CN109374821A - The measuring method of zirconium content in rutile - Google Patents
The measuring method of zirconium content in rutile Download PDFInfo
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Abstract
The invention belongs to technical field of analytical chemistry, and in particular to the measuring method of zirconium content in a kind of rutile.Method for zirconium content in existing measurement rutile sample is all instrumental method, determination of the upper limit is less than 3%, not the problem of not being suitable for the measurement of high-content zirconium in titanium dioxide, the present invention provides a kind of measuring method of zirconium content in rutile, the following steps are included: a, addition sodium peroxide and di-iron trioxide, add the melting of rutile sample；B, it by fusing sample water extraction, boils；C, hydrochloric acid is added；D, stannous chloride is added, until solution is become colorless by yellow, adds xylenol orange indicator, is titrated with EDTA standard solution；E, zirconium content in rutile is calculated.Measuring method of the invention can ensure the dissolution of titanium dioxide sample completely, and measurement result is accurate, and preci-sion and accuracy is all very high；The present invention is classical analysis method simultaneously, can measure the sample that zirconium content reaches 20%, the scope of application is wider.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to the measuring method of zirconium content in a kind of rutile.
Background technique
Rutile is one of numerous beach placers, since rutile has widely in industrial production, daily life
Purposes, old friends are increasing to rutile demand, also higher and higher to rutile quality requirements, to rutile at product examine
It is also essential to the detection of the impurity elements such as iron, zirconium, silicon except the inspection to host element titanium dioxide in testing.For rutile
The measurement of middle zr element, the country have more research, the representational " ICP- that spectrographic laboratory is published in for Wu Tianliang etc.
Zirconium dioxide, di-iron trioxide, dioxide-containing silica in AES measurement rutile ", old figure outstanding person " river sand mine and the golden red delivered
The spectrum analysis of zirconium oxide in stone ", " ICP-AES that delivers of Yang Xue " ICP-AES measurement rutile in zirconium ", the Li Rong that newly deliver
Zirconium in measurement rutile and ilmenite " and raw clean " ICP-AES method measures zirconium, zirconium in rutile " delivered of analogy.Wherein, " ICP-
AES measures zirconium dioxide, di-iron trioxide, dioxide-containing silica in rutile ", " ICP-AES measure rutile in zirconium ",
" zirconium in ICP-AES measurement rutile and ilmenite " and " zirconium, zirconium in ICP-AES method measurement rutile " document is all made of ICP-
AES measures zirconium content in rutile；" spectrum analysis of zirconium oxide in river sand mine and rutile " measures golden red using direct-current arc
Zirconium content in stone.The above method is all made of zirconium content in instrumental method rutile, and determination of the upper limit is not suitable for less than 3%
The measurement of high-content zirconium in titanium dioxide.
Summary of the invention
The technical problem to be solved in the present invention are as follows: the method for zirconium content is all instrumental method in existing measurement rutile sample,
Determination of the upper limit is less than 3%, the problem of not being suitable for the measurement of high-content zirconium in titanium dioxide.
The technical solution of present invention solution above-mentioned technical problem are as follows: a kind of measuring method of zirconium content in rutile is provided.
Method includes the following steps:
A, sodium peroxide and di-iron trioxide are added in crucible, adds rutile sample, is melted at 700~800 DEG C
Melt；
B, the samples with water after step a melting is leached, boils 1~5min；
C, hydrochloric acid is added in the solution obtained to step b, additional amount is that 1.1~1.3mol/L is with concentration of hydrochloric acid in solution
It is quasi-；
D, stannous chloride is added in the sample solution obtained to step c, until solution is become colorless by yellow, adds two
Cresols orange indicator is titrated with EDTA standard solution, until sample solution is yellow, records EDTA standard solution usage amount V；It presses
Above-mentioned steps carry out blank test, titrate blank test solution, and record EDTA standard titration solution volume is V0；
E, zirconium content in rutile is calculated；Calculation formula are as follows:
In formula:
C --- EDTA standard titration solution substance withdrawl syndrome, unit mol/L；
V --- titration sample solution EDTA standard titration solution volume, unit mL；
V0--- titration blank test solution E DTA standard titration solution volume, unit mL；
M --- sample amount, unit g；
91.22 --- zirconium, unit g/mol.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, sodium peroxide described in step a, di-iron trioxide and
The additional amount of rutile sample are as follows: sodium peroxide 2g~3g, di-iron trioxide are added in every 0.25g~0.5g rutile sample
0.1g~0.2g.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, the time of melting described in step a is 15~25min.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, the concrete operations of melting described in step a are as follows: first 700
DEG C~750 DEG C of 5~10min of melting, it is warming up to 790~810 DEG C of 10~15min of melting.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, the liquor capacity that step c is obtained is 150~200mL.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, stannous chloride described in step d is that analysis is pure, and concentration is
40~60g/L.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, indicator xylenol orange described in step d is that analysis is pure,
Concentration is 1.5~2.5g/L.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, EDTA concentration of standard solution described in step d be 0.01~
0.02mol/L。
Wherein, in above-mentioned rutile in the measuring method of zirconium content, drop fixed time temperature described in step d is 60~70 DEG C.
