Le laboratoire SMS possède les outils de préparation de l'échantillon suivants (cliquez pour accéder directement au contenu):

 
 
 
 
 
- High Energy Milling:
 

 

 

 

 

 

 

 

  •  Mini Spray Dryer B-290

  

Supplier: Büchi         

Principle: Spray-drying is a process which consists of isolating a solid phase from a fast solvent vaporization from solution droplets. This technique leads in one step to a dry product displaying appropriate Particle Size Distribution resulting in some cases to the appearance of a new polymorph (notably metastable) or an amorphous material. 

Type of analyses performed: This device is ideal for small volumes, which is particularly interesting for using high-value-added products.

Highlights:

- G. Baaklini, V. Dupray, G. Coquerel. Inhibition of the spontaneous polymorphic transition of pyrazinamide γ form at room temperature by co-spray drying with 1,3-dimethylurea.  Int. J. Pharm., 2015, 479, 163-170.

- Applicant: IPSEN PHARMA. Inventors: Delahaye, D.; Diolez, C.; Rolland, A.; Diancourt, F.; Brochard, A.; Mondoly, N.; Poirot, B.; Coquerel, G.; Martins, D.; Houssin, O.; Petit, M.-N. New polymorphic form, crystalline dimethyl sulfoxide solvate and crystalline 1, 4-dioxane hemisolvate of 6-oxo-6, 7, 8, 9, 10, 11-hexahydrocyclohepta(c)chromen-3-yl sulfamate, are steroid sulfatase inhibitors, useful to treat cancer. French patent application FR2942226 filed on 13/02/2009.

- Applicant: SERVIER; Inventors: Martins, D.; Coquerel, G.; Linol, J.; Langlois, P. Novel process for obtaining the crystalline form V of Agomelatine. International patent application WO2010/015747 filed on 04/08/2009 under priority filed on 05/08/2008.

 
 
 
 
 
 
  • Spin-coater SCS 6800

  

Supplier: Speciality Coating Systems         

Principle: The Spin-coater is a device used to produce thin films, whose thickness would vary from few nanometers up to few hundreds of nanometers, of organic compounds initially dissolved in a solvent.

Type of analyses performed: Every kind of substrate could be used (glass, silicium, gold, polymers, …) and also any kind of solvent (in which the solute is soluble enough). The thickness of the film, when keeping spin-coating parameters constant (speed of rotation, rotation time), is directly dependant from the solute concentration in solution. It is therefore possible to change the films thickness over a large range and to study its effect on crystallization (polymorphism, phase transitions as a function of the thickness, formation of amorphous states,...).

Highlights:

- D. E. Martínez, G. Gbabode, C. Ruzié, B. Chattopadhyay, G. Schweicher, A. R. Kennedy, Y. H. Geerts, M. Sferrazza, Self-assembled p-conjugated organic nanoplates: from hexagonal to triangular motifs. RSC Adv. 2016, 6, 44921-44931.

- G. Gbabode, M. Dohr, C. Niebel, J.-Y. Balandier, C. Ruzié, P. Négrier, D. Mondieig, Y. H. Geerts, R. Resel, M. Sferrazza, X-ray structural investigation of nonsymmetrically and symmetrically alkylated [1]benzothieno[3,2-b]benzothiophene derivatives in bulk and thin films. ACS Appl. Mater. Interfaces 2014, 6, 13413-13421.

 
 
 
 
  • Planetary mill Fritsch Pulverisette P7 Premium Line

 

Supplier: Fritsch        

Principle: Milling of materials in dry mode, liquid-assisted or under inert gas. Milling jars which contains the sample and milling balls rotate on themselves (from 100 up to 1100 rotations/min). The jars are disposed on the principal disk which turns on the opposite side. Several jars and ball types are available in the laboratory (agate, zirconium oxide) . 

Type of analyses performed: This device leads to a very thin PSD, may generate phase transformations (polymorphic transitions) or an amorphous state when milling is performed below Tg.  The device is in majority dedicated to molecular crystals.

Highlights:

- Linol, J., Morelli, T., Petit, M. N., Coquerel, G. Inversion of the relative stability between two polymorphic forms of (±) modafinil under dry high-energy milling: comparisons with results obtained under wet high-energy milling. Crystal Growth & Design, 7(9), 2007, 1608-1611.

- Schammé, B., Couvrat, N., Malpeli, P., Dudognon, E., Delbreilh, L., Dupray, V., Dargent, E. Coquerel, G. Transformation of an active pharmaceutical ingredient upon high-energy milling: A process-induced disorder in Biclotymol. International journal of pharmaceutics, 499(1), 2016, 67-73.

 
 
 
 
  • Vibrating cryo-mill/siever Fritsch Pulverisette 0

 

Supplier: Fritsch        

Principle: The P0 pulverisette mills the sample through chocs and friction effects. The mortar is submitted to a vibratory moving via an electro magnet, the moving being transmetted then to the ball and the sample. Cryogenic mill may be performed using the  « Cryo-box » module. This device may also be transformed into a vibrating siever. Numerous sieves are available for PSD analysis of solid substances.

Type of analyses performed:  This laboratory device helps to break solids which are difficultly milled by other devices. 

 

  • Vibro-mill Retsch MM 400

 

Supplier: Retsch      

Principle: Millings may be performed in dry mode, liquid-assisted mode or cryogenic mode in MM400 jars. The latter produces vibrations on a horizontal plan at a given frequency. Due to their inertia, balls hit the sample located on the inner surface (rounded) and thus mill the sample. 

Type of analyses performed: MM400 device helps to mix and homogenize powder sampoles in few seconds but also to refine PSD of molecular materials. Peculiar crystalline phases (metastabe polymorphs, cocrystals) could also be isolated with this device.

 
 

 

 

  •  Sublimation furnace (secondary vacuum) 

Supplier: Lecordier Siverso, Cerhec, Edwards         

Principle: This device helps to purifiy volatile substances thermally stable: the purification acts through via a sublimation step and the separation is due to volatilities differences between the compounds. Recrystallization from the gaseous phase is controlled by a temperature gradient occurring inside a segmented tube in quartz. The experiment occurs under secondary vacuum (fixed, 10-10 bar).

Type of analyses performed: Purification to ultra-purification of thermally stable volatile compounds.