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BOJ 2009 Page 1


CHAPTER 1 The Periodic Table
1.1 Chemical & Physical Properties of Elements & Compounds
Definitions

Chemical properties of elements and compounds refer to what they do when they
react with other elements and compounds. For example, sodium metal is highly
reactive. That is, it will change very willingly when placed with other chemicals.
Therefore a chemical property can be thought of as properties that change the
matter.

Physical properties are those which describe the nature of the element or compound
without changing its chemical structure. E.g. appearance, colour, smell etc. For
example, water is colourless and odourless. Therefore a physical property can be
thought of as one that describes rather than changes the matter.

An element consists of only ONE type of atom. A compound is made up of two or more
DIFFERENT types of atoms. E.g. O2 is an element and H2O is a compound. Both are molecules!

Classify the following as chemical or physical properties:

(a) Paper burns in


oxygen_____________________________________

(b) Gold is shiny and


soft______________________________________

(c) Potassium nitrate is used in cold packs because when it mixes


with water (dissolves) it absorbs
heat_____________________________

(d) Hydrochloric acid has a low


pH______________________________

1.2 The Modern Periodic Table


The Periodic Table is the organised listing of all elements known to humans including the
ones that dont occur naturally! It is purposely arranged in rows (periods), columns (groups)

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and blocks. The position of an element in the Periodic Table is dependent upon the atomic
number (Z). Remember an elements atomic number is the number of protons (+) it has in
the nucleus (middle) of the atom. In an electrically neutral atom (overall zero charge) the
number of electrons (-) also equals the atomic number. Neutrons, also found in the nucleus,
have zero charge. The number of neutrons in an atom is NOT related to its position in the
Periodic Table.

www.accessscience.com

1.2.1 Periods

A period is a row of elements. Elements are purposely placed in a particular period


according to how many occupied electron shells it has.

An electron shell is a region of space around the nucleus of an atom where electrons can be
found. Two electrons can fit in the first shell, eight in the second and 18 in the third. The rule
that tells you how many electrons can fit into a shell is 2n 2 where n is the shell number.

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How many electrons can fit in the fourth
shell?___________________________

There are only two elements in the first period. These are hydrogen (H) and helium (He).
The next element, lithium (Z=3) is located in the second period. As lithium has three
electrons, it needs two shells to fit them because the first electron shell can only have a
maximum of two electrons.

Lets examine the entire second period. Elements three (Li) through to 10 (Ne) are located in
this period. Neon has 10 electrons and is the last member of Period II. Sodium (Na, Z=11) is
the first member of Period III.

Why are elements three to 10 in Period II but sodium is in Period III?

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1.2.2 Groups

A group is a column of elements that are also put there for a reason. Lets investigate the
first three members of Group I. They are Hydrogen (H), Lithium (Li) and Sodium (Na).

Many element symbols originate from the Latin or Greek meaning. For example, natrium is the
Latin word for sodium. This is why sodium has the symbol Na.

The corresponding atomic numbers for those elements are 1, 3 and 11. In addition to
starting a new period, each has something else in common.

What do H, Li and Na have in common that could be responsible for them being
placed in Group I of the Periodic Table?

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1.2.2.1 Group I (Alkali Metals)

Group I metals are called the Alkali Metals because the form basic solutions when placed in
water. They are extremely reactive and most have to be stored in oil because they will react
with oxygen in the atmosphere. Reactivity increases down the group. That is, sodium is

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more reactive than lithium and potassium (K) is more reactive than sodium. They are
generally soft metals and can be cut very easily.

Fr is only found in rocks and is extremely rare. www.webelements.com

Sodium (pictured left) can be cut


with a kitchen knife. It is a shiny
metal but is white on the outside
due to it reacting slightly with
oxygen.

http://www.vanderkrogt.net/elements/images/sodium.jpg

A basic solution is one that has a HIGH pH. An acidic solution is one that has a LOW pH.
Concentrated acidic and basic solutions are dangerous and can cause major damage to the
eyes and skin. They should never be ingested (eaten)!

1.2.2.2 Group II (Alkaline Earth Metals)

Group II metals will also form a basic solution but they are less reactive and less soluble in
water than Group I. They are also harder than Group I metals.

www.webelements.com

1.2.2.3 Transition Elements

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www.myoops.org

The Transition Elements can be thought of as being part of Group II. However, their
chemical and physical properties are quite different to those of the Alkaline Earth Metals.
They are hard, dense and relatively unreactive compared to the first two groups of metals.
The reason is to do with their different electron configuration. The value of these metals to
society cant be understated. They are used extensively in construction and engineering.
Iron is used in many industries and is used to make useful things like cars and bridges.
Copper is a very good electrical conductor and is used as telephone cabling as well.
Unfortunately, many years of price increases have seen the theft of copper become a major
problem. Even BHS has had copper plumbing stolen!

Transition elements form coloured compounds. In fact, one transition element can give off
many different colours. Again this is to do with their unique electron configuration.

Did you know that many of the precious gemstones people covet contain transition metal ions
that give off spectacular colour? Rubies are red and emeralds are green due to the presence of
chromium. Sapphires are blue due to the presence of titanium and iron.

An ion is an atom that has gained or lost electron(s) to become charged. Atoms that lose
electrons become positively charged and are called Cations (Cat-irons). Atoms that gain
electrons become negatively charged and are called anions (an-irons).

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www.webelements.com

1.2.2.4 Halogens

The word halogen means to form a salt. They are very reactive and will react readily with
metals to form ionic compounds called salts. The most famous of course is sodium chloride
(NaCl).

An ionic compound is formed when metals give their electrons to non-metals. The positive and
negative ions that result attract strongly and join together. This force of attraction is called an
electrostatic force. Static means not moving.

Halogens are unique because they exist as solids, liquids and gases. They vary greatly in their
use. Fluorine is used in refrigeration while the fluoride ion helps form strong teeth. Chlorine
is used as an anti-bacterial agent in water supplies and in chemical warfare. Iodine is used as
an antiseptic and is an important part of peoples diets because it helps metabolic
processes.

www.webelements.com

1.2.2.5 Noble Gases

The noble gases get their name due to their inertness. This means they dont like to react
with other chemicals at all. They all, with the exception of helium, have eight electrons in
their outer shell so they are classified as Group VIII elements.

Helium (He) does not have eight electrons in it outer shell but is classified as a
Group VIII element. Why?

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Noble Gas Uses Property

Argon Light bulbs Doesnt react with the metal


filament

Helium Used with O2 for deep sea Low solubility of helium in the
dives blood.

Helium To inflate the tyres of large Non-flammable


aircraft

Helium To fill airships and weather Low density, does not burn
balloons

Neon In advertising signs because it Conductor of electricity at


glows red when electricity high voltage
passes

Krypton/Xenon In lamps used in photographic Gives out a lot of light when


flash units, in stroboscopic electricity passes through
lamps used in lighthouses
http://www.drbateman.net/gcse2003/gcsesums/chemsums/noblegases/noblegases.htm

All of the noble gases are colourless and odourless by themselves. It takes electricity to
make them glow.

1.3 Predicting Chemical & Physical Properties Using The Periodic Table
We will use period III to examine trends across a period. First of all we need to introduce
some new terms and definitions.

In addition to ionic bonding, metal atoms can bond with one another by still kicking out
electrons to become stable, but the electrons are not given to a non-metal rather they are still
held close to the positive metal nucleus.

Definitions

Melting Point the temperature at which a chemical in a solid state becomes a


liquid.

Boiling Point the temperature at which a chemical in a liquid state becomes a gas.

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Atomic Radius half the distance between two atoms of an element.

Electronegativity the ability of an atom to pull bonded electrons towards itself.

Bond the attractive force that hold two or more elements together

Metallic Character the resemblance of an element to a metal

Trends

Name of Element Sodium Magnesium Aluminium Silicon Phosphorus Sulfur Chlorine Argon
Symbol Na Mg Al Si P S Cl Ar

Atomic Number, z 11 12 13 14 15 16 17 18

Electronic
2,8,1 2,8,2 2,8,3 2,8,4 2,8,5 2,8,6 2,8,7 2,8,8
Configuration

Atomic Radius
186 160 143 118 110 102 99 192
(picometers)

Electronegativity 0.9 1.3 1.6 1.9 2.2 2.6 3.2 -

Melting Point (oC) 98 639 660 1410 44 113 -101 -189

Boiling Point (oC) 883 1090 2467 2680 280 445 -35 -186

semi-metal non- non-


Metallic Character metal metal metal non-metal non-metal
(metalloid) metal metal

http://www.ausetute.com.au/trendpd3.html

1.3.1 Atomic radius

As we move from left to right across a period, the atomic radius of each element decreases.
This is because the number of protons in the nucleus increases. Therefore there is a greater
overall positive charge in the nucleus. This increased positive charge pulls more strongly on
the electrons in the surrounding shells. So the space they occupy shrinks and makes the
element smaller.

