CN108613936A - The rapid analysis method of nickel in a kind of cu-ni sulphide ore stone - Google Patents
The rapid analysis method of nickel in a kind of cu-ni sulphide ore stone Download PDFInfo
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Abstract
The invention discloses a kind of rapid analysis methods of nickel in cu-ni sulphide ore stone.This method mainly includes the following steps that：Sample is weighed, the molten sample of acid adding is cooling；Add boiling to boil dissolved salts, moved into volumetric flask after cooling, constant volume, this solution is liquid to be pipetted；Part liquid to be pipetted is pipetted, ammonium hydroxide to ferric hydroxide precipitate is added dropwise and is precipitated, then is neutralized with hydrochloric acid to precipitation and just dissolves.It is diluted with water.Sodium citrate solution, potassium sodium tartrate solution, ammonium persulfate solution, dimethylglyoxime ethanol solution, ammonium hydroxide, sodium oxalate solution are sequentially added, is stood, EDTA solution, constant volume is added, this solution is liquid to be determined；The absorbance for measuring above-mentioned liquid to be determined at 530nm wavelength with 3cm absorption vessels is carried out at the same time blank test with analysis sample.The present invention shelters iron and aluminium by the way that sodium citrate and sodium oxalate is added, and the addition for reducing sodium potassium tartrate tetrahydrate eliminates muddiness, realizes the rapid and accurate determination of nickel in cu-ni sulphide ore stone.
Description
Technical field
The present invention relates to a kind of rapid analysis methods of nickel in cu-ni sulphide ore stone.
Background technology
For the mass percent of copper 1% or so, the mass percent of nickel is less than 2%, contains simultaneously in cu-ni sulphide ore stone
The elements such as a large amount of iron, magnesium, aluminium and a small amount of calcium, zinc, cobalt, chromium, manganese.Currently, nickel-silicon nitride method master in cu-ni sulphide ore stone
There are dimethylglyoxime spectrophotometry, flame atomic absorption spectrometry, inductively coupled plasma emission spectrography etc..Using fire
Flame atomic absorption spectrography (AAS) or inductively coupled plasma emission spectrography measure nickel in cu-ni sulphide ore stone and need to be pre-separated, and walk
It is rapid various, it is cumbersome；If not detaching, there are the interference of serious spectral line and background interferences, and pollute sampling system, lead to mist
Change system jams.Traditional dimethylglyoxime spectrophotometry eliminates interference, potassium tartrate by the way that a series of screening agent is added
Sodium is usually used in sheltering iron and aluminium in ammonia solution, and a large amount of additions of sodium potassium tartrate tetrahydrate cause chromophoric solution muddiness often occur,
The measurement for influencing absorbance causes measurement result inaccurate.
Invention content
The purpose of the present invention is to provide a kind of rapid analysis methods of nickel in cu-ni sulphide ore stone, by the way that citric acid is added
Sodium and sodium oxalate masking iron and aluminium, the addition elimination for reducing sodium potassium tartrate tetrahydrate is muddy, and nickel is fast in realization cu-ni sulphide ore stone
Fast Accurate Determining.
To achieve the above object, the present invention uses following technical scheme：
The rapid analysis method of nickel, includes the following steps in a kind of cu-ni sulphide ore stone：
(1) sample is weighed, hydrochloric acid is added, is dissolved by heating, it is cooling；Nitric acid is added to continue to be heated to sample to decompose completely, it is cold
But；Sulfuric acid is added, heating evaporation to sulfur trioxide white cigarette emits to the greatest extent, cooling；Add boiling to boil dissolved salts, volumetric flask is moved into after cooling
In, constant volume obtains liquid to be pipetted；
(2) part liquid to be pipetted is pipetted, ammonium hydroxide to ferric hydroxide precipitate is added dropwise and is precipitated, then is neutralized with hydrochloric acid to precipitation just
Dissolving；It is diluted with water, it is molten to sequentially add sodium citrate solution, potassium sodium tartrate solution, ammonium persulfate solution, dimethylglyoxime ethyl alcohol
Liquid, ammonium hydroxide, sodium oxalate solution are stood, and EDTA solution is added, and constant volume obtains liquid to be determined；
(3) absorbance for measuring the liquid to be determined at 530nm wavelength with 3cm absorption vessels, with analysis sample simultaneously into
Line blank test.
