EXPERIMENT REPORT GAS CHROMATOGRAPHY

By : Ulifatul Laili 103194035

Meyta Rosemala Dewi 103194057 Rizki Putri Wardani 103194080

INTERNATIONAL CHEMISTRY EDUCATION 2010

SURABAYA STATE UNIVERSITY MATHEMATICS AND SCIENCES FACULTY CHEMISTRY DEPARTMENT 2012
Experiment Result GAS CHROMATOGRAPHY

A. Title

: Gas Chromatography (GC)

B. Purpose

: To understand preparation of Gas Chromatography (GC) instrument To solve condensation problem in Gas

Chromatography (GC) : December 12th , 2012

instrument

C. Date of Experiment

D. Basic theory

Gas chromatography, the components of a Vaeporized sample are separated as a consequence of being partitioned between a mobi gaseous phase and a liquid or a solid stationary phase held in a column. In performing a gas chromatpgraphic separation, the sample is vaporized and;injected onto the head of a chromatographic column is brought about by the flow of an inert gaseous mobile phase. Tn contrast to most other type of chromatography, the mobile phase does not (interact with molecules of the analyte; its only function is to transport the analyte through the column. There are two types of gas chromatography: gas-liquid chromatography (GLC) and gas-solid chromatugraphv (GSC). OLC finds widespread use in all fields of science; its name is usually shortened to gas chromatography (GC).'In GLC the analyte is partitioned between a gaseous mobile phase and a liquid phase immobilized on the surface of an inert solid packing or on the walls of a capillary tubing. The concept of OLC was first suggested in 1941 by Martin and Synge, who were also responsible for the development of liquidliquid partitiun chromatography. More than a decade was to ellapse, however, before the value of GLC was demonstrated experimentally' and this technique began to be used as a routine laboratory tool. In 1955 the first commercial apparatus for GLC appeared on the market. Since that time, the growth in applications of this technique has been phenomenal. Currently, nearly a million gas chromatographs are in use throughout the world In the procedural GC instrument, there are 3 tubes in the instrumkent laboratory, oxygen, nitrogen and hydrogen.

Experiment Result GAS CHROMATOGRAPHY

Instrument of GC

The mobile-phase gas in GC is called the carrier gas and must be chemically inert. Helium is the most common mobile-phase gas used, although argon, nitrogen, and hydrogen are also used. These gases are available in pressurized tanks. Pressure regulators, gauges, and flow meters are required to control the flow rate of the gas. In addition, the carrier gas system often contains a molecular sieve to remove impurities and water. Flow rates are normally controlled by a two-stage pressure regulator at the gas cylinder and some sort of pressure regulator or flow regulator mounted in the chromatograph. Inlet pressures usually range from 10 to 50 psi (Ib fin. ') above room pressure, which lead to flow rates of 25 to 150 mL/min with packed columns and 1 to 25 mL/min for open tubular capillary columns. Generally, it is assumed that flow rates will be constant if the inlet pressure remains constant. Flow rates can be established by a rotometer at the column head. Gas chromatography - specifically gas-liquid chromatography - involves a sample being vapourised and injected onto the head of the chromatographic column. The sample is transported through the column by the flow of inert, gaseous mobile phase. The column itself contains a liquid stationary phase which is adsorbed onto the surface of an inert solid. Have a look at this schematic diagram of a gas chromatograph:

Experiment Result GAS CHROMATOGRAPHY

Instrumental components Carrier gas The carrier gas must be chemically inert. Commonly used gases include nitrogen, helium, argon, and carbon dioxide. The choice of carrier gas is often dependent upon the type of detector which is used. The carrier gas system also contains a molecular sieve to remove water and other impurities.

Sample injection port For optimum column efficiency, the sample should not be too large, and should be introduced onto the column as a "plug" of vapor - slow injection of large samples causes band broadening and loss of resolution. The most common injection method is where a micro syringe is used to inject sample through a rubber septum into a flash vaporizer port at the head of the column. The temperature of the sample port is usually about 50C higher than the boiling point of the least volatile component of the sample. For packed columns, sample size ranges from tenths of a micro liter up to 20 micro liters. Capillary columns, on the other hand, need much less sample, typically around 10-3 mL. For capillary GC, split/split less injection is used.

Experiment Result GAS CHROMATOGