X-ray fluorescence analysis of metal distributions in cryogenic biological samples using large-acceptance-angle SDD detection and continuous scanning at the Hard X-ray Micro/Nano-Probe beamline P06 at PETRA III

J Synchrotron Radiat. 2020 Jan 1;27(Pt 1):60-66. doi: 10.1107/S1600577519014048. Epub 2020 Jan 1.

Abstract

A new Rococo 2 X-ray fluorescence detector was implemented into the cryogenic sample environment at the Hard X-ray Micro/Nano-Probe beamline P06 at PETRA III, DESY, Hamburg, Germany. A four sensor-field cloverleaf design is optimized for the investigation of planar samples and operates in a backscattering geometry resulting in a large solid angle of up to 1.1 steradian. The detector, coupled with the Xspress 3 pulse processor, enables measurements at high count rates of up to 106 counts per second per sensor. The measured energy resolution of ∼129 eV (Mn Kα at 10000 counts s-1) is only minimally impaired at the highest count rates. The resulting high detection sensitivity allows for an accurate determination of trace element distributions such as in thin frozen hydrated biological specimens. First proof-of-principle measurements using continuous-movement 2D scans of frozen hydrated HeLa cells as a model system are reported to demonstrate the potential of the new detection system.

Keywords: HeLa cells; SDD; XRF; cryogenic; solid angle.

MeSH terms

  • Calcium / analysis
  • Chlorides / analysis
  • Cryopreservation
  • Electrodes
  • Equipment Design
  • HeLa Cells / chemistry
  • Humans
  • Phosphorus / analysis
  • Potassium / analysis
  • Silicon Compounds
  • Spectrometry, X-Ray Emission / instrumentation*
  • Spectrometry, X-Ray Emission / methods
  • Sulfur / analysis
  • Synchrotrons*
  • X-Rays

Substances

  • Chlorides
  • Silicon Compounds
  • Phosphorus
  • Sulfur
  • silicon nitride
  • Potassium
  • Calcium