On site heavy metal testing and monitoring using monochromatic XRF methods

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1 On site heavy metal testing and monitoring using monochromatic XRF methods

2 X-Ray Fluorescence Analysis hn o hn i 8/5/2017 XOS Confidential File 2

3 Counts (100 seconds) Limitation of XRF High scattering background Difficult in sub-ppm level Matrix effect and interference Ca V Fe Zn Fe Ge As/Pb Pb Ge As Sr PbZr Mo Mo Energy (kev) 8/5/2017 XOS Confidential File 3

4 Limitation of current field XRF Hand Held XRF/Portable XRF Powerful tools for high level contaminations testing Low cost Non-destructive, no sample preparation Limitation of HHXRF and Portable XRF Ineffective for Cd, As, and Hg Inability of measure 1-20ppm range for most of metals 8/5/2017 XOS Confidential File 4

5 Quantitative analysis in Lab Current State - Certification: Wet Chemistry/ICP Wet Chemistry/ICP High testing costs Long time for results Sample Preparation Acid Digestion Multi-step process increases result variability Scale, moisture determination, microwave, ICP instrument Trained operators required Introduces likliehood of operator error Requires expensive consumables (Gas, acid, multiple sample tubes) 8/5/2017 XOS Confidential File 5

6 Needs for Site Testing Accurate assessment of a contaminated site often required a large number of sampling Large number of the samples sent to lab for analysis Lack of an effective site testing method is a major bottle neck for both economic cost and regulatory enforcement 8/5/2017 XOS Confidential File 6

7 As and Hg Site Testing Meaningful As testing at a contaminated site is difficult if Pb level is relatively high Meaningful level of Hg on site testing is almost impossible 8/5/2017 XOS Confidential File 7

8 Doubly Curved Crystal Optic Point Focusing Geometry Solid angle: ~ 0.01 to 0.05 Sr. Beam spot size: mm, depending on the source spot Reflection efficiency ~ 10% Beam flux: ~ photons/s Highly monochromatic 8/5/2017 XOS Confidential File 8

9 DCC Beam Profile Source Focal Circle Crystal Y X R Focus The deviation of incident angle from the Bragg angle Dq = q -q B 0.5 (x/2r) 2 cotq B

10 Coutns (600 seconds) Monochromatic EDXRF--HDXRF DCC Optic Polychromatic excitation Fe Zn Cu Pb(As) Ni Br Pb Zn Se Br Cr Sr Monochromatic excitation Energy (kev) Sample Very low background Clean Spectrum Better Precision Superior reproducibility 8/5/2017 XOS Confidential File 10

11 Portable HDXRF Source 3 Monochromatic beams DCC Optics Low background Selected excitation Silicon drifted Detector SDD (SDD) 8/5/2017 XOS Confidential File 11

12 Counts Mid-energy Spectrum 1.00E+07 NIST2586 Raw 1.00E E E E E E E E(keV)

13 Counts Mid-energy Spectrum 1.00E+07 NIST E E E E E E E E(keV) Raw SPP

14 Counts As/Pb in soil 1.00E+07 NIST E E E E E E+01 Raw SPP C R Background 1.00E Energy (kev)

15 System Accuracy NIST Standards 8/5/2017 XOS Confidential File 15

16 System Accuracy GSS Standards Part # Description Cr Ni Cu Zn As Pb GSS2 Chinese National Soil Standard GSS3 Chinese National Soil Standard GSS4 Chinese National Soil Standard GSS5 Chinese National Soil Standard GSS7 Chinese National Soil Standard GSS8 Chinese National Soil Standard GSS13 Chinese National Soil Standard GSS14 Chinese National Soil Standard /5/2017 XOS Confidential File 16

17 Comparison with ICP 8/5/2017 XOS Confidential File 17

18 ASTM D8064 Element LOD (mg/kg) Method Range (mg/kg) Cr Ni As Cd Hg Pb /5/2017 XOS Confidential File 18

19 NIST SRM 1646a Estuarine Sediment Results for Single Site Repeatability Study (mg/kg) SRM 1646a Cr Ni As Cd Hg Pb <1.12 < <1.16 < <1.15 < <1.16 < <1.14 < <1.16 < <1.01 < <1.16 < <1.18 < <1.17 < Average Stand. Dev RSD 4.39% 8.33% 2.05% 1.58% ARV Bias 1.86% -4.04% 6.90% 1.11%

