Las Positas College, Chemistry 1A Lab Manual Fall 2017 Page 61

Experiment 8

Determination of Copper in a Coin

Prelab: Complete the Prelab questions at the end before lab.

PURPOSE

The purpose of this experiment is to determine the mass percent copper in a nickel coin.

Method

A nickel coin is an alloy of two metals, copper and nickel. The alloy dissolves readily in
nitric acid, yielding a solution of Cu2+ ions and Ni2+ ions. Excess nitric acid, a volatile
acid, is removed by adding the less volatile sulfuric acid, and heating.

The acidity of the solution is reduced somewhat by adding a controlled amount of

ammonia water. Under these conditions, the Cu2+ ion can be reduced to Cu1+ by the
hydrogen sulfite ion, HSO3-, and then precipitated as CuSCN by the thiocyanate ion,
SCN-. The precipitate, copper(I) thiocyanate, is collected on a filter paper, washed, dried
and weighed. From the two weights-- that of the original alloy sample and of the final
precipitated compound-- the mass percent copper in the original alloy can be calculated.

PROCEDURE

Safety First
As is usual, goggles must be worn throughout this experiment. Hot solutions of nitric
and sulfuric acids are involved. Wash with water at once after any accidental contact of
skin with acid. At the beginning of the experiment, evolution of noxious gases (oxides of
nitrogen) will require use of the fume hoods.
Some more safety notes: NH4SCN: toxic by ingestion; CuSCN: moderately toxic;
DMG: no particular hazards; Ni(NO3)2: strong oxidizing agent, tolerance (as dust) = 1
mg/m3, dangerous fire risk for solid; NaHSO3: contact with solid causes burns to
skin/eyes, strong irritant to skin and tissue, tolerance (as dust) = 5 mg/m3; SO3:
poisonous if inhaled, highly toxic, strong irritant to tissue, oxidizing agent, fire risk with
organics, forms H2SO4 with water producing heat

This procedure assumes a sample size of about 1.25 g, or one-fourth of a nickel. A whole
nickel can be used if the amounts or reagents are scaled up (four times), but the problem
with using the larger size sample is that longer times are required for filtering, washing
and drying the precipitate at the end.

The nickel will have been cut for you. You will be provided with one piece along with
the year and mint of issue. You will do only one run.
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Work independently or in pairs if directed by your instructor. You will pre-dissolve the
coin in nitric acid by letting it sit for a few days (Steps 1 and 2) before completing the
rest of the lab work. Steps 3 through 15 must be completed on the first full day of lab
work. Read labels carefully; be certain to use the specified concentration. Several
reagents are used with different concentrations at different times during this experiment.

Part I Separation of copper and precipitation as copper(I) thiocyanate.

As instructed by your instructor, Steps 1 and 2 will be done the lab day before the
scheduled 2 full lab days for the lab.
1. Rub the piece of coin with a paper towel and avoid touching it with your fingers
thereafter. Weigh it to ±0.001 g in a pre-weighed plastic weighing dish.

2. Transfer the sample to a 250 mL Erlenmeyer flask. Under your fume hood, add 15
mL of 6 M HNO3. Allow about 10 minutes then note the color changes and fumes
emitted. Do not breathe the fumes. Once the fumes have dissipated, cover the
Erlenmeyer flask loosely with a parafilm and place in the designated tray for storage
in the stockroom until the next lab day.

Begin here on the first full day of Exp 8 lab work.

3. a) Retrieve your Erlenmeyer flask from the tray. If your coin is completely dissolved,
proceed to Step 3b below. If your coin is not completely dissolved, under your fume
hood, heat the flask gently (hot plate, no flame) to get (react) all the coin into
solution. Do not breathe the fumes. CAUTION! DO NOT LET THE FLASK
DRY OUT OR THE SOLID WILL BEGIN TO "BUMP!" Have some extra 6 M
HNO3(aq) readily available in order to add more 6 M HNO3 as needed to always keep
some liquid in the flask. If someone else cannot use your extra nitric acid, dispose of
any excess nitric acid in the appropriate waste container.

