Supervisor científico: Manuel González-Guerrero - Professor

contrAA 800 D – Combined device for flame and graphite tube techniques

The contrAA 800 is a high-resolution continuum source atomic absorption spectrometer for flame and graphite tube techniques. It is suited for the sequential detection of metallic and non-metallic traces in liquid and dissolved samples. Combined with an autosampler the contrAA 800 can be used as a multielement automatic unit to be used during routine analysis.

Graphite tube system

The autosampler AS-GF is used in the graphite tube technique for feeding liquid samples. The autosampler AS-GF accepts defined volumes of different solutions and places them into the graphite tube. It enables: the addition of up to five modifiers to the sample solution; transport of the sample solution to the thermal pretreatment in the tuve; enrichment of samples; placement of components in the preheated tuve; separate transport of components with intermediate washing; automatic preparation of standards by dilution or by different volumes; fixed, preselected or intelligent sample dilution and fully automatic multi-element mode.

Protocols available for the determination of Fe, Mo, Cu Zn and P. For other determinations, consult in advance.

Flame system

Flame atomic absorption spectroscopy is used for the determination of trace elements in the concentration range from µg/L to mg/L and for the determination of main components. It requires a flame with constant properties. The flame composition must also be compatible with the respective element.

The contrAA 800 D can be operated with the following types of flames and their corresponding burners: 

1. Acetylene-air flame with 50 mm one-slit burner (universal burner)
2. Acetylene nitrous oxide flame with a 50 mm one-slit (not available)

The acetylene-air flame can be used for most elements.

The autosampler facilitates the automated operation during multiple element analysis. The device parameters for the sample supply are configured with the control software ASpect CS. The autosampler AS-FD: is an automatic autosampler, also has a dilution function. The autosampler has sample tray with 54 positions for 50 mL cups.

Responsable: Inmaculada Gude Rodríguez - Technician

Supervisor científico: María Garrido Arandia - Assistant Professor

MicroCal PEAQ-ITC

The MicroCal PEAQ-ITC is a highly sensitive, low volume isothermal titration calorimeter for the label-free in solution study of biomolecular interactions. It delivers direct measurement of all binding parameters in a single experiment and can analyze weak to high affinity binders. 

Features and benefits

MicroCal PEAQ-ITC is designed for ease-of-use and exceptional sensitivity. The system directly measures heat released or absorbed during biochemical binding events, from which it calculates binding affinity (KD), stoichiometry (n), enthalpy (ΔH), and entropy (ΔS). With minimal sample preparation and system optimization data is generated quickly and easily. The wide affinity range enables analysis of weak to high affinity binders, with excellent reproducibility.

A wide range of applications can be investigated with MicroCal PEAQ-ITC, including characterization of molecular interactions of small molecules, proteins, antibodies, nucleic acids, lipids and other biomolecules. It can also be used to measure enzyme kinetics.

How it Works

Isothermal titration microcalorimeters measure the heat change that occurs when two molecules interact. Heat is released or absorbed as a result of the redistribution and formation of non-covalent bonds when the interacting molecules go from the free to the bound state. ITC monitors these heat changes by measuring the differential power, applied to the cell heaters, required to maintain zero temperature difference between the reference and sample cells as the binding partners are mixed. The reference cell usually contains water, while the sample cell contains one of the binding partners (the sample, often but not necessarily a macromolecule) and a stirring syringe which holds the other binding partner (the ligand). The ligand is injected into the sample cell, typically in 0.5 to 2 μL aliquots, until the ligand concentration is two- to three-fold greater than the sample. Each injection of ligand results in a heat pulse that is integrated with respect to time and normalized for concentration to generate a titration curve of kcal/mol vs molar ratio (ligand/sample). The resulting isotherm is fitted to a binding model to generate the affinity (KD), stoichiometry (n) and enthalpy of interaction (ΔH).

 
ITC-TEORIA Y PRACTICA

Responsable: Inmaculada Gude Rodríguez - Technician

Supervisor científico: Antonio Molina Fernández - Professor

Dionex HPIC System ICS-6000

The Dionex ICS 6000 chromatography system is a compact, modular, and versatile system designed to perform various types of isocratic and gradient ion exchange separations. The entire system is inert and metal-free, ensuring that no metallic components come into contact with the sample or eluent, allowing operation at extreme pH levels. It is a high-pressure system designed for the determination of ions and charged molecules in diverse applications.

