CN106596429B - The measuring method of silica in fluorine-containing sample - Google Patents
The measuring method of silica in fluorine-containing sample Download PDFInfo
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Abstract
The present invention relates to steel and ferroalloy chemical analysis technology fields, disclose a kind of measuring method of silica in fluorine-containing sample, this method comprises: (1) is in the presence of borax, fluorine-containing sample is subjected to the first calcination, fluorine-containing sample after obtaining the first calcination, the fluorine-containing sample include fluorine-containing clinker and/or pre-melted slag；(2) in the presence of natrium carbonicum calcinatum, the fluorine-containing sample after first calcination is subjected to the second calcination, obtains molten mixture；(3) solution of the molten mixture containing perchloric acid and aluminium chloride is leached, obtains fluorine-containing sample mother liquor；(4) dioxide-containing silica in the fluorine-containing sample mother liquor is measured using Silicon Molybdenum Blue Spectrophotometry.Silica in fluorine-containing clinker and pre-melted slag can accurately be detected using the above method of the invention, moreover, the corrosion of glassware will not be caused when detecting silica in fluorine-containing clinker and pre-melted slag using the above method of the invention.
Description
Technical field
The present invention relates to steel and ferroalloy chemical analysis technology fields, and in particular, to silica in fluorine-containing sample
Measuring method.
Background technique
When the country chemically measures dioxide-containing silica in fluorine-containing sample (such as fluorine-containing clinker and pre-melted slag) now
It generallys use sample by borax-sodium carbonate high-temperature fusion, then uses perchloric acid to be dehydrated with hydrochloric acid or perchloric acid leaching
Gravimetric method measures silicone content.Since fluorine ion a large amount of in sample exists, in emitting perchloric acid cigarette dehydration, silicon is formed with fluorine
Silicon tetrafluoride gas is run away, and is be easy to cause the detected value of silica serious relatively low or even be can't detect silica.
In addition, also there is the prior art contain using silica in Silicon Molybdenum Blue Spectrophotometry measurement fluorite and its concentrate
Amount, this method include weighing 0.10 gram of sample in silver crucible, with 3.0 grams of sodium hydroxides in 680 DEG C of high-temperature fusion samples, are being moulded
After being leached in material beaker with hot water, then it is transferred to and fills 0.5 gram of AlCl in advance3.6H2In in the plastic beaker of O and 100 milliliter of hydrochloric acid
With and 1 minute slightly boiled, cold room temperature processed with being transferred in plastic beaker immediately after 250 milliliters of Glass capacity bottle constant volumes obtain mother liquor；
Then 2.00~20.00 milliliters of mother liquors are pipetted in 100.00 milliliters of volumetric flasks, add water to about 30 milliliters of solution, 8.0 millis are added
Ethyl alcohol is risen, the ammonium molybdate solution of 5.0 milliliters (50g/L) is added, is mixed, it is cooling after being heated 30 seconds in boiling water bath, 10 millis are added
Sulfuric acid is risen, is mixed, 5.0 milliliters of (10g/L) ascorbic acid solutions are added, mixes, with water constant volume, measures absorbance after 30 minutes.
However, this method can only measure dioxide-containing silica in fluorite, and dioxide-containing silica in pre-melted slag cannot be measured；And it uses
When this method, fluorine ion masking is not thorough, so that mother liquor cannot be placed in glassware；And it will when containing in the mother liquor
When ammonium molybdate solution is reduced to the substance of blue, the accuracy of the testing result obtained using this method can be seriously affected.
Therefore, it is necessary to develop a kind of analysis side that can accurately detect silica in fluorine-containing clinker and pre-melted slag
Method.
Summary of the invention
The object of the present invention is to provide the analysis sides that one kind can accurately detect silica in fluorine-containing clinker and pre-melted slag
Method.
To achieve the goals above, the present invention provides a kind of measuring method of silica in fluorine-containing sample, this method packet
It includes:
(1) in the presence of borax, fluorine-containing sample is subjected to the first calcination, the fluorine-containing sample after obtaining the first calcination, institute
Stating fluorine-containing sample includes fluorine-containing clinker and/or pre-melted slag；
(2) in the presence of natrium carbonicum calcinatum, the fluorine-containing sample after first calcination is subjected to the second calcination, is melted
Melt mixture；
(3) solution of the molten mixture containing perchloric acid and aluminium chloride is leached, obtains fluorine-containing sample mother liquor；
(4) dioxide-containing silica in the fluorine-containing sample mother liquor is measured using Silicon Molybdenum Blue Spectrophotometry.
