CRITICAL BOOK REPORT

CRITICAL
BOOK REPORT

Separation
Chemistry

Bilingual
Chemistry
Education Study
Program

SCORE

Prepared to Fulfil The Duties of Separation Chemistry Course

Guided By :

Dr.Sri Adelila Sari,S.Pd.,M.Si

Made By :

Name : Auliya Rahman

Nim :4183131032

Class : Bilingual Chemistry 2018

Study Program : S-1 Bilingual Chemistry Education

MEDAN STATE UNIVERSITY

THE FACULTY OF MATHEMATICS AND SCIENE

CHEMICAL EDUCATION STUDY PROGRAM

SEPTEMBER 2020
 FOREWORD

Praise to the presence of Allah SWT who has provided favors that do not count,
including health favors and opportunities so that as a writer I can complete the KKNI
assignment in the form of Critical Book Report, on this occasion the author carries the title
“Gas Chromatography” .

I also say thank you to the lecturer in Separation Chemistry course, Dr.Sri Adelila
Sari,S.Pd.,M.Si. who has provided guidance to me so that the completion of this Critical
Book Report task,then I would also like to thank those who supported the author in
completing this Critical Book Report task.The author is aware that in writing this Critical
Book Report paper is far from perfect, for that the writer psti accepts any constructive
criticism in the future improvement.

Finally, I would like to thank all of my readers of this Critical Book Report
assignment, I hope that with this Critical Book Report assignment I can benefit and can also
provide insight into the content of my Critical Book Report assignments.

Panyabungan, 24rd September

2020

Auliya Rahman

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 TABLE OF CONTENTS

FOREWORD............................................................................................................i

TABLE OF CONTENTS.........................................................................................ii

CHAPTER I : INTRODUCTION..........................................................................1

1.A.Background.........................................................................................................1

1.B.The Formula of the Problems..............................................................................1

1.C.Purposes...............................................................................................................1

1.D.Benefit.................................................................................................................1

CHAPTER II : SUMMARY OF THE BOOK......................................................2

2.A.Book Identity.......................................................................................................2

2.B.Summary of the Book I.......................................................................................3

2.C.Summary of the Book II......................................................................................12

CHAPTER III : ADVANTAGES AND DISADVANTAGES..............................17

3.A.Advantages and Diadvantages of Book I............................................................17

3.B.Advantages and Diadvantages of Book II...........................................................17

CHAPTER IV : CLOSING.....................................................................................18

4.A.Conclusion ..........................................................................................................18

REFFERENCES......................................................................................................19

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 CHAPTER I

INTRODUCTION

1.A.Background

The background of the writing of this critcal book report is to make it easier for
students to find the right book to become a reference in studying gas chromatography. The
things that need to be criticized are the contents of the book, such as the completeness of the
material, the systematics of writing, and the ease of understanding the contents of the
material.

Gas chromatography (GC) is a type of chromatography that is commonly used in

chemical analysis for the separation and analysis of compounds that can vaporize without
undergoing decomposition. Common uses of GC include testing the purity of a particular
compound, or separating the different components in a mixture (relative levels of the
component can also be determined). In some circumstances, GC can help identify
compounds. In preparative chromatography, GC can be used to prepare pure compounds
from a mixture..In gas chromatography, 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 layer of
microscopic liquid or polymer on top of the solid support for the stationary phase, which is in
a glass or metal tube called a column. The instrument used to perform gas chromatography is
called a gas chromatograph (or "aerograph" or "gas separator").

1.B.The Formula of the Problem

 What is the systematics of writing the material in the two books?

 How is the completeness material content of the two books?
 How is the choice of words used by the two books in explaining the content of the
material?

1.C.Purpose

 To know the systematics of writing the material in the two books

 To know the completeness material content of the two books
 To know the choice of words used by the two books in explaining the content of the
material

1.D.Benefit

By completing the critical book report assignment, students can develop critical
thinking skills in criticizing the contents of the two books in a particular chapter. Students can
also compare the contents of the two books based on the completeness of the content of the
material, give suggestions and give accurate conclusions about the results of the comparison
of the two books.

