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Analytical Chemistry

The Analytical Chemistry Department provides all of the necessary analytical data in support of ecotoxicology and mammalian toxicology testing.

Analytical data is required to confirm the identity and purity of the test materials used in the studies. Stability, test solution concentration and homogeneity checks are also performed to ensure the solution concentrations are correctly maintained throughout the duration of a toxicology study.

The department also has a wealth of experience in providing and reporting experimental data for the world-wide submission of Plant Protection Products. Using a purpose built facility, testing programs which satisfy the UK PSD, Council Directive 91/414/EEC and the US EPA are routinely undertaken. To support the studies, analytical method validation to satisfy the relevant competent authority is also offered.

 


In addition, SafePharm Laboratories boasts a fully equipped, state of the art analytical laboratory, the techniques and instrumentation of which are detailed below:

Department of Analytical Chemistry Capability Statement
 

Chromatographic Techniques

Gas chromatography is performed using Hewlett-Packard HP5890 and HP6890 gas chromatographs. Each is equipped with a combination of split/splitless, packed and on-column injection parts combined with FID, ECD, NPD, FPD and MSD detector systems. Most systems is equipped with an autosampler and is connected to a Hewlett-Packard ChemstationsTM for instrument control, and data acquisition and processing. An automatic headspace sampler is also available.

Liquid chromatography is performed using Hewlett-Packard HP1050, HP1090 and HP1100 high performance liquid chromatographs. LCMS is performed using a Agilent 1100 Series LC-MSD. Each is equipped with a gradient pumping system, autosampler and UV/Vis detector. Other detectors, fluorescence, pulsed electrochemical, conductivity, differential refractometry and evaporative light scattering are available and can be configured into each system. Each system is connected to a Hewlett-Packard ChemstationsTM for instrument control, and data acquisition and processing.

Gel permeation chromatography is performed using two Waters systems. One system consists of a 600E pump controller, WISPTM 700 autosampler, 994 diode array detector and 410 differential refractometer, the other consists of an AllianceTM HPLC system with 2487 UV/Vis detector and 2410 differential refractometer. Each system is connected to a Millennium 32TM workstation for instrument control and data acquisition and processing.

Spectroscopic Techniques

UV/Vis spectrophotometry is performed using either a Perkin Elmer Lambda 20 or Lambda 2 spectrophotometer. The Lambda 20 is connected to a UVWINLABTM workstation, the Lambda 2 to a PECCSTM workstation to provide instrument control, and data acquisition and processing.
IR spectrophotometry is performed using a Perkin Elmer 1620 FTIR spectrophotometer. Data processing is carried out using Perkin Elmer Report ManagerTM software.

Atomic spectrophotometry is carried out on a Perkin Elmer PE 1100 AAS capable of use for both absorption and emission spectroscopy.

 
External Facilities
 

SafePharm laboratories Limited has recently forged close links with Universities enabling us to extend the already extensive range of analytical instrumentation available.

A Jeol DX 303 high resolution mass spectrometer with a DA 5000 data system enhances the services offered by providing GC-MS using electron impact (EI), chemical ionisation (CI) and fast atom bombardment (FAB) isonisation techniques.

A sophisticated Joel GSX 270 MHz FT-NMR spectrometer offers 1H and 13C capabilities allowing important structural information to be gained from nOe, DEPT, INEPT, COSY and Inadaquate-2D spectra for example.
Supporting these techniques is a highly experienced team of experts able to offer specialised interpretational skills. In association with the expertise within SafePharm a highly specialised structural characterisation service can be offered.

 
Physico-Chemical Properties
 

SafePharm are able to offer an extensive range of services to the agrochemical industry, including determining 'Physical and Chemical Properties of the Active Substance' and 'Physical and Technical Properties of the Plant Protection Product', in accordance with Council Directive 91/414/EEC. In addition to this, we can offer testing for US EPA in accordance with FIFRA legislation.

With a large, world-wide client base SafePharm has over ten years experience in providing the necessary scientific and technical procedures to fulfil the requirements for regulatory submission for all types of active ingredients and plant protection products.

Study design and reporting are always such that they satisfy regulatory requirements and can be tailored to meet customer preferences.

Services offered include, but are not limited to the following :

  • Analytical method development and validation
  • Analytical profile of batches
  • Accelerated and real time storage stability studies
  • CIPAC testing
  • Testing as required for purified active substances, technical substances and plant protection formulated products ECs, SCs, WGs, CSs etc.

A purpose-built testing station allows for a wide range of hazardous physico-chemical testing including :

  • Flammability
  • Auto-flammability
  • Flash point
  • Explosive properties
  • Oxidizing properties

Melting and Boiling Point determinations are preformed routinely using a Mettler Toledo DSC12E Differential Scanning Calorimeter.

Vapour pressure is determined using a custom built Vapour Pressure Balance.

Trace analysis if metals is also determined by voltammetry using a Metrohmn 757 VA Computrace analyser.

 
 
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