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1) Selecting a method
2) Sampling
3) Preparing the laboratory sample
4) Defining replicate samples
5) Preparing of solutions of samples
6) Eliminating interferences
7) Measurement of analyte concentration
8) Calculations
9) Determining reliability of data
Selecting the method
Making your choice: Will the method selected be adequate for the
decision you have to take when the result is available?
Sampling
o Water of constitution
present as H and OH groups which combine to give
H2O
takes higher T to expel from samples
Ex. C6H12O6 6C + 6H2O
Non-essential water superficially held water or water bound to the
sample physically and removed at a much lower T range (100-120oC)
o Adsorbed water retained on surface of solid
o Sorbed water condensed water in interstices of capillaries of
colloidal solids
o Occluded water liquid water entrapped in microscopic pockets
spaced irregularly throughout solid crystals
Common Practices
1) remove moisture from samples prior to weighing or to bring water content
to some reproducible level
2) determine water content at the time samples are weighed for analysis so
that results can be corrected to a dry basis
Example: A food sample analyzed as received, is found to contain 14.57%
protein and 10.4% water. Calculate % protein on a dry basis.
Example: 1.000 gram of soil as received, gave a moisture content of 14.0%.
The oven-dried sample, completely moisture-free, showed 18.00% K. Find
the % K in the sample as received.
Methods of Moisture Determination
1) Application of Heat
a. Drying done to make sample anhydrous or to remove adsorbed
moisture but retain chemically combined water
i. Air-drying
ii. Oven-drying
1. conventional oven
2. vacuum oven 50-100 mm Hg
3. microwave oven
iii. Dessicator
iv. IR lamps
Disadvantages of drying:
Time-consuming
b. Freeze-drying or lyophilization
Oxidizing mixtures
Aqua regia 3:1 mixture of HCl:HNO3
Br2 or H2O2 hasten oxidation of organic materials
HNO3 + HClO4 useful also for organics
Hydrofluoric acid primary use is for decomposition of silicate
rocks and minerals in the determination of species other than
silica
Microwave Decompositions
Elimination of Interferences
Interference arises whenever a species in the sample matrix either
produces a signal that is indistinguishable from that of the analyte or,
alternatively, attenuates the analyte signal
2 Methods:
1) use of a masking agent immobilizes or chemically binds the
interfering species in a form in which it no longer contributes to or
attenuates the signal from the analyte
> Ex. use of F- to prevent Fe3+ from interfering in the iodometric
determination of Cu2+
2) Converting either the analyte or the interferences into a separate
phase that can be separated mechanically
> Most common method: chromatography
> Others: precipitation, extraction, ion-exchange, distillation