CN101806747A - Methylene blue adsorption testing method of bentonite - Google Patents
Methylene blue adsorption testing method of bentonite Download PDFInfo
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- CN101806747A CN101806747A CN 201010120816 CN201010120816A CN101806747A CN 101806747 A CN101806747 A CN 101806747A CN 201010120816 CN201010120816 CN 201010120816 CN 201010120816 A CN201010120816 A CN 201010120816A CN 101806747 A CN101806747 A CN 101806747A
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Abstract
The invention relates to a methylene blue adsorption testing method of bentonite, which belongs to the field of methods for testing components of clay sand casting material, and solves the problems that a traditional detection method is quite complicated to operate, has lower determination precision, may titrate repeatedly and causes longer testing process. The testing method sequentially comprises a sample solution treatment step, a mixed solution forming step, a quantitative reagent shifting step, a drop spot image acquisition step and an image processing step. Aiming at bentonite methylene blue adsorption testing on a casting production line and the effective bentonite content determination in clay sand, the methylene blue adsorption testing method of bentonite can be realized on a computer, artificially and manually inputs an initial titration value, fully automatically sets and works, automatically acquires drop spot images and judges the final titration destination, can automatically calculate the methylene blue adsorption of bentonite and the effective bentonite content determination in clay sand, has accurate results, reduces the labor intensity of an experimenter, and improves the accuracy in judging the titration destination.
Description
Technical field
The invention belongs to the method for testing of casting clay-bonded sand material composition, be specifically related to a kind of methylene blue adsorption testing method of bentonite, be used for the test of bentonite blue suction quantity and the effective bentonite content of clay old sand on the foundry production line.
Background technology
During the clay-bonded sand mold casting is produced, can adsorb dyestuffs such as methylene blue according to containing montmorillonite mineral in the bentonitic clay, effective bentonite content that dust, sand grains, the no cohesive action materials such as invalid bentonitic clay that are scorched to death then do not adsorb or the characteristic of minute quantity absorption methylene blue dye is carried out in bentonite blue suction quantity test and the old sand is measured.
At present, the assay method of bentonite blue suction quantity has three kinds:
First method be according to " casting handbook Modeling Material volume (and on) the national standard detection method, adopt pure manual titration.Its test procedure is: take by weighing oven dry sample 5g, add massfraction respectively and be 1% sodium pyrophosphate solution 20mL and distilled water 50mL, rock even back heated and boiled 5min on electric furnace, be cooled to room temperature in air, splashing into massfraction with buret is 0.2% methylene blue solution.During titration, can add for the first time expectation the methylene blue solution amount about 2/3, each later on 1-2mL that drips.The method of check terminal point is, drip methylene blue solution at every turn after, rock 30s, dip in a reagent on the middling speed quantitative filter paper with glass bar, observe around the dark blue color dot of central authorities, to have or not and nattier blue halo occurs, if occur, continue to drip methylene blue solution.Like this repeatable operation, when beginning light blue halo to occur, reagent left standstill 1min after, dip in a reagent with glass bar again,, illustrate and do not arrive terminal point if do not occur nattier blue halo again all around, should drip methylene blue solution again, be test endpoint up to tangible light blue halo occurring.[casting branch of Chinese Mechanical Engineering Society compiles. casting handbook (4) [M]. and Beijing: China Machine Press, 2002.]
The test speed of this method is slow, the time is long, and test result relies on unaided eye discrimination, and precision is not high.
Second method is to utilize SND type methylene blue clay analyzer, and this instrument comprises sample dispersion treatment device and titration parts, adopts ultrasonic scattering method dispersion treatment sample, adopts automatic buret, and cooperative mechanical stirs.(casting branch of Chinese Mechanical Engineering Society compiles. casting handbook (4) [M]. and Beijing: China Machine Press, 2002.) this instrument employing semi-hand half mechanical test, the manual operation inflatable ball, its operating process and above-mentioned first method process are similar, different is to make manually to control the manual titration in the first method into inflatable ball to produce air pressure, utilize air pressure to control titer, realize semi-automatic titration, the craft after the titration is rocked reagent and is made mechanical raking reagent into.This method adopts manual control air pressure to carry out titration, artificial observation titration value, and titer and observed reading all are easy to generate error, and the same with pure manual titration, and net result is judged the dependence naked eyes, and precision is not high.
