CN107192629A - A kind of ion regulating agent and its application in aluminum fluoride in fluorine content determination method - Google Patents
A kind of ion regulating agent and its application in aluminum fluoride in fluorine content determination method Download PDFInfo
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Abstract
A kind of application the invention discloses ion regulating agent and its in aluminum fluoride in fluorine content determination method, belongs to aluminum smelting technology technical field, with solve Oil repellent in current aluminum fluoride can not accurately, quickly determine the problem of.The present invention is calculated including Oil repellent in sample solution preparation, standard liquid preparation, ion regulating agent preparation, Drawing of Curve, sample concentration measure and solution.The present invention sets up new ion mediator agent, and the pH value of detected solution is adjusted to 56, the testing conditions of fluoride ion selective electrode is reached most preferably, makes solution close to fluorine and the existing forms of sodium；Shorten sample processing time, the measure of Oil repellent is quick, accurate；Less using analytical reagent, analysis cost is low；Technical process is non-toxic, safe operation；Operating cost is low, and analysis is quick, saves manpower.
Description
Technical field
The invention belongs to aluminum smelting technology technical field, and in particular to a kind of ion regulating agent and its Oil repellent survey in aluminum fluoride
Determine the application in method.
Background technology
It is main in the technique of production remelting aluminium ingot to occur production metallic aluminium using cryolite-alumina electrolysis, it is normal raw
Need to be continuously replenished a number of fluoride salt in production as the flux of electrolysis of aluminum oxide, and the index of fluorine is most attached most importance in fluoride salt
Will, examine at present using equipment such as photo-electric direct reading spectrometer, X-ray diffractometer, ICP in detection and analysis, can be in main original used
Lack corresponding corollary equipment in material aluminum fluoride, the analysis of the host element fluorine of ice crystal, and analytical cycle is long, matter often occurs
Amount control is the general layout managed afterwards.
The content of the invention
A kind of application it is an object of the invention to provide ion regulating agent and its in aluminum fluoride in fluorine content determination method,
With solve Oil repellent in current aluminum fluoride can not accurately, quickly determine the problem of.
In order to solve the above problems, the technical solution adopted by the present invention is：
A kind of ion regulating agent, is made up jointly per 1000ml of the raw material of following parts by weight and parts by volume：The wherein original of parts by weight
Material includes 125-175 parts of 25-35 parts of sodium chloride and sodium citrate, and the raw material of parts by volume includes 25-40 parts of glacial acetic acid, and surplus is
Water.
In order to further realize the present invention, ion regulating agent is common by the raw material of following parts by weight and parts by volume per 1000ml
It is made：Wherein the raw material of parts by weight includes 135 parts of 29 parts of sodium chloride and sodium citrate, and the raw material of parts by volume includes glacial acetic acid 30
Part, surplus is water.
