Standard working procedure for estimation of Nickel / Standard Working procedure for Nikel estimation by using AAS Methods.
Principle:
The Nickel content in the sample is determined by aspirating the sample into the flame of an Atomic Absorption Spectrophotometer after pre-concentration. Measured the Absorbance at 232 nm using a Nickel Hollow Cathode Lamp.
Limit of Detection: The limit of detection is 0.01 mg/L.
Reagents used for estimation of Nickel:
- Concentrated HCL
- Concentrated Nitric Acid
- Dilute Nitric Acid (1:499)
- Nickel Stock Solution: Merck 1000 mg/L NIST (National Institute of Standards and Technology) Certified Reference Material or 1.0 gm of pure metal dissolved in concentrated HNO3, heated for complete dissolution. After cooling, transfer quantitatively to a 1000 ml volumetric flask, dilute to the mark with water, and mix. (1 ml of standard solution contains 1 mg of Ni)
Procedure for estimation of Nickel:
Preparation of Standard Solution:
Prepare a reagent blank and a series of 100 ml standards containing 0.1, 0.2, 0.3, 0.4, and 0.5 mg/L of Nickel by diluting a suitable volume of the standard solution with dilute nitric acid.
Sample Preparation:
- Take a 1000 ml well-mixed sample, transfer it to the evaporation dish, and add 3 ml nitric acid.
- Heat and evaporate to 20 ml (avoid boiling).
- Cool, add 3 ml nitric acid, and heat until digestion is complete.
- Add 2 ml HCl (1:1 v/v) and heat gently to dissolve the residue.
- Wash the evaporation dish 3 to 4 times with water, filter, and discard the filter.
- Dilute the filtrate to make up a 100 ml volume with water. (Sample is concentrated 10 times)
Analysis:
- Operate the instrument by following the Standard procedure.
- Aspirate dilute nitric acid (1:499) as a blank.
- Aspirate a series of standards and then the sample solution.
- Read the concentration of Nickel directly in mg/L.
- Apply the dilution factor of 0.1 due to the sample being concentrated 10 times.
Reference: IS 12122 (1987) ✔Latest
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