CN103674868A - Method for determining content of silicon dioxide in rubber through spectrophotometer - Google Patents
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Abstract
The invention relates to a method for determining the content of silicon dioxide in rubber through a spectrophotometer. The method comprises the steps as follows: subjecting a rubber sample to ashing treatment; adding potassium hydroxide into the ashed sample for treatment so as to convert silicon in the sample into soluble silicate; then reacting a silicon-containing solution with ammonium molybdate in a hydrochloric acid medium; then using ammonium ferrous sulfate for reducing a reaction product in the last step to silicon molybdenum blue, and measuring the absorbance of the silicon molybdenum blue in a position with a set wavelength of 700-880 nm. The method is applied to all rubber except silicon-containing rubber.
Description
Technical field
The present invention relates to a kind of method of measuring the dioxide-containing silica in rubber, more specifically, relate to a kind of spectrophotometer that utilizes and use silicon molybdenum blue method to measure the method for the dioxide-containing silica in rubber.
Background technology
Silicon dioxide is extensively present in occurring in nature, has jointly formed rock with other mineral.Naturally occurring silicon dioxide is also silica, is a kind of solid of hard infusibility.Quartzy principal ingredient is also silicon dioxide, and transparent quartz crystal is exactly the crystal that we often say.Having many uses of silicon dioxide, the fibre-optic primary raw material of high-performance communication material having been used is at present exactly silicon dioxide.General purer quartz can be used to manufacture quartz glass.Quartz glass is usually used in manufacturing resistant to elevated temperatures chemical apparatuses.Crystal is commonly used to manufacture vitals, the optical instrument of electronics industry, is also used for making advanced industrial product and lens etc.
At present, measuring silicon dioxide has Lung biopsy, waves arching pushing, gravimetric method, molybdenum yellow or silicon molybdenum blue photometry, volumetric method and spectroscopic methodology that is:.If the content of silicon dioxide is more than 98% in sample, application hydrofluorite volatilization weight difference subtraction (waving arching pushing) is measured SiO
2content; If the content of silicon dioxide is between 20%～98% in sample, can measure by gravimetric method; If the content of silicon dioxide is between 0.5-10% in sample, can measure by photometry; If the content of silicon dioxide is more than 0.2% in sample, can measure by volumetric method; If the dioxide-containing silica in sample lower than 0.2% time, just need select spectrum, mass spectrum quasi-instrument to measure.
These the five kinds methods of measuring dioxide-containing silica respectively have relative merits, and the selection of concrete grammar also will be according to the content of silicon dioxide, sample mineral composition, and accuracy requirement, analytical cycle etc. considers, and makes suitable assay method.
Along with the heavy demand of people to green tire, environmental protection tire, high-performance tire, the application of white carbon (hydrated SiO 2) is more and more extensive.White carbon can be used as reinforcing agent, can form binding system with other component, also can be used as the carrier of some adjuvant, be mainly used in the important tire position formulas such as tyre surface, triangle, belt, bringing into play very important effect, therefore in tire formulation dissects, the accurate Fast Measurement of dioxide-containing silica is also more and more important.
In the measurement rubber generally adopting in rubber industry at present, the method for dioxide-containing silica is ASTM D297-1993(2006) mensuration of dioxide-containing silica in the standard test method-chemical analysis (Standard Test Methods for Rubber Products-Chemical Analysis) of rubber and GB/T 18174-2000 rubber.The former adopts to wave arching pushing, and the latter is that arching pushing is waved in employing and silicon molybdenum blue photometry combines.The latter is on the former basis, increased the detection of soluble silicate in sample, improved accuracy, but still had following shortcoming: (1) need to measure respectively the silicon dioxide of insoluble silicon dioxide and mensuration dissolubility silicic form, introduced 2 components, error is larger; (2) testing process is complicated, and complex operation is consuming time; (3) detection vessel used adopt platinum crucible, expensive; (4) in testing process, need to wave the silicon tetrafluoride that sheds, environmental pollution is larger, higher to human injury.
Therefore, need a kind of more succinct, fast, accurately, cost is lower, environmental pollution is less, the detection method lower to human injury.
Summary of the invention
The object of the invention is to set up a kind of method of effectively measuring fast dioxide-containing silica in rubber.