Argon has more protons than all of the period III elements yet its atomic radius is
larger than all the elements in period III. Suggest a reason for this. [Hint: look at
the electron configuration of Ar]

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1.3.2 Electronegativity

Electronegativity increases as we move across a period. This is because electrons in a bond


are closer to the more positive nucleus of the more electronegative element. Its like an
atomic tug of war.
BOJ 2009 Page 9
Again Argon does not follow this trend. Why?

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1.3.3 Metallic Character

Metallic character (metal behaviour) decreases across a period. This is because it becomes
increasingly harder to remove electrons from the outer shell.

Why do you think it is harder to remover outer shell (valence) electrons moving
across a period from left to right?

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1.3.4 Melting & Boiling Point

Covalent bonding is the name given to bonds where electrons are shared between atoms. This
bonding can be seen in bonds between non-metal atoms. Because electrons are being shared,
there is no charge on either atom

Metals have strong forces of attraction between the delocalised (kicked out) electrons and
the positive nucleus. This means a lot of energy has to be provided to break this attractive
force. This results in high melting points.

Ionic Compounds also have strong attractive forces but these are between the positive
and negative ions that form as a result of the transfer of electrons. Again it takes a lot of
energy to break these apart so these too have high melting points.

Covalent Molecules although strongly bonded within the molecule, the forces of
attraction between the molecules are small. This means a lot less energy is required to
overcome these attractive forces. This gives rise to relatively low melting and boiling points.

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CHALLENGE! Water (H2O) and oxygen (O2) are both covalent compounds.
Water has a boiling point of 100OC at sea level whereas oxygen has a boiling
point of -183OC. Can you explain why? [Hint: look at the electronegativity of the
elements in each compound and the effects on the forces between molecules.]

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1.3.5 Trends Down A Group (top to bottom)

PROPERTY EXPLANATION

Atomic radius
increases

Metallic
character
increases

Melting and
boiling points

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increase
(usually*)

Electronegativity
decreases

* 3d structure can affect the melting point of solids and elements also have a number of
structures.

CHAPTER 1 REVIEW QUESTIONS


1. What is the difference between a chemical and physical property. Use examples,
other than those in this booklet, to help your explanation.

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2. What are the differences and similarities between elements, compounds and
molecules?

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3. What are protons, neutrons and electrons and where in an atom are they found?

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4. Explain how the modern Periodic Table uses atomic numbers, groups and periods to
organise elements.

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5. What are the similarities and differences between the Group I, II and transition
metals?

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6. Explain why halogens fluorine and chlorine are gases whereas bromine is a liquid and
iodine is a solid.

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7. Why are noble gases unreactive? Explain in terms of their electron configuration.

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8. Complete the following table:

ELEMENT HIGH LARGE LARGE ATOMIC


MELTING/BOILING ELECTRONEGATIVITY RADIUS (YES/NO)
POINT (YES/NO) (YES/NO)

Magnesium (Mg)

Fluorine (F)

Neon (Ne)

9. Sodium and potassium are both Group I metals. Explain why potassium has a higher
melting point than sodium, is less electronegative and is more reactive than sodium.

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10. Explain why, in theory, calcium has a higher melting point than magnesium.

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11. What type of bonding would be observed in the following elements/compounds?

(a) Be________________________________________________________________

(b) BaCl2______________________________________________________________

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(c) OF2_______________________________________________________________

12. Which of the elements/compounds in Question 11 would have the lowest melting
point?

___________________________________________________________________________

CHAPTER 2 Chemical Equations


Definitions

A skeleton equation has all reactants and products listed but they are not balanced.
In other words, there are not equal numbers of each element on both sides of the
equation.

A reactant is a substance that is involved in a chemical change (reaction) with


another reactant(s).

A product is a chemical that forms as a result of two or more reactants undergoing a


chemical change.

A physical state is basically whether a chemical is in the solid state(s), liquid state(l),
gaseous state(g) or aqueous state(aq). Aqueous means dissolved in water. DO NOT
CONFUSE AQUEOUS WITH LIQUID. A liquid is a melted solid. It doesnt necessarily
mean it is water.

2.1 Writing Formulae


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To write skeleton equations you need to be able to write chemical formulae. Last year you would
have used a table of ions to write ionic formulae. A few rules for writing ionic formula must be
followed.

The total charge on the formula must be zero

The positive ion is written first in the formula

Brackets are used when more than one polyatomic ion is in the formula. A polyatomic
ion is one that is made up at least two atoms. E.g. OH-, SO42-, NH4+.

2.1.1 Writing Formulae of Ionic Compounds

Cations (Positively Charged)

Name Formula Name Formula

aluminium Al 3+ iron (II) Fe 2+

ammonium NH4 + iron (III) Fe 3+

barium Ba 2+ lead (II) Pb 2+

cadmium Cd 2+ lead (IV) Pb 4+

calcium Ca 2+ lithium Li +

chromium (II) Cr 2+ magnesium Mg 2+

chromium (III) Cr 3+ nickel (II) Ni 2+

copper (I) Cu + nickel (IV) Ni 4+

copper (II) Cu 2+ potassium K+

gold (I) Au + silver Ag +

BOJ 2009 Page 16


gold (III) Au 3+ sodium Na +

hydrogen H+ tin (II) Sn 2+

zinc Zn 2+

Anions (Negatively Charged)

Name Formula Name Formula

acetate CH3COO - hydroxide OH -

bicarbonate
(hydrogen HCO3 - iodide I-
carbonate)

bisulfate
(hydrogen HSO4 - nitrate NO3 -
sulfate)

bromide Br - hydride H-

carbonate CO3 2- nitride N 3-

chlorate ClO3 - oxalate C2O4 2-

chloride Cl - oxide O 2-

chromate CrO4 2- permanganate MnO4 -

cyanate OCN - phosphate PO4 3-

cyanide CN - sulfate SO4 2-

dichromate Cr2O7 2- sulfide S 2-

dihydrogen
H2PO4 - thiocyanate SCN -
phosphate

fluoride F- thiosulfate S2O3 2-

BOJ 2009 Page 17


What do the cations with more than one possible charge have in common? [Hint:
find them in the Periodic Table.]

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The tables above are just some of the ions that form as a result of electron transfer. You
arent expected to remember all of these, however if you plan on doing VCE Chemistry, it
might be a good idea.

Lets have a go at a nice, easy one to begin with. Well write the formula for sodium iodide.
Locating each in the tables above shows us that sodium has a +1 charge and iodide has a -1
charge. When we put them together the number of positive charges equals the number of
negative charges ( they equal zero overall - +1 1 = 0 ). This means we need one of each.

Na1I1 the 1 is left off the bottom so it is simply as NaI.

Time to try a harder one! Lets write the formula for aluminium chloride. Locating each in
the table of ions above shows us that aluminium is +3 and chloride is -1. When we put them
together, there are two extra positive charges (+3 1 = +2). This means we need an extra
two negative charges. Since chloride has one negative charge, we need another two
chloride ions to balance the positive and negative charges (+3 3 = 0).

Al1Cl3 the 1 is left off the Al but the 3 remains of the Cl so its AlCl 3

What about the formula for potassium dichromate?

Potassium is +1 and dichromate is -2. When we put them together, there is one extra
negative charge (+1 2 = -1). This means we need one extra potassium ion.

K2Cr2O7

Did you know that potassium dichromate was used by police in hand-held breathalysers for
many years; It would turn green if a driver had too much alcohol on their breath.

In our last example we will look at the formula for ammonium sulfate. When the two are
added together there is one extra negative charge. This means we need two ammonium
ions to balance it.

NH42SO4 this is wrong because it reads as 42 H. Therefore we need to use brackets.

(NH4)2SO4 is the correct formula.

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Complete the following table:

NAME CATION ANION FORMULA


Copper(I)bromide

Copper(II)bromide

Calcium hydroxide

Magnesium sulfate

Barium bisulfate

Aluminium
carbonate

2.1.2 Writing formulae of covalent elements & compounds

Non-metals and non-metals joined together in fixed ratios.