The third method is automatic analysis and detection instrument for bentonite blue suction quantity and the detection method thereof that the people such as Ren Ruichen of Liaoning Project Technology University propose, (number of patent application: 200810013428.4, patent publication No.: CN101493451A), this analyser is made up of automatic titration system, sampling system and Color Recognition System, the same with the SND type tester in the second method, adopt ultrasonic dispersing to handle the bentonitic clay sample.This instrument can detect bentonite blue suction quantity automatically, adopt the amount of splashing into of interactive system control methylene blue, its Color Recognition System adopts given color calibration, under the fluorescence irradiation, sensor is dripped spot and the light green color halo whether occurred, and with given color calibration to recently judging titration end-point.The titration process of whole instrument has used 5 stepper motors altogether, and the operation with control crossbearer and two telescopic rods comprises the rotation of crossbearer and sliding up and down of expansion link.In general, the testing tool of the third method and method can realize that basically robotization detects, the test result precision is also higher relatively, but the whole order of instrument operational process is complicated, in driven by motor telescopic rod mechanical movement process, drop on the expansion link has the possibility of drippage in advance, can cause situations such as sky drips.
Summary of the invention
The invention provides a kind of methylene blue adsorption testing method of bentonite, the existing detection method operation of solution is complicated, the mensuration precision is lower, the problem that may repeat titration, cause test process to prolong is used for the effectively test of bentonite content of bentonite blue suction quantity test and clay old sand.
A kind of methylene blue adsorption testing method of bentonite of the present invention, order comprises:
One. the sample solution treatment step: to the heating of bentonitic clay sample solution or clay old sand sample solution, stir, described bentonitic clay sample solution is that 1% sodium pyrophosphate solution 20mL and distilled water 50mL mix and constitute by 0.2g bentonitic clay, massfraction; Described clay old sand sample solution is that 1% sodium pyrophosphate solution 20mL and distilled water 50mL mix and constitute by 5g clay old sand, massfraction;
Two. form the mixed liquor step: pipette mass percentage concentration and be 0.2% pure methylene blue solution to bentonitic clay sample solution or clay old sand sample solution and stir and form mixed liquor, the amount of pipetting is that the clay old sand is inhaled blue 85% of the daily test volume of measuring on bentonitic clay or the production line, changes step 4;
Three. quantitatively pipette the reagent step: in bentonitic clay sample solution of handling well or clay old sand sample solution, quantitatively pipette mass percentage concentration and be 0.2% pure methylene blue solution and stir and form mixed liquor, the area that calculates according to the process 5.4 of step 5 is than the amount of pipetting of T control methylene blue, when area than T less than 8%, the amount of pipetting is each 1mL, when area than T 8～11% the time, the amount of pipetting is each 0.5mL, when area than T greater than 11% the time, the amount of pipetting is each 0.1mL, changes step 4;
Four. drip the spot image acquisition step: titration 0.1mL mixed liquor forms and drips spot to the middling speed quantitative filter paper, utilizes the industrial camera collection to drip the spot image;
Five. image processing step: carry out Digital Image Processing to dripping the spot image, order comprises following process:
5.1. the spot picture breakdown of dripping that will collect becomes red, green and blue triple channel image;
5.2. red, green and blue triple channel image are carried out the gray-scale value subtraction, obtain the light blue halo in outer ring:
Gray values of pixel points in the red channel image is deducted the gray-scale value of corresponding pixel points in the green channel image, carries out following computing again, obtain transfer image acquisition, its gray values of pixel points P:
P＝α×(R-G)+β，α＝0.1～3，β＝0～256；
Gray values of pixel points in the transfer image acquisition is deducted the gray-scale value of corresponding pixel points in the blue channel image, carries out following computing again, obtain the light blue halo in outer ring, its gray values of pixel points Q:
Q＝γ×(P-B)+λ，γ＝0.1～3，λ＝0～256；
In the formula: R, G, B represent the gray values of pixel points in redness, green and the blue triple channel respectively, and when a spot image effect was dark partially, α and γ span were at 1～3, and a spot image is dark more, and value is big more; When a spot figure kine bias was bright, α and γ span were at 0.1～1, and a spot image is bright more, and value is more little;
β＝α×|(R-G)|
min，λ＝γ×|(P-B)|
min；
Obtain complete spot image 5.3. fill:
According to the light blue halo gray values of pixel points in outer ring, use filling algorithm the ring inner region of the light blue halo in described outer ring is filled, obtain complete spot image R
F
5.4. calculate the area ratio of light blue halo in outer ring and inner ring mazarine spot:
The area S of the light blue halo in outer ring
QArea S with inner ring mazarine spot
DBe respectively:
S
Q＝f(d)×∫S
Q(d)，
S
D＝S
F-S
Q，
Wherein, S
FArea for complete spot:
S
F＝f(d)×∫S
F(d)，
The area of light blue halo in outer ring and inner ring mazarine spot than T is:
T＝S
Q/S
D，
In the formula: d is the resolution of digital camera, and f (d) is the single elemental area under the corresponding digital camera resolution, ∫ S
Q(d) be the number of outer ring pixel that light blue halo comprises, ∫ S
F(d) for comprising the number of pixel in the complete spot region;
5.5. whether the area of judging described light blue halo and inner ring mazarine spot more than or equal to 15%, is then to turn over journey 5.6 than T, quantitatively pipettes the reagent step otherwise change;
5.6. the termination titration process calculates and always moves liquid measure value V:
V＝V
1+V
2+……V
i+……+V
N，
In the formula, V
1Be the pure methylene blue solution of the described step 2 amount of pipetting, V
iBe the i time amount of pipetting of the pure methylene blue solution of described step 3, V
NBe the pure methylene blue solution of the described step 3 amount of pipetting for the last time, i, N are natural number; Always move liquid measure value V and be bentonite blue suction quantity; If the effective bentonite content of test clay old sand is then proceeded process 5.7;
5.7. calculate effective bentonite content;
According to always moving the corresponding interval range that liquid measure value V judges the effective bentonite content of clay old sand, determine corresponding titrimetric factor K and titration constant B, with K, B substitution following formula, calculate effective bentonitic clay quality percentage composition M=((V-B)/K) * 100%,
B, K are following to be determined: get fresh sand and bentonitic recombined sample 5g, measure bentonitic clay quality percentage composition in the recombined sample and be respectively 2%, 4%, 6%, 8% and blue the measuring of suction of 10% o'clock recombined sample, draw bentonitic clay standard titration curve; Rate of curve and y y-intercept when the corresponding interval of calculating bentonitic clay quality percentage composition is (2%, 4%), (4%, 6%), (6%, 8%) and (8%, 10%) are respectively corresponding interval titrimetric factor K and titration constant B.
When the ring inner region of the light blue halo in described outer ring was filled, the various filling algorithms that conventional images is handled all were suitable for, as line sweep filling algorithm, four-way connected region seed fill algorithm, eight to the connected region seed fill algorithm; Can be referring to Sun Jiaguang etc. computer graphics (third edition) [M]. Beijing: publishing house of Tsing-Hua University, 1998.
The present invention is directed to bentonite blue suction quantity test on the foundry production line and the effective bentonite content mensuration in the clay old sand, can realize on computers, input manually initially splashes into value, the full-automatic setting and operation, automatically gather and drip the spot image and judge final titration end-point, can calculate bentonitic effective bentonite content of inhaling in blue amount and the old sand automatically, the result is accurate, alleviate experimenter's labour intensity, improved the accuracy of judging titration end-point.
Description of drawings
Fig. 1 is a FB(flow block) of the present invention;
Fig. 2 is the image processing step FB(flow block).
Embodiment
As shown in Figure 1, the present invention comprises the sample solution treatment step in proper order, forms the mixed liquor step, drips spot image acquisition step and image processing step.
The process of image processing step as shown in Figure 2.
The present invention is further described below in conjunction with embodiment.
