UJIAN AKHIR SEMESTER

PROGRAM S1 PRASETIYA MULYA

SEMESTER GANJIL ANGKATAN 2019

Mata Kuliah : FBTU2113 - ANALYTICAL CHEMISTRY

Hari & Tanggal : Senin, 11 Januari 2021
Waktu : 14:00 – 16:30 WIB (150 menit)
Sifat : Open notes, Calculator allowed

Section A – Fill in the blank

Directions for Section A

Fill in the blank with the name of each equipment.
A correct answer scores 1, an incorrect answer scores 0.

1 2 3 4 5 6 7 8 9 10

Name of Common Laboratory Equipment in

No
Indonesian English
1 Buret Burette
2 Pipet Volumetrik Volumetric pipette
3 Pipet tetes Drop pipette
4 Mikropipet Micropipette
5 Gelas ukur Measuring cylinder glass
6 Labu ukur Volumetric flask
7 Labu erlenmeyer Erlenmeyer lask
8 Gelas beaker Beaker glass
9 Botol semprot Wash bottle
10 Cincin gabus Flask cork stand

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Section B – Matching

Instruction for Section B

Match the following terms to the corresponding description on the question paper. (1 point for each
correct response).

Analytical method types:

1. High-performance liquid chromatography (HPLC); 2. Gas-liquid chromatography (GLC), also called gas
chromatography (GC); 3. Colorimeter; 4. Atomic absorption spectroscopy (AAS); 5. Inductively coupled
plasma spectrometry (ICP); 6. Flame photometry; 7. Fluorometry (fluorescence spectroscopy or
spectrofluorometry); 8. Titrimetry/titration; 9. Gravimetric analysis; 10. Mass spectrometer (MS)

Number of term Description of analytical method types

The method uses emission spectroscopy in the ultraviolet and visible regions to identify
Flame
and estimate the amounts of various minerals excited in a flame, an arc or high voltage
photometry
spark.
The method uses a device to test the concentration of a solution by measuring its
Colorimeter absorbance of a specific wave length of light. Important issues are calibration, size of
the filter and wave length of the light.
It is an analytical technique for the determination of the elemental composition of a
Mass sample or molecule. Its principle consists of ionizing chemical compounds to generate
spectrometer charged molecules or molecule fragments and measurement of their mass-to-charge
ratios. It can be used alone or in combination with other instruments.
The method is a separation technique in which the mobile phase is a liquid. It can be
carried out in a column. In general, it uses very small particles and a relatively high inlet
HPLC
pressure, and is used extensively in food composition (e.g. fatty acids, amino acids,
sugars, polyols, oligosaccharides, vitamins and many non-nutrients).
The method determines the quantity of a substance A by gradually adding known
concentrations of another substance B with provision for some means of indicating the
endpoint, at which essentially all of A has reacted with B. The amount of A to be
Titrimetry calculated from the known amount of B added up to this endpoint and the reacting
weight ratio of A to B should be known from stoichiometry or otherwise. The method
can be used for vitamin C, calcium, magnesium and protein O even though it is not the
preferred method for any of these compounds.
This method is capable of determining simultaneously a range of metals and several
ICP non-metals but is highly expensive. If it is coupled with mass spectrometer, the method
is highly sensitive even at low concentrations and can determine isotopic speciations.
The method is a type of electromagnetic spectroscopy that analyses fluorescence from
a sample. It involves using a beam of light, usually ultraviolet light, that excites the
Fluorometry electrons in molecules of certain compounds and causes them to emit light of lower
energy, typically, but not necessarily, visible light. It can be used to determine vitamin
C, thiamin or riboflavin.
The method is used for the quantitative determination of an analyte based on its mass
in a solid form. The analyte can be removed from a solution or from the food through
Gravimetric filtration or vaporization and then weighed; or it must first be converted to a solid by
analysis precipitation with an appropriate reagent. The precipitate can then be collected by
filtration, washed, dried to remove traces of moisture from the solution, and weighed.
The amount of analyte in the original sample can then be calculated from the mass of
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 the precipitate and its chemical composition. This is used for water, dietary fibre
(Prosky method) or sulphur.
The method is a technique for determining the concentration of a particular mineral in
a sample. The electrons of the atoms in the atomizer can be promoted to higher
orbitals for an instant by absorbing a specific quantity of energy (i.e. light of a given
AAS
wave length). This amount of energy (or wave length) is specific to a particular electron
transition in a particular element and, in general, each wave length corresponds to only
one element. This gives the technique its elemental selectivity.
The method is a type of chromatography in which the mobile phase is a carrier gas,
usually an inert gas such as helium or an unreactive gas such as nitrogen. The
stationary phase is a microscopic layer of liquid or polymer on an inert solid support
Gas inside a column. The interactions of these gaseous analytes with the walls of the
chromatography column (coated by different stationary phases) cause different compounds to elute at
different times, called retention time. The comparison of these retention times is the
analytical power of this technique, which is used, for example, in the analysis of fatty
acids, alcohol, sugars, polyols, oligosaccharides, iodine, and vitamins D, E and C.

Section C – Essay

Instruction for Section C

Answer all questions on the answer sheet.