20 Low As and Cd level with high Pb SRM 2586 Cr Ni As Cd Hg Pb < < Average Stand. Dev RSD 2.56% 0.78% 9.49% 12.31% 37.70% 0.65% ARV Bias 4.06% -2.79% -6.21% 6.64% 71.66% -2.13% 8/5/2017 XOS Confidential File 20

21 Hg contamination SRM 2711a Cr Ni As Cd Hg Pb Average Standard Deviation RSD 5.06% 2.32% 2.27% 1.50% 4.37% 0.11% ARV Bias 3.82% % -2.30% 1.74% 0.94% 0.33% 8/5/2017 XOS Confidential File 21

22 Screening Hg at 1 ppm level SRM 2709a Cr Ni As Cd Hg Pb < < < < < < < < < < Average Stand. Dev RSD 2.18% 0.78% 5.10% 27.47% 1.02% ARV Bias 2.82% 2.36% 10.76% 6.67% 4.45% 8/5/2017 XOS Confidential File 22

23 Comparison with HHXRF 8/5/2017 XOS Confidential File 23

24 Case Study Upstate NY As Site 8/5/2017 XOS Confidential 24 File 24 XOS

25 Case Study Geneva NY As Site

26 Matrix Spiked NY Geneva Soil Result and Matrix Spike Recovery Soil H2O (Pb, As, Ni Cr) Air dried Spiked Soil Pb As Ni Cr unspiked mean spiked mean STD R STD (%) Recovery (%)

27 The Cd problem Cd is highly toxic element Cd contamination in agriculture soil and can be transported from soil to plants and crops The safety limits for wheat are at level of 0.2ppm The critical limits for soil is at 0.3ppm The only effective testing method for Cd at such level is ICP/MS at sophisticated labs 8/5/2017 XOS Confidential File 27

28 MXRF solution Sample SDD High energy monochromatic beam excitation Low power x-ray tube Small and transportable system 8/5/2017 XOS Confidential File 28

29 Spectrum of low Cd sample NIST2709a 0.37ppm Cd, 300s Cd 8/5/2017 XOS Confidential File 29

30 Cd calibration and detection limit Sample ARV (ppm) Measured (ppm) NIST NIST2709a NIST NIST Limit of Detection(LOD) = 0.09 ppm 8/5/2017 XOS Confidential File 30

31 Repeatability NIST SRM2702 Soil # test C(ppm) Aver ARV Stdev NIST SRM2709a Soil # test C(ppm) Aver ARV Stdev NIST SRM1646a Soil # test C(ppm) Aver ARV Stdev Limit of Detection(LOD) = 0.05 ppm 8/5/2017 XOS Confidential File

32 Repeatability NIST SRM1573a Leaf # test C(ppm) Aver Stdev 0.02 ARV 1.52 NIST SRM1568b rice powder # test C(ppm) Aver Stdev ARV Limit of Detection(LOD) = 0.03 ppm 8/5/2017 XOS Confidential File

33 Power Plant discharging Se problem Power plant can discharge harmful level of As and Se No effective on-site/online testing of Se discharge 8/5/2017 XOS Confidential File 33

34 Monochromatic WDXRF Solution DCC Optic1 DCC Optic2 X-ray Sourc e Sample X-ray Count er Low Power Single/dual Elements Ultra-low Background High E Resolution 8/5/2017 XOS Confidential File 34

35 Preliminary As testing results 25 20ppb sample ppb sample LOD=2ppb 8/5/2017 XOS Confidential File 35

36 On-going work Improve optic sensitivity Improve source efficiency Achieve ~1ppb LOD for Se feasible 8/5/2017 XOS Confidential File 36

37 Conclusion A breakthrough development for heavy metal analysis in soil for contaminated sites First time to achieve non-destructive analysis at site in 1-10ppm concentration range for metals in soil with portable HDXRF method Quantitative analysis of NIST and other national standards show excellent accuracy Successfully achieve low level Cd analysis in agriculture soil and crops Demonstrate a path for on-site monitoring of low ppb level of Se or As in discharging water 8/5/2017 XOS Confidential File 37

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