CN109596407A - A method of aluminium content in measurement molten iron slag gathering agent - Google Patents
A method of aluminium content in measurement molten iron slag gathering agent Download PDFInfo
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Abstract
The present invention provides a kind of method for measuring aluminium content in molten iron slag gathering agent, method provided by the invention is a kind of high sensitivity, finding speed is fast, it is easy to operate and small relative to other methods interference, there is good selectivity simultaneously, the method that microwave-acid dissolution sample-villiaumite method of substitution of accurate data measures aluminium content in molten iron slag gathering agent can be provided to smelt Composition Control process.
Description
Technical field
The invention belongs to metallurgical analysis technical fields, and in particular to a kind of to use microwave digestion technology, utilize nitric acid, hydrochloric acid
Sample is decomposed, the method that villiaumite method of substitution measures aluminium content in molten iron slag gathering agent.
Background technique
Molten iron slag gathering agent is a kind of important industrial materials, is mainly used for assembling the insoluble matter on molten iron surface, thirdly oxidation
Two aluminium contents are 1-18%, dioxide-containing silica 50-90%.The measurement of aluminum oxide is generally using enterprise in clinker, foaming agent
Industry standard Q/BGJH-07-203-2008 " measurement of aluminum oxide in clinker ", the method hydrochloric acid is by mistake after sample predissolve
Filter, then use sodium carbonate-boric acid mixed flux melt process residue, solution merge after with weak aqua ammonia adjust acidity, separation iron aluminium after
Titrimetry is carried out using villiaumite method of substitution, method is complex for operation step, process tedious.Feng Chaojun etc. has studied " in silver preparation concentrate
Aluminum oxide Improvement in determination method ", this method uses sodium hydroxide, sodium peroxide sample, and precipitation and separation removes dry
It disturbs and titrimetry aluminum oxide is carried out with villiaumite method of substitution after element.Liu Wei etc. discusses " aluminium measurement in aluminum-magnesium-calcium-iron alloy
The experimental study of method ", the method is dripped using after dissolving with hydrochloric acid sample constant volume, liquid separation, adjusting acidity with villiaumite method of substitution
Setting analysis aluminium content, sample of this method not by the molten iron slag gathering agent containing higher silicate decompose completely.But the above existing skill
The method that aluminium content in molten iron slag gathering agent is measured in art is complex for operation step, takes a long time, and sensitivity is not high, does not spend accurately
Also not high, need a kind of high sensitivity, the method that finding speed is fast, easy to operate to contain to measure the aluminium in molten iron slag gathering agent at present
Amount.
The content of background technology part is only the technology that inventor is known, not the existing skill of natural representative this field
Art.
Summary of the invention
For the prior art there are one or more of problem, the present invention provides aluminium in a kind of measurement molten iron slag gathering agent and contains
The method of amount, the method includes the steps:
S1: weighing 0.2000g sample, is placed in the first micro-wave diminishing pot, sequentially adds 7mL nitric acid, 7mL hydrofluoric acid；Separately
The second micro-wave diminishing pot is taken, sequentially adds 7mL nitric acid, blank sample is made in 7mL hydrofluoric acid, then by first micro-wave digestion
Tank and second micro-wave diminishing pot are put into microwave dissolver；
S2: starting the microwave dissolver and cleared up, and after clearing up EP (end of program), when temperature to room temperature takes out described first
Micro-wave diminishing pot and second micro-wave diminishing pot, the sample and blank sample are transferred in beaker；
S3: Xiang Suoshu sample addition hot water is diluted to 150mL, after boiling, ammonium hydroxide is added dropwise and is neutralized to the appearance of iron aluminum precipitation, then
It is secondary boil after filter, wash the beaker and precipitating with thermal chlorination ammonium, the precipitating, into beaker, is tried with hot dissolving with hydrochloric acid
Sample sample solution, same method obtain blank sample solution；
S4: Xiang Suoshu specimen sample solution is added dropwise phenolphthalein indicator 3 and drips, and adjusts solution acidity to powder with sodium hydroxide solution
Red is added hot water to the specimen sample solution to 100mL, then is boiled after adding 8g sodium hydroxide, and room temperature is then cooled to,
Solution is transferred to constant volume in 250mL volumetric flask, obtains testing sample solution, same method obtains blank sample solution to be measured；
S5: 100mL filtrate will be pipetted in 500mL conical flask after testing sample solution filtering, 40.00mL is added
EDTA standard solution adds one piece of Congored test paper, and adjusting acidity with hydrochloric acid makes test paper just from red to blue, 20mL acetic acid-be added
Sodium acetate buffer boils 3-4min, adds 8 drop PAN indicator, and being titrated to solution with copper sulphate standard solution is purple, is added
Enter 2~3g sodium fluoride and boil 3-4min, then plus 8 drop PAN indicator, being titrated to solution with the copper sulphate standard solution is purple
Do not become terminal；
It is calculated by the following formula the content of aluminium in sample:
W%=C × (V-V0) × M × 100/ (m × K × 1000)
In formula:
C- is with copper sulphate standard solution (0.01783mol/L)；
Consumptive use copper sulphate standard solution volume (mL) when V0- titrates blank solution；
Consumptive use copper sulphate standard solution volume (mL) when V- titrates sample solution；
The molal weight (26.98g/mol) of M- aluminium；
M- sample mass (g)；
K- sample solution liquid separation ratio.