1. Molecules that absorb in the UV-vis region generally contain a double bond in the form of C=C, C=O or
a benzene ring. The longer the conjugated chain (delocalised system), the longer the wavelength of
radiation absorbed. Arrange the following molecules in order of the wavelength of ultraviolet/visible
radiation that they absorb (shortest first): (15 pts).

Answer:

V ; II ; I ; IV ; VI ; III

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2. An experiment was carried out to determine the amount of nickel present in a sample of shellfish. 0.200
g of the shellfish flesh was taken and heated with concentrated nitric acid. The sample was made up to
a total volume of 100.0 cm3 with de-ionised water and the absorbance measured in an atomic
absorption spectrometer at 232 nm. The absorbance of the sample was 0.320. The calibration curve for
nickel at 232 nm is shown below. (15 pts)

a. Explain how the calibration

curve could be obtained.

b. Determine the amount of nickel

that would be present in 1.00 g of
shellfish flesh.

Answer:

A. 1. Mempersiapkan larutan standar : larutan standar dipersiapkan dengan konsentrasi nikel

sebesar 0, 20, 40, 60, 80, dan 100 mikrogram/dm-3.
2. Pengukuran absorbansi : larutan standar dengan konsentrasi tersebut diukur absorbansinya
menggunakan spektrofotometer dengan Panjang gelombang sebesar 232 nm.
3. Pembuatan kurva : kurva dibuat dengan mengisi absorbansi larutan standar sebagai absis y dan
konsentrasi larutan standar sebagai absis x.
B. Y = 200x + 0
0,32 = 200x
0,0016 mikrogram/dm-3 = x
Konsentrasi (x) ini mewakili jumlah nikel dalam gram per satuan volume. Karena sampel dibuat
hingga volume total 100,0 cm³, jumlah nikel dalam sampel 0,200 g dapat dihitung menggunakan
konsentrasi:

Sekarang, untuk menentukan jumlah nikel dalam 1,00 g daging kerang, kita dapat membuat
perbandingan:

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3. A sample containing compounds 1, 2, and 3 is analyzed via LC using a column packed with a silica-based
C18 bonded phase. A 1:5 solution of ethanol and H2O was used as the mobile phase. The following
chromatogram was obtained. (15 pts)

Assuming that the separation of compounds is

based on their polarity,

a. Is this normal- or reversed-phase

chromatography? Explain your answer.

b. Which compound is the most polar?

c. How would you change the mobile phase so

that compound 3 would elute sooner, without
changing the relative positions of compounds 1
and 2? Explain why this would work.

d. What could possibly happen if you maintained an isocratic elution mode at low solvent strength?

Answer:

a. Penggunaan fase terikat C18 berbasis silika menunjukkan bahwa pemisahan kromatografi cair ini
beroperasi dalam mode fase terbalik karena fase diamnya yaitu silika bersifat non polar,
sementara fase geraknya yaitu etanol dan air bersifat polar.
b. Senyawa yang paling polar yaitu senyawa 1 karena dalam kromatografi cair, senyawa yang paling
polar akan terelusi lebih awal.
c. Untuk membuat senyawa 3 terelusi lebih cepat dalam kromatografi cair fase terbalik tanpa
mengubah posisi relatif senyawa 1 dan 2, komposisi fase gerak dapat diatur. Secara khusus,
peningkatan kandungan organik pada fase gerak dapat menyebabkan elusi senyawa 3 lebih awal.
Hal ini terjadi karena kandungan organik yang lebih tinggi dalam fase gerak mengurangi retensi
senyawa polar, seperti senyawa 3, yang menyebabkan lebih awalnya elusi senyawa 3 elusi.
Perubahan urutan elusi disebabkan oleh perubahan interaksi antara analit dan fase diam sebagai
akibat dari modifikasi komposisi fase gerak. Oleh karena itu, dengan meningkatkan kandungan
organik pada fase gerak, senyawa 3, karena lebih polar, akan lebih cepat terelusi, sedangkan
posisi relatif senyawa 1 dan 2 tetap tidak berubah.
d. Jika mode elusi isokratik dipertahankan pada kekuatan pelarut yang rendah, hal ini dapat
mengakibatkan pemisahan yang buruk dan resolusi analit yang rendah. Hal ini karena kekuatan
pelarut yang rendah mungkin tidak memberikan daya elusi yang cukup untuk memisahkan analit

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 secara efektif. Selain itu, kekuatan pelarut yang rendah dapat menyebabkan waktu retensi yang
lebih lama dan puncak yang lebih luas, sehingga sulit untuk membedakan senyawa yang
berkerabat dekat.
4. 1.235 g of a solute with a molar mass of 117.3 g/mol is dissolved in 10.00 mL of water. After extracting
with 5.00 mL of toluene, 0.889 g of the solute is recovered in the organic phase. (a) What is the solute’s
distribution ratio between water and toluene? (b) If we extract 20.00 mL of an aqueous solution
containing the solute with 10.00 mL of toluene, what is the extraction efficiency? (c) How many
extractions will we need to recover 99.9% of the solute? (15 pts)

Answer:
a. Langkah :

b. Langkah :

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c. Langkah :

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