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影响DSC分析结果的主要因素(The main factors influencing the analysis results of DSC)
影响DSC分析结果的主要因素(The main factors influencing the analysis results of DSC)
The main factors influencing the analysis results of DSC
1. The sample weight
The sample size is small, the sample has high resolution, but the sensitivity declines, and the sample size is generally adjusted according to the sample heat effect size, generally 3 ~ 5mg.
On the other hand, the amount of samples affected the temperature measured. With the increase of sample size, the initial temperature of the peak is basically unchanged, but the peak temperature increases, and the temperature of the peak ends is also increased, so if the same sample is to be different from each other, it is best to use the same amount.
2. Heating rate
The rate range is usually 5 ~ 20 degrees/min. Generally speaking, the faster the heating rate, the higher the sensitivity and the lower resolution. The sensitivity and resolution are a pair of contradictions, people generally choose slower heating rate to maintain good resolution, and appropriately increase the sample size to improve the sensitivity.
In general, as the heating rate increases, the initial temperature of the melting peak changes little, while the peak and peak end temperature rise, and the peak becomes wider.
3. The atmosphere
Generally, inert gases such as nitrogen, argon, helium, etc., will not produce the peak of oxidation, while reducing the corrosion of the sample volatiles to the monitor. The flow velocity must be constant (such as 10ml/min), or it will cause baseline fluctuations.
The nature of the gas has a significant influence on the determination of the gas. Such as helium gas thermal conductivity than that of nitrogen and argon gas thermal conductivity is about 4 times, so doing the DSC using helium as shielding gas of low temperature and cooling speed, shorten test time, but because the helium gas thermal conductivity high, lower the peak detection sensitivity, is about 40% of the nitrogen, therefore, when the heat is measured in the heli
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