Silica in fluorine-containing clinker and pre-melted slag can accurately be detected using the above method of the invention, moreover, adopting
When detecting silica in fluorine-containing clinker and pre-melted slag with the above method of the invention, the corrosion of glassware will not be caused.
Further, in above-mentioned fluorine-containing sample of the invention silica measuring method have it is easy to operate, at low cost
Honest and clean advantage.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of measuring methods of silica in fluorine-containing sample, this method comprises:
(1) in the presence of borax, fluorine-containing sample is subjected to the first calcination, the fluorine-containing sample after obtaining the first calcination, institute
Stating fluorine-containing sample includes fluorine-containing clinker and/or pre-melted slag；
(2) in the presence of natrium carbonicum calcinatum, the fluorine-containing sample after first calcination is subjected to the second calcination, must be melted
Mixture；
(3) solution of the molten mixture containing perchloric acid and aluminium chloride is leached, obtains fluorine-containing sample mother liquor；
(4) dioxide-containing silica in the fluorine-containing sample mother liquor is measured using Silicon Molybdenum Blue Spectrophotometry.
Preferably, it is 1005-1050 DEG C that the condition of first calcination, which includes: temperature, time 10-45min.Further
It is preferred that it is 1015-1030 DEG C that the condition of first calcination, which includes: temperature, time 20-25min.The present inventor's hair
Existing, it is 1015-1030 DEG C that the condition for controlling first calcination, which includes: temperature,, can be more accurate when the time is 20-25min
Ground measures the content of silica in fluorine-containing sample.
Preferably, in step (1), the dosage weight ratio of the borax and the fluorine-containing sample is 6-10:1.
Preferably, before carrying out the step (2), first the fluorine-containing sample after first calcination is cooled to room temperature.
Preferably, it is 900-910 DEG C that the condition of second calcination, which includes: temperature, and the time is no less than 30min.Into one
Preferably, the condition of second calcination includes: that temperature is 900-910 DEG C to step, time 30-40min.The present inventor
It was found that it is 900-910 DEG C that the condition of control second calcination, which includes: temperature, it, can be more accurate when the time is 30-40min
Ground measures the content of silica in fluorine-containing sample.
Preferably, in step (2), the dosage weight of the fluorine-containing sample in the natrium carbonicum calcinatum and step (1)
Than for 20-40:1.
Preferably, before carrying out the step (3), the molten mixture that step (2) obtains first is cooled to room
Temperature.
Preferably, in step (3), the dosage weight ratio of the perchloric acid and the fluorine-containing sample in step (1) is
The dosage weight ratio of 150-225:1, the aluminium chloride and the fluorine-containing sample in step (1) is 40-80:1.
Preferably, in step (3), by the molten mixture step of the solution leaching containing perchloric acid and aluminium chloride
Suddenly include: successively to mix the perchloric acid with water and aluminium chloride, form the solution containing perchloric acid and aluminium chloride,
Then the molten mixture is leached containing the solution of perchloric acid and aluminium chloride by described.It was found by the inventors of the present invention that using
First the perchloric acid is successively mixed with water and aluminium chloride, forms the solution containing perchloric acid and aluminium chloride, then
When the solution containing perchloric acid and aluminium chloride is leached the step of the molten mixture, it can more accurately measure and contain
Dioxide-containing silica in fluorine sample.
It is further preferred that solution of the molten mixture containing perchloric acid and aluminium chloride is soaked in step (3)
The condition taken includes: that temperature is room temperature to being heated to boiling, and the time, which is that fusant is immersed, to be taken entirely.
Preferably, the content of fluorine element is greater than 0 weight % to less than to be equal to 50 weight % in the fluorine-containing sample；It is more excellent
Selection of land, the content of fluorine element is 3-30 weight % in the fluorine-containing sample.
Preferably, the fluorine-containing clinker is pre-melted slag and copper smelter slag containing calcirm-fluoride.
It preferably, include in calcirm-fluoride, calcium oxide, magnesia, aluminium oxide, iron oxide and silica in the pre-melted slag
At least one.
