CN106404764B - The detection method of low content germanium in zinc calcine - Google Patents
The detection method of low content germanium in zinc calcine Download PDFInfo
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Abstract
The invention belongs to the detection fields of germanium, and in particular to the detection method of low content germanium in a kind of zinc calcine.The method of low content germanium in calcining is not detected for the prior art, detection difficulty is high, the big problem of error, the present invention provides a kind of detection method of low content germanium in zinc calcine, comprising the following steps: Specification Curve of Increasing, sample preparation, chromogenic reaction, blank control, the operation such as calculate Ge content first pass through acid and all dissolve germanium, and exclude the interference of other impurities element, network occurs with germanium with phenylfluorone again and reacts, according to the absorbance of reaction complex compound, measures wherein Ge content.The method of the present invention is easy to operate, favorable reproducibility, and testing result error is small, and accuracy is high, it is thus also avoided that is suitable for promoting the use of using polluting caused by when carbon tetrachloride method extracted germanium.
Description
Technical field
The invention belongs to the detection fields of germanium, and in particular to the detection method of low content germanium in a kind of zinc calcine.
Background technique
Germanium is the important materials of modern high technology, is widely used in electrical equipment industry, defense military, space flight and aviation, doctor
The stratospheres such as medicine health.Because germanium is rare element, and value is very high, and each chemical company is existing to the purification of germanium very much
Germanium is improved company's income as byproduct by research, so the analysis requirement of germanium is also higher and higher.
The method of detection germanium mostly uses greatly extraction spectrophotometric method at present, but is related to toxic organic reagent first in method
Benzene, carbon tetrachloride etc. damage the health of testing staff, the waste liquor contamination environment of discharge, and detection process is cumbersome, not easily-controllable
System, in addition antimony and germanium keep germanium determination result inaccurate there is also interfering with each other in same system.In electric zinc industry,
Contain a small amount of germanium in calcining, because its content is lower, about 0.005~0.015%, the more difficult implementation of above-mentioned detection method, inspection
Survey result inaccuracy.
Summary of the invention
The technical problem to be solved in the present invention is the detection method that the prior art does not detect low content germanium in calcining, detection
Difficulty is high, the big problem of error.
The present invention solve above-mentioned technical problem technical solution be provide it is a kind of easy to operate, at low cost, fast and accurately
The detection method of low content germanium in zinc calcine, comprising the following steps:
A, Specification Curve of Increasing
The germanium standard solution of compound concentration 10mg/L, then it is made into the germanium mark of concentration 10,5,2.5,1,0.5,0.1mg/L respectively
Quasi- solution；The standard solution of 1~2ml various concentration is taken to measure the absorbance value at 510nm respectively, using absorbance as ordinate,
Germanium concentration of standard solution is abscissa, draws standard curve；
B, sample preparation
The zinc calcine M mg that drying to constant weight is taken, phosphoric acid is added, heats 2~3min, adds nitric acid, heats 2~3min,
The concentrated sulfuric acid is added, it is bright and emit white cigarette to be heated to solution, is cooled to room temperature, being diluted to volume with distilled water is V L；
C, chromogenic reaction
In the V L sample after step b dilution, phosphoric acid, boric acid is added, adds liquor potassic permanganate to solution by purple