Wherein, the mass percent concentration of the sodium citrate solution is 30wt%.The matter of the potassium sodium tartrate solution
Amount percent concentration is 40wt%.The mass percent concentration of the sodium oxalate solution is 30wt%.
The advantage of the invention is that：
The present invention shelters iron and aluminium by the way that sodium citrate and sodium oxalate is added, and the addition elimination for reducing sodium potassium tartrate tetrahydrate is muddy
It is turbid, realize the rapid and accurate determination of nickel in cu-ni sulphide ore stone.The method of the present invention has quick, accurate, high repeatability and other advantages.
Specific implementation mode
With reference to embodiment, the present invention will be further described, and embodiments of the present invention are not limited thereto.
The analytic process of nickel includes the following steps in cu-ni sulphide ore stone in following embodiment：
(1) 0.5 ± 0.1g samples are weighed in 250mL beakers, 15mL hydrochloric acid (ρ=1.19g/ is added after being soaked with water
ML), 10min is dissolved by heating, it is cooling, 5mL nitric acid (ρ=1.42g/mL) is added, continues to be heated to sample to decompose completely, it is cooling,
5mL sulfuric acid (ρ=1.84g/mL) is added, heating evaporation to sulfur trioxide white cigarette will emit to the greatest extent, cooling；Boiling boiling is added to make solvable
Salt dissolves, and is moved into 100mL volumetric flasks after cooling, cleans beaker and uses water constant volume, this solution for next step liquid to be pipetted；
(2) part liquid to be pipetted is pipetted in 100mL volumetric flasks, and the ammonia spirit of a concentration of 50% (V/V) is added dropwise to hydrogen
Iron oxide Precipitation, then be neutralized to precipitation with the hydrochloric acid solution of a concentration of 50% (V/V) and just dissolve, it is diluted with water to 30~
40mL；Sequentially add in order 3~5mL mass percent concentrations be respectively 30% sodium citrate solution (masking iron and chromium), 5
The potassium sodium tartrate solution (masking iron and aluminium) of~8mL 40%, 5% ammonium persulfate solution (masking cobalt), 1% diacetyl
Oxime ethanol solution, 10mL ammonium hydroxide, the sodium oxalate solution (masking iron, aluminium, manganese) that 5~10mL mass percent concentrations are 30%, it is quiet
15min is set, the EDTA solution (masking magnesium, calcium, copper) that mass percent concentration is 5% is added, with water constant volume, this solution is next
The liquid to be determined of step；
(3) absorbance for measuring above-mentioned liquid to be determined at 530nm wavelength with 3cm absorption vessels, with analysis sample simultaneously into
Line blank test.
The drafting of working curve：The nickel standard solution of nickeliferous 0,10,20,40,60,80,100 μ g is pipetted respectively in 100mL
In volumetric flask, it is diluted with water to 30~40mL, presses step (2) below, (3) operate.
Embodiment 1
0.4996g samples are weighed in 250mL beakers, 15mL hydrochloric acid (p=1.19g/mL), heating are added after being soaked with water
10min is dissolved, it is cooling, 5mL nitric acid (ρ=1.42g/mL) is added, continues to be heated to sample to decompose completely, it is cooling, add 5mL
Sulfuric acid (ρ=1.84g/mL), heating evaporation to sulfur trioxide white cigarette will emit to the greatest extent, cooling.Add boiling boiling that soluble salt is made to dissolve, it is cold
But afterwards move into 100mL volumetric flasks in, clean beaker and use water constant volume, this solution for next step liquid to be pipetted.