Application of the ion regulating agent of the present invention in aluminum fluoride in fluorine content determination method, comprises the following steps：
Step 1: sample solution is prepared：
It is accurate to weigh the aluminum fluoride 0.2000g through 120 DEG C of drying, 1.0-2.0g sodium hydroxides are added, 30ml platinum crucibles are put into,
0.1-0.2ml water is added dropwise, 1.5-2.5h is melted at 150-300 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, shifts
To 250ml polyvinyl chloride volumetric flasks, sample solution is made；
Step 2: standard liquid is prepared：
It is accurate respectively after Oil repellent is dried through 120 DEG C respectively for 54.07%, 57.72%, 60.88%, 64.97% aluminum fluoride standard specimen
Aluminum fluoride standard specimen 0.2000g is really weighed, 1.0-2.0g sodium hydroxides are added, 30ml platinum crucibles are put into, 0.1-0.2ml is added dropwise
Water, melts 1.5-2.5h at 150-300 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polychlorostyrene second
Alkene volumetric flask, is made sample solution；
Step 3: Drawing of Curve：
The standard liquid 5ml of Oil repellent in step 2 54.07% is accurately pipetted into 100ml volumetric flasks, by the fluorine in step 2
Content is accurately pipetted into 100ml volumetric flasks for 54.07%, 57.72%, 60.88%, 64.97% each 20ml of aluminun fluoride solution, will
Oil repellent in step 2 is accurately pipetted into 100ml volumetric flasks for 64.97% aluminun fluoride solution 25ml, is separately added into 5-
20ml ion regulating agents, with water constant volume to 100ml；
Above-mentioned solution is moved into 200ml polyvinyl chloride beakers respectively, magnetic stir bar is put into and stirs, is dripped with automatic current potential
Determine instrument at room temperature, be worth using sequentially determining millivolt between fluoride ion selective electrode and reference electrode, complete Drawing of Curve；
Step 4: sample concentration is determined：
The accurate sample 0.2000g for weighing drying processing, adds 1.0-2.0g sodium hydroxides, is put into 30ml platinum crucibles, drips
Plus 0.1-0.2ml water, 1.5-2.5h is melted at 150-300 DEG C, is taken out after cooling, is diluted with water and is settled to 250ml, be transferred to
250ml polyvinyl chloride volumetric flasks, are made sample solution；
Pipette samples solution 20ml, adds 10ml ion regulating agents constant volume to 100ml volumetric flasks, is then transferred into 200ml polychlorostyrene
Ethene beaker, measures sample concentration；
Step 5: Oil repellent is calculated in solution.
In order to further realize that the rotating speed of magnetic stir bar in the present invention, step 4 turns/min for 900-1100.
In order to which the rotating speed for further realizing magnetic stir bar in the present invention, step 4 is 1000 turns/min.
Beneficial effect of the present invention compared to prior art：
1st, aluminum fluoride used for aluminium electrolysis is insoluble in all kinds of acid, but is fused to sodium hydroxide at low temperature, and the present invention sets up new ion and adjusted
Agent is solved, selective chlorination sodium, sodium citrate and glacial acetic acid composition ion regulating agent adjust the pH value of detected solution to 5-6, make fluorine
The testing conditions of ion-selective electrode reach most preferably, make solution close to fluorine and the existing forms of sodium；
2nd, the low temperature molten sample time of sodium hydroxide is short in the present invention, and sample treatment total duration is controlled within 2.5h, shortens sample
Processing time, the measure of Oil repellent is quick, accurate；
3rd, the present invention is less using analytical reagent, and analysis cost is low；
4th, present invention process process is non-toxic, safe operation；
5th, operating cost of the present invention is low, and analysis is quick, saves manpower.
Embodiment
With reference to embodiment, the present invention is further illustrated.
The reagent and instrument used in the present invention by market commercially available from.
The automatical potentiometric titrimeter used in the present invention is the logical production of Switzerland ten thousand, the Titrando of model 905.
The water used in the present invention is distilled water.
Oil repellent calculation formula is in solution of the present invention：
；
In formula：C is the concentration for measuring fluorine in test solution；
M is the quality for weighing sample；
106For the conversion coefficient gram with microgram；
250 be solution dose volume；
20 take amount of solution to divide（Unit：ml）；
100 be final configuration liquor capacity.