Preferably, the concentration of above-mentioned nitric acid is 16mol/L；The concentration of the hydrofluoric acid is 22.5mol/L.
Preferably, the control parameter of above-mentioned microwave dissolver are as follows: power 1600W；Temperature program: 5min rises to 120 DEG C,
Keep the temperature 2min；15min rises to 200 DEG C from 120, keeps the temperature 15min；Cooling time is 45min.
Preferably, the temperature of hot water described in above-mentioned steps S3 are as follows: 50 DEG C~60 DEG C；The ammonium hydroxide is by concentrated ammonia liquor and height
Pure water is mixed with to obtain in equal volume；The temperature of the thermal chlorination ammonium are as follows: 50 DEG C~60 DEG C, concentration 10g/L；The hot hydrochloric acid
Temperature are as follows: 50 DEG C~60 DEG C, concentrated hydrochloric acid is mixed to prepare by the hydrochloric acid in equal volume with high purity water；The thermal chlorination ammonium washs institute
It states beaker 3 times and precipitates 7 times.
Preferably, phenolphthalein indicator described in above-mentioned steps S4 is with 2g/L in ethanol solution；The sodium hydroxide solution
Concentration be 200g/L.
Preferably, in above-mentioned steps S5, the hydrochloric acid is to be mixed to prepare concentrated hydrochloric acid in equal volume with high purity water；The vinegar
Acid-sodium acetate buffer concentration is 0.1-1mol/L；The concentration of the EDTA standard solution and copper sulphate standard solution is equal
For 0.01783mol/L；The concentration of the PAN indicator is 1g/L.
Preferably, the range for detecting aluminium content in the molten iron slag gathering agent of the above method are as follows: 0.10at~20.0at%.
Based on above technical scheme, the present invention proposes a kind of based on microwave-acid dissolution sample-villiaumite method of substitution measurement molten iron
The method of aluminium content in Slag conglomeration agent.
The invention has the following advantages:
It is of the present invention to be used for Al-single crystal in molten iron slag gathering agent, pass through microwave dissolver using hydrofluoric acid, nitric acid and dissolves
Sample, using aluminium content in the measurement molten iron slag gathering agent of villiaumite method of substitution.The present invention passes through the multiple inspection to molten iron slag gathering agent sample
It tests, application effect is good.The present invention has high sensitivity, easy to operate, accurate, the reliable feature of analysis result.
Aluminium in molten iron slag gathering agent is measured using this method, can be completed in 4 hours, when shortening sample treatment
Between, range 0.10at~20.0at% of analysis method.In addition, the present invention only uses 7mL nitric acid, 7mL hydrofluoric acid decomposition samples,
Solvent usage amount is greatly reduced, environmental protection and energy-saving is conducive to.
Specific embodiment
Hereinafter, certain exemplary embodiments are simply just described.As one skilled in the art will recognize that
Like that, without departing from the spirit or scope of the present invention, described embodiment can be modified by various different modes.
Therefore, description is considered essentially illustrative rather than restrictive.
The object of the present invention is to provide a kind of high sensitivities, and finding speed is fast, easy to operate and relative to other methods
It interferes small, while having good selectivity, microwave-acid dissolution examination of accurate data can be provided to smelt Composition Control process
The method of aluminium content in sample-villiaumite method of substitution measurement molten iron slag gathering agent.To realize goal of the invention, the technology of invention
Scheme is as follows:
A kind of improvement measuring aluminium content method in molten iron slag gathering agent is incited somebody to action using microwave digestion technology, using nitric acid, hydrochloric acid
Sample decomposes, and villiaumite method of substitution measures aluminium content in molten iron slag gathering agent.
