Determination of Arsenic

EXPERIMENTAL
NOTES Optima™ 8000 ICP-OES
ICP-OES-ENV Author
Mr. Sachin Salunkhe
Inorganic - Application Specialist
Customer Knowledge Centre for Analytical Sciences
PerkinElmer (India) Pvt. Ltd.
Thane – 400 615 India.
Email: [email protected]
Determination of Arsenic,
Mercury and Selenium in
Seawater by Continuous Flow
Hydride Generation Inductively
Coupled Plasma Optical Emission
Spectrometery (ICP-OES)
Abstract
The analysis of Arsenic, Mercury and Selenium in sea water at trace level is challenging
because of matrix interference from salt. The commonly employed analysis method for
these trace metals using ICP-MS is challenging due to matrix and spectral interferences.
In this work we demonstrated the capability of a Perkin Elmer® OptimaTM 8000 ICP-OES
coupled to a FIAS Manifold hydride Kit to analyse very low levels of As, Hg and Se in such
high matrix sample. This method provides fast analysis, good repeatability and freedom
from interferences.
Standard and sample preparation

Reducing solution (For Arsenic): 5 g each of pure grade Ascorbic 50 mL in polypropylene vial with deionized water (18 mΩ). All
acid was mixed with 5 g of Potassium iodide and dissolved in 100 standard solutions for Selenium were treated in same way before
mL deionized water (18 mΩ) in a polypropylene vessel. dilution.
Pre-reduction of samples and standards: Mercury: Added 2-3 drops of 5% KMnO4 in all standard and
Arsenic: 25 mL of sample was taken in 50 mL polypropylene sample solutions in order to oxidise mercury.
vessel. 5mL concentrated HCl (suprapure grade) and 5 mL Reductant Solution: NaBH4 was used as a reductant. Its
reducing solution were added into the vessel. The treated samples concentration was 0.2% in 0.05% NaOH.
were then allowed to stand for 30-40 minutes. After prereduction
All above chemicals were of high purity grade.
the solutions were diluted to 50 mL with deionised water
(18 mΩ). All calibration standards for Arsenic were prepared in
same way.
Selenium: 25 mL of sample was taken in 100 mL glass beaker.
The solution was prereduced prior to analysis by adding 5 mL
concentrated HCl (suprapure grade) followed by heating at 90oC
for 20 minutes. After prereduction the solutions were diluted to
Instrumental conditions Element Wavelength Results Spiked sample %
(nm) (ng/mL) concentration Recovery
OptimaTM 8000 Optimized Experimental Conditions
(ng/mL)
Plasma gas flow 8 L/min
Arsenic, As 193.696 <0.4 5.1 100.8
Auxiliary gas flow 0.4 L/min
Mercury, Hg 253.652 <0.7 4.7 88.0
Nebulizer gas flow 0.7 L/min
Selenium, 196.026 <0.6 4.6 90.0
RF power 1500 Watts
Se
Viewing height 15 mm
Plasma view Axial The values reported are the minimum quantification limits for the
Read parameters Auto above method developed for the sea water samples. An accurate
Peristaltic pump flow rate 1.0 mL/min and highly reproducible method was developed for the analysis
Processing Peak Area of very low level impurities in very high matrix sample Sea water.
Calibration Linear Calculated Intercept ICP-OES is an excellent technique for the determination of trace
Injector Alumina 2.0 mm i.d. level elements in sea water as it provides good detection limit.
Quartz torch 1- slot
For Hydride Generation
Equipment FIAS Manifold
Analytical results & conclusions

The prepared sample solutions were analyzed using a FIAS
manifold coupled with an OptimaTM 8000 ICP-OES (PerkinElmer,
Inc., Shelton, CT, USA) equipped with WinLab32™ for ICP,
Version 7.0 software. The three point calibration curves (1, 5
and 10 ng/mL) gave correlation coefficients better than 0.999.
A quality control check (QC) was performed at the midpoint of
calibration and was monitored to ensure that the recovery for all
analytes to fall within the 90 -110% range. As the concentrations
were in low ppb levels axial mode was used for the said analysis.
The wavelengths used for the analysis and results are given in
below table. For further confirmation the spiked recoveries was
done at concentration 5 ng/mL.

Determination of Arsenic

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EXPERIMENTAL

NOTES Optima™ 8000 ICP-OES

Standard and sample preparation

Analytical results & conclusions

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