Leeman Mats, Islam Mohammad T, Haseltine William G
Cytec Industries Inc., 1937 West Main Street, Stamford, CT 06904, USA.
J Chromatogr A. 2007 Nov 23;1172(2):194-203. doi: 10.1016/j.chroma.2007.10.006. Epub 2007 Oct 10.
The molar mass distributions of ultra-high molar mass polyacrylamide-based flocculants were measured using asymmetrical flow field-flow fractionation (AFFFF) coupled with multi-angle light scattering and refractive index detectors. The mass load onto the separation channel was found to be critical in obtaining a good size separation. The detailed investigation with ultra-high molar mass polyacrylamides found that the injected amount should be </=1microg to ensure separation according to AFFFF mechanism. As a consequence of the limited sample mass load, the signal-to-noise ratio (S/N) of the detector responses was low. To overcome this limitation and thereby to obtain more accurate and precise molar mass and radius information, each sample was injected 10 times and the resulting signals were averaged before calculating the molar mass and radius. In addition, the channel was equipped with a slotted outlet to increase the concentration of sample passing through the detectors. After implementing the above strategies, it was possible to perform separation of polymers having molar mass and size as high as 10(8)gmol(-1) and root-mean-square radius of approximately 250nm, respectively. The resulting weight-average molar mass of the highest MW sample was in excess of 18x10(6)gmol(-1).
采用不对称流场-流分级法(AFFFF)结合多角度光散射和折射率检测器,测定了超高分子量聚丙烯酰胺基絮凝剂的摩尔质量分布。发现分离通道上的质量负载对于实现良好的尺寸分离至关重要。对超高分子量聚丙烯酰胺的详细研究发现,进样量应≤1μg,以确保根据AFFFF机制进行分离。由于样品质量负载有限,检测器响应的信噪比(S/N)较低。为克服这一限制,从而获得更准确和精确的摩尔质量及半径信息,每个样品进样10次,并在计算摩尔质量和半径之前对所得信号进行平均。此外,通道配备了狭缝出口,以提高通过检测器的样品浓度。实施上述策略后,能够分别对摩尔质量高达10⁸ g/mol且均方根半径约为250nm的聚合物进行分离。最高分子量样品的重均摩尔质量超过18×10⁶ g/mol。