To achieve these goals, the present inventor has developed a kind of method of measuring dioxide-containing silica in rubber, and the method is applicable to all rubber except silicon rubber.According to the method for dioxide-containing silica in mensuration rubber of the present invention, comprise: rubber sample is carried out to ashing processing; In the sample of processing to ashing, add potassium hydroxide to process that silicon is wherein converted into soluble silicate; Then in hydrochloric acid medium, make siliceous solution and ammonium molybdate reaction; Then with iron ammonium sulfate, upper step reaction product is reduced to silicon molybdenum blue, in the setting wavelength place of 700～880nm, measures its absorbance.
Particularly, according to the method for the dioxide-containing silica in mensuration rubber of the present invention, comprise the steps:
1, drawing standard curve
Accurately take benchmark silicon dioxide in crucible, add potassium hydroxide, be heated to whole meltings, add water extraction it is all dissolved, be then mixed with silicon dioxide standard solution;
Accurately measure the silicon dioxide standard solution of different volumes in volumetric flask, adding hydrochloric acid to make pH is about 1.0-1.5, adds ammonium molybdate aqueous solution, after standing, add ferrous sulphate aqueous ammonium, constant volume, measures drawing standard curve in the setting wavelength place of 700～880nm;
2, sample preparation and measurement
Accurately take sample and be placed in crucible, at 550 ℃ ± 25 ℃ ashing complete, then add potassium hydroxide, be heated to whole meltings, add water extraction it all dissolved, be then mixed with sample solution;
Accurately measure sample solution in volumetric flask, adding hydrochloric acid to make pH is about 1.0-1.5, adds ammonium molybdate aqueous solution, adds ferrous sulphate aqueous ammonium after standing, and constant volume is measured in the setting wavelength place of 700～880nm;
3, calculate
Solution absorbance value calculates the concentration C of silicon dioxide in sample solution on typical curve per sample
t;
According to formula (1), calculate the content of silicon dioxide in rubber:
SiO
2%=C
t* V*100/m formula (1)
C
tthe concentration of silicon dioxide in the-sample solution that detects, mg/L;
The volume of V-sample solution, L;
The quality of m-rubber, mg.
In the methods of the invention, potassium hydroxide is for silicon dioxide is converted into soluble silicate, and the approximately 5-20 that its consumption is silica weight doubly, is preferably about 8-10 doubly.
In the methods of the invention, hydrochloric acid, for the pH of test solution is adjusted to about 1.0-1.5, is preferably approximately 1.2, makes silicon dioxide be converted into silicic acid.Preferably use the hydrochloric acid of 1:1.
In the methods of the invention, ammonium molybdate is used for and silica reaction, generates yellow soluble silicon-molybdenum heteropoly acid [H
4si (Mo
3o
10)
4].The concentration of ammonium molybdate aqueous solution is preferably 30g/L-50g/L, and preferably the concentration of ammonium molybdate aqueous solution is about 40g/L.
In the methods of the invention, iron ammonium sulfate is used for the soluble silicon-molybdenum heteropoly acid [H of yellow
4si (Mo
3o
10)
4] be reduced to silicon molybdenum blue.1:2-1:6, preferably the mol ratio of ammonium molybdate and ferrous sulfate amine is 1:5.The concentration of ferrous sulphate aqueous ammonium is 30g/L-50g/L, and the concentration of the ferrous amine aqueous solution of preferably sulfuric acid is about 40g/L.
In the methods of the invention, described crucible can be any suitable crucible, and such as platinum crucible, nickel crucible etc., is preferably nickel crucible.The in the situation that of nickel crucible, can reduce costs.
The silicon dioxide concentration of standard solution scope that the inventive method is particularly suitable for drawing standard curve is below 5.0mg/L, be preferably 0.1～5.0mg/L, in the sample solution that is particularly suitable for measuring, the concentration of silicon dioxide is, below 4.0mg/L, to be preferably 0.1～4.0mg/L.
In the methods of the invention, the order of the step of the step of described drawing standard curve and sample preparation and measurement is unrestricted, for example can first carry out the step of drawing standard curve, carry out again the step of sample preparation and measurement, also can first carry out the step of sample preparation and measurement, carry out again the step of drawing standard curve, or both carry out simultaneously.
In the methods of the invention, preferred beaker used and volumetric flask are plastic products, to avoid the pollution of silicon dioxide in glass.
In one of the present invention preferred embodiment, the inventive method comprises:
Step 1: the preparation of silicon dioxide standard reserving solution
Accurately take about 0.1g benchmark silicon dioxide in nickel crucible, add 1g potassium hydroxide, on electric furnace, be heated to whole meltings, add water extraction it is all dissolved, be transferred in 100mL volumetric flask, constant volume shakes up to prepare the silicon dioxide standard reserving solution of the about 950mg/L～1100mg/L of concentration;
Step 2: the preparation of silicon dioxide standard solution
Accurately pipette 10mL silicon dioxide standard reserving solution, be settled to 100mL volumetric flask with the silicon dioxide standard solution of the about 95mg/L～110mg/L of preparation concentration;
Step 3: the drafting of silicon dioxide typical curve
Accurately measure 0.0,0.5,1.0,1.5,2.0,2.5mL silicon dioxide standard solution is in 50mL volumetric flask, add 1:1 hydrochloric acid 0.85mL, shake up, add ammonium molybdate aqueous solution (40g/L) 5mL, shake up, place 15min, then add iron ammonium sulfate (40g/L) aqueous solution 10mL, shake up constant volume, use ultraviolet-visible spectrophotometer to measure in the setting wavelength place of 700～880nm, drawing standard curve;
Step 4: take 100.0mg-150.0mg and cut thin sample, be accurate to 0.1mg, be placed in the nickel crucible of capacity suitable, complete by the ashing at 550 ℃ ± 25 ℃ of GB/T 4498-1997A method;
Step 5: after cooling, add 1g potassium hydroxide, remaining operation is identical with the preparation of step 1 silicon dioxide standard reserving solution, obtains sample solution;
Step 6: get solution in 1.0mL step 5 in 50mL volumetric flask, add 1:1 hydrochloric acid 0.83mL, shake up, add ammonium molybdate aqueous solution (40g/L) 5mL, shake up, place 15min, then add ferrous sulphate aqueous ammonium (40g/L) 10mL, shake up constant volume;
Step 7: start ultraviolet-visible spectrophotometer, instrument stabilizer at least starts to measure after half an hour.Take 0 of typical curve be blank, distilled water is reference, the setting wavelength place at 700～880nm, measures.
Step 8: calculate dioxide-containing silica
First according to the silica concentration C in typical curve calculation sample solution
t, then according to formula below, calculate the dioxide-containing silica in rubber sample:
Computing formula: SiO
2, %=C
t* V*100/m
C
tthe concentration of silicon dioxide in the-sample solution that detects, mg/L;
V-sample solution volume, L;
The quality of m-rubber, mg.
Beneficial effect:
The method according to this invention and current national standard method (GB/T 18174-2000) are carried out to strengths and weaknesses analysis, the results are shown in Table 1.
Table 1
As can be seen from Table 1: (1) this method is not used hydrofluorite, pollution on the environment and the injury to human body have been reduced.
(2) the mensuration wavelength coverage that this method is chosen is very wide, can choose suitable wavelength according to actual conditions and measure, so this method to have sampling amount few, the feature that measurement range is wide.
(3) this method crucible used is nickel crucible, and beaker and volumetric flask require to be plastics, reduces the pollution of silicon dioxide.
(4) this method replaces five aqueous sodium carbonates and potassium acid sulfate as melting agent with potassium hydroxide, make silicon dioxide all be converted into mensuration dissolubility silicic, compare with the mensuration that adopts mode that photometry combines with gravimetric method to carry out dioxide-containing silica in GB/T 18174-2000 GB, more succinct, fast, accurately.
Therefore, the method according to this invention accurately Quick Measuring make the content of silicon dioxide in rubber.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated.These embodiment are only for purpose of explanation, and do not limit the scope of the invention and essence.
The experimental facilities model and the manufacturer that in the embodiment of the present invention, use see the following form shown in 1.
Table 2 experimental facilities model and manufacturer
| Title and model | Manufacturer |
| GZX-9070MBE baking oven | BOXUN |
| MARS240/50 microwave Muffle furnace | CEM U.S. training peace |
| SX2-4-10 high temperature box type resistance furnace | Shanghai Medical Equipment Plant of Bo Xun Industrial Co., Ltd. |
| AB204-S balance | METTLER?TOLEDO |
| Uitra-6600A ultraviolet-visible spectrophotometer | RIGOL |
Preparation Example 1: the preparation of vulcanized rubber A
Formula 1(mass parts):
Component 1:
Component 2:
Sulphur: (Puyang are Simon Rex Chemical Co., Ltd. not) 1.5,
Accelerator CZ: (Flexsys (Flexsys)) 1.2;
Vulcanized rubber preparation technology: in 1.6 liters of Banbury Banbury mixeies (production of FARREL company), add component 1, be warming up to gradually 160 ℃ and mix 5 minutes, thereby obtain masterbatch, and described masterbatch is cooled to below 90 ℃; Then use XK-160 opening rubber mixing machine (production of Qingdao Xin Chengyiming rubber manufacturing machinery company limited) to blending ingredients 2 in masterbatch, at the temperature of 70 ℃, said mixture is carried out to mixing 10min, thereby obtain rubber composition; By the composition being obtained by said method, on BH-25T vulcanizing press, vulcanized rubber flat board or thin slice are made in (production of Zhen Wu town, Jiangdu district Bo Hai test machines factory) moulding (160 ℃ of curing temperatures, cure time 30min), make vulcanized rubber sample A.The gross mass of sample A is 162 parts, and dioxide-containing silica theoretical value is 2.35%.
Dioxide-containing silica in embodiment 1, the method according to this invention working sample A
(1) drawing standard curve
Step 1, accurately take 109.2mg benchmark silicon dioxide in nickel crucible, add 1g potassium hydroxide, be heated to whole meltings on electric furnace, add water extraction it is all dissolved, be transferred in 100mL volumetric flask, constant volume shakes up.The concentration of this standard reserving solution is 1092mg/L.
Step 2, accurately pipette 10mL silicon dioxide standard reserving solution, be settled to 100mL volumetric flask, the concentration of this standard solution is 109.2mg/L.
Step 3, accurately measure 0.0,0.2,0.4,0.6,0.8,1.0mL silicon dioxide standard solution in 50mL volumetric flask, add 1:1 hydrochloric acid 0.85mL, shake up, add ammonium molybdate aqueous solution (40g/L) 5mL, shake up, place 15min.Then add iron ammonium sulfate (40g/L) aqueous solution 10mL, shake up constant volume.In 811nm place, measure successively uv absorption, measurement result is as follows.
Table 3
With the above results drawing standard curve, normalization method obtains typical curve formula: Y=0.3261X+0.0292 R
2=0.9993
(2) sample pre-treatments and test
Step 4, by Preparation Example 1 preparation vulcanized rubber sample A be cut into about 1mm
2the granule of left and right, takes respectively Duplicate Samples 1(141.1mg) sample (being accurate to 0.1mg) of and Duplicate Samples 1 ' (149.8mg), be placed in the nickel crucible of 100mL, the ashing at 550 ℃ ± 25 ℃ of use microwave Muffle furnace is complete.
Step 5, cooling after, add 2g potassium hydroxide, on electric furnace, be heated to whole meltings, add water extraction it all dissolved, be transferred in 100mL volumetric flask, constant volume shakes up.
Step 6, get solution in 1.0mL step 5 in 50mL volumetric flask, add 1:1 hydrochloric acid 0.85mL, shake up, add ammonium molybdate aqueous solution (40g/L) 5mL, shake up, place 15min.Then add ferrous sulphate aqueous ammonium (40g/L) 10mL, shake up constant volume.
Step 7, startup ultraviolet-visible spectrophotometer, instrument stabilizer at least starts to measure after half an hour.Take 0 of typical curve be blank, distilled water is reference, at 811nm place, measures.Calculate dioxide-containing silica, the results are shown in following table 5.
Comparative example 1: according to the dioxide-containing silica in GB/T 18174-2000 working sample A
(1) sample pre-treatments
Step 1, taking 1.0023g(m) the vulcanized rubber sample A of preparation in the Preparation Example 1 that shredded is in porcelain crucible, method by the rubber ash content calcination of the regulation of GB/T4498-1997 is carried out calcination, uses microwave Muffle furnace ashing at 550 ℃ ± 25 ℃ complete.
Step 2, with glass bar, ash is divided into fine powder, take 3g potassium acid sulfate and pour porcelain crucible into, with glass bar, stir until mix, claim again on potpourri that 1g potassium acid sulfate is covered in ash content and potassium acid sulfate, get fritter quantitative filter paper glass bar is cleaned, move into melting 25min. in 650 ℃ ± 25 ℃ muffle furnaces after filter paper is dropped into crucible
After step 3, sample melted are cooling, in crucible, add proper amount of boiling water, after frit is separated with crucible, move in 100mL beaker, in crucible, add 15mL hydrochloric acid solution (volume ratio 1:5) again, heating for dissolving residue, moves into beaker in the lump, with boiling water washing crucible and lid, washing lotion is incorporated to beaker.Heating beaker, to micro-boiling, is uniformly dispersed frit dissolving and insolubles, and cooling rear use at a slow speed quantitative filter paper is filtered.With warm water washing beaker and insolubles, extremely with liquor argenti nitratis ophthalmicus, check without till chlorion.Gained filtrate A, retains this filtrate for the mensuration of mensuration dissolubility silicic.
(2) mensuration of insoluble silicon
Step 4, insolubles is moved in platinum crucible together with filter paper, carbonization on electric furnace now, then move into that in 850 ℃ of muffle furnaces, calcination is to constant weight, m weighs
1.In platinum crucible, add several salpeter solutions and 10mL hydrofluorite, at the medium and small fire of fuming cupboard, be heated near dry.By in 850 ℃ of muffle furnaces of platinum crucible immigration, calcination is to constant weight, m weighs
2.
Dioxide-containing silica X in step 5, calculating rubber
1with mass percent (m/m), represent, by formula (2)
In formula: the quality of platinum crucible and content before m1--hydrofluoric acid treatment, g;
The quality of platinum crucible and residue after m2--hydrofluoric acid treatment, g;
The quality of m--sample, g.
(3) mensuration of soluble silicon
The drafting of step 6, typical curve
Draw blank reagent solution 10mL, move into respectively in 50mL volumetric flask, the silicon dioxide standard solution that adds respectively 0.00,0.15,0.30,0.45,0.60,0.75, obtains in embodiment 1 step 2 of 0.90mL with microdial suction pipe.Add 5mL ammonium molybdate solution, place 15min complete to colour developing, adding 10mL oxalic acid-sulfuric acid mixed solution shakes up, add immediately 5mL l ferrous ammonium sulfate solution, be diluted with water to scale, park 15min, on spectrophotometer, under 650nm wavelength, use 1cm absorption cell, with the zeroing of reagent reference solution, difference bioassay standard solution series absorbance, measurement result is as follows.
Table 4
With the above results drawing standard curve.Normalization method obtains typical curve formula: Y=0.3545X+0.0153 R
2=0.999
The mensuration of step 7 filtrate absorbance
The filtrate A that use is obtained by step 3 moves in 250mL volumetric flask, is diluted with water to scale, shakes up.Accurately remove 10mL filtrate in 50mL volumetric flask, by the absorbance of the colour developing of step 6 operation steps, constant volume and mensuration silicon dioxide.On typical curve, check in the content m of silicon dioxide
3, the mass percent X of calculating soluble silica
2.
(4) the mass percent X of total silicon dioxide calculates as shown in the formula (3):
M
1--the quality of platinum crucible and content before hydrofluoric acid treatment, g;
M
2--the quality of platinum crucible and residue after hydrofluoric acid treatment, g;
M
3--the dioxide-containing silica checking on typical curve, mg;
The quality of m--sample.
Test result is in Table 5.
Table 5
Preparation Example 2: the preparation of vulcanized rubber B
Formula 2(mass parts):
Component three: sulphur (Puyang are Simon Rex Chemical Co., Ltd. not) 2.2;
Accelerator CZ (Flexsys) 1.8;
Accelerator D PG-80(Lianyungang Lianlian Chemicals Co., Ltd.) 0.75.