No charges on elements in the formula.
Use prefixes to indicate how many atoms of a particular element are present in the
formula.

Table of prefixes

Number of atoms Prefix Number of atoms Prefix


1 Mono 6 Hexa
2 Di 7 Hetpa
3 Tri 8 Octa
4 Tetra 9 Nona
5 Penta 10 deca

Examples

CO2 monocarbon dioxide*

* simplified to carbon dioxide because only one carbon will bond with two oxygen atoms so
you dont have to specify it. This is often the case with many compounds.

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SO3 sulfur trioxide, SO2 sulfur dioxide

H2O dihydrogen monoxide**

**When the prefixes come before an element that starts with a vowel like oxide, the prefix
will drop its a or o as seen above.

E.g. P2O5 diphosphorus pentoxide**

Complete the following table:

NAME FORMULA
Carbon tetrachloride

OF2

N2O5

2.2 Skeleton Equations

Require formulae of reactants and products


Require states

E.g. Write the skeleton equation for the reaction between a solution of silver nitrate and
a solution of sodium chloride to give solid silver chloride and aqueous sodium nitrate.

Silver nitrate Ag+ and NO3- gives AgNO3


Sodium chloride Na+ and Cl- gives NaCl
Silver chloride Ag+ and Cl- gives AgCl
Sodium nitrate Na+ and NO3- gives NaNO3

Therefore AgNO3 + NaCl AgCl + NaNO3

Put in the states a solution means dissolved in water, i.e. (aq)

AgNO3(aq) + NaCl(aq) AgCl(s) + NaNO3(aq)

Eg2 Write the skeleton equation for hydrogen gas reacting with nitrogen gas to give
nitrogen trihydride gas

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Nitrogen trihydride is commonly known as ammonia. It is used to make fertiliser, cleaning
products and is weak base that can neutralise weak acids. It is quite soluble in water.

Remember gases like hydrogen, nitrogen, chlorine and oxygen dont exist as single
atoms. They are diatomic (two atoms) molecules. So hydrogen gas is H2 etc
Hydrogen H2
Nitrogen N2
Nitrogen trihydride NH3

H2(g) + N2(g) NH3(g)

Eg3 Write the skeleton equation for the reaction when solid carbon is burnt in excess
oxygen gas to produce carbon dioxide gas.

Carbon C
Oxygen O2
Carbon dioxide CO2

C(s) + O2(g) CO2(g)

2.3 Balancing Equations

To balance an equation is to make sure there are equal numbers of each element in the
reactants AND products.

The crucial thing to remember when balancing equations is that you cannot change the
chemical formula of the reactants and products.

Therefore, you can only change the amount of each reactant and/or product by placing a
number in front. E.g. 2CO2(g)

This translates to two lots of CO2 that is 2 C atoms and 4 O atoms in total.

E.g. Balance the following skeleton equation:

H2(g) + O2(g) H2O(l)

The number of hydrogen atoms (H) on the left is two and the number on the right is
two also. These are balanced.
The number of oxygen atoms (O) on the left is two but there is only one on the right.
These are NOT balanced.

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Remember you cant change the formula but you can put big numbers in front of the
formula. Lets start by putting a 2 in front of the H2O on the right.

H2(g) + O2(g) 2H2O(l)

This means there are two oxygens on the right so they are balanced. BUT now
there are four hydrogen atoms (2 2 = 4) on the right side.
To correct this, we will place a 2 in front of the H2 on the left to give four H atoms.

2H2(g) + O2(g) 2H2O(l)

Eg2 Balance the following skeleton equation:

Pb(NO3)2(aq) + KI(aq) PbI2(s) + KNO3(aq)

There is one I on the left but two on the right. We will place a 2 in front of the KI
on the left to correct this. This also means we have two K on the left.

Pb(NO3)2(aq) + 2KI(aq) PbI2(s) + KNO3(aq)

There are two NO3 on the left and one on the right. We place a 2 in front of the
KNO3 on the right to correct this. This has also balanced the K on the right.

Pb(NO3)2(aq) + 2KI(aq) PbI2(s) + 2KNO3(aq)

Eg3 Balance the following skeleton equation:

C3H8(g) + O2(g) CO2(g) + H2O(l)

Balance the C by placing a 3 in front of CO2

C3H8(g) + O2(g) 3CO2(g) + H2O(l)

Balance the H by placing a 4 in front of H2O

C3H8(g) + O2(g) 3CO2(g) + 4H2O(l)

Balance the O by placing a 5 in front of the O2

C3H8(g) + 5O2(g) 3CO2(g) + 4H2O(l)

C3H8 is called propane gas. Propane gas is obtained by cracking (splitting up) large molecules
found in oil. Propane is a part of LPG and is a fuel for heating and BBQs.

Complete the following table:

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SKELETON EQUATION BALANCED EQUATION
H2(g) + N2(g) NH3(g)

SO2(g) + O2(g) SO3(g)

Zn(s) + CuSO4(aq) Cu(s) + ZnSO4(aq)

H2(g) + I2(g) HI(g)

C6H12O6(aq) + O2 CO2(g) + H2O(l)

CHAPTER 2 REVIEW QUESTIONS


1. Write the formula for the following ionic compounds:

potassium chloride chromium(III)acetate

lithium hydroxide zinc chlorate

calcium chromate ammonium oxalate

sodium phosphate magnesium


bicarbonate

2. Write the formula for the following covalent elements/ compounds:

sulfur dioxide nitrogen monoxide

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phosphorous Dicarbon
trihydride hexahydride

silicon tetrahydride tricarbon


octahydride

oxygen dichloride dinitrogen tetroxide

3. What is the name of the following elements/compounds?

NH4Cl C4H10
CuNO3 NH2
Ca(SCN)2 CS2
KMnO4 O2

4. Balance the following equations:

(a) _____P4(s) + _____O2(g) _____P2O3(s)

(b) _____Mg(OH)2(s) + _____HCl(aq) _____MgCl2(aq) + _____H2O(l)

(c) _____K3PO4(aq) + _____CaCl2(aq) _____Ca3(PO4)2(s) + _____KCl(aq)

(d) _____Al(s) + _____HCl(aq) _____AlCl3(aq) + _____H2(g)

(e) _____C5H12(l) + _____O2(g) _____CO2(g) + _____H2O(g)

5. Write balanced equations for the following reactions:

(a) magnesium metal is reacted with hydrochloric acid to produce magnesium


chloride and hydrogen gas.

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(b) A solution of barium chloride is reacted with aqueous sodium sulfate.

_____________________________________________________________________
BOJ 2009 Page 24
(c) Liquid hydrogen peroxide (H2O2) decomposes into water and oxygen gas.

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(d) hydrogen and oxygen gas are reacted to together to make water vapour.

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CHAPTER 3 Quantitative Analysis By Mass


Definitions

Analyte chemical element or compound of interest


Filtrate the liquid that goes through the filter paper
Residue the solid mass left in the filter paper (usually discarded)
Quantitative analysis involves standard analytical procedures to calculate the
amount of a known substance (analyte) in a sample.
Qualitative analysis involves standard analytical procedures to find out what
unknown substance(s) are in a sample.

Just about all consumer products have information on the packaging. Particularly important
is the nutritional information on food packaging. It is the job of a food chemist or analytical
scientist to test products to make sure the statement on the package is correct. This is called
Quality Assurance (QA). Companies are required to adhere to a set of standards issued by
the International Organization for Standardization (ISO). Companies that dont follow these
can be prosecuted or at least wont be in business very long!

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http://www.iso.ch/iso/home.htm

This means that there are set procedures for doing things. These are not negotiable.

In this topic, although largely doing bucket chemistry as our Lab Technician Leigh calls it,
you will look at some simple methods of analysis by mass.

3.1 Percentage Composition By Mass

Definitions

Relative Atomic Mass (Ar) the mass of an element relative to carbon twelve.
Carbon 12 has 6 protons and 6 neutrons.
Relative Molecular Mass (Mr) all the Ar in a molecule added together. (Note this is
called a formula mass in ionic compounds!)

Carbon is assigned an Ar of 12.0. This is because a measureable amount of carbon twelve


(called a mole) weighs 12 grams exactly.

One mole of carbon represent 6 1023 carbon atoms. Thats a six in front of 23 zeros. Quite a
large number!

