a breakthrough in portable heavy metal analysis in soil - xos · 2017. 11. 20. · xos quantify...
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A Breakthrough in Portable
Heavy Metal Analysis in Soil
HDXRF Technology
HD Rocksand Product and Application
Brown field heavy metal investigation
Geneva Foundry Case Study
© XOS
Technology Overview
XRF Technology
雷达和微波
Wavelength: 0.01~20nm
Primary x-ray radiation
ICP-MS
ICP-AES
GFAAS
AAS
Analysis Range
1 ppq 1 ppt 1 ppb 1 ppm 1,000 ppm 100%
Arc-Spark OES
TOC; TN; TS, TOX
Element Range: From Al to U
XRF
Liquid
Solid
Sample
Traditional X-ray Fluorescence
TRADITIONAL XRF TECHNOLOGY
E
Co
un
ts
E
Co
un
ts
S Cl
With traditional XRF High Signal-to-Background ratio drives moderate detection limits and longer test times
HDXRF
2 4 6 8 10 12 14 16 18 20
1
10
100
1000
10000
SrBrBr
PbSe
Pb(As)
Zn
Cr
Ni
Cu
Zn
Fe
Co
utn
s (
60
0 s
eco
nd
s)
Energy (keV)
Sample
DCC
Background from source obscures reading
Patented DCC optics provide high definition sample spectrum
© XOS
HD Rocksand
Portable test stand eliminates
scattered x-ray exposure for the
user.
Integrated cooling for continuous
operation.
No separate computer for test stand operation.
Lightweight and highly portable.
Comfortable
handle for carrying all day.
Hands free
measurements for quantification and
screening.
Handheld capability.
Quickly switch from bagged
samples to sample cups.
Sample cups rotate
and oscillate to increase
measurement area.
Hands free
measurement key advantage for XOS.
HD Rocksand
4/5/2016 © XOS 10
• Hands free testing feature
• Push measure and collect the next sample
• Integrated test stand fans keeps you testing even in hot conditions
• The measurement window is tough to prevent downtime from punctures or tears
HD Rocksand
4/5/2016
Industry Leading Sensitivity
*Limits of Detection are for a measurement in clean SiO2. Screening LOD is for a 1 minute measurement. Quantification LOD is for a 5 minute measurement. ** Longer Measurement
LOD in ppm*
HD Rocksand Screen
HD Rocksand Quantify
As 1.5 0.5
Cd 5 0.8**
Hg 2 0.5
Cr 15 5
Cu 5 1.5
Ni 12 3
Pb 1.8 0.5
Sb 16 5
Se 1.5 0.4
Ag 20 5
Tl 1.8 0.5
Zn 3 1
Ba 20 15
• Improved measurement sensitivity means getting the results you need faster
• Delineate contamination boundaries with improved accuracy
• Reduced measurement uncertainty means less laboratory validation
4/5/2016 © XOS 12
ASTM Certified
© XOS
Quantitative analylsis of Heavy Metals in Soil
• Laboratory Analytical methods require valuable time and do not provide fast enough feedback
• Analyzing samples in a laboratory setting is relatively complex, expensive, and requires professional operation
• On-site analysis provides quick feedback and the operation is simple to learn
• By performing quantitative analysis on-site, it is possible to test many more samples
• Ensuring successful remediation on-site can be done at far lower costs than laboratory analysis
Lab Testing Limitations
Cost and Time Limitations • Large sites 2-2000 km2 • Lab testing costs $30-150/sample • Must collect, package, and ship off-
site • Delayed decisions waiting for
analytical results
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© XOS
Handheld XRF Testing Limitations
• Portable and easy to use • On-site analysis • Quick Results • Widely used for elemental
analysis in many applications
Advantages
• Limited sensitivity • Unable to detect low
concentrations to validate successful remediation
Disadvantages
Currently, handheld XRF analyzers are not able to meed the analytical requirements in soil for Hg, As, Cd, and Cr.
Test at Regulatory Level
Pollutants English name
Shanghai
Standard “Target”
Level
(mg·kg-1)
RCRA Levels
(mg·kg-1)
(Solid Waste)
EPA Priority
Pollutant Levels
(mg·kg-1)
(Soil
Remediation)
XOS Quantify
LOD(ppm)
(5 – 15 minute
measurement)
XOS Screening
LOD(ppm)
(1 minute
measurement)
Market Leader
Screening LOD(mg·kg-
1)
(1 minute measurement)
Antimony 12 5 5 16 45
Arsenic, inorganic 20 5 5 .5 1.5 15
Beryllium 16 .5 N/A N/A N/A
Cadmium 1 1 1 .8 5 25
Chromium 190 5 1 5 15 80
Copper 63 1 1.5 5 30
Lead 140 5 5 .5 1.8 12
Nickel 50 1 3 12 75
Selenium 39 1 10 .4 1.5 10
Silver 39 5 1 5 20 15
Thallium 2 1 .5 1.8 Not published
Zinc 200 10 1 3 25
Mercury, inorganic 1.5 0.2 .1 .5 2 15
Barium 100 15 20 90
© XOS
© XOS
Cleanup of groundwater, soil, operating facilities, and contaminated
buildings and sites.
