Spectrometric techniques utilizing the phenomena of optical emission (OE) and X-ray fluorescence (XRF) have been used for years for QA/QC purposes by metals manufacturing and reprocessing industries. The advent of portable, OE and XRF based alloy analyzers — stimulated by the development in electronics and computer technology — made possible in-situ grade identification and analysis of metals of construction either before their use or in post-factum verification. The advantages of portable OE and XRF alloy analyzers were quickly discovered by petroleum refining, nuclear, aviation and power generating industries, in which a 100% positive materials identification, (PMI), is routinely required.

Technical Papers of ISA

Improved detection limits for sulfur measurements by EDXRF

Author: Sipilae, Heikki ; Patterson, John I. H. ; Kiuru, Erkki ; Hietala, Matti ; Preucil, Robert

Energy dispersive x-ray fluorescence (EDXRF) has long been recognized as a good method for the measurement of sulfur in petroleum products in the range of 300 to 500 ppm.New environmental regulations in both North America and Europe require sulfur levels in gasoline and diesel be lowered to 10 to 30 ppm.Thus, the detection limits of EDXRF be improved to continue its use.A new low background detector technol. and improved electronics has made it possible to achieve a detection limit of 1 ppm using EDXRF.The new detector dramatically reduces the low energy background by rejecting any counts that are generated as a result of incomplete charge collection.In the standard proportional counter detector, some x-rays cause ionization close to the wall of the detector.This causes part of the charge to be lost in the detector wall and cause the x-ray to be counted at an apparent energy which is lower than the actual energy.This is a statistical process and is the major cause of the background at all energies lower than the backscatter peak.It is possible to reduce the background in the sulfur region by a factor of ten by detecting and rejecting incomplete charge collection.The measurement error at low concentration is related to the level of the background, as a result this background reduction leads to improvement in the detection limit.This paper describes a system for significantly reducing the background and increasing the count rate used in EDXRF resulting in standard deviations below 0.4 ppm (at 10 ppm) for the measurement of sulfur.

On-site, in-situ characterization of contaminated soil and liquid hazardous waste with field portable X-ray analyzer. A cost effective approach

Author: Piorek, S.

Within the last few years, new developments occurred in the area of on-site, in-situ characterization of soil contaminated with hazardous metals, using field-hardened, portable x-ray analyzers.Improvements of the anal. performance of com. available XRF analyzers have been successfully tested by the US Environmental Protection Agency during field trials performed at two Superfund sites under innovative technologies demonstration program.The results of those trials served as a basis for a new SW-846 Method 6200 for field-portable XRF for soil screening.The Field-Hardened, Portable X-Ray Analyzer, Model X-MET 940, and the results of the field tests are described.Addnl., the instrument's capability to analyze liquid hazardous waste (LHW) on-site, after minor sample preparation, is reported.Both soils and LHW can be quantified to below 100 mg/kg levels.

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