CHALLENGE! The relative atomic mass of carbon is actually 12.01. Carbon-12


weighs 12 grams exactly. Why is the Ar of carbon 12.01? [Hint: find out what an
isotope is]

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The Ar of an element is usually listed underneath the symbol in the Periodic Table.

3.1.1 Calculating Mr

To calculate the Mr of a compound, we look at all the elements in its formula and add them
together.

E.g. Water (H2O) = (2 1.0) + 16.0 = 18.0

E.g.2 carbon dioxide (CO2) = 12.0 + (2 16.0) = 44.0

3.1.2 Calculating Percentage Composition

To calculate the percentage composition by mass of an element in a compound, you add up


the total Ar of that element and divide it by the Mr of the compound and then multiply the
result by 100%.

E.g. Calculate the percentage composition/by mass of carbon in carbon dioxide.

%C = 12.0 / 44.0 100% = 27.3%

E.g.2 Calculate the percentage by mass of hydrogen in hydrogen peroxide (H2O2).

%H = (2 1.0) / (2 1.0 + 2 16.0) 100% = 5.9%

E.g.3 Calculate the percentage composition of water in hydrated copper(II)sulfate


(CuSO4.5H2O)

%H2O = (5 18.0) / (5 18.0 + 63.5 + 32.0 + 4 16.0) 100% = 36.1%

Exercises

Complete the following table:

Element Compound % composition of element


C CH4

O ZnSO4

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Al Al2O3

H2O ZnSO4.7H2O

O K2Cr2O7

3.2 Determining Water Content of Consumer Products

This is the simplest gravimetric technique. Finding out the water content of something is
usually as simple as evaporating the water in an oven set to about 105-110OC. You compare
the mass of the sample before heating to that obtained after heating. The mass of water is
usually expressed as a percentage. It is important to weigh the final mass, heat it again and
reweigh until a constant value is achieved. This is done to make sure the sample is
completely dry.

E.g. A 5.00 g sample of cat food was placed in an oven at 110OC and weighed again after
20 minutes. This procedure was repeated until a constant mass of 3.15 g was recorded.
Calculate the percentage of water in the cat food.

Answer: (5.00 3.15)/5.00 100% = 37.0%

Question

Which of the following brands of cat food represent the best value for money? Justify your
answer.

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BRAND MASS OF CAT FOOD MASS OF DRY CAT COST PER CAN ($)
(NET) FOOD (NET)
Stripy tail 450 g 275 g 1.25
Gold cat 400 g 200 g 1.10
No name 600 g 280 g 1.15

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3.3 The Mole

The mole is a quantity, a number a very large number. In fact one mole is equal to 6.02
1023 (602 000 000 000 000 000 000 000). The mole is a significant number in chemistry
because 1mole of 12C weighs 12g exactly. This means 1 mole of any element is its relative
atomic mass in grams. Eg 1 mole of oxygen weighs 16 g; one mole of chlorine weighs 35.5g
and 1 mole of water weighs 18g. Water is made up of two hydrogen atoms plus one oxygen
atom. Therefore, water has a mass of 16 + 1 + 1 = 18g.

3.3.1 Mole Calculations

Two important formulas you need to remember are:

n = N / NA where n = mole; N = number of particles; NA is 6.02 1023


n=m/M where n = mole; m = mass; M = mass of one mole (Molar Mass)

the units for these formulae are:

n moles (mol)
m grams (g)
M grams/mole (g/mol or gmol-1)
N and NA are numbers and have no units

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E.g.1 Calculate the number of moles in 64 grams of oxygen gas (O2).

The first step to solving this problem is to identify what quantity you need to find out and
what formula you need to use. The example asks you to calculate the number of moles. This
is lower case (little) n. The other information you are given in the example is the mass and
you can find the molar mass from the Periodic Table; therefore you will need to use n = m /
M.

n=m/M

n = 64 / (2 16)

n = 64 / 32

n = 2.0

E.g.2 What is the mass of 2.5 mol of methane gas (CH4)?

This time you are required to convert moles into a mass, however you will use the same
formula rearranged. If n = m / M then m = n M. In other words, the mass is equal to the
number of moles multiplied by the mass of one mole of the chemical you have.

m=nM

m = 2.5 (12 + 1 + 1 + 1 + 1)

m = 2.5 16

m = 40 g

E.g.3 3.0 moles of a diatomic element (molecule made from two atoms) has a mass of 84
g. Write the formula of the molecule.

n = 3.0, m = 84, M = ?

M=m/n

M = 84 / 3

M = 28 g/mol

The molecule is N2

Questions and Exercises

1. Calculate the mass of the following:

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a. 1.0 mol of Ne
b. 1.0 mol of H2
c. 2.5 mol of OF2

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2. Calculate the number of moles of the following:

a. 32 g of O2
b. 72 g of C
c. 0.44g of CO2

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3. Calculate the molar mass of a compound if 3.0 moles has a mass of:

a. 36g
b. 48g
c. 180g

3.4 Gravimetric Analysis

Gravimetric analysis takes advantage of the solubility of chemicals, many of which you
explored in Experiment 1. Basically, you extract a soluble compound out of a sample and
then precipitate it with an excess amount of another chemical. Then you weigh it and
calculate the mass of the previously soluble chemical. One commonly used procedure is to
determine the mass of table salt (NaCl) in food.

3.3.1 Steps in gravimetric analysis

1. Weigh the dried sample.

BOJ 2009 Page 31


2. Dissolve the sample and filter. Discard the residue.

3. Add an excess of the precipitating compound to the filtrate.

4. Filter the precipitate.

5. Dry and weigh the precipitate.

6. Continue drying and weighing until a constant mass is obtained.

E.g. A sausage roll was analysed for its salt content using gravimetric analysis. A 5.0 g
sample of sausage roll was mashed using a mortar and pestle. The mashed sample was then
placed in 50 ml of hot water to dissolve the salt. The mixture of sausage roll and water was
allowed to cool and then filtered. Excess silver nitrate (AgNO3) was added to the filtrate and
a grey/white precipitate was formed. The precipitate was filtered, dried and weighed to a
constant mass. This mass was 0.0300 g. Calculate the mass of salt in the 5.0 g sample.

Mortar and pestle (far


left )and the Buchner
vacuum filtration
apparatus (left)

www.creative-chemistry.org.uk
upload.wikimedia.org

Answer

First of all, you need to identify the precipitate formed. Weve added AgNO 3 to precipitate
NaCl. However, Na is soluble all the time! So why does adding AgNO3 work? The answer is
that the Ag+ ions will precipitate the Cl- ions to form AgCl(s).

Assuming that all the Cl- ions come from NaCl, if you can work out the mass of Cl- you can
work out the mass of NaCl. Heres how you do it!

1. Work out the percentage by mass of Cl- in AgCl.

%Cl- = (35.45 / 107 + 35.45) 100% = 24.89%

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2. Work out the mass of Cl- in the AgCl precipitate.

Mass of Cl- = 24.89% 0.0300 = 0.2489 0.0300 = 0.007467 g

3. Work out the percentage by mass of Cl- in NaCl. Remember that all of the Cl- has
come from NaCl.

%Cl- = (35.45 / 23.0 + 35.45) 100% = 60.65%

This means 60.65% of the NaCl in the 5.0 g sample = 0.007467 g. So what does 100%
equal?

4. Its a ratio calculation like the ones you did in maths last year.

0.007467 : 60.65% as x : 100%

Therefore x = 100 / 60.65 0.007467 = 0.0123 g = 12.3 mg

Dont be too concerned if you found this difficult. It is a calculation normally associated with
students enrolled in Unit 3 Chemistry.

Exercises

A food chemist was asked to determine the mass of salt in a 25 g biscuit. She decided to use
gravimetric analysis to find the answer.

(a) Describe the steps she would take to determine the salt content of the biscuit.

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(b) The dried and weighed precipitate of AgCl was 125 mg. Calculate the mass of NaCl in
the biscuit.

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3.4 Volumetric Analysis

Volumetric analysis is quantitative analysis using concentration and volume.

Definitions

Concentration the comparison of the amount of solute in a solvent.


Solute the chemical that is dissolved /mixed into the solvent
Solvent the substance in which something is dissolved in, The most common
solvent is water.

3.4.1 Units of Concentration

Mass/mass (w/w) mass of solute compared to the total mass of the solution. Expressed in
grams per kilogram (g/kg), milligrams per gram (mg/g), milligrams per kilogram (mg/kg).