Embodiment 1：（The present embodiment is most preferred embodiment）
Ion regulating agent is prepared：
Accurately weigh 58.0g sodium chloride, 270.0g sodium citrates, in the mixture add 60ml glacial acetic acid, dissolving constant volume in
1000ml volumetric flasks, are made ion regulating agent；
Step 1: sample solution is prepared：
It is accurate to weigh the aluminum fluoride sample 0.2000g through 120 DEG C of drying, 1.5g sodium hydroxides are added, 30ml platinum crucibles are put into,
0.1ml water is added dropwise, 2h is melted at 200 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polychlorostyrene second
Alkene volumetric flask, is made sample solution；
Step 2: standard liquid is prepared：
It is accurate respectively after Oil repellent is dried through 120 DEG C respectively for 54.07%, 57.72%, 60.88%, 64.97% aluminum fluoride standard specimen
Aluminum fluoride standard specimen 0.2000g is really weighed, 1.5g sodium hydroxides are added, 30ml platinum crucibles are put into, 0.1ml water is added dropwise, at 200 DEG C
Lower melting 2h, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride volumetric flasks, is made different dense
Standard liquid is spent, its Oil repellent is respectively 0.4326mg/ml, 0.4617mg/ml, 0.4870mg/ml, 0.5198mg/ml；
Step 3: Drawing of Curve：
The standard liquid 5ml of Oil repellent in step 2 54.07% is accurately pipetted into 100ml volumetric flasks, by the fluorine in step 2
Content is accurately pipetted into 100ml volumetric flasks for 54.07%, 57.72%, 60.88%, 64.97% each 20ml of aluminun fluoride solution, will
Oil repellent in step 2 is accurately pipetted into 100ml volumetric flasks for 64.97% aluminun fluoride solution 25ml, is separately added into 10ml
Ion regulating agent, with water constant volume to 100ml, its fluorinion concentration is respectively 21.628 μ g/ml, 86.512 μ g/ml, 92.352 μ
G/ml, 97.408 μ g/ml, 103.952 μ g/ml, 129.94 μ g/ml, 200ml polyvinyl chloride beakers are moved into by above-mentioned solution respectively
In, sequentially determining millivolt value completes Drawing of Curve；
Above-mentioned solution is moved into 200ml polyvinyl chloride beakers respectively, magnetic stir bar is put into and is stirred with 1000 turns/min,
With automatical potentiometric titrimeter at room temperature, it is worth using sequentially determining millivolt between fluoride ion selective electrode and reference electrode, is completed
Drawing of Curve；
Step 4: sample concentration is determined：
The accurate sample 0.2000g for weighing drying processing, adds 1.5g sodium hydroxides, is put into 30ml platinum crucibles, is added dropwise
0.1ml water, melts 2h at 200 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, is transferred to 250ml polyvinyl chloride appearance
Measuring bottle, draws 20ml, adds 10ml ion regulating agents constant volume to 100ml volumetric flasks, is then transferred into 200ml polyvinyl chloride burning
Cup, measuring sample concentration result is：99.57μg/ml；
Step 5: Oil repellent is calculated in solution：
The concentration of the fluorine of aluminum fluoride sample will be measured（C）99.57 μ g/ml substitute into lower formula and calculated
=62.23%。
Embodiment 2：
Ion regulating agent is prepared：
Accurately weigh 58.0g sodium chloride, 270.0g sodium citrates, in the mixture add 60ml glacial acetic acid, dissolving constant volume in
1000ml volumetric flasks, are made ion regulating agent；
Step 1: sample solution is prepared：
It is accurate to weigh the aluminum fluoride 0.2000g through 120 DEG C of drying, 2.0g sodium hydroxides are added, 30ml platinum crucibles are put into, are added dropwise
0.2ml water, melts 2.5h at 150 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride
Volumetric flask, is made sample solution, and its Oil repellent is 0.543mg/ml；
Step 2: standard liquid is prepared：
It is accurate respectively after Oil repellent is dried through 120 DEG C respectively for 54.07%, 57.72%, 60.88%, 64.97% aluminum fluoride standard specimen
