CN105388084B - The detection method of silicone content in a kind of Mn-rich slag - Google Patents
The detection method of silicone content in a kind of Mn-rich slag Download PDFInfo
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Abstract
The invention discloses a kind of detection method of silicone content in Mn-rich slag, including the dissolving of sample pretreatment, sample, acidifying, precipitation, filtration washing, calcination, cubage step.The method of the invention is at present without national standard and professional standard, in terms of the accuracy of testing result, the analytical procedure and parameter setting that the method for the invention uses, it is complete to be advantageous to sample dissolving, noresidue, without heterogeneous interference, reduce experimental error, testing result has good stability, reappearance and accuracy.In terms of detection speed, the method for the invention has the characteristics of analyze speed is fast, and detection cycle is short, and analysis efficiency is high, has not only saved detection time, alleviates the labor intensity of test analysis personnel, also reduces energy consumption, is advantageous to enterprise's cost efficiency.In terms of testing process, the method for the invention is simple to operate, easily learns well and understands, to test analysis personnel without excessive demand, has preferable popularizing application prospect.
Description
Technical field
The invention belongs to detection technique field, and in particular to the detection method of silicone content in a kind of Mn-rich slag.
Background technology
In smelting iron and steel production, a kind of Mn-rich slag is when producing high carbon ferromanganese using acid slag pracitice, slant acidity slag method
Byproduct, because wherein manganese, silicone content are higher, for improve resource utilization rate, the manganese in Mn-rich slag can be extract or
Person is used with manganese compound.
Because the content of manganese and silicon is higher in Mn-rich slag, and when smelting manganese-silicon due to rate of recovery problem, it is desirable to its
The content of manganese is greater than 40% in raw material, and the content of silicon also requires higher, therefore Mn-rich slag can be fully used as smelting manganese-silicon
Raw material, while it is also used as producing the raw material of manganese metal, can also be used as production blast furnace ferromanganese, electric furnace ferromanganese and low Carbon Manganese
The dispensing of iron.The Design of Chemical Composition of production is smelted for optimization, is enterprise's cost efficiency.Therefore the survey to silicone content in Mn-rich slag
Surely there is extremely important produce reality meaning.
Mn-rich slag main component is C, Si, Mn, S, P equal size.Therefore, it is necessary to research and develop a kind of accuracy height, stability
Good, analytical cycle is short, and testing cost is low, the detection method of the Mn-rich slag sample for silicone content >=10% that is particularly suitable for use in, to adapt to
Modernization smelt production to upgrading, drop this, the active demand of synergy.
The content of the invention
It is an object of the invention to provide a kind of detection method of silicone content in Mn-rich slag.
The object of the present invention is achieved like this, comprises the following steps：
A, sample is crushed to granularity≤0.125mm, in 105~110 DEG C of dry 1.5~2.5h to constant weight, weighed
0.2000g samples and 3.0~4.0g sodium carbonate-boric acid mixed flux are mixed, and melting 20~25min in 890~910 DEG C is melted
Melt thing, fused mass is dissolved in 30ml hydrochloric acid, it is limpid to be heated to solution in 60~90 DEG C, removes and naturally cools to 20~25
DEG C, 55~65ml perchloric acid is added, is heated to releasing perchloric acid white cigarette in 100~200 DEG C, cap upper surface ware, continue at 60~
80 DEG C of 20~25min of heating start to crystallize and present thick to the residue of smoke, remove and naturally cool to 50~60 DEG C, slowly
Add 15~25ml hydrochloric acid, then add 70~90ml 80~100 DEG C of hot water, then be added dropwise 0.6~1.2ml hydrogen peroxide it is molten
Liquid, heat 2~3min in 60~80 DEG C and obtain test solution a；
On the Medium speed filter paper that test solution a is filtered to the 12.5cm in glass funnel B, with the glass rod with rubber tip and 80~
100 DEG C of hydrochloric acid lotion washing beaker 5~6 times, washing lotion washes precipitation and filter paper on filter paper with 80~100 DEG C of hydrochloric acid lotion
Being dripped to by filtrate drop 3 on the surface plate for filling 1ml ammonium thiocyanate solution, ammonium thiocyanate solution is non-discolouring, then with 80~100 DEG C
