Hello, I have little time in the use of a NETZSCH device. Currently I know that the calibration must be done according to the following parameters: gas flow, type of atmosphere, type of crucible and heating rate.
If I usually use alumina crucibles with a lid for my tests, and I now want to perform a test without a lid, will I need to perform a new calibration (temperature and sensivity)?
The DSC instrument should be calibrated at similar experimental conditions to those used with the actual sample; namely, in terms of heating rate and thermal schedule, type of pans, selected gas and its flow rate. If the sample pan is to be used covered with a lid; calibration should be made also with the (empty) sample pan covered with a lid. If the sample pan is to be used sealed; calibration should proceed accordingly. That follows the concept of a blank essay. You may usually consider to calibrate the instrument either with both pans empty, or with the reference filled with inert (standard) substance, often powdered calcined α-alumina ─ in principle using the same initial mass that would be used for the sample. The reference used for the actual run (with the sample) may be either the empty reference pan, or that same pan filled with the inert (standard) substance. This kind of calibration chiefly aims to correct the thermogram baseline. DSC instruments can also be calibrated for temperature accuracy. Heat-flux based DSC instruments should be also calibrated for their calorimetric scale, with selected standard substance(s); that may be not strictly required for power-compensated DSC instruments. Other calibration directives may possibly apply to the actual instrument being considered, or to specific types of analysis.
Yes please calibrate under identical condition. Also please read.
Pure & Appl. Chem., Vol. 67, No. 11, pp. 1789-1800, 1995.
As you mentioned, you have less time to perform the test, you can use the existing calibration by keeping all other parameter constant, like: purge gas type, heating rate, identical reference pan and sample holding pan and keep both the pan open to maintain the identical condition. Hope it will work for you. But always it is recommended to perform new calibration.
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