Vulcanized rubber preparation technology: in 1.6 liters of Banbury Banbury mixeies (production of FARREL company), add component 1, be warming up to gradually 160 ℃ and mix 6 minutes, obtain one section of elastomeric compound, park 20 hours in room temperature; Then continue in Banbury Banbury mixer, be warming up to gradually 145 ℃ one section of elastomeric compound and component 2 are mixed 5 minutes, thereby obtain masterbatch, and described masterbatch is cooled to below 90 ℃; Then use XK-160 opening rubber mixing machine (production of Qingdao Xin Chengyiming rubber manufacturing machinery company limited) to blending ingredients 3 in masterbatch, at the temperature of 70 ℃, said mixture is carried out to mixing 10min, thereby obtain rubber composition; By the composition being obtained by said method, on BH-25T vulcanizing press, vulcanized rubber thin slice is made in (production of Zhen Wu town, Jiangdu district Bo Hai test machines factory) moulding (160 ℃ of curing temperatures, cure time 30min), makes vulcanized rubber test sample B.The gross mass of sample B is 265.25 parts, wherein in Si69, contains 10% silicon, with SiO
2massfraction be added and show that dioxide-containing silica theoretical value is 27.75%.
Embodiment 2, according to the inventive method, measure the dioxide-containing silica in rubber sample B
Vulcanized rubber sample B is cut into about 1mm
2the granule of left and right.Accurately take sample 3(130.5mg), Duplicate Samples 3 ' (102.2mg), except accurately measuring 0.0,0.5,1.0,1.5,2.0 in step 3,2.5mL silicon dioxide standard solution, and step 7 with ultraviolet-visible pectrophotometer respectively beyond 700nm, 770nm, 850nm bioassay standard solution and sample solution, other operation stepss are identical with the operation steps of embodiment 1.The results are shown in following table 6.
Table 6
Claims (10)
1. a method of measuring the dioxide-containing silica in rubber, comprises the steps:
(1), drawing standard curve
Accurately take benchmark silicon dioxide in crucible, add potassium hydroxide, be heated to whole meltings, add water extraction it is all dissolved, be then mixed with silicon dioxide standard solution;
Accurately measure the silicon dioxide standard solution of different volumes in volumetric flask, adding hydrochloric acid to make pH is 1.0-1.5, adds ammonium molybdate aqueous solution, adds ferrous sulphate aqueous ammonium after standing, and constant volume is measured drawing standard curve in the setting wavelength place of 700～880nm;
(2), sample preparation and measurement
Accurately take sample and be placed in crucible, at 550 ℃ ± 25 ℃ ashing complete, then add potassium hydroxide, be heated to whole meltings, add water extraction it all dissolved, be then mixed with sample solution;
Accurately measure sample solution in volumetric flask, adding hydrochloric acid to make pH is 1.0-1.5, adds ammonium molybdate aqueous solution, adds ferrous sulphate aqueous ammonium after standing, and constant volume is measured in the setting wavelength place of 700～880nm;
(3), calculate
Solution absorbance value calculates the concentration C of silicon dioxide in sample solution on typical curve per sample
t;
According to formula (1), calculate the content of silicon dioxide in rubber:
SiO
2%=C
t* V*100/m formula (1)
C
tthe concentration of silicon dioxide in the-sample solution that detects, mg/L;
The volume of V-sample solution, L;
The quality of m-rubber, mg.
2. according to the process of claim 1 wherein, the middle potassium hydroxide consumption of step (1) and step (2) is 5-20 times of silica weight.
3. according to the process of claim 1 wherein, the middle potassium hydroxide consumption of step (1) and step (2) is 8-10 times of silica weight.
4. according to the process of claim 1 wherein, the concentration of ammonium molybdate aqueous solution is 30g/L-50g/L.
5. according to the process of claim 1 wherein, the concentration of ferrous sulphate aqueous ammonium is 30g/L-50g/L.
6. according to the process of claim 1 wherein, the ammonium molybdate adding and the mol ratio of iron ammonium sulfate are 1:2-1:6.
7. according to the process of claim 1 wherein, described crucible is nickel crucible.
