Determine Hydrogen Concentration in New Materials Using the G4 PHOENIX

The G4 PHOENIX DH hot extraction analyzer from Bruker is the ideal solution for accurate and fast diffusible hydrogen measurement to prevent hydrogen-induced cracking, embrittlement, and other expensive failures.

Hydrogen-induced damage is a common and worrying occurrence. It reveals in such a manner that a component fails under the impact of mechanical stress—even without a visible sign. Thus, hydrogen in welds or steel is important to evaluate because of hydrogen-induced cracking or hydrogen-assisted cracking (HIC/HAC), embrittlement, or hydrogen-delayed fracture among other damaging effects. Getting accurate information about the hydrogen concentration in the material is vital for quality control and in developing new materials.

The G4 PHOENIX DH, applying the carrier gas hot extraction technique, facilitates a quick and automatic determination of diffusible hydrogen in a wide range of matrices. The evolved hydrogen is sensed by a sensitive and long-term stable thermal conductivity detector (TCD). Simple and dependable calibration is ensured by the in-built, automatic gas dosing unit having 10 different volumes.

The analyzer is fitted with a quick heating (and cooling) infrared-heated clamshell furnace (up to 900 °C). The quartz tube with a diameter of 30 mm allows the examination of large samples like steel sheet strips as well as weld coupons according to AWS A4.3 and ISO 3690. The versatile infrared furnace also allows the use of temperature programs and ramping to evaluate information about various forms of trapped hydrogen.

For higher temperatures, particularly for the determination of both diffusible hydrogen and residual hydrogen, for example, in steel, the G4 PHOENIX DH can be fitted with an extra wire-heated tube furnace, operable at temperatures up to approximately 1100 °C.

The groundbreaking new method of coupling a mass spectrometer to the carrier gas hot extraction analyzer G4 PHOENIX DH, enhances the limit of detection by over one order of magnitude compared to a TCD. It also allows the determination of ultra-low hydrogen concentrations, for example, in high-strength steels. Apart from providing selectivity, for example, for isotopic species such as deuterium, this Thermal Desorption Mass Spectrometry (TDMS) method offers kinetic information relating to the diffusible hydrogen when used along with various heating rates.

Software

The G4 PHOENIX’s intuitive analysis software offers a clear user interface. Various tasks from the user’s workflow like method setup, calibration, measurement, and data evaluation are plainly separated into different views.

Diffusible Hydrogen Analyzer G4 PHOENIX - Analysis Screen

Diffusible Hydrogen Analyzer G4 PHOENIX - Analysis Screen

Features and Benefits

  • Fast heating (and cooling) infrared tube furnace provides wide-ranging analytical functionalities in temperature programming (steps and ramps)
  • Quartz tube diameter of 30 mm allows the investigation of large samples such as weld coupons and steel sheet strips according to ISO 3690 and AWS A4.3
  • Automatic and dependable gas calibration with helium or hydrogen over the whole measurement range by means of the integrated gas dosing unit with 10 distinct volumes
  • Optional quadrupole mass spectrometer enhances the detection limit by over one order of magnitude, thus enabling the assessment of ultra-low diffusible hydrogen concentrations and evaluation of various hydrogen traps in steel

Technical Details

Measuring Range

  • 0.05–1000 μg/g hydrogen

Hot Extraction Furnaces

  • Infrared furnace: 900 °C maximum, quartz tube diameter 30 mm
  • Wire-heated furnace: 1100 °C maximum, quartz tube diameter 18 mm

Analysis Time*

  • Approximately 3 minutes to 2 hours
  • For weld samples normally 15–20 minutes

* Depending on sample material, weight, and analysis temperature

Resolution

  • 0.01 μg/g

Precision*

  • ±0.05 μg/g or 1 % RSD (whichever is greater)

* Depending on sample material, weight, and analysis temperature

Carrier Gas

  • Nitrogen 99.999% purity, minimum pressure 2 bar (~50 psi)

Cooling Water

  • Approximately 1 l/minute (only for IR furnace and only when heating)

Dimensions and Weight

  • 630 x 640 x 650 mm (WxDxH); 50 kg
  • 24.8 x 25.2 x 25.6”; 110 lbs.

Electrical Supply

  • Analyzer: 230 VAC, 50/60 Hz, 1 kVA
  • Peripherals: 230 VAC, 50/60 Hz, 300 VA

PC Requirements

  • Standard WindowsTM-PC, operating system Windows XP/7*
  • HDD > 200 GB, DVD drive, two serial ports RS 232

*Windows is a registered trademark of Microsoft Corporation

Optional Mass Spectrometer

Detection limit

  • 50–100 ppb hydrogen at 1 g sample weight

m/z range

  • 1–100 amu, optimized for mass 2 (hydrogen)
  • Calibration

With H2 gas via the gas dosing unit G4 PHOENIX DH

  • 230 VAC, 50/60 Hz, 250 VA
  • Electrical supply

Dimensions and weight

  • 24.8 x 25.2 x 18.9”; 132 lbs.
  • 630 x 640 x 480 mm (WxDxH), approximately 60 kg

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