Aluminum fluoride standard specimen 0.2000g is really weighed, 2.0g sodium hydroxides are added, 30ml platinum crucibles are put into, 0.2ml water is added dropwise, at 150 DEG C
Lower melting 2.5h, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride volumetric flasks, difference is made
Concentration standard liquid, its Oil repellent is respectively 0.4326mg/ml, 0.4617mg/ml, 0.4870mg/ml, 0.5198mg/ml；
Step 3: Drawing of Curve：
The standard liquid 5ml of Oil repellent in step 2 54.07% is accurately pipetted into 100ml volumetric flasks, by the fluorine in step 2
Content is accurately pipetted into 100ml volumetric flasks for 54.07%, 57.72%, 60.88%, 64.97% each 20ml of aluminun fluoride solution, will
Oil repellent in step 2 is accurately pipetted into 100ml volumetric flasks for 64.97% aluminun fluoride solution 25ml, is separately added into 10ml
Ion regulating agent, with water constant volume to 100ml, its fluorinion concentration is respectively 21.628 μ g/ml, 86.512 μ g/ml, 92.352 μ
G/ml, 97.408 μ g/ml, 103.952 μ g/ml, 129.94 μ g/ml, 200ml polyvinyl chloride beakers are moved into by above-mentioned solution respectively
In, sequentially determining millivolt value completes Drawing of Curve；
Above-mentioned solution is moved into 200ml polyvinyl chloride beakers respectively, magnetic stir bar is put into and is stirred with 900 turns/min,
With automatical potentiometric titrimeter at room temperature, it is worth using sequentially determining millivolt between fluoride ion selective electrode and reference electrode, is completed
Drawing of Curve；
Step 4: sample concentration is determined：
The accurate sample 0.2000g for weighing drying processing, adds 2.0g sodium hydroxides, is put into 30ml platinum crucibles, is added dropwise
0.2ml water, melts 2.5h at 150 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride
Volumetric flask, draws 20ml, adds 10ml ion regulating agents constant volume to 100ml volumetric flasks, is then transferred into 200ml polyvinyl chloride burning
Cup, measures sample concentration for 94.20 μ g/ml；
Step 5: Oil repellent is calculated in solution：
The concentration of the fluorine of aluminum fluoride sample will be measured（C）94.20 μ g/ml substitute into lower formula and calculated
=58.88%。
Embodiment 3：
Ion regulating agent is prepared：
Accurately weigh 58.0g sodium chloride, 270.0g sodium citrates, in the mixture add 60ml glacial acetic acid, dissolving constant volume in
1000ml volumetric flasks, are made ion regulating agent；
Step 1: sample solution is prepared：
It is accurate to weigh the aluminum fluoride 0.2000g through 120 DEG C of drying, 1.0g sodium hydroxides are added, 30ml platinum crucibles are put into, are added dropwise
0.1ml water, melts 1.5h at 300 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride
Volumetric flask, is made sample solution, and its Oil repellent is 0.543mg/ml；
Step 2: standard liquid is prepared：
It is accurate respectively after Oil repellent is dried through 120 DEG C respectively for 54.07%, 57.72%, 60.88%, 64.97% aluminum fluoride standard specimen
Aluminum fluoride standard specimen 0.2000g is really weighed, 1.0g sodium hydroxides are added, 30ml platinum crucibles are put into, 0.1ml water is added dropwise, at 300 DEG C
Lower melting 1.5h, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride volumetric flasks, difference is made
Concentration standard liquid, its Oil repellent is respectively 0.4326mg/ml, 0.4617mg/ml, 0.4870mg/ml, 0.5198mg/ml；
Step 3: Drawing of Curve：
The standard liquid 5ml of Oil repellent in step 2 54.07% is accurately pipetted into 100ml volumetric flasks, by the fluorine in step 2
Content is accurately pipetted into 100ml volumetric flasks for 54.07%, 57.72%, 60.88%, 64.97% each 20ml of aluminun fluoride solution, will
Oil repellent in step 2 is accurately pipetted into 100ml volumetric flasks for 64.97% aluminun fluoride solution 25ml, is separately added into 10ml