Preferably, the step of dioxide-containing silica in the fluorine-containing sample mother liquor being measured using Silicon Molybdenum Blue Spectrophotometry
Include: by the fluorine-containing sample mother liquor successively with ammonium molybdate solution, liquor potassic permanganate, oxalic acid solution and l ferrous ammonium sulfate solution
Mixing, and measure the absorbance of the solution obtained after mixing.
Preferably, the Silicon Molybdenum Blue Spectrophotometry is by the content of silica in measurement fluorite standard sample to make
Standard curve.
According to the first preferred embodiment, when content >=8 weights of the silica in the fluorine-containing sample
When measuring %, this method of the invention further comprises: before ammonium molybdate solution is added, it is described fluorine-containing that perchloric acid adjusting is first added
The acidity of sample mother liquor color acidity to needed for forming silicon-molybdenum heteropoly acid.
According to second of preferred embodiment, when 8 weight of content < of the silica in the fluorine-containing sample
When measuring %, the fluorine-containing sample mother liquor of the invention need not first mix with perchloric acid and it is direct successively with ammonium molybdate solution, Gao Meng
Sour potassium solution, oxalic acid solution and l ferrous ammonium sulfate solution mixing.It was found by the inventors of the present invention that the first is preferred using above-mentioned
When specific embodiment and second of preferred embodiment carry out the measurement of the dioxide-containing silica in fluorine-containing sample, obtain
The measurement result obtained is more preferably accurate.
Preferably, the dosage of the liquor potassic permanganate makes the solution that joined the liquor potassic permanganate in purplish red
Color.
Preferably, the absorbance of solution obtained after the measurement contact be wavelength be 660nm and/or 730nm at light
Absorption value.
In order to more accurately measure the content of the silica in the fluorine-containing sample of the invention, this field skill
Art personnel can carry out multiple dilution before preparing the fluorine-containing sample mother liquor and later to the solution of acquisition, this is for ability
Well known to field technique personnel, details are not described herein by the present invention.
Method of the invention does not limit operation instrument or container etc. involved in Silicon Molybdenum Blue Spectrophotometry particularly
It is fixed, it can be conventional use of instrument in the art or container.
It further include the production of standard curve, the preferably described standard curve of the present invention in the Silicon Molybdenum Blue Spectrophotometry
It is obtained by the corresponding absorbance of content of silica in measurement series of standards sample, also i.e. by two in standard sample
Silica content corresponds to absorbance progress linear regression and seeks standard curve function.It is illustratively given in subsequent embodiment of the invention
The production method of standard curve is gone out.
A kind of preferred embodiment according to the present invention, the method comprise the steps that
(1) in the presence of borax, fluorine-containing sample is subjected to the first calcination, the fluorine-containing sample after obtaining the first calcination, institute
Stating fluorine-containing sample includes fluorine-containing clinker and/or pre-melted slag；
(2) first the fluorine-containing sample after first calcination is cooled to room temperature；It then, will in the presence of natrium carbonicum calcinatum
Fluorine-containing sample after being cooled to first calcination of room temperature carries out the second calcination, obtains molten mixture；
(3) first the molten mixture is cooled to room temperature, then successively mixes perchloric acid with water and aluminium chloride,
The solution containing perchloric acid and aluminium chloride is formed, then solution of the molten mixture containing perchloric acid and aluminium chloride
Leaching, obtains fluorine-containing sample mother liquor；
(4) by the fluorine-containing sample mother liquor successively with ammonium molybdate solution, liquor potassic permanganate, oxalic acid solution and ferrous sulfate
Ammonium salt solution mixing, and measure the absorbance of the solution obtained after contact.
The characteristics of measuring method of silica, specifically includes that in fluorine-containing sample of the invention
1) measurement of the content of the silica suitable for the fluorine-containing sample containing fluorine clinker and/or pre-melted slag；
2) present method avoids the corrosion to glass container；
3) method of the invention is easy to operate, low in cost, and accuracy is high.
The present invention will be described in detail by way of examples below.
Various raw materials used below are all from commercially available.
Unless otherwise indicated, Jin Shiyong is confirmed as analytically pure reagent and distilled water or deionized water or suitable in analysis
The water of purity.
Spectrophotometry point is carried out according to 7729 metallurgic product chemical analysis method of GB-spectrophotometry general rule
Analysis.
