Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
Reagents:
None.
Safety Precautions:
Use standard precautions when working around electrical equipment or
glassware.
Make sure that all electrical equipment is properly grounded and installed and
maintained by qualified electricians.
Procedure:
Hot Weigh Method
1. If only moisture is to be determined on the sample, use an aluminum dish. If
ash determination is to follow on the dry matter residue, use a porcelain
crucible. Dry the appropriate containers and three empty crucibles or dishes to
be used for warming balance at 100oC (or 105oC) for at least 2 hr.
2. Warm balance by sequentially placing the three empty crucibles or dishes on
balance for 20 sec each.
3. Removing one at a time from the oven, weigh container (W4), recording weight
to nearest 0.1 mg. Weigh rapidly, recording minimum weight (as soon as
balance has stabilized, usually within 15 sec after removing from oven).
Whenever weighing is interrupted, balance should be re-warmed according to
step (2).
4. After all containers have been weighed, allow balance and sample containers to
cool.
5. Tare empty container to zero and weigh (W7) approximately 2 g ground sample
into each container or weigh approximately 2 g into each container and record
weight of sample and container (W5) to nearest 0.1 mg.
6. Shake container gently to uniformly distribute the sample and expose the
maximum area for drying.
7. Place samples into an oven which has been preheated to 100oC (or 105oC) for
at least 3 hr. Oven should return to temperature within 1 hr after samples in
containers have been placed into it.
5. Shake dish or crucible gently to uniformly distribute the sample and expose the
maximum area for drying.
6. Place samples (with covers removed to the side) into oven that has been
preheated to 100oC (or 105oC) at least 3 hr prior to use. Oven should return to
temperature within 1 hr after samples have been placed into it.
7. Leave uncovered samples in oven for 24 hr at 100oC or 16 hr (or overnight) at
105oC.
8. Move samples to desiccator and place cover on each container as it is
transferred. Seal desiccator and allow to cool for at least 1 hr but not more than
2 to 3 hr.
9. Weigh container with cover and dried sample (W6), recording weight to nearest
0.1 mg.
Comments:
Samples should be placed in drying oven so that air can circulate freely.
Containers should not touch each other.
Desiccator seals should be kept clean and well greased and the lid should
always slide easily on or off. If the lid "grabs," it is time to remove the old
grease and apply fresh lubricant.
Open a loaded desiccator very slowly after samples have cooled. A vacuum
forms during cooling and abrupt opening results in turbulence which can blow
samples out of uncovered containers.
Slide the desiccator lid open. Do not place the lid on the countertop with the
grease side down. The grease will pick up dirt, preventing formation of a seal.
If a lid can be directly lifted off the desiccator, either the desiccator was not
properly sealed or, more likely, it needs fresh lubricant.
Rubber stoppers in the lid should always be pliable.
Sample dishes should not be packed excessively tight in a desiccator. Air
movement is necessary to cool sample dishes. Dishes should not touch each
other.
confidence limits warn of possible problems with the analytical system. Results
outside the 99 percent confidence limits indicate loss of control, and results of the run
should be discarded. If more than five or six points in succession fall on one side or
the other of the 50 percent line, it is a strong indication that something has changed
and is cause for investigation.