Ion regulating agent, with water constant volume to 100ml, its fluorinion concentration is respectively 21.628 μ g/ml, 86.512 μ g/ml, 92.352 μ
G/ml, 97.408 μ g/ml, 103.952 μ g/ml, 129.94 μ g/ml, 200ml polyvinyl chloride beakers are moved into by above-mentioned solution respectively
In, sequentially determining millivolt value completes Drawing of Curve；
Above-mentioned solution is moved into 200ml polyvinyl chloride beakers respectively, magnetic stir bar is put into and is stirred with 1100 turns/min,
With automatical potentiometric titrimeter at room temperature, it is worth using sequentially determining millivolt between fluoride ion selective electrode and reference electrode, is completed
Drawing of Curve；
Step 4: sample concentration is determined：
The accurate sample 0.2000g for weighing drying processing, adds 1.0g sodium hydroxides, is put into 30ml platinum crucibles, is added dropwise
0.1ml water, melts 1.5h at 300 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride
Volumetric flask, draws 20ml, adds 10ml ion regulating agents constant volume to 100ml volumetric flasks, is then transferred into 200ml polyvinyl chloride burning
Cup, measures sample concentration for 97.79 μ g/ml；
Step 5: Oil repellent is calculated in solution：
The concentration of the fluorine of aluminum fluoride sample will be measured（C）97.79 μ g/ml substitute into lower formula and calculated
=61.12%。
Embodiment 4：
Ion regulating agent is prepared：
Accurately weigh 50.0g sodium chloride, 250.0g sodium citrates, in the mixture add 50ml glacial acetic acid, dissolving constant volume in
1000ml volumetric flasks, are made ion regulating agent；
Step 1: sample solution is prepared：
It is accurate to weigh the aluminum fluoride 0.2000g through 120 DEG C of drying, 1.5g sodium hydroxides are added, 30ml platinum crucibles are put into, are added dropwise
0.2ml water, melts 2.5h at 150 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride
Volumetric flask, is made sample solution, and its Oil repellent is 0.543mg/ml；
Step 2: standard liquid is prepared：
It is accurate respectively after Oil repellent is dried through 120 DEG C respectively for 54.07%, 57.72%, 60.88%, 64.97% aluminum fluoride standard specimen
Aluminum fluoride standard specimen 0.2000g is really weighed, 1.5g sodium hydroxides are added, 30ml platinum crucibles are put into, 0.2ml water is added dropwise, at 150 DEG C
Lower melting 2.5h, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride volumetric flasks, difference is made
Concentration standard liquid, its Oil repellent is respectively 0.4326mg/ml, 0.4617mg/ml, 0.4870mg/ml, 0.5198mg/ml；
Step 3: Drawing of Curve：
The standard liquid 5ml of Oil repellent in step 2 54.07% is accurately pipetted into 100ml volumetric flasks, by the fluorine in step 2
Content is accurately pipetted into 100ml volumetric flasks for 54.07%, 57.72%, 60.88%, 64.97% each 20ml of aluminun fluoride solution, will
Oil repellent in step 2 is accurately pipetted into 100ml volumetric flasks for 64.97% aluminun fluoride solution 25ml, is separately added into 20ml
Ion regulating agent, with water constant volume to 100ml, its fluorinion concentration is respectively 21.628 μ g/ml, 86.512 μ g/ml, 92.352 μ
G/ml, 97.408 μ g/ml, 103.952 μ g/ml, 129.94 μ g/ml, 200ml polyvinyl chloride beakers are moved into by above-mentioned solution respectively
In, sequentially determining millivolt value completes Drawing of Curve；
Above-mentioned solution is moved into 200ml polyvinyl chloride beakers respectively, magnetic stir bar is put into and is stirred with 950 turns/min,
With automatical potentiometric titrimeter at room temperature, it is worth using sequentially determining millivolt between fluoride ion selective electrode and reference electrode, is completed
Drawing of Curve；
Step 4: sample concentration is determined：
The accurate sample 0.2000g for weighing drying processing, adds 1.5g sodium hydroxides, is put into 30ml platinum crucibles, is added dropwise