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 CHAPTER II

SUMMARY

2.A.Book Identity

2.A.1 Book Identity I

Book Title : Chromatography Basic Principles,

Sample Preparations and Related
Methods

Writer : Elsa Lundanes, Léon Reubsaet and

Tyge Greibrokk

Publisher : WILEY-VCH

Publication Year : 2014

Place of Publication : Oslo Norway

ISBN : 978-3-527-67520-3

2.A.2 Book Identity II

Book Title :Chromatography 6th edition

fundamentals and applicationsof
chromatography and related
differential migration methods

Writer : Francesca Antonucci, Yoshinobu

Baba, and Maciej J. Bogusz

Publisher : Elsevier

Publication Year : 2004

Place of Publication : Amsterdam The Netherlands

ISBN : 0-444-51108-3

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2.B.Summary of the Book I

2.B.1.Introduction

In gas chromatography (GC), the mobile phase is a gas and the analytes need to have
suf ficient volatility to be carried through the column. In addition, the analytes need to be
stable at the temperatures exposed to in the injector and/or in the column. Analytes that are
not volatile, for example, fatty acids, can be made volatile by derivatization, for example, the
fatty acids can be converted to esters.

In GC, separation o ccurs m ainly according to two p rinciples: adsorption and p ar

tition chromatography. In adsorption c hromatog raph y, separation is obtained wh en the
analytes have differ ent adsorptivity to a sol id stationary phase. Gas adsorption c hroma-
tography, also c alled g as–solid chrom atography (GSC), is m ainly u sed f or separation of
permanent g ases. In p ar tition chromatography, a lso c alled gas–liquid chr omatography (G
LC), th e s t a tio n ary p hase is a n on vol a tile liqu id and separation is o bt ained if t he
analytes have diff eren t d istribut ion between the mobile and the stationary p hases. In GC,
the separation takes place in a column that is located in a heated compart-ment (column
oven), providing temperature control of the separation (Figure 2.1).

The mobile phase (the carrier gas) is delivered from a pressurized gas container (gas
flask). In order to provide a suitable gas flow to the column, a reduction valve is attached to
the gas flask. The sample to be analyzed is introduced into the column through the injection
system, which is temperature controlled. The detector that is located at the column outlet is
also temperature controlled. The detector is connected to a data system that is used for both
data handling and instrument control. The instrumentation used for GC is called a gas
chromatograph.

2.B.2.Mobile Phase/Carrier Gas

The mobile phase must be an inert gas, reacting with neither the stationary phase nor
the sample components. The gas that is used must be of high purity, and, if necessary, can be
purifi ed to remove traces of oxygen, water, and hydrocarbons.

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 Adsorbent tubes containing charcoal and molecular sieves are used to remove low
molecular mass hydrocarbons and water, respectively. Water may degrade some stationary
phases and both water and hydrocarbons may give detector problems. A tube containing a
catalyst is used to remove oxygen, which may degrade some stationary phases and give
unstable baseline with the electron capture detector (ECD).

The gas should be easily available and inexpensive, provide high safety at use, and
give good detector response for the analytes. The most common carrier gases are helium,
hydrogen, and nitrogen. A comparison of the conventional gases is given in Table 2.1.

