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Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Presentation of Tim Brunst in the context of his Masters Thesis Institute for

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KIT – University of the State of Baden-Wuerttemberg and National Research Center of the Helmholtz Association Institute for Technical Physics – Tritium Laboratory Karlsruhe

www.kit.edu

Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Presentation of Tim Brunst in the context of his Master‘s Thesis

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Institute for Technical Physics Tritium Laboratory Karlsruhe 2 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Closed tritium cycle of fusion reactors

Brunst, Tim:

Storage / Delivery Torus Torus D + T 4He + n + 17,6 MeV D2,T2

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Institute for Technical Physics Tritium Laboratory Karlsruhe 3 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Closed tritium cycle of fusion reactors

Brunst, Tim:

Detriitiation / exhaust treatment Storage / Delivery Torus Torus

4He, T2, D2, …

D + T 4He + n + 17,6 MeV D2,T2

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Institute for Technical Physics Tritium Laboratory Karlsruhe 4 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Closed tritium cycle of fusion reactors

Brunst, Tim:

Isotopologue separation Storage / Delivery Torus Torus D2,T2 H2, D2, T2, HD, HT, DT

4He, T2, D2, …

D + T 4He + n + 17,6 MeV H2 D2,T2 Exhaust Detriitiation / exhaust treatment Large amounts (~kg/h) of hydrogen (H, D, T) must be recycled continuously.

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Institute for Technical Physics Tritium Laboratory Karlsruhe 5 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

How do we separate hydrogen isotopologues?

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 6 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

How do we separate hydrogen isotopologues?

Brunst, Tim:

Cryogenic distillation.

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Institute for Technical Physics Tritium Laboratory Karlsruhe 7 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

How do we separate hydrogen isotopologues?

Brunst, Tim:

Cryogenic distillation. Tritium Enrichment Test Assembly (TRENTA)

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Institute for Technical Physics Tritium Laboratory Karlsruhe 8 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

TRENTA and cryogenic distillation

Brunst, Tim:

hot cold

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Institute for Technical Physics Tritium Laboratory Karlsruhe 9 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

TRENTA and cryogenic distillation

Brunst, Tim:

Input Improved separation through several distillation steps Condenser Column Reboiler

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Institute for Technical Physics Tritium Laboratory Karlsruhe 10 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

TRENTA and cryogenic distillation

Brunst, Tim:

Isot. TB /K

(1 bar)

H2 20.3 HD 22.1 HT 22.9 D2 23.6 DT 24.4 T2 25.0

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Institute for Technical Physics Tritium Laboratory Karlsruhe 11 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

TRENTA and cryogenic distillation

Brunst, Tim:

Continuous, real-time monitoring of column content necessary Isot. TB /K

(1 bar)

H2 20.3 HD 22.1 HT 22.9 D2 23.6 DT 24.4 T2 25.0

Every isotopologue can occur highly concentrated

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Institute for Technical Physics Tritium Laboratory Karlsruhe 12 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

How do we monitor the column content?

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Institute for Technical Physics Tritium Laboratory Karlsruhe 13 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

How do we monitor the column content? Infrared spectroscopy.

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Institute for Technical Physics Tritium Laboratory Karlsruhe 14 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

How do we monitor the column content? Infrared spectroscopy. Tritium Absorption Infrared Experiment (TApIR)

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Institute for Technical Physics Tritium Laboratory Karlsruhe 15 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Monitoring with TApIR

Brunst, Tim:

IR source Analyser „white“ light Total spectrum

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Institute for Technical Physics Tritium Laboratory Karlsruhe 16 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Monitoring with TApIR

Brunst, Tim:

IR source Sample Detector Analyser „white“ light Total spectrum Absorption spectrum Absorption length

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Institute for Technical Physics Tritium Laboratory Karlsruhe 17 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Monitoring with TApIR

Brunst, Tim:

peak position

concentration of isotopologues type of isotopologues

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Institute for Technical Physics Tritium Laboratory Karlsruhe 18 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Non-linear calibration functions