It is sampled and makes according to 20066 steel of GB/T and the sampling of iron-chemical composition sample and method for making sample
Sample.
Perchloric acid solution: there are two types of tools, wherein when leaching molten mixture, the perchloric acid that is mixed with liquor alumini chloridi
The perchloric acid for being 1.67g/mL for density；As the content of the silica in the fluorine-containing sample >=8 weight %, molybdenum is being added
Before acid ammonium solution, before ammonium molybdate solution is added, first be added perchloric acid (by density be 1.67g/mL perchloric acid and water with
The volume ratio of 1:9 mixes) adjust the acidity to formation silicon-molybdenum heteropoly acid of the fluorine-containing sample mother liquor needed for color acidity.
Liquor alumini chloridi: 500g/L.
Ammonium molybdate solution: 25g/L.
Oxalic acid solution: 100g/L.
L ferrous ammonium sulfate solution: 60g/L, medium therein are that the sulfuric acid that the concentrated sulfuric acid and the water that volume ratio is 5:95 are formed is molten
Liquid.
Liquor potassic permanganate: 40g/L.
Fluorine-containing clinker standard items: it is purchased from Anshan iron and steel plant steel research institute.
Table 1 is that the permitted measurement of the fluorine-containing sample of different dioxide-containing silicas is poor.
Table 1
| Dioxide-containing silica, weight % | It is poor to allow to measure |
| 0.010~0.025 | 0.003 |
| > 0.025~0.050 | 0.005 |
| > 0.050~0.100 | 0.010 |
| > 0.100~0.20 | 0.05 |
| > 0.20~1.00 | 0.07 |
| > 1.00~2.00 | 0.10 |
| > 2.00~3.00 | 0.15 |
| > 3.00~5.00 | 0.18 |
| > 5.00~10.00 | 0.20 |
| > 10.00~20.00 | 0.25 |
| > 20.00~40.00 | 0.30 |
Make standard curve
5 parts of fluorite standard items are weighed, dioxide-containing silica is in a series of, in control sample to be tested dioxies from low to high
SiClx content is within the dioxide-containing silica range of series standard sample.Above-mentioned 5 parts of fluorite standard items are respectively adopted as follows
Identical method measures absorbance:
With the 5g borax calcination 20min at 1020 DEG C after evenly mixing, then it is cooled to room temperature (25 DEG C)；It is anhydrous that 10g is added
Sodium carbonate obtains molten mixture in 900 DEG C of calcination 40min, and the molten mixture is cooled to room temperature；By the high chlorine of 60mL
Acid is mixed with the liquor alumini chloridi of 40.0mL, is formed the solution containing perchloric acid and aluminium chloride, is contained high chlorine using described
The solution of acid and aluminium chloride is complete by molten mixture heating leaching, solution is cooled to room temperature and is diluted with water is settled to
500.00mL mixes, obtains fluorine-containing sample mother liquor；When dioxide-containing silica≤8%, when, the fluorine-containing sample mother liquor of 10.00mL is pipetted,
20.0mL ammonium molybdate solution is added；As dioxide-containing silica > 8%, when, the fluorine-containing sample mother liquor of 5.00mL is pipetted, and successively to it
Middle addition 5.0mL perchloric acid solution (1+9) and 20.0mL ammonium molybdate solution mix；
Then it is in stable aubergine that liquor potassic permanganate to solution is added dropwise into solution, is placed in 30 DEG C of water-baths
10min takes out, and 10.0mL oxalic acid solution is then added into solution, 5.0mL l ferrous ammonium sulfate solution is added after mixing immediately,
It mixes, is diluted with water to 100.00mL.After placing 10min at room temperature, 1cm absorption vessel is chosen, using water as reference, in 660nm
Or absorbance is measured at 730nm.
Linear regression, which is carried out, according to the content of silica in absorbance value and standard items obtains calibration curve equation.
