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Analytical Chemistry
2A Selecting and Handling Reagents and Other Chemicals
NIST (The National Institute of Standards and Technology)
Primary-Standard Grade
in addition to extraordinary purity and the assay is printed on the container label.
reference standards, complex substances that have been exhaustively analyzed.
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2C Evaporating Liquids
Fig. 2-1
Arrangement for the evaporation of a liquid
2D Measuring Mass
2D-1 Types of Analytical Balances
Max. capacity Precision
at max. capacity
Analytical balance 1 g to few kg 1 part in 105~106
Macrobalance 160 to 200 g 0.1 mg
Semimicroanalytical balance 10 to 30 g 0.01 mg
Microanalytical balance 1 to 3 g 0.001 mg (1g)
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buoyancy error : weighing error that develops when the object being weighed has a
significantly different density than the weights.
-0.10
Ex. 2-1
A bottle weighed 7.6500 g empty and 9.9700 g after introduction of an organic
liquid with a density of 0.92 g-cm-3. The balance was equipped with stainless steel
weights (d = 8.0 g-cm-3). Correct the mass of the sample for the effects of
buoyancy.
mass of the liquid = 9.9700 - 7.6500 = 2.3200 g.
0.0012 0.0012
W1 = 2.3200 + 2.3200( ) = 2.3227 g
0.92 8.0
Temperature Effects
1. a buoyant effect on the pan and object
2. warm air trapped in a closed container weighs less than the same volume at a
lower temperature.
Both effects cause the apparent mass of the object to be low.
Allow heated objects to return to room temperature before being weighed.
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Fig. 2-6
Effect of temperature on weighing data.
Absolute error in mass as a function of lime
after the object was removed from a 110C
drying oven. A: porcelain filtering crucible.
B: weighing bottle containing about 7.5 g of
KC1.
0 10 20
Time after removal from oven, min
A
2E-2 Desiccators and Desiccants
Oven drying is the most common way.
Desiccatora device for drying substances or objects.
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Fig. 2-8
Components of a typical desiccator. The
base contains a chemical drying agent.
Desiccator plate
Ground-glass
surfaces Desiccant: chemical drying agent, such
as anhydrous calcium chloride, calcium
sulfate (Drierile), anhydrous
magnesium perchlorate (Anhydrone
or Dehydrite), or phosphorus
pentoxide.
Desiccant
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2. Filtering Crucibles
Containers + filters
Sintered-glass (frittled-glass) crucibles:
fine, medium, and coarse porosities
(marked f, m & c). (200C)
3. Filter Paper
Ashless: (9- or 11-cm) leave a residue 0.1 mg
Table 2-1 Comparison of Filtering Media for Gravimetric analyses
Gooch
Glass Porcelain Al2O3
Characteristic Paper crucible,
crucible Crucible crucible
Glass Mat
Speed Slow Rapid Rapid Rapid Rapid
Convenience Troublesome, Convenient Convenient Convenient Convenient
and ease of inconvenient
preparation
Max. ignition None >500 200-500 1100 1450
temp. C
Chemical C (reducing Inert Inert Inert Inert
reactivity properties)
Porosity Many Several Several Several Several
available available available available available
Convenience Satisfactory Unsuitable; Unsuitable; Unsuitable; Unsuitable;
with gelatinous filter tends filter tends filter tends filter tends
precipitate to clog to clog to clog to clog
Cost Low Low High High High
4. Heating Equipment
Oven: max. temp ranges from 140 to 260C; for many ppts: 110C .
Microwave laboratory ovens: shorten drying cycles.
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2F-2 Filtering and Igniting Precipitates
Preparation of Crucibles
Filting and Washing Precipitates
decantation, washing, and transfer
Fig. 2-12 (a) Washing by
decantation. (b)
transferring the
precipitate.
Decantation: pouring a
liquid gently so as to not
disturb a solid in the
bottom of the container.
Do not permit a gelatinous precipitate to dry until it has been washed completely.
Fig. 2-16 Train for vacuum filtration. The trap isolates the
filler flask from the source of vacuum.
2G Measuring Volume
2G-1 Units of Volume
liter (L), milliliter (mL)
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2G-2 The Effect of Temperature on Volume Measurements
The coefficient of expansion: 0.025%/C, standard temp: 20C
Ex. 2-2 A 40.00-mL sample is taken from an aqueous solution at 5C. What
volume does it occupy at 20C?
0.025%
V20o = V5o + (20 5)(40.00) = 40.00 + 0.15 = 40.15mL
100%
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Fig. 2-19
Burets:
(a) glass-bead valve,
(b) Teflon valve
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2G-6 Directions for Using a Buret
1. Cleaning
2. Lubrication of a Glass Stopcock
3. Filling
4. Titration
Buret readings should be estimated to the nearest 0.01
mL.
Ex 2-3 A 25-mL pipet delivers 24.076 g of water weighed against stainless steel
mass at 25 C. Calculate the volume delivered by this pipet at 25 C and 20C.
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