CN109827955A - A kind of nickel aluminium composite powder nickel content detection method - Google Patents
A kind of nickel aluminium composite powder nickel content detection method Download PDFInfo
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- CN109827955A CN109827955A CN201811571006.9A CN201811571006A CN109827955A CN 109827955 A CN109827955 A CN 109827955A CN 201811571006 A CN201811571006 A CN 201811571006A CN 109827955 A CN109827955 A CN 109827955A
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Abstract
The present invention relates to a kind of nickel aluminium composite powder nickel content detection method, sample is placed in polytetrafluoroethylene beaker, is slowly added to mixed acid, and after vigorous reaction stopping, low-temperature heat is cooled to room temperature, constant volume obtains acid hydrolysis solution to dissolving completely;It is divided to materials two parts of solution and is respectively placed in volumetric flask, oxidant ammonium persulfate solution is added in portion, the chromophoric solution that 10ml contains sodium potassium tartrate tetrahydrate sodium hydroxide and dimethylglyoxime is added, place 3-5min, add the hidden Cu of 5ml EDTA solution, it is diluted with water to scale, shakes up and does chromophoric solution, nickel element and dimethylglyoxime is made to develop the color.Add chromophoric solution to make reference solution again in another solution plus after EDTA solution, absorbance is measured at spectrophotometer 480nm wavelength, reference standard curve calculates nickel content.The present invention is suitble to detect nickel aluminium composite powder product of the nickel content 0.02~10%.The advantages that analytical equipment is simple, and molten sample is easy, easy to operate quick, and testing result accuracy is high, and stability is good.
Description
Technical field
The present invention relates to the detections of chemical element content, in particular to nickel aluminium composite powder nickel content detection method.
Background technique
Nickel aluminium composite powder is a kind of new material, and aluminium powder plating nickel on surface forms fine and close nickel coated layer on aluminium powder surface.
Nickel aluminium composite powder is a kind of new material that can be used for plasma surface spray technique, has wear-resisting, corrosion-resistant, increase workpiece surface
The properties such as intensity are widely used in aviation, space flight, military project, the fields such as machine-building.It can also be used for modified double base propulsion
Agent.The detection of regulation chemical component is decided through consultation by both sides of supply and demand in nickel alclad composite powder national standard, and the present invention is mentioned for nickel aluminium composite powder
A kind of detection method of fast and accurately nickel content is supplied.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of nickel aluminium composite powder nickel content detection methods, meet user and want
It asks.
To achieve the above object, the present invention is implemented with the following technical solutions:
A kind of nickel aluminium composite powder nickel content detection method, specifically includes the following steps:
1) it samples
Sample mass is weighed, 0.0001g is accurate to
2) preparation analysis test solution
Sample is placed in polytetrafluoroethylene beaker, is slowly added to mixed acid, and after vigorous reaction stopping, low-temperature heat is to molten
Solution completely, is cooled to room temperature, and is taken part to move into volumetric flask and is diluted with water, mixes;
3) working curve is drawn
It is separately added into 0,5ml, 10ml nickel standard solution in 3 100ml volumetric flasks, is equivalent to concentration 0,0.5PPm,
1PPm draws working curve to nickel content in solution with the absorbance value measured by sample analysis step operation;
4) analytical procedure
It is divided to take and is respectively placed in 100ml volumetric flask for two parts of sample solution made from step 2), 10ml over cure is added in portion
Acid ammonium solution, 10ml chromophoric solution, place 3-5min, add 5ml EDTA solution, be diluted with water to scale, shake up do colour developing it is molten
Liquid adds chromophoric solution to make reference solution, surveys at spectrophotometer 480nm wavelength again in another solution plus after EDTA solution
Absorbance is measured, analysis result is acquired from standard curve;
5) result calculates
Nickel content %=measures test solution concentration * extension rate * 10-6* 100%.
The mixed acid is formed by 3 parts by weight hydrochloric acid (1+1) and 1 parts by weight nitric acid (1+1) mixed preparing.
