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Analytical Chemistry:

The Science of Analysis.

Introduction
Aspects of Analytical Science
Analytical Chemistry:
The Science of Analysis.

• Objectives: separation, identification and


determination of the relevant components
within a sample matrix.
Analytical Chemistry:
The Science of Analysis.

• Objectives: separation, identification and


determination of the relevant components
within a sample matrix.

 Qualitative analysis
Analytical Chemistry:
The Science of Analysis.

• Objectives: separation, identification and


determination of the relevant components
within a sample matrix.

 Qualitative analysis
 Quantitative analysis
Aspects of Analytical Science
• Obtaining a sample –
– Representative, integrity, identification

Population

Sample
Aspects of Analytical Science
• Accurate record keeping
– Sample storage, labelling, workbooks.
Aspects of Analytical Science

• Measurement and uncertainty


– Accuracy & precision of analysis
Measurement of Uncertainty
Significant Figures
• The number of certain digits and the first of the uncertain
digits.

Rules for Significant Figures


• In a product or quotient the number of significant figures
equals that of the datum containing the least number of
significant figures.
e.g. 4.197 x 2.1 = 8.8137  8.8

Question: How many significant figures are there in the


following?
5.12 x 4.978
0.01 x 2.12
Measurement of Uncertainty
Significant Figures
• The number of certain digits and the first of the uncertain
digits.

Rules for Significant Figures


• In a sum or difference, the value that terminates in the
highest decimal level determines the number of
significant figures.
e.g. 264.7 – 24.145 = 288.845  288.8

Question: How many significant figures are there in the


following?
64 + 4.978
1.234 + 2.12
Rounding off.
• Last digit is unchanged if digit to be removed is
<5
• Last digit is increased if digit to be removed is >
5
• Round to an even if digit to be removed = 5.
Method Description
• Pay Attention to the language of the experimental:
informs you of -
– the equipment required.
– the level of accuracy in preparation.

• Prepare 250 mL of a 0.04 M solution of NaOH by


suitable dilution of a stock 2 M NaOH solution.

This is a qualitative
1 significant preparation – so use a
figure measuring cylinder and
storage bottle or beaker
• Weigh approximately 1.0 g (0.0001 g) of KHP into a
weighing boat then quantitatively transfer your sample of
KHP into a 100 mL volumetric flask. Make up to the mark
with distilled water.

The mass must be known


4 decimal to 4 decimal places so
places measure using an
analytical 4 decimal place
balance – quantitative.
• Transfer a 25.00 mL aliquot of the KHP solution into a
250 mL conical flask. Add 2 drops of phenolphthalein
indicator and titrate with the standardised NaOH solution
until the pink color persists for approximately 30
seconds.
4-significant figures
requires the transfer to be
4 Significant
undertaken using a
Figures pipette
Laboratory notebook
• Detailed description of what was done and what was
observed.

• Must contain sufficient information to be understood


even several years later.

• Allows others to reproduce your experimental results.

• Record in your notebook experimental procedure,


quantities and times, names of computer disks and file
names of data stored. Printed copies of results (graphs
etc.) should be pasted into the note book.
Chemicals.
• Analytical reagent grade (AR)
Chemicals.
• Inferior grade CP, LR, Technical, or BP
Chemicals.
• Special High Purity: BDH Aristar, Merck
Suprapure, Spectroscopically pure HPLC grade.
Chemicals.
• A primary standard substance is a substance
whose purity is such that it can be weighed out
and made up to volume to give a solution of
known concentration.

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