Mass/volume (m/v) mass of solute compared to volume of solution. Expressed as grams


per litre (g/L), milligrams per litre (mg/L) and micrograms per litre (g/L)

Volume/volume (v/v) volume of solute compared to volume of solution. Expressed as


millilitres per litre (ml/L), microlitres per litre (l/L).

Parts Per Million (ppm) an old measure of concentration. It means how many parts of a
solute are in a million parts of the solution. E.g. a 10 ppm solution of mercury in sea water
means 10 mg/L*.

* 1 mL of water weighs 1 gram. Therefore one litre of water (1000 mL) weighs 1000 grams (1
kg). There are 1 million milligrams in 1 kilogram.

Parts Per Billion (ppb) 1 ppb = 1g/L = 1 l/L

Calculations

E.g. Convert 0.05 grams of salt in a 1.0 L solution to mg/L

BOJ 2009 Page 34


Change grams into milligrams ( 1000), therefore its a 50 mg/L (w/v) solution.

E.g.2 Convert 0.025 g of salt in 250 mL of water to mg/L.

25 mg in 250 mL. Again another ration conversion.

25 : 250 as x : 1000

Therefore x = 1000/250 25 = 100 mg/L (w/v)

E.g.3 Convert 0.50 mL of salt in 100 mL of solution to ppm

1 g = 1 ml; therefore there is 0.50 g, therefore 500 mg.

500 mg : 100 mL as x mg : 1000 mL

Therefore x = 1000/100 500 = 5000 mg/L = 5000 ppm

3.4.2 Titration
Titrations involve reacting a precise volume of a reactant of known concentration to an
analyte of unknown concentration. If you know the reaction that takes place, it is possible to
work out exactly how much of the analyte is present, and therefore the concentration.
Titrations are often used for acid-base reactions. A known amount of acid will neutralise a
known amount of base.

Definitions
Indicator a chemical that changes colour according to pH.
Burette a glass cylinder that delivers precise volumes of solution.
End point the point at which there is slightly excess acid or base in a solution.
Meniscus the curved shape associated with the level of solution in a burette.
Pipette apparatus designed to transfer an exact volume of solution.
pH a scale from 0-14 indicating how acidic a solution is. 1 is very acidic.

APPARATUS USED IN TITRATIONS

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BURETTE there are a number of different sizes for
burettes. The ones we use at school hold a volume
of 50.00 ml. Each ml is divided into 10 parts. In
effect, you can read the amount of solution
delivered in millilitres to two decimal places (on the
line or half way between). The picture on the right
shows a burette that has delivered 30.00 ml;
assuming it was filled up to the top. Notice the
curvature of the liquid. This is called the meniscus.
The liquid moves up the side of the burette due to
forces of attraction. This is why the best way to read
the level of a burette is AT THE BOTTOM OF THE culturesciences.chimie.ens.fr
MENISCUS.
BULB PIPETTE the bulb pipette is an important
piece of equipment used in titrations. It is calibrated
to precisely (with a slight error) to deliver a set
volume. This means the scientist can decide exactly
what volume of solution they want to react with the
solution in the burette. The contents of a pipette
are usually transferred to a volumetric flask or
conical flask.

www.camlab.co.uk
VOLUMETRIC FLASK again another very important
piece of glassware. These flasks are very accurate
and hold a specific volume of solution. At the
bottom of the meniscus, you can see a thin line
etched into the glass. This line is the 250 ml line.
There are no other measuring lines. So its 250 or
nothing! They are primarily used in titrations to
dilute solutions. A known volume of a solution is
added to a volumetric flask by a bulb pipette and
the volume is made up to the mark with distilled
water.
www.enasco.com

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RETORT STAND used to hold the burette straight
and upright so the scientist can operate the burette
tap comfortably. A boss head is attached to the
stand and holds the clamp that holds the burette.

www.rapidonline.com
CONICAL (Erlenmeyer) FLASK holds either the
known or unknown concentration solution. They
require constant swirling to ensure the chemical
from the burette mixes quickly with the solution in
the conical flask. A white tile is placed underneath
the conical flask so that colour changes by the
indicator are noticed easily.

www.sci-journal.org

3.4.2.1 The Indicator


An indicator is vitally important in a titration. As mentioned earlier, an acid-base indicator
changes colour according to pH. You have probably used universal indicator before, it shows
a range of pH by changing different colours. Universal indicators are not very useful for
titrations. Acid-base titrations require the scientist to be able to see an indicator change on
a drop-by-drop basis. These indicators are pH specific. In other words, they only work in a
particular pH range. The main indicators used in high school titration experiments are:
phenolphthalein (fennel thay lean). Is clear in acidic and neutral environments
and turns pink in basic (alkaline) environments.
Methyl orange orange/yellow in pH greater than 3. Red in pH less than 3.
Methyl red often used for weak acids. Is red under a pH of 4, yellow over a pH of 6
and orange in between.

3.4.2.2 The End Point


The end point of a titration is where the indicator has a significant colour change. The end
point represents the point at which too much (excess) acid or base is present. This means all
of the analyte has reacted. When an end point is reached, the volume of acid or base added
from the burette is taken.
BOJ 2009 Page 37
3.4.2.3 Titration Calculations

E.g. 20.0 ml of NaOH (concentration unknown) is placed in a conical flask. Three drops of
methyl orange indicator is added to the conical flask. A burette was filled with hydrochloric
acid. The concentration of hydrochloric acid was 3.55 mg/ml. It is known that 1.00 mg of HCl
reacts with 1.13 mg of NaOH.
Slowly the acid in the burette was added to the NaOH in the conical flask. After 28.50 ml of
HCl was added to the conical flask, the indicator changed to a bright pink/red colour.
(a) Calculate the mass in milligrams of NaOH in the conical flask.
(b) What is the concentration of NaOH in mg/ml?

Answer
(a) Before we can calculate the mass of NaOH in the flask, we need to calculate what
mass of HCl was added from the burette. We can do this because we know the
concentration of HCl. For every 1.00 ml of acid we add from the burette, we are
adding 3.55 mg of HCl.
Therefore, mass(HCl) = 28.50 ml 3.55 mg/ml = 101.175 mg.

Now if 1.00 mg of HCl reacts with 1.13 mg of NaOH, the mass of NaOH = 1.13
101.175 = 114 mg.

(b) We have 114 mg in 20 ml so how many mg do we have in 1.0 ml?


114:20 as x:1.0 so x = 114/20 = 5.7 mg/ml

Exercises
1. 20.0 ml of HCl (concentration unknown) is placed in a conical flask with three drops
of indicator. 18.00 ml of NaOH (5.0 mg/ml) was added from a burette and the colour
changed from clear to pink.
(a) Calculate the mass of HCl in the conical flask. (1 mg NaOH reacts with 0.885 mg HCl).
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(b) Calculate the concentration of HCl (mg/ml) in the conical flask.
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(c) What was the indicator used in this titration?
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CHALLENGE! Explain why the indicator from the previous problem was used.

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2. The concentration of acid (ethanoic) in white vinegar was to be determined using a


titration. A 50.0 ml sample of white vinegar was placed in a conical flask. Three drops
of phenolphthalein indicator was also added to the conical flask. A burette was filled
with NaOH (4.0 g/L). A colour change was observed after 21.50 ml of NaOH was
added. This procedure was repeated a further two times to get an average volume
(titre). The volumes from the second and third titres were 21.65 ml and 21.55 ml. It
is known that 1.00 g of NaOH reacts with 0.667 g of ethanoic acid.
(a) Calculate the average volume of NaOH added from the burette.
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(b) Using the average volume of NaOH added, calculate the mass, in grams, of ethanoic
acid in a 50.0 ml sample of white vinegar.
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(c) Calculate the concentration of ethanoic acid (g/L) in the white vinegar.
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(d) Calculate the percentage (w/v) of ethanoic acid in the white vinegar.
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3.5 Colorimetry
Definitions
Standard solution a solution of known concentration
Absorbance the amount of light a chemical absorbs

Colorimetry is a technique that takes advantage of the fact that many solutions absorb light.
The reason this occurs is beyond the scope of this course, however most materials absorb
some light. This is why they appear coloured.

3.5.1 Preparing standards


A standard solution is made by dissolving an exact amount of solute in a known volume so
that the concentration is exactly known. Sometimes scientists will even react these
standards in a titration to confirm the accuracy of the known concentration.
For example, lets say we want to make standard salt solutions of 1%, 5%, 10% and 20% w/v.
Remember, a percentage is a number out of 100. A 1% w/v solution of NaCl means 1 gram
of NaCl per 100 ml of water; 5% means 5 g per 100 ml and so on.

