UNIVERSITY OF ENGINEERING AND TECHNOLOGY
Submitted to:
Dr. Nida Iqbal
Assistant professor
Department of Biomedical
UET Lahore
Submitted by:
IRAJ FATIMA
2017-BME-46
Assignment:
Lab report 5
Department:
Bio Medical Engineering
LAB REPORT 5
(Make a Pallets of Ceramic Powder using Hydraulic Press)
OBJECTIVE:
To make a pellets of ceramic powder by using hydraulic press.
APPARATUS:
Figure 1 Hydraulic press Figure 2 Ceramic podwer
THEORY:
M
Sample Preparation for Pressed Pellets:
The process of making pressed pellets for XRF analysis includes grinding the sample to a fine
particle size, mixing it with a binder/ grinding aid in a grinding or mixing vessel, pouring the
mixture into a pressing die and pressing the sample at a pressure of between 15 and 35T. The
resulting pellet or tablet is then ready for analysis. While this is a common and relatively
straightforward approach to preparing samples for XRF analysis, there are several important
aspects that should be considered when designing a sample preparation protocol. These include
the particle size of the sample, the choice of binder, the dilution ratio, the amount of pressure
applied to the sample and the thickness of the final pellet. An additional consideration is sample
contamination.
Binder:
The sample binder is literally the glue that holds the sample together. The optimal binder is
usually a cellulose/wax mixture that homogenizes with the sample during grinding and will
recrystallize under pressure to bind the sample together. These binders are available under
various commercial names but are generally similar. Sometimes acrylic binders are used, but
these are difficult to homogenize with a sample in a mill and need to be mixed by hand. Some
binder grinding agents are available as pre-mixed pellets that can be automatically added to a
mill during grinding.
Dilution:
The amount of binder added to a sample is an important consideration because it dilutes the
sample and must also be added in the same proportion to every sample in order to avoid dilution
errors. Since most modern XRF instruments provide substantial intensity for major elements it is
safe to use a significant amount of binder in order to insure a good strong pellet. Weak pellets
run the risk of breaking in the spectrometer potentially causing damage to the instrument. A 20-
30% binder to sample ratio will almost always produce a very strong pellet that can be dropped
onto the ground from a half a meter without breaking. If consumable costs are a concern, a lower
binder/sample ratio can be used with some experimentation in order to determine the optimal
dilution level.
Pressure:
Once a sample and binder are mixed, the material is pressed in a die using a hydraulic sample
press. The pressure applied to a sample should be sufficient to compress the sample completely
and recrystallize the binder. One of the most important factors is making sure that the sample is
fully compressed so that no void spaces remain in the pellet. A pellet may look good but still
contain void spaces which can result in a lowered intensity for lighter elements. You should
experiment with your samples using increasing pressure until the intensity for the light elements
reaches a maximum and stabilizes. Most samples will reach this maximum at 25-35T of pressure
applied for 1-2 minutes. It's also important to release the pressure applied to a sample slowly to
prevent cracking of the sample surface.
PROCEDURE:
Take 0.5g of powdered form ceramic and put it on the plate to weight it.
Then put the plate in electrical balance.
Placed the powder inside the filler of Hydraulic jack.
Pressing the work to be pressed centrally on the lower bolster face.
Lower top bolster pressing face, by turning the lead screw handle clockwise.
Pull and push the pump handle to smoothly build up pressure.
Applied a pressure of 50 Bar through piston.
Waited until it comes to its previous reading (original) pressure.
To release the pressure load, turn the pressure release handle anticlockwise by one
turn.
Turn the lead screw handle anticlockwise to raise the pressing face, then remove the
work from inside.
Now checked the space filler, powdered shape ceramic was converted into pellet
shape.
Measured its diameter.
Weighed it again after making pallet.
OBSERVATION:
Weight before making pallet = 0.50g
Weight after making pallet = 0.49g
Diameter of pallet = 12.81mm
Volume= 0.136m^3
Density of ceramics = 3.6gm^-3
RESULT:
We get this type of shape
Pallet of ceramic powder
DISCUSSION:
The easiest way is to make the PVA solution (5-10%) with water. Add few drops of the solution
in your powder and then mix them with mortar and pestle. After that it will be agglomerated. So,
you should sieve it to get the fine powder. Now you can compact it in a die. Don't forget to
lubricate the internal walls of the die with some lubricating agents such as zinc stearate so that
sample may not stick the walls and can be removed easily. It will affect the porosity, if you will
increase the amount of the binder, but it is not too much because you are adding very few drops.
CONCLUSION:
The most common contributors to error in the preparation of pressed pellets include the particle
size of the sample, the choice of binder, the dilution ratio, the amount of pressure applied to the
sample, the thickness of the final pellet and sample to sample cross contamination. The best
practices for limiting this error require good method development coupled with attention to detail
and consistency.
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