Embodiment 1: the bentonite blue suction quantitative determination
One. solution treatment steps: with 0.2g bentonitic clay sample, massfraction is 1% sodium pyrophosphate solution 20mL and the heating of distilled water 50mL mixed solution, and solution boils and stops heating after 5 minutes, is stirred to solution and is uniformly dispersed;
Two. form the mixed liquor step: daily bentonitic clay methylene blue examination value is 38mL, estimating first, the methylene blue titer is 30mL, in the bentonitic clay sample solution of handling well, quantitatively pipette mass percentage concentration and be 0.2% pure methylene blue solution 30mL and stir and form mixed liquor, change step 4;
Three. quantitatively pipette the reagent step: in the bentonitic clay sample solution of handling well, quantitatively pipette mass percentage concentration and be 0.2% pure methylene blue solution and stir and form mixed liquor; The area that calculates according to the process 5.4 of step 5 is than the amount of pipetting of T control methylene blue, when area than T less than 8%, the amount of pipetting is each 1mL, when area than T 8～11% the time, the amount of pipetting is each 0.5mL, when area than T greater than 11% the time, the amount of pipetting is each 0.1mL, changes step 4;
Four. drip the spot image acquisition step: titration 0.1mL mixed liquor forms and drips spot to the middling speed quantitative filter paper, utilizes the industrial camera collection to drip the spot image;
Five. image processing step: carry out Digital Image Processing to dripping the spot image, calculate the area ratio of light blue halo in outer ring and inner ring mazarine spot, judge that whether the area ratio is more than or equal to 15%; Be then to be judged as titration end-point, add up total methylene blue titer, quantitatively pipette the reagent step otherwise change;
The final titer of present embodiment is 36mL, and then the blue amount of this bentonitic suction is 36g.
Embodiment 2: the effective bentonite content in the clay old sand is measured
One. solution treatment steps: with 5g clay old sand, the massfraction for preparing is the old sand mixed solution heating of 1% sodium pyrophosphate solution 20mL and distilled water 50mL, and solution boils and stops heating after 5 minutes, is stirred to solution and is uniformly dispersed;
Two. form the mixed liquor step: daily old sand methylene blue adsorption testing value is 85mL, estimating first, the methylene blue titer is 70mL, in the old sand solution of handling well, quantitatively pipette mass percentage concentration and be 0.2% pure methylene blue solution 70mL and stir and form mixed liquor, change step 4;
Three. quantitatively pipette the reagent step: in the old sand solution of handling well, quantitatively pipette mass percentage concentration and be 0.2% pure methylene blue solution and stir and form mixed liquor, the area that calculates according to the process 5.4 of step 5 is than the amount of pipetting of T control methylene blue, when area than T less than 8%, the amount of pipetting is each 1mL, when area than T 8～11% the time, the amount of pipetting is each 0.5mL, when area than T greater than 11% the time, the amount of pipetting is each 0.1mL, changes step 4;
Four. drip the spot image acquisition step: titration 0.1mL mixed liquor forms and drips spot to the middling speed quantitative filter paper, utilizes the industrial camera collection to drip the spot image;
Five. image processing step: carry out Digital Image Processing to dripping the spot image, calculate the area ratio of light blue halo in outer ring and inner ring mazarine spot, judge that whether the area ratio is more than or equal to 15%, be then to be judged as titration end-point, add up total methylene blue titer, quantitatively pipette the reagent step otherwise change;
The final titer of present embodiment is 80mL, the corresponding interval of bentonitic clay quality percentage composition is a bentonitic clay standard titration curve (6%, 8%) interval, the titrimetric factor K of this interval correspondence and titration constant B are respectively 12 and 2, effectively bentonite content value M=((80-2)/12) * 100%=6.5%.
