Angeles University Foundation Prelims

ANALYTICAL
CHEMISTRY

Tools and Techniques in Analytical Chemistry


Analytical Chemistry Type to
• often is describe as the area of chemistry • With doors so that dust does not collect any air
responsible for characterising the composition of current in the room and would not affect the
matter
balance operation

• Qualitatively (Is there lead in this paint chip)

• Quantitatively (How much lead is in this paint How To Use

chip)
1. Calibrate the Analytical Balance

2. Set the Mode for the desired unit

3. Open door and put your weighing boat

pH meter 4. Tare the balance to recalibrate

• “power of hydrogen”
5. Put desired amount of substance

• used an electrode to measure the pH of solution

6. Wait for the asterisk (*) or circle symbol as
• Buffer Solution: used to maintain pH of this indicate the final weight of the
substance (e.g. PBS - Phosphate Buffer System)
measurement

• 2 Substances to use to adjust pH:

• 0.4M NaOH Top Loading Balance

• base
• To weigh solid material when precision of 0.1g is
• increases pH
adequate

• charge is (-) negative

•  Affected by air

• 0.2M NaCl
• Acid Desiccator and Desiccant
• Decreases pH
•  Dried materials are stored while they cool as to
• Standard Material: pH 4, pH 7, pH 10
minimise the uptake of moisture

• Drying Agents:
Oven Dryer • Anhydrous calcium chloride

• Used for removing moisture from solids

• Calcium sulfate

• Necessary since you cannot use pipet, test tubes • Anhydrous magnesium perchlorate

or other equipment if they are not dried as this • Phosphorus pentoxide

affects accuracy
• Rubber: inhibits the formation of moisture

• Less pressure = less moisture

Analytical Balance
• a weighing instrument with a maximum capacity Pipets
that ranges from 1g to few kg with a precision at • Glass tubes used for transferring or measuring

least 1 part in 10 5 at maximum capacity

• A class of balanced designed to measure small Graduation of Pipets:

mass
• “TC” (to contain): contain the necessary volume
but do not deliver exact volume, due to tendency

Tools and Techniques in Analytical Chemistry 1

Angeles University Foundation Prelims

fluids to cling in the glass surface; has no Wash Bottle

calibration; e.g: glass dropper
• A squeeze bottle with a nozzle

• “TD” (to deliver): will deliver exact volume, small • Used to rinse various pieces of laboratory
amount left in the tip should be blown out; with glassware

calibration

Reagents
Rings/Bands in the Pipet:
• Single Painted Ring: drain out; drain liquid by Technical or Commercial Reagent
touching the tip of the pipet of the receiving • superficial purification

vessel; last drop is dripped/touched at the •  preparation of cleaning solution

receiving vessel
• seldom used in analytical chemistry

• Double Painted Ring: blown out; completely

empty the contents by blowing out all the USP and NF Reagent
remaining liquid in the pipet using an aspirator • Used by pharmacist

bulb
• Has impurities which would make the substance
unfit for medical/medicinal use

Types of Pipet: • Comply of exceed to the standards or criteria set

• Mohr Pipet: graduation always end before the forth by the agencies

tip (TD)
• USP: United States Pharmacopoeia
• Serological Pipet: graduation mark continues up • NF: National Formulary

to the tip

• Volumetric Pipet: delivers a single fixed volume CP Reagents (chemically pure)

between 0.5 and 200mL • With high degree of purity

• Micropipet:
• Impurities are too small to cause interference

• Usually automatic
• Used in molecular laboratory

• Deliver adjustable uL of volume of liquid

• 10 to 2,500uL
Reagent Chemical Grade
• A.k.a: Analytical Reagent/Certified Reagent

• first stop: to draw/aspirate

•  Labelled with “meet the ACS Specification”

