Kuliah Analisa Organik-Ppt-3

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AKM21354 - Analisis Organik

2 SKS/ KELAS B

Ismiyarto, S.Si., M.Si., Ph.D


Ngadiwiyana, S.Si., M.Si

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Bahan Kajian Sampai Dengan UTS
1. Sistematika Identifikasi Senyawa Organik
2. Identifikasi Senyawa Unknown  Uji pendahuluan, sifat fisik dan uji
kelarutan
3. Analisis elemen dalam senyawa organik secara kualitatif dan kuantitatif.
4. Identifikasi Senyawa Unknown  Penentuan berat molekul, Penentuan
rumus molekul
5. Korelasi struktur dan sifat fisik : titik lebur, titik beku dan titik didih
6. Korelasi struktur dan sifat fisik : indeks bias, spesifik gravity dan
putaran optik.
7. Penentuan metode kemurnian : kromatografi, titik lebur
distilasi
8. UTS

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Bahan Kajian Setelah UTS
1. Metode Pemurnian Senyawa Organik : ekstraksi , distilasi & sublimasi
2. Metode Pemurnian Senyawa Organik : kromatografi Lapis Tipis, HPLC , GC
dan Kolom Kromatografi
3. Klasifikasi senyawa Organik berdasar kelarutan : penentuan kelarutan,
teori kelarutan, Strutur molekul & kelarutan
4. enentuan gugus fungsi secara kimia : asam anhidrida, asil halida, alkohol,
aldehid dan Amina
5. Identifikasi Penetuan gugus fungsi secara kimia : karbohidrat , b.asam
karboksilat, ester, eter, halida, dan hidrokarbon
6. hhhPenetapan struktur kimia senyawa baru
7. Elusidasi struktur senyawa organik
8. UAS

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Komposisi Penilaian
Tugas 1/ UTS  20% dan 30%
Tugas 2/ UTS  20% dan 30%

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Media Pembelajaran
Kuliah Analisa Organik
1. KULON UNDIP 2020
2. MT yang tersedia di SIAP UNDIP 2020

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Pustaka
Dr. Ramy Y. Morjan, 2009, Chemical Identification of Organic
Compounds-PPT, Assistant Professor of Organic Chemistry Chemistry
Department-IUG

https://www.slideserve.com/hei/shriner-hermann-morril-curtin-and-fuson-
the-systematic-identification-of-organic-compounds-j-wiley-and-sons-inc-8

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Organic Analysis
Organic chemists regularly needs to identify the
compounds that are formed in chemical reactions or
isolated from natural sources.
In order to identify an unknown organic compound
you must first find which functional groups it
contains and then determining its molecular and
three-dimensional structure.
Chemical and Spectroscopic methods are used by
organic chemists to determining the molecular and
three-dimensional structure of any unknown sample.
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As a result of the advance developments of the spectroscopic
and analytical methods, the chemical methods of
identification of unknown organic compounds in no longer
existed.

However; the chemical methods are still used as important


way to enhance the students laboratory skills as well as to
improve the students understanding of many different aspects
of organic chemistry.

In this course you will have the opportunities to learn and use
the techniques of organic qualitative analysis while
determining the identity of sample compounds whose
identities are unknown to you

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Chemical Analyses (CA)
C.A. are generally divided into two broad categories

Qualitative Analysis Quantitative Analysis

Qualitative analysis deals with the determination of what


is present i.e. N, Cl, S……etc

Quantitative analysis deals with the determination of how much is present.

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IDENTIFICATION OF UNKNOWNS

In simple words the identification of unknown organic


compound means the establishing of its molecular and
structural formula. This can be achieved either by
spectroscopic methods or via chemical methods

Spectroscopic methods:
Involve using I.R, Mass Spectrometry,
H NMR, C NMR any few other techniques.
(Kuliah Elusidasi Struktur Molekul Organik)

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Chemical methods:
Involve the examination of :
1. the physical properties of the unknown
and
2. classification by solubility and
3. elemental analysis by sodium fusion
classification tests for functional groups
and
4. synthesis of solid derivatives

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Pure Sample Impure Sample

Needs purification
Physical state
Distillation

Solubility class
Chromatography
Elemental Analysis
Recrystalization
Functional group test
Sublimation
Synthesis of derivatives
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Bahan Kajian Sampai Dengan UTS
1. Sistematika Identifikasi Senyawa Organik
2. Identifikasi Senyawa Unknown  Uji pendahuluan, sifat fisik dan uji
kelarutan
3. Analisis elemen dalam senyawa organik secara kualitatif dan
kuantitatif.
4. Identifikasi Senyawa Unknown  Penentuan berat molekul,
Penentuan rumus molekul
5. Korelasi struktur dan sifat fisik : titik lebur, titik beku dan titik didih
6. Korelasi struktur dan sifat fisik : indeks bias, spesifik gravity dan
putaran optik.
7. Penentuan metode kemurnian : kromatografi, titik lebur
distilasi
8. UTS

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Uji pendahuluan
1. The physical appearance of an unknown will be your
first datum in the search to discover its identity

2. Simply knowing that the compound is a solid rather


than a liquid at room temperature narrows the
search considerably.

3. A few solids have characteristic bright colors that


may be of great significance in reaching a final answer.

4. The color of a liquid sample must be interpreted more


cautiously, because many liquid compounds oxidize
when they are stored for a long time.

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Colour
Colour: Many liquid and solid organic compounds are
coloured. They are coloured because of the presence of
chromophoric groups in the molecules.