While choosing the most appropriate carrier gas, all factors listed in Table 2.1 need to
be taken into consideration. When packed columns of large inner diameter (ID) are used and
hence large volumetric flow of gas is required, N2 is chosen because of its lower price.
However, when analysis time and chromatographic efficiency are more important, H2 or He
is chosen due to its beneficial plate number versus gas flow relation. In Figure 2.2, the plate
height as a function of linear gas flow (centimeter per second) is shown for the gases. This
figure shows that the marginally best efficiency (lowest plate height) can be obtained for N 2,
although at a low flow rate and thus resulting in very long analysis time. H 2 provides the best
efficiency at higher flow rates (low analysis time), although the reactivity of H2 requires some
safety precautions. Hence, despite being the most expensive, He is often the preferred carrier
gas in GC as it provides good efficiency even at rather high flow rates. Due to the limited
availability of helium, hydrogen may, however, soon become the most common carrier gas in
GC. With a l in ea r flow rate of 50 cm s -1 , the volumetric flow rate in a 250 m m ID column
will be about 1.5 ml min-1 and the tM will be about 50 s in a 25 m long column.

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 For the chromatographic separation, a constant gas flow rate is required. For
isothermal separations (i.e., constant temperature throughout the separation), a constant flow
rate can be obtained by constant column inlet pressure. The pressure of carrier gas from the
gas flask is reduced by the reduction valve (with pressure meters) attached to the gas flask; in
addition, pressure control is provided at the gas chromatograph.

For temperature gradient separations, where the temperature is increased throughout

the separation time, a flow rate controller is needed. Modern gas chromatographs are
equipped with fl ow (and pressure) control units.

2.B.3.Injection Systems

Different sample introduction methods can be used in GC. If the sample is a liquid or
a solid dissolved in an appropriate solvent, it may be introduced by a syringe into the injector.
The choice of injection system depends on the column type and the sample composition. In
packed columns, the sample is injected directly into the column inlet (Figure 2.3). In smaller
inner diameter columns, split injection, splitless injection, and on-column injection
techniques are used for liquid samples. The injections can be carried out manually by a
handheld syringe or mechanically by an autoinjector, which is now standard for GC
instrumentation.

Packed Column Injector (Evaporation Injector)

The inlet of the column or a glass tube (liner) located just in front of the column is
placed in a heated metal block, which has a separate temperature control. The temperature of
the injection part is usually kept higher than the column tempera-ture, and high enough to
allow rapid evaporation of the sample, both solvent and sample components, when the
sample is introduced. About 2 –10 m l of sample is transferred from the injection syringe,
which is equipped with a thin needle having a sharp beveled tip, to the column inlet through

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the septum, which is made of a synthetic rubber (silicone) (Figure 2.3). When the liquid
evaporates, it occupies a gas volume that is about 1000 times larger than the liquid volume.
The septum is kept in place by the metal septum holder and when the syringe needle is
withdrawn, the elasticity of the septum closes the puncture hole made by the needle, keeping
the septum gas tight. However, after a number of injections, a permanent hole in the septum
is formed and the septum needs to be replaced. The injection temperature de fi nes the choice
of septum material.

As shown in Figure 2.3, the carrier gas is heated to the same temperature as the
column inlet. As a rule of thumb, the injection temperature should be 50 0C above the boiling
point (Bp) when the Bp is known, or 50 0 C above the column temperature when the Bp is
unknown.

The purpose of this injection technique is to introduce the entire injected sample into
the column and use it for trace determination. Different techniques can be used, but the most
common is the solvent effect technique, which uses the same instrumenta-tion as used for
split injection (Figure 2.4). In splitless injection, the sample is introduced into the heated liner
as in split injection and brought into the gas phase. Contrary to the split injection, the splitter
outlet valve is now closed. Hence, the total sample volume (1–2 ml of gas) is transferred to
the column. When splitless injection is carried out, the column inlet temperature is kept at a
temperature that is 20–50 0C lower than the solvent Bp. Hence, when the sample arrives at
the column inlet, the solvent condenses as a thick film on the column wall. This film will act
as a plug of stationary phase into which the sample components will be dissolved. Following
the sample transfer to the column, which will take 2 min when 2 ml i s i njected and the car
rier gas flow rate is 1 ml min-1, the column oven temperature is increased.