• second stop: to dispense

• ACS: American Chemical Society

• MicropipetTips: size depends on the volume

Less volume = less size of tip

Primary Standards
Biuret/Buret • Has a purity of greater than 99.5%

• Used to standardise a solution to a very high

• Used in titration

degree of accuracy

• Has a stopcock

• Contain specific amount of concentration/volume

• Glass stopcock: Acid
of specific analyte

• Rubber tubing: Base

• Teflon stopcock: Acid/Base

Specific Purpose Regent Chemicals

• Teflon is not destroyed by either acid or • Prepared for specific application 

base

Volumetric Flask • For spectrophotometry and HPLC

• Usually calibrated to contain a specified volume • HPLC: High performance liquid chromatography

when filled to a line etched on the neck

• Include its absorbance at selected wavelengths
• Capacity: 5mL to 5L
and is ultraviolet cut off wavelength

Tools and Techniques in Analytical Chemistry 2

Angeles University Foundation Prelims

ANALYTICAL
CHEMISTRY

Methods of Expressing Concentrations


Solution Percent Concentration by
• Homogenous mixture of substance (solute)
dissolve in another substance (solvent)
Mass-Mass (%m/m)
• Solute: Substance being dissolved
• The amount of solute in grams present in 100
• Solvent: Substance that dissolves the solute
grams solution

m a ss of sol u te
m /m = × 100

Concentration: m a ss of sol u t i on
• Ratio of amount of solute to the amount of Ma ss of s ol u t i on = s ol u t e + s ol v e nt

solvent

Molarity Percent Concentration by

Mol a r it y =
m ol es of sol u te

Volume-Volume (%v/v)
liters of sol ve nt • Volume of solute in mL present in 100 mL
solution

w e i g h t (g r a m s) vol u m e of sol u te
m a ss of s ol u t e =
v /v = × 100

m ol a r m a ss (g /m ol ) vol u m e of sol u t i on

What is the molarity of a 125mL solution containing Percent Concentration by

0.050 moles of hydrochloric acid Mass-Volume (%m/v)
• The number of grams of solute dissolved in each
100 mL of solution

m a ss of sol u te
m /v = × 100

vol u m e of sol u t i on
Dilution
• Process in which more solvent is added to a Parts per Million (PPM)
solution in order to lower the concentration
• The mass of ration of grams of solute to one
C1V 1 = C 2V 2
million grams of sample

• C1: concentration of original stock solution

m a ss of sol u te
pp m = × 106

• V1: volume of original stock solution

m a ss of sol u t i on
• C2: concentration of final solution

What is the concentration of a solution in ppm if 0.02

• V2: volume of final solution

g NaCl is dissolved in 1000 g of solution

How many mL of a 2.50 M NaOH solution are

required to make 525mL of a 0.150 M NaOH
Solution?

1 gram = 1 mL

Methods of Expressing Concentration 3

Angeles University Foundation Prelims

ANALYTICAL
CHEMISTRY

Factors Affecting Rate of Chemical Reaction


Chemical Reaction Collision Theory
• Reaction rate depend on collision between
• Process in which at least one new substance is
reacting particles

produced as a result of chemical change

• The particles collide and make new substances

• Reactants Products

To Have a Successful Chemical

Evidences of Chemical Change
• Color Change

Reaction
• Particles collide with each other

• Precipitate

• Particles have proper orientation

• Gas bubbles

• Particles have sufficient kinetic energy to break

• Heat/Light

bonds

Types of Chemical Reaction Activation Energy (Ea)

Combination • Minimum energy required for a reaction to occur

• Two reactants combined to form a new product

• Depends on the reactants

• Low activation energy = faster reaction rate

• A + B ➜ AB

Decomposition Activated Complex

• Transitional structure which exist where old
• Single compound breaks into 2 or more simpler
bonds break and new bonds are being formed

substances

• AB ➜ A + B
Factors Affecting the Rate
Single Displacement Temperature
• Active element kicks out less active element
• Directly proportional to the rate of reaction

• A + BC ➜ AC + B
• Increased in Temperature would lead to an
increase in Kinetic Energy thus increase the
Double Displacement frequency and number of collision between
• Switching of partners

particles

• AB + CD ➜ AC + BD
• Increase Temperature = more opportunities for
collision

Reaction Rate • HCl + Na 2 S2O3 = S + NaCl + H2O

• Expressed as the amount of reactant changing

• S which is sulfur is a yellow precipitate that is a
per unit of time
product due to temperature

