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This international round robin test served to scrutinize the procedures specified in ISO/DIS 3690:2009 for determining the diffusible hydrogen content in weld metals with bcc-lattice structure. It was specifically intended to check in what respect the specifications defined in the indicated standards for specimen preparation, storage and hydrogen analysis provide comparable measurement results. The round robin test is presented comprising comparative measurements at various degassing temperatures using hot extraction techniques and a thermal conductivity detector (TCD). A major focus of this investigation was the examination of the maximum degassing temperature for analysing the diffusible hydrogen in materials with bcc-lattice structure. The analyses were performed using two different stick electrodes and three different filler wires. As a significant result it was found that no deviations or increases, were detected in the measured contents of diffusible hydrogen for the investigated degassing temperatures ranging between 45 degrees C and 400 degrees C. Hydrogen analyses for contents below HD = 1.5 ml/100 g with the hot extraction techniques in conjunction with TCD applied in this study led to considerable relative standard deviations.
Comparative study between hot extraction methods and mercury method - a national round robin test
(2010)
Comparative study between hot extraction methods and mercury method - a national round robin test
(2010)
A round robin test is presented comprising comparative measurements using hot extraction at different degassing temperatures as well as the mercury method. A major focus of the investigation was verification of the maximum degassing temperature for analysing the diffusible hydrogen in weld metals with bcc-lattice structure. The analyses were executed using a basic stick electrode with high weld metal cracking, a high-alloyed supermartensitic filler wire with different hydrogen contents in the shielding gas and a high-strength solid wire. The results show that degassing temperatures of 150 degrees C and 400 degrees C do not lead to an increase in the measured contents of diffusible hydrogen as compared to measurements at room temperature. The measuring techniques and procedures specified in ISO/DIS 3690:2009 for determining the diffusible hydrogen content in weld metals with bcc-lattice structure yield approximately the same results. This is to say that the mercury method and the hot extraction methods with thermal conductivity detector (TCD) can be regarded as equivalent reference methods.
The purpose of the present study is to show the feasibility of examining hydrogen desorption in technical iron samples using neutron radiography at the ANTARES facility of the FRM II research reactor, Technische Universität München. It has been shown that this method is appropriate for in situ determination of hydrogen Desorption for concentrations as low as 20 ppmH. Experiments were carried out in the temperature range from room temperature up to 260 °C. Measurement was based on direct comparison between electrochemically hydrogen-loaded iron samples and hydrogen-free reference samples at the same temperature.
This enables the determination of hydrogen concentration as a function of time and temperature. Ex situ carrier gas hot extraction experiments using the same temperature–time profiles as the neutron radiography experiments have been used to calibrate the greyscale values of the radiographs to defined hydrogen concentrations. It can be stated that hydrogen desorption correlates with sample temperature.
Thermo Analytic Investigation of Hydrogen Effusion Behavior - Sensor Evaluation and Calibration
(2011)
The well established carrier gas analysis (CGA) method was used to test different hydrogen detectors comprising a thermal conductivity detector (TCD) and a metal oxide semiconducting (MOx) sensor. The MOx sensor provides high hydrogen sensitivity and selectivity, whereas the TCD exhibits a much shorter response time and a linear hydrogen concentration dependency. Therefore, the TCD was used for quantitative hydrogen concentration measurements above 50?µmol/mol. The respective calibration was made using N2/H2 gas mixtures. Furthermore, the hydrogen content and degassing behaviour of titanium hydride (TiH2-x) was studied. This material turned out to be a potential candidate for a solid sample calibration. Vacuum hot extraction (VHE) coupled with a mass spectrometer (MS) was then calibrated with TiH2-x as transfer standard. The calibration was applied for the evaluation of the hydrogen content of austenitic steel samples (1.4301) and the comparison of CGA-TCD and VHE-MS.
In this study, hydrogen absorption and diffusion were investigated for various high-alloyed ferritic-austenitic duplex steels. On account of the specific transformation and solidification behaviour, respectively, of duplex steels as compared to single-phase ferritic and austenitic steels, special conditions have to be considered concerning hydrogen absorption which may ultimately lead to microstructure-dependent hydrogen-assisted weld metal cracking. Hydrogen absorption during welding may occur via the shielding gas, moisture from the surroundings or via the welding filler material. As a contribution to the interpretation and prediction of hydrogen-induced cracking in welded duplex steels, the actual hydrogen absorption via the arc as well as the weld metal hydrogen diffusion was investigated for the first time in a duplex steel DS (1.4462), a super duplex steel SDS (1.4501) and in a lean duplex steel LDS (1.4162). Isothermal heat treatment using carrier gas hot extraction enabled quantification of the amounts of hydrogen trapped in the respective microstructure areas. The hydrogen diffusion coefficients were determined by analytical and numerical calculation. The total hydrogen concentrations and the diffusion coefficients were found to be nearly identical. Trapped hydrogen was however observed to be dependent on the material and on the microstructure condition. The influence of hydrogen on the mechano-technological properties of the weld metal was characterized with the help of tensile tests. In addition, the hydrogen embrittlement effect was detected in scanning electron microscopic analyses.
Revealing hydrogen embrittlement mechanisms in steels is of great interest to scientists and engineers. Neutron radiography makes it possible to measure in-situ hydrogen diffusion with high spatial and temporal resolution at concentrations as low as 20 ppm. We compare hydrogen-charged specimens with hydrogen-free reference specimens and use calibration standards to normalize the hydrogen concentrations. This allows quantitative tracking of the hydrogen concentration evolution as a function of time, space and temperature. Furthermore, a view into the material with 'neutron eyes' facilitates the detection of cavities that contain molecular hydrogen.
Hydrogen generally causes lattice distortions and phase transformations when introduced into a metallic crystal lattice. For the investigations reported in this contribution, hydrogen thermal desorption analysis has been carried out to observe the influence of hydrogen desorption on the lattice of super martensitic stainless steel during continuous heating. The lattice expansion parameter and the phase transformations have been monitored during the thermal desorption process, and the influence of hydrogen on such characteristics has been evaluated. It was found that hydrogen has a significant influence on both the lattice parameter and on the thermal expansion. However, hydrogen has no influence on phase transformation during thermal desorption. The hydrogen's desorption behavior in this process was also observed and it turned out that hydrogen desorbs in two stages, i.e., firstly diffusible hydrogen and trapped hydrogen afterward.