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Chemistry laboratory

logo laboratoire chimie SOLEIL synchrotron

Two laboratories are available at the Synchrotron SOLEIL.

Their mission is to ensure a technical and scientific support to the users for the sample preparation as part of experiences on the beamlines. They also supply to the SOLEIL scientists infrastructures and the necessary equipment to the specific research projects in the field of chemistry.

Which laboratory to choose?

The user’s choice between Chemistry lab 1 and Chemistry lab 2 depends on the location of the beamline where the experiment is carried on, because of the long beamlines (NANOSCOPIUM, ANATOMIX, PUMA), which force users to use the stairs to reach their laboratory.

To a lesser extent, the choice between the two labs depends on the equipment that is needed for the samples’ preparation and whether it is present in the laboratory or not.

Access conditions

Users and SOLEIL scientist (standard projects and out of program committee review)

 

During the submission of the project in the SUN set, the main proposer has to indicate if he intends to use the chemistry laboratory.
If the project is accepted, the main proposer must get in touch with the laboratory manager. Then, one month before his arrival and no later, he confirms the access request on-line on SUN set 

Support Laboratory access (for Main proposer)

Then he indicates the activities that he plans to carry out in the lab and can request a technical support. Finally, he specifies their needs :

  • in scientific equipment among those available
  • in chemicals and material that he planned to use.

 

 SOLEIL staff

 

For temporary needs or long term needs (trainees, students…) out of the proposals on the beamlines, a permanent access to the laboratories is possible. A justified request (description of the activities that he plans to carry out in the lab) has to be addressed at the person in charge of the laboratory

 

Theses laboratories offer a technical support, an infrastructure and an usual available equipment and chemical in a chemistry lab.

Services

The lab team offers to the users and SOLEIL personnel a technical support (installation of the materiel, feasibility) and a scientific support (advices and skills, within the limits of its competences). The team is present from Monday to Friday, during usual working hours.

Some experiments, especially those classified “red” by the security group (particularly dangerous experiment), require the presence of a chemist from the laboratory. You have to make sure of the availability of staff before your arrival.

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Equipment

The equipment localization is specified by the mention Chemistry 1 or Chemistry 2. Without indications, they are available in the two laboratories.

 

Conditioning equipment

- Gloves box (Jacomex)

Boites à gants Jacomex SOLEIL Synchrotron

  • Stainless steel Gloves box, with a purification system in O2/H2O  under argon atmosphere  (Chemistry 2)
  • Pumping chamber for the preparation and the transfer ofsamples under nitrogen atmosphere (Chemistry 1)

 

 

 

- Tube furnace (Carbolite)

Four tubulaire Carbolite SOLEIL Synchrotron

Chemistry 2

  • Rated temperature =+1200°C ; internal diameter : 170mm
  • Under specific or ambient atmosphere  (Ar/N2/dry air/H2 (5%)-Ar)

 

 

- Muffle furnace  (Nabertherm) 

Four à moufle Nabertherm SOLEIL Synchrotron

  • Rated temperature= 1100°C under ambient atmosphere (chemistry 1)
  • Rated temperature= 1700°C under ambient atmosphere or argon atmosphere (chemistry 2)

 

 

  • Ventilated oven
  • Vacuum oven
  • Combined refrigerator/freezer
  • Glass vacuum dessicator                    
  • Gloves bag

 

 

    Preparing equipment

    Precision balances

    Precision Brand Quantity Range remark
    1/100 mg Mettler Toledo 1 0-220 g chemistry 2 in the glove box
    1 mg
    Mettler Toledo
    1 0-610 g chemistry 2
     
    1/10 mg Mettler Toledo 2 0-220 g chemistry 1
    10 mg Sartorius 1 0-4200 g chemistry 2
     
    1/100 mg Mettler Toledo 1 0-220 g chemistry 2 : 
    With or without contac for toxic compound/CMR
    10 mg Ohaus 1 0-10 g chemistry 1: 
    Portable
    • Automatic pipets(Eppendorph research)
    • Overhead stirrer
    • Magnetic stirrers included 2 with several positions
    • Heating magnetic stirrers with accessories for balloons of different volumes
    • Orbital shaker
    • Vortex
    • Hot plates
    • Centrifuges (chemistry 1)
    • disphragm pump, chemical products - Flow 6L.min-1 ; final vacuum : 100mbar - Flow 20L.min-1 ; final vacuum : 8mbar
    • Vacuum filtration system
    • Syringue pump
    • Ultrasonic baths
    • Heated baths T = -25 to 150 °C (Huber Ministat 125) T = ambient to 100 °C(Thermo Haake) T = -40 to 200 °C (Huber Ministat 240)
    • Heating mantle
    • Rotary evaporator (Buchi) (Chemistry 2)

    • Lyophilizer (Christ) (Chemistry 2)

     

     

     

     

    Shaping equipment

    • Hand press (Chemistry 2) Weight max : 2 tonnes In the gloves box Mould : diameter of  7 mm
    • Semi-automatic hydraulic press (Chemistry 2) Pmax : from 2 to 15 tonnes Mould :diameter of 6, 10, 13, 20 mm
    • Sieves (Retsch) (Chemistry 1)
    • Planetary crusher (Retsch) (Chemistry 2) PM100, granulation <10mm 

    Mortars + pestles

     

    Measuring equipment

     

    • pH-meter  (Mettler Toledo)
    • Titrator (Mettler Toledo)
    • Turbidimeter (Hach Lange) (Chemistry 1) From 0 to 10 000 NTU
    • Conductimeter  (Mettler Toledo) (Chemistry 1)
    • Thermometer
    • Glass pycnometer (Chemistry 2)

     

    Chemistry Material

     

    • Daily use glassware (beaker, flask, crystallizer, vial…)
    • Synthesis glassware (still, round bottom flasks, inner connectors, reducers, bulbous vessel…)
    • PTFE ustensils
    • Syringes, needles
    • etc

     

    Others

     

    • Fan tailed Burners
    • Hair dryer
    • Adjustable laboratory jack, stands, clamps…
    • Purified water system(Millipore) Reverse osmosis purified water and ultra-pure water 18.2 mΩ
    • Optical microscope  (Bresser) (Chemistry 1) Working distance : Max : 200mm, Min 25mm magnification : 10 to 40 x

    Caracterisation equipment

     

     

    Characteristics

     

    • Geometry : Bragg Bentano theta-theta
    • Angular range : 0-130°
    • l RX : 1.54 Å (Anode Cu)
    • Generator power:30kV/10mA=300 W
    • Solid-state detector 1-D Lynxeye
    • Résolution : 0,02°

    X ray diffractometer  (XRD)

    (Bruker)

    Chemistry 2

     

    Characteristics

     

    • Measure of particle size in solution(0,8 nm -6µm)

     

    DLS Granulometer

    (Nanotrac)

    Chemistry  2

     

     

    Characteristics

     

    • Motorised XYZ stand with a resolution of 0.1mm
    • Holomap software (Matlab): cartography recording point by point
    • Possible magnification : x10 x50
    • Excitation laser λ = 785mm

     

    Raman Microscope

    (Kaiser)

    Chemistry 1

     

     

     

     

     

     

    Characteristics

     

    • Excitation: laser diode λexcitation  =785 nm or 532 nm
    • High sensitive CCD detector : spectral coverage+100 to 3450 cm-1( at 785 nm) to 4325 cm-1( at 532 nm)
    • Pnominal : 400mW
    • Holographic Notch filters
    • Can be connected to a microscope or optical head with optical fibers (excitation and collection)
    • Non-contact or immersion optics (immersion probe or gas probe)
    • Can be easily coupled with either other classic characterization tools or SR techniques (XAS, XRD….)

     

    Raman Spectrometer *

    (KOSI)

    Chemistry 1

     

     

     

     

     

    Characteristics

     

     

    CARY 50 *

    CARY 4000

    Spectral range

    190< λ<1100 nm        

    175(190) < λ < 900 nm

    Source

    Xenon-pulse lamp

    Deuterium (UV) & tungtsen halogen (Vis) lamp

    Detector

    Si diode

    PMT

    Solids, thin films and liquids : different accessories

     

    Solids : measure diffusely/absolute scattered reflection and transmission at variable angle and polarization

    Liquids : possibility to combine with another techniques

    • Optical fiber used in transmission or immersion probe : 1 or 10 mm
    • Kinetics with a rate VScan < 24000 nm/min

     

    Spectrometer UV-Vis *

    (Agilent)

    Chemistry 1

    FTIR

     

    Characteristics

     

    • Range : 7800 cm-1-370 cm-1 (proche IR)
    • Resolution : 0.5 cm-1 (Ge-KBr beamsplitter)
    • Sourcelamp : HeNelaser
    • monocristal detector
    • ATR accessory

     

    FT-IR Spectrometer

    (Perkin Elmer)

    Chemistry 2

     

     

     

     

     

     

    Characteristics

     

    Labsys Evo

    • TGA/DSC (Differential Scanning Calorimeter / thermogravimetric method)  Temperature range: 30 +1600°C (0.01 à 100°C/min)
    • Carrier gas ; He, Dry air
    • +/- 1000mg and +/- 200 mg
    • Monitoring of thermal transitions (Tg, Tc, Tm) materials and mass changes depending on the temperature under controlled atmosphere

    Dsc 111

    • DSC (Differential Scanning Calorimeter)
    • -80°C à 800°C
    • Possible coupling with other synchrotron techniques

    Thermal Analysis *

    (Setaram)

    Chemistry 1

     

    Les couplages des techniques des laboratoires (instrument*) avec celle du rayonnement synchrotron peuvent être envisagées sur les lignes de lumière

    Lien vers document Samba    http://www.synchrotron-soleil.fr/Recherche/LignesLumiere/SAMBA/EquipementDetaille/CombinedTechniques

    Lien vers document Rock http://www.synchrotron-soleil.fr/Recherche/LignesLumiere/ROCK/EquipementDetaille/CombinedTechniques

     

    Declaration of sample

    • During the submission of a project to SOLEIL synchrotron, all the chemicals and materials necessary for samples preparation have to be declared on line. Each sample has to be identified and specifically declared according to is nature ( Samples and substances declaration).
    • Only gases and chemicals approved by the safety group of SOLEIL synchrotron can be used.

    Experiment in the laboratories

    • Each sample or handled chemicals must be labelled. The following information has to be mentioned :

    -The name of the product

    -The date

    -The name of the project and phone number of persons to be contacted

    • Warnings and indications in the laboratory must be respected.
    • Individual protection against hazardous substances must be used for any handling (lab-coats, gloves, glasses, steel toed shoes and working under fume hood if necessary).
    • Handling hazardous chemicals alone in the laboratory is forbidden.
    • Chemical waste must be disposed of in suitable containers (separation of inflammable products, acid, halogenous solvents...)
    • Any drinking or any eating in the room is forbidden. 

    Chemical risks

    Collective and individual protections

    The following equipment is available in each laboratory:

    Masks (FFP1,FFP2, FFP3) Fume hoods Safety shower
    Standard and specific overalls Acid fume hood (chemistry 2) Eye wash
    Glasses Ventilated cabinets for solvants and acids/bases  
    Gloves (latex, nitril, neopren)    

     

    Waste management in the chemistry laboratory

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