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The Chinese University of Hong Kong
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Course Examination 1st Term, 2016-2017
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Course Code & Title : CHEM 4440 Food Testing & Environmental Analysis
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Time allowed:

Student I.D. No.:

2 hours
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Seat No.:
0 minutes

Important Note:
1. Attempt all questions.
2. Write your student I.D. No. and Seat No. on the question book, on the answer book
and on ALL submitted attachments.
3. Write answers in the answer book, clearly marking which question and its parts
your answer corresponds to.
4. Mark on the front cover of the answer book the question numbers of ALL
attempted questions.
5. Answer in English.

Question 1
In the analysis of sorbic acid in food by GC-MS, the following sample pre-treatment steps
are involved:
a) The chopped and blended sample was acidified with sulphuric acid. Ethyl acetate
and sand, and also the internal standards phenylacetic acid and caproic acid, were added.
b) The mixture from above was centrifuged and the upper liquid layer was extracted
with NaOH and saturated NaCl solution.
c) The NaOH extract is transferred to solvent/solvent extraction apparatus, acidified
with HCl to methyl orange and dichloromethane is added. This mixture is shaken and
the dichloromethane layer is collected,
d) The dichloromethane extract is filtered with anhydrous Na2SO4 added to the filter
paper.

I. For the steps listed in a) to d) above, explain the following:

i) Why is sulphuric acid added in a)? (2 marks)
ii) Why is sand added in a)? (2 marks)
iii) What is the upper layer liquid in b)? (2 marks)
iv) Why is NaOH used in b)? (2 marks)
v) What is the purpose of adding saturated NaCl in b)? (2 marks)
vi) Why was the NaOH extract acidified in c)? (2 marks)
Course Code : _ _,C"'H,.,_.,E""M.,__..:.:4.::.4:,,;40e,__ _ _ _ _ __ Page 2 of3

Question 1 (cont'd)
vii) Why is the dichloromethane extract filtered over anhydrous Na2SO4? (2 marks)

II. Sorbic acid may be analysed by HPLC/UV or by GC/MS. Compare and contrast these
two anlaysis techniques in terms of accuracy, precision, sensitivity, detection limit,
selectivity and cost. (6 marks)

Question 2
a) Give 2 reasons why we need to refer to their respective regulations for our food and
environmental analysis. (4 marks)
b) Which of the following (international) standard method(s) is/are most frequently used
in Hong Kong for the chemical analysis of water quality: ASTM, BS, AOAC, USEPA
and/or APHA? (2 marks)
c) Which of the following regulations (Cap 133, Cap 132, Cap 311, Cap 358) are used for
monitoring
i. sulphur dioxide in food?
ii. sulphur dioxide in air?
(2 marks)

Question 3
You were given a river water sample for analysis of soluble phosphate and total
phosphorus.
a) Describe how you would pre-treat the sample to generate samples for each of these 2
analyses (i.e., the samples fo1· Jill & assay),
(5 marks)
b) Outline, with the chemical principles behind, the colorimetric method for the analysis
of soluble silicate in the presence of soluble phosphate in a water sample.
(chemical names instead of molecular formulae are acceptable.) (5 marks)

Question 4
a) The conventional method for protein analysis in milk powder is by determination of
total N. One of the methods is by oxidation and then titration with HCl. ~
briefly outline the procedure, (6 marks)

b) On the other hand, a common method for determination of total N in river water is by
colorimetry, One of the colorimetric methods is by oxidation and reaction with the
colorimetric reagent N-(1-napthyl)-ethylenediamine dihydrochloride (NNED). State
what is the chemical form of the N after oxidation (2 marks). For the reaction with
NNED, two other reagents are required. Name these 2 reagents and their purpose (4
marks). State the inorganic form of N which is required for the reaction with NNED
(2 marks),
Course Code : CHEM 4440 Page 3 of3

Question 4 (Cont'd)
c) Compare and contrast these two anlaysis techniques (total N by titration and total N
by colorimetric reaction) in terms of accuracy, sensitivity, detection limit, selectivity
and efficiency. (5 marks)

d) Recovery is one of the QC parameters used to monitor the performance of the analysis.
It was found that in the analysis of total N for a batch of river water samples, the
recovery of the (total N) spiked sample was 130%. If the recovery criterion is
80-120%, has the analysis passed this QC parameter? Suggest 3 possible causes for
such recovery result. (4 marks)

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