Water washing and precipitating and filter paper 3 dripped to by filtrate drop on the surface plate for filling 1ml silver nitrate solutiones, silver nitrate solution is non-discolouring,
B must be precipitated；
C, precipitation b and filter paper are placed in the porcelain crucible of constant weight, porcelain crucible are placed in high temperature furnace, by the temperature of high temperature furnace
Degree rises to 1050~1150 DEG C, and the precipitation in porcelain crucible and filter paper are evaporated, are ashed, 1.5~2.5h of calcination, takes out porcelain earthenware
Crucible, 30~40 DEG C are cooled to, porcelain crucible is placed in drier and is cooled to 10~30 DEG C, weighing is calculated as follows to obtain in sample
Silicone content：
In formula：
m1--- precipitation and the quality of crucible, g；
m2--- the quality of crucible, g；
m0--- the quality of sample, g；
0.4674 --- silica is scaled the conversion coefficient of silicon.
Thus the content of silicon in Mn-rich slag is determined.Methods described has good accuracy, reappearance and stability, especially
Detected suitable for the Mn-rich slag silicone content of silicone content >=5%.
The analytical procedure and parameter setting that the present invention uses, it is complete to be advantageous to sample dissolving, noresidue, without heterogeneous interference,
Reduce experimental error, testing result has good stability, reappearance and accuracy.In terms of detection speed, the present invention
Methods described has the characteristics of analyze speed is fast, and detection cycle is short, and analysis efficiency is high, has not only saved detection time, alleviates
The labor intensity of test analysis personnel, also reduces energy consumption, is advantageous to enterprise's cost efficiency.In terms of testing process, the present invention
Methods described is simple to operate, easily learns well and understands, to test analysis personnel without excessive demand, has preferable popularizing application prospect.
Embodiment
With reference to embodiment, the present invention is further illustrated, but the present invention is not any limitation as in any way,
Based on present invention teach that any conversion or replacement made, belong to protection scope of the present invention.
The detection method of silicone content, comprises the following steps in Mn-rich slag of the present invention：
A, sample is crushed to granularity≤0.125mm, in 105~110 DEG C of dry 1.5~2.5h to constant weight, weighed
0.2000g samples and 3.0~4.0g sodium carbonate-boric acid mixed flux are mixed, and melting 20~25min in 890~910 DEG C is melted
Melt thing, fused mass is dissolved in 30ml hydrochloric acid, it is limpid to be heated to solution in 60~90 DEG C, removes and naturally cools to 20~25
DEG C, 55~65ml perchloric acid is added, is heated to releasing perchloric acid white cigarette in 100~200 DEG C, cap upper surface ware, continue at 60~
80 DEG C of 20~25min of heating start to crystallize and present thick to the residue of smoke, remove and naturally cool to 50~60 DEG C, slowly
Add 15~25ml hydrochloric acid, then add 70~90ml 80~100 DEG C of hot water, then be added dropwise 0.6~1.2ml hydrogen peroxide it is molten
Liquid, heat 2~3min in 60~80 DEG C and obtain test solution a；
On the Medium speed filter paper that test solution a is filtered to the 12.5cm in glass funnel B, with the glass rod with rubber tip and 80~
100 DEG C of hydrochloric acid lotion washing beaker 5~6 times, washing lotion washes precipitation and filter paper on filter paper with 80~100 DEG C of hydrochloric acid lotion
Being dripped to by filtrate drop 3 on the surface plate for filling 1ml ammonium thiocyanate solution, ammonium thiocyanate solution is non-discolouring, then with 80~100 DEG C
Water washing and precipitating and filter paper 3 dripped to by filtrate drop on the surface plate for filling 1ml silver nitrate solutiones, silver nitrate solution is non-discolouring,
B must be precipitated；
C, precipitation b and filter paper are placed in the porcelain crucible of constant weight, porcelain crucible are placed in high temperature furnace, by the temperature of high temperature furnace
Degree rises to 1050~1150 DEG C, and the precipitation in porcelain crucible and filter paper are evaporated, are ashed, 1.5~2.5h of calcination, takes out porcelain earthenware
Crucible, 30~40 DEG C are cooled to, porcelain crucible is placed in drier and is cooled to 20~30 DEG C, weighing is calculated as follows to obtain in sample
Silicone content：
In formula：
m1--- precipitation and the quality of crucible, g；
m2--- the quality of crucible, g；
m0--- the quality of sample, g；
0.4674 --- silica is scaled the conversion coefficient of silicon.