• Related to the properties of atoms, ions and

• Reaction rate is doubled every 10-degree Celsius
molecules through a model called the collision
increase in temperature.

theory

Factors Affecting Rate of Chemical Reaction 4

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Concentration Presence of Catalyst

• Directly proportional to the rate of reaction
• Catalyst: compound which increase the reaction
• Increased in Concentration = increase rate without being consumed

opportunities for collision due to the increase in • It lowers the activation energy needed.

the number of particles participating in the • The more complex, the more it won’t react

reaction

• HCl + Mg = Mg Cl2 + H2

• Increase in solution = increase in no of reacting

substance present

Nature of Reactants
• Inversely proportional to the rate of reaction

• Substances vary in tendencies to react

• Increased in the Complexity of the particles

would only mean an increased in the energy
needed to break bonds, thus reaction rate is
slower

• Metal + Aci d s = H2 g a s + Salt

• HCl > H2 SO2 > HNO3 > H2 PO4

• HCl + Mg = Mg Cl2 + H2

• H2 SO4 + Mg = MgSO4 + H2

• HNO3 + Mg = Mg (NO3)2 + H2

• H2 PO4 + Mg = Mg3(PO4 )2 + H2

• Z n> Fe > Cu (m or e to less r ea ct ive)

• Z n+ HCl = Z nCl2 + H2
• Fe + HCl + FeCl2 + H2
• Cu + HCl = Cu Cl2 + H2

Surface Area
• Directly proportional to the rate of reaction

• Increased in Surface Area = Decreased in

Particle Size  

• When surface area increases in means that more

area of the particles is exposed thus an
increased in the availability of reactants

• Increased in availability of reactant = increased in

collision = faster reaction rate

• Ca + CO3 + HCl = CaCl2 + H2CO3

Factors Affecting Rate of Chemical Reaction 5

Angeles University Foundation Prelims

ANALYTICAL
CHEMISTRY

Le Chatelier’s Principle

Effect of a Catalyst
Le Chatelier’s Principle • Catalyst increases rate of a reaction without
• A.K.A. Law of Equilibrium
being consumed in the reaction

• Named after Henry Louis le Chatelier, who • The use of a catalyst does not affect the position
discovered it independently

and composition of the equilibrium of a reaction

• It states that: “If a stress is applied to a system in • Both forward and backward reaction are sped up
equilibrium, equilibrium shifts in a way that tends by the same factor 

to undo the effect of the stress”
same thing w/ noble gas: do not affect
equilibrium

Change in Concentration
• Changing the concentration of a chemical will
shift the equilibrium to the side that would
Results
reduce that change in concentration
A. Silver Ion Equilibria
• The chemical system will attempt to partly
oppose the change affected to the original state Reaction Shift Result
of equilibrium. In turn, the rate of reaction extend Right White ppt
and yield of product will be altered
corresponding to the impact on the system
Left Ppt
dissolution
•A+B C+D

Right White ppt

• increase in concentration of A & B = right shift

• increase in concentration of C & D = left shift

Left Ppt
dissolution
Change in Temperature Right Yellow ppt
• Effects in temperature depends whether heat is a
product or reactant
Left Gray ppt
• If a chemical reaction uses heat for the reaction
to take place, it is an endothermic reaction 

(immediate formation of heat and would
Equilibrium Systems
eventually subside)
1. Silver Carbonate Equilibrium
• If a chemical radiates heat after the reaction
A g2CO3 = 2A gCO3

takes place, it is an exothermic reaction

2. Silver Chloride Equilibrium

Exothermic Endothermic
A g+ Cl = A gCl
Increase in Left Shift Right Shift 3. Silver Iodide Equilibrium
Temperature A gI = A g+ I
Decrease in Right Shift Left Shift
Temperature

Le Chatelier’s Principle 6
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Silver Carbonate Equilibrium • NH3 reacts with Ag causing the decrease in

amount; to undo the stress, the equilibrium will
Gross Molecular Equation shift to the left