In the preferred embodiment of the invention, the present invention provides aluminium content in a kind of measurement molten iron slag gathering agent
Method, the method includes the steps:
S1: weighing 0.2000g sample, is placed in the first micro-wave diminishing pot, sequentially adds 7mL nitric acid, 7mL hydrofluoric acid；Separately
The second micro-wave diminishing pot is taken, sequentially adds 7mL nitric acid, blank sample is made in 7mL hydrofluoric acid, then by first micro-wave digestion
Tank and second micro-wave diminishing pot are put into microwave dissolver；
S2: starting the microwave dissolver and cleared up, and after clearing up EP (end of program), when temperature to room temperature takes out described first
Micro-wave diminishing pot and second micro-wave diminishing pot, the sample and blank sample are transferred in beaker；
S3: Xiang Suoshu sample addition hot water is diluted to 150mL, after boiling, ammonium hydroxide is added dropwise and is neutralized to the appearance of iron aluminum precipitation, then
It is secondary boil after filter, wash the beaker and precipitating with thermal chlorination ammonium, the precipitating, into beaker, is tried with hot dissolving with hydrochloric acid
Sample sample solution, same method obtain blank sample solution；
S4: Xiang Suoshu specimen sample solution is added dropwise phenolphthalein indicator 3 and drips, and adjusts solution acidity to powder with sodium hydroxide solution
Red is added hot water to the specimen sample solution to 100mL, then is boiled after adding 8g sodium hydroxide, and room temperature is then cooled to,
Solution is transferred to constant volume in 250mL volumetric flask, obtains testing sample solution, same method obtains blank sample solution to be measured；
S5: 100mL filtrate will be pipetted in 500mL conical flask after testing sample solution filtering, 40.00mL is added
EDTA standard solution adds one piece of Congored test paper, and adjusting acidity with hydrochloric acid makes test paper just from red to blue, 20mL acetic acid-be added
Sodium acetate buffer boils 3-4min, adds 8 drop PAN indicator, and being titrated to solution with copper sulphate standard solution is purple, is added
Enter 2~3g sodium fluoride and boil 3-4min, then plus 8 drop PAN indicator, being titrated to solution with the copper sulphate standard solution is purple
Do not become terminal；
It is calculated by the following formula the content of aluminium in sample:
W%=C × (V-V0) × M × 100/ (m × K × 1000)
In formula:
C- is with copper sulphate standard solution (0.01783mol/L)；
Consumptive use copper sulphate standard solution volume (mL) when V0- titrates blank solution；
Consumptive use copper sulphate standard solution volume (mL) when V- titrates sample solution；
The molal weight (26.98g/mol) of M- aluminium；
M- sample mass (g)；
K- sample solution liquid separation ratio.
According to a preferred embodiment of the present invention, the concentration of above-mentioned nitric acid is 16mol/L；The concentration of the hydrofluoric acid is
22.5mol/L。
According to a preferred embodiment of the present invention, the control parameter of above-mentioned microwave dissolver are as follows: power 1600W；It rises
Warm program: 5min rises to 120 DEG C, keeps the temperature 2min；15min rises to 200 DEG C from 120, keeps the temperature 15min；Cooling time is 45min.
According to a preferred embodiment of the present invention, the temperature of hot water described in above-mentioned steps S3 are as follows: 50 DEG C~60 DEG C；Institute
Stating ammonium hydroxide is to be mixed with to obtain in equal volume with high purity water by concentrated ammonia liquor；The temperature of the thermal chlorination ammonium are as follows: 50 DEG C~60 DEG C, dense
Degree is 10g/L；The temperature of the hot hydrochloric acid are as follows: 50 DEG C~60 DEG C, concentrated hydrochloric acid is mixed system with high purity water by the hydrochloric acid in equal volume
?；The thermal chlorination ammonium washs the beaker 3 times and precipitates 7 times.
According to a preferred embodiment of the present invention, phenolphthalein indicator described in above-mentioned steps S4 is with 2g/L in ethanol solution
In；The concentration of the sodium hydroxide solution is 200g/L.
According to a preferred embodiment of the present invention, in above-mentioned steps S5, the hydrochloric acid is by concentrated hydrochloric acid and high purity water etc.
Volume mixture is made；The concentration of the NaAc_HAc buffer solution is 0.1-1mol/L；The EDTA standard solution and sulfuric acid
The concentration of copper standard solution is 0.01783mol/L；The concentration of the PAN indicator is 1g/L.
According to a preferred embodiment of the present invention, the range for detecting aluminium content in the molten iron slag gathering agent of the above method
Are as follows: 0.10at~20.0at%.