Sodium carbonate-boric acid mixed flux described in step A is by mass ratio 2：1 sodium carbonate and boric acid mixes.
The hydrochloric acid that hydrochloric acid described in step A is 1+1.
Perchloric acid mass concentration described in step A is 70~72%.
Hydrogenperoxide steam generator volumetric concentration described in step A is 30%.
The hydrochloric acid that hydrochloric acid lotion described in step B is 5+95.
The concentration of ammonium thiocyanate solution described in step B is 10g/L.
The concentration of silver nitrate solution described in step B is 1g/L.
The detection method of silicone content in Mn-rich slag of the present invention, specifically include sample pretreatment, sample dissolving, acid
Change, precipitation, filtering, washing, calcination and cubage process, are specifically included：
A, sample pretreatment：Sample is crushed to granularity≤0.125mm, is placed in 105-110 DEG C of dry 1.5-2.5h dry
Room temperature is cooled in dry device.
B, sample dissolves：Weigh 0.2000g samples to mix with 3.0-4.0g sodium carbonate-boric acid mixed flux, be placed in graphite
In rebasing high alumina crucible, 20-25min is melted in 900 ± 10 DEG C, takes out, obtains fused mass.
C, it is acidified：Fused mass obtained by step B is placed in the 400ml beakers for filling 30.0ml hydrochloric acid, on electric hot plate plus
Heat is limpid to solution, removes, slightly cold, adds 60ml perchloric acid, obtains test solution；
D, precipitate：By test solution obtained by step C in being heated to releasing perchloric acid white cigarette on electric hot plate, cap upper surface ware, continue
The residue for being heated to smoke starts to crystallize and presents thick, removes, slightly cold, slowly adds people's 20ml hydrochloric acid along beaker inwall, adds
80ml 80-100 DEG C of hot water, add 10 drop hydrogenperoxide steam generators, the micro-boiling on low temperature electric hot plate, stirred with the glass rod with rubber tip
To solution without minute bubbles, test solution is obtained；
E, filtration washing：Test solution obtained by step D is filtered on the Medium speed filter paper of the 12.5cm in glass funnel, with band rubber
The hydrochloric acid lotion washing beaker of the glass rod of leather point and 80-100 DEG C 5-6 times, washing lotion is on filter paper, with 80-100 DEG C of hydrochloric acid lotion
Precipitation and filter paper to be washed to drip on the surface plate for filling 1ml ammonium thiocyanate solution to by filtrate drop 3, ammonium thiocyanate solution is non-discolouring,
Dripped again with 80-100 DEG C of water washing and precipitating and filter paper to by filtrate drop 3 on the surface plate for filling 1ml silver nitrate solutiones, silver nitrate
Solution is non-discolouring, must precipitate；
F, calcination：Precipitation and filter paper obtained by step E are placed in the porcelain crucible of constant weight, porcelain crucible is placed in high temperature furnace
In, the temperature of high temperature furnace is risen to 1100 ± 50 DEG C from room temperature, the precipitation in porcelain crucible and filter paper are evaporated, be ashed, burnt
Burn, the calcination 2h when the temperature of high temperature furnace rises to 1100 ± 50 DEG C, take out crucible, it is slightly cold, porcelain crucible is placed in cold in drier
But to room temperature, weigh；
G, cubage：Silicone content calculates according to the following formula in sample：
In formula：
m1--- precipitation and the quality of crucible, g；
m2--- the quality of crucible, g；
m0--- the quality of sample, g；
0.4674 --- silica is scaled the conversion coefficient of silicon.
