Heavy Metal Monitoring in

Environmental Samples
using ICP-OES

Uwe Oppermann and Nils Garnebode

Shimadzu Europa GmbH

Water Analysis

Environmetal Protection

)Water
)Soil
)Air

Water Analysis

Overview

Atomic Absorption
(AAS)

Inductively Coupled
Plasma (ICP)

UV-VIS Spectrometry

Overview
Legislation/ Definitions
Systemconfigurations
Measurements/ Results

Norms and Directives

European Drinking water regulation

Medicines Law
Foodstuffs and Commodities Act
Mineralwater regulation
Standards of gas and water supply industry
(DVGW)

Drinking Water Regulation

Purpose:
Protection of all human beings from the
dangerous influence of contaminated water
Application area:
since 01.01.2003
for Drinking water
not for Mineralwater, and other types of water

What is Drinking Water?

for drinking, cooking, preparation of foods
and drinks
household purpose:
personal hygiene and cleaning
cleaning of goods in touch with foods and
drinks
cleaning of goods in touch with the human body,
such as clothes, bedclothes, towels.
Water for food and drink producing industries

Chemical Requirements
No chemical substances in concentrations which
will be harmful for the human health
No chemical substances in concentrations higher
than the max. allowable concentrations listed in
App. 2
All substances which will be able to participate in
any water contamination have to be restricted and
must be kept as low as possible according to the
actual state of technology

Organic Compounds

Acrylamid
Benzol
1,2-Dichlorethan
Pflanzenschutzmittel und Biozidprodukte
Tetrachlorethen and Trichlorethen
Benzo-(a)-pyren
Epichlorhydrin
Polycyclic aromatic Hydrocarbons
Trihalogenmethane
Vinylchloride
Total organic Carbon (TOC)

Inorganic Compounds (App. 2)

Drinking Water Regulation
Parameter

Europe
Limit [mg/l]

TVO
Limit [mg/l]

Aluminium
Antimony
Arsenic
Barium
Boron
Cadmium
Calcium
Chromium
Copper
Iron
Potassium
Lead
Magnesium
Manganese
Mercury
Nickel
Selenium
Sodium
Silver
Zinc

0.2
0.005
0.01
n. i.
0.3
0.005
n. i.
0.05
2
0.2
n. i.
0.01
50
0.05
0.001
0.02
0.01
200
n. i.
n. i.

0.2
0.01
0.01
1
1
0.005
400
0.05
3
0.2
12
0.04
50
0.05
0.001
0.05
0.01
150
0.01
5

Latest Norms in Water Analysis

DIN/ ISO Norms:

Water Quality Control using
ICP-OES Spectrometry &
UV-VIS Spectrometry

TVO 2005: Chapter 2 Part II

. Maximum concentration levels of
elements have been reduced as
follows:
) Lead 0,05 >>>> 0,01 mg/l
) Copper 3 >>>> 2 mg/l
) Nickel 0,05 >>>> 0,02 mg/l

Determination of 32 Elements
using ICP-OES Spectrometry: ICPE-9000

Determination of 32 Elements

Multielement Calibration.

Systemsetup ICPE-9000
Ignition Mode:
Ultrasonic
Nebulizer
Attached Instruments:
Mini Torch,
Ultrasonic Nebulizer, Peristaltic Pump
Radio Frequency Power: 1.00 kW
Plasma Gas:
8.00 L/min
Auxiliary Gas:
0.60 L/min
Carrier Gas:
0.60 L/min
View Direction:
Axial/ Radial

Axial & Radial View

Emission Spectrum
Fe1ppm

Fe1000ppm

Spectral Interferences
Spectral
Interference
Element profile overlap and
are observed as a large
measurement profile

Target element
profile

+
Coexistent element
profile

Measurement profile

Target element +
coexisting element
profile

Cd Analysis in Fe Matrix
Identification

Identification

Cd 226.502

2000
1000

Fe

Intensity

4000
3000

2500

Cd
Intensity

Intensity

5000

Cd 228.802 Best

2000

Cd

1500
1000
Optimal wavelength
with no interference

The optimal wavelength differs with the matrix and

concentration

Cd Determination in Soil
Separation is difficult with simultaneous spectrometers

4000
3000
2000

2500

1500

Cd
F
e

Cd 214.438

Quantitative value Identification

1

18ppb

2000

Cd
As

1500

Intensity
Intensity

Intensity
Intensity

5000

Cd 228.802 Best

Quantitative value Identification

100ppb

Intensity
Intensity

Cd 226.502
Identification

1000

500

1000
1000

Which values should we use?

Quantitative value
40ppb

Cd
F
e

Measure IEC Sample As 20ppm

Cond 1

Cond 1

500

189.041
As 189.042
Pd 189.041

Intensity

Cd 228.802 Best

Intensity

As 189.042

228.804
Cd 228.802
5000

IEC Wavelength 189.042/ Cd Wavelength 228.802

Calculate Interfering element correction factor FI

Measure Unk Sample incl. As

IEC sample

Unknown sample

Cd
As

As
As

As

Cd 228.802nm

As 189.042nm

Cd228.802nm

As 189.042nm

Measure Unk at As 189.042 & Cd 228.802

Wavelength
Multiply the Intensity at As 189.042 with FI to
calculate the Intensity of As at 228.802
Cd Result is obtained by subtracting As

International Reference Material

Sample
Element

River water standard JACJAC-0032

quantitative

guaranteed

Pb

9.7

9.9 +/+/- 0.2

Cr

10.1

Cd

1.0

Cu

10.3

10.5 +/+/- 0.2

Fe

56.4

57 +/+/- 2

10.1 +/+/- 0.2

1.00 +/+/- 0.02

Mn

5.4

5.4 +/+/- 0.1

Zn

10.9

11.3 +/+/- 0.4

60.3

59 +/+/- 2

Al

61.2

61 +/+/- 2

Ni

9.9

10.2 +/+/- 0.3

Mo

0.4

Ca

12.3

Mg

2.8

2.86 +/+/- 0.04

Na

4.4

4.5 +/+/- 0.1

12.5 +/+/- 0.2

All Data [g/L], except * [mg/L]

Conclusion
ICPE-9000 is a state of the art tool for
easy determination of heavy metals in
environmental samples such as
drinking water!

Thank You