Ko University

Fall 2015
CHEM 101 GENERAL CHEMISTRY LABORATORY
EXPERIMENT 3

Synthesis of a Compound Using a Limiting Reagent

OBJECTIVES:

Introduce stoichiometry of a chemical equation.

Use mole ratios to determine the limiting reactant.
Calculate the theoretical yield of a synthesis.
Determine the percent yield of a synthesis.

INTRODUCTION:
The study of quantitative relationships in chemical changes is called stoichiometry. A
chemical equation gives the formulas of the reactants and the products. The mole ratios
(ratios of the stoichiometric coefficients) in the balanced chemical equation provide the
quantitative connection between the amounts of reactants consumed and products
produced. Sometimes only a limited amount of one of the reactants is available the reaction
whereas another is present in great excess. The maximum amount of product that can be
formed is determined by the amount of the reactant that is consumed first. This reactant is
called the limiting reactant.
In this experiment you will try your skill as a synthetic chemist and will use the
reaction stoichiometry to identify the limiting reagent in the reaction. The synthesis, while
relatively straightforward, introduces the formation of a coordination compound (or
complex). A comparison of the actual yield of product with its calculated theoretical yield
permits you to determine the percent yield.
Chemical equations involving the transfer of protons (H+ ions) are commonly
classified as Bronsted-Lowry acid-base reactions. Many reactions that occur without a
proton can be classified as Lewis acid-base reactions. Substances with empty electron
orbitals that can accept a pair of electrons are Lewis acids; those substances that can donate
a pair of electrons in the formation of a covalent bond are called Lewis bases. The reaction
of a Lewis acid and a Lewis base results in the formation of an adduct, which has a bond
called a coordinate covalent bond. The Lewis base supplies both of the electrons required
for the formation of this bond. The term coordination refers the process in which one or
more Lewis bases donate a pair of electrons to a Lewis acid to form adducts or complexes.
The transition metal ions, with their many empty valence orbitals, often act as Lewis acids
toward atoms having non-bonding electron pairs to form coordination complexes. The Lewis

basesthe electron-pair donors in the complexare called ligands. The number of ligand
atoms, or molecules, or units attached to the central ion is defined as the coordination
number of the complex.
Many ligands are bifunctional or polyfunctional in nature; that is, they are able to act
as Lewis bases at more than one site. When one ligand can coordinate through two sites, it
is called bidentate. When the bidentate (literally two teeth) ligand forms a ring structure
with the metal ion, it is termed a chelate ring. The formation of transition metal complexes
and chelates greatly increases the solubility of the metal ions in aqueous solution. The
ligand used in this experiment-1,2-diaminoethane (H2NCH2CH2NH2), commonly called
ethylenediamine- is a bidentate ligand. You will prepare a complex of nickel (II) that contains
three ethylenediamine ligands.
In addition to calculations involving chemical formulas, the most important use of
stoichiometric calculations is in the prediction of the maximum yield of the product that can
be produced from a given amount of reactants according to a specified balanced chemical
equation, the relative number of moles of the species involved in the reaction. The balanced
equation for the synthesis reaction in this experiment is
NiCl2 .6H2O(aq) + 3H2NCH2CH2NH2 (aq)

[Ni(H2NCH2CH2NH2)3]Cl2 (s) + 6H2O (l)

Figure 1. Reaction of Nickel (II) chloride hexahydrate with 1 unit ethylenediamine.

The equation tells us that one mole of nickel (II) chloride hexahydrate reacts with
three moles of ethylenediamine to produce one mole of tris (ethylenediamine) nickel (II)
chloride and six moles of water. Based on this relationship, and knowing the masses of the
starting materials used, we can calculate the maximum masses of product obtainable from
these reactants -the theoretical yield- of the reaction. It is theoretical because very few
reactions go to 100% completion. The ratio of the actual yield to the theoretical yield
multiplied by 100 and reported in percentage is referred to as the percent yield of the
synthesis.
From the masses of NiCl2.6H2O and ethylenediamine used and their molar masses, the
number of moles of the reactant can be calculated. We can determine which one is the
limiting reactant and which reactant is present in excess by comparing these numbers with
those required by the stoichiometry in the above reaction. We can then calculate the
2

maximum of moles and mass of [Ni(en)3]Cl2 that can be produced under our experimental
conditions. This is the theoretical yield. The actual yield can be measured in the laboratory,
and the percent yield can be calculated.