In the step A, sample is crushed to granularity≤0.125mm, drying is placed in 105-110 DEG C of dry 1.5-2.5h
Room temperature is cooled in device.
In the step B, 0.2000g samples are weighed, with sodium carbonate-boric acid mixed flux dissolved samples in high temperature furnace.
In the step B and step C, sodium carbonate-boric acid mixed flux is by 2:1 sodium carbonate and boric acid ground and mixed and
Into hydrochloric acid (1+1), perchloric acid is concentrated acid, and using 50ml high alumina crucible and 400ml beakers, graphite powder purity is 98-99%.
In the step D and step E, hydrochloric acid (1+1), hydrochloric acid lotion (5+95), hydrogenperoxide steam generator concentration is 30%, sulphur
Cyanic acid ammonia solution 10g/L, silver nitrate solution 1g/L.
It is slightly cold to refer to that beaker removes placement 2-3min from electric furnace in the step C and step B,
In the step F, porcelain crucible uses the porcelain crucible in 1100 ± 50 DEG C of calcinations to the 30ml of constant weight, the temperature of high temperature furnace
Degree from room temperature rise to 1100 ± 50 DEG C be the precipitation in porcelain crucible and filter paper are evaporated, are ashed, the step of calcination one is completed.
Measure of the detection method especially suitable for the sample of silicon >=5% in Mn-rich slag.
Here is that the present invention will be further described for specific implementation case：
Embodiment 1
--- the detection of silicone content in Mn-rich slag
(1) preparation of experiment reagent
Sodium carbonate-boric acid mixed flux is by mass ratio 2：1 sodium carbonate and boric acid mixes, hydrochloric acid 1.19g/ml
Hydrochloric acid mixed in equal volume with distilled water, perchloric acid concentration is 70-72%, and hydrogenperoxide steam generator volumetric concentration is 30%, hydrochloric acid
Washing lotion is that 1.19g/ml hydrochloric acid 5ml mixes with 95ml distilled water, and the concentration of ammonium thiocyanate solution is 10g/L, and silver nitrate is molten
The concentration of liquid is 1g/L.
(2) detection of silicone content
Sample is crushed to granularity≤0.125mm, in 105~110 DEG C of dry 1.5~2.5h to constant weight, weighs 0.2000g
Sample and 3.0~4.0g sodium carbonate-boric acid mixed flux mix, and melting 20~25min in 890~910 DEG C obtains fused mass, will
Fused mass is dissolved in 30ml hydrochloric acid, and it is limpid to be heated to solution in 60~90 DEG C, is removed and is naturally cooled to 20~25 DEG C, adds 55
~65ml perchloric acid, it is heated to releasing perchloric acid white cigarette in 100~200 DEG C, cap upper surface ware, continues at 60~80 DEG C of heating 20
~25min starts to crystallize and presents thick to the residue of smoke, removes and naturally cools to 50~60 DEG C, it is slowly added to 15~
25ml hydrochloric acid, then adds 70~90ml 80~100 DEG C of hot water, then 0.6~1.2ml hydrogenperoxide steam generator is added dropwise, in 60
~80 DEG C of heating 2~3min of micro-boiling obtain test solution a, on the Medium speed filter paper that test solution a is filtered to the 12.5cm in glass funnel, use
The hydrochloric acid lotion washing beaker of glass rod with rubber tip and 80~100 DEG C 5~6 times, washing lotion is on filter paper, with 80~100 DEG C
Hydrochloric acid lotion is washed precipitation and filter paper and dripped to by filtrate drop 3 on the surface plate for filling 1ml ammonium thiocyanate solution, ammonium thiocyanate solution
It is non-discolouring, then dripped with 80~100 DEG C of water washing and precipitating and filter paper to by filtrate drop 3 in the surface plate for filling 1ml silver nitrate solutiones
On, silver nitrate solution is non-discolouring, must precipitate b, and precipitation b and filter paper are placed in the porcelain crucible of constant weight, porcelain crucible is placed in into height
In warm stove, the temperature of high temperature furnace is risen to 1050~1150 DEG C, the precipitation in porcelain crucible and filter paper are evaporated, be ashed, burnt
1.5~2.5h is burnt, porcelain crucible is taken out, is cooled to 30~40 DEG C, porcelain crucible is placed in drier and is cooled to 20~25 DEG C, is weighed
It is calculated as follows to obtain silicone content in sample：
In formula：
m1--- precipitation and the quality of crucible, g；
m2--- the quality of crucible, g；
m0--- the quality of sample, g；
0.4674 --- silica is scaled the conversion coefficient of silicon.