On-Column Injection

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 This technique is more dif ficult to perform and is carried out only when the analytes
are temperature labile. The liquid sample is introduced at room temperature by a syringe
through a valve directly into the column entrance, or more commonly through a retention
gap, when the gas fl ow through the column is stopped.

Large-Volume Injectors

Larger volumes of samples can be introduced to the column using programmed

temperature vaporizing (PTV) injector. The PTV injector resembles the split/ splitless
injector, but the vaporization chamber (liner) can be heated and cooled rapidly. This is
obtained using a liner with low thermal mass. The sample is introduced at a low initial
temperature, eliminating the problem of discrimination and thermal degradation associated
with the conventional split/splitless injection.

Headspace Techniques

The static and dynamic headspace techniques are the most common techniques for
determination of volatile analytes from aqueous samples. In the latter, also called purge-and-
trap , a gas is passed over the sample or through the sample as small bubbles and the volatile
compounds in the sample are transported by the gas to a cryogenic or a sorbent trap, before
subsequent GC separation. In the more common static headspace technique, the sample vial is
thermostated (Figure 2.5) until equilibrium is established. Pressure is applied with an inert
gas to ensure that the pressure and the volume of the headspace sampled are same for all
samples and standards. After pressurization, a valve is opened to allow a quick transfer of the
headspace volume (0.5– 3.0 ml of gas) to a trap column (sampling). The trapped sample is
subsequently transferred to the separation column by either splitting or cryogenic trapping.
Internal standards are a necessity with headspace techniques.

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 2.B.4.Columns

GC separations can be carried out on packed or open tubular columns (OTCs). The
column is connected directly with the injector and the detector by nuts and ferrules. Typical
column dimensions are given in Table 2.2.

2.B.5.Detectors

The outlet of the column is directly connected to the detector in the gas
chromatograph. The detector must be heated to avoid condensation of components eluted
from the column, and generally the detector temperature is kept at least 200C above the
highest column temperature. A large variety of GC detectors exist, both selective and more
universal detectors. Only a few, but the most used, detectors are described in some detail in
this book.

Detectors can be classi fi ed as mass- or concentration-sensitive detectors. The

chromatographic peak area using a mass-sensitive detector is independent of the flow rate
used, while the peak area using a concentration-sensitive detector depends on the flow rate.
Hence, for quantitative determinations, good fl ow control is needed with the concentration-
sensitive detectors.

Thermal Conductivity Detector

The thermal conductivity detector (TCD) consists of a heated metal block with two
channels. Each channel is equipped with a fi lament (metal wire) (see Figure 2.7), and the
filaments are connected to a Wheatstone bridge. The carrier gas going into the
injector/column is led through one of the channels, while the carrier gas from the column is
led through the other channel. The filament temperature depends on the heat conductivity of
the gas passing. Both He and H2 have rather large conductivity, while N2 has less. When a
compound eluted from the column passes the filament, the conductivity of the gas is
decreased and the fi lament temperature increases. This increase in temperature results in a
change in the electrical resistance of the filament, and this change is registered by the
Wheatstone bridge system and a change in detector signal is observed.

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Mass Spectrometry

The mass spectrometer (Section 3.6.2) has become a very important detector in gas
chromatography. The mass spectrometry (MS) instrument basically consists of an ionization
unit (ion source), a mass/charge (m / z ) separation unit (analyzer), and an ion detector. The
MS is a mass-sensitive detector, where the signal ( S ) depends on the concentration (C), the
mobile phase flow rate (F), and the split ratio in the chromatographic system (R ).

Positive Ionization

In gas chromatography, the most common ionization technique is electron ionization

(EI). Electrons formed in a filament are sent as an electron beam with energy 70 Ev through
the relatively open ion source. The molecules (analytes) that are in gas phase at low pressures
are ionized, and positive monoisotopic molecular ions (M+ ) are formed.

