Expanding the analytical range utilizing 1013 Ω amplifier technology: Measurement of 100 pg Nd samples

Applications | 2018 | Thermo Fisher ScientificInstrumentation
Elemental Analysis, GC/HRMS, GC/MSD
Industries
Environmental
Manufacturer
Thermo Fisher Scientific

Significance of the topic


The ability to measure neodymium isotope ratios in picogram quantities addresses a critical need in isotope geochemistry when material is scarce or isotopic signals are weak. Conventional ion counters offer low noise but limited dynamic range and require frequent calibration of dead time and yield, constraining external reproducibility. The adoption of high-ohm amplifier technology on Faraday detectors significantly lowers noise, enables full duty cycle multicollection, and expands the measurable intensity range, unlocking high-precision analyses on extremely small samples relevant to fields such as cosmochemistry, paleoceanography, sedimentology and QA/QC in geochemical laboratories.

Study objectives and overview


This work demonstrates the performance of a Triton Plus thermal ionization mass spectrometer equipped with 1013 Ω amplifiers and a 3.3 pA calibration board for the determination of 143Nd/144Nd ratios in 100 pg loads of the JNdi-1 reference standard. The goal is to establish accuracy and precision limits at this low sample size, to benchmark against values obtained on much larger loads, and to identify key factors influencing measurement quality.

Methodology


A controlled loading protocol employed paraffin film dams to confine 1 µL aliquots of 0.25 M H3PO4 and 100 pg/µL Nd solution on double-filament Re zone-refined filaments. Filaments were outgassed, loaded at 1.2 A, dried, and heated to burn off the paraffin layer before glow-heating. The multicollection configuration monitored isotopes 142Nd to 146Nd on five 1013 Ω amplifiers. An integration period of 8.389 s per cycle was used, with 28 to 71 cycles per run, depending on signal evolution. Data reduction included tau correction for amplifier response, exponential mass fractionation correction using a fixed 146Nd/144Nd ratio of 0.7219, a two-sigma outlier test, and rejection of cycles below an 11 mV 143Nd threshold to optimize precision.

Instrumentation


  • Thermo Scientific Triton Plus TIMS
  • Five 1013 Ω amplifiers with inter-channel gain stability better than 15 ppm over 24 h
  • 3.3 pA current calibration board

Main results and discussion


Ten of thirteen filaments yielded valid data, giving a mean 143Nd/144Nd ratio of 0.512110 ± 0.000051 (2 SD). This value agrees with published ratios obtained on 100–1000 ng loads, despite working with samples 1,000 to 10,000 times smaller. The external reproducibility of 99 ppm (2 RSD) matches internal precision levels, demonstrating that counting statistics, rather than electronic noise, set the ultimate precision limit. The 100 % duty cycle of Faraday multicollection and stable amplifier gains eliminate uncertainties associated with ion counter yield and dead time calibrations. Observed extreme evaporation-induced fractionations underscore the need for a consistent cutoff signal to discard low-intensity measurements and maintain analytical accuracy.

Benefits and practical applications of the method


  • High-precision Nd isotope analysis on sub-nanogram samples
  • Reduced sample consumption and simplified calibration compared to ion counting
  • Improved duty cycle and signal stability for sequential measurements
  • Applicability to trace element-limited geological materials and micro-samples in cosmochemistry and marine studies

Future trends and potential applications


Ongoing advances in amplifier design and filament loading techniques may push precision measurements towards even smaller sample sizes and other isotopic systems. Integration of automated loading and heating protocols could further reduce blank contributions and mixing effects on the filament. The technology holds promise for routine high-precision analyses in fields requiring minimal sample amounts, such as single-grains, microfossil studies, and environmental micro-sampling.

Conclusion


The deployment of 1013 Ω amplifier technology on a Triton Plus TIMS permits accurate determination of 143Nd/144Nd ratios in 100 pg Nd loads with precision at the counting statistics limit. The approach overcomes ion counter dynamic range constraints and simplifies calibration, offering a robust pathway for high-precision isotope geochemistry on minute samples.

References


  1. Craig G et al Dynamic time correction for high precision isotope ratio measurements Thermo Fish Sci Tech Note 30396 2017
  2. Faure G Mensing T M Isotopes Principles and Applications Wiley 2005
  3. Frank M Radiogenic isotopes Rev Geophys 40 1001 2002
  4. Garcon M et al Factors influencing precision and accuracy of Nd isotope measurements Chem Geol 476 493–514 2018
  5. Hart S R Zindler A Isotope fractionation laws Int J Mass Spectrom Ion Process 89 287–301 1989
  6. Koornneef J M et al Measurement of small ion beams using new 1013 ohm resistors Anal Chim Acta 819 49–55 2014
  7. Palme H ONeill H S C Cosmochemical estimates of mantle composition Treatise on Geochemistry 3.1 1–39 2014
  8. Russell W A et al Ca isotope fractionation on Earth and other materials Geochim Cosmochim Acta 42 1075–1090 1978
  9. Tanaka T et al JNdi-1 neodymium isotopic reference Chem Geol 2000
  10. Vollstaedt H et al How low can you go SmartNote 30439 Thermo Fish Sci 2017

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