Brunst, Tim:

Trend unpredictable

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Institute for Technical Physics Tritium Laboratory Karlsruhe 19 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Non-linear calibration functions

Brunst, Tim:

Calibration spectra of the entire phase space of concentrations Trend unpredictable

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Institute for Technical Physics Tritium Laboratory Karlsruhe 20 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Calibration with reference samples

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 21 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Calibration with reference samples

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 22 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Calibration with reference samples

Brunst, Tim:

Calibration through extrapolation to highly concentrated HD

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Institute for Technical Physics Tritium Laboratory Karlsruhe 23 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Objectives

Production of highly concentrated HD (>50%) Cryogenic distillation with TRENTA

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 24 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Objectives

Production of highly concentrated HD (>50%) Cryogenic distillation with TRENTA Verification of extrapolated calibration of TApIR Comparison with other spectroscopic systems

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 25 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Objectives

Production of highly concentrated HD (>50%) Cryogenic distillation with TRENTA Verification of extrapolated calibration of TApIR Comparison with other spectroscopic systems Stability analysis of highly concentrated HD Long-term measurements in gaseous and liquid phase

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 26 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Production of highly concentrated HD

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 27 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Production of highly concentrated HD

Brunst, Tim:

Extraction

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Institute for Technical Physics Tritium Laboratory Karlsruhe 28 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Production of highly concentrated HD

Brunst, Tim:

Extraction Simulation to determine operating parameters

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Institute for Technical Physics Tritium Laboratory Karlsruhe 29 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Production of highly concentrated HD

Brunst, Tim:

Input preparation Catalysis Distillation HD Extraction RUN A

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Institute for Technical Physics Tritium Laboratory Karlsruhe 30 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Production of highly concentrated HD

Brunst, Tim:

Input preparation Catalysis Distillation HD Extraction RUN A RUN Amount (ls) HD concentration (%) A 138 80.1 B 150 85.8 Goal achieved: HD concentration >50%

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Institute for Technical Physics Tritium Laboratory Karlsruhe 31 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Objectives

Production of highly concentrated HD (>50%) Cryogenic distillation with TRENTA Verification of extrapolated calibration of TApIR Comparison with other spectroscopic systems Stability analysis of highly concentrated HD Long-term measurements in gaseous and liquid phase

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 32 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Comparison of spectroscopic methods

Brunst, Tim:

Gaseous sample in Raman cell Raman scattering of the laser photons Spectroscopic investigation of scattered light Extraction of 3 l/h from the sample Ionisation of isotopologues Mass-to-charge ratio selection in an electrical field

Raman System Quadrupole Mass Spectrometer

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Institute for Technical Physics Tritium Laboratory Karlsruhe 33 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Comparison of spectroscopic methods

Brunst, Tim:

RUN A

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Institute for Technical Physics Tritium Laboratory Karlsruhe 34 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Comparison of spectroscopic methods

Brunst, Tim:

RUN A Usage of extrapolated calibration leads to deviations. IR calibration has to be expanded for highly concentrated HD.

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Institute for Technical Physics Tritium Laboratory Karlsruhe 35 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Summary

Simulation of TRENTA cryogenic distillation performance with non-radioactive isotopologues developed

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 36 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Summary

Simulation of TRENTA cryogenic distillation performance with non-radioactive isotopologues developed Method for the production of large amounts of highly concentrated HD with TRENTA developed

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 37 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Summary

Simulation of TRENTA cryogenic distillation performance with non-radioactive isotopologues developed Method for the production of large amounts of highly concentrated HD with TRENTA developed Three relevant spectroscopic methods at TLK compared and necessity for expansion of IR calibration identified

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 38 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Summary

Simulation of TRENTA cryogenic distillation performance with non-radioactive isotopologues developed Method for the production of large amounts of highly concentrated HD with TRENTA developed Three relevant spectroscopic methods at TLK compared and necessity for expansion of IR calibration identified Worldwide first two data points of highly concentrated HD in liquid phase for IR calibration measured

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 39 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Thank you for your attention. Questions?

