Cbm 40 system controller

To confirm that the principal peak obtained in the radiochemical purity measurement was that of [²¹¹At]At⁻, LC-MS analysis was performed on the radioactive solution obtained using the same procedure as that in the 3-lot tests. This analysis was performed using an LCMS-9030 system including the CBM-40 system controller, SPD-M40 photodiode array detector, CTO-20AC column oven, SIL-20ACHT autosampler, LC-20AD pump and DGU-405 degasser, Shimadzu, Kyoto, Japan and a radioactivity detector (Gabi-Nova) connected in front of the MS introduction. The Shodex HILICpak VT-50 2D (Resonac, Tokyo, Japan) 150 mm × 2.0 mm analysis column was used with a mobile phase containing 50 mM ammonium formate/acetonitrile (20/80). The flow rate and the column oven were set at 0.3 mL/min and 40 °C, respectively.

GPC analysis of polymers obtained in solution was performed using a Shimadzu modular system consisting of a CBM-40 system controller, RID-20A differential refractive-index detector, a SIL-20AHT automatic injector, and three PSS GRAM combination columns made of stainless steel (V4A) with pore size: 100 Å, 3000 Å (2 columns), and one precolumn, with the temperature at 30 °C by a CTO-20A oven. The eluent in chromatographic separation was N,N-Dimethylformamide (HPLC grade with 0.01% w/v LiCl) with the flow rate set at 1 mL min⁻¹. A molecular weight calibration curve was created with the application of monodispersed polystyrene standards (PSS, Polymer Standards Service). The apparent molecular weights (MWs) and molecular weights distributions (MWD) were determined using GPC Postrun Analysis software provided by Shimadzu Corporation.

The Varian (Palo Alto, CA, USA) Mercury Plus 400 MHz and VNMRS 600 MHz FT-NMR spectrometers provided the NMR spectra. HRSIMS was performed by using a Bruker APEX II spectrometer (Bremen, Germany). The V-650 spectrophotometer from Jasco (Tokyo, Japan) was utilized to measure the UV data. For measuring infrared data, the Jasco FT/IR-4X spectrophotometer was selected. Circular dichroism data were recorded using a Jasco J-815 CD spectrometer. A Jasco P-2000 polarimeter was used to quantify specific optical rotation. Merck KGaA (Darmstadt, Germany) silica gel 60 (0.015–0.040 mm) was utilized to pack columns. For high-performance liquid chromatography (HPLC), Phenomenex (Torrance, CA, USA) C18, phenyl-hexyl, and biphenyl columns were utilized. The LC-40D solvent delivery module, DGU-405 de-gassing unit, CBM-40 system controller, CTO-40S column oven, SPD-M40 photo diode array detector, and FRC-10A fraction collector made up the Shimadzu (Kyoto, Japan) HPLC apparatus.