CN107621519A - A kind of assay method to metal aluminum content in magnesia carbon brick - Google Patents
A kind of assay method to metal aluminum content in magnesia carbon brick Download PDFInfo
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- CN107621519A CN107621519A CN201710882813.1A CN201710882813A CN107621519A CN 107621519 A CN107621519 A CN 107621519A CN 201710882813 A CN201710882813 A CN 201710882813A CN 107621519 A CN107621519 A CN 107621519A
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Abstract
A kind of assay method to metal aluminum content in magnesia carbon brick, belong to metallic aluminium quantitative determination technical field.First prepare main agents, iodohydrin solution；Absolute ethyl alcohol；1+1 sulfuric acid；0.01~0.02mol/L EDTA standard liquids etc.；Sample is leached with iodohydrin solution, insoluble matter is filtered off after suction filtration, excessive EDTA standard liquids are added in filtrate, in the presence of acetic acid ammonium acetate buffer solution, with the excessive EDTA of copper sulphate standard liquid residual titration, sodium fluoride is added, boils the EDTA in displacement Al EDTA complex compounds, the EDTA displaced with the titration of copper sulphate standard liquid, the content of metallic aluminium in sample is determined with this.Advantage is, using iodohydrin as leaching liquid, selective extracts aluminium of the metallic aluminium without bringing other existence forms into, eliminates interference effect well, as a result accurately.
Description
Technical field
The invention belongs to metallic aluminium to quantitative determine technical field, more particularly to a kind of survey to metal aluminum content in magnesia carbon brick
Determine method.Leach especially with iodohydrin-villiaumite substitution EDTA volumetric methods are to the assay method of metal aluminum content in magnesia carbon brick.
Background technology
The primary raw material of magnesia carbon brick includes magnesia, graphite and organic bond.Various raw materials are first in high speed mixing smelting machine
Middle mixing, then by compressing, finally magnesia carbon brick is made in drying at a temperature of 200 DEG C or so.
Magnesia carbon brick is a kind of high-quality refractory material, because there is this kind of carbon-containing refractory article refractoriness height, anti-slag to invade performance
Good, the advantages that resistance to heat shocks is strong and high-temerature creep is small, application is widely available on electric furnace, converter and refining furnace, service life is big
Amplitude improves.To be burnt till simultaneously as magnesia carbon brick is not required to high temperature, save the energy, manufacture craft is simple, thus by many states in the whole world
The rapid popularization and application of family.
In recent years, the research to magnesia carbon brick deepened continuously, and research direction is increasingly extensive.Antioxidant research is exactly wherein one
Individual highly important research direction.The low wetability of carbon makes magnesia carbon brick have good resistance to slag and resist the ability of erosion, but
It is that carbon is easy to aoxidize at high temperature, magnesia carbon brick is destructurized after oxidation of coal, so, the addition of antioxidant can improve magnesia carbon brick
Corrosion resistance.Metallic aluminium powder is conventional antioxidant, and antioxidant metallic aluminium can be prior to the O in C and air2And CO2
Reaction.Antioxidant and slag, which react, to be formed magnesium aluminate spinel and olivine and can effectively weaken, prevent the oxidation of magnesia carbon brick,
Improve the ability of the anti-refining scouring of magnesia carbon brick.Therefore particularly significant is seemed to the measure of metal aluminum content in magnesia carbon brick.
At present, there is no national standard method to metal Al-single crystal in magnesia carbon brick, the method that reporting to look into has following several：
1) sodium hydroxide or hydrochloric acid leaching-EDTA volumetric methods.2) ferric trichloride leaching-EDTA volumetric methods.Above-mentioned 2 method is to utilize leaching
Liquid reacts with metallic aluminium, after the interference elements such as iron and aluminium element precipitation separation, substitutes-EDTA volumetric methods to drip with villiaumite
It is fixed, obtain metal aluminum content.But when containing aluminate in sample, the part chemical combination aluminium will be dripped simultaneously by acid or alkali soluble solution
It is fixed, content that is obtaining and being not all metallic aluminium.3) sodium hydroxide dissolves-determined hydrogen method.With sodium hydroxide come dissolved samples,
Measure reacts the volume of the hydrogen separated out by metallic aluminium and sodium hydroxide or pressure calculates the content of metallic aluminium indirectly.The method result
Accurately, but Hydrogen collection needs special equipment, and air-proof condition requires harsh, not easy to operate.
