Chemical Analysis Lab

Micronanoplastics Unit

IMDEA Water has a specialized unit for the analysis of micronanoplastic particles environmental in samples. For this it has specific techniques: Pyrolysis system coupled to Gas Chromagraphy-Mass spectrometry (Py-GC-MS); FT-IR Microscopic Based Imaging System coupled to RAMAN (ÎŒFTIR-Raman); and field-flow fractionation system coupled to ultraviolet/refractive index detector with dynamic light scattering (FFF-UV/IR-DLS).

The equipments ÎŒFTIR-Raman and FFF-UV/IR-DLS were purchased thanks to the grant EQC2021-007037-P funded by:

Equipment Description
Py-GC-MS. Pyrolysis coupled to GC-MS is the most common technique used for the quantification of MNPs in a diversity of samples. During the pyrolysis process, the fragmentation of the plastic polimers occurs due to the high temperatures applied, and specific fragments are separated and detected in the GC-MS. Thus, identification and quantification of different types of polimers as polyethylene, polystyrene, polypropylene, PET, PVC
 that are present in the samples.
”FTIR-Raman. The combination of these infrared microscopy techniques allows the MNP particles location (10 ”m or lower sizes), the count, identification and size and type distribution. Information obtained from this analysis is complementary to the one obtained by Py-GC-MS. This equipment was purchased thanks to the grant EQC2021-007037-P funded by MCIN/AEI/10.13039/501100011033 and by the European Union NextGenerationEU/PRTR.
Field-flow fractonation system. With this system the separation of MNP particles from 10 nm to 20 ”m is possible, thus different fractions of a sample with different particle sizes can be recovered. Then these fractions can be analyzed by Py-GC-MS or ”FTIR-Raman, so complementary information about size distribution, molecular weight and surface charge can be obtained. This equipment was purchased thanks to the grant EQC2021-007037-P funded by MCIN/AEI/10.13039/501100011033 and by the European Union NextGenerationEU/PRTR.

Chromatography Unit

High resolution liquid chromatography (HPLC) is one of the most widely used separation techniques, due to its versatility and broad field of application. Chromatography is essentially a physical method of separation, in which the components to be separated are distributed in two phases: the stationary phase, with a large surface area and the mobile phase, which runs continuously throughout the stationary phase. Chromatographic processes take place as a result of the repeated absorptions and desorptions during movement of the sample components throughout the stationary phase, achieving separation of the same according to their distribution coefficients. The final outcome is that the components of the mix come out separated depending on their retention times, which constitutes the chromatogram. Through the chromatogram it is possible to identify the separated substances qualitatively and quantitatively.

Applications

The field of application for this technique is very wide-ranging. Some of the applications are listed here:

  • Determination of organic pollutants (pesticides, herbicides, phenols, PCBs)
  • Pharmaceutical products (antibiotics, sedatives, painkillers)
  • Foodstuffs: artificial sweeteners, antioxidants, additives
  • Quantitative analysis of compounds of interest

Equipment

The HPLC Model 1200 (Agilent Technologies) apparatus includes a vacuum degasser, quaternary pump, automatic injector, thermostatted column compartment and diode detector (DAD).

HPLC1200

Ion Chromatography is a variant of High Performance Liquid Chromatography (HPLC). Separation and determination of ions is carried out, based on the use of ion exchange resins. This type of chromatography is subdivided into cation and anion exchange chromatography, with the latter featuring most applications.

Applications

With detection by conductivity.

  • Anion analysis (F-, Cl-, NO2-, Br-, NO3-, PO43-, SO42-) in aqueous matrices
  • Cation analysis (Na+, NH4+, K+, Mg2+, Ca2+) in aqueous matrices

Equipment

Dual channel Ion Chromatography system model 861 Advances compact IC (Metrohm), with sequential chemical suppression and samples ultrafiltration. Simultaneous determination of anions and cations with conductivity detector.

ICP-MS Unit

Inductively Coupled Plasma Mass Spectrometry

The analytical technique with the greatest potential for determination of trace level elements in all types of matrices. It is usually necessary to perform a sample digestion. The liquid sample is introduced through a misting system and transformed into a fine spray which is directed towards the torch where a plasma is generated, whose temperature can reach up to 10,000 K, by submitting a flow of argon gas to the action of an oscillating magnetic field induced by a high frequency current. The sample is subjected to various processes (desolvation, vaporisation, atomisation and ionisation). The ions generated pass into the mass spectrometer through a conditioning interface, where they are focused and aimed towards the analyser, usually quadrupole type, where they are separated according to their mass/charge ratio (m/z).