Negative Ionization

Negative ions can be formed at conditions used for chemical ionization, that is, when
using an ion source that is relatively closed and with a reagent gas (or moderating gas) of
high pressure. A moderating gas does not provide negative ions, but due to its presence
generate electrons of low energy (thermal electrons) by slowing down 200– 500 eV electrons
coming from a filament. Thermal electrons can be captured by the analyte and a negative ion
is formed. When reagent gases are used, the formation of negative ions is due to ion–
molecule reactions between the analyte and the negative ions from the reagent gas. The
combination of negative ionization and chromatogra-phy has so far not been widely used.
Negative MS is, however, especially useful for molecules with high electron affinity as in the
case of the EC detector.

Temperature

The column temperature controls the retention of compounds in the column. Equation
2.4 shows the dependence of retention on p, which is the compound saturation pressure at the
column temperature T. The column temperature should be as high as possible to provide short
analysis time and still maintaining separation of the components. Isothermal separation , that
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is, constant temperature throughout the separation, is most suited for separations of
components having similar boiling points. Temperature programming , where the temperature
is increased during the separa-tion, is used for separation of complex samples wherein the
components have large variations in Bp (Figure 2.16). Temperature-programmed separations
are common in capillary GC, where long columns can provide high ef fi ciency required for
high-resolution separations. For trace determinations, where splitless injection is required,
temperature programming must be used.

2.B.6 Two-Dimensional Separations

When a sample is very complex, containing several hundreds or thousands of

compounds, a single column is not suffi cient to provide separation of all com-pounds, even
when a long column with long gradient time is used, because of limited peak capacity. A
better separation can be achieved by subjecting the sample separated by the ( fi rst) GC
column to an additional separation in a second column, which provides separation based on a
different mechanism. When two columns are used in this way, the separation is called two
dimensional (2D) and is described as GC GC. The best resolution is obtained when the
separation mechanism in the two columns is completely different, and this is called
orthogonal separation. The total theoretical peak capacity of the method is the product of the
peak capacities of each dimension. The instrumentation used is shown in Figure 2.17. Two-
dimensional separations can be performed in different ways. In a compre-hensive analysis,

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the eluate from the fi rst column is transferred to the second column in such a way that three
fractions from each first dimension peak is injected and separated by the second dimension
column one by one. This requires that the time for the second separation is very fast and
equal to or smaller than the first dimension fractionation time.

2.B.7.Qualitative and Quantitative Analyses

GC has a very wide fi eld of applications. The main areas of use are analyses of
complex mixtures such as essential oils and petroleum oils (Figure 2.16). Other important
areas are trace determinations in pollution and forensics. Depending on the need, GC can be
used for both qualitative and quantitative determinations.

In qualitative determinations , compounds can be identi fied by comparing their

retention time tR with those of standards using at least two different stationary phases.
However, the most used technique for qualitative determination to date is the combination of
gas chromatography and mass spectrometry.

Quantitative determinations by GC are always carried out using internal standard(s)

(IS), since it is almost impossible to make repeatable injections. If MS is used for detection, a
labeled IS, for example, deuterated, can be used. Otherwise, a similar compound, which is
chromatographically separated from the analytes, is used.

In general, GC analyses are fast, provide the highest ef fi ciency per time unit, and
give good resolution and low limits of detection (LOD). These are the reasons for GC being
preferred in many areas.

2.B.8.Derivatization

Nonvolatile compounds, which cannot be chromatographed by GC, can be made

volatile by derivatization. Typically, compounds containing polar functional groups like
-COOH, -OH , a nd -NH2 are nonvolatile, and thermally stable derivatives with nonpolar

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groups are made by different derivatization reactions. In some cases, the detectability of the
resulting derivatives can be improved compared to the original compounds. This is especially
utilized for electron capture detection, where the analytes are derivatized with electron
capture responsive reagents.