b) When the coin is completely dissolved, under the fume hood, SLOWLY add 10
mL of 3 M H2SO4 (aq) to the flask. (Note: If you had to heat the flask as in Step 3a,
you need to be extra careful in adding the sulfuric acid to the already hot solution to
prevent any splatter.). Heat the solution to boiling. CAUTION! DO NOT LET
THE FLASK DRY OUT OR THE SOLID WILL BEGIN TO "BUMP!" Have
some extra 3 M H2SO4 (aq) readily available in order to add more 3 M H2SO4 (aq) as
needed to always keep some liquid in the flask. If a solid forms, add 2 mL more of
the 3 M H2SO4. White fumes should appear, at least faintly, above the mouth of the
flask when moist breath is blown across it. This would be gaseous SO3 (from
decomposition of H2SO4) reacting with water vapor to re-form a fog of H2SO4. This
usually takes 10 to 20 minutes also.

4. Allow the flask to cool (Never put a very hot flask in cold water, but you may speed
the cooling by setting the flask in cool water).

5. Add about 25 mL of deionized water.

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6. Measure out into your graduated cylinder 15 mL of 6 M NH3. Start adding the
ammonia in small increments to the solution in the flask. You will soon see a milky
blue precipitate, Cu(OH)2, form where the ammonia hits the acidic solution, and then
go away as you swirl the flask. The object is to continue adding ammonia only until
that light blue precipitate just persists after swirling. (It may be necessary to use more
than 15 mL of the ammonia, possibly as much as 25 to 30 mL more, depending on the
amounts of nitric and sulfuric acids used earlier, to get the light blue precipitate. If a
dark blue solution containing NO precipitate forms, you have added too much NH3.
See the instructor.) This step takes a lot of ammonia. After you have slowly added
the 15 mL of ammonia, add more using small increments. It is critical not to
overshoot. Be patient! Discard the unused ammonia solution in the appropriate waste
container.

7. Add 15 mL of 1.0 M H2SO4. This solution will be prepared especially for this
experiment, and is not the reagent shelf sulfuric acid used earlier. The precipitate
should dissolve leaving a clear blue or blue-green solution. The solution is now at the
proper acidity, ready for the reducing agent.

8. Add 15 mL of 5% NaHSO3 (sodium hydrogen sulfite, or sodium bisulfite solution).

Note, very cautiously, the characteristic choking odor of SO2 that emanates. Very
little additional change will be observed at this point.

9. Promptly add 15 mL of 10% NH4SCN, ammonium thiocyanate solution, the

precipitating agent. Swirl the flask as the precipitate forms. Continue to swirl the
flask from time to time as the precipitate coagulates; that is, changes from a very fine
grain to a larger grain size. The larger grain size will be more filterable. Warming
will help this process, but do not boil the mixture. If you do not coagulate the
precipitate, there is a good chance that much will pass through the filter paper and be
lost. Contact instructor in this case before disposing of the filtrate.

10. While the precipitate is coagulating, prepare the funnel and filter paper for filtration.
Obtain a piece of 15 cm filter paper (Whatman #40 or equivalent). Fold the paper as
directed by your instructor. Briefly, the directions are to fold the paper in half, then
fold again but stop short of a 90o fold. Weigh the folded portion (after the corner is
torn off). Do not wet the paper while folding; it must be weighed dry.

11. Open up the larger quadrant of the weighed filter paper and fit it snugly into the
funnel. With your wash bottle, moisten the filter paper and press its top edge against
the glass to make a tight seal.

12. Start filtering the reaction mixture. Make a quantitative (without loss) transfer of
precipitate to the filter cone, using squirts of water from the wash bottle to assist you.
The filtrate should be collected in a beaker or flask and saved for proper disposal
later.
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13. After all the precipitate has been collected on the filter paper, it must be washed until
free of Ni2+ ions. A suitable test for traces of nickel ion in the wash water is provided
by the reaction of Ni2+ with DMG in the presence of ammonia. DMG is
dimethylglyoxime, an organic compound that forms a bright red precipitate with the
nickel ion. Of course, what we want here is the absence of a red color, proving the
absence of nickel ion in the wash water.

a. Squirt about 1 mL of deionized water onto the solid and let it drain through. Repeat
this twice more.

b. Collect the last mL of wash water directly from the funnel stem in a test tube. Be
very careful to avoid ANY contamination from previous washings as you collect
this mL sample of wash.

c. Then add about 1 mL of 6 M NH3 and about 1 mL of 1% DMG solution to the test
tube containing the last mL of wash.

d. Repeat the washing process until the test sample does not show the presence of Ni2+
ion. Collect a fresh sample of the latest washing, that is NOT contaminated with
any of the earlier wash solutions, for each repeated test to determine whether the
precipitate is now free of Ni2+ ion.

