NAME:DO HOANG HIEP

Class:k60 Advanced Chemistry

Prelab: Determination of arsenic by hydride generation vapor

atomic absorption spectrometry (HVG-AAS)

1.Purpose

The focus of this experiment is the quantitative method for the determination of total
inorganic arsenic As(III) and As(V) by using NaBH4 in acid media

2. Procedure used to determine the total As (III) and As(V) by HVG-

AAS in this experiment.
The arsine gas (from sodium borohydride and strong acid) produced were then carried into a
separator, in which the gas phase was separated from the liquid phase and was passed on
to the absorption cell by argon gas, while the liquid phase was drained off. The absorption
cell was heated by an air-acetylene flame to pyrolyze hydride to arsenic atoms.(HVG) Back-
ground-corrected (continuous deuterium lamp) absorbance values were recorded, and the
peak heights were used for quantitative determination using the wizAAard software
(Shimadzu).
The atomic absorption spectrometry (AAS)uses absorption of light of intrinsic wavelengths
by atoms. All atoms are classified into those having low energies and those having high
energies. The state having low energies is called the ground state and the state having high
energies is called the excited state.
The atom in the ground state absorbs external energies and is put in the excited
state.
The difference between energies in the ground state, and in the excited state is fixed by the
element and wavelength of light to be absorbed.

the As(V) oxidation state of arsenic, is reduced relatively slowly by sodium borohydride to
As(III), which is then instantaneously converted to AsH3. The AsH3 atomic absorption peaks
commonly are decreased by one-fourth to one-third for As(V) when compared to As(III).
Determination of total arsenic requires that all inorganic arsenic compounds be in the As(III)
state. Organic and inorganic forms of arsenic are first oxidized to As(V) by acid digestion.
The As(V) then is quantitatively reduced to As(III) with sodium or potassium iodide before
reaction with sodium borohydride.

Procedure:
Sample collection, preservation, and handling
− All samples must have been collected using a sampling plan.
− All samples plastic containers must be prewashed with detergents, acids, and
water. Both plastic and glass containers are suitable.
➢ Sampling:
− All water samples must be filtered through paper filter and then acidified at the time
of collection with HCl (5 mL/L).
− Other samples must be treated to transfer solution before determination arsenic in
those by HVG-AAS.
Instrument setup
Connect inlet of reaction cell with auxiliary purging gas controlled by flow meter. Before
using the hydride generation/analysis system, optimize operating parameters. Align quartz
atomizers for maximum absorbance. Aspirate a blank until memory effects are removed.
Establish purging gas flow, concentration and rate of addition of sodium borohydride
reagent, solution volume, and stirring rate for optimum instrument response for the chemical
species to be analyzed. Optimize quartz cell temperature. If sodium borohydride reagent is
added too quickly, rapid evolution of hydrogen will unbalance the system. If the volume of
solution being purged is too large, the absorption signal will be decreased.

➢ Other parameters:- Wavelenght: 193.7 nm; slit width is 0.5 nm; The lamp current was 10
mA.
- Height burner: 14 mm
- Fuel gas flow rate: 1.4L/min C2H2 + 8.0L/min Air
- Sample solution flow rate: 5.0 6.0 mL/min.
Instrument calibration standards
Pipet 0.00, 0.10, 0.20, 0.30, 0.40 mL of working standard solutions of As(III) to 25mL
volumetric flasks and bring to volume with water containing the same acid concentration and
the same prereductant one used for sample preservation (commonly 2% HCl and 0.5% KI).
This yields blank and standard solutions of 0, 2, 4, 6, 8 ppb (See Table 1).
Prepare fresh daily. In all cases, standards must be carried through the same digestion
protocol as the samples to monitor digestion effectiveness.

Determination of As with sodium borohydride

To 10.0 mL digested water sample and 1.0 mL other sample in volumetric flasks add 2.0 mL
HCl (1:1). Then, add 1.0 mL KI (10%) prereductant solution, mix, and wait at least 15 min for
the reduction of As (V) to As( III). Blanks and standards were prepared in the same manner.
Turn on strip-chart recorder and wait until the base line is established by the purging gas and
all air is expelled from the reaction cell. After the instrument absorbance has reached a
maximum and returned to the base line, remove beaker, rinse dispersion tube with water,
and proceed to the next standard and sample.

3. Calculate arsenic content in the samples.

Calculation
Construct a standard curve by plotting peak heights or areas of standards versus
concentration of standards. Measure peak heights or areas of samples and read
concentrations from curve. If sample was diluted (or concentrated) before sample digestion,
apply an appropriate factor. On instruments so equipped, read concentrations directly after
standard calibration.

4. Which other technique can be used to determine total As by AAS

methods ?
F-AAS GF-AAS ETA-AAS but sensitivity of these method could not to
compare with HVG-AAS