Become red, ascorbic acid to solution red is added and disappears, solution is colourless at this time, and it is molten that cetyl trimethylammonium bromide is added
Liquid adds phenylfluorone, until solution in stable orange red, takes 1~2ml colorimetric in spectrophotometer 510nm at, record suction
Shading value OD1；
D, blank control
Taking volume is the distilled water of V L, and phosphoric acid, boric acid, potassium permanganate, ascorbic acid, 16 with step c equivalent is added
Alkyl trimethyl ammonium bromide and phenylfluorone take 1~2ml colorimetric at spectrophotometer 510nm, record absorbance value OD2；
E, Ge content calculates in calcining
The germanium concentration at OD value=OD1-OD2 is found according to the standard curve in step a, multiplied by V, is obtained in sampling sample
Ge content obtain the percentage composition of germanium in zinc calcine divided by sampling amount M mg.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, the germanium standard solution preparation side of 10mg/L in step a
Method are as follows: weigh 0.1440g germanium dioxide reagent in 300ml beaker, the sodium hydroxide solution that 10ml l5% is added is complete to sample
Fully dissolved is neutralized to acid and excessive 2ml with the sulfuric acid of 1:5, moves in 1000ml volumetric flask, be diluted to graticule with distilled water,
It shakes up, pipettes this standard liquid 1ml into 100ml volumetric flask, be diluted to scale, be made into the standard solution that concentration is 10mg/L.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, phosphoric acid described in step b, nitric acid and the concentrated sulfuric acid
It is that analysis is pure.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, phosphoric acid, nitric acid and the sulphur of addition described in step b
The amount of acid is equal are as follows: phosphoric acid, nitric acid, each 10~15ml of the concentrated sulfuric acid are added in every 0.2g zinc calcine.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, dilution described in step b refers to: every 0.2g zinc
Calcining sample is diluted to 50~100ml.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, phosphoric acid described in step c is that analysis is pure, described
Boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is concentration 0.5~1.5%
Cetyl trimethylammonium bromide ethanol solution, the phenylfluorone is 0.08~0.1% phenylfluorone ethanol solution of concentration, described
Potassium permanganate be concentration 0.5~1.5% potassium permanganate solution, the ascorbic acid is the anti-of 15~25g/l of concentration
Bad hematic acid aqueous solution.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, the amount that phosphoric acid is added in step c is sampling amount V's
0.2~0.3 times, the amount of boric acid is added is 0.5~0.7 times of sampling amount V.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, the cetyl trimethyl bromination that is added in step c
The amount of ammonium is 0.2~0.3 times of sampling amount V.
The invention has the benefit that the present invention dissolves zinc calcine using phosphoric acid, nitric acid and sulfuric acid, it can be effectively by zinc
Germanium in calcining is dissolved in acid, while the impurity such as other Fe, Si are also dissolved in acid, and the present invention is not added hydrochloric acid, when dissolution
Germanium will not be reacted with acid, and testing result is accurate；In chromogenic reaction, the present invention joined phosphoric acid, boric acid again, make miscellaneous in sample
Matter is first aoxidized, and the interference of impurity is further eliminated；In addition, present invention adds potassium permanganate, it can be by low price germanium oxygen
It is melted into high price germanium, is sufficiently reacted with phenylfluorone, testing result is more acurrate.The method of the present invention is easy to operate, favorable reproducibility, inspection
It is small to survey resultant error, accuracy is high, it is thus also avoided that be suitable for promoting the use of using polluting caused by when carbon tetrachloride method extracted germanium.
