WAN HAFIZAH HUSNA BT WAN MUDA

2015826752
AS2533B1

ASSIGNMENT 1 CHM561
Question 1
State the standard method used for the analysis of PAHs in this
study.
-

US Enviromental Protection Energy (EPA)

Question 2
Identify the samples pretreatment involve in this work?
-

Soil preparation : Contaminated land soil was sampled from a known

site and then transported to the laboratory where it was air-dried for
24 hour prior to sieving through a 2 mm mesh at room temperature.
The fine powdered soil was then stored in an air-tight container until
required.

Question 3
What are the ASE experimental parameters considered and state
their levels.
-

Pressure : 1000psi, 1300psi, 1700psi, 2100psi, 2400psi

Temperature : 40oC, 70oC, 120oC, 170oC, 200oC
Extraction time : 2min, 6min, 9min, 13min, 16min

Question 4
Name the software used for DoE in this study.
-

Central composite design

Question 5
Explain the advantages of using this approach compare to
conventional method (COST Method).
-

It requires less resources like time, money and materials

It will estimate of the effects of each factor more precisely
Factor interactions can be estimated
Factor effects are studied over a wider range of levels of the other
factors

Questions 6
State the responses used in the optimization of ASE for the
extraction of PAHs.
-

Naphthalene
Acenaphthene
Phenanthrene
Fluoranthene
Benz[a]anthracene
Benzo[b]fluoranthene
Benzo[a]pyrene
Dibenzo[a,h]anthracene

Acenaphthylene
Fluorene
Anthracene
Pyrene
Chrysene
Benzo[k]fluoranthene
indeno[123-cd]pyrene
benzo[ghi]perylene

Question 7
Briefly explain how the results of this work are evaluated.
-

Design of experiment is an experiment that uses statistical tools and

methods to successfully study multiple factors in a single
experiment. So that this analysis was conducted by using ANOVA.
Multilinear regression was applied to the result of the central
composite design. Statistical treatment of the data for 16 individual
PAHs was collected. If the p value is less than 0.05, the individual
was significant.
When the result of this experiment was analyzed and evaluated,
they may help to identify optimal condition, the factors that most
influence the result and those that do not, as well as details such as
the existence of interactions and synergies between factors.

Question 8
The robustness of ASE for the extraction of PAH in contaminated
soil is demonstrated. How do the authors arrive with the
conclusion?
-

The robustness of a procedure is a measure of its capacity to remain

unaffected by small but deliberate variations in the method
parameters and provides an indication of its reliability in normal
usage
This robustness was involves internal factors to the method.
So that within the operating limits of the technique, the technique
was found to provide good recoveries.

Question 9
Why the authors used GC-MSD to report the results?
-

In case to report the result, GC-MSD was used to obtain the

comparison of the concentrations with GC-FID. Besides that, the
author used GC-MSD to report the results because there were no
notable differences observed between the data (correlation
coefficient, r=0.9240, r2=0.8537, n=224 determinations).
GC-MSD was done as it was not possible to separate all 16 PAHs
using the column in the GC-FID.
The enchanced sensitivity if the GC-MSD operated in SIM mode will
allow individual of PAHs that were not totally separated which were
benzo[b]fluoranthene and benzo[k]fluoranthene can be determined.

Question 10
If you are required to extract PAHs in sediment sample, what type
of solvent will you select? Give the reason for your answer.
-

All solvents used were analytical grade which were acetone,

dichloromethane, methanol, hexane and acetonitrile.
The selection of organic solvents, singly or in combination, was
chosen to investigate their influence on the recovery of PAHs.