Applications

  • The majority of elements in the periodic table can be analysed using this technique
  • Semi-quantitative multi-element analysis To determine the major and minor elements in a sample. Allows semi-quantitative determinations of elements for which there is no commercial standard with an error lower than 15%
  • Quantitative analysis of elements of interest Linear dynamic range of 8 orders of magnitude (ng/L (ppt) – mg/L (ppm) and low detection limits (ng/L (ppt) for most elements
  • Gauging the isotopic ratios of an element
  • Analysis of small sampling volumes (< 600 uL)
  • Analysing solid biological, organic and inorganic samples by acid digestion and microwave treatments
  • Environmental applications (waters, soils, sediments and residues)
  • Determining metals and possible contaminants in soils (fertilisers) and inland drinking waters (dumping)
  • Speciation of metals in complex matrices
  • Quantification of inorganic nanoparticles

Inductively coupled plasma – mass spectrometer (ICP-MS), model 7700 x (Agilent Technologies). High levels of performance, reliability and automation. Includes a collision cell system in helium mode; greater sensitivity, less background noise, increased removal of spectral interferences and ‘no gas’ mode. Option of coupling separation techniques such as high performance liquid chromatography (HPLC).

Mass Spectrometry Unit

Mass Spectrometry (MS) is a highly sensitive instrumental analytical technique able to quali- and quantitatively assess all types of mixtures of substances. In addition, this technique also determines the molecular mass of a compound, as well at the different fragments resulting from controlled break-up of the same, providing highly valuable information on the molecular structure. Mass Spectrometry is a powerful analytical technique based on the different behaviours of the ions formed by different ionisation techniques when passing through electrical and magnetic fields. The ions are separated according to their mass/charge (m/z) ratio and detected. The great advantage of high-resolution mass spectrometry compared to low resolution is the greater precision and accuracy of the mass, due to the more high-performance features of the time of flight-quadrupole analysers (TOF and QTOF). These allow unequivocal identification of the exact mass of a compound.

Mass Spectrometry Lab

Applications

The laboratory analyses the different types of organic/inorganic contaminants in line with current regulations on maximum residue limits. The following features are highlighted:

  • Analysis of organic micropollutants in waters by GC-MS/MS (organochlorine and organophosphorus pesticides, trihalomethanes, polyaromatic hydrocarbons) by means of LC-MS(TOF) y LC-MS/MS(QTOF) (drug and multi-residue).
  • Determination of impurities in pesticide products.
  • Assays to determine exact mass and fragmentation studies.
  • Identifying compounds, or fragments of the same, by their mass spectrum in comparison with GC-MS libraries.

New analytical methods are constantly being developed to adapt to the new requirements laid down in current legislation on monitoring water quality and control parameters.

Equipment Description
Bidimensional Gas Chromatography/ MS (GC x GC/TOF) equipment. Pegasus 4D GC x GC TOFMS (LECO) and GC model 7890A.
Bidimensional Gas Chromatography/ MS (GC x GC/TOF)equipment. Pegasus 4D GC x GC TOFMS (LECO) and GC model 7890A.
Gas Chromatography / Triple Quadrupole (GC-MS/MS (QqQ)) equipment. GC model 7890A and triple quadrupole detector model 7000. This system is coupled to a Gerstel twister brand Autosampler (MultiPurpose Sampler model 2XL).
Gas Chromatography/Triple Quadrupole (GC-MS/MS (QqQ))equipment. GC model 7890A and triple quadrupole detector model 7000. This system is coupled to a Gerstel twister brand Autosampler (MultiPurpose Sampler model 2XL),
Liquid Chromatography /Triple TOF (LC-QTOF) equipment.
Liquid Chromatography /Triple TOF (LC-QTOF) equipment. Triple TOF 5600 model (AB sciex).
Liquid Chromatography/MS (LC-TOF) equipment
Liquid Chromatography/MS (LC-TOF) equipment
Liquid Chromatography /Triple Quadrupole (LC-MS/MS (QqQ)) equipment. 6495A model, Agilent Technologies.
Liquid Chromatography/Triplex Quadrupole (LC-MS/MS (QqQ)) equipment. 6495A model.
Liquid chromatography system (1290 Infinity II) coupled to mass spectrometry with a triple quadrupole analyser (6495C) (LC-MS/MS(QqQ)). (REACT-UE)

Basic Analysis Unit

In this unit we analyse several physical and chemical parameters laid down in the regulations on control of water quality and dumping.

Basic Analysis Lab

Applications

  • Organoleptic assays: Colour and turbidity
  • Physical-chemical testing: Basic parameters such as pH, conductivity, temperature, redox potential, TKN (Total Kjeldahl Nitrogen), total phosphorus, free and total chlorine, alkalinity, suspended solids (TSS), total organic carbon (TOC), DBO 5, DQO, total nitrogen, etc.

Equipment Description
Particle counter for water samples. This equipment is able to count particles of sizes ranging between 0.2 microns and 2 microns. LS_200 model from Particle Measuring System Inc.
Visible UV spectrophotometer. Measurements at different wavelengths and obtaining Vis-UV spectra of compounds (190-1.100 nm). UV-1800 model from Shimadzu.
Total Organic Carbon (TOC) Analyser. TOC-V CSH model. Shimadzu brand.

Water Laboratory of IMDEA Water belongs since 2009 to the Network of Laboratories of the Community of Madrid with the reference number 267.

The scientific responsible for the laboratory is Dr. Leonor Nozal MartĂ­nez and the technical staff that carries out the tests can be consulted here.