::: Product Information Silicon Carbide Vessels Silicon carbide (SiC) is a chemically inert material which strongly absorbs microwave energy. Due to its outstanding heat conductivity it supports to heat non-absorbing solvents with heating rates beyond 10 °C/sec. Furthermore, it can be used for chemical applications, which are corrosive to glass under high temperature and pressure conditions. With the Monowave series a 10 mL and a 30 mL SiC vessel can be employed to serve these conditions up to 20 mL operation volume. An Alternative to Glass Vials Many industrial processes employ corrosive reactants at high temperatures and pressures (e.g. for fluorination chemistry). In such applications glass cannot be used as a vessel material since it will be degraded. This means, it not only contaminates the reaction mixture, but it will also not withstand elevated pressures anymore. Obviously, there is need for an inert vessel material, which is chemically resistant up to high temperatures and pressures. Furthermore, since microwave chemistry generally relies on the ability of a reaction mixture to efficiently absorb microwave energy, microwave heating of weak absorbing mixtures will always be an issue. In principle, the monomode reactors Monowave 100, 200, 400, and 450 can heat even non-polar solvents far above their boiling points, due to their extremely high field density. However, heating those solvents beyond 200 °C may take a few minutes (Figure 1, gray curves). Fig.1. Toluene (5 mL) heated in a glass vial (G10) and in a SiC vessel (C10) in Monowave 400 (employing the Ruby Thermometer) Employing SiC as a vessel material not only helps to shorten the heating phase and therefore the overall process time, it also helps to reduce the required power to a minimum (Figure 1, red curves). However, due to the excellent microwave absorptivity and heat capacity, virtually no electromagnetic irradiation can interact with the reaction mixture inside the SiC vessel. Nevertheless, due to the high heat conductivity, the reaction mixture is heated most efficiently, and therefore the major advantage of microwave chemistry (rapid heating) is still present, also for volumes >10 mL of even low-absorbing mixtures. For a comprehensive description on the application range of SiC vessels, refer to the application report E07IA002EN. Advantages of SiC Fields of Application Strongly microwave absorbing Chemistry, which is corrosive to glass vials Resistance to glass-corrosive reagents Method development/optimization in non-polar media High thermal conductivity Academic studies (Microwave effects, etc.) Very low thermal expansion coefficient Extractions in low-absorbing solvents (C30 Wide Neck) E07IE007EN-B 1 www.anton-paar.com ::: Product Information Common Design - Use with the different Monowave Models The 10 mL SiC vessel has similar dimensions to the G10 vial, whereas the 30 mL SiC vessel is shaped like the G30 Wide Neck vial (see Fig. 2). Therefore, although entirely made of silicon carbide, the common caps and septa can be used for these vessels. For details in handling refer to chapter 8.1 of the instruction manual E07IB001EN-C or higher. Fig.2. Close-up of silicon carbide vessels C10 (left) and C30 Wide Neck (right) in comparison to the respective glass vials Both vessels are optionally available for Monowave 400 and 450, whereas Monowave 100 and 200 can only operate the C10 vessel as an option. The adjustment factors for the SiC vessels are already stored on the respective reactors upon delivery. Just make sure that the correct vial type is selected in the experiment programming dialog (Figure 3). Note: For SiC vessels the benefit of reusability of consumables is restricted. Depending on the reaction temperature and time, septa might have to be disposed after each run (please refer to the instruction manual, chapter 10.1, for details). Also check the caps regularly if they still sit properly on the vessel neck. If they feel loose replace them as well. Note: For opening of the C30 Wide Neck vessel the use of the Decapper Wide Neck Vessels is required. Both SiC vessels can also be handled with the autosampler MAS 24 of Monowave 400 and 450. As with a single manual experiment, just select C10 or C30 Wide Neck, respectively, as a vial type in the experiment programming dialog (see Figure 3, A) and place them in the corresponding carousel positions. Monowave 100 can only operate 10 mL vessels, therefore the selection is simply between glass and SiC (see Figure 3, B). A B Fig.3. Screen shots of (A) Monowave 200/400/450 and (B) Monowave 100, where the SiC vessel is chosen as a vial type. Smallest Filling Volumes In Monowave 200, 400, and 450, the SiC vessels can be used with or without the Ruby Thermometer. Since the ruby crystal has to immerse into the reaction mixture, a minimum filling volume (2 mL for C10, 6 mL for C30 Wide Neck, respectively) has to be observed when using the Ruby Thermometer for reaction control. However, if only IR temperature measurement is employed, the filling volume can be significantly lower (down to 0.1 mL). Since the heat distribution of the SiC material is extremely high, the IR sensor will measure similar vessel surface temperatures regardless of the filling volume. E07IE007EN-B 2 www.anton-paar.com ::: Product Information Distinct Operation Limits Both silicon carbide vessels follow the operation limits of their glass counterparts, therefore the applicable values of the key parameters differ among each other (see Table 1). C10 C30 Wide Neck Filling Volume 6 mL 20 mL Max. Temperature 300 °C 200 °C Max. Pressure 30 bar 15 bar Max. Run time 100 h 4h Table 1. Operation limits of SiC vessels Note: Although SiC can withstand reagents which would otherwise attack glass it does not mean that the use of corrosive mineral acids is allowed. The limiting factor for those chemicals is still the lacking resistance of the Monowave instruments itself. Therefore the restrictions of use have to be observed still (refer to the Appendix of the instruction manual). Ordering Information 93486 Reaction Vessel C10 Single 10 mL silicon carbide vessel without any additional consumables. 93487 Reaction Vessel C10 Package Convenient set for experiments with the 10 mL silicon carbide vessel, comprising one reaction vessel C10 (93486) with one package each of snap caps (83214) and silicone septa (88883). 173574 Reaction Vessel C30 Wide Neck assembled Single 30 mL silicon carbide vessel with wide neck with one Snap Cap Wide Neck and one corresponding PTFE Septum Wide Neck. 161692 Decapper Wide Neck Vessels Supporting tool for decapping of the reaction vessels G30 Wide Neck and C30 Wide Neck. E07IE007EN-B 3 www.anton-paar.com
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