Specific embodiment
The present invention provides a kind of detection methods of low content germanium in zinc calcine, comprising the following steps:
A, Specification Curve of Increasing
The germanium standard solution of compound concentration 10mg/L, then it is made into the germanium mark of concentration 10,5,2.5,1,0.5,0.1mg/L respectively
Quasi- solution；The standard solution of 1~2ml various concentration is taken to measure the absorbance value at 510nm respectively, using absorbance as ordinate,
Germanium concentration of standard solution is abscissa, draws standard curve；
B, sample preparation
The zinc calcine M mg that drying to constant weight is taken, phosphoric acid is added, heats 2~3min, adds nitric acid, heats 2~3min,
The concentrated sulfuric acid is added, it is bright and emit white cigarette to be heated to solution, is cooled to room temperature, being diluted to volume with distilled water is V L；
C, chromogenic reaction
In the V L sample after step b dilution, phosphoric acid, boric acid is added, adds liquor potassic permanganate to solution by purple
Become red, ascorbic acid to solution red is added and disappears, solution is colourless at this time, and it is molten that cetyl trimethylammonium bromide is added
Liquid adds phenylfluorone, until solution in stable orange red, takes 1~2ml colorimetric in spectrophotometer 510nm at, record suction
Shading value OD1；
D, blank control
Taking volume is the distilled water of V L, and phosphoric acid, boric acid, potassium permanganate, ascorbic acid, 16 with step c equivalent is added
Alkyl trimethyl ammonium bromide and phenylfluorone take 1~2ml colorimetric at spectrophotometer 510nm, record absorbance value OD2；
E, Ge content calculates in calcining
The germanium concentration at OD value=OD1-OD2 is found according to the standard curve in step a, multiplied by V, is obtained in sampling sample
Ge content obtain the percentage composition of germanium in zinc calcine divided by sampling amount M mg.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, the germanium standard solution preparation side of 10mg/L in step a
Method are as follows: weigh 0.1440g germanium dioxide reagent in 300ml beaker, the sodium hydroxide solution that 10ml l5% is added is complete to sample
Fully dissolved is neutralized to acid and excessive 2ml with the sulfuric acid of 1:5, moves in 1000ml volumetric flask, be diluted to graticule with distilled water,
It shakes up, pipettes this standard liquid 1ml into 100ml volumetric flask, be diluted to scale, be made into the standard solution that concentration is 10mg/L.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, phosphoric acid described in step b, nitric acid and the concentrated sulfuric acid
It is that analysis is pure.
Wherein, in above-mentioned zinc calcine in the detection method of low content germanium, phosphoric acid described in step c is that analysis is pure, described
Boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is concentration 0.5~1.5%
Cetyl trimethylammonium bromide ethanol solution, the phenylfluorone is 0.08~0.1% phenylfluorone ethanol solution of concentration, described
Potassium permanganate be concentration 0.5~1.5% potassium permanganate solution, the ascorbic acid is the anti-of 15~25g/l of concentration
Bad hematic acid aqueous solution.
In order to be fully dissolved in the germanium in zinc calcine in acid, and do not react with acid, the present invention using phosphoric acid, nitric acid and
Concentrated sulfuric acid dissolution zinc calcine, the weight ratio of the phosphoric acid of addition, nitric acid and the concentrated sulfuric acid are 1:1:1, and phosphorus is added in every 0.2g zinc calcine
Each 10~15ml of acid, nitric acid, the concentrated sulfuric acid.
In order to exclude the interference of the impurity such as Fe, Si, phosphoric acid, boric acid, impurity and phosphorus is first added before chromogenic reaction in the present invention
Oxidation reaction first occurs for acid, boric acid, reduces the influence to Ge content, the amount that phosphoric acid is added is 0.2~0.3 times of sampling amount V,
The amount that boric acid is added is 0.5~0.7 times of sampling amount V.
In order to make the germanium in solution react more complete with phenylfluorone, keep Ge content measurement result more acurrate, the present invention also exists
Germanium and phenylfluorone carry out network and reacts to joined cetyl trimethylammonium bromide before, additional amount for sampling amount V 0.2~
0.3 times.
Explanation is further explained to a specific embodiment of the invention below in conjunction with embodiment, but will be not of the invention
Protection scope be limited in range described in embodiment.
Phosphoric acid, nitric acid and the concentrated sulfuric acid in embodiment are that analysis is pure, and boric acid is the boric acid aqueous solution of concentration 2.5%, institute
The cetyl trimethylammonium bromide stated is the cetyl trimethylammonium bromide solution of concentration 1%, and the phenylfluorone is dense
0.09% phenylfluorone ethanol solution is spent, the potassium permanganate is the potassium permanganate solution of concentration 1%, and described is anti-bad
Hematic acid is the aqueous ascorbic acid of concentration 20g/l.
Embodiment 1 detects the germanium in calcining with the method for the present invention
A, Specification Curve of Increasing
0.1440g germanium dioxide reagent is weighed in 300ml beaker, the sodium hydroxide solution of 10ml l5% is added to sample
Product are completely dissolved, and are neutralized to acid and excessive 2ml with the sulfuric acid of 1:5, are moved in 1000ml volumetric flask, be diluted to mark with distilled water
Line shakes up, and pipettes this standard liquid 1ml into 100ml volumetric flask, is diluted to scale, is made into the standard solution that concentration is 10mg/L, then
It is diluted to the germanium standard solution of concentration 10,5,2.5,1,0.5,0.1mg/L respectively；The standard solution of 1ml various concentration is taken to distinguish
The absorbance value at 510nm is measured, using absorbance as ordinate, germanium concentration of standard solution is abscissa, draws standard curve；
B, sample preparation
It takes the zinc calcine 0.2g that drying to constant weight in 105 DEG C of baking ovens in 300ml beaker, little water is added and soaks sample
Afterwards, add 15ml phosphoric acid, heat 3min, add 15ml nitric acid, heat 3min, add the 15ml concentrated sulfuric acid, steam to bright and emit
White cigarette removes cooling, completely cooling to sample, with distilled water flushing wall of cup to volume in 50ml or so, boils, after removing cooling
It is transferred in 100ml volumetric flask, is diluted to scale；
C, chromogenic reaction
Take sample 10ml in step b that 2ml phosphoric acid, 5ml boric acid is added, adds water to 25ml scale in 50ml colorimetric cylinder, then
Potassium permanganate is added and becomes red by purple to solution, shakes up, aoxidizes 5min, 2ml ascorbic acid to solution red is added and disappears,
Solution is colourless at this time, and 2ml cetyl trimethylammonium bromide solution is added, adds phenylfluorone, until solution is in stable
It is orange red, 1ml orange-red solution colorimetric at spectrophotometer 510nm is taken, absorbance value OD1 is recorded；
D, blank control
Distilled water 10ml is taken, phosphoric acid, boric acid, potassium permanganate, ascorbic acid, cetyl three with step c equivalent is added
Methyl bromide ammonium and phenylfluorone take 1ml solution colorimetric at spectrophotometer 510nm, record absorbance value OD2；
E, Ge content calculates in calcining
The Ge content concentration at OD value=OD1-OD2 is found according to the standard curve in step a, multiplied by V, obtains measurement sample
The Ge content of product obtains the percentage composition of germanium in zinc calcine divided by sampling amount 0.2g.
Ge content measurement result in embodiment 1 in zinc calcine is as shown in table 1 below.Measurement accuracy rate=Ge measurement content/
Ge known content * 100%.
Germanium percentage composition in 1 zinc calcine of table
| Parallel number | Ge known content (%) | Ge measures content (%) | It measures accuracy rate (%) |
| 1 | 0.046 | 0.045 | 97.83 |
| 2 | 0.046 | 0.046 | 100 |
| 3 | 0.046 | 0.046 | 100 |
| 4 | 0.046 | 0.047 | 97.83 |
| 5 | 0.046 | 0.046 | 100 |
For the stability for verifying detection method, embodiment 1 is repeated, as a result as shown in table 2 below.
Germanium percentage composition in 2 zinc calcine of table
| Parallel number | Ge known content (%) | Ge measures content (%) | It measures accuracy rate (%) |
| 1 | 0.046 | 0.046 | 100 |
| 2 | 0.046 | 0.046 | 100 |
| 3 | 0.046 | 0.045 | 97.83 |
| 4 | 0.046 | 0.047 | 97.83 |
| 5 | 0.046 | 0.046 | 100 |
Can be seen that by the above results, the present invention be arranged altogether when detecting 5 it is parallel, it is each it is parallel between it is reproducible, accurate
Degree is high；In addition, the present invention repeats 2 times, testing result degree of error is minimum twice, and testing result is stable, repeatability is high.
Embodiment 2 detects the germanium in calcining with the method for the present invention
Another zinc calcine sample is taken, wherein Ge content is detected, in addition to sample is different, remaining step is obtained with embodiment 1
Testing result is as shown in table 3 below.
Germanium percentage composition in 3 zinc calcine of table
Comparative example 3 does not use the germanium in the method for the present invention detection calcining
Ge content in the zinc calcine sample in embodiment 2 is measured with fluorescence spectrophotometry method, as a result as shown in table 4 below.
The more general photometry of fluorescence spectrophotometry sensitivity is high, but the range of linearity is relatively narrow, using phenylfluorone with
Germanium develops the color in sodium acetate buffer solution, then its fluorescence intensity is measured in 0.3mol/L hydrochloric acid medium, as a result such as the following table 4 institute
Show.
Germanium percentage composition in 4 zinc calcine of table
| Number | Ge known content (%) | Ge measures content (%) | It measures accuracy rate (%) |
| 1 | 0.0041 | 0.0036 | 87.80 |
| 2 | 0.0041 | 0.0035 | 85.37 |
| 3 | 0.0041 | 0.0034 | 82.93 |
| 4 | 0.0041 | 0.0036 | 87.8 |
| 5 | 0.0041 | 0.0038 | 92.68 |
Comparative example 4 detects the germanium in calcining with carbon tetrachloride extraction method
Ge content in the zinc calcine sample in embodiment 2 is measured with carbon tetrachloride extraction method, as a result as shown in table 5 below.
The zinc calcine in 0.2g embodiment 2 is taken, 50mg anhydrous sodium sulfite is added, it is accurate that 20ml carbon tetrachloride is added, add
Hydrochloric acid 30ml, extracts immediately, stratification.Organic phase 10ml is released in 25ml dry colorimetric cylinder, isoamyl alcohol is accurately added
2ml, acetylacetone,2,4-pentanedione 4 are dripped, are shaken up, accurate that phenylfluorone solution 1ml is added, and are shaken up, after placing colour developing 5min, in spectrophotometer
Absorbance is measured at 510nm, and it is as shown in table 5 below that Ge content is calculated.
Germanium percentage composition in 5 zinc calcine of table
| Number | Ge known content (%) | Ge measures content (%) | It measures accuracy rate (%) |
| 1 | 0.0041 | 0.0034 | 82.93 |
| 2 | 0.0041 | 0.0033 | 80.49 |
| 3 | 0.0041 | 0.0032 | 78.05 |
| 4 | 0.0041 | 0.0034 | 82.93 |
| 5 | 0.0041 | 0.0035 | 85.36 |
It, can will be in zinc calcine by embodiment and comparative example it is found that detection method is improved when acid is molten
Germanium be completely dissolved out, testing result is accurate, reproducibility is high；Compared to the atomic absorption method and tetrachloro of traditional detection Ge content
Change carbon method, the method for the present invention testing result is more acurrate, reproducibility is more preferable.
Claims (18)
1. the detection method of low content germanium in zinc calcine, which comprises the following steps:
A, Specification Curve of Increasing
The germanium standard solution of compound concentration 10mg/L, then it is made into the germanium standard of 10,5,2.5,1,0.5,0.1 mg/L of concentration respectively
Solution；The standard solution of 1~2 ml various concentration is taken to measure the absorbance value at 510nm, using absorbance as ordinate, germanium respectively
Concentration of standard solution is abscissa, draws standard curve；
B, sample preparation
It takes the zinc calcine Mmg that drying to constant weight, phosphoric acid is added, heat 2~3min, add nitric acid, heat 2~3min, then plus
Enter the concentrated sulfuric acid, it is bright and emit white cigarette to be heated to solution, is cooled to room temperature, being diluted to volume with distilled water is V L；
C, chromogenic reaction
In the V L sample after step b dilution, phosphoric acid, boric acid is added, adds liquor potassic permanganate and is become to solution by purple
Red is added ascorbic acid to solution red and disappears, and solution is colourless at this time, and cetyl trimethylammonium bromide solution is added,
Phenylfluorone is added, until solution in stable orange red, takes 1~2ml colorimetric in spectrophotometer 510nm at, record extinction
Angle value OD1；
D, blank control
Taking volume is the distilled water of V L, and phosphoric acid, boric acid, potassium permanganate, ascorbic acid, cetyl with step c equivalent is added
Trimethylammonium bromide and phenylfluorone take 1~2ml colorimetric at spectrophotometer 510nm, record absorbance value OD2；
E, Ge content calculates in calcining
The germanium concentration at OD value=OD1-OD2 is found according to the standard curve in step a, multiplied by volume V, is obtained in sampling sample
Ge content obtain the percentage composition of germanium in zinc calcine divided by sampling amount M mg.
2. the detection method of low content germanium in zinc calcine according to claim 1, it is characterised in that: described in step b
Phosphoric acid, nitric acid and the concentrated sulfuric acid are that analysis is pure.
3. the detection method of low content germanium in zinc calcine according to claim 1, it is characterised in that: add described in step b
The amount of the phosphoric acid, nitric acid and the sulfuric acid that enter is equal are as follows: phosphoric acid, nitric acid, each 10~15ml of sulfuric acid are added in every 0.2g zinc calcine.
4. the detection method of low content germanium in zinc calcine according to claim 2, it is characterised in that: add described in step b
The amount of the phosphoric acid, nitric acid and the sulfuric acid that enter is equal are as follows: phosphoric acid, nitric acid, each 10~15ml of sulfuric acid are added in every 0.2g zinc calcine.
5. the detection method of low content germanium in zinc calcine according to claim 1, it is characterised in that: described in step b
Dilution refers to: every 0.2g zinc calcine sample is diluted to 50~100ml.
6. the detection method of low content germanium in zinc calcine according to claim 2, it is characterised in that: described in step b
Dilution refers to: every 0.2g zinc calcine sample is diluted to 50~100ml.
7. the detection method of low content germanium in zinc calcine according to claim 3, it is characterised in that: described in step b
Dilution refers to: every 0.2g zinc calcine sample is diluted to 50~100ml.
8. the detection method of low content germanium in zinc calcine according to claim 4, it is characterised in that: described in step b
Dilution refers to: every 0.2g zinc calcine sample is diluted to 50~100ml.
9. the detection method of low content germanium in zinc calcine according to claim 1, it is characterised in that: described in step c
Phosphoric acid is that analysis is pure, and the boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is
The cetyl trimethylammonium bromide ethanol solution of concentration 0.5~1.5%, the phenylfluorone are 0.08~0.1% benzene fluorenes of concentration
Ketone ethanol solution, the potassium permanganate are the potassium permanganate solution of concentration 0.5~1.5%, and the ascorbic acid is concentration
The aqueous ascorbic acid of 15~25g/l.
10. the detection method of low content germanium in zinc calcine according to claim 2, it is characterised in that: described in step c
Phosphoric acid is that analysis is pure, and the boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is
The cetyl trimethylammonium bromide ethanol solution of concentration 0.5~1.5%, the phenylfluorone are 0.08~0.1% benzene fluorenes of concentration
Ketone ethanol solution, the potassium permanganate are the potassium permanganate solution of concentration 0.5~1.5%, and the ascorbic acid is concentration
The aqueous ascorbic acid of 15~25g/l.
11. the detection method of low content germanium in zinc calcine according to claim 3, it is characterised in that: described in step c
Phosphoric acid is that analysis is pure, and the boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is
The cetyl trimethylammonium bromide ethanol solution of concentration 0.5~1.5%, the phenylfluorone are 0.08~0.1% benzene fluorenes of concentration
Ketone ethanol solution, the potassium permanganate are the potassium permanganate solution of concentration 0.5~1.5%, and the ascorbic acid is concentration
The aqueous ascorbic acid of 15~25g/l.
12. the detection method of low content germanium in zinc calcine according to claim 4, it is characterised in that: described in step c
Phosphoric acid is that analysis is pure, and the boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is
The cetyl trimethylammonium bromide ethanol solution of concentration 0.5~1.5%, the phenylfluorone are 0.08~0.1% benzene fluorenes of concentration
Ketone ethanol solution, the potassium permanganate are the potassium permanganate solution of concentration 0.5~1.5%, and the ascorbic acid is concentration
The aqueous ascorbic acid of 15~25g/l.
13. the detection method of low content germanium in zinc calcine according to claim 5, it is characterised in that: described in step c
Phosphoric acid is that analysis is pure, and the boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is
The cetyl trimethylammonium bromide ethanol solution of concentration 0.5~1.5%, the phenylfluorone are 0.08~0.1% benzene fluorenes of concentration
Ketone ethanol solution, the potassium permanganate are the potassium permanganate solution of concentration 0.5~1.5%, and the ascorbic acid is concentration
The aqueous ascorbic acid of 15~25g/l.
14. the detection method of low content germanium in zinc calcine according to claim 6, it is characterised in that: described in step c
Phosphoric acid is that analysis is pure, and the boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is
The cetyl trimethylammonium bromide ethanol solution of concentration 0.5~1.5%, the phenylfluorone are 0.08~0.1% benzene fluorenes of concentration
Ketone ethanol solution, the potassium permanganate are the potassium permanganate solution of concentration 0.5~1.5%, and the ascorbic acid is concentration
The aqueous ascorbic acid of 15~25g/l.
15. the detection method of low content germanium in zinc calcine according to claim 7, it is characterised in that: described in step c
Phosphoric acid is that analysis is pure, and the boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is
The cetyl trimethylammonium bromide ethanol solution of concentration 0.5~1.5%, the phenylfluorone are 0.08~0.1% benzene fluorenes of concentration
Ketone ethanol solution, the potassium permanganate are the potassium permanganate solution of concentration 0.5~1.5%, and the ascorbic acid is concentration
The aqueous ascorbic acid of 15~25g/l.
16. the detection method of low content germanium in zinc calcine according to claim 8, it is characterised in that: described in step c
Phosphoric acid is that analysis is pure, and the boric acid is the boric acid aqueous solution of concentration 2.0~2.5%, and the cetyl trimethylammonium bromide is
The cetyl trimethylammonium bromide ethanol solution of concentration 0.5~1.5%, the phenylfluorone are 0.08~0.1% benzene fluorenes of concentration
Ketone ethanol solution, the potassium permanganate are the potassium permanganate solution of concentration 0.5~1.5%, and the ascorbic acid is concentration
The aqueous ascorbic acid of 15~25g/l.
17. according to claim 1~16 in described in any item zinc calcines low content germanium detection method, it is characterised in that: step
The amount of addition phosphoric acid is 0.2~0.3 times of sampling amount V in rapid c, the amount of addition boric acid is sampling amount V 0.5~0.7 times.
18. the detection method of low content germanium in zinc calcine according to claim 17, it is characterised in that: be added in step c
The amount of cetyl trimethylammonium bromide be 0.2~0.3 times of sampling amount V.
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Address after: Ya'an City, Sichuan province 625400 Shimian County Huilong Xiang Zhu Ma Industrial Park Ring Zinc Germanium Polytron Technologies Inc Patentee after: Sichuan Sihuan Zinc Germanium Technology Co., Ltd Address before: Ya'an City, Sichuan province 625400 Shimian County Huilong Xiang Zhu Ma Industrial Park Ring Zinc Germanium Polytron Technologies Inc Patentee before: SIHUAN ZINC & GERMANIUM TECHNOLOGY CO., LTD. |
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