Experiment 4: Flow Injection Analyst System(FIAS)

1.0 Introduction

The determination and monitoring of sub-ppb concentration of mercury

has always been of special importance in the field of trace metal analysis.
For more than 500 years, mercury has been recognized as a poison. Today,
mercury pollution is a global problem. To control the amount of mercury
polluting our environment, mercury has to be monitored in all areas of
modern life. This requires fast, cost-efficient and easy-to-use methods and
instrumentation that permit the determination of mercury at levels as low as
a few ng/L. By using Flow Injection Analyst System (FIAS), we conduct an
experiment to determine the calibration curve for mercury.

2.0 Objectives

1. To determine the calibration curve for mercury standard, Hg.

3.0 Procedures

Spectrometer:

Technique AA
Integration Time(s) 20
Data Processing Peak Height, Smoothing 0.5 sec or 19
points
Lamp HCL or EDL
Slit (nm) 0.7 (Low or Alt)
Wavelength (nm) 253.7

FIAS-System
• Cell Temperature : 100
Reagents:
a. Carrier Solution : 3% (v/v) HCL
b. Reducing Agent : 0.2% NaBH4 in 0.05% NaOH
c. Sample solution: Hg2+ in slightly acidified solution.

Sensitivity Check:
Analysis of 500 L of a 10 L mercury solution should provide a signal of
about 0.07 A.

3.1 Experimental
Reagent preparation

(a) Preparation of 3% (v/v) HCL

 30 mL of HCL was prepared in 1000 mL volumetric flask to obtained 3%
(v/v) of HCL.
(b)Preparation of reductant, NaBH4
0.50g of NaOH was weighed and transferred to a 1000 ml volumetric flask
and distilled water was added. Shake until all is dissolved. 2g of NaBH4
was dissolved in 1000mL of volumetric flask using distilled water. Both of
them were mixed together.

(c) Mercury stock solution, 1000 ppm

1000 ppm mercury stock solution was used to prepare for standard
solutions.

(d) Mercury standard solution, 1 ppm

1 ppm mercury stock solution was prepared by transferring 0.1mL of 1000
ppm stock solution and diluting to 100 mL volumetric flask using distilled
water.

(e) Working standard solution

Various Hg working standard solutions were prepared in 100 mL
volumetric flask. The volume of Cu stock solution that needs to be taken
to prepare standard solution is represented in Table 1.0 below
Table 1.0 Various concentration of standard solution.

Concentration of Hg Volume of 1.00 ppm

(ppb) Hg Std.Sol. (mL)
10 1.00
20 2.00
30 3.00

*1-2 drops of a 5% (w/v) KMnO4 were added in each standard solution to

stabilize.

(f) Sample mercury solution , 10 ppb

10 ppb Hg was analyzed as a sample.
 Figure 1 : FIAS Tubing Setup
4.0 Discussion

The calibration curve, absorbance versus concentration of mercury, Hg

was plotted and the linear coefficient (R2 = 0.991) was obtained. Analysis
of sample 10 ppb showed that the solution is containing 10 ppb of Hg with
the absorbance of 0.089. Sensitivity check was conducted and the
absorbance reading for 10 ppb obtained was 0.086. This shows that FIAS
is a sensitive instrument.

5.0 Conclusion

As a conclusion, FIAS is a sensitive instrument which can detect elements

concentration up to ppb. By using FIAS, we can determine the concentration of
mercury in our sample.

6.0 References

1. Holler, Skoog, Crouch (6th Edition). Flow Injection Analysis: Principle of

Instrumental Analysis.
2. Trojanowicz, Marek (2000). Flow injection analysis: instrumentation
and applications. Singapore: World Scientific. ISBN 981-02-2710-8