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ELEMENTAL ORGANIC ANALYSIS SERVICE

 

CE Instruments CHNS1100 Elemental Analyser

This technic provides the content of Carbon, Hydrogen, Nitrogen and Sulphur presents in a sample. The analytical method is based on full and instant oxidation of the sample through oxygen combustion at a temperature of 1020°C approximately. Combustion products are transported by carrier gas to a chromatographic column where the separation is performed. A thermal conductivity detector provides the signal for each element which is translated into a percentage content.

The samples (solids or viscous non-volatile liquids) must be solvent free and homogeneous, solids must be maximum powdered. 10 mg is the minimum quantity of sample to carry out the analysis.

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ELEMENTAL INORGANIC ANALYSIS SERVICE

 

Thermo Scientific ICE 3000 atomic spectrometer

This technic uses the atomic absorption or emission of spectrometry to evaluate the inorganic elements concentration presents in a sample.

When using a nebulizer, the dissolving sample turns into mist and it atomized taking advantage of the energy coming from a flame. During the absorption technic, atoms are exposed to certain wavelength, characteristic of the element, and the quantity of absorbed light allows to calculate the element concentration in the sample. During the emission technic, the quantity of light emitted by the element is what allows to calculate its concentration.

This is a high sensitivity technic, with work intervals for concentrations vary greatly depending on the element (0.1-50 mg / L).

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Inductively coupled plasma spectrometer

Inductively coupled plasma mass spectrometry (ICP-MS) is highly sensitive and able to determine almost all of the elements present in the periodic table at trace concentrations (nanogram/litre or part per trillion, ppt). These elements susceptible of being determined must have an ionization potential lower than that of argon. The technic is based on the attachment of a method to generate ions (inductively coupled plasma) and other method to separate and detect ions (mass spectrometer).

The dissolving sample, transported through a peristaltic pump to the nebulizer system where it is transformed into aerosol thanks to the Argon gas action. This aerosol is conducted to a ionization zone, consisting in a plasma generated when submitting the Argon gas to the action of an oscillating magnetic field induced by a high frequency current. The ions pass into the quadrupole filter through a rising vacuum interface, where they are separated according to their charge / mass ratio. Each of the tuned masses reaches the detector where its abundance is evaluated in the sample.

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Flash Point Apparatus

 

Small-scale Flash Point Apparatus

The flash point of a liquid is the minimum temperature at which it gives off sufficient vapour to form a flammable mixture in the air surrounding the surface of the liquid or inside the vessel used at standard atmospheric pressure Ignites when approaching an ignition source. It is an index used by government regulatory agencies to classify liquids into flammable or combustible.

The test equipment available uses the closer cup tester preventing the loss of components. It is applicable to products having a flash point between 0 and 110 ° C and a viscosity of less than 150 st at 25 ° C.

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INFRARED SPECTROSCOPY SERVICE

 

Agilent Cary 630 infrared spectrometer with ATR

Infrared radiation, when affecting a sample, is capable of causing changes in the vibrational states of its constituent molecules. he absorption of radiation by a sample is indicative of the type of bonds and functional groups it presents.

ATR Mode: It is a sampling mode in which the IR beam is projected onto a high refractive index crystal. The beam is reflected on the inner side of the crystal and creates an evanescent wave that penetrates the sample. It must be in close contact with the glass. A part of the energy of the evanescent wave is absorbed and the reflected radiation (with the chemical information of the sample) is taken to the detector. It is a very versatile method that allows the measurement of liquid and solid samples without practically any previous preparation.

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SPECTROMETER OF RAMAN SERVICE

 

Spectrometer of Raman Emission Horiba-MTB Xplora

The analysis through Raman spectroscopy is based in the scan of scattered light on a concrete material when a beam of monochromatic light falls on it. A small portion of light is automatically scattered, experiencing light frequency changes that are characteristic in this analysed material and independent from the frequency of the incident light.

The spreading Raman spectrometer is endowed with a microscope with focal and three lines of laser stimulation (longitude of wave 514, 632 and 785 nm), four diffraction nets (600, 1200, 1800 and 2400 lines/mm) and a CCD detector cooled by Peltier effect. It allows to map in 3D due to the incorporation of an computerised auto stage XYZ. The maximum resolution is 3cm-1 and the measuring range is 60 - 8000 cm-1.

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SPECTROFLUOROMETRY SERVICE

 

Spectrofluorometer Fluoromax Horiba-MTB

The spectroscopy of molecular fluorescence is an non-destructive analytic technique, characterised by its speed, its high selectivity and sensibility.

Irradiated samples with electromagnetic radiation absorb energies passing through its molecules to stimulated energy levels. These stimulated molecules go back to their essential state freeing the excess of energy in form of photons. This light emission allows the elemental, molecular determination of a substance.

This equipment counts with a xenon light source that is vertically built, which increases its stability as well as its lifespan. The xenon light source shines a light on the entrance slit of the stimulating monochromator with an elliptic mirror. The reflecting surface, as well as guarantying the effective collection of the beam, holds all wave longitudes focused on the slit.

This equipment allows the reading in static, the registration of stimulating spectres and 2D emission (to set waves longitudes) and 3D emission (to several wave longitudes) and the reading of simple points in fixed stimulating and emission conditions.

The service provides macro, semi and micro quartz sells to measure samples in dissolution and solid matrix for solid samples in film.

 

 

SAMPLES PREPARATION SERVICE

 

Weighing
AT21 Comparator Analytical Balance (Mettler Toledo)

The general characteristics of the balance are an accuracy of indication of 1 μg, a weighing field of 22 g and a subtractive zone of taring from 0 to 22 g. The balance automatically performs daily internal self-calibrations. An external calibration is performed annually.

 

Grinding sample
Mixer mill MN400 (Retsch)

It allows to perform the grinding process of small volumes of sample by dry, humid and cryogenic means. It is capable of mixing and homogenize powder and suspensions in matter of seconds, thus obtaining a final granulometry of 5µm. The duration of the grinding is from 30 s. to 2 min. The dry volume which can be processed is 2 x 20 mL.

 

Sample digestion plate
Dry Bath FB 15103 (Fischer Scientific)

Digital temperature control plate, in a range from ambient temperature + 5 ° C to 130 ° C. Accuracy at ± 5 ° C. The heating blocks can accommodate 10 mm diameter tubes.

 

High pressure microwave digestion for samples
Ethos Easy Milestone

The digester is equipped with two magnetrons that achieve a total power of 950 Watt and a rotating diffuser to evenly distribute the microwaves, which favours the complete digestion of the most difficult samples. Two operational modes are possible: glass digestion with sample amounts in the range 0.1-1g and micro-insert digestion for samples in quantities less than 0.1 g.

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Acid distillation
DST-1000 Savillex

Acid Purification System requiring no cooling water.

It is prepared to obtain a profitable and efficient supply of high purity nitric acid (suitable for the analysis of trace elements) from ACS grade acid.

 
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