The content of the invention
It is an object of the invention to provide a kind of assay method to metal aluminum content in magnesia carbon brick.Solve in magnesia carbon brick
Metallic aluminium is difficult to the problem of accurate and effective is extracted and determined.
The present invention is leached using iodohydrin, and the metallic aluminium in sample is converted into aluminium ion, then substituted using villiaumite-
EDTA volumetric determination aluminium contents.
A kind of assay method to metal aluminum content in magnesia carbon brick, specific steps and parameter are as follows：
1st, main agents are prepared：50~100g/L iodohydrin solution；Absolute ethyl alcohol；1+1 sulfuric acid；30wt% peroxide
Change hydrogen；0.01~0.02mol/L EDTA (disodium ethylene diamine tetraacetate) standard liquid；0.2wt% methyl orange solution；ρ
0.90g/mL ammonium hydroxide；Acetic acid-ammonium acetate buffer solution, PH=4.5；0.2wt% PAN methanol solutions；0.01~
0.02mol/L copper sulphate standard liquid and sodium fluoride.
2nd, 0.25~0.5g samples are weighed in iodine flask, 50mL iodohydrin solution (50~100g/L) is added, is vibrating
On device vibrate 30~60min, remove it is dry filter in beaker, wash 3~5 times with absolute ethyl alcohol, into filtrate addition 1+1 sulphur
20~25mL of acid, low-temperature heat remove cooling to smokeing clogging, and add 30wt% 3~5mL of hydrogen peroxide, continue to be heated to purple
Cigarette is emitted to the greatest extent, and 100mL water is added after cooling, and 2~3min is boiled in heating, is moved into after cooling in 200mL volumetric flasks, quarter is diluted to water
Degree, mix.
3rd, divide and take the above-mentioned solution of 50mL in beaker, add 10~30mLEDTA standard liquids, need excessive 3~6mL during addition,
Add 1~2 drop 0.2wt% methyl orange solution, solution is adjusted to ammonium hydroxide (ρ 0.90g/mL) and just turned yellow, addition 15~
2~3min is boiled in 25mL acetic acid-ammonium acetate buffer solution, heating, removes the PAN 3~4mL of methanol solution for adding 0.2wt%, takes advantage of
Heat is in aubergine with copper sulphate standard liquid residual titration to solution, is not counted, and heats then plus after the stirring of 1~2g sodium fluorides and boils 2
~3min, then stable aubergine is titrated to as terminal using copper sulphate standard liquid, count lower reading.Metal aluminum content is calculated with this.
It is an advantage of the current invention that using iodohydrin as leaching liquid, selective extracts metallic aluminium without bringing into
The aluminium of other existence forms, interference effect is eliminated well, and it is easily operated, as a result accurately.
Embodiment
Embodiment 1
Leached using iodohydrin-villiaumite substitution EDTA volumetric methods to the assay method of metal aluminum content in magnesia carbon brick, specifically
Step and parameter are as follows：
1st, main agents are prepared
Iodohydrin solution (50g/L)；Absolute ethyl alcohol；1+1 sulfuric acid；30wt% hydrogen peroxide；0.01783mol/L's
EDTA standard liquids；0.2wt% methyl orange solution；Ammonium hydroxide (ρ 0.90g/mL)；Acetic acid-ammonium acetate buffer solution, is weighed
40g ammonium acetates are soluble in water, add 36% acetic acid 150mL, are diluted with water to 1000mL, mix；0.2wt% PAN methanol is molten
Liquid；0.01783mol/L copper sulphate standard liquid；Sodium fluoride.
