HYDRIDE GENERATION OPTIMIZATION

APPLIED TO As DETERMINATION IN WATER

BY MICROWAVE PLASMA ATOMIC EMISSION SPECTROMETRY.
Azcarate Rosana V. 1,2, Azcarate Silvana M.1,2, Camiña José M. 1,2, Savio Marianela1,2*.
1
Facultad Ciencias Exactas y Naturales, Universidad Nacional de La Pampa, Av.Uruguay 151, L6300XAI Santa Rosa, La Pampa, Argentina.
2
Instituto de Ciencias de la Tierra y Ambientales de La Pampa (INCITAP), Mendoza 109, L6302EPA Santa Rosa, La Pampa, Argentina.
*Author to whom correspondence should be addressed: marianelasavio@gmail.com QMT-0 61

I. Introduction
The World Health Organization (WHO) considers arsenic as one of the top most concern chemicals for public health. Arsenic is one of the most abundant element in earth crust, his released
compounds are associated with natural and human processes.
Design of Experiment (DoE) is superior compared to the classical ‘one variable at a time’ (OVAT). The quality of the information obtained by DoE is higher, and the number of experiments
required is smaller than the number of experiments performed with an OVAT approach.
The goal of this work is to show the advantages in terms of reduced experimental effort and improved quality of information, to reach the best experimental parameters in the
determination of arsenic throughout HG-MPAES.

II. Sample Preparation

Hydride generation was performed
As in sample by the Multimode Sample
Introduction System (MSIS),
HCl
Standards and samples
+ KI
Arsine generation which uses thin film hydride
technology for significantly better
were prepared using: performance than conventional
5% HCl NaBH4 nebulization
2.75 % KI Prereduction 30 minutes

III. Results
As HYDRIDE GENERATION OPTIMIZATION
Factor Selection
Central composite desing (CCD) face centered
Factors and level used in the 28-3 Fractional factorial desing

CCD face centered used to obtain the response surfaces.

Central Surface plot of signal
Factors Units Low (-) Point (0) High (+) Experiment RC SFR RT RAS*
1 - - - 41,4
2 + - - 41,5 The selected optimal values
A NaBH4 Concentration (RC) % 1 1,5 2
3 - + - 88,8 for these factors were:
B Acid Concentration (AC) % 5 27,5 50 4 + + - 100,0
5 - - + 41,6 2 % for RC
C Pre-reductant Concentration (PRC) % 0,5 2,75 5 6 + - + 39,8 48 rpm for SFR
7 - + + 86,2 5 s for RT
D Sample Flow Rate (SFR) rpm 10 29 48 8 + + + 94,6
9 -α 0 0 71,1
E Reagent/Acid Flow Rate (RFR) rpm 10 29 48 10 +α 0 0 75,8
11 0 -α 0 39,7
F Reading Time (RT) s 10 20 30 12 0 +α 0 94,4
13 0 0 -α 74,9
G Viewing Position (VP) -30 0 30 14 0 0 +α 76,6
15 0 0 0 75,5
H Nebulizer Gas Pressure (NGP) kPa 80 160 240 16 0 0 0 75,4
17 0 0 0 75,6
18 0 0 0 75,4
19 0 0 0 75,7
20 0 0 0 76,1
*Relative analytical signal (%).

MPAES optimized conditions

For As Hydride determination
MP-AES Analytical Performance
Nitrogen 140 psi
Air injection flow rate Low As
We are working to
Nebulizer/spray chamber Cyclonic spray chamber, Single Pass. LOD [μg.L ] -1
10.4 improve LODs
Arsenic Wavelenght (nm) 193.696 LOQ [μg.L-1] 29.8
Nebulizer pressure (kPa) 140
Viewing position 10
Acquisition mode Continuum Analytical Application
Integration time (s) 3
The variables SFR, RC and RT and its Background correction Auto The developed method was applied to
interaction are significantly affecting Number of pixels 3 underground water of La Pampa, Argentina.
the As hydride measurement efficiency Sample Flow Rate (rpm) 48 As levels in all samples were lower than
(95% confidence level) NaBH4 Flow Rate (rpm) 10 detection limits.
Uptake time(s) 15 The accuracy of the method has been verified
Stabilization time (s) 5 by using Standard Reference Material 1643e,
Cleaning time (s) 30 Trace Elements in Water.

IV. Conclusion
Systematic optimization procedures were carried out by selecting an objective The use of Experimental desing reduced experimental effort and improved
function; the most important factors were found and the relationship between quality of information, reaching the best experimental conditions for Arsenic
responses and factors were investigated using Response Surface Methods (RSM). determination by HG- MPAES

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