Chemistry 353, Laboratory 2a

Gravimetric Determination of Nickel in Nickel Oxides

Objective: To determine the amount of Nickel in an unknown sample of Nickel oxide. Grading: 15 points for the pre-lab, complete lab notebook, and problems. 10 points for the analysis of a known solution of Nickel. 75 points for a correct determination of Nickel in an unknown sample. Synopsis: You will be provided with a solution of Nickel of known concentration and a sample of Nickel oxide with an unknown weight fraction of Nickel (range, 1-3.2 wt % Ni). In the case of the oxide, you will dissolve the solid using strong acids before analysis. The amount of Nickel in solution will be determined through a precipitation with diglyme (dimethyglyoxime) using gravimetric analysis techniques. It is expected that you will be able to determine quantitatively the amount of Nickel to an accuracy of 1% or better. The precipitation reaction of the nickel with the DMG is:

Associated Reading: Chapter 27 in Harris. Procedure: Dry solid until weights agree to .0005 grams. Dont handle crucible or initial weigh beaker with hands! If using the microwave for drying, include a "dummy load" of 200 ml ice water to protect the magnetron. Use heavy green nitrile gloves for protection from acid fumes. Do all heating in a hood and dont put your head inside hood.
Last modified 15 January 2003

Step 1. (only for solid unknown) Dissolving the Nickel Oxide. Clean and dry suitable beaker(s) and Gooch crucibles carefully (put in oven). Dry your unknown for at least an hour also. Pre-weigh (3 replicates) when cool. ( a good time to work on the problems) Route A: Place approximately Route B: Place at least three grams one gram of your unknown in of your unknown in a beaker OR each beaker (as many trials as you plan) Traditional: Heat the solid in the Alternative: Radiate the solid in the oven for 10-20 minutes; cool, microwave for 3 minutes at 500 W; OR then weigh. cool, then weigh. Reheat the solid and cool until weights differ by less than .0005 grams. Add about 30 ml 1 M HCl to the beaker for each gram of unknown. Heat on hot plate to a simmer and stir with glass rod until solid is dissolved (30 minutes or so). If necessary, add more HCl or perhaps some HNO3. Route A: Dilute to approx. 250 Route B: Transfer solution to a ml with hot dI water suitable (probably 100 ml) OR volumetric flask. Rinse beaker with hot dI water and add to flask. Dilute up to mark with dI water. Step 2. Creating optimal solution conditions for diglyme precipitation. Quantitatively pipet an appropriate volume of a Ni solution into a beaker (5 ml of the stock Ni solution, probably 25 ml of your unknown solution). Dilute using hot dI water up to approximately 250 ml. Based on your approximate calculation, add a 50% excess of DMG (1% in ethanol). Add slowly, while stirring, sufficient 7 M ammonium hydroxide until slightly basic (use pH paper). Allow solution to coagulate at least 30 minutes. Either cover the solution and leave for 1-2 days for precipitation or move on to filtration. Step 3. Recovering and weighing solid precipitate. Reheat, recool and reweigh Gooch crucibles until weight agrees to .0005 gm. Filter solution through crucible, rinsing with 0.7 M ammonium hydroxide and hot dI water. Dispose of solution appropriately (not in the sink!). Dry the Gooch crucibles plus product in the oven or microwave, cool and weigh. Repeat final drying/cooling until weights agree to .0005 grams. General Notes: Start on Tuesday with the known solution and one measurement of your unknown. As your time permits (and you become more skilled with the technique) you should try to complete at least two replicate measurements of your unknown. Plan what glassware you will need and when you need to have it washed up; make use of the drying cycles to wash glassware and do calculations. Consider how you will carry your crucibles around (on a watch glass?) during the drying stage; tongs will not be sufficiently secure.

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Data Analysis: 1) Liquid KNOWN: You will have quantitatively measured out a known volume of the solution and diluted appropriately. You will calculate the expected weight of Ni(DMG)2 by first calculating the moles Nickel delivered:

Moles _ Nickel =

VolumeNickelSolution ( ml ) 1000 ml / L

MolarityofNickelKnown

Then you will convert this to the weight of Ni(DMG)2 through:

moleNi ( DMG ) 2 288.91gramsNi ( DMG ) 2 moleNickel moleNi( DMG ) 2 You will report in your final table the volume of solution analyzed, its reported concentration, weight Nickel expected, weight Nickel found and the random and systematic error of this measurement. Weight _ Ni ( DMG ) 2 = Moles _ Nickel

2) Solid UNKNOWN: The key measurements you will collect in this lab are the weight of the initial solid unknown (UNK_WT), the volume of your unknown solution, the volume of unknown solution used in each replicate, and the weight(s) of the diglyme precipitate (PPT_WT). To find the weight Nickel in your unknown sample first calculate the moles Nickel in the precipitate:
Moles _ Ni PPT = PPT _ Wt moleNi ( DMG ) 2 moleNickel 288.91gramsNi ( DMG ) 2 moleNi ( DMG ) 2

Then convert this to the weight of Nickel in the unknown sample: Route A:
Weight _ Ni = Moles _ NiPPT Route B: Weight _ Ni = Moles _ Ni PPT TotalVolSolution 58.69 gramsNi VolSolutionUsed moleNi 58.69 gramsNi moleNi

To get the weight fraction, divide this number by the weight of the unknown (UNK_WT). You should report in table form the mass of unknown analyzed, the weight of Nickel found, the wt % Nickel in the unknown, and the error of your wt % number. The type of error you can report definitely includes error propagation, may include random error if you took more than one replicate, and should include a comparison to the expected value.

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Problems:

1) You are analyzing a steel material that contains some Nickel. If you find that 1.1634 grams of steel gave 0.1795 grams of Ni(DMG)2 what is the weight percent Nickel in the steel? (FW Ni(DMG)2 = 288.91; FW Ni = 58.69).

2) For the problem above, assuming you used class A balances, what is the uncertainty in your determination of the weight percent Nickel?

3) Given 5.00 ml of a solution 0.100 molar in Ni2+, what volume of a 1% (w/v) solution of DMG in ethanol should you add to have a 50% excess of DMG?

4) Given a 1.000 g sample containing approximately 3% Ni by weight, what volume of a 1% (w/v) solution of DMG in ethanol should you add to have a 50% excess of DMG?

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