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On the use of Modulated Temperature Differential Scanning Calorimetry to assess wax crystallization in crude oils

机译：关于使用调制温差扫描量热法评估原油中蜡的结晶

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In this paper, measurements of the Wax Precipitation Temperature (WPT) of waxy crude oil samples by a type of Modulated Temperature Differential Scanning Calorimetry, commercially termed StepScan (TM) (SSDSC), are reported. Repeatable and reliable measurements of WPT by SSDSC are found to depend on specific experimental cooling parameters used with this technique. When appropriate parameters are used, two exothermic peaks can be detected on the non-reversing component and one peak on the reversing component (RC) of SSDSC thermograms. We also present indications that the onset of the peak on RC is related to the change in phase angle detected by sinusoidal temperature modulation programs and that it likely does not correspond to a measurement of the WPT. Additionally, by further adjusting SSDSC experimental parameters, because SSDSC is not based on a sinusoidal temperature modulation, reproduction of SSDSC cooling programs by rheometry and Polarized Light Microscopy (PLM) is possible. It was found that the different values used for the SSDSC cooling parameters, when reproduced on the rheometer, do not impact the oil's rheology significantly at the applied shear rate. Moreover, it is shown that the onset of the peak detected on the RC portion of SSDSC thermograms is associated with a significant increase in average wax crystal number, as indicated by microscopy; while the consequences on average wax crystal size are found to depend on the initial cooling temperature. Furthermore, comparisons of WPT determination by SSDSC and by conventional DSC analysis show the potential of SSDSC in obtaining comparable and more reliable WPT measurements depending on crude oil composition and SSDSC cooling parameters. (C) 2017 Elsevier Ltd. All rights reserved.
机译：在本文中，报告了通过一种调制温度差示扫描量热法（商业上称为StepScan（TM）（SSDSC））测量蜡质原油样品的蜡沉淀温度（WPT）。发现SSDSD对WPT的可重复和可靠的测量取决于该技术使用的特定实验冷却参数。当使用适当的参数时，可以在SSDSC温度记录图的不可逆分量上检测到两个放热峰，而在反向分量（RC）上检测到一个峰。我们还提出了这样的迹象，即RC上峰值的出现与正弦温度调制程序检测到的相角变化有关，并且它很可能与WPT的测量不符。另外，通过进一步调整SSDSC实验参数，由于SSDSC并非基于正弦温度调制，因此可以通过流变法和偏振光显微镜（PLM）复制SSDSC冷却程序。已经发现，当在流变仪上再现时，用于SSDSC冷却参数的不同值不会在施加的剪切速率下显着影响油的流变性。而且，如显微镜所显示的，表明在SSDSC热分析图的RC部分上检测到的峰的出现与平均蜡晶体数的显着增加有关。而发现平均蜡晶尺寸的后果取决于初始冷却温度。此外，通过SSDSC和常规DSC分析确定WPT的比较表明，根据原油成分和SSDSC冷却参数，SSSC在获得可比较且更可靠的WPT测量中的潜力。 （C）2017 Elsevier Ltd.保留所有权利。

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