The hydrogen-oxygen that the chromophoric solution is the potassium sodium tartrate solution that 25ml concentration is 20% and 70ml concentration is 20%
Add 0.5g dimethylglyoxime after changing sodium solution mixing, is settled to 100ml with water.
The nickel concentration of standard solution 10ug/ml is held by the nickel standard solution that 1.0ml concentration is 1mg/ml in 100ml
In measuring bottle, it is diluted with water to scale, is shaken up.
Compared with prior art, the beneficial effects of the present invention are:
1. the present invention provides a kind of fast and accurately nickel content detection method for nickel aluminium composite powder new material, it is added
Ammonium persulfate improves stability as oxidant.The hidden Cu of EDTA is added.The hidden Fe of sodium potassium tartrate tetrahydrate, Mn, Co, Cr is added.
2. being suitble to nickel aluminium composite powder product of the detection nickel content 0.02~10%.
The advantages that 3. analytical equipment is simple, molten sample is easy, easy to operate quick, and testing result accuracy is high, and stability is good.
Specific embodiment
Below with reference to embodiment, the present invention is further described:
The present invention will be described in detail for following embodiment.These embodiments be only to preferred embodiment of the invention into
Row description, does not limit the scope of the present invention.
A kind of nickel aluminium composite powder nickel content detection method, sample are placed in polytetrafluoroethylene beaker, are slowly added to mixed acid,
After vigorous reaction stopping, low-temperature heat is cooled to room temperature, constant volume obtains acid hydrolysis solution to dissolving completely;It is divided to solution two of materialsing
Part is respectively placed in volumetric flask, oxidant ammonium persulfate solution is added in portion, it is (hidden that addition 10ml contains sodium potassium tartrate tetrahydrate
Fe, Mn, Co, Cr), the chromophoric solution of sodium hydroxide and dimethylglyoxime places 3-5min, adds the 5ml hidden Cu of EDTA solution,
It is diluted with water to scale, shakes up and does chromophoric solution, nickel element and dimethylglyoxime is made to develop the color.In another solution plus EDTA is molten
Add chromophoric solution to make reference solution again after liquid, absorbance, reference standard curve, meter are measured at spectrophotometer 480nm wavelength
Calculate nickel content.Specifically includes the following steps:
1. reagent
A. hydrochloric acid (1+1) (being prepared using ρ 1.19g/ml excellent pure grade)
B. nitric acid (1+1) (being prepared using ρ 1.42g/ml excellent pure grade)
C. mixed acid: 3 parts of hydrochloric acid (3.1) and 1 part of nitric acid 3.2 mix.
D.EDTA solution (5%)
E. ammonium persulfate solution (5%)
F. potassium sodium tartrate solution (20%)
G. sodium hydroxide solution (20%)
H. chromophoric solution: after 25ml potassium sodium tartrate solution (20%) is mixed with 70ml sodium hydroxide solution (20%) plus
0.5g dimethylglyoxime is settled to 100ml with water.
I. nickel standard solution (10ug/ml): point taking 1.0ml nickel standard solution (1mg/ml) in 100ml volumetric flask, uses water
It is diluted to scale, is shaken up.
2. instrument
Spectrophotometer
3. analytical procedure
A. sample weighting amount and test solution amount is pipetted
According to the form below 1 weighs sample mass, is accurate to 0.0001g;
B. number is measured
It is independently measured twice, takes its average value.
C. the preparation of test solution is analyzed
It will be placed in 250ml polytetrafluoroethylene beaker by the weighed sample of table 1, and be slowly added to 25ml mixed acid (3.3), to
After vigorous reaction stops, low-temperature heat is cooled to room temperature to dissolving completely, is moved into dilute with water in the volumetric flask of 1 respective volume of table
It releases to scale, mixes, when necessary, according to working curve range, dilute solution to be measured.