E.g. What mass of NaCl would be required to make a 5% w/v standard solution using a
250 ml volumetric flask?

Answer
5% w/v means 5 grams in 100 ml. However, we are using a 250 ml flask. 250 ml is 2.5 times
greater than 100 ml. To keep the concentration at 5%, you need 2.5 times the mass of NaCl.

5g : 100 ml as x : 250 ml, therefore x = 250/100 5 = 12.5 g

E.g. 2 What volume of ethanol would be required to make a 40% v/v solution using a 25.0
ml volumetric flask?

Answer
40% v/v means 40 ml in 100 ml. However, this flask only contains 25.0 ml one quarter of
100 ml. To keep the concentration we would add one quarter of 40 ml, i.e. 8 ml of ethanol.

40 ml : 100 ml as x : 25 ml, therefore x = 25/100 40 = 8 ml.

Exercise
What mass of NaCl should be added to an 80.0 ml volumetric flask to make a 12.0% w/v
standard solution?
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CHALLENGE! What volume of ethanol should be added to a 50.0 ml
volumetric flask to make a .05% v/v standard solution?

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3.5.2 Selecting The Right Colour (wavelength) of Light

Visible light (all the colours) is made up of different wavelengths. The wavelength of light is
measured in nanometres (nm). I nm = 0.000000001 m. Red light has a wavelength of around
650 nm. Blue light has a shorter wavelength of around 475 nm.

Chemical compounds absorb many wavelengths of light but they absorb some better than
others. Lets look at copper(II)sulfate as an example. In the visible spectrum of light, copper
sulfate absorbs orange light the best and blue light the worst.

What evidence is there to suggest that copper sulfate absorbs blue light the worst
out of the visible colours?

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So when analysing the concentration of a copper sulfate solution, we would set the colour
of light to orange. If this is not available, red would be the next best choice.

What colour of light would you use to analyse orange potassium dichromate?
What could you do to prove you are correct?

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3.5.3 Absorbance v Concentration curves
Once the series of standards have been made, they are put in the colorimeter and their
absorbance is checked. Absorbance versus concentration is plotted as a graph and a line of
best fit is ruled between the points.

www.epa.gov

Using the graph above, suggest an absorbance reading for a 0.24 mg/L
phosphorus solution.

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Absorbance is proportional to concentration. That is, the higher the concentration the
higher the absorbance and the greater the intensity of the colour. So provided you know the
colour produced by the standards, you can even just by looking at the solutions roughly
estimate the concentration. A colorimeter however gives you a greater accuracy.

3.5.4 Determining The Concentration of The Analyte


Once you have determined the absorbance readings for all of your standards, it is time to
check the absorbance of your analyte. Using the graph above, lets say our analyte gave an
absorbance of 0.10. Tracing directly to the graph and then down to the concentration axis,
this equates to approximately 0.105 mg/L of phosphorus.

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CHAPTER 3 REVIEW QUESTIONS
1. Explain the difference between quantitative analysis and qualitative analysis. Provide
examples of each.
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2. Determine the percentage by mass of Cl in NaClO3.
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3. A 50.0 g piece of bread was analysed for its water content. It was dried and weighed
to a constant value of 29.95 g. Calculate the percentage by mass of water in the
piece of bread.
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4. Using the percentage mass of water from Question 3, calculate the mass of water in
a 2.25 kg loaf of the same bread.
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5. Outline the steps and chemicals you would use to determine the percentage by mass
of salt in a tomato by means of gravimetric analysis.
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6. Convert a 0.0600 g/L solution of KNO3 to ppm.
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7. Why should burette reading be taken from the bottom of the solution meniscus?
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8. What is the role of an indicator in an acid-base titration?
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9. Why is universal indicator not a good choice for acid-base titrations?
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10. Draw the experimental setup you would use to determine the unknown
concentration of a sodium hydroxide (NaOH) solution.

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11. Why is orange light used to analyse blue solutions in colorimetry?
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12. What mass of phosphorus would be contained in a 2.50 L bottle of detergent if a
sample gave an absorbance of 0.15

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13. What is the percentage by mass (w/v) of phosphorus in the detergent sample from Q.12?
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CHAPTER 4 QUALITATIVE ANALYSIS
Qualitative Analysis involves finding out what chemicals are present in the analyte..

Qualitative Analysis is done nowadays using sophisticated and very expensive machines that
can detect parts per billion (ppb) of a substance in an analyte. Many of these machines
perform qualitative and quantitative analysis simultaneously.
We however will only be looking at a few techniques. These are:
Flame tests
Atomic Emission Spectroscopy (AES)
Chromatography TLC, HPLC and GC

4.1 Flame Tests


You may have done flame tests in junior science, maybe even in primary school. They are
used to identify unknown compounds by seeing what colour the chemical burns.
Unfortunately, flame tests are limited in their application for a number of reasons:
Borderline colours may be difficult to see
Other chemicals can cause colours to blend
Many chemicals burn the same colour
Not all elements produce a flame colour

4.1.1 What Causes The Colour


When sodium chloride is burnt in the flame of a Bunsen Burner, an amber flame colour is
produced. When sodium nitrate is burnt it also produces an amber flame. However, when
barium chloride and barium nitrate are burnt, a green flame colour is observed.

What causes the colour?_______________________________________________________

4.1.2 Excited Electrons


The reason a flame colour is observed is because of excited electrons. Excited electrons are
those that have jumped to a higher energy level in terms of the shell they occupy. For
example, a sodium atom normally has the electron configuration 2,8,1. An excited sodium
atom may have an electron configuration of 2,7,2. You can see that one of the electrons
from the second shell has jumped into the third shell. The promoted electron has more
energy than it did before.
However, the electron will not stay there for long before returning to its original position
(ground state). When it does return, it gets rid of the excess energy in the form of light. This
light is in the form of a photon.

Photon comes from the Greek language meaning light. Think of a photon as a particle of light,
or a piece of light that has energy.

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imagine.gsfc.nasa.gov

4.1.3 Why Different Colours?


Okay we have established that:
Metals are responsible for the colour in an ionic salt flame test
The light is caused be excited electrons returning to their ground state and giving off
photons that carry the excess energy.

Why do different metals produce a different colour or the same colour?

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metal flame colour

barium green

calcium orange/red

copper blue/green

lead blue/white

potassium lilac

sodium orange

Strontium red

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CHALLENGE! Find out about the equations E = h and v = f and how they can
explain why we see different coloured flames in flame tests.

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4.2 Atomic Emission Spectroscopy (AES)

Definitions
Emission spectrum all the colours (wavelengths) of light emitted by an element
Spectroscope an optical device that allows you to see an emission spectrum
Spectroscopy name given to the method of obtaining a spectrum light in this case
Spectrometer a machine that can use spectroscopy as an analytical technique to
perform qualitative or quantitative analysis (spectrometry) or both.

4.2.1 How Does AES Work


Without going into too much detail, for our purposes, AES is fancy flame testing. It splits the
wavelengths of light that make up a flame colour into lines. It can be used for non-metals
too!

intro.chem.okstate.edu

BOJ 2009 Page 48


Only hydrogen atoms produce this emission spectrum. Other elements produce unique
spectrums of their own, making them identifiable.

4.3 - Chromatography
To write with colours -- literally translated from its Greek roots chroma and graphein ,
chromatography was first developed by the Russian botanist Mikhail Tswett in 1903 as he
produced a colourful separation of plant pigments through a column of calcium carbonate.
Chromatography has since developed into an invaluable laboratory tool for the separation and
identification of compounds. Although colour usually no longer plays a role in the process, the
same principles of chromatography still apply. 1

Definitions
Mobile phase the solvent used to transport chemical components through the
stationary phase. It is sometimes referred to as the eluent.
Stationary phase a medium of which chemical components and the solvent move
through.
Solvent front the first part, or front part, of the mobile phase working its way
through the stationary phase.
Chromatogram a graph/data block/Rf calculations based on a chromatography
experiment.

Confused? Dont worry, it will make sense shortly.

4.3.1 Thin Layer Chromatography (TLC)


You may have actually done some TLC before. Have you separated the dye in a texta or pen?
If you have then you have done basic TLC. Try and think back to what you did to achieve the
separation of dyes. You used a piece of filter paper (stationary phase) to put a dot of texta
or ink on. You then dangled the filter paper in water (mobile phase) which slowly climbed
the paper and took the different colours with it. Eventually the water stopped climbing and
finished at a particular level (solvent front). The experiment was finished.