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 40 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Appendix

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 41 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

Exemplary IR spectrum

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Institute for Technical Physics Tritium Laboratory Karlsruhe 42 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

Exemplary Raman spectrum

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Institute for Technical Physics Tritium Laboratory Karlsruhe 43 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

Exemplary QMS spectrum

Rein, A. 2015. Abschätzung und Analyse von Verunreinigungen in Kalibriergasmischungen für das Tritium-Hydrogen-Deuterium-Experiment (TRIHYDE), Masterarbeit, Karlsruher Institut für Technologie

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Institute for Technical Physics Tritium Laboratory Karlsruhe 44 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

IR absorption measurements

Brunst, Tim:

Vibration Rotation H2 T2 D2 HD HT DT Q2 ∆𝜘 ∆𝐾

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Institute for Technical Physics Tritium Laboratory Karlsruhe 45 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Dimers – double transitions

Brunst, Tim: Wozniewski, S. 2014. Relative Kalibrierung der IR-Absorptionsspektren gegen die 𝐼2-, HD- und 𝐸2-Konzentrationen, Bachelorarbeit, Karlsruher Institut für Technologie.

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Institute for Technical Physics Tritium Laboratory Karlsruhe 46 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

Exemplary Raman spectrum

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Institute for Technical Physics Tritium Laboratory Karlsruhe 47 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

Boiling-point diagram

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Institute for Technical Physics Tritium Laboratory Karlsruhe 48 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

Distillation set-up

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Institute for Technical Physics Tritium Laboratory Karlsruhe 49 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

Simulated column content

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Institute for Technical Physics Tritium Laboratory Karlsruhe 50 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Production of highly concentrated HD

Brunst, Tim:

Input preparation Catalysis Distillation HD Extraction Recycling RUN B

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Institute for Technical Physics Tritium Laboratory Karlsruhe 51 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

Distillation cycles

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Institute for Technical Physics Tritium Laboratory Karlsruhe 52 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe Brunst, Tim:

Column profile

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Institute for Technical Physics Tritium Laboratory Karlsruhe 53 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

LARA (Laser Raman System)

Brunst, Tim:

Gaseous sample in Raman cell Raman scattering

  • f the laser photons

Spectroscopic investigation of scattered light

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Institute for Technical Physics Tritium Laboratory Karlsruhe 54 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

LARA (Laser Raman System)

Brunst, Tim:

Gaseous sample in Raman cell Raman scattering

  • f the laser photons

Spectroscopic investigation of scattered light

Linear calibration functions for all isotopologues

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Institute for Technical Physics Tritium Laboratory Karlsruhe 55 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

mQMS (mobile Quadrupole Mass Spectrometer)

Brunst, Tim:

Extraction of 3 l/h from the sample Ionisation of isotopologues Mass-to-charge ratio selection in an electrical field

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Institute for Technical Physics Tritium Laboratory Karlsruhe 56 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

mQMS (mobile Quadrupole Mass Spectrometer)

Brunst, Tim:

Extraction of 3 l/h from the sample Ionisation of isotopologues Mass-to-charge ratio selection in an electrical field

calibration functions H2, HD: linear D2: second order

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Institute for Technical Physics Tritium Laboratory Karlsruhe 57 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Comparison of spectroscopic methods

Brunst, Tim:

RUN B

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Institute for Technical Physics Tritium Laboratory Karlsruhe 58 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Stability analysis

Brunst, Tim:

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Institute for Technical Physics Tritium Laboratory Karlsruhe 59 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Stability analysis

Brunst, Tim:

RUN A

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Institute for Technical Physics Tritium Laboratory Karlsruhe 60 16-06-27 Production and Utilisation of highly concentrated HD for the Validation of the Calibration of Hydrogen Analysis Systems at the Tritium Laboratory Karlsruhe

Stability analysis

Brunst, Tim:

RUN B