0.2ml water, melts 2.5h at 150 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride
Volumetric flask, draws 20ml, adds 20ml ion regulating agents constant volume to 100ml volumetric flasks, is then transferred into 200ml polyvinyl chloride burning
Cup, measures the μ g/ml of sample concentration 89.56；
Step 5: Oil repellent is calculated in solution：
The concentration of the fluorine of aluminum fluoride sample will be measured（C）89.56 μ g/ml substitute into lower formula and calculated
=55.97%。
Embodiment 5：
Ion regulating agent is prepared：
Accurately weigh 70.0g sodium chloride, 350.0g sodium citrates, in the mixture add 80ml glacial acetic acid, dissolving constant volume in
1000ml volumetric flasks, are made ion regulating agent；
Step 1: sample solution is prepared：
It is accurate to weigh the aluminum fluoride 0.2000g through 120 DEG C of drying, 2.0g sodium hydroxides are added, 30ml platinum crucibles are put into, are added dropwise
0.1ml water, melts 1.5h at 200 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride
Volumetric flask, is made sample solution, and its Oil repellent is 0.543mg/ml；
Step 2: standard liquid is prepared：
It is accurate respectively after Oil repellent is dried through 120 DEG C respectively for 54.07%, 57.72%, 60.88%, 64.97% aluminum fluoride standard specimen
Aluminum fluoride standard specimen 0.2000g is really weighed, 2.0g sodium hydroxides are added, 30ml platinum crucibles are put into, 0.1ml water is added dropwise, at 200 DEG C
Lower melting 1.5h, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride volumetric flasks, difference is made
Concentration standard liquid, its Oil repellent is respectively 0.4326mg/ml, 0.4617mg/ml, 0.4870mg/ml, 0.5198mg/ml；
Step 3: Drawing of Curve：
The standard liquid 5ml of Oil repellent in step 2 54.07% is accurately pipetted into 100ml volumetric flasks, by the fluorine in step 2
Content is accurately pipetted into 100ml volumetric flasks for 54.07%, 57.72%, 60.88%, 64.97% each 20ml of aluminun fluoride solution, will
Oil repellent in step 2 is accurately pipetted into 100ml volumetric flasks for 64.97% aluminun fluoride solution 25ml, be separately added into 5ml from
Sub- conditioning agent, with water constant volume to 100ml, its fluorinion concentration is respectively 21.628 μ g/ml, 86.512 μ g/ml, 92.352 μ g/
Ml, 97.408 μ g/ml, 103.952 μ g/ml, 129.94 μ g/ml, 200ml polyvinyl chloride beakers are moved into by above-mentioned solution respectively
In, sequentially determining millivolt value completes Drawing of Curve；
Above-mentioned solution is moved into 200ml polyvinyl chloride beakers respectively, magnetic stir bar is put into and is stirred with 1050 turns/min,
With automatical potentiometric titrimeter at room temperature, it is worth using sequentially determining millivolt between fluoride ion selective electrode and reference electrode, is completed
Drawing of Curve；
Step 4: sample concentration is determined：
The accurate sample 0.2000g for weighing drying processing, adds 2.0g sodium hydroxides, is put into 30ml platinum crucibles, is added dropwise
0.1ml water, melts 1.5h at 200 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polyvinyl chloride
Volumetric flask, draws 20ml, adds 5ml ion regulating agents constant volume to 100ml volumetric flasks, is then transferred into 200ml polyvinyl chloride burning
Cup, measures the μ g/ml of sample concentration 103.80；
Step 5: Oil repellent is calculated in solution：
The concentration of the fluorine of aluminum fluoride sample will be measured（C）103.80 μ g/ml substitute into lower formula and calculated
=64.88%。
Claims (5)
1. a kind of ion regulating agent, it is characterised in that：The ion regulating agent is per 1000ml by following parts by weight and parts by volume
Raw material is made jointly：Wherein the raw material of parts by weight includes 25-35 parts of sodium chloride and 125-175 parts of sodium citrate, the original of parts by volume
Material includes 25-40 parts of glacial acetic acid, and surplus is water.
