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Experiment 2: Acid Digestion &

Heavy Metal Analysis


Date of prelab: 26th of May 2017
Date of lab: 6th of June 017
Group: 7

Role Name Student ID


Planner Wan Nurliayana Wan Bahanudin 2014103797
Experimenter Muhammad Julfikar Jamal 2014577253
Analyzer Nooreffandi Ariffin 204364663

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OBJECTIVES
To design experiment procedure for the
heavy metal analysis
To identify the presence of heavy metal in the
soil sample.
To determine the heavy metal elements in
soil by using AAS

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LIST OF FORMULA
100
, =

Where:

A = concentration of metal in digested solution (mg/L)


B = final volume of digested solution, mL (100 mL)
C = total solid, (%) refer Standard Method APHA 2005 Section 2540G

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PROCEDURE
a) Acid Digestion Procedure
1. Compose sample is dry and grind to size < 150m. Then,
weight the compose sample to 1 g and add to 50 ml beaker.
2. Pour 10ml concentrated nitric acid into the beaker and close
the beaker with glass lid. Heat the mixture on hot plate for 10
min and cool the mixture.
3. Add 5ml concentrated nitric acid once more for 30 min. if the
brownish gas is release add more 5 ml of concentrated nitric
acid until the reaction stop. Then let the mixture cool down.

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PROCEDURE (CONT.)
4. Add 2 ml of distilled water and 3 ml of hydrogen peroxide
to mixture and then heat up the mixture. Add 1 ml of
hydrogen peroxide continuously but not exceed to 10 ml.
The step is repeated until there is no changes occur with
the volume 5 ml. let the sample cool down.
5. Add 10 ml of concentrated HCL acid into mixture and
heat up for 15 min.
6. Filter the digested sample solution and then dilute with
100 ml of distilled water (volume = 100 ml (filter + distilled
water).
7. Analyze the sample using Atomic absorption spectroscopy
(AAS) to determine the heavy metal such as Fe, Cu, Zn,
and Cd.

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PROCEDURE (CONT.)
b) Analysis procedure
START UP
1. Turn on the computer, Double click on the WizAArd shortcut on
the desktop.
2. The Operation tab should be highlighted. Click on the picture of
the AAS.
3. Enter admin for the user id and hit ok.
4. The program opens with wizard selection.
5. Select the " element selection" Icon and press OK.
6. Element selection window will appear .
7. First click on the "select Element" Than load parameters will
appear.
8. Instrument check list for Flame analysis will open. Tick all the
boxes and press OK
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PROCEDURE (CONT.)
OPERATING PROCEDURE
1. Add 2 ml of distilled water and 3 ml of hydrogen peroxide to
mixture and then heat up the mixture. Add 1 ml of hydrogen
peroxide continuously but not exceed to 10 ml. The step is
repeated until there is no changes occur with the volume 5
ml. let the sample cool down.
2. Add 10 ml of concentrated HCL acid into mixture and heat up
for 15 min.
3. Filter the digested sample solution and then dilute with 100
ml of distilled water (volume = 100 ml (filter + distilled water).
4. Analyze the sample using Atomic absorption spectroscopy
(AAS) to determine the heavy metal such as Fe, Cu, Zn, and
Cd.
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PROCEDURE (CONT.)
SHUT DOWN PROCEDURE
1. Press the Extinguish button on the front of the instrument.
2. Close the main tank valve on the acetylene tank.
3. Purge the line of acetylene by pressing the Purge button.
4. Close the air valve which is below the bench.
5. Make sure that both the meters are showing zero reading
(One on the acetylene gas cylinder and one below the bench
of AA instrument.)
6. Turn off the power to the AAS. Exit out of the software

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RAW DATA TABLE
Table 1 : Heavy metal analysis in solution

Type of metal Concentration (mg/L)

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CALCULATED DATA TABLE
Table 1 : Heavy metal analysis in solution

Type of metal Concentration (mg/kg)

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