Materials and Reagents

1. Absolute ethanol (99.5%) (EMD Millipore, catalog number: 107017 )
   
2. Toluene (99.5%) (Merck KGaA, catalog number: 107019 )
   
3. Acetylacetone (99%) (Merck KGaA, catalog number: 109600 )
   
4. Dioxane (99.5%) (Merck KGaA, catalog number: 109671 )
   
5. Fuming hydrochloric acid (37%) (Merck KGaA, catalog number: 101834 )
   
6. Methanol (99.8%) Merck KGaA, catalog number: 107018 )
   
7. Ultrapure water
   Note: It is produced by Millipore Simplicity^® 185 (UV)  ultrapure water purification system (EMD Millipore).
   
8. Pyridine (99.5%) (Merck KGaA, catalog number: 109728 )
   
9. Phenyl isocyanate (99%) (Merck KGaA, catalog number: 107255 )
   
10. Tetrahydrofuran (99.8%) (Merck KGaA, catalog number: 109731 )
    

Equipment

1. Chainsaw, bandsaw, abrasive belt machine and woodworking lathe
   
2. Analytical balance (accurate to 1 mg or 0.1 mg)
   
3. Desiccator and oven for drying of samples (set to 50 ± 3 °C, 70 ± 3 °C, and to 105 ± 3 °C)
   
4. Polymix (Kinematica, model: PX-MFC 90D )
   
5. Analysette 3 vibratory sieve shaker (Fritsch)
   
6. Soxhlet extraction apparatus (Sigma–Aldrich, catalog number: 64825 )
   
7. Boiling flasks (50 ml) (Sigma–Aldrich, catalog number: Z418773 )
   
8. Water bath (Harry Gestigkeit Gmbh, model: W 16 )
   
9. Fritted-glass filtering crucible of medium porosity (16–40 µm) (VWR International, catalog number: 511-2403 )
   
10. Dropping flasks (50 ml) (Smith Scientific Limited, catalog number: 8029/50 )
    
11. High performance liquid chromatography system (degasser, pump, autosampler, heater and diode-array ) (Agilent Technologies, model: 1200 series )
    
12. Captiva Premium Syringe Filter (0.45 mm PTFE membrane, 15 mm) (Agilent Technologies, catalog number: 5190-5085 )
    
13. PLgel (10 μm, 7.5 x 300 mm, two pieces) (Agilent Technologies, model: MIXED-B column )
    
14. PLgel (10 μm, 7.5 x 50 mm) (Agilent Technologies, model : Guard-column )
    
15. Solid-state NMR spectrometer (Varian, model: 400-MHz ) with the following assembly (Figure 1):
    Magnet: superconducting actively shielded magnet, B = 9.4 T, wide bore – 89 mm
    Console: three high-power linear RF channels, all with spin lock and decoupling capability, output power up to 1000 W,
    
    1. channel – high band RF, narrow band amplifier 375–400 MHz
       
    2. channel – broad band amplifier 18–240 MHz
       
    3. channel – broad band amplifier 10–130 MHz
    Probes:
    a: ¹H – ¹⁹F / ³¹P – ⁷⁹Br / ²³Na – ¹⁵N , 4 mm T3-HXY for solids, double and triple resonance, MAS up to 18 kHz
    b: ¹H – ¹⁹F / ³¹P – ⁷⁹Br / ²³Na – ¹⁵N, 7.5 mm T3-HXY for solids, double and triple resonance, MAS up to 7 kHz
    c: Double channels goniometric static HX probe
    X channel – 5, 10 mm coils, resonance from ³¹P to ¹⁵N
    Accessories:
    Variable temperature control unit, range –150 °C ↔ +250 °C
    Accessory for low-band measurements – down from ¹⁵N
    Accessories for sample preparation and measurements:
    a.ZrO rotors with diameters of 4 and 7.5 mm
    b. Rotor packing and cleaning tools, isopropyl alcohol, liquid nitrogen
    c. Assembly for hydration and dehydration of samples
    d. Primary and secondary standards for calibration of NMR ppm scale
    
    
    Figure 1. Solid-state ¹³C MAS NMR equipment
    

Software

1. ChemStation for LC 3D systems (Agilent Technologies)
   
2. Clarity, GPC module, version 5.0.3.180 (DataApex)
   
3. VnmrJ 3.2 (Varian)
   
4. Mnova 8.1, or a higher version (Mestrelab Research)
   

Procedure