AgNO3(aq) + Na2CO3(aq) = Ag2CO3(s) + 2Na NO3 • Visually the precipitate (AgCl) dissolves to form
White ppt the species left of the equilibrium

Ionic Molecular Formula Effect of HCl & NH3

Na + Ag+ NO3 + CO3 = AgCO3(s) + Na + No3 A g(aq) + Claq) + HCl(aq) = A gCl(s)

• Spectator ions are cancelled from the equation A g(aq) + NH3(aq) = [A g(NH3)2 ](aq)

forming the net ionic equation:

• Addition of HCl increases the amount of Cl on

• Serves as a byproduct: do not participate in
the left side of the equilibrium; to undo the
the next equation

stress, the equilibrium will shift to the right

• These are those who did not bind with the

• Ag reacts with increased Cl which visually forms
metal because metals are reactive compounds

as white precipitate

A gCO3(s) = 2A g(aq) + CO3(aq)

• Conversely adding NH3 to this solutin re-
White ppt dissolves the white ppt to reform the Ag(NH3)2

Effect of Addition of HNO3 Silver Iodide Equilibrium

A gCO3(s) = 2A g(aq) + CO3(aq) + HNO3
Gross Equation
White ppt Reacts with CO3 [A g(NH3)2 ](aq) + I(aq) = A gI(s) + NH3(aq)

• HNO3 reacts with CO3 causing the decrease Ionic Equation

in its amount to undo the stress, the
A g(aq) + (NH3)(aq) + I(aq) = A gI(s) + NH3(aq)

equilibrium will shift to the right

• Visually, the ppt(Ag2(CO3)) dissolved to form Net Ionic Equation

the species to the right of the equilibrium
A gI(s) = A g(aq) + I(aq)

Silver Chloride Equilibrium Effect of Addition of Na2 S

Effect of Addition of HCl A gI = A g+ I + Na 2 S

• Take note that Ag and NO3 are still on the A g+ S = A g2 S

solution
Gray ppt
A g(aq) + NO3(aq) + H(aq) + Cl(aq) = A gCl(s) + H(aq) + NO3(aq)
• Na2s reacts with Ag causing the decrease in
• Spectator ions are cancelled from the equation amount of Ag; to undo the stress the equilibrium
forming the ionic equation
will shift to the right

A g(aq) + Cl(aq) = A gCl(s)

• Visually forms gray precipitate (Ag2S) and the
yellowish precipitate (AgI) disappears

White ppt
• Visually forms white precipitate (AgCl) again

Effect of Addition of NH3 Left shift will cause the dissolution of

precipitate while right shift will cause its
A g(aq) + Claq) + NH3(aq) = A gCl(s)

formation

NH3 reacts with Ag
A g(aq) + NH3(aq) = [A g(NH3)2 ](aq)

Diamine Silver Ion

(complex ion)

Le Chatelier’s Principle 7
Angeles University Foundation Prelims

B. Saturated NH4Cl Solution

• This equation can be broken down

NH4Cl + H2O = NH4(aq) + Cl(aq) + H2O

• First equation

NH4 + H2O = NH3 + OH

• Second equation

Cl + H2O = HCl + H

• Addition of products will shift he equilibrium of

a chemical reaction to the left thus reforming
the initial reactants

Endothermic Reaction
• In this chemical reaction heat is consumed so
that ammonium chloride can be dissolve in H20
and degrade into ammonium and chloride Ion

• The reaction gives a “cold” feeling because heat

is being utilised as a source of energy for the
reaction to proceed

C. [Co(H2O)6] and [CoCl4]

[Co(H2O)6] + 4Cl = [CoCl4 )] + 6H2O
PINK BLUE

Left Shift Right Shift

Addition of Water Addition of HCl

Decrease Temperature Increase Temperature

Cobalt Chloride when heated, removes

water in the solution and precipitates
Cobalt Chloride into anhydrous form

A+B C+D

Left Shift Right Shift

Increase in Reactants Increase in Products

Decrease in Temperature Increase in Temperature

Le Chatelier’s Principle 8