The preferred embodiment of the present invention is described below, it will be appreciated by those skilled in the art that of the invention is preferred
Embodiment is served only for helping to be best understood from the present invention, is not intended to restrict the invention.
The embodiment of the present invention uses following methods:
0.2000g sample is weighed, acid is placed in and boils in clean micro-wave diminishing pot, sequentially add 7mL nitric acid, 7mL hydrofluoric acid,
Separately an acid is taken to boil clean micro-wave diminishing pot, sequentially add 7mL nitric acid, blank sample is made in 7mL hydrofluoric acid, then will be equipped with
The counteracting tank and blank sample of Slag conglomeration agent sample are all put into microwave dissolver.Start microwave dissolver, sets control parameter, disappear
After solving EP (end of program), when temperature to room temperature, takes out counteracting tank, and sample is shifted in 400mL beaker.Heating water is diluted to 150mL and sets
It boils, remove in electric furnace, ammonium hydroxide (1+1) is added dropwise and is neutralized to iron aluminum precipitation appearance (PH=7-8), a moment filtering is stood after boiling,
With thermal chlorination ammonium (10g/L) washing beaker 3 times and precipitating 7 times, precipitating is dissolved in former beaker with hot hydrochloric acid (1+1).
Be added dropwise phenolphthalein indicator (2g/L ethanol solution) 3 drip, with sodium hydroxide solution (200g/L) adjust solution acidity to
Pink adds hot water to sample solution volume to 100mL, crosses after adding 8g sodium hydroxide and boil a moment in low-temperature furnace, remove
It is cooled to room temperature, solution is transferred in 250mL volumetric flask, is diluted and constant volume, shakes up.
100mL sample solution (filtrate) is pipetted after solution is filtered in 500 conical flasks, and 40.00mLEDTA standard is added
Solution (0.01783mol/L) adds one piece of Congored test paper, and adjusting acidity with hydrochloric acid (1+1) has added test paper just from red to blue,
Enter 20mL NaAc_HAc buffer solution, boils 3min.Add 8 drop PAN indicator (1g/L), with copper sulphate standard solution
It is purple that (0.01783mol/L), which is titrated to solution, and 2~3g sodium fluoride is added and boils 3-4min, then plus 8 drop PAN indicator (1g/
L), being titrated to solution with copper sulphate standard solution is that purple does not become terminal.
The content of Al is calculated as follows in sample:
%=C × (V-V0) × M × 100/m × K × 1000 W (Al)
In formula:
C- is with copper sulphate standard solution (0.01783mol/L)；
Consumptive use copper sulphate standard solution volume (mL) when V0- titrates blank solution；
Consumptive use copper sulphate standard solution volume (mL) when V- titrates sample solution；
The molal weight (26.98g/mol) of M- aluminium；
M- sample mass；
K- sample solution liquid separation ratio；
This method detection range: Al0.10at~20.0at%.
W(Al2O3) % × 1.896 %=W (Al)
Embodiment 1:
Weigh the higher mild-clay containing silica (GBW03115), clay (GBW03102a) and calcium-magnesium-containing blast furnace
Slag (YSBC13835-96), vessel slag (GBW01704a) are measured according to the above method, as a result see the table below 1.
Table 1: standard sample measurement result
| Standard sample | Al2O3Asserting value % | Al2O3Measured value % |
| Mild-clay (GBW03115) | 28.57 | 28.69 |
| Clay (GBW03102a) | 31.32 | 31.47 |
| Blast furnace slag (YSBC13835-96) | 7.73 | 7.59 |
| Vessel slag (GBW01704a) | 1.14 | 1.18 |
Embodiment 2:
Molten iron slag gathering agent 1#, 2#, 3#, 4#, 5# sample is weighed, is measured according to the above method, as a result see the table below 2.
