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Contaminants and Errors01:16

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Effective sample preparation is crucial for accurate and reliable laboratory analysis. During this process, two significant sources of error can arise: concentration bias from improper sample splitting and contamination caused by methods used to reduce particle size, such as grinding or homogenization. Identifying and minimizing these potential errors is crucial to ensuring the validity of the analysis.
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Polarography is a classical voltammetric technique used to analyze electrochemical reactions. This method applies a linear potential sweep to a dropping mercury electrode (DME), and the resulting current is measured. A dropping mercury electrode is commonly used as the working electrode in polarography. It consists of a capillary tube filled with mercury, where the tiny droplet forms at the tip. This droplet continuously drops from the capillary, creating a new electrode surface for each...
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Correcting sensitivity drift during long-term multi-element signal measurements by solid sampling-ETV-ICP-MS.

A Martin-Esteban1, B Slowikowski, K H Grobecker

  • 1Institute for Reference Materials and Measurements, Joint Research Centre, European Commission, Retieseweg, B-2440 Gel, Belgium.

Talanta
|October 31, 2008
PubMed
Summary

Directly analyzing solid samples using electrothermal vaporisation-inductively coupled plasma-mass spectrometry (SS-ETV-ICP-MS) can suffer from sensitivity drift. A combination of argon dimer internal standard and modified ETV-ICP connection tube stabilizes sensitivity for trace element analysis.

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Area of Science:

  • Analytical Chemistry
  • Environmental Science

Background:

  • Solid sampling-electrothermal vaporisation-inductively coupled plasma-mass spectrometry (SS-ETV-ICP-MS) enables direct trace element determination in solids.
  • Long-term studies, such as reference material homogeneity assessment, reveal instrument sensitivity drift.
  • Deposits on cones and ion lenses are the likely cause of this sensitivity decrease.

Purpose of the Study:

  • To propose and evaluate methods for correcting and suppressing sensitivity drift in SS-ETV-ICP-MS.
  • To monitor trace elements (Cd, Cu, Hg, Mn, Pb, Sb, Se, Sn, Tl, U, V) in diverse reference materials.
  • To identify optimal strategies for stable instrument performance during extended analytical runs.

Main Methods:

  • Implementation of SS-ETV-ICP-MS for direct solid sample analysis.
  • Investigation of various drift correction and suppression techniques.
  • Utilisation of the argon dimer as an internal standard.
  • Modification of the electrothermal vaporisation-inductively coupled plasma (ETV-ICP) connection tube.

Main Results:

  • Several methods were evaluated for their effectiveness in mitigating sensitivity drift.
  • The combined approach of using argon dimer and modifying the ETV-ICP connection tube proved most effective.
  • Stable instrument sensitivity was achieved for at least 60 consecutive ETV runs.

Conclusions:

  • The proposed method significantly improves the reliability of SS-ETV-ICP-MS for long-term trace element analysis.
  • This technique is crucial for accurate homogeneity assessment of reference materials.
  • The findings offer a practical solution for enhancing the stability and usability of SS-ETV-ICP-MS.