The invention has the benefit that the present invention provides a kind of measuring method of zirconium content in rutile, the party is owned by France
In one of classical analysis method, pass through fusing sample under given conditions, it can be ensured that the dissolution of titanium dioxide sample is complete.This
Inventive method compensates for rutile zirconium content analysis method blank in classical analysis method, also solves high-content zirconium in rutile
Measurement problem, the sample that zirconium content reaches 20% can be measured.The method of the present invention is easy to operate, and measurement result is accurate and reliable,
Practicability is good, is suitable for promoting the use of.
Specific embodiment
The present invention provides a kind of measuring methods of zirconium content in rutile, comprising the following steps:
A, in the corundum crucible in advance added with 2g sodium peroxide, 0.1g~0.2g ferric oxide powder is added, weighs
0.25g~0.5g sample covers surface in corundum crucible, and with a small amount of sodium peroxide, in 700 DEG C~750 DEG C melting 5min,
800 DEG C of melting 10min are warming up to, it is cooling；
B, crucible is placed in 400mL beaker, with water extraction, washes out crucible, it will boil 1 under solution slight boiling condition~
5min；
C, precipitated with dissolving with hydrochloric acid and adjust solution acidity be 1.1~1.3mol/L, keep liquor capacity be 150~
200mL；
D, heating is boiled, slightly cold, and it is colourless, 4 drop xylenol orange indicator of addition, 60 that Reduction with Stannous Chloride solution, which is added,
Between~70 DEG C, sample solution is titrated to as yellow using EDTA standard solution, records EDTA standard solution usage amount V；By above-mentioned step
It is rapid to carry out blank test, blank test solution is titrated, record EDTA standard titration solution volume is V0；
E, zirconium content in rutile is calculated；Calculation formula are as follows:
In formula:
C --- EDTA standard titration solution substance withdrawl syndrome, unit mol/L；
V --- titration sample solution EDTA standard titration solution volume, unit mL；
V0--- titration blank test solution E DTA standard titration solution volume, unit mL；
M --- sample amount, unit g；
91.22 --- zirconium, unit g/mol.
Wherein, in order to improve the accuracy of measuring method, convenient for claiming sample, in step a samples taken be preferably 0.25g~
0.5g.2~3g of sodium peroxide, di-iron trioxide 0.1g~0.2g are added in every 0.25g~0.5g rutile sample.Sodium peroxide
For fusing sample, ferric oxide powder can ensure that titanium dioxide sample dissolves in complete and subsequent titration process and inhibit titanium water
Solution, eliminates the influence of titanium, to keep measurement result more accurate.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, stannous chloride described in step d is that analysis is pure, and concentration is
40~60g/L.After stannous chloride is added, solution can be made to be become colorless by yellow, discoloration is sharp, convenient for observation.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, indicator xylenol orange described in step d is that analysis is pure,
Concentration is 1.5~2.5g/L.In order to guarantee good indicating effect, the best matching while using of indicator, additional amount is 2~4 drops.
Wherein, in above-mentioned rutile in the measuring method of zirconium content, EDTA concentration of standard solution described in step d be 0.01~
0.02mol/L。
Wherein, in above-mentioned rutile in the measuring method of zirconium content, in order to make zirconium be quick on the draw with EDTA, measurement result is more
Accurately, step d drop fixed time temperature is 60~70 DEG C.
Measuring method key of the present invention is that melt stage joined sodium peroxide and di-iron trioxide melts jointly, peroxide
Change sodium and be used for fusing sample, ferric oxide powder can ensure that titanium dioxide sample dissolves in complete and subsequent titration process and inhibit titanium
Hydrolysis, eliminates the influence of titanium, to keep measurement result more accurate.Meanwhile present invention adds stannous chlorides to eliminate iron interference,
And solution titratable acidity is controlled, concentration of hydrochloric acid is 1.1~1.3mol/L in solution, is titrated at 60~70 DEG C, above-mentioned
Process cooperates jointly, constitutes the technical solution of an entirety, so that measurement result of the present invention is more accurate, has also started using warp
Allusion quotation analysis method measures the beginning of zirconium content in rutile, since the present invention is classical analysis method, can be suitable for measurement zirconium
Content reaches 20% sample, and measurement sample is more extensive.