Why did the dyes in the texta or ink separate?

___________________________________________________________________
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___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
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___________________________________________________________________

1
http://www.umich.edu/~orgolab/Chroma/chromahis.html

BOJ 2009 Page 49


4.3.1.1 Rf (retardation factor) values

Rf values are used to catalogue if you like, how far a chemical component moves up the
stationary phase compared to the mobile phase in a TLC setup.
The Rf is measured by dividing the distance travelled by a component (measurement taken
from the middle of the component) by the distance travelled by the mobile phase.

www.instructables.com
Exercise
Calculate the Rf values of the three components above.

Red (Highest)___________________

Green (middle)_________________

Blue (lowest)___________________

BOJ 2009 Page 50


Which component appeared to be most attracted to the stationary phase? Explain
your answer

___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________

What might happen to the TLC chromatogram if the mobile phase was changed
from water to oil?

___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________

Exercises
1. A TLC plate is made from glass with a coating of aluminium oxide. A sample of plant
pigment is spotted on to the plate. The plate is then placed in a shallow reservoir of
ethanol. After five minutes the ethanol has stopped moving up the aluminium oxide
coated plate. The ethanol has climbed a height of 10 cm. Also on the plate were
three coloured bands. Band A had climbed 3 cm, Band B 5 cm and Band C 7.5 cm.

(a) The stationary phase is:__________________________________________________

(b) The mobile phase is:____________________________________________________

(c) The eluent is:__________________________________________________________

(d) The Rf value of Band B is:________________________________________________

(e) The band least attracted to the stationary phase is:___________________________

BOJ 2009 Page 51


2. Calculate the Rf values of the four components in the chromatogram below.

www.malariajournal.com
1:___________

2:___________

3:___________

4:___________

3. Is it possible for a component on a TLC chromatogram to have an Rf value greater


than one? Explain your answer.
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

BOJ 2009 Page 52


4.3.2 Column Chromatography
Column chromatography operates on the same principles as TLC. However, the depth and
type of chemical analysis that column chromatography is capable of is far superior to that of
TLC. The catch is that column chromatography costs substantially more to set up, operate
and maintain.

The simplest type of column chromatography involves a glass tube (burettes are often used)
packed with a stationary phase like powdered aluminium oxide. The mobile phase (eluent) is
poured into the top and gravity causes the mobile phase and sample to head down the
column. Separation is the same as for TLC, that is, components that are more attracted to
the aluminium oxide stationary phase will not move as far down the column as those less
attracted or more attracted to the mobile phase.

www.ipfw.edu

How would changing the particle size of the stationary phase impact the
separation of components if at all?

___________________________________________________________________
___________________________________________________________________
___________________________________________________________________

BOJ 2009 Page 53


___________________________________________________________________
___________________________________________________________________
___________________________________________________________________
___________________________________________________________________

4.3.2.1 High Performance Liquid Chromatography (HPLC)


This type of column chromatography is also called High Pressure Liquid Chromatography
because the liquid mobile phase is pumped through a very narrow column. These narrow
columns are called capillary columns. They, like the previous technique, are packed with a
solid stationary phase.

HPLC is performed using a chromatograph. A chromatograph is the name given to the


expensive machine (instrument) that can both qualitatively and quantitatively analyse
samples.

www.waters.com

The chromatogram produced in this instance is a graph of peak area versus retention time.
What are they you may ask?
Peak area, as the name suggests, is the area underneath a peak. Peak area is
proportional to concentration. In simple terms the more there is of something the
larger the peak area. Peak area is used for quantitative analysis.
Retention time (RT) refers to how long it takes a component to come out of (elute)
the column. The printout is read from left to right. So those peaks on the left took
less time than those on the right to come out the end of the column. RT is used for
qualitative analysis because different components spend different amounts of time
coming through the column.

BOJ 2009 Page 54


www.statisticaldesigns.com

How can a components retention time be related to its attraction to the


stationary and mobile phase?

_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________

Can you think of any alterations you could do to an HPLC setup to change the R T
(separation) of components?

_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________

BOJ 2009 Page 55


CHALLENGE! HPLC chromatographs are often used to analyse biological
samples. Suppose you wanted to check if a racehorse had been injected with a
particular banned steroid. How would you test for this steroid using HPLC?
[Hint: Retention time is important]

_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________
_________________________________________________________________

4.3.2.2 Gas Chromatography (GC)


Another sensitive and accurate technique. The two main differences between HPLC and GC
are the makeup of the stationary and mobile phase.
The mobile phase is an unreactive (inert) gas like nitrogen (N2) or helium (He)
The stationary phase is a liquid stuck to the inside of the column
The gas is pressurised so it flows through the column. Samples are vaporised (turned into a
gas) before they enter the column. Detection and chromatograms produced are the same.

commons.wikimedia.org

Why do you think an inert gas like nitrogen is used as the mobile in a GC as
opposed to other gases like oxygen and chlorine etc?

_________________________________________________________________
_________________________________________________________________

BOJ 2009 Page 56


CHAPTER 4 REVIEW QUESTIONS
1. Using the table of flame colours on page 44, assign a flame colour for the following
compounds:

(a) KNO3________________________________________________________________

(b) CuSO4_______________________________________________________________

(c) Cu(NO3)2____________________________________________________________

2. Is a magnesium atom with the electron configuration 2,8,2 in its ground state or an
excited state?
___________________________________________________________________________
___________________________________________________________________________
3. What is a spectrum?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
4. Provide two reasons as to why AES is a better qualitative technique than flame
testing.
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
5. What is the difference between the mobile phase and stationary phase used in
chromatography?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
6. What are the reasons that components in sample can be separated using a
chromatographic technique?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
7. How is an Rf value calculated?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

BOJ 2009 Page 57


8. What are the similarities and differences between TLC and HPLC?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
9. Why do you think there is a heated injection port for samples before the column in a
GC?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
10. Use the chromatogram below to answer this question:

www.lipidlibrary.co.uk
(a) Circle the peak that has the least affinity (attraction) for the stationary phase.
(b) Using the peak area numbers at the top of each peak, what is the approximate
retention time for the component in greatest concentration?
___________________________________________________________________________
___________________________________________________________________________
(c) If the flow rate of the carrier gas was decreased, what would you expect to happen
to the retention time of each component?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
BOJ 2009 Page 58
EXPERIMENT 1

PREDICITNG PRECIPITATES FROM IONIC SALTS


Aim:
To predict and verify precipitates forming from the reaction of solutions of various ionic
salts.

Equipment: test tubes, test tube rack, pipettes (eye dropper), various ionic solutions

Procedure:
1. Place six clean test tubes into a test tube rack.
2. Place a small amount (2-3 mL) of one solution in each tube.
3. Place the same amount of different solutions in each of the six test tubes.
4. Record your observations in the results table below.
5. Wash your test tubes and repeat 1-5 using a different starting solution. Continue
using new solutions until the table below is complete.

Results & Calculations


Cl- CO32- NO3- OH- Cr2O72- SO42-
Al3+
Ag+
Ca2+
Cu2+
K+
Na+
NH4+

KEY: S (soluble) SS (slightly soluble) I(insoluble)

Discussion:
1. What do you notice, in terms of solubility, about salts that have sodium and
potassium in them?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

BOJ 2009 Page 59


2. Are there any other ions that resemble the solubility of K+ and Na+? What evidence
do you have?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

3. What do you notice about solutions of Al3+ and Ca2+?


___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

4. Are there any patterns to be observed in terms of the solubility of both the cations
and anions in your experiment?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

Conclusion: Write a conclusion on the solubility of various ions based upon your research.
___________________________________________________________________________
___________________________________________________________________________
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___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

EXPERIMENT 2
WATER CONTENT DETERMINATION OF GARDEN SOIL
AND COMMERCIAL POTTING MIX
Modified from http://www.uic.edu/classes/cemm/cemmlab/Experiment%201-Water%20Content.pdf
Aim:
This test is performed to determine the water (moisture) content of soils. The
water content is the ratio, expressed as a percentage, of the mass of pore or
free water in a given mass of soil to the mass of the dry soil solids.
Standard Reference:
BOJ 2009 Page 60
ASTM D 2216 - Standard Test Method for Laboratory Determination of
Water (Moisture) Content of Soil, Rock, and Soil-Aggregate Mixtures
Significance:
For many soils, the water content may be an extremely important index used
for establishing the relationship between the way a soil behaves and its properties. The
consistency of a fine-grained soil largely depends on its water content.
Equipment: Drying oven, Balance, Moisture can, Gloves, Spatula.