2nd, 0.5000g samples are weighed in 300mL iodine flasks, add 50mL iodohydrin solution (50g/L), on the oscillator
Vibrate 30min, remove it is dry filter in 250mL beakers, wash 5 times with absolute ethyl alcohol, into filtrate addition 1+1 sulfuric acid
20mL, low-temperature heat remove cooling to smokeing clogging, and add 30wt% hydrogen peroxide 5mL, continue to be heated to purple cigarette and emit to the greatest extent, cold
But 100mL water is added afterwards, and 3min is boiled in heating, is moved into after cooling in 200mL volumetric flasks, scale is diluted to water, mixes.
3rd, divide and take the above-mentioned solution of 50mL to add 20mLEDTA standard liquids in 250mL beakers, add 1 drop 0.2wt% methyl
Orange solution, solution is adjusted to ammonium hydroxide (ρ 0.90g/mL) and just turned yellow, add 25mL acetic acid-ammonium acetate buffer solution, heating
2min is boiled, removes the PAN methanol solutions for adding 4mL 0.2wt%, while hot with copper sulphate standard liquid residual titration to solution in purple
Red, do not count, then plus after the stirring of 1g sodium fluorides heating boil 2min, then be titrated to copper sulphate standard liquid stablize it is purplish red
Color is terminal, counts lower reading.
3 magnesia carbon brick samples are chosen, are operated by above-mentioned experimental method, each sample independently determines 10 times, obtains metallic aluminium
Content, carries out precision test, and analysis result is shown in Table 1.Analysis result relative standard deviation, can between 0.37%~2.66%
See that precision is good.
The analysis result of the magnesia carbon brick Gold Samples category aluminium of table 1
In view of magnesia carbon brick does not have national standard sample, the not asserting value as degree of accuracy reference, therefore use and more may be used
The sodium hydroxide leaned on dissolves-determined hydrogen method method as a comparison, and this law is respectively adopted in same sample and hydrogen method is measured,
Analysis result is shown in Table 2.Analysis result difference is between -0.08%~0.13%, it is seen that the degree of accuracy is good.
This law of table 2 contrasts with hydrogen method analysis result
Claims (2)
1. a kind of assay method to metal aluminum content in magnesia carbon brick, it is characterised in that specific steps and parameter are as follows：
1) main agents are prepared：50~100g/L iodohydrin solution；Absolute ethyl alcohol；1+1 sulfuric acid；30wt% peroxidating
Hydrogen；0.01~0.02mol/L EDTA standard liquids；0.2wt% methyl orange solution；ρ 0.90g/mL ammonium hydroxide；Vinegar
Acid-ammonium acetate buffer solution；0.2wt% PAN methanol solutions；0.01~0.02mol/L copper sulphate standard liquid and fluorination
Sodium；
2) 0.25~0.5g samples are weighed in iodine flask, add 50mL iodohydrin solution, on the oscillator vibrate 30~
60min, remove it is dry filter in beaker, washed 3~5 times with absolute ethyl alcohol, into filtrate add 1+1 20~25mL of sulfuric acid,
Low-temperature heat removes cooling to smokeing clogging, and adds 30wt% 3~5mL of hydrogen peroxide, continues to be heated to purple cigarette and emits to the greatest extent, cooling
100mL water is added afterwards, and 2~3min is boiled in heating, is moved into after cooling in 200mL volumetric flasks, scale is diluted to water, mixes；
3) divide and take the above-mentioned solution of 50mL in beaker, add 10~30mLEDTA standard liquids, need excessive 3~6mL during addition, add 1
~2 drop 0.2wt% methyl orange solution, is adjusted to solution with ammonium hydroxide and just turns yellow, and adds 15~25mL acetic acid-ammonium acetate and delays
Rush solution, 2~3min is boiled in heating, removes the PAN 3~4mL of methanol solution for adding 0.2wt%, molten with copper sulphate standard while hot
Liquid residual titration to solution is in aubergine, is not counted, and heats then plus after the stirring of 1~2g sodium fluorides and boils 2~3min, then with copper sulphate
It is terminal that standard liquid, which is titrated to stable aubergine, counts lower reading；Metal aluminum content is calculated with this.
2. according to the method for claim 1, it is characterised in that acetic acid-ammonium acetate buffer solution described in step 1)
PH=4.5.
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