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Site Investigation and Remediation
© XOS
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Phase I,II – Environmental Site Assessment
• Assess site history: What contaminants could be present? • Review processes and wastes that could have been
discharged • Preliminary sampling to assess contamination sources • Purpose is to determine if further investigation is warranted • Based on phase I results, phase II assessment creates a
conceptual model of potential contamination pathways • Purpose is to determine if environmental remediation is
needed
© XOS
Phase III – Detailed Investigation and Remediation Plan
• Site is thoroughly tested to identify the scope, type, and location of contamination
• Remediation plan is developed including where and how remediation is to be conducted
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© XOS
Phase IV – Remediation Performed
• Site cleanup is performed to reduce contamination to acceptable levels • Excavation and removal of contaminated soil is the most
common method for heavy metals
• Additional testing is performed to validate that target have been achieved by the remediating firm
• Validation by regulatory body may be required
Phase V – Remediation Verified
4/5/2016 © XOS 21
NIST SRM 2710a Cr Ni As Cd Pb
1 27.12 8.51 1495.17 11.53 5429.34
2 20.93 8.64 1498.30 11.83 5438.01
3 21.55 9.30 1507.92 11.17 5421.98
4 27.88 9.57 1513.33 11.95 5414.42
5 20.66 8.28 1503.02 12.05 5411.54
6 25.26 8.58 1517.23 11.48 5425.08
7 22.69 7.98 1510.12 11.74 5424.48
8 21.19 8.89 1482.83 11.29 5413.40
9 23.81 9.43 1522.45 12.38 5419.97
10 21.43 9.34 1515.16 11.35 5427.32
AVG 23.25 8.85 1506.55 11.68 5422.55
STD 2.66 0.54 11.90 0.38 8.14
RSTD 11.44% 6.12% 0.79% 3.27% 0.15%
Cert. (mg/kg) 23 8 1540 12.3 5520
Practical Data-NIST
4/5/2016 © XOS 22
NIST SRM 2711a Ni As Cd Hg Pb
1 18.67 100.94 56.35 7.49 1403.99
2 18.69 107.21 55.54 7.01 1407.32
3 19.13 105.80 55.05 7.27 1403.86
4 17.97 107.46 55.21 8.00 1404.81
5 18.29 103.68 55.03 7.32 1404.96
6 19.00 102.58 55.63 7.61 1402.01
7 19.47 105.00 54.21 7.30 1403.83
8 18.65 106.58 53.44 7.21 1406.61
9 18.65 104.93 54.44 7.74 1404.13
10 19.12 101.17 55.48 7.93 1404.67
AVG 18.76 104.54 55.04 7.49 1404.62
STD 0.43 2.37 0.83 0.33 1.49
RSTD 2.32% 2.27% 1.50% 4.37% 0.11%
Cert. (mg/kg) 21.7 107 54.1 7.42 1400
Practical Data-NIST
CRM/Element Cr Ni Cu Zn As Cd Pb
Cert. Test Cert. Test Cert. Test Cert. Test Cert. Test Cert. Test Cert. Test
(GSS-1) 62 60.4 20.4 21 21 20.9 680 674 33.5 35.2 4.3 4.3 98 99.6
(GSS-2) 47 46.9 19.4 20.6 16.3 16.4 42.3 42 13.6 13.1 0.071 ND<2.1 20.2 20.3
(GSS-3) 32 28.5 12.2 13.3 11.4 11.1 31.4 31.7 4.4 4.1 0.059 ND<3.1 26 27.8
(GSS-4) 370 335 64.2 64.9 40.5 42.2 210 217 58 58.4 0.35 ND<3.2 58.5 61.6
(GSS-5) 118 131 40 40.8 144 141 494 493 412 391 0.45 ND<2.1 552 588
(GSS-6) 75 79.3 53 51.4 390 405 96.6 98.8 220 218 0.13 ND<3.4 314 340
(GSS-7) 410 432 276 265 97 100 142 148 4.8 3.7 0.08 ND<3.7 13.6 15.7
(GSS-8) 68 70 31.5 30.8 24.3 23 68 68.9 12.7 12.9 0.13 ND<2.2 21 20.5
(GSS-13) 65 58.9 28.5 28.4 21.6 22.5 65 64.7 10.6 10.8 0.13 ND<3.3 21.6 22.6
(GSS-14) 70 69.7 33 34 27.4 26.8 96 94.5 6.5 8.7 0.2 <3.4 31 32.8
