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All About Discovery! New Mexico State University nmsu.edu Rapid and in situ analysis of metal concentrations in agricultural fields in San Juan County using Portable X ray fluorescence (PXRF) Gaurav Jha Department of Plant and

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Rapid and in‐situ analysis of metal concentrations in agricultural fields in San Juan County using Portable X‐ray fluorescence (PXRF)

Gaurav Jha Department of Plant and Environmental Sciences

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Basic Principle of PXRF Applications in environmental sciences Extension and Outreach Response to GKM spill

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  • Soil scientists have long differentiated

soils based on chemical properties.

Pedocal Pedalfer Curtis Marbut’s Normal Soil concept

  • Soil scientists have long differentiated

soils based on chemical properties.

Curtis Marbut’s Normal Soil concept

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  • Historically, many chemical

determinations were made via titration or colorimetry.

  • More recently, lab based

instruments have offered greater accuracy

  • ICP-AES/MS
  • AAS

Rapid Large number

  • f

samples Cost Effective

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http://www.sun.org/encyclopedia/electromagnetic-spectrum

The colors we see!

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Working Principle of PXRF

Activation of X-Ray Tube Sample Excitation Fluorescence Capture Spectrum Results

https://www.olympus-ims.com/en/xrf-xrd/delta-handheld/delta- mining/#!cms[tab]=%2Fxrf-xrd%2Fdelta-handheld%2Fdelta- mining%2Fapplications http://www.equipcoservices.com/support/tutorials/introduction-to-xrf-spectrometry/ https://www.olympus-ims.com/en/applications/portable-xrf-technology-archaeometry- authentication-conservation-art-objects/

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Specifications for GKM sample analysis

  • X Ray tube operated at 10-40 keV. Not an active source of radiations.
  • Standards: Stainless steel ‘316’ alloy chip
  • 16.13% Cr
  • 1.78% Mn
  • 68.76% Fe
  • 10.42% Ni
  • 0.20% Cu
  • 2.10% Mo
  • Verified by NIST soil standards
  • Scan time- 90 seconds for three beams (30 seconds per beam)
  • Instrument is operated in proprietary standard configurations :

1. Geochem mode 2. Soil mode 3. Mining mode

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Note-PXRF reports total elemental concentration; not ionic species (e.g. Fe+2 vs. Fe+3) or compounds (gypsum, calcite, etc.)

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Disadvantages

  • Cannot determine H,C or Na
  • Soil heterogeneity (example Fe and Mn concretions)

Advantages

  • Portable
  • Simple, non-destructive analysis
  • Rapid (90 sec scan)
  • Multi-element analysis
  • Low limit of detection and wide dynamic range
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Basic Principle of PXRF Applications in environmental sciences

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On-site metal determination via PXRF

  • Heavy metal content
  • Sediment and soil spatial analysis
  • Plant tissue analysis
  • Water analysis

Site specific proxy-determinations of soil parameters via PXRF

  • Soil cation exchange capacity (CEC)
  • Soil pH
  • Soil salinity
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Proxy-determinations of soil CEC via PXRF

  • CEC is directly associated with soil fertility.
  • Lab methods are very accurate but

arduous.

http://scienceofagriculture.org/ch-cation.php

Sharma et al. (2015)

  • In-situ prediction of soil CEC to develop a

predictive model based on enhanced lab based data. R2 = 0.908

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Proxy-determinations of soil pH via PXRF

  • PXRF cannot read Hydrogen ion directly.
  • Soil system pH is commonly associated with
  • ther elements.

Alkaline system-Ca, Mg Acidic system-Al, Fe

  • These elements can be used as a proxy for pH

determination specially where traditional sampling is not possible-frozen and lithified soils.

https://cosmosmagazine.com/climate/what-happens-if-permafrost- disappears https://maui-mike.smugmug.com/keyword/lithified%20sand%20dunes/ https://www.uidaho.edu/cals/soil-and-water- systems/research/pedology-laboratory/fosberg-monoliths

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Basic Principle of PXRF Applications in environmental sciences Response to GKM spill

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  • Monitor selected metal concentrations in agricultural

fields and crop grown within the Animas and San Juan River watershed.

  • Characterize spatial variability of selected metals

Gold King Mine Spill- A case study using PXRF

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Sampling sites with increasing distance from the GKM (Colorado and NM border through Shiprock)

Colorado New Mexico

Shiprock Farmington Bloomfield Aztec

Sampling locations

P F V P F V

Pasture (Grass) Forage (Alfalfa) Vegetables

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On-site Metal determination for soil spatial analysis

Total Arsenic concentration (parts per million)

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What we observed?

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Metal RSL

(mg kg-1)

Concentration (mg kg-1) in Pasture land Concentration (mg kg-1) in Forage land Concentration (mg kg-1) in Vegetable Field Arsenic 7.07 7.19 6.92 7.13 Lead 400 83.28 48.09 17.50 Calcium

  • 10450

16609 37006 Zinc 2300 223.46 116.64 71.47 Copper 310 38.98 29.43 21.35 Manganese 180 874.92 545.04 312.84 Iron 5500 23838 23160 22860

Average total metal(loid) concentrations (mg kg-1) in fields irrigated by Animas river water

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Spatial distribution of Arsenic in agricultural fields

Pasture grass 14.1 hectares Aztec Forage (alfalfa) 3.04 hectares Farmington

Vegetables 1.27 hectares Shiprock Total Arsenic concentration (parts per million)

RSL-7.07 mg kg-1

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Spatial distribution of Manganese in agricultural fields

Pasture grass 14.1 hectares Aztec Forage (alfalfa) 3.04 hectares Farmington

Vegetables 1.27 hectares Shiprock Total Manganese concentration (parts per million)

RSL-180 mg kg-1

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Soil Arsenic and Plant growth

  • Environmental toxin.
  • Inhibits root proliferation and extensions.
  • Slows expansion and biomass accumulation.