Embodiment 2
--- the detection of silicone content in Mn-rich slag
The preparation of experiment reagent with embodiment 1.
The detection of silicone content is the same as embodiment 1.
The calculating of silicone content is carried out as the following formula in the Mn-rich slag sample：
Embodiment 3
--- the detection of silicone content in Mn-rich slag
The preparation of experiment reagent with embodiment 1.
The detection of silicone content is the same as embodiment 1.
The calculating of silicone content is carried out as the following formula in the Mn-rich slag sample：
Embodiment 4
--- the detection of silicone content in Mn-rich slag
The preparation of experiment reagent with embodiment 1.
The detection of silicone content is the same as embodiment 1.
The calculating of silicone content is carried out as the following formula in the Mn-rich slag sample：
Embodiment 5
--- the precision of detection method of the present invention, the degree of accuracy, rate of recovery experiment
(1) Precision Experiment
Experimental method：5 Mn-rich slag samples are selected, carry out assay, meter by detection method of the present invention respectively
Relative standard deviation is calculated, experimental result is shown in Table 1.
The Precision Experiment result of 1 detection method of the present invention of table
| Sample | Measured value (%) | Average value (%) | Relative standard deviation RSD |
| Sample 1 | 5.79,5.84,5.75,5.82,5.73, | 5.79 | 0.80 |
| Sample 2 | 9.79,9.88,9.74,9.74,9.866 | 9.80 | 0.67 |
| Sample 3 | 15.12,15.10,15.05,15.19,15.21 | 15.13 | 0.44 |
| Sample 4 | 18.65,18.56,18.60,18.63,18.70 | 18.63 | 0.28 |
| Sample 5 | 20.05,19.98,20.03,20.10,20.12 | 20.06 | 0.28 |
(2) degree of accuracy is tested
Experimental method：Experimental method：4 standard samples are selected, carrying out manganese by detection method of the present invention respectively contains
It is fixed to measure, and each sample parallel determination 5 times, experimental result is shown in Table 2.
The degree of accuracy experimental result of 2 detection method of the present invention of table
(3) rate of recovery is tested
Experimental method：1 Mn-rich slag sample is selected, different amounts of manganese is separately added into, by detection method of the present invention
It is measured, each sample parallel analysis 4 times, averages, tries to achieve the rate of recovery as 98.7~101.4%, experimental result is shown in Table
3。
The rate of recovery experimental result of 3 detection method of the present invention of table
| Sample | Standard value (mg) | Addition (mg) | Measure total value (mg) | The rate of recovery (%) |
| Sample | 19.58 | 4.67 | 24.21 | 99.1 |
| Sample | 19.58 | 9.35 | 28.98 | 100.1 |
| Sample | 19.58 | 14.02 | 33.75 | 101.1 |
| Sample | 19.58 | 18.69 | 38.19 | 99.6 |
From above-mentioned experimental result, the analysis result deviation of detection method of the present invention is small, precision, and the rate of recovery is equal
It can meet that analysis requires, and analyze speed is fast, it is simple to operate, it is easily mastered, there is higher application value.