Chromophore :A chemical group capable of selective light


absorption resulting in the coloration of certain organic
compounds. Chromophores are generally groups of atoms
having delocalized electrons. For example;
C=N, C=S, NO2, N=N,

The more conjugated a compound is the more the absorption


is, as the conjugation in a molecule make the absorption to
appear at higher wavelength

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Odor
Odor: Many organic compounds have a characteristic
Odor. Generally specking the odor is more clear for
Compounds with lower molecular weight.

The following compounds are common in the lab and


They have characteristic odor.You will be able to recognised
their odour Easley.

Benzaldehyde has the odor of bitter almond


Esters have nice odor
Anotrher examples are
Alcohol, acetone and diethyl ether

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Melting and Boiling points:
In the previous slides we have seen the importance of
Mp and bp in the determination of the compound purities.
Now let us look at another importance of them in identifying
An organic compounds.

if you can be sure that the boiling point of a liquid alcohol


is 132° (+,-) 2°C, you have narrowed the choice to only
three or four possibilities from more than 40 liquid alcohols

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Where to Begin?
When you are asked to identify an unknown
organic sample the first thing to do is to check
the purity of the Sample.

(Normally we give you a pure sample), but if not


You need to make sure that the sample is pure
otherwise you learn nothing definitive from any
test carried out on an impure compound.

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How to check the purity of your sample?
The best techniques are:

1. Melting Point for solid sample.


2. Boiling Point for liquid sample
3. Thin layer chromatography TLC for both
liquid and solid samples.

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Melting Point
1. The melting point (mp) of a substance is one of the physical
properties that chemists use to identify a substance and/or to check
the purity of a substance.

2. The melting point is the temperature at which a substance changes


from a solid to a liquid state.

3. Pure crystalline organic compound usually has a sharp and


characteristic melting point range of 0.5 to 1°C.

4. The melting point range is determined by recording the temp at


which melting first begins and the temp at which melting is
complete. So, if your sample gave you sharp M.P. that means it’s a
pure sample.

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Link Penentuan Melting Point secara sederhana
https://youtu.bue/ggXHDZFsQBc
https://www.youtube.com/watch?v=nQNaTfqXECk
https://www.youtube.com/watch?v=ggXHDZFsQBc

Link Penentuan Melting Point dengan Alat yang lebih Modern


https://www.youtube.com/watch?v=WjCWk9HJlqQ

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Boiling Point

1. The boiling point of a compound is the temperature at


which it changes from a liquid to a gas.
2. B.P. is a physical property often used to identify
substances or to check the purity of the compound.
3. Boiling points are approximately related to their
molecular weight, the higher the molecular weight, the
higher the boiling point.
4. Like melting points, boiling points are characteristic
properties of pure materials.

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Penentuan Boiling Point Secara Sederhana

https://www.youtube.com/watch?v=QEvo0CJ3GP8
https://www.youtube.com/watch?v=8b5Ha-8QGhY
https://youtu.be/8b5Ha-8QGhY

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Bahan Kajian Sampai Dengan UTS
1. Sistematika Identifikasi Senyawa Organik
2. Identifikasi Senyawa Unknown  Uji pendahuluan, sifat fisik dan uji
kelarutan
3. Analisis elemen dalam senyawa organik secara kualitatif dan kuantitatif.
4. Identifikasi Senyawa Unknown  Penentuan berat molekul, Penentuan
rumus molekul
5. Korelasi struktur dan sifat fisik : titik lebur, titik beku dan titik didih
6. Korelasi struktur dan sifat fisik : indeks bias, spesifik gravity dan
putaran optik.
7. Penentuan metode kemurnian : kromatografi, titik lebur
distilasi
8. UTS

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Thin Layer Chromatography
Theory of chromatography uses the different polarities of the stationary
phase, mobile phase and the liquid mixture of different compound to be
separated.

The compounds that have the most similar polarity to the mobile phase
i.e. solvent or eluant will move the fastest and be closer to the solvent
line than the other types of molecules which have less similar polarity
to the solvent.

The compounds more attracted to the stationary phase i.e. thin layer
plate will also move more slowly. Thus, molecules can be separated
from each other based on their different polarities.

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TLC

Jar

solvent

Pure Impure
sample sample

07/09/2020
PERTEMUAN KE-3 ==> Senin, 7 September 2020

1. Identifikasi Senyawa Unknown  Uji pendahuluan, sifat fisik dan


uji kelarutan (TLC dan Kelarutan)
https://www.youtube.com/watch?v=qdmKGskCyh8

2. Analisis Elemen dalam senyawa organik secara


kualitatif dan kuantitatif.

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Solubility Test

Likes dissolve likes is our rule of thumb. It means that


Polar compounds dissolve in polar solvents and non polar
Compounds dissolve in non- polar solvents.

1. In general; low molecular weight organic compounds


containing polar functional groups are soluble in water,
and in polar solvents like MeOH, EtOH, etc
2. As the chain length increases, the solubility decreases.
3. For two isomeric structure, the one with the more
branched structure will be more soluble in a given
solvent.
4. A compound is soluble if it dissolves to the extent of
about 30 mg of solid or 1 drop pf liquid in 1 ml of solvent

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Solubility in 0.6 M (5%) NaHCO3
(Untuk membedakan Asam Organik dan Fenol)

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Solubility in 1.5 M (5%) HCl

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Solubility in Conc H2SO4 (96%)

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