The fluorinated derivatives have better chromatographic properties and higher

volatility than chlorine and bromine derivatives, which have longer retention time and may
have less stability. Even though mono- and dichlorinated derivatives often give better ECD
response than the fluorinated derivatives, the latter are mostly used. By using a reagent, which
results in a higher number of fl uorine, a derivative with good detectability and with little
addition to retention time is obtained. Hepta fl uor-obutyric anhydride is a reagent giving a
derivative that is a good compromise between volatility and ECD response. Most polar
groups with a replaceable hydrogen atom can be acylated; however, acids cannot be acylated.
Alkylation describes the reaction where an active hydrogen is replaced with an alkyl group,
for example, a methyl group. Most polar groups can be alkylated, and many reagents can be
used, for example, alkyl halogenides, diazo alkanes, and N, N0 -dimethylformamide dialkyl
acetal. An example of an alkylation is the formation of methyl esters of fatty acids by using
methanolic BF3 , where boron tri fl uoride (BF3 ) acts as a catalyst.

2.C. Summary of the Book II

2.C.1.Introduction

Gas chromatography coupled to highly selective detection systems, based on atomic

(or molecular) spectrometry or mass spectrometry, provides very sensitive methods of
quantitation, even for elements that are difficult to determine, such as H, C, O, Cl, Br, I, S, P,
B, and Si. The advantages of these techniques are the provision of element-selective data plus
time-based monitoring that allows speciation studies . Guidelines for the definition of
concepts related to speciation of elements and, more particularly, speciation analysis of
chemical compounds have been provided .

Sanz-Medel and Lobinski agree that speciation is a complex and challenging

problem but differ in their assessment of the state of maturity of the field. “An analysis of
speciation-relevant issues leads to the conclusion that, despite the rapidly increasing number
of reports, the field has reached a level of virtual stagnation in terms of research originality
and market perspectives. A breakthrough is in sight but requires an advanced
interdisciplinary collaboration of chemical-analysts with clinicians, ecotoxicologists, and
nutritionists” . Sanz-Medel observes that the current state of real-life analytical speciation
involves use of hybrid techniques, combining an adequate separation technique for physical
species separation with element-specific detectors, such as those based on atomic
spectrometry. The present demand is for “innovative chemical speciation strategies and
analytical technologies.” Sanz-Medel also noted the urgent plea for quality assurance in non-
routine analysis.

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 An early review of coupled element-selective techniques by Ebdon et al. covered the
period to 1985 and contains information that remains relevant. Several more recent reviews
emphasize various aspects of element-selective detection and speciation.

The majority of applications of combination techniques deal with either organic

compounds containing P, S, Si, B, or halogens or with organometallic compounds of Hg, As,
Se, Pb, and Sn. For the latter group, speciation and analyses of a broad range of sample types,
including biological and environmental materials, air, water, fuels, and standard reference
materials, have been carried out. Volatile compounds can be determined directly, following
extraction, clean-up, and pre-concentration. Analysis by these techniques is particularly
suitable for complex, volatile mixtures, e.g., pyrolyzates or synthetic fuels originating from
coal or shale oil, containing compounds of S, P, Se, As, and Si. Nonvolatile species can be
converted to volatile alkyl, silyl, or hydride derivatives prior to analysis. Alternatively, such
samples (e.g., oil shales for the determination of geopophyrins) can be analyzed by
combination with HPLC or SFC . Purely inorganic compounds or metal chelates have been
studied to a much lesser degree. Indeed, where total-element determinations are required,
there may be no advantage in GC separation, as determinations can be effected
spectroscopically. Thus, speciation of tin in poisoned human organs was measured by
GC/AES (flame photometry) while major trace metal elements in the same sample were
measured directly by ICP-MS.