(Finnegan et al, 2012)

https://edu.glogster.com/glog/arse nic/2dxuahjh3rg http://arsenic-33.narod.ru/groundwater-arsenic- contamination-in-west-bengal-india.html

Keratosis

Hyperaccumulation Into Food chain

https://www.aljazeera.com/indepth/features/2016/01/indias-arsenic-belt- water-project-brings-relief-160128090612395.html

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Metal Conc. (mg/kg) 35 ND ND 82 50 3 78 6334 13

CORN

Metal

Guideline value (mg/kg)

Al 7-3410 As 1.7 Cr N/A Fe 48 Mn 300 Pb 10 Zn 150 Ca N/A Cu 30

Leaves Soil Corn Cob

Designed by-Mathews A.

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Metal Conc. (mg/kg) 406 0.5 ND 387 30 3 32 51955 8 Metal Guideline value (mg/kg) Al 7-3410 As 1.7 Cr N/A Fe 48 Mn 300 Pb 10 Zn 150 Ca N/A Cu 30

WATER MELONS Soil Leaves Melon

Designed by-Mathews A.

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Metal Conc. (mg/kg) 397 0.9 ND 355 33 ND 33 65650 10

SQUASH

Metal Guideline value (mg/kg) Al 7-3410 As 1.7 Cr N/A Fe 48 Mn 300 Pb 10 Zn 150 Ca N/A Cu 30

Soil Leaves Honeydew HONEYDEW

Designed by-Mathews A.

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Basic Principle of PXRF Applications in environmental sciences Response to GKM spill Extension and Outreach

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Scanning contaminated river sediment samples using VisNIR and PXRF at Indian Institute of Technology (India)

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Conclusions

  • Portable X-Ray Fluorescence is a rapid, in-situ and non-destructive

technique for site specific proxy determination of soil properties and total concentration of metal content.

  • Exceeded As and Mn total concentration at some of the hotspots in the fields

across Animas and San Juan watershed did not correspond to the increased concentration in leaf tissue of plants.

  • Metal analysis using PXRF helped to respond quickly when GKM spill

happened and also to reach the farmers and growers at teach-in, radio talks and through factsheets.

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References

  • Peason D., Weindorf, D.C., ., Chakraborty, S, Li B., Koch J., Deventer P.V.. 2018. Analysis of

metal-laden water via PXRF. Journal of Hydrology 561, 267-276

  • Sharma, A., Weindorf, D.C., Man, T., Aldabaa, A.A.A., Chakraborty, S., 2014. Characterizing

soils via portable X-ray fluorescence spectrometer: 3. Soil reaction (pH). Geoderma 232– 234, 141–147.

  • Weindorf, D.C., Paulette, L., Man, T., 2013. In-situ assessment of metal contamination via

portable X-ray fluorescence spectroscopy: Zlatna, Romania. Environ.Pollut. 182, 92e100.

  • Weindorf, D.C., Bakr, N., Zhu, Y., 2014. Advances in portable X-ray fluorescence (PXRF) for

environmental, pedological, and agronomic applications. Adv. Agron.128, 1e45.

  • Weindorf, D.C., Zhu, Y., Haggard, B., Lofton, J., Chakraborty, S., Bakr, N., Zhang, W.,

Weindorf, W.C., Legoria, M., 2012b. Enhanced pedon horizonation using portable Xray fluorescence spectroscopy. Soil Sci. Soc. Am. J. 76 (2), 522– 531.http://dx.doi.org/10.2136/sssaj2011.0174.

  • Weindorf, D.C., Zhu, Y., McDaniel, P., Valerio, M., Lynn, L., Michaelson, G., Clark, M., Ping,

C.L., 2012c. Characterizing soils via portable X-ray fluorescence spectrometer: 2. Spodic and Albic horizons. Geoderma 189–190, 268–277. http://dx.doi.org/10.1016/j.geoderma.2012.06.034.

  • Weindorf, D.C., Herrero, J., Bakr, N., Swanhart, S., 2013a. Direct soil gypsum quantification

via portable X-ray fluorescence spectrometry. Soil Sci. Soc. Am. J. 77 (6), 2071–2077.

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  • Farmers in Aztec, Farmington and Navajo nation who allowed access to fields for long

term monitoring of contaminations.

  • EPA-NMED State Cooperative Agreement 01F22301

Assistance Program 66.204, Multipurpose Grants to Tribes and States.

  • Advisors-Dr. April Ulery, Dr.Kevin Lombard, Dr.Colby Brungard
  • B. Hunter, B. Francis, T. Charley, R. Ghorbani, E.Pointer, A. Matthews, H.Winsor,

J.Grijalva.

Acknowledgement

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