2. ion regulating agent according to claim 1, it is characterised in that：The ion regulating agent is per 1000ml by following weight
The raw material of part and parts by volume is made jointly：Wherein the raw material of parts by weight includes 29 parts of sodium chloride and 135 parts of sodium citrate, parts by volume
Raw material include 30 parts of glacial acetic acid, surplus is water.
3. application of the ion regulating agent described in claim 1 or 2 in aluminum fluoride in fluorine content determination method, it is characterised in that
Comprise the following steps：
Step 1: sample solution is prepared：
It is accurate to weigh the aluminum fluoride 0.2000g through 120 DEG C of drying, 1.0-2.0g sodium hydroxides are added, 30ml platinum crucibles are put into,
0.1-0.2ml water is added dropwise, 1.5-2.5h is melted at 150-300 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, shifts
To 250ml polyvinyl chloride volumetric flasks, sample solution is made；
Step 2: standard liquid is prepared：
It is accurate respectively after Oil repellent is dried through 120 DEG C respectively for 54.07%, 57.72%, 60.88%, 64.97% aluminum fluoride standard specimen
Aluminum fluoride standard specimen 0.2000g is really weighed, 1.0-2.0g sodium hydroxides are added, 30ml platinum crucibles are put into, 0.1-0.2ml is added dropwise
Water, melts 1.5-2.5h at 150-300 DEG C, takes out after cooling, is diluted with water and is settled to 250ml, be transferred to 250ml polychlorostyrene second
Alkene volumetric flask, is made sample solution；
Step 3: Drawing of Curve：
The standard liquid 5ml of Oil repellent in step 2 54.07% is accurately pipetted into 100ml volumetric flasks, by the fluorine in step 2
Content is accurately pipetted into 100ml volumetric flasks for 54.07%, 57.72%, 60.88%, 64.97% each 20ml of aluminun fluoride solution, will
Oil repellent in step 2 is accurately pipetted into 100ml volumetric flasks for 64.97% aluminun fluoride solution 25ml, is separately added into 5-
20ml ion regulating agents, with water constant volume to 100ml；
Above-mentioned solution is moved into 200ml polyvinyl chloride beakers respectively, magnetic stir bar is put into and stirs, is dripped with automatic current potential
Determine instrument at room temperature, be worth using sequentially determining millivolt between fluoride ion selective electrode and reference electrode, complete Drawing of Curve；
Step 4: sample concentration is determined：
The accurate sample 0.2000g for weighing drying processing, adds 1.0-2.0g sodium hydroxides, is put into 30ml platinum crucibles, drips
Plus 0.1-0.2ml water, 1.5-2.5h is melted at 150-300 DEG C, is taken out after cooling, is diluted with water and is settled to 250ml, be transferred to
250ml polyvinyl chloride volumetric flasks, are made sample solution；
Pipette samples solution 20ml, adds 10ml ion regulating agents constant volume to 100ml volumetric flasks, is then transferred into 200ml polychlorostyrene
Ethene beaker, measures sample concentration；
Step 5: Oil repellent is calculated in solution.
4. application of the ion regulating agent in aluminum fluoride in fluorine content determination method according to claim 3, it is characterised in that：
The rotating speed of magnetic stir bar described in step 4 is that 900-1100 turns/min.
5. application of the ion regulating agent in aluminum fluoride in fluorine content determination method according to claim 4, it is characterised in that：
The rotating speed of magnetic stir bar described in step 4 is 1000 turns/min.
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| CN201710288309.9A CN107192629A (en) | 2017-04-27 | 2017-04-27 | A kind of ion regulating agent and its application in aluminum fluoride in fluorine content determination method |
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| CN201710288309.9A CN107192629A (en) | 2017-04-27 | 2017-04-27 | A kind of ion regulating agent and its application in aluminum fluoride in fluorine content determination method |
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| CN107271530A (en) * | 2017-07-17 | 2017-10-20 | 云南云天化股份有限公司 | A kind of method of Oil repellent in fluorine-containing organic solvent of Accurate Determining |
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