尼龙6的半微米级GPC分析

为了对尼龙（一种聚酰胺合成纤维）进行室温分析，将样品溶解在六氟异丙醇（HFIP）中进行样品制备。然而，最近HFIP的成本增加使该分析更加昂贵，并且HFIP被认为对环境不友好。半微分离的使用通过减少流动相的消耗对于这类应用具有显著的优势。为了减少分析时间和溶剂消耗，用于快速分析的较小柱尺寸现在可用于GPC分析。在本报告中，使用LC-4000系列RHPLC系统和RI-4035折射率检测器对尼龙6薄膜和纤维进行测量，该检测器设计用于提供高性能分析的半微GPC柱。所使用的溶剂为每个分析循环约8mL，并且与传统分析相比节省了75%的溶剂。使用ChromNAV GPC计算平均分子量，并使用聚甲基丙烯酸甲酯（PMMA）标准构建分子量校准曲线。Application Note 2/5Analysis of Nylon 6 by Semi-micro Scale GPC Analysis of Nylon 6 by Semi-micro Scale GPC I ntroduction For the room temperature analysis of Ny l on (a pol y amide synthetic f iber)， sample preparati o n is made by disso l ving samples in hexafluoroisopropanol (HF I P). However， a recent cost increase in HFIP ha s made this anal y sis more expensive and HFIP i s considered environmentally unfriendly. The use of semi-micro separations has a sig n ificant advantage for t his type of application by reducing the consumption of m obile phase. To reduce analys i s t ime and solvent consumption， smaller column sizes for rapid analysis are now available for use w i th GPC analysis. In this repor t ， t he measurement of Nylon 6 fi lms and f ibers was performed using the LC-4000 Series RHPLC system with RI -4035 refractive index detector designed for use wi t h semi -micro GPC columns offer i ng high performance analysis. The solvent used is approximately 8mL pe r analysis cycle and represents a 75%so l vent saving compared with conven t ional analysis. The average molecular weight was calculated using ChromNAV-GPC， and a molecular weight calibration curve was constructed using a polymethy l methacrylate (PMMA) standard. Keyword： Nylon 6， HFIP， semi -micro sca l e， PMMA， GPC， Ref r active index detector， Molecular weight dis t ribution program ChromNAV-GPC Experimental Ny l on 6 [Equipmen t ][Condi t ions]Pump： PU-4185Column：2x Shodex LF-404 (4.6mml.D. x250mmL，Autosampler： AS-41506pm each)*1(100 uL Sample Loop)Eluent：5 mM Sodium tri f l uoroacetate in HFIP*2Column oven： CO-4060Flow rate：0.2 mL/min Detector： RI-4035Column temp.：40°℃Injection volume：20 pL Structur e Sta n dard Sample：Sugar a l coh o ls mi x ture (5 mg/mL each) Calibra t ion stand a rds for GPC： PMMA standards mixture (0.025 (w/v)% each in eluent) PMMA STD (1)； Mp 1520000，211000，21700， 2200 PMMA STD (2)； Mp 772000， 51900，6900，645 Sample： 0.1 (w/v)% Nylon 6 film and fiber in eluent *1 The column d e dicat e d for us e with TH F was r epl aced b y H FIP. Results Fig.1 Chromatograms of PMMA standard . Figure 1. Chromatogram of PMMA stand a rd (The values on the chromatogram ind i cate the Mp ， peak top m olecular weight， for each PMMA standard) Fig. 2 shows the molecular weight calibration curve using PMMA standard. Fig. 3 d i splays the chromatogram of Nylon 6 f ilm and molecular weight calibration curve， and its molecular weight distribution curve i s in Fig. 4. F i g. 5 i s the chromatogram of Nylon 6 fiber and molecu l ar weight calibration curve， and its molecular weight distribution curve is in Fig. 6. Table 1 shows the result of each average molecular weight calculation converted to PMMA. Figure 2 Mo l ecular we i ght cal i bration curve by the PMMA standard. Figure 3 Chromatogram of Nylon 6 f ilm and molecula r weight calibration curve (The values i ndicate each Mp conve r ted by PMMA) Applicatio n Library： http：//www.j ascoinc .com/appl i c a t i ons Figure 4 Molecul a r we i ght dist r ibut i on c u rve of Nylon 6 f ilm Figure 5 Chromatogram of Nylon 6 fiber and molecular we i g h t calibration curve (The i nt e grated indicate each Mp convert e d by PMMA) Figure 6 Molecular weight distribution c u rve of Nylon 6 fiber JASCO INC. Applicatio n Library： http：//www.j ascoinc .com/appl i c a t i ons Table 1 Average molecular weight calculation o f Nylon 6 film and f iber converted by PMMA Mn Mw Mz Mv Mw/Mn Mz/Mw Film 16570 70258 130381 70258 4.24 1.86 Fiber 12854 40210 69148 40210 3.13 1.72 7003-J014A PU-4185 RHPLC Semi-micro Pump (Base Unit) 7021-J002A CO-4060 Column Oven 7031-J002A RI-4035 Refractive Index Detector， for Semi-micro LC 7058-J011A BS-4000-1 Bottle stand 6688-H564A LC-Net CG cable (3x) 7059-J012A ChromNAV Ver.2 Chromatography Data System 7001-H403A RHPLC/UHPLC Start Up Kit for LC-4000 7001-H405A Maintenance tool kit 2x Shodex GPC LF-404 (4.6 mml.D. x250 mmL，6 pm)