ESS3 98 104 33.7 32.8 29.4 29.6 89.3 90.4 15.9 18.2 0.044 ND<2.1 33.3 32.8
ESS4 70.4 69.1 32.8 33.9 26.3 26.1 69.1 69.1 11.4 11.7 0.083 ND<3.2 22.6 22.8
GSR-2 32 29 17 17.2 55 55.4 71 70.7 2.1 1.8 0.061 ND<3.3 11.3 9.6
GSD-04 81 84.5 40 39.4 37 37.1 101 104 19.7 20.3 0.19 ND<3.5 30 31.6
GSD-08 7.6 6.7 2.7 4.1 4.1 5.1 43 44 2.4 1.9 0.081 ND<3.1 21 23.7
GSD-11 40 40.8 14.4 15.7 78.6 78 373 374 188 178 2.3 2.3 636 666
GSD-12 35 35.4 12.8 13.8 1230 1252 498 506 115 103 4 3.8 285 310 4/5/2016 © XOS 23
Practical Data-GSS
4/5/2016 © XOS 24
Sample As
HDXRF HHXRF ICP
SB01-3.2 7.7 < LOD 5.41
SB01-7.9 3.4 < LOD 2.65
SB02-0.2 7.8 16.25 6.21
SB02-8.5 16.3 < LOD 8.28
SB03-9.2 3.8 10.87 2.32
SB03-11.8 14 12.84 8.8
SB04SQ1 8.8 < LOD 5.42
SB04-0.2 7.1 < LOD 5.81
SB04-8.3 2.8 1.88
SB06-2.5 13.8 11.75 9.24
SB06-6.9 5.6 < LOD 4.56
SB09-1.8 9.8 < LOD 4.34
SB09-3.5 7.5 < LOD 5.48
SB09-5.8 3.2 < LOD 3.26
SB10-6.8 48.3 39.45 33.4
SB10-7.9 47.8 33.5 33.2
SB10-9.8 5.2 < LOD 2.97
SB12-3.2 13.3 11.66 8.89
Site Sample Comparison Data(mg/kg)
y = /通用格式x
R² = /通用格式
/通用格式
/通用格式
/通用格式
/通用格式
/通用格式
/通用格式
/通用格式
/通用格式 /通用格式 /通用格式 /通用格式 /通用格式 /通用格式 /通用格式 /通用格式 /通用格式
HD
XR
F ICP
HDXRF
y = /通用格式x
R² = /通用格式
0
5
10
15
20
25
30
35
40
45
/通用格式 /通用格式 /通用格式 /通用格式 /通用格式 /通用格式 /通用格式 /通用格式 /通用格式
HHXRF
4/5/2016 © XOS 25
HDXRF VS. Lab (mg/kg)
Cr Cu Zn Pb
样品 ICP1# ICP2# HDXR
F ICP1# ICP2#
HDX
RF ICP1# ICP2#
HDX
RF ICP1# ICP2#
HDX
RF
1 85.2 93.0 89.2 51.5 34.0 53.9 80.1 80.0 84.1 72.8 37.0 38.9
2 58.2 62.0 63.6 29.5 22.0 31.3 86.7 89.0 98.0 374.0 182.0 210.5
3 102.0 113.0 146.0 114.0 99.0 139.0 152.0 157.0 182.0 76.5 30.0 41.1
4 89.4 110.0 119.0 104.0 96.0 122.0 176.0 191.0 198.0 138.0 66.0 59.9
5 87.3 100.0 109.5 170.0 180.0 185.5 255.0 288.0 291.0 280.0 150.0 154.0
6 54.8 56.0 66.1 22.2 18.0 24.0 61.3 63.0 73.3 56.7 18.0 22.0
7 44.7 69.0 62.4 16.4 14.0 20.1 62.0 46.0 73.7 49.2 24.0 26.6
4/5/2016 © XOS 26
HDXRF VS. Lab (mg/kg)
Influence Factors
4/5/2016 © XOS 27
4/5/2016 © XOS 28
• Metals contamination may selectively bond to heterogeneous portions of soil causing “nuggets” of contamination
• Small lab samples decrease likelihood of identifying contamination, particularly at low concentrations
• Field samples by XRF are much larger and are much more likely to identify contamination
Image Source: “Advanced Design Application and Data Analysis for FP_XRF in Soil Matrices”, CERCLA Education Center, US EPA, Jan 2010.
Heterogeneity Between Samples
4/5/2016 © XOS 29
Heterogeneity Between Samples
4/5/2016 © XOS 30
Heterogeneity Within Sample
Sample Preparation for Quantification
4/5/2016 © XOS 31
4/5/2016 © XOS 32
Moisture Effect
1. All heavy metal elements show same trend for different moisture.
2. In general, 40%-60% moisture will be maximum.
3. Moisture can cause result lower, 20% moisture cause about 20%-30% lower.
Geneva Foundry Case Study
4/5/2016 © XOS 33
Geneva Foundry Case Study
4/5/2016 © XOS 34
Geneva Foundry Case Study
4/5/2016 © XOS 35
Geneva Foundry Case Study
4/5/2016 © XOS 36
Thank you!
Phone: +1 518.880.1500
Email: info@xos.com
Web: https://xos.com/products/hd-rocksand/
Demo request: http://www.xos.com/request-information
4/7/2016 © XOS 37
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