Embodiment 1
Weigh fluorine-containing clinker standard items (the dioxide-containing silica value of 0.5gIt is practicalFor 30.00 weight %), uniformly mixed with 6g borax
After conjunction at 1020 DEG C calcination 20min, be then cooled to 25 DEG C；12g natrium carbonicum calcinatum calcination 40min at 900 DEG C is added, obtains
The molten mixture is cooled to room temperature by molten mixture；The liquor alumini chloridi of the perchloric acid of 60mL and 40.0mL is mixed
It closes, forms the solution containing perchloric acid and aluminium chloride, using the solution containing perchloric acid and aluminium chloride by molten mixture
Leaching completely, and the solution obtained after leaching is diluted with water and is settled to 500.00mL, obtains fluorine-containing sample mother liquor；Then it pipettes
The fluorine-containing sample mother liquor of 5.00mL, and 5.0mL perchloric acid solution (1+9) and 20.0mL ammonium molybdate solution are successively added thereto, it mixes
Even, it is in stable aubergine that liquor potassic permanganate to solution is then added dropwise into solution, places 10min in 30 DEG C of water-baths, takes
Out.
Then 10.0mL oxalic acid solution is added thereto, and 5.0mL l ferrous ammonium sulfate solution is added immediately, mixes, uses water
It is diluted to 100.00mL.After placing 10min at room temperature, 1cm absorption vessel is chosen, using water as reference, extinction is measured at 660nm
Degree.
As a result: dioxide-containing silica value is calculated according to the absorbance and calibration curve equation that measureIt measuresFor 29.99 weights
Measuring the difference between %, with actual value is 0.01 weight %.
Embodiment 2
Weigh fluorine-containing clinker standard items (the dioxide-containing silica value of 0.5gIt is practicalAfter evenly mixing for 20 weight %) and 5g borax
The calcination 25min at 1030 DEG C, is then cooled to 25 DEG C；In the presence of 15g natrium carbonicum calcinatum, the sample for being cooled to room temperature is existed
Calcination 40min, obtains molten mixture at 905 DEG C, and the molten mixture is cooled to room temperature；By the perchloric acid of 60mL with
The liquor alumini chloridi of 40.0mL is mixed, and the solution containing perchloric acid and aluminium chloride is formed, using it is described containing perchloric acid and
The solution of aluminium chloride leaches molten mixture completely, and the solution obtained after leaching is diluted with water and is settled to 500.00mL,
Obtain fluorine-containing sample mother liquor；Then the fluorine-containing sample mother liquor of 5.00mL is pipetted, and 5.0mL perchloric acid solution (1+ is successively added thereto
9) it with 20.0mL ammonium molybdate solution, mixes, it is in stable aubergine that liquor potassic permanganate to solution is then added dropwise thereto, in 30
10min is placed in DEG C water-bath, is taken out.
Then 10.0mL oxalic acid solution is added thereto, and 5.0mL l ferrous ammonium sulfate solution is added immediately, mixes, uses water
It is diluted to 100.00mL.After placing 10min at room temperature, 1cm absorption vessel is chosen, using water as reference, extinction is measured at 660nm
Degree.
As a result: dioxide-containing silica value is calculated according to the absorbance and calibration curve equation that measureIt measuresFor 20.00 weights
It measures between %, with actual value without difference.
Embodiment 3
Weigh fluorine-containing clinker standard items (the dioxide-containing silica value of 0.5gIt is practicalFor 1.07 weight %), uniformly mixed with 4g borax
The calcination 20min at 1015 DEG C afterwards, is then cooled to 25 DEG C；15g natrium carbonicum calcinatum calcination 30min at 910 DEG C is being added, is obtaining
The molten mixture is cooled to room temperature by molten mixture；The liquor alumini chloridi of the perchloric acid of 60mL and 40.0mL is mixed
It closes, forms the solution containing perchloric acid and aluminium chloride, it is using the solution containing perchloric acid and aluminium chloride that the melting is mixed
It closes object leaching completely, and the solution obtained after leaching is diluted with water and is settled to 500.00mL, obtain fluorine-containing sample mother liquor；Then it moves
20.0mL ammonium molybdate solution is added in fluorine-containing sample mother liquor after taking 10.00mL constant volume, mixes, permanganic acid is then added dropwise thereto
Potassium solution to solution is in stable aubergine, places 10min in 30 DEG C of water-baths, is taken out.
Then 10.0mL oxalic acid solution is added thereto, and 5.0mL l ferrous ammonium sulfate solution is added immediately, mixes, uses water
It is diluted to 100.00mL.After placing 10min at room temperature, 1cm absorption vessel is chosen, using water as reference, extinction is measured at 730nm
Degree.
As a result: dioxide-containing silica value is calculated according to the absorbance and calibration curve equation that measureIt measuresFor 1.07 weights
It measures between %, with actual value without difference.