Claims (1)
1. methylene blue adsorption testing method of bentonite, order comprises:
One. the sample solution treatment step: to the heating of bentonitic clay sample solution or clay old sand sample solution, stir, described bentonitic clay sample solution is that 1% sodium pyrophosphate solution 20mL and distilled water 50mL mix and constitute by 0.2g bentonitic clay, massfraction; Described clay old sand sample solution is that 1% sodium pyrophosphate solution 20mL and distilled water 50mL mix and constitute by 5g clay old sand, massfraction;
Two. form the mixed liquor step: pipette mass percentage concentration and be 0.2% pure methylene blue solution to bentonitic clay sample solution or clay old sand sample solution and stir and form mixed liquor, the amount of pipetting is that the clay old sand is inhaled blue 85% of the daily test volume of measuring on bentonitic clay or the production line, changes step 4;
Three. quantitatively pipette the reagent step: in bentonitic clay sample solution of handling well or clay old sand sample solution, quantitatively pipette mass percentage concentration and be 0.2% pure methylene blue solution and stir and form mixed liquor, the area that calculates according to the process 5.4 of step 5 is than the amount of pipetting of T control methylene blue, when area than T less than 8%, the amount of pipetting is each 1mL, when area than T 8～11% the time, the amount of pipetting is each 0.5mL, when area than T greater than 11% the time, the amount of pipetting is each 0.1mL, changes step 4;
Four. drip the spot image acquisition step: titration 0.1mL mixed liquor forms and drips spot to the middling speed quantitative filter paper, utilizes the industrial camera collection to drip the spot image;
Five. image processing step: carry out Digital Image Processing to dripping the spot image, order comprises following process:
5.1. the spot picture breakdown of dripping that will collect becomes red, green and blue triple channel image;
5.2. red, green and blue triple channel image are carried out the gray-scale value subtraction, obtain the light blue halo in outer ring:
Gray values of pixel points in the red channel image is deducted the gray-scale value of corresponding pixel points in the green channel image, carries out following computing again, obtain transfer image acquisition, its gray values of pixel points P:
P＝α×(R-G)+β，α＝0.1～3，β＝0～256；
Gray values of pixel points in the transfer image acquisition is deducted the gray-scale value of corresponding pixel points in the blue channel image, carries out following computing again, obtain the light blue halo in outer ring, its gray values of pixel points Q:
Q＝γ×(P-B)+λ，γ＝0.1～3，λ＝0～256；
In the formula: R, G, B represent the gray values of pixel points in redness, green and the blue triple channel respectively, and when a spot image effect was dark partially, α and γ span were at 1～3, and a spot image is dark more, and value is big more; When a spot figure kine bias was bright, α and γ span were at 0.1～1, and a spot image is bright more, and value is more little;
β＝α×|(R-G)|
min，λ＝γ×|(P-B)|
min；
Obtain complete spot image 5.3. fill:
According to the light blue halo gray values of pixel points in outer ring, use filling algorithm the ring inner region of the light blue halo in described outer ring is filled, obtain complete spot image R
F
5.4. calculate the area ratio of light blue halo in outer ring and inner ring mazarine spot:
The area S of the light blue halo in outer ring
QArea S with inner ring mazarine spot
DBe respectively:
S
Q＝f(d)×∫S
Q(d)，
S
D＝S
F-S
Q，
Wherein, S
FArea for complete spot:
S
F＝f(d)×∫S
F(d)，
The area of light blue halo in outer ring and inner ring mazarine spot than T is:
T＝S
Q/S
D，
In the formula: d is the resolution of digital camera, and f (d) is the single elemental area under the corresponding digital camera resolution, ∫ S
Q(d) be the number of outer ring pixel that light blue halo comprises, ∫ S
F(d) for comprising the number of pixel in the complete spot region;
5.5. whether the area of judging described light blue halo and inner ring mazarine spot more than or equal to 15%, is then to turn over journey 5.6 than T, quantitatively pipettes the reagent step otherwise change;
5.6. the termination titration process calculates and always moves liquid measure value V:
V＝V
1+V
2+……V
i+……+V
N，
In the formula, V
1Be the pure methylene blue solution of the described step 2 amount of pipetting, V
iBe the i time amount of pipetting of the pure methylene blue solution of described step 3, V
NBe the pure methylene blue solution of the described step 3 amount of pipetting for the last time, i, N are natural number; Always move liquid measure value V and be bentonite blue suction quantity; If the effective bentonite content of test clay old sand is then proceeded process 5.7;
5.7. calculate effective bentonite content;
According to always moving the corresponding interval range that liquid measure value V judges the effective bentonite content of clay old sand, determine corresponding titrimetric factor K and titration constant B, with K, B substitution following formula, calculate effective bentonitic clay quality percentage composition M=((V-B)/K) * 100%,
B, K are following to be determined: get fresh sand and bentonitic recombined sample 5g, measure bentonitic clay quality percentage composition in the recombined sample and be respectively 2%, 4%, 6%, 8% and blue the measuring of suction of 10% o'clock recombined sample, draw bentonitic clay standard titration curve; Rate of curve and y y-intercept when the corresponding interval of calculating bentonitic clay quality percentage composition is (2%, 4%), (4%, 6%), (6%, 8%) and (8%, 10%) are respectively corresponding interval titrimetric factor K and titration constant B.
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