TGA-FTIR-GCMS

The non-conventional high-sensitive thermogravimetric analyzer (TGA), in-line coupled with an infrared and a mass spectroscope (FTIR, MS) and a gas chromatograph (GC), all from Perkin Elmer, enables to achieve exhaustive and complementary information about the amount and nature of gas evolved during thermogravimetric analysis. The simultaneous measurements FTIR-GCMS are obtained by a propietary interface (Trlogy, from Red Shift) with a pressurized and heated  (up to 350 °C) transfer line.

The high sensitivity ultra-microbalance TGA (Pyris 1), sensitivity: 0.1 μg, works in a temperature range from ambient to 1000 °C, with standard furnace, and from 50 to 1500°C with the high temperature furnace. The installed furnace chiller allows operation from sub-ambient temperature (-20 °C) and enables measurement also of ultra-volatile gases adsorbed on particle surface.

The Gas Chromatograph/Mass Spectrometer (Clarus® 560 S/500S) delivers high-sensitivity analyses through a combination of state-of the-art electronics and ion optics, the widest mass range (1-1200 u.a) and high scanning rates. The MS may acquire spectra in full scan mode or in Selected Ion Monitoring (SIM). The GC is equipped with a nonpolar fused silica capillary column (DB5 MS) coated with a 5% diphenyl-dimethylpolysiloxane stationary phase.

The FT- Infrared spectroscope (Spectrum 100T) is equipped with a DLaTGS detector, operates in the 8300 a 350 cm-1 range with a resolution of 0,4 cm-1

Technical features

The termogravimetric balance

TGA Design: A vertical design with a high sensitivity balance and quick response furnace. The balance is located above the furnace and is thermally isolated from it. A precision hang-down wire is suspended from the balance down into the furnace. At the end of the hang-down wire is the sample pan. The sample pan’s position is reproducible.

Sample Atmosphere: Static or dynamic, including nitrogen, argon, helium, carbon dioxide, air, oxygen, or other inert or reactive gases. Analyses done at normal or reduced pressures

Standard Furnace Temperature Range: Subambient to 1000°C
Scanning Rates: 0.1°C/minute to 200°C/minute
Temperature Precision: ±2°C

High Temperature Furnace Temperature Range: 50°C to 1500°C
Scanning Rates: 0.1°C/minute to 50°C/minute
Temperature Precision: ±5°C

Balance Tare: Reproducible to ±2 μg
Sensitivity: 0.1 μg
Accuracy: Better than 0.02%
Precision: 0.001%
Capacity: 1300mg

Sample Mass Range Up to 1300 mg

Cooling Forced air cooled with an external fan and internal booster purge
Standard Furnace: 1000°C to 40°C in less than 15 minutes under normal operation
High Temp Furnace: 1500°C to 100°C in less than 30 minutes under normal operation

Gas Switching Fast, thorough and efficient due to reduced furnace volume
Less than 3 minutes to purge the sample area of ambient gases (remove 99% of oxygen) and replace the volume with an inert purge gas 10 minutes to achieve a 99.99% oxygen-free environment

The mass spectrometer

Mass range 1.0-1200 u (amu)

Detector Sealed long-life photomultiplier

Analyzer Quadrupole with prefilter: 131 mm x 12 mm circular rods; 16 mm x 12 mm prefilter rods
Mass stability ±0.1 m/z mass accuracy over 48 hours

EI voltage 10-100 eV

Pump Air-cooled 75-L/sec turbomolecular

Vacuum gauge Standard, single wide-range gauge for all pumping options

GC transfer line Settable from 20 °C to 350 °C

Ion source emperature settable up to 350 °C; No wires – plug and play

Scan rate Up to 12,500 amu/sec

Maximum Up to 65 scans/second full scan, depending on mass range

Acquisition rate Up to 100 scans/second, selected ion monitoring (SIM)

Linear dynamic range Electronic: 106-107 depending on acquisition rate

Scan functions/run 32 sets (full scan/SIM) of up to 32 ions per function

Sensitivity Test: EI full scan Amount: 1 pg of octafluoronaphthalene

Detection Limits: (S/N) 150:1 RMS at m/z 272