The Chemistry and Microimaging Laboratories of the ESRF are located on the ground floor and 1st floor of the Science Building (SB; labs SB 018 to 021 and labs 102/103, 114, 118 - 121), respectively.

The laboratory facilities provide a glovebox (with stereo microscope), fume cupboards and bench-top space. Standard laboratory equipment (such as pH-meter, deionized and ultrapure water, stirrers, balances, an extensive stock of glassware, refrigerator/freezer, ice-machine, furnaces, ultrasonic bath) and frequently used solvents/chemicals/consumables are available.

Preparation of experiments/proposals

Please note that the proper preparation of a given experiment is solely your responsibility and that of your local contact.

In case your experiment requires access to or support from the Chemistry and Microimaging Lab, you are kindly requested to get in touch with lab staff as early as possible (email).

User access to the Chemistry Lab

If you wish to use the Chemistry Laboratory please:

  • consult the "Instructions for the use of the Chemistry Lab."
     
  • download the "User Declaration Form: Use of the Chemistry Lab" (Chemistry Form in .doc format or .pdf format), and return it duly filled in and signed to the User Office at least 15 days before the starting date of experimental work. For safety reasons, it is mandatory that detailed information about the intended manipulations is provided well in advance of the starting date of a given experiment.

Provision of chemicals and gases

Chemicals for a scheduled experiment can be ordered via the lab, provided the products are available from a supplier with a rapid delivery service (SIGMA, ALDRICH, FLUKA). Please specify clearly the required quantities and purities and allow for a sufficient delivery time.

Sorry, but we cannot handle last minute orders.

The order and transport of gas-bottles has to be arranged by your local contact. Pressure regulators for inert gases (N2, He, Ar, CO2) and hydrogen (or mixtures of hydrogen and inert gases) can be borrowed from the lab. Regulators for corrosive gases have to be provided by your local contact.

Manipulations in inert atmosphere

If your experiment requires manipulations in inert atmosphere, please define in advance the specifications (glove-box, glove-bag, Schlenk-type glass-ware, inert gas). It is not possible to use water, aqueous solutions, organic solvents or compounds with an appreciable vapour pressure in the glove-box. A change of the inert gas (Ar) to nitrogen or helium is not feasible.

An introduction to the use of the glove-box is mandatory for all persons who wish to work unattended.

Interventions of lab staff outside of normal working hours

This may be necessary for certain manipulations in inert atmosphere, the use of open flames and for particularly hazardous experiments. In such cases, make sure you clarify the availability of staff sufficiently in advance of your arrival.

Microimaging and micromanipulation capabilities

  • Sample preparation (cutting, polishing and sectioning)

  • Sample supporting (grids, frames and cells)

  • Sample locating in the beam (X-ray imaging)

  • Sample observation before and after X-ray experiments (AFM, SEM, optical microscopy)

  • Mapping on the samples' area of interest (optical microscope with micro hardness tester)

  • Testing of X-ray optical elements: Bragg-Fresnel optics, Fresnel zone plates, Compound Refractive

  • Lenses, mirrors, multilayers, gratings (AFM, SEM, optical microscope)

Microimaging and micromanipulation equipment

LEO 1530 Scanning Electron Microscope

The LEO 1530 is a state-of-the-art scanning electron microscope (SEM) which uses a Schottky-type field-emission electron source. A beam booster is used to maintain optimum electron optical performance at all accelerating voltages. In addition, the patented Gemini optical column has no crossovers and utilizes a magnetic/electrostatic objective lens for outstanding imaging capabilities, especially at low voltage (due to reduced chromatic aberration).

Resolution: 1 nm at 20 keV WD 2mm
2.1 nm at 1 keV WD 1mm
  Detectors: In-lens annular
Secondary electron
Accelerating voltage:
Magnification:
100 eV to 30 keV
20x to 900Kx
    Backscattered Electron
EDX
Electron gun: Thermal field emission   Analytical distance: 8.5 mm

Specimen chamber and stage:

Dimensions: 330 mm inner diameter
270 mm height
  Specimen stage: 5 axis eucentric
4-axis motorized
Camber viewing: Infrared camera      

The SEM is equiped with Si(Li) solid state detector with INCA microanalysis system. Detector resolution is 137 eV at 5.8 keV. These are some examples of SEM images.

Sputter for gold and carbon

The EDWARDS SI50B sputter coater can be used for coating with a 10-20 nm layer of metal (Au) or carbon. This prevents the caharging of the specimen under observation and the increase of secondary electron emission.

Inverted optical microscope with micromanipulator

The NIKON inverted microscope is ideal for biological sample investigations and any technique requiring micromanipulation. The microscope is equipped with a 3-D manual coarse manipulator MN 188 for coarse and fast displacement of pipette or capillary to the sample and a 3-D hydraulic MO 188 joystick manipulator for ultra-fine manipulations. Since this micromanipulation system is mounted directly to the stage of the inverted optical NIKON microscope, this results in minimum vibration, little space occupancy and a maximum working distance. A microinjector to inject solutions into or extract fluids out of the specimen is also available. The microscope is equipped with a colour video camera. Images can be printed directly on the colour printer or can be transferred to the computer using a frame grabber.

