Of course it is possible to test liquid samples in hermetic closed sample pans in a DSC. There is no problem to see transitions, melting and Tg for such substances and to measure the heat capacity. You should however take care to be enough away from the boiling point to avoid burst of the pan. Furthermore you should test the tightness of the pan by comparing the mass before and after the run to see whether possible evaporation has occurred. I usually tested the liquid substance in the same temperature range in a TGA first to see whether there are components in the liquid which would evaporate at elevated temperatures. The heat of evaporation could possibly lead to a falsification of the DSC result. Good luck!
It is not clear what kind of TE analysis you are talking about (decomposition?). Model of device is alos important... I general it is possible to use liquid oils or waxes Be careful wil liquid oil, because they can escape from your pan and contaminate the cell, however, if you are making any decomposition test in DSC it does not matter.
In this case I do not see any problems with experiment. Just check the pan and lid after hermetization carefully. Do not forget to specify cooling rate (problem of recrystallization during heating afterwards).
DSC is a thermoanalytical technique in which the difference in the amount of heat required to increase the temperature of a sample and reference is measured as a function of temperature. Both the sample and reference are maintained at almost same temperature throughout the experiment.
I have done the DSC for the powders samples. I am not sure about the liquid but there are many reports about the liquid crystals.
Using DSC, it is possible to observe the small energy changes that occur as matter transitions from a solid to a liquid crystal and from a liquid crystal to an isotropic liquid.
Of course it is possible to test liquid samples in hermetic closed sample pans in a DSC. There is no problem to see transitions, melting and Tg for such substances and to measure the heat capacity. You should however take care to be enough away from the boiling point to avoid burst of the pan. Furthermore you should test the tightness of the pan by comparing the mass before and after the run to see whether possible evaporation has occurred. I usually tested the liquid substance in the same temperature range in a TGA first to see whether there are components in the liquid which would evaporate at elevated temperatures. The heat of evaporation could possibly lead to a falsification of the DSC result. Good luck!
G. W. H. Höhne, Actually I will test some PCM material in DSC so may be I will set the temperature -20 to +30 only. I think boiling point of PCM's are not near about set temperature.
I advise you to test the sealing oh the pan before any DSC experiments, on a heating plate for exemple or in à furnace. I've experienced some dramatic leakages with inorganic PCMs which actually broke the furnace of the calorimeter.
Do not buys cheap pans from third vendor. Buy directly from the vendor of the instrument such as TA, Instruments or Perkin Elmer. Quality of pans varies with suppliers.
As mentioned above, you can easily do the DSC study using cooling upto minimum 20 degreeC below Tg. If the handling of liquid is a problem, use inert salt, Al2O3, SiO2 etc., which will not show any transition in the region, to soak the liquid and carry out the scan.
DSC technique can be used also for studying transformations in weakly volatile liquids, otherwise the signal will reveal mainly the vaporisation phenomenon which is accompanyed by an endothermal effect very large in comparison to that acoompanying the transformation appearing in the liquids.
Thanks all for your valuable answers. I have done successfully the DSC of liquid sample using TA aluminium pan and lid. I don't face any kind of problem. Important factor is set the temperature limit is below 100 for safe analysis. High temperature may affect the condition of analysis.
I did my DSC analysis of liquid without using any absorbent however my temperature range is only -50 to 50. If you set DSC temperature near to boiling point of liquid it will dangerous better to use absorbent. If set temperature is not near to boiling point then It's OK to use without absorbent.
Dear Samir Bhargava, of course it is possible to make DSC measurements of oils with adsorbent, but you should have in mind, that the result cannot be compared directly with the measurement of pure oil because of the following reasons: There may be an interaction between the oil and the adsorbent resulting in a different behavior. The desorption of oil during heating may be visible as en thermal effect. The vapor pressure may be influenced and with it the boiling/evaporation temperature. Furthermore it may happen, that the oil "creeps" from the pan into the measuring cell of the DSC and pollute the DSC. The heat capacity of the oil may be changed by the interaction with the adsorbent. I recommend to use hermetic closed pans even for the adsorbed oil to avoid evaporation heat effects and pollution. Good luck!
Dear Samir Bhargava, of course it is possible to make DSC measurements of oils with adsorbent, but you should have in mind, that the result cannot be compared directly with the measurement of pure oil because of the following reasons: There may be an interaction between the oil and the adsorbent resulting in a different behavior. The desorption of oil during heating may be visible as en thermal effect. The vapor pressure may be influenced and with it the boiling/evaporation temperature. Furthermore it may happen, that the oil "creeps" from the pan into the measuring cell of the DSC and pollute the DSC. The heat capacity of the oil may be changed by the interaction with the adsorbent. I recommend to use hermetic closed pans even for the adsorbed oil to avoid evaporation heat effects and pollution. Good luck!
Dear Samir Bhargava, of course it is possible to make DSC measurements of oils with adsorbent, but you should have in mind, that the result cannot be compared directly with the measurement of pure oil because of the following reasons: There may be an interaction between the oil and the adsorbent resulting in a different behavior. The desorption of oil during heating may be visible as en thermal effect. The vapor pressure may be influenced and with it the boiling/evaporation temperature. Furthermore it may happen, that the oil "creeps" from the pan into the measuring cell of the DSC and pollute the DSC. The heat capacity of the oil may be changed by the interaction with the adsorbent. I recommend to use hermetic closed pans even for the adsorbed oil to avoid evaporation heat effects and pollution. Good luck!
Dear Samir Bhargava, of course it is possible to make DSC measurements of oils with adsorbent, but you should have in mind, that the result cannot be compared directly with the measurement of pure oil because of the following reasons: There may be an interaction between the oil and the adsorbent resulting in a different behavior. The desorption of oil during heating may be visible as en thermal effect. The vapor pressure may be influenced and with it the boiling/evaporation temperature. Furthermore it may happen, that the oil "creeps" from the pan into the measuring cell of the DSC and pollute the DSC. The heat capacity of the oil may be changed by the interaction with the adsorbent. I recommend to use hermetic closed pans even for the adsorbed oil to avoid evaporation heat effects and pollution. Good luck!
In DSC we can use liquid samples. For liquid samples we have to use high volume cells called Hermitic cells (pans) and the crimp cover should have a hole.
DSC can be done to identify the melting temperature, enthalpy of fusion and transition etc for solid samples. You can use TA aluminium sample pans for the same.