2.C.2. Elemental analysis

Elemental analysis for carbon, hydrogen, nitrogen, etc., by reaction GC is of interest

to inorganic as well as organic chemists . Elemental composition obtained by GC/AES
provides empirical formulas with errors of a few percent, if the calibrating reference
substance is closely related – by structure, elemental composition, molecular weight, and
amount – to the compounds to be identified. Selectivity and sensitivity are improved by
using the cyanogen molecular band at 388 nm instead of the 174 nmatomic emission line.
However, response factors depend on the concentration of elements, and this affects the
accuracy of the determination of empirical formulas. PFPD has brought within reach the
possibility of universal heteroatom-selective detection and, hence, empirical formula
determination. The system exploits the dependence of the flame-chemiluminescence emission
time.

2.C.3.Binary compounds

The main groups to be considered here comprise monomeric hydrides and halides
sufficiently volatile to be determined by conventional GC or by thermochromatography. The
gaseous species, CH4, CO, CO2,NH3, and SO2 are not discussed.

GC is a very selective and sensitive method for the determination of water, as

previously described . Such methods involve either direct measurement, usually based on
chromatographic separation on porous polymers or open-tubular columns with thermal-
conductivity detection, or indirect measurement by reaction GC. In the latter, water is
converted to hydrogen, methane, acetylene, or other organic compounds with the advantage

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that more sensitive detectors, such as the FID can be used. The most widely favored indirect
method requires the conversion of water to acetylene according to Eqn.

2.C.4.Co-ordination compounds

The GC of co-ordination complexes encompasses trace determinations of metals,

physicochemical measurements, the study of on-column reactions, the separation of isomers,
and the utilization of complexes as components of the stationary phase for enhancing
selectivity.

The b-diketones and their analogs (Fig. 13.1) comprise the largest and most
extensively studied GC reagents for metal ions. The parent b-diketones are broad-spectrum
reagents, forming complexes with nearly all metallic ions . Unfortunately, methods for trace
determinations based on these reagents are limited essentially to the ions in Table 13.1.

Other ligand analogs of the b-diketones, such as those represented by Structures II –

IV and VII, are more selective and have been applied only to the trace determination of Ni(II)
. Tetradentate ligands of the type represented in Structure V, due to the greater stability of the
complexes, have been more successful . Trace determinations with fluorinated reagents of
this type have been developed for Cu(II), Ni(II), Co(II), Pd(II), and V(IV)O. The ligand
bis(acetylpivalylmethane)ethylenediimine has been used for the determination of vanadium
in rock samples. The vanadium was complexed with ligand, extracted, and separated on a
capillary column from free ligand, Cu(II), Ni(II), Pd(II), and Pt(II) chelates. However, high
concentrations of Fe(II) suppressed the oxovanadium(IV) response.

2.C.5.Anions

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 The determination of inorganic anions by GC can be considered to be complementary
to that by ion chromatography and conventional HPLC. The basic requirement for anion
determination by GC is the facile conversion of an anion to a neutral, volatile derivative,
which is usually produced by the formation of a relatively stable covalent bond. Typically,
the latter is selected to have favorable detection properties as well. In the simplest case,
anions of weak acids are converted by acidification to the corresponding conjugate acids or
acid anhydrides, and the gaseous products (e.g.,CO2,H2S, HCN, and SO2) are determined. A
more general procedure involves nucleophilic displacement, where the analyte anion (A -)
displaces a ready leaving group, L- , from the neutral reagent, RL (Eqn. 13.2), to give the
derivative AR.

2.C.6.Organometallics

Organometallics studied to date by GC include various alkyl, aryl, vinyl, and silyl
compounds of Be and the III A, IV A, V A, II B element groups, Si compounds (silanes,
chloroalkyl and chloroaryl silanes, silatranes), carbonyl, arylcarbonyl, and trifluoropho-
sphinocarbonyl complexes of transition metals, and metallocenes and their substituted
derivatives. The GC separation of organometallics is usually not problematic, but difficulties
may arise due to limited stability with respect to one or more of thermolysis, hydrolysis,
oxidative or photo-oxidative decomposition, and catalytic decomposition. For the less stable
compounds, great care in all aspects of their GC, including sampling, transfer, injection,
column selection, and deactivation is required. Solvents should be de-aerated, nonreactive
toward the solute, and free of reactive impurities, such as peroxides. Where organometallics
are involatile or highly reactive, derivatization by alkylation, silylation, hydridization, co-
ordination, or other reactions can be utilized. Novel reagents that extend the application of
such derivatizations continue to be reported.