Procedure:
(1) Record the moisture can and lid number. Determine and record the
mass of an empty, clean, and dry moisture can with its lid (MC)

(2) Place the moist soil in the moisture can and secure the lid.
Determine and record the mass of the moisture can (now containing
the moist soil) with the lid (MCMS).

(3) Remove the lid and place the moisture can (containing the moist
soil) in the drying oven that is set at 105 C. Leave it in the oven
overnight.

(4) Remove the moisture can. Carefully but securely, replace the lid on
the moisture can using gloves, and allow it to cool to room
temperature. Determine and record the mass of the moisture can
and lid (containing the dry soil) (MCDS).
(5) Repeat Steps 1-4 for the supplied potting mix.

(6) Empty the moisture cans and clean the cans and lids.

Results & Calculations:


Complete the table below using your scale measurements and the following calculations:
(1) Determine the mass of soil solids.
Ms = MCDS MC

(2) Determine the mass of pore water.


Mw = MCMS MCDS
BOJ 2009 Page 61
(3) Determine the percentage free water content.
w = (Mw / Ms) 100%

GARDEN SOIL POTTING MIX


Moisture can and lid number

MC = Mass of empty, clean can + lid


(grams)

MCMS = Mass of can, lid, and moist soil


(grams)

MCDS = Mass of can, lid, and dry soil


(grams)

Ms = Mass of soil solids (grams)

Mw = Mass of pore water (grams)

w = Water content, w%

Discussion
1. Using your analysis results, comment on the ability of potting mix to hold water
compared to the garden soil.
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
2. What are some of the errors associated with the experiment and how do they
impact on your results?
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

BOJ 2009 Page 62


___________________________________________________________________________
___________________________________________________________________________
3. Suggest at least one modification to the experimental procedure that could minimise
one of the errors listed in the previous question.
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

Conclusion
Write a brief conclusion you have drawn from comparing the ability of soil and potting mix
to hold water.
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

BOJ 2009 Page 63


THE ETHANOIC ACID CONCENTRATION IN WHITE VINEGAR

Aim: To determine the ethanoic acid concentration of white vinegar using acid-base
titration.

Procedure:
1. Using a 20.0 ml pipette, take 20.0 ml of vinegar and place in into a 250 ml volumetric
flask. Fill the rest of the flask up to the line with water.
2. Using a new 20.0 ml pipette, take 20.0 ml of the dilute vinegar from the volumetric
flask and place it in a conical flask.
3. Fill your burette with 0.10 M sodium hydroxide (NaOH) solution.
4. Add three drops of phenolphthalein indicator to the conical flask.
5. Place the conical flask on a white tile and put it directly under the opening of the
burette.
6. Add NaOH from the burette to the dilute vinegar until the colour changes to a
permanent pink. (Remember to slow down when the colour starts to linger!)
7. Repeat steps 1-6 another two times so you have three results in total.
Theory:
According to the chemical equation that shows the reaction of ethanoic acid with sodium
hydroxide:

CH3COOH(aq) + NaOH(aq) CH3COONa(aq) + H2O(l)

One mole of ethanoic acid reacts with one mole of sodium hydroxide. So lets say that you
added 15.0 ml of 0.10 M NaOH from the burette before the colour changed to a permanent
pink. If we work out the number of moles of NaOH by using the formula n = c v, we can
work out the number of moles of ethanoic acid.
So the number of moles of NaOH = 0.10 0.015 = 0.0015 mol. Therefore the amount of
ethanoic acid in the dilute vinegar is also 0.0015 mol.
BUT THIS IS NOT THE TOTAL NUMBER OF MOLES FROM THE UNDILUTED VINEGAR!

Remember, you took 20.0 ml out of a total of 250 ml of the original vinegar sample so you
allow for this in your calculation by multiplying 0.0015 by (250/20). So in this example the
total number of moles of ethanoic acid in the original 20.0 ml sample of vinegar is 0.01875
mol.
To change this into a mass, you use the formula m = n M;
Therefore m = 0.01875 (12 + 3 + 12 + 16 + 16 + 1)
= 0.01875 60
= 1.125 grams in 20.0 ml of vinegar
Therefore the concentration of ethanoic acid (w/v) is:
1.125/20 100%
= 5.6% w/v

BOJ 2009 Page 64


Questions
1. Calculate the average volume (titre) of sodium hydroxide added from the burette in
your three titrations. Use the average volume for your calculations.
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
2. Calculate the average amount (moles) of sodium hydroxide added from the burette.
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
3. Calculate the amount (moles) of ethanoic acid in the dilute vinegar.
_____________________________________________________________________
_____________________________________________________________________
4. Calculate the amount (moles) of ethanoic acid in the original 20.0 ml sample of
vinegar.
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
5. Calculate the mass of ethanoic acid in the original 20.0 ml sample of vinegar.
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
6. Calculate the concentration (% w/v) of ethanoic acid in the original sample of
vinegar.
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________

Discussion:__________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
Conclusion:__________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

BOJ 2009 Page 65


COLORIMETRIC DETERMINATION OF THE PHOSPHOROUS CONTENT OF LAWN
FERTILISER

Aim: To determine the phosphorous content of a lawn fertiliser by colorimetric analysis.

Procedure:

Part A
1. Record the brand and phosphorous content of the fertiliser.
2. Accurately weigh about 0.0310 g of finely ground fertiliser into a 100 ml beaker and
record the mass.
3. Add about 20 ml of hot water and stir to dissolve the powder.
4. Transfer the solution from the beaker into a 250 ml volumetric flask and make up to
the mark with water. Invert the flask back and forth a few times to ensure the
concentration is even.
5. Take 25 ml of the fertiliser solution using a 100 ml measuring cylinder and place it
into a clean 250 ml measuring cylinder. Make up to 250 ml with water.
6. Label six test tubes as follows: 10 mg/L, 7.5 mg/L, 5.0 mg/L, 2.5 mg/L and 0.0 mg/L
and unknown.
7. Place about 20 ml of the dilute fertiliser solution into the test tube labelled
unknown.
8. Use the following table to make the right concentrations for your remaining test
tubes:
Test Tube (mg/L) Volume of 10.0 mg/L Volume of water (ml)
phosphate solution
10.0 20 0
7.5 15 5
5.0 10 10
2.5 5 15
0.0 0 20
9. Add 2 ml ammonium molybdate reagent and a few crystals of ascorbic acid to each
of the six test tubes. Stir each test-tube to dissolve the crystals.
10. Place the six test-tubes in a 600 ml beaker containing 200 ml of boiling water. Heat
them for 5 minutes. The solutions should turn blue upon heating.
11. Remove all test-tubes at the same time and allow to cool.
12. Compare the colour of the unknown with the colour of the standards and estimate
the concentration of phosphate in the fertiliser. Record this estimation.

Part B Using the colorimeter


1. Fill a cell to full with 0 mg/L solution. Select orange or yellow light on the
colorimeter and press the CAL button on the colorimeter.
2. Make sure the colorimeter setting is on absorbance and repeat step 1 using the
other five phosphate standards plus the unknown. Record the absorbance for each
standard and unknown.

BOJ 2009 Page 66


Results & Calculations:

Mass of fertiliser used:_________________________

Estimated concentration from Part A:_____________

Phosphate Standards Absorbance Reading on Colorimeter


10.0
7.5
5.0
2.5
0.0
Unknown

Plot a graph of Absorbance v Phosphate concentration on the grid below.

Draw a line of best fit through points on the graph.

The concentration of phosphate from the graph is:__________________________________


BOJ 2009 Page 67
Discussion:
1. The original fertiliser solution was diluted 10 times. Therefore, what is the
concentration of phosphorous (as phosphate ions) in the original fertiliser?
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
2. What mass of phosphorous was in the original 250 ml solution?
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
3. Calculate the percentage by mass (w/w) of phosphorous in the original fertiliser
sample.
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
4. Compare your result with the stated percentage on the fertiliser packet. Try to
account for any difference.
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
5. Why was orange light used and not blue light for the colorimeter setting?
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
Conclusion:__________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________
___________________________________________________________________________

BOJ 2009 Page 68

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