8. according to the process of claim 1 wherein, the silicon dioxide concentration of standard solution scope that is applicable to drawing standard curve is below 5.0mg/L.
9. according to the process of claim 1 wherein, in the sample solution that is applicable to measuring, the concentration of silicon dioxide is below 4.0mg/L.
10. according to the method for claim 1, comprise the steps:
Step 1: the preparation of silicon dioxide standard reserving solution
Accurately take 0.1g benchmark silicon dioxide in nickel crucible, add 1g potassium hydroxide, on electric furnace, be heated to whole meltings, adding water extraction all dissolves it, be transferred in 100mL volumetric flask, it is that 950mg/L～1100mg/L(embodiment is 1092mg/L that constant volume shakes up to prepare concentration) silicon dioxide standard reserving solution;
Step 2: the preparation of silicon dioxide standard solution
Accurately pipette 10mL silicon dioxide standard reserving solution, be settled to 100mL volumetric flask with the silicon dioxide standard solution of the about 95mg/L～110mg/L of preparation concentration;
Step 3: the drafting of silicon dioxide typical curve
Accurately measure 0.0,0.5,1.0,1.5,2.0,2.5mL silicon dioxide standard solution is in 50mL volumetric flask, add 1:1 hydrochloric acid 0.85mL, shake up, add ammonium molybdate aqueous solution (40g/L) 5mL, shake up, place 15min, then add iron ammonium sulfate (40g/L) aqueous solution 10mL, shake up constant volume, use ultraviolet-visible spectrophotometer to measure in the setting wavelength place of 700～880nm, drawing standard curve;
Step 4: take 100.0mg-150.0mg and cut thin sample, be accurate to 0.1mg, be placed in the nickel crucible of capacity suitable, complete by the ashing at 550 ℃ ± 25 ℃ of GB/T 4498-1997A method;
Step 5: after cooling, add 1g potassium hydroxide, remaining operation is identical with the preparation of step 1 silicon dioxide standard reserving solution, obtains sample solution;
Step 6: get solution in 1.0mL step 5 in 50mL volumetric flask, add 1:1 hydrochloric acid 0.83mL, shake up, add ammonium molybdate aqueous solution (40g/L) 5mL, shake up, place 15min, then add ferrous sulphate aqueous ammonium (40g/L) 10mL, shake up constant volume;
Step 7: start ultraviolet-visible spectrophotometer, instrument stabilizer at least starts to measure after half an hour.Take 0 of typical curve be blank, distilled water is reference, the setting wavelength place at 700～880nm, measures;
Step 8: calculate dioxide-containing silica
First according to the silica concentration C in typical curve calculation sample solution
t, then according to formula below, calculate the dioxide-containing silica in rubber sample:
Computing formula: SiO
2%=C
t* V*100/m
C
tthe concentration of silicon dioxide in the-sample solution that detects, mg/L;
V-sample solution volume, L;
The quality of m-rubber, mg.
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| CN105866110A (en) * | 2016-03-28 | 2016-08-17 | 同济大学 | Detection agent for determining content of silica in water |
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| CN114034696A (en) * | 2021-12-07 | 2022-02-11 | 中国第一汽车股份有限公司 | Silicon content detection device and application thereof |
| CN114460018A (en) * | 2021-12-22 | 2022-05-10 | 内蒙古工业大学 | Method for measuring content of silicon dioxide in fly ash silicon extraction liquid |
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| CN105866110A (en) * | 2016-03-28 | 2016-08-17 | 同济大学 | Detection agent for determining content of silica in water |
| CN113447393A (en) * | 2020-03-28 | 2021-09-28 | 北京橡院橡胶轮胎检测技术服务有限公司 | Method for quantitatively determining content of silicon dioxide in silicone rubber |
| CN114034696A (en) * | 2021-12-07 | 2022-02-11 | 中国第一汽车股份有限公司 | Silicon content detection device and application thereof |
| CN114034696B (en) * | 2021-12-07 | 2024-03-15 | 中国第一汽车股份有限公司 | Silicon content detection device and application thereof |
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| CN114460018A (en) * | 2021-12-22 | 2022-05-10 | 内蒙古工业大学 | Method for measuring content of silicon dioxide in fly ash silicon extraction liquid |
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