EXPERIMENT No OBJECTIVE: Determination of % Ni in steel PRINCIPLE: The most common grade of steel is type 304 which has about

8% Ni. It can be used at temperatures of about 290C. By adding more nickel along with 2% molybdenum and 18% chromium, a new alloy called type 316 is produced which has about 12 13 % nickel and is aggressively corrosion resistance in industrial environments. To estimate nickel, the steel sample should be free of Mo, Cr, and Fe. The solution free from all elements other than nickel, is then titrated with EDTA solution. An initial treatment of the solution of Ni2+ ions with Murexide indicator, gives a yellow colored unstable Ni-Murexide complex at basic pH of 10-11. Titration of this unstable complex with EDTA, results in the formation of the more stable Ni-EDTA complex. The consequent release of the free Murexide indicator, changes the color of the solution to persistent purple, at the end point of the titration. REQUIRED REAGENTS: Standard ZnCl2 solution, EDTA, NH4Cl-NH3 buffer solution, Eriochrome black T (EBT) indicator, Murexide indicator, steel solution. PROCEDURE: PART.1: STANDARDISATION OF EDTA SOLUTION: 1. Pipette out 10 mL of standard ZnCl2 solution in an Erlenmeyer flask. 2. Add 2 mL of NH4Cl-NH3, buffer followed by the addition of 3-4 drops of EBT indicator. 3. Titrate it with EDTA solution until the color changes from wine red (or purple) to a persistent blue or bluish green color. 4. Note the burette reading in Table I and perform two more trials. Use the constant burette reading for calculating the exact molarity of the given EDTA solution. PART II : ESTIMATION OF NICKEL IN STEEL 1. Pipette out 10 mL of steel sample solution in an Erlenmeyer flask. 2. Add 2 mL of NH4Cl-NH3 buffer followed by the addition of 2 drops of Murexide indicator.

3. Titrate the yellow solution against EDTA solution until the color changes from yellow to a persistent purple color. 4. Note the burette reading in Table II and perform two more trials. Use the constant burette reading for calculations. OBSERVATIONS: TABLE I (STANDARDIZATION OF EDTA) (B.R. = burette reading)

Obs.No. 1 2 3

Initial B.R. (in mL) 0 0 0

Final B.R. (in mL)

Difference (in mL)

Constant burette reading = V1 mL Molarity of EDTA solution: M1V1 ( EDTA ) = M2V2 (ZnCl2)

(Molarity of EDTA)

TABLE II (ESTIMATION OF NICKEL IN STEEL) (B.R. = burette reading)

Obs.No. 1 2 3

Initial B.R. (in mL) 0 0 0

Final B.R. (in mL)

Difference (in mL)

Constant burette reading = X mL

CALCULATIONS: 1000mL 1M EDTA = 58.71 g Ni

X mL of M1 M EDTA

Given steel sample = 20 g steel present in 1000 ml of the given solution

Result: The given sample of steel has ________________ % of Nickel.