: table 2: sample specimens measurement result
| Molten iron slag gathering agent sample | Al2O3Measured value % |
| 1# | 9.82 |
| 2# | 9.08 |
| 3# | 7.26 |
| 4# | 1.43 |
| 5# | 3.67 |
Pass through the verifying of above-mentioned embodiment, it can be seen that the present invention is molten by microwave dissolver using hydrofluoric acid, nitric acid
Sample is solved, preferable result is obtained using aluminium content in the measurement molten iron slag gathering agent of villiaumite method of substitution.The model of analysis method of the present invention
0.10at~20.0at% is enclosed, and analysis method precision is high, accuracy is high.This method quickly, it is easy, can produce in push away
Extensively, it uses.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (7)
1. a kind of method of aluminium content in measurement molten iron slag gathering agent, which is characterized in that the method includes the steps:
S1: weighing 0.2000g sample, is placed in the first micro-wave diminishing pot, sequentially adds 7mL nitric acid, 7mL hydrofluoric acid；Separately take the
Two micro-wave diminishing pots, sequentially add 7mL nitric acid, blank sample is made in 7mL hydrofluoric acid, then by first micro-wave diminishing pot and
Second micro-wave diminishing pot is put into microwave dissolver；
S2: starting the microwave dissolver and cleared up, and after clearing up EP (end of program), when temperature to room temperature takes out first microwave
Counteracting tank and second micro-wave diminishing pot, the sample and blank sample are transferred in beaker；
S3: Xiang Suoshu sample addition hot water is diluted to 150mL, after boiling, ammonium hydroxide is added dropwise and is neutralized to the appearance of iron aluminum precipitation, boils again
It is filtered after boiling, washs the beaker and precipitating with thermal chlorination ammonium, the precipitating, into beaker, obtains sample sample with hot dissolving with hydrochloric acid
Product solution, same method obtain blank sample solution；
S4: Xiang Suoshu specimen sample solution is added dropwise phenolphthalein indicator 3 and drips, and adjusts solution acidity to pink with sodium hydroxide solution
Color is added hot water to the specimen sample solution to 100mL, then is boiled after adding 8g sodium hydroxide, and room temperature is then cooled to, will
Solution is transferred to constant volume in 250mL volumetric flask, obtains testing sample solution, and same method obtains blank sample solution to be measured；
S5: 100mL filtrate will be pipetted in 500mL conical flask after testing sample solution filtering, 40.00mL EDTA is added
Standard solution adds one piece of Congored test paper, and adjusting acidity with hydrochloric acid makes test paper just from red to blue, 20mL acetic acid-acetic acid be added
Sodium buffer solution, boils 3-4min, adds 8 drop PAN indicator, and being titrated to solution with copper sulphate standard solution is purple, and addition 2~
3g sodium fluoride boils 3-4min, then plus 8 drop PAN indicator, being titrated to solution with the copper sulphate standard solution is that purple is constant
For terminal；
It is calculated by the following formula the content of aluminium in sample:
W%=C × (V-V0) × M × 100/ (m × K × 1000)
In formula:
C- is with copper sulphate standard solution (0.01783mol/L)；
Consumptive use copper sulphate standard solution volume (mL) when V0- titrates blank solution；
Consumptive use copper sulphate standard solution volume (mL) when V- titrates sample solution；
The molal weight (26.98g/mol) of M- aluminium；
M- sample mass (g)；
K- sample solution liquid separation ratio.
2. method described in claim 1, which is characterized in that the concentration of the nitric acid is 16mol/L；The concentration of the hydrofluoric acid
For 22.5mol/L.
3. method described in claim 1, which is characterized in that the control parameter of the microwave dissolver are as follows: power 1600W；
Temperature program: 5min rises to 120 DEG C, keeps the temperature 2min；15min rises to 200 DEG C from 120, keeps the temperature 15min；Cooling time is
45min。
4. method described in claim 1, which is characterized in that the temperature of hot water described in the step S3 are as follows: 50 DEG C~60 DEG C；
The ammonium hydroxide is to be mixed with to obtain in equal volume with high purity water by concentrated ammonia liquor；The temperature of the thermal chlorination ammonium are as follows: 50 DEG C~60 DEG C,
Concentration is 10g/L；The temperature of the hot hydrochloric acid are as follows: 50 DEG C~60 DEG C, the hydrochloric acid mixes concentrated hydrochloric acid with high purity water in equal volume
It is made；The thermal chlorination ammonium washs the beaker 3 times and precipitates 7 times.
5. method described in claim 1, which is characterized in that phenolphthalein indicator described in the step S4 is molten in ethyl alcohol with 2g/L
In liquid；The concentration of the sodium hydroxide solution is 200g/L.
6. method described in claim 1, which is characterized in that in the step S5, the hydrochloric acid is by concentrated hydrochloric acid and high purity water
It is mixed to prepare in equal volume；The concentration of the NaAc_HAc buffer solution is 0.1-1mol/L；The EDTA standard solution and sulphur
The concentration of sour copper standard solution is 0.01783mol/L；The concentration of the PAN indicator is 1g/L.
7. method described in claim 1, which is characterized in that the model of aluminium content in the detection molten iron slag gathering agent of the method
It encloses are as follows: 0.10at~20.0at%.
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| CN112305152A (en) * | 2020-09-30 | 2021-02-02 | 西北工业大学 | Method for determining components of composite propellant condensed-phase combustion product by EDTA titration method |
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