Department of Chemical Organic Technology and Petrochemistry RCH 5

Gas chromatograph coupled with a mass spectrometer (GC-MS)

• The GC-MS device (Agilent Technologies 7890A/5975C) can perform tests in the EI and CI ionization system
• Possibility to analyze liquid samples that must be prepared in the following solvents, e.g.: methanol, water, acetone, hexane, diethyl ether, hexane, ethyl acetate
• It is possible to directly introduce the sample into the MS (DIP probe)

Gas chromatographs (GC)

• Gas chromatograph (Clarus 500 GC system, PerkinElmer) is equipped with two detectors:
  • flame ionization detector FID (Flame Ionization Detector)
  • electron capture detector ECD (Electron Capture Detector)
• Gas chromatograph (GC-2010 Plus, Shmadzu) equipped with:
  • flame ionization detector FID (Flame Ionization Detector)

Ultra-high-performance chromatograph coupled with a mass spectrometer (UPLC MS/MS)

• UPLC MS/MS system (ACQUITY UPLC system and Xevo G2 QTof by Waters Corporation) equipped with:
  • PAD diode array detector (ACQUITY Photodiode Array Detector)
  • Fluorescence detector (ACQUITY Fluorescence Detector)
  • ELS (ACQUITY Evaporated Light Scattering Detector)
  • Autosampler (ACQUITY Autosampler)
• Mass spectrometer (Xevo G2 QTof, Waters Corporation) with a hybrid quadrupole analyzer – time of flight TOF (Time of Flight); equipped with:
  o atmospheric pressure ionization module (API) with an electrospray probe (ESI) and an APCI chemical ionization probe at atmospheric pressure
• The UPLC MS/MS system enables the separation of mixtures of compounds and their simultaneous analysis using a mass spectrometer
• The mass spectrometer allows the use of two types of ionization: ESI and APCI
• Positive and negative ionization is possible, as well as the ability to work in two resolution options: Sensitivity mode and Resolution mode
• The mass spectrometer allows the probe to be used to analyze solid samples in the atmospheric pressure ionization mode
• Samples can also be introduced into the MS spectrometer directly, without the involvement of UPLC

High performance liquid chromatograph (HPLC)

• HPLC (Waters 2690 system, Waters Corporation) enables qualitative and quantitative analysis of samples containing compounds in liquid or solid form.
• High-performance liquid chromatograph equipped with:
  • PAD diode array detector (PhotodiodeArrayDetector, Waters 2996)
  • autosampler (Waters 717 plus Autosampler).

Pressure reactors

• The Department offers the opportunity to conduct research using pressurized reactors. We have various types of reactors, differing in volume and operating parameters, including:
• Pressure reactor from “Autoclave Engineers Inc. USA” with parameters and equipment:
  • with a volume of 100 ml,
  • made of Hastelloy C 276 steel,
  • maximum operating temperature 315°C,
  • maximum working pressure: 200 bar,
  • mixer with a speed range of up to 3600 rpm,
  • sampling port, an automatic valve for conducting flow processes,
  • digital temperature and mixing controller.
• Pressure reactor from “PARR” with parameters and equipment:
  • with a volume of 600 ml,
  • a glass vessel or made of Hastelloy C 276 steel,
  • maximum operating temperature 225°C,
  • maximum working pressure: 10 bar (glass reactor) and 65 bar (metal reactor),
  • a mixer with a speed range of up to 1700 rpm,
  • sampling port,
  • digital temperature and mixing controller,
  • gas burette for measuring oxygen consumption,
  • reflux condenser with receiver.
• EasyMax™ 102 research station, for conducting processes under atmospheric and increased pressure:
  • a reaction system for carrying out parallel syntheses using both glass reactors with volumes ranging from 1 to 100 ml and a pressure reactor with a volume of 100 ml
  • EasyMax™ 102 system is a compact heating technology system allowing simultaneous, independent operation of two reactors in the temperature range from -25°C to 160°C
  • The station is equipped with a pressure reactor with a capacity of 100 ml EM-60-100-SS-HC and a permissible pressure of 60 bar
  • The system also has a set of gas consumption control up to 100 bar M100, which allows you to calculate the gas consumed in the reaction expressed in moles. Based on the recorded pressure drops during the reaction, the program calculates gas consumption
  • EasyMax™ 102 system provides control of heating/cooling (in reaction temperature Tr and jacket temperature Tj), mixing rates and displays measurement curves online
  • Each reactor chamber has a built-in magnetic stirrer or mixing can be provided by a mechanical stirrer
  • A built-in window on the front of the thermostat with backlight allows you to view the reaction mixture during the process

Automatic reactor with FTIR analytical module

• The reactor with an in-situ FT-IR probe allows you to track the reaction in real time and observe reactive species whose analysis is not possible using off-line methods. Camera parameters and equipment:
  • RC1e reaction calorimeter operating in the temperature range from -50 to +230°C, with the ability to measure the thermal effect of the reaction in real time.
  • Glass reaction vessels with a volume of 500 cm³ and 2000 cm³.
  • Temperature range of the heating and cooling jacket: from -53 to +180°C, pressure range: from 0 to 1 bar.
  • Mixer drive enabling control of the rotational speed in the range from 0 to 1500 rpm. and torque measurement.
  • Dosing pumps for dosing raw materials into the reactor or receiving the product in the case of a continuous process.
  • pH probes enabling measurement in the range from 0 to 14 pH. Possibility to stabilize the pH of the reaction mixture by dosing acid or base.
  • Mettler-Toledo iC10 FT-IR spectrometer with ATR probe. Measuring range from 4000 to 650 cm-1. Resolution 4, 8 or 16 cm-1. Operating temperature range from -80 to +200°C.
  • Set for dosing and measuring gas consumption.
  • Mettler-Toledo OFS12H-4071 turbidity sensor made of HC-22 alloy and Trb8300D transducer. This device is used to measure the turbidity of the reactor contents. Using it, it is possible to determine the solubility curve and the metastable area in crystallization processes depending on temperature and pH. The additional use of infrared spectroscopy (FTIR) makes it possible to determine the degree of solution supersaturation, as well as the dependence of solubility on the solvent composition.
    o Distillation set with automatic reverse control and measurement of the heat of condensation.
• Software capabilities:
  • Controlling the reactor operation according to the introduced procedure.
  • Manual control.
  • Collecting and processing data from sensors.
  • Import and export of data from/to external programs, and import of data from previous experiments for comparison purposes.
  • Analysis of the thermal safety of the process – predicting the behavior of the reaction mixture in the event of a cooling failure and, on this basis, assigning an appropriate risk category.

Automatic digital polarimeter

• JASCO P-2000 five-band polarimeter is a fully automatic, high-accuracy device enabling quick and precise examination of light polarization in samples
  • It is possible to measure dark samples
  • The polarimeter enables quick measurement, reading and archiving in various operating modes. The instrument directly measures rotation, specific rotation, concentration, sugar content, Brix and optical purity.

UV-VIS spectrophotometer

• JASCO V-650 dual beam spectrophotometer
  • Allows for quantitative analysis, measurements as a function of wavelength, as a function of time, for a constant wavelength

Compact Karl Fischer titration apparatus

• 915 KF Ti-Touch is a volumetric Karl Fischer titration apparatus
  • Autonomous titrator with maximum integration of system components
  • Precise and safe handling of KF reagents thanks to the Dosino dosing system and integrated diaphragm pump
  • FDA Compliance: Meets FDA 21 CFR requirements