Claims (6)
1. the detection method of silicone content in a kind of Mn-rich slag, it is characterised in that comprise the following steps：
A, sample is crushed to granularity≤0.125mm, in 105 ~ 110 DEG C of dry 1.5 ~ 2.5h to constant weight, weighs 0.2000g samples
With 3.0 ~ 4.0g, mass ratio 2:1 sodium carbonate-boric acid mixed flux is mixed, and melting 20 ~ 25min in 890 ~ 910 DEG C is melted
Thing, fused mass is dissolved in 30ml, 1+1 hydrochloric acid, it is limpid to be heated to solution in 60 ~ 90 DEG C, removes and naturally cools to 20 ~ 25
DEG C, 55 ~ 65ml perchloric acid is added, is heated to releasing perchloric acid white cigarette in 100 ~ 200 DEG C, cap upper surface ware, continues at 60 ~ 80 DEG C
20 ~ 25min of heating starts to crystallize and presents thick to the residue of smoke, removes and naturally cools to 50 ~ 60 DEG C, is slowly added to 15
~ 25ml hydrochloric acid, then adds 70 ~ 90ml 80 ~ 100 DEG C of hot water, then 0.6 ~ 1.2ml hydrogenperoxide steam generator is added dropwise, in 60 ~ 80
DEG C heating 2 ~ 3min of micro-boiling obtain test solution a；
On the Medium speed filter paper that test solution a is filtered to the 12.5cm in glass funnel, with the glass rod with rubber tip and 80 ~ 100 DEG C B,
Hydrochloric acid lotion washing beaker 5 ~ 6 times, washing lotion washes precipitation and filter paper to by filtrate on filter paper, with 80 ~ 100 DEG C of hydrochloric acid lotion
Drop 3 is dripped on the surface plate for filling 1ml ammonium thiocyanate solution, and ammonium thiocyanate solution is non-discolouring, then is sunk with 80 ~ 100 DEG C of washing
Form sediment and filter paper is dripped on the surface plate for filling 1ml silver nitrate solutiones to by filtrate drop 3, silver nitrate solution is non-discolouring, must precipitate b；
C, precipitation b and filter paper are placed in the porcelain crucible of constant weight, porcelain crucible are placed in high temperature furnace, by the temperature liter of high temperature furnace
To 1050 ~ 1150 DEG C, the precipitation in porcelain crucible and filter paper are evaporated, are ashed, 1.5 ~ 2.5h of calcination, taking out porcelain crucible, it is cold
But to 30 ~ 40 DEG C, porcelain crucible is placed in drier and is cooled to 20 ~ 25 DEG C, be calculated as follows to obtain silicon in sample after weighing and contain
Amount：
In formula：
m1--- precipitation and the quality of crucible, g；
m2--- the quality of crucible, g；
m0--- the quality of sample, g；
0.4674 --- silica is scaled the conversion coefficient of silicon.
2. according to claim 1 in Mn-rich slag silicone content detection method, it is characterised in that perchloric acid matter described in step A
It is 70 ~ 72% to measure concentration.
3. according to claim 1 in Mn-rich slag silicone content detection method, it is characterised in that hydrogen peroxide described in step A
Liquor capacity concentration is 30%.
4. according to claim 1 in Mn-rich slag silicone content detection method, it is characterised in that hydrochloric acid lotion described in step B
For 5+95 hydrochloric acid.
5. according to claim 1 in Mn-rich slag silicone content detection method, it is characterised in that ammonium thiocyanate described in step B
The concentration of solution is 10g/L.
6. according to claim 1 in Mn-rich slag silicone content detection method, it is characterised in that silver nitrate is molten described in step B
The concentration of liquid is 1g/L.
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