14. When washed free of Ni2+ ions, the precipitate is allowed to drain in the funnel. With
a spatula, open up a channel between the paper and the glass to allow the stem to
drain. Later, carefully lift the paper plus precipitate and rest it on a watch glass. Still
later, as it dries, open up the filter paper with your spatula, being careful not to lose
precipitate. In the meantime, dispose of the filtrate in the large jar labeled for this
purpose.

15. Place the watch glass in a safe place in your drawer to dry for two days or more. If
time remains in this lab period, you may start drying your sample in an oven set at
95oC for one hour and you may start the test tube experiments described later in the
section entitled "Some Reactions of Nickel and Copper Ions." Otherwise, do this part
next lab period. It is safe to stop the experiment at this step.

16. On the next lab day, complete the drying of the paper and precipitate by placing the
watch glass either (a) in an oven set at 95oC for one hour, or, (b) under a heat lamp
for one hour. While the sample is drying, perform Part II.

17. Allow the glass to cool, and then weigh just the paper and precipitate. Protect the
balance pan with a piece of paper which has been previously weighed, so that you can
quantitatively determine the weight of only your precipitate and filter paper.

18. If time permits, continue the drying operation for a half hour more, or so. Cool and
reweigh. If the second weighing is within 0.01 g of the first, the sample may be
considered dry. If there is a loss in weight greater than 0.01 g, you would ideally heat
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it again until there was no significant change. Such a routine is known as "drying to
constant weight". Dispose of the precipitate in the disposal jar provided.

19. Calculate the mass percent of copper in the nickel coin, assuming that all of the
copper in your alloy sample has ended up as CuSCN.
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DATA
Enter the sample data report form below in your notebook before coming to lab. During
the experiment, record all data (with proper units and number of significant digits)
directly into your notebook in ink. Show sample calculations for all calculated data
for at least one trial if multiple runs were made.

Part I Description of coin: Date: _______ Mint: _______

Observations on dissolving the nickel coin piece:

Trial #1 Trial #2
Mass of weighing paper ____________ ____________
Mass of weighing paper and nickel ____________ ____________
Mass of sample of nickel ____________ ____________
Mass of dry filter paper ____________ ____________
Mass of protective paper (optional) ____________ ____________
Mass of papers + precipitate (1st) ____________ ____________
Mass of papers + precipitate (2nd) ____________ ____________
Mass of papers + precipitate (3rd) ____________ ____________
(if necessary)
Mass of precipitate ____________ ____________

Calculation of copper content Preserve proper precision, significant digits, in all

calculations!

Mass of copper present ............. ____________ ____________

(Show a clear sample calculation.)

Mass percent copper in coin ........ ____________ ____________

(Show a clear sample calculation.)

Average.................................. ____________

Precision

Deviation from average.............. ____________ ____________

Average deviation ............................ ____________
Relative average deviation, % ............... ____________
(Average deviation/average mass percent)*100%
Accuracy (to be filled in by instructor) ____________% Error
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Part II - Reactions of nickel and copper ions

PURPOSE

In this second part of the experiment we will investigate some reactions of nickel(II) and
copper(II) ions which will allow us to tell them apart.

Method

A solution containing Ni2+ ions and a separate solution containing Cu2+ ions will be
subjected to the following test reactions (which are run independent of one another):
1) add aqueous ammonia solution
2) add aqueous sodium hydroxide solution
3) add ammonia followed by DMG (dimethylglyoxime) solution

PROCEDURE

For this part of the experiment you will need seven clean test tubes in all. You may work
with a partner, provided that each of you participates in all tests and that each of you
records your own observations. NO more than two students should be working together
on these test reactions!

1. Place 1 mL (20 drops) of 0.1 M Ni(NO3)2 in each of three test tubes. Now in three
other clean test tubes place 1 mL (20 drops) of 0.1 M Cu(NO3)2.

2. Ammonia test.

a. To one of the test tubes containing Ni(NO3)2 add 6 M NH3 drop by drop
until 10 drops have been added. Record your observations after the first
drop has been added and after all 10 drops have been added.

b. To one of the test tubes containing Cu(NO3)2 add 6 M NH3 dropwise as

before until 10 drops have been added. Record your observations.

