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BASIC REQUIREMENTS
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FOR
ANALYSIS
SAMPLING
Sampling is the most critical aspect of an analysis.
The significance and accuracy of the measurements
can be limited by the sampling process.
SAMPLING
Is a process to get
homogeneous sample.
representative
and
CLASSIFICATION OF ANALYSIS
Method
i) Meso
>100
>100
ii) Semimicro
10 100
50 - 100
iii) Micro
1 10
< 50
iv) Ultramicro
<1
ii)
Minor
0.1 1 %
iii)
Trace
< 0.1 %
iv)
SAMPLING
Deciding
1)
2)
3)
sample.
An aliquot of this sample is taken for the analysis sample.
SAMPLING SOLID
Inhomogeneity of the material, make sampling of
solids more difficult.
SAMPLING SOLID
CONING AND QUARTERING
This process is continued until the gross sample is
small enough to be transported to the laboratory.
SAMPLING SOLID
CONING AND QUARTERING
There is no specific technique that can be used for taking the
samples. Using an example, explain how to sample either a solid,
liquid, or gas sample. (5 marks)
Sampling solid
Using the method cone and quarter.
Divide a pile of material into quarter.
Take a sample from each quarter of the pile and crush these
sample and form into a smaller conical pile.
Flatten the conical pile and cut into equal quarters. Two
opposite quarters are chosen at random.
Crush the quarter further.
The whole steps are repeated until a laboratory samples obtain.
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SAMPLING SOLID
TABLET SAMPLER
Designed to take a sample of
tablets and capsules as
containers are filled.
SCOOPER
A stainless steel scoop
with a capacity of 5 oz,
148 ml. Perfect for
sampling powder, soil,
gravel, and other
materials.
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SAMPLING LIQUID
Liquid
If
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SAMPLING LIQUID
Sampling depends on the types of liquids:
BIOLOGICAL FLUIDS
The timing of sampling biological fluids is very
important (blood composition varies before and after
meals)
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SAMPLING LIQUID
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SAMPLING GASES
Tend to be homogeneous.
Large volume of samples is required because of their
low density.
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SAMPLING GASES
Hi-Vol sampler
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3.
4.
5.
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Precipitation
Loss
Loss
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Dry
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DEFINING:
REPLICATE SAMPLES
Replicate
Replicate
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PREPARING SOLUTIONS
OF THE SAMPLE
A solvent is chosen that dissolves the whole
sample without decomposing the analytes
SOURCES OF ERROR
i) Incomplete dissolution of the analyte.
ii)
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1. DRY ASHING
The sample is slowly combusted at a high
temperature (400 700oC) in a muffle furnace.
Atmospheric O2 serves as the oxidant, that is
organic matter is burned off, leaving behind
inorganic residue that is soluble in dilute acid.
Oxidizing aids may be employed.
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1. DRY ASHING
SIMPLE DRY ASHING
no chemical aids.
Pb, Zn, Co, Cr, Mo, Sr, Fe traces can be recovered with little loss by
retention and volatilization.
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1. DRY ASHING
IF THE SAMPLE ARE LIQUIDS AND WET TISSUES:
DRY
ASHING
ADVANTAGES
Simpilicity
Free from
contaminations since
few or no reagents are
added
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DISADVANTAGES
Volatilization of elements
and
losses by retention on the walls
of the vessels.
Adsorbed metals on the
vessel may in turn
contaminate future samples.
2-4 hour are needed for dry
ashing
2. WET DIGESTION
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2. WET DIGESTION
Principle:
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2. WET DIGESTION
Principle:
8. If the organic matter persists, more HNO3 may be
added.
9. Digestion is continued until the solution clears.
10. All digestion procedures must be performed in a
FUME HOOD.
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WET
DIGESTION
ADVANTAGES
Superior in term of
RAPIDITY
Freedom from loss by
retention
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DISADVANTAGES
Introduction of
impurities from the
reagent necessary for
the reaction.
ELIMINATING
INTERFERENCES
Interferences are substances that prevent
direct measurement of the analyte and MUST BE
REMOVED.
May included separation steps:
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i)
Precipitation
ii)
Chromatography
iii)
Distillation
iv)
Dialysis
v)