10.00mL liquid to be pipetted is pipetted in 100mL volumetric flasks, the ammonia spirit of a concentration of 50% (V/V) is added dropwise to hydrogen
Iron oxide Precipitation, then be neutralized to precipitation with the hydrochloric acid solution of a concentration of 50% (V/V) and just dissolve.It is diluted with water to
40mL.It is respectively 30% sodium citrate solution 5mL, 40% sodium potassium tartrate tetrahydrate to sequentially add mass percent concentration in order
Solution 5mL, 5% ammonium persulfate solution 10mL, 1% dimethylglyoxime ethanol solution 10mL, 10mL ammonium hydroxide, mass percent are dense
Degree is 30% sodium oxalate solution 5mL, stands 15min, and the EDTA solution 5mL that mass percent concentration is 5% are added, fixed with water
Hold, this solution is the liquid to be determined of next step.
The absorbance for measuring above-mentioned liquid to be determined at 530nm wavelength with 3cm absorption vessels is carried out at the same time sky with analysis sample
White experiment.The mass percent for calculating nickel in cu-ni sulphide ore stone is 1.73%.
Embodiment 2
0.5001g samples are weighed in 250mL beakers, 15mL hydrochloric acid (ρ=1.19g/mL), heating are added after being soaked with water
10min is dissolved, it is cooling, 5mL nitric acid (ρ=1.42g/mL) is added, continues to be heated to sample to decompose completely, it is cooling, add 5mL
Sulfuric acid (ρ=1.84g/mL), heating evaporation to sulfur trioxide white cigarette will emit to the greatest extent, cooling.Add boiling boiling that soluble salt is made to dissolve, it is cold
But afterwards move into 100mL volumetric flasks in, clean beaker and use water constant volume, this solution for next step liquid to be pipetted.
20.00mL liquid to be pipetted is pipetted in 100mL volumetric flasks, the ammonia spirit of a concentration of 50% (V/V) is added dropwise to hydrogen
Iron oxide Precipitation, then be neutralized to precipitation with the hydrochloric acid solution of a concentration of 50% (V/V) and just dissolve.It is diluted with water to
40mL.It is respectively 30% sodium citrate solution 5mL, 40% sodium potassium tartrate tetrahydrate to sequentially add mass percent concentration in order
Solution 5mL, 5% ammonium persulfate solution 10mL, 1% dimethylglyoxime ethanol solution 10mL, 10mL ammonium hydroxide, mass percent are dense
Degree is 30% sodium oxalate solution 10mL, stands 15min, and the EDTA solution 5mL that mass percent concentration is 5% are added, use water
Constant volume, this solution are the liquid to be determined of next step.
The absorbance for measuring above-mentioned liquid to be determined at 530nm wavelength with 3cm absorption vessels is carried out at the same time sky with analysis sample
White experiment.The mass percent for calculating nickel in cu-ni sulphide ore stone is 0.75%.
Embodiment 3
0.4995g samples are weighed in 250mL beakers, 15mL hydrochloric acid (ρ=1.19g/mL), heating are added after being soaked with water
10min is dissolved, it is cooling, 5mL nitric acid (ρ=1.42g/mL) is added, continues to be heated to sample to decompose completely, it is cooling, add 5mL
Sulfuric acid (ρ=1.84g/mL), heating evaporation to sulfur trioxide white cigarette will emit to the greatest extent, cooling.Add boiling boiling that soluble salt is made to dissolve, it is cold
But afterwards move into 100mL volumetric flasks in, clean beaker and use water constant volume, this solution for next step liquid to be pipetted.
20.00mL liquid to be pipetted is pipetted in 100mL volumetric flasks, the ammonia spirit of a concentration of 50% (V/V) is added dropwise to hydrogen
Iron oxide Precipitation, then be neutralized to precipitation with the hydrochloric acid solution of a concentration of 50% (V/V) and just dissolve.It is diluted with water to
40mL.It is respectively 30% sodium citrate solution 5mL, 40% sodium potassium tartrate tetrahydrate to sequentially add mass percent concentration in order
Solution 5mL, 5% ammonium persulfate solution 10mL, 1% dimethylglyoxime ethanol solution 10mL, 10mL ammonium hydroxide, mass percent are dense
Degree is 30% sodium oxalate solution 10mL, stands 15min, and the EDTA solution 5mL that mass percent concentration is 5% are added, use water
Constant volume, this solution are the liquid to be determined of next step.
