Multi-element Reference Materials for XRF (and Filter Orientation) Nicole Hyslop, Krystyna Trzepla, and Sinan Yatkin Crocker Nuclear Laboratory University.

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Presentation transcript:

Multi-element Reference Materials for XRF (and Filter Orientation) Nicole Hyslop, Krystyna Trzepla, and Sinan Yatkin Crocker Nuclear Laboratory University of California, Davis Presented at Cape Romain, SC October 15, 2014

Multi-element (ME) XRF Reference Filters Quickly evaluate instrument performance for multiple elements Assess spectral interferences between elements Limited multi-element reference filters for XRF – NIST Standard Reference Material (SRM) created with dust collected from HVAC system Does not contain all the elements of interest Only some elements are certified, others are qualitative only ICPMS uses multi-element standard solutions – Using these solutions in the aerosol chamber to create reference filters for the XRF instruments 2

UCD Evaluation of ME Standards

Inter-laboratory Comparison of Multi-element (ME) samples Labs 1.CNL, XRF (Epsilon 5) 2.DRI, XRF (Epsilon 5) and ICPMS 3.South Coast Air Quality Management District, XRF (Epsilon 5) and ICPMS 4.New Zealand (NZ), XRF (Epsilon 5) and PIXE 5.United Kingdom (UK), XRF (Epsilon 5) and ICPMS 6.PANalytical, XRF (Epsilon 5) 7.RTI, XRF (Quant’X with linear calibration) 8.JRC, XRF (Quant’X with standardless) 6 MEs samples from each o Low : Mimicking the medians of IMPROVE o High : Trace elements over than the QLs, major elements the same as Low o 28 elements, IMPROVE + Co, Cd, Mo and Ba

Methodology for ME Study

Laboratory Inter- Comparison Results: K

Laboratory Inter- Comparison Results: S

Laboratory Inter- Comparison Results: V

Laboratory Inter- Comparison Results: Se

Deposit Area ICPMS analysis yields g/filter while XRF analysis yields g/cm 2 o Convert between units using filter area o Pall 47 mm PTFE filter internal diameter measures ~38 mm, thus cm 2 o EPA uses cm 2 for Partisol sampler for MTL filters

SEM Images of Multi-element Deposit

SEM XRF Results of 47mm filter with deposit on PTFE-face

Laser Ablation Inductively Coupled Plasma Mass Spectrometry (ICPMS)

ME Solution Samples (Na, Si, K, Ti, Mo and Zr) on 47 mm

SiO 2 Samples on 47mm Filters

(NH 4 ) 2 SO 4 Samples 25 mm

Filter Orientation Still assessing the impacts of filter orientation on our operations?