Embodiment 4
The present embodiment is carried out using method same as Example 1, except that:
The temperature of the first calcination is 1000 DEG C in the present embodiment.
Remaining is in the same manner as in Example 1.
As a result: dioxide-containing silica value is calculated according to the absorbance and calibration curve equation that measureIt measuresFor 29.96 weights
Measuring the difference between %, with actual value is 0.04 weight %.
Test case 1
Test case 1 is carried out using method same as Example 1, except that:
Sample detected is all from commercially available in test case, specifically as shown in table 2.
As a result also as shown in table 2.
Accordingly, it is also found in using the result and standard value and tolerance of the commercially available sample of the method detection of the prior art
In table 2.
Table 2
It can be seen from the results above that using of the invention when measuring the content of silica in fluorine-containing sample, it is resulting
As a result thus accuracy illustrates that method of the invention has significantly higher accuracy in claimed range.Moreover, upper
During stating embodiment, no glass is corroded phenomenon.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (12)
1. the measuring method of silica in a kind of fluorine-containing sample, which is characterized in that this method comprises:
(1) in the presence of borax, fluorine-containing sample is subjected to the first calcination, the fluorine-containing sample after obtaining the first calcination is described to contain
Fluorine sample includes fluorine-containing clinker and/or pre-melted slag；
(2) in the presence of natrium carbonicum calcinatum, the fluorine-containing sample after first calcination is subjected to the second calcination, it is mixed to obtain melting
Close object；
(3) solution of the molten mixture containing perchloric acid and aluminium chloride is leached, obtains fluorine-containing sample mother liquor；
(4) dioxide-containing silica in the fluorine-containing sample mother liquor is measured using Silicon Molybdenum Blue Spectrophotometry；
Wherein, in step (3), the step of solution leaching of the molten mixture containing perchloric acid and aluminium chloride, is wrapped
It includes: the perchloric acid is successively mixed with water and aluminium chloride, form the solution containing perchloric acid and aluminium chloride, then
The molten mixture is leached containing the solution of perchloric acid and aluminium chloride by described.
2. the condition of first calcination includes: that temperature is 1005-1050 DEG C according to the method described in claim 1, wherein,
Time is 10-45min.
3. according to the method described in claim 1, wherein, in step (1), the dosage weight of the borax and the fluorine-containing sample
Amount is than being 6-10:1.
4. the condition of second calcination includes: that temperature is 900-910 DEG C according to the method described in claim 1, wherein, when
Between for no less than 30min.
5. the institute according to the method described in claim 1, wherein, in step (2), in the natrium carbonicum calcinatum and step (1)
The dosage weight ratio for stating fluorine-containing sample is 20-40:1.
6. method described in any one of -5 according to claim 1, wherein in step (3), the perchloric acid and step
(1) the dosage weight ratio of the fluorine-containing sample in is 150-225:1, the fluorine-containing examination in the aluminium chloride and step (1)
The dosage weight ratio of sample is 40-80:1.
7. method described in any one of -5 according to claim 1, wherein the content of fluorine element is big in the fluorine-containing sample
In 0 weight % to less than it is equal to 50 weight %.
8. according to the method described in claim 1, wherein, being measured in the fluorine-containing sample mother liquor using Silicon Molybdenum Blue Spectrophotometry
Dioxide-containing silica the step of include: by the fluorine-containing sample mother liquor successively with ammonium molybdate solution, liquor potassic permanganate, oxalic acid
Solution and l ferrous ammonium sulfate solution mixing, and measure the absorbance of the solution obtained after mixing.
9. according to the method described in claim 8, wherein, the Silicon Molybdenum Blue Spectrophotometry passes through in measurement fluorite standard sample
The content of silica is to make standard curve.
10. according to the method described in claim 8, wherein, as content >=8 weight % of the silica in the fluorine-containing sample
When, before ammonium molybdate solution is added, perchloric acid is first added, and to adjust the acidity of the fluorine-containing sample mother liquor miscellaneous more to formation silicon molybdenum
Color acidity needed for acid.
11. according to the method described in claim 8, wherein, the dosage of the liquor potassic permanganate to joined the Gao Meng
The solution of sour potassium solution is in aubergine.
12. the method according to any one of claim 8-11, wherein the absorbance be wavelength be 660nm and/or
Absorbance value at 730nm.
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