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

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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

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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

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• 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

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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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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

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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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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

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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

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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

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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

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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

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HDXRF VS. Lab (mg/kg)

Influence Factors

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• 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

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Heterogeneity Between Samples

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Heterogeneity Within Sample

Sample Preparation for Quantification

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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

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Geneva Foundry Case Study

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Geneva Foundry Case Study

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Geneva Foundry Case Study

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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