ELUENT DELIVERY SYSTEM

The Dionex ICS-6000 system features a dual-piston, high-pressure quaternary pumping system with internal vacuum degassing for eluent delivery. It has the capability to perform unlimited gradients of varying concentrations using up to four different mobile phases.

AUTOSAMPLER MODULE

It includes an autosampler for 50 vials of 5 mL or 0.5 mL, incorporating a sample filtration system vial by vial. It has individual plugs and filters for each vial to prevent cross-contamination.

DETECTOR MODULE

The system incorporates a column oven that can heat guard and analytical columns within a temperature range from 10°C to 70°C (at least 5°C above ambient temperature). The bioanalysis unit provides CarboPac PA1, PA20 and PA100 columns.

Furthermore, the detector compartment can operate within a temperature range of 18 to 40°C to enhance analyte signals and improve sensitivity. 

The electrochemical detector contains a gold electrode, which is essential for the analysis of inorganic ions, carbohydrates, and contaminant determination.

APPLICATIONS

The Dionex ICS-6000 HPIC system is a high-pressure ion chromatography equipment designed for the separation and quantification of ions and charged molecules in various applications, ranging from water and wastewater analysis to biological research and environmental studies.

Responsable: Inmaculada Gude Rodríguez - Technician

Supervisor científico: Araceli Díaz Perales - Professor

Agilent HPLC System (1260 Infinity II Quaternary System)

The LC 1260 Infinity II is a versatile HPLC system that offers the highest functionality and operational convenience for analytical and preparative HPLC.

The Agilent 1260 Infinity II quaternary pump is ideal for a wide range of applications and columns. The formation of quaternary gradients with low-pressure mixing makes it the ideal pump for applications requiring maximum flexibility in solvent combination, as well as for UHPLC separations (including the use of STM columns) to reduce analysis times by over 70%. With a maximum pressure of 600 bars, a vacuum degasser for four channels, and flow rates of up to 5 ml/min, it allows for injection overlapping to increase productivity.

The column compartment has two independently temperature-controlled zones using Peltier technology. It allows for preheating of the solvent in the precolumn. With a temperature range of 10⁰C below room temperature (minimum of 4⁰C) up to 85⁰C. The Bioanalysis Unit is equipped with Poroshell 120 EC-C18 and ZORBAX HC-C18 / TC-C18 columns, suitable for the chromatographic separation of small-molecule compounds.

The 1260 Infinity II system is equipped with two detectors:

1. Variable and programmable ultraviolet/visible wavelength detector. Dual-beam photometer and deuterium lamp for high sensitivity, low detection limits with very low noise and baseline drift.
2. Fluorescence detector with a long-lasting pulsating xenon lamp that stabilizes in microseconds, reducing costs by allowing it to be turned off when data is not being acquired.

Additionally, the system includes a fraction collector that allows us to recover the separated and detected analytes by the HPLC, with the minimum possible dead volume to avoid peak dispersion. The equipment allows us to trace the different samples and their fractions, being able to select them by retention times, peaks, or analyte mass of the required fractions.

ASE 350 Accelerated Solvent Extractor

1. The pressure mode is a static mode of extraction that minimizes solvent usage by  maintaining a fixed cell pressure and eliminating the introduction of fresh solvent during the heating and static cycles. This mode uses less solvent than any other ASE 350 extraction mode.
2. The flow mode is a continuous dynamic extraction mode in which small aliquots of solvent are delivered to the cell at the specified Flow rate throughout the static step. The cell temperature remains constant throughout the run.

Solvent saver methods are recommended for:

1. Modifying and enhancing existing extraction methods
2. Exploring new extraction methods
3. Simulating extraction on a small scale before scale-up to a plant scale extraction module.

During a run, the cell is filled with solvent and then heated and pressurized to maintain the solvent in a liquid state. After the run, the extract is rinsed from the cell into a collection vessel (a bottle or vial). If adsorbents are used in the sample cell, post-extraction cleanup may not be required. If adsorbents are not used, sample cleanup may be required.

Theory of ASE

Responsable: Inmaculada Gude Rodríguez - Technician

Supervisor científico: Stephan Pollmann - Professor

GC-QqQ-MS/MS System (SCION TQ)

The equipment consists of:

Ion Source

In the ion source, sample components are exposed to conditions that generate ions. These conditions can be gentle or harsh enough to fragment molecules.

1. Electron Ionization: It is the traditional ionization technique in GC/MS and is suitable for all compounds in the gas phase.
2. Chemical Ionization: It is a good strategy when no molecular ion is observed in electron ionization and to confirm the mass-to-charge ratio of the molecular ion.