analysis and detection instrument for bentonite blue suction quantity and detection method thereof |
| CN101806747A (en) * | 2010-03-05 | 2010-08-18 | 华中科技大学 | Methylene blue adsorption testing method of bentonite |
| CN201788154U (en) * | 2010-03-05 | 2011-04-06 | 华中科技大学 | Bentonite methylene blue absorption amount testing device |
-
2017
- 2017-10-19 CN CN201710974382.1A patent/CN107677842A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101493451A (en) * | 2008-09-27 | 2009-07-29 | 辽宁工程技术大学 | Automatic analysis and detection instrument for bentonite blue suction quantity and detection method thereof |
| CN101806747A (en) * | 2010-03-05 | 2010-08-18 | 华中科技大学 | Methylene blue adsorption testing method of bentonite |
| CN201788154U (en) * | 2010-03-05 | 2011-04-06 | 华中科技大学 | Bentonite methylene blue absorption amount testing device |
Non-Patent Citations (1)
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| 陈光昀: "《铸造测试技术》", 30 April 1983 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112595709A (en) * | 2020-10-27 | 2021-04-02 | 重庆建工建材物流有限公司 | Automatic device and method for machine-made sand methylene blue test |
| CN113960244A (en) * | 2021-10-09 | 2022-01-21 | 武汉科技大学 | Method for measuring content of montmorillonite in metallurgical pellets |
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