D. the drafting of working curve
It is separately added into 0,5,10ml nickel standard solution in 3 100ml volumetric flasks, is equivalent to (the inspection of concentration 0,0.5,1PPm
Standard curve should be adjusted by sample size to 4 to 5 points when survey requires accuracy higher), by sample analysis step operation, to measure
Absorbance value in solution nickel content draw working curve.
E. analytical procedure
It is divided to materials two parts of solution by table and is respectively placed in 100ml volumetric flask.10ml ammonium persulfate solution is added in portion
As oxidant, 10ml chromophoric solution places 3-5min, adds the 5ml hidden Cu of EDTA solution, be diluted with water to scale, shake up and do
Chromophoric solution.Chromophoric solution is added to make reference solution again in another solution plus after EDTA solution.In spectrophotometer 480nm wave
Strong point measures absorbance, and analysis result is acquired from standard curve.
F. result calculates
Nickel content %=measures test solution concentration * extension rate * 10-6* 100%.
Embodiment
Nickel content > 2.00%~10.00% in nickel aluminium composite powder sample, specific nickel content detection method weigh sample
0.25 gram, by experimental procedure sample dissolution, it is settled to 500ml volumetric flask, 2ml test solution is therefrom drawn and is put into clean 100ml appearance
Measuring bottle sequentially adds drug by experimental procedure, and constant volume detects absorbance, and reference standard curve finds color solution concentration and is
Nickel content %=0.65*100000*100%=6.5% is calculated by formula in 0.65ppm, and obtaining nickel content result is 6.5%.
Claims (4)
1. a kind of nickel aluminium composite powder nickel content detection method, which is characterized in that specifically includes the following steps:
1) it samples
Sample mass is weighed, 0.0001g is accurate to
2) preparation analysis test solution
Sample is placed in polytetrafluoroethylene beaker, is slowly added to mixed acid, and after vigorous reaction stopping, low-temperature heat is to having dissolved
Entirely, it is cooled to room temperature, takes part to move into volumetric flask and be diluted with water, mix;
3) working curve is drawn
It is separately added into 0,5ml, 10ml nickel standard solution in 3 100ml volumetric flasks, is equivalent to concentration 0,0.5PPm, 1PPm, presses
Sample analysis step operation draws working curve to nickel content in solution with the absorbance value measured;
4) analytical procedure
It is divided to take and is respectively placed in 100ml volumetric flask for two parts of sample solution made from step 2), 10ml ammonium persulfate is added in portion
Solution, 10ml chromophoric solution place 3-5min, add 5ml EDTA solution, be diluted with water to scale, shake up and do chromophoric solution, in
Add chromophoric solution to make reference solution again in another solution plus after EDTA solution, measures and inhale at spectrophotometer 480nm wavelength
Luminosity acquires analysis result from standard curve;
5) result calculates
Nickel content %=measures test solution concentration * extension rate * 10-6* 100%.
2. a kind of nickel aluminium composite powder nickel content detection method according to claim 1, which is characterized in that the mixed acid
It is formed by 3 parts by weight hydrochloric acid (1+1) and 1 parts by weight nitric acid (1+1) mixed preparing.
3. a kind of nickel aluminium composite powder nickel content detection method according to claim 1, which is characterized in that the colour developing is molten
Liquid is to add 0.5g after the potassium sodium tartrate solution that 25ml concentration is 20% is mixed with the sodium hydroxide solution that 70ml concentration is 20%
Dimethylglyoxime is settled to 100ml with water.
4. a kind of nickel aluminium composite powder nickel content detection method according to claim 1, which is characterized in that the nickel standard
Solution concentration 10ug/ml, by 1.0ml concentration be 1mg/ml nickel standard solution in 100ml volumetric flask, be diluted with water to quarter
Degree, shakes up.
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Cited By (2)
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CN112557316A (en) * | 2020-11-20 | 2021-03-26 | 上海仪电科学仪器股份有限公司 | Method for measuring content of nickel ions in water |
CN113884450A (en) * | 2021-09-15 | 2022-01-04 | 五邑大学 | Turbidity chromaticity correction method for automatic water quality monitor |
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