Explanation will be further explained to a specific embodiment of the invention by embodiment below, but do not indicated this
The protection scope of invention is limited in range described in embodiment.
Embodiment 1 is using zirconium content in the method for the present invention measurement rutile
5 corundum crucibles are taken, 2g sodium peroxide is added in each, then 0.2g ferric oxide powder is added in each, respectively
It weighs five parts of 0.5g samples to make an addition in each corundum crucible, and covers surface with a small amount of sodium peroxide, melted in 750 DEG C
5min is warming up to 800 DEG C of melting 10min, cooling.Crucible is placed in 400mL beaker, is leached with warm water, crucible, solution are washed out
It is placed on low temperature electric stone or metal plate for standing a stove on as a precaution against fire, 5min is boiled under slight boiling condition, hydrochloric acid (1+1) 30mL dissolution precipitating, transfer solution to 500mL is added
In conical flask, make-up solution volume about 200mL.Heating is boiled, slightly cold, and it is colourless, 4 drop of addition that Reduction with Stannous Chloride solution, which is added,
Xylenol orange indicator, solution to be titrated are cooled between 60 DEG C~70 DEG C, with disodium ethylene diamine tetraacetate (EDTA) standardized titration
Solution to yellow is terminal.Blank test is done in company with sample.Calculate zirconium content in rutile；Calculation formula are as follows:.
In formula:
C --- EDTA standard titration solution substance withdrawl syndrome, unit mol/L；
V --- titration sample solution EDTA standard titration solution volume, unit mL；
V0--- titration blank test solution E DTA standard titration solution volume, unit mL；
M --- sample amount, unit g；
91.22 --- zirconium, unit g/mol.
Zirconium content is as shown in table 1 below in 1 sample of embodiment.
The measurement result of 1 zirconium content of table
In the sample of embodiment 1, RSD (n=5) < 3% illustrates that the method for the present invention has very high precision.
Embodiment 2 is using zirconium content in the method for the present invention measurement rutile
4 corundum crucibles are taken, 2g sodium peroxide is added in each, then 0.1g ferric oxide powder is added in each, weighs 4
The sample of part 0.25g is loaded in corundum crucible respectively, and adduction covers surface with a small amount of sodium peroxide, in 700 DEG C of melting 5min, temperature
Degree rises to 800 DEG C of melting 10min, cooling.Crucible is placed in 400mL beaker, is leached with warm water, crucible is washed out, respectively to burning
Zirconium standard solution (zirconium concentration of standard solution 1.00mg/mL) 0.00mL, 5.00mL, 10.00mL, 15.00mL, solution are added in cup
It is placed on low temperature electric stone or metal plate for standing a stove on as a precaution against fire, 5min is boiled under slight boiling condition, hydrochloric acid (1+1) 30mL dissolution precipitating, transfer solution to 500mL is added
In conical flask, make-up solution volume about 200mL.Heating is boiled, slightly cold, and it is colourless, 4 drop of addition that Reduction with Stannous Chloride solution, which is added,
Xylenol orange indicator, solution to be titrated are cooled between 60 DEG C~70 DEG C, with disodium ethylene diamine tetraacetate (EDTA) standardized titration
Solution to yellow is terminal.Blank test is done in company with sample.Calculate zirconium content in rutile；Calculation formula are as follows:.
In formula:
C --- EDTA standard titration solution substance withdrawl syndrome, unit mol/L；
V --- titration sample solution EDTA standard titration solution volume, unit mL；
V0--- titration blank test solution E DTA standard titration solution volume, unit mL；
M --- sample amount, unit g；
91.22 --- zirconium, unit g/mol.
It is as shown in table 2 below that embodiment 2 measures obtained zirconium content.
The experiment of the 2 zirconium amount rate of recovery of table
| Zirconium amount, mg is added | 0.0 | 5.00 | 10.00 | 15.00 |
| Measure zirconium amount, mg | 3.85 | 8.96 | 13.65 | 18.65 |
| Recycle zirconium amount, mg | / | 5.11 | 9.80 | 11.8 |
| The rate of recovery, % | / | 102.2 | 98.0 | 98.67 |
In the sample of embodiment 2, the rate of recovery is between 98~103%, it was demonstrated that the method for the present invention has very high accuracy.
