CH 02

silicate glassware (Pyrex, Kimax) is normally used because it
is thermally stable.
Modern balances are electronic. They still compare one mass against another since they
are calibrated with a known mass. Common balances are sensitive to 0.1 mg.
Fig. 2.1. Electronic analytical balance.

Electronic balances operate
on the principle of emf
compensation – the
compensation current to
bring the pan back to its position
original position is scanner
proportional to the sample
weight.
hanger
coil
temperature
sensor
Fig. 2.2. Operating principle of electronic balance.
The density of brass weights is 8.4 and that of stainless steel weights is 7.8
Weighing bottles are used for drying samples. Hygroscopic samples are weighed by
difference, keeping the bottle capped except when removing the sample.
Fig. 2.3. Weighing bottles.

Volumetric flasks are calibrated
to contain an accurate volume.
See the inside back cover of the
text for tolerances of Class A
volumetric glassware.
Fig. 2.4. Volumetric flask.

Volumetric pipets accurately deliver a fixed volume.
A small volume remains in the tip.
Fig. 2.5. Transfer or volumetric pipets.

Measuring pipets are straight-bore pipets marked at different volumes.
They are less accurate than volumetric pipets.
Fig. 2.6. Measuring pipets.

Syringe pipets precisely deliver microliter volumes.
They are commonly used to introduce samples into a gas chromatograph.
Fig. 2.7. Hamilton microliter syringe.

These syringe pipets can reproducibly deliver a selected volume.
They come in fixed and variable volumes. The plastic tips are disposable.
Fig. 2.8 Single-channel and multichannel digital

displacement pipets and microwell plates.
The DIN error gives the range for which we are 95% confident the delivery will fall.
These accuracies and precisions are typical for single-channel variable volume pipets
A 50-mL buret is marked in 0.1 mL increments.
You interpolate to 0.01 mL, good to about ±0.02 mL.
Two readings are taken for every volume measurement.
Fig. 2.9. Typical buret.

Position the black field just below the meniscus.
Avoid parallax error by reading at eye level.
Fig. 2.10. Meniscus illuminator.

Place the flask on a white background.
Place the buret tip in the neck of the flask while your swirl.
Fig. 2.11. Proper technique for titration.

These are calculated volumes
for 1 gram of water in air at
atmospheric pressure,
corrected for buoyancy with
stainless steel weights.
You can substitute a specific
weight in column B to obtain
the corresponding volume
(web spreadsheet).
Use a desiccator to cool a dried or ignited sample.
Cool a red hot vessel before placing in the desiccator.
Do not stopper a hot weighing bottlle (creates a partial vacuum on cooling).
Fig. 2.12. Desiccator and desiccator plate.

CaCl2 is commonly used.
It needs periodic replacement when wet or caked.
Used to ignite samples at high temperatures, e.g., to dry ash organic matter.
Fig. 2.13. Muffle furnace.

Used to dry samples before weighing.
Usually 110o C used.
Fig. 2.14. Drying oven.

A fume hood is “dirty” since it draws in
laboratory air.
A laminar-flow hood filters air (0.3 m
HEPA filter) and flows it out into the
room.
Use it as a workstation for trace analysis.
Fig. 2.15. Laminar-flow workstation.

Use for filtering non-gelatinous precipitates.
Fig. 2.16. Filtering crucibles: (a) Gooch crucible;

(b) sintered-glass crucible; (c) porcelain filter crucible.
Mount the filtering crucible in a crucible holder
and connect the
filtering flask to a water aspirator.
Fig. 2.17. Crucible holders.

These are ashless filter papers.
They are ignited away after collection of the precipitate.
Use for gelatinous precipitates.
This provides a good seal and prevents air bubbles from being drawn in.
Suction from the weight of the water in the stem increases the filtration rate.
Let the precipitate settle in the beaker before beginning filtration.
Fig. 2.18. Properly folded filter paper.

Decant the solution by pouring down the stirring rod.
After decantiing the mother liquor, add wash water to the precipitate and decant again, repeating 2-3
times.
Then wash the precipitate into the filter.
Fig. 2.19. Proper technique for transfer of a precipitate.

Use this to scrub the walls of the beaker and collect all the precipitate (by washing).
Fig. 2.20. Rubber policeman.

Heat or ignite the crucible to a constant weight (to 0.3-0.4 mg) before adding the
filtered precipitate.
Fold the filter paper over the precipitate.
Drive off moisture at low heat. Then gradually increase heat till the paper begins to char.
After the paper is gone, ignite the precipitate.
Fig. 2.21. Crucible and cover supported on a wire

triangle for charring off paper.
Microwave ovens provide rapid drying.
Acid decomposition times are reduced from hours to minutes.
Lower blank levels are achieved with reduced amounts of reagents.
Fig. 2.22. Schematic of a microwave system.

Use these for acid digestions.
They are tilted while heating to avoid losses from “bumping”.
Fig. 2.23. Kjeldahl flasks.

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silicate glassware (Pyrex, Kimax) is normally used because it

Fig. 2.1. Electronic analytical balance.

Fig. 2.3. Weighing bottles.

Fig. 2.4. Volumetric flask.

Fig. 2.5. Transfer or volumetric pipets.

Fig. 2.6. Measuring pipets.

Fig. 2.7. Hamilton microliter syringe.

Fig. 2.8 Single-channel and multichannel digital

Fig. 2.9. Typical buret.

Fig. 2.10. Meniscus illuminator.

Fig. 2.11. Proper technique for titration.

Fig. 2.12. Desiccator and desiccator plate.

Fig. 2.13. Muffle furnace.

Fig. 2.14. Drying oven.

Fig. 2.15. Laminar-flow workstation.

Fig. 2.16. Filtering crucibles: (a) Gooch crucible;

Fig. 2.17. Crucible holders.

Fig. 2.18. Properly folded filter paper.

Fig. 2.19. Proper technique for transfer of a precipitate.

Fig. 2.20. Rubber policeman.

Fig. 2.21. Crucible and cover supported on a wire

Fig. 2.22. Schematic of a microwave system.

Fig. 2.23. Kjeldahl flasks.

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