The organometallics as a class have progressed from the status of “laboratory

curiosities” to important industrial chemicals. An increasing number, mainly certain
compounds of Pb, Hg, Sn, As, and Sb can now be determined at low concentrations in natural
waters and sediments. Research into biomethylation has also led to the realization that some
organometallics, e.g., those of Pb, Hg, As, Sn, Se, Tl, and Sb, can originate from biochemical
conversions of inorganic substrates. The speciation and determination of organometallics is
usually carried out by GC after selective extraction, derivatization, and pre-concentration.
The selectivity of SPME is being exploited in an increasing number of applications and may
be combined with the derivatization step to eliminate the need for extraction with organic
solvents. Derivatization may be important, since a variety of species of a particular element
can be determinedsimultaneously . Usually, the species of interest represent various stages of
alkylation or dealkylation of the original organometallic compounds due to weathering or
biological transformation. The simultaneous determination of such species is of value in
environ-mental studies. Surprisingly, many environmental organometallics of Pb, Hg, and Sn
can be determined at ng- to pg-levels without problems of decomposition, irreversible
adsorption, or alkyl-group exchange, a fact that reflects the relatively high stability of these
species.

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 CHAPTER III

ADVANTAGES AND DISADVANTAGES

3.A.Advantages and Disadvantages Book I

3.A.1.Advantages

 This book is written in a structured and systematic manner because it always starts
with an introduction which is then continued with a discussion of the next material.
 This book uses easy to understand words so that the information conveyed by the
book is easily understood by the reader.
 This book contains quite a lot of pictures such as drawing tools, tables, and graphs of
observations.
 This book explains the material quite clearly and completely because this book
describes the tools and their uses as well as other gas chromatography materials.

3.A.2.Disadvantages

 This book does not explain specifically about elemental analysis, binary compound,
coordination compound, and organometalic.

3.B.Advantages and Disadvantages Book II

3.B.1.Advantages

 This book is written in a structured and systematic manner because it always starts
with an introduction which is then continued with a discussion of the next material.
 This book uses easy to understand words so that the information conveyed by the
book is easily understood by the reader.

3.B.2.Disadvantages

 This book does not explain the tool or how to use it in the gas chromatography
method.
 This book displays very few pictures, tables or graphics to support the explanation of
the material.
 This book does not specifically explain Qualitative and Quantitative Analyzes,
Derivatization.

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 CHAPTER IV

CLOSING

4.A.Conclusion

Based on the results of the criticism in the previous chapter, we can see that the two
books both have strengths and weaknesses. However, the first book has more advantages
than the second book such as this book is written in a structured and systematic manner
because it always starts with an introduction which is then continued with a discussion of
the next material,this book uses easy to understand words so that the information
conveyed by the book is easily understood by the reader,this book contains quite a lot of
pictures such as drawing tools, tables, and graphs of observations,this book explains the
material quite clearly and completely because this book describes the tools and their uses
as well as other gas chromatography materials.The first book has fewer weaknesses than
the first book. Secondly, we can conclude that the first book is preferable to be a
reference book in studying gas chromatography.

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 REFERENCES

Antonucci, Francesca., Baba, Yoshinobu., Bogusz, Maciej J.(2004). Chromatography

6th edition fundamentalsand applicationsof chromatography and related
differential migration methods. Elsevier : Amsterdam The Netherlands.

Lundanes, Elsa., Reubsaet, Léon., Greibrokk, Tyge.(2014). Chromatography Basic

Principles, Sample Preparations and Related Methods.WILEY-VCH : Oslo
Norway.

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