MATERIALS:

Solution
bottles

Spatula

Laboratory
balance

Pasteur pipette

Measuring
pipettes

Funnel

Safety
pipette
bulb

Beaker

Graduated
cylinder

Ring
clamp
holder

Glass Stirring rod

Filter paper

EXPERIMENTAL PROCEDURE
CAUTION: WEAR PERSONAL PROTECTION EQUIPMENT (LAB COAT, GOGGLES, GLOVES)
1. Fold your filter paper that will be used in the last step of procedure according to the
following scheme, write your hood number (with pencil) on it and record its weight.
(Use the same balance for all your measurements).

2. Accurately weigh (to the nearest 0.01 g) a 1.0 g sample of nickel (II) chloride
hexahydrate (NiCl2 .6H2O) into the beaker. Use an empty, dry beaker of 100 mL
capacity. Note the appearance of the compound.
3. Completely dissolve this sample by stirring in a maximum of 2 mL of deionized water.
Note the color of the solution. Record the temperature of the solution using a
thermometer.
4. Slowly add 4.0 mL (use a bulbed glass pipette) of 25% ethylenediamine solution to
the beaker while constantly and gently stirring.
The solution of 25.0%
ethylenediamine is by mass and has a density of 0.950g/mL. Note any changes that
take place. Record any temperature changes.
5. To induce precipitation, add 15 mL of acetone in 5 mL increments (use a 25 mL
graduated cylinder) while stirring well after each addition. The product is ionic and
soluble in water, but is not soluble in the less polar acetone.
6. Continue to stir gently until precipitation begins.
7. Record the temperature change after precipitation begins.
8. After precipitation has begun, allow the beaker to stand undisturbed for about 10
minutes. Note the appearance of the mixture.

9. Cool the beaker in an ice bath to maximize precipitation of the product.

10. Fix the ring support on stand and place your funnel.
11. Place your folded filter paper in the funnel.
12. Place 150 ml beaker under the funnel.
13. Mix the slurry (the mixture of the solid and liquid) gently until it forms a homogenous
suspension and without waiting transfer the slurry to the funnel in one gentle
motion. If any precipitate remains in the beaker, wash it with the filtrate, and
transfer any remaining crystals into the funnel. (Do not use a glass rod for this.)
14. Wait for the solvent to drain.
15. If the filtrate contains product crystals, re-filter the filtrate. If your filtrate still
contains crystals, check your filter paper for any holes.
16. Wash the solid with two additional 2 mL portions of acetone.
17. Transfer the solid (your product) together with the filter paper onto an aluminum foil
and place it into the oven. Make sure your filter paper is labeled.
18. Leave the material to dry for at least 15 minutes in the oven (120 C). Weigh the
product.
19. Dry your product in the oven for 2 additional minutes and weigh again. Continue this
drying process until the difference between two successive dryings is less than 10
mg.
20. Pour and rinse the liquid waste into the organic waste container.
21. Wash all of the equipment and place them upside down on a piece of paper towel in
your set-up box. Clean up your working area.

DATA SHEET
Student Name:
Mass of NiCl2.6H2O (g)
Appearance of solid NiCl2.6H2O
Color of NiCl2 solution in water
Temperature of NiCl2 solution in water
Volume of 25 % ethylenediamine solution (ml)
Appearance of ethylenediamine solution
Appearance of the mixture after adding
ethylenediamine
Temperature of the mixture after adding
ethylenediamine
Amount of acetone added (ml)
Appearance after adding acetone
Temperature change upon precipitation
Color of product (complex)
Weight of filter paper (g)
Weight of filter paper + product after drying for
15 mins (g)
Weight of filter paper + product after drying for
15 mins + 2 mins (g)
Weight of filter paper + product after drying for
15 mins + 2 mins + 2 mins (g)
Weight of filter paper + product after drying for
15 mins + 2 mins + 2 mins+ 2 mins (g)
Weight of product (g)