The absorbance for measuring above-mentioned liquid to be determined at 530nm wavelength with 3cm absorption vessels is carried out at the same time sky with analysis sample
White experiment.The mass percent for calculating nickel in cu-ni sulphide ore stone is 0.67%.
Accuracy is tested
Accuracy is carried out to the content of nickel in cu-ni sulphide ore stone (1#, 2#, 3#) using method described in embodiment 1 respectively
Experiment, i.e. recovery testu, the results are shown in Table 1, and the rate of recovery of nickel between 97.65-102.30% (generally want by the rate of recovery
Ask in 95-105%), illustrate that the measurement result of the method for the present invention is accurate and reliable.
1 accuracy experimental result of table
Precision Experiment
Essence is carried out to the content of nickel in cu-ni sulphide ore stone (4#, 5#, 6#, 7#) using method described in embodiment 1 respectively
The data measured are made Mathematical Statistics Analysis, the results are shown in Table 2, relatively by density experiment, experiment parallel determination 6 times (n=6)
Standard deviation (relative standard deviation generally requires to be less than 5%) within the scope of 1.5-4.0%, illustrates the measurement knot of the method for the present invention
Fruit precision is good.
2 Precision Experiment result of table
Claims (4)
1. the rapid analysis method of nickel in a kind of cu-ni sulphide ore stone, which is characterized in that this approach includes the following steps：
(1) sample is weighed, hydrochloric acid is added, is dissolved by heating, it is cooling；Nitric acid is added to continue to be heated to sample to decompose completely, it is cooling；Add
Enter sulfuric acid, heating evaporation to sulfur trioxide white cigarette emits to the greatest extent, cooling；Add boiling to boil dissolved salts, is moved into volumetric flask after cooling, it is fixed
Hold, obtains liquid to be pipetted；
(2) part liquid to be pipetted is pipetted, ammonium hydroxide to ferric hydroxide precipitate is added dropwise and is precipitated, then is neutralized with hydrochloric acid just molten to precipitating
Solution；It is diluted with water, it is molten to sequentially add sodium citrate solution, potassium sodium tartrate solution, ammonium persulfate solution, dimethylglyoxime ethyl alcohol
Liquid, ammonium hydroxide, sodium oxalate solution are stood, and EDTA solution is added, and constant volume obtains liquid to be determined；
(3) absorbance for measuring the liquid to be determined at 530nm wavelength with 3cm absorption vessels is carried out at the same time sky with analysis sample
White experiment.
2. the rapid analysis method of nickel in cu-ni sulphide ore stone as described in claim 1, which is characterized in that the sodium citrate
The mass percent concentration of solution is 30wt%.
3. the rapid analysis method of nickel in cu-ni sulphide ore stone as described in claim 1, which is characterized in that the potassium tartrate
The mass percent concentration of sodium solution is 40wt%.
4. the rapid analysis method of nickel in cu-ni sulphide ore stone as described in claim 1, which is characterized in that the sodium oxalate is molten
The mass percent concentration of liquid is 30wt%.
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Cited By (2)
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| CN109827955A (en) * | 2018-12-21 | 2019-05-31 | 鞍钢实业微细铝粉有限公司 | A kind of nickel aluminium composite powder nickel content detection method |
| CN113049736A (en) * | 2021-03-11 | 2021-06-29 | 青海西钢特殊钢科技开发有限公司 | Method for determining nickel in nickel-chromium pig iron smelted in blast furnace |
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| CN109827955A (en) * | 2018-12-21 | 2019-05-31 | 鞍钢实业微细铝粉有限公司 | A kind of nickel aluminium composite powder nickel content detection method |
| CN113049736A (en) * | 2021-03-11 | 2021-06-29 | 青海西钢特殊钢科技开发有限公司 | Method for determining nickel in nickel-chromium pig iron smelted in blast furnace |
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