3 existing method of comparative example measures zirconium content in rutile
4 corundum crucibles are taken, 2.5g sodium peroxide is added in each, then 0.2g ferric oxide powder is added in each, point
4 different taste rutile sample 0.5g are also known as taken to cover surface in corresponding corundum crucible, and with a small amount of sodium peroxide, in
750 DEG C of melting 5min are warming up to 800 DEG C of melting 10min, cooling.Crucible is placed in 400mL beaker, is leached with warm water, is washed out
Crucible, solution are placed on low temperature electric stone or metal plate for standing a stove on as a precaution against fire, and 5min is boiled under slight boiling condition, and hydrochloric acid (1+1) 30mL dissolution precipitating is added, shifts molten
Liquid is into 500mL conical flask, make-up solution volume about 200mL.Heating is boiled, slightly cold, and addition Reduction with Stannous Chloride solution is nothing
3 drop xylenol orange indicator are added in color, and solution to be titrated is cooled between 60 DEG C~70 DEG C, with disodium ethylene diamine tetraacetate
(EDTA) standard titration solution to yellow is terminal.Blank test is done in company with sample.Calculate zirconium content in rutile；Calculation formula
Are as follows:
In formula:
C --- EDTA standard titration solution substance withdrawl syndrome, unit mol/L；
V --- titration sample solution EDTA standard titration solution volume, unit mL；
V0 --- titration blank test solution E DTA standard titration solution volume, unit mL；
M --- sample amount, unit g；
91.22 --- zirconium, unit g/mol.
It is as shown in table 3 below that comparative example 3 measures obtained zirconium content.
The measurement result of zirconium in 3 rutile of table
| 1# | 2# | 3# | 4# | |
| ICP-AES | 0.550 | 0.776 | 0.920 | 1.25 |
| The method of the present invention | 0.532 | 0.755 | 0.948 | 1.28 |
By embodiment and comparative example it is found that being contained the present invention provides a kind of using zirconium in classical analysis method measurement titanium dioxide
The method of amount, accuracy is high, and precision is good, easy to operate, has extensive popularization and application foreground.
Claims (9)
1. the measuring method of zirconium content in rutile, which comprises the following steps:
A, sodium peroxide and di-iron trioxide are added in crucible, adds rutile sample, is melted at 700~800 DEG C；
B, the samples with water after step a melting is leached, boils 1~5min；
C, it is added hydrochloric acid in the solution obtained to step b, it is 1.1~1.3mol/L that additional amount, which is subject to concentration of hydrochloric acid in solution,；
D, stannous chloride is added in the sample solution obtained to step c, until solution is become colorless by yellow, adds xylenol
Orange indicator is titrated with EDTA standard solution, until sample solution is yellow, records EDTA standard solution usage amount V；By above-mentioned
Step carries out blank test, titrates blank test solution, and record EDTA standard titration solution volume is V0；
E, zirconium content in rutile is calculated；Calculation formula are as follows:
In formula:
C --- EDTA standard titration solution substance withdrawl syndrome, unit mol/L；
V --- titration sample solution EDTA standard titration solution volume, unit mL；
V0--- titration blank test solution E DTA standard titration solution volume, unit mL；
M --- sample amount, unit g；
91.22 --- zirconium, unit g/mol.
2. the measuring method of zirconium content in rutile according to claim 1, it is characterised in that: peroxide described in step a
Change the additional amount of sodium, di-iron trioxide and rutile sample are as follows: sodium peroxide 2g is added in every 0.25g~0.5g rutile sample
~3g, di-iron trioxide 0.1g~0.2g.
3. the measuring method of zirconium content in rutile according to claim 1, it is characterised in that: melted described in step a
Time be 15~25min.
4. the measuring method of zirconium content in rutile according to claim 1, it is characterised in that: melted described in step a
Concrete operations are as follows: first 700 DEG C~750 DEG C 5~10min of melting, be warming up to 790~810 DEG C of 10~15min of melting.
5. the measuring method of zirconium content in rutile according to claim 1, it is characterised in that: the solution that step c is obtained
Volume is 150~200mL.
6. the measuring method of zirconium content in rutile according to claim 1, it is characterised in that: protochloride described in step d
Tin is that analysis is pure, and concentration is 40~60g/L.
7. the measuring method of zirconium content in rutile according to claim 1, it is characterised in that: indicator described in step d
Xylenol orange is that analysis is pure, and concentration is 1.5~2.5g/L.
8. the measuring method of zirconium content in rutile according to claim 1, it is characterised in that: the mark of EDTA described in step d
Quasi- solution concentration is 0.01~0.02mol/L.
9. the measuring method of zirconium content in rutile according to claim 1, it is characterised in that: titrated described in step d
Shi Wendu is 60~70 DEG C.
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