3. Sodium hydroxide test.

a. To another portion of Ni(NO3)2 add 6 M NaOH dropwise until 10 drops have

been added. Record your observations.

b. To a sample of Cu(NO3)2 add 6 M NaOH dropwise as above.

4. Dimethylglyoxime test.

a. Place 1 drop of Ni(NO3)2 solution in the seventh clean test tube.

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b. To the tube with 1 drop of Ni2+ solution add 20 drops of deionized water.
Observe the effect of dilution on the color of the Ni2+ by comparing the color
in this test tube to the color in the one remaining tube containing the 20 drops
of Ni(NO3)2 solution that you prepared above.

c. To both of these solutions in b. immediately above (the test tube with 1 drop
of Ni2+ and 20 drops of water AND the remaining tube with the 20 drops of
Ni2+) add 1 drop of 6 M NH3 followed by 10 drops of DMG solution. Do you
get a positive test for Ni2+ in both?

d. Perform this test on the remaining Cu(NO3)2 solution from above. Record
your observations.

DATA
Report in ink all observations on mixing reactants directly into your notebook. See
sample observations table below.

Solutions Test tube with 1 mL 0.1 M Test tube with 1 mL 0.1 M

Ni(NO3)2 Cu(NO3)2
6 M NH3
(1st drop)
6 M NH3
(10 drops)
6 M NaOH
(10 drops)

Test tube with 1 drop Test tube with 1 Test tube with 1 mL
Ni(NO3)2 + 20 drops mL Ni(NO3)2 0.1 M Cu(NO3)2
H2O (blank)
6 M NH3 +1%
DMG

Answer the post-lab questions on the following page.

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POST-LAB Name_________________
(Problems and discussion to be turned in with the lab report)

Experiment 8 Part II: Reactions of nickel and copper ions

1. How do Ni2+ and Cu2+ differ in their reactions with NH3? with NaOH?

2. Calculate the concentration after 1 drop of 0.1 M Ni2+ solution was diluted with 20 drops
of water. (HINT: M1V1 = M2V2 where M1 and M2 are the molarities before and after
dilution and V1 and V2 are the volumes before and after dilution.)

3. Could you still see the green color of Ni2+ even after dilution with water?

4. Could you still detect the characteristic color of the DMG test for Ni2+ in the diluted
solution?

Equations - Complete and balance these ionic equations:

Ni2+(aq) + NH3(aq) + H2O(l)  Ni(OH)2(s) + NH4+(aq)

Cu2+(aq) + NH3(aq) + H2O(l)  Cu(OH)2(s) + NH4+(aq)

Ni(OH)2(s) + NH3(aq)  Ni(NH3)62+(aq) + OH-(aq)

Cu(OH)2(s) + NH3(aq)  Cu(NH3)62+(aq) + OH-(aq)

Ni2+(aq) + OH-(aq) 

Cu2+(aq) + OH-(aq) 
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PRE-LAB NAME___________________
(To be completed before coming to lab)

Experiment 8 Determination of Copper in a Coin

1. Why does nitric acid dissolve (react with) so many more metals than does either
sulfuric or hydrochloric acid? They are all strong acids. (Hint: Dissolving (reacting) a
metal in an acid is an oxidation-reduction reaction.)

2. What is a volatile acid? (See a dictionary).

Which of the following are volatile? HCl HNO3 H2SO4 H3PO4

(Circle the volatile ones. Hint: look up the boiling points and characteristics of each acid,
possibly in the Merck Index).

3. Balance the following net ionic equations:

a. For dissolving metals into solution by reaction with nitric acid

-
Cu(s) + H+(aq) + NO3 (aq)  Cu2+(aq) + NO2(g) + H2O(l)

-
Ni(s) + H+(aq) + NO3 (aq)  Ni2+(aq) + NO2(g) + H2O(l)

b. For reducing Cu(II) to Cu(I):

- -
Cu2+(aq) + HSO3 (aq) + H2O(l)  Cu+(aq) + HSO4 (aq) + H+(aq)

c. To precipitate Cu(I) as copper(I) thiocyanate:

Cu+(aq) + SCN-(aq) 

4. What is the mass percent copper in copper(I) thiocyanate?

Show clear calculations.
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