Metallographic optical microscope

The optical microscope LEITZ DMRX is fitted for all metallographic examinations, quality control of machined surfaces, and for all applications in biology and medicine in reflected and transmitted light. A speciality of this microscope is that all contrast modes (brightfield, darkfield, phase and polarisation) can be freely combined. Optical microscope images can be transferred using a colour high-resolution video camera installed on the microscope and connected to the colour printer or can be captured from a video camera using LG-3 Scientific frame grabber (Scion corporation) and sent to the PC, where image processing and analysis programs (contrast enhancement, density profiling, smoothing, sharpening, editing) are installed.

P.A.L.M. Laser Microdissection System

Laser microdissection system is combination of ZEISS inverted Axiovert AX 200M fully motorized microscope and a pulsed ultra-violet (UV-A) laser. High quality laser beam is interfaced into the microscope and focused through an objective to a beam spot size of less than 1 micrometer in diameter for the cutting action. The principle of laser cutting is a locally restricted ablative process without heating of the adjacent material and results in a clear cut gap between your desired sample area and the surrounding tissue. The effective laser energy is concentrated on the minute focal spot only. After microdissection, the isolated specimens are ejected out of the object plane and catapulted directly into the cap of a common microfuge tube. This is performed in an entirely non-contact manner with the help of a single defocused laser pulse. The sample is driven with high speed and can be "beamed" several millimeters away, even against gravity. As opposed to other techniques, with LMPC the desired specimen is captured without contamination, only with the help of laser light. LMPC is a capture method without any mechanical contact to the samples.

Apart from "standard“ fields of application like DNA, RNA or protein investigation, laser microdissection also offers almost unlimited possibilities for experiments with various biological or inorganic materials. The exceptional advantages of high-precision microscopic control and non-contact micromanipulation are used in our case to cut polymer fibers, starch particles, and protein crystals.

Stereomicroscope

A LEICA M3Z stereo microscope is available with a 1:6 zoom magnification changer which enables the total magnification to be continuously altered from 6.5x to 40x. Incident and transmitted light illuminations are possible. The microscope is equipped with two independent mechanical micromanipulators. One is equipped with a 3 axis coarse movement plus an extra fine control on the X-axis. The coarse movement is 25 mm on all axes plus a 8 mm, 5 micron read-out on the fine X-axis. The other has only coarse 25 mm strokes. A black and white video camera allows to transfer images to the monitor and the monochrome videoprinter.

Microtome with cryoattachment

The JUNG 2055 AUTOCUT microtome for automated sectioning of either plastic or paraffin embedded materials is available. The section thickness range is from 0.5 to 60 mm. The speed of the cutting motor is continuously variable. Two modes of automatic operation are available: single cut and continuous cuts. A separate control key-pad centralises all sectioning functions and a motorised fast advance allows to cover larger distances at two different speeds (200 and 1200 mm/s). The maximum sample size is 40*55 mm using standard specimen clamps. The low temperature sectioning system LN20 CRYOSYSTEM is available for critical sectioning applications and for very soft specimen, which has to be cut in frozen conditions.

Cutting machine

The ACCUTOM-5 (STRUERS) is a microprocessor controlled cut-off machine with diamond and carbon wheels. This machine is equipped with a high-precision stepper motor enabling positioning in steps of 5 mm with variable speed and a digital read-out. The cutting process is controlled from the cutting menu where all parameters necessary for the cutting are set, which can be saved in the database for later use. Different specimen holders for cutting small samples are available.

Polishing machine

 

The DAP-V is a small motor-driven machine for wet grinding and for diamond and alumina polishing of metallographic, ceramic and mineralogical specimens. It consists of a circular turntable on which grinding, lapping and/or polishing discs (200mm) can be mounted. The turntable is supported by precision ball bearings and belt driven by an electric motor, which ensures uniform and silent running. On the control panel DAP-V has an adjusting knob for a preselection of speed, an on/off and a speed indicator. A wide range of abrasive papers, polishing cloths and diamonds sprays are available for users.

 X-ray imaging with high-resolution films

Xrayimaging2

High resolution X-ray films are available (resolution of 1 - 10 microns). A dark room in PluoE 111 is equipped with developers, fixers and drying cabinet.

 

 

 

 

 

 

 

 

Mechanical micromanipulators

A 3 axis coarse manipulator with 25 mm movement on the X axis, 20 mm movement on the Y-axis, and 25 mm movement on the Z-axis is ready to use

Small items

  • sample cell
  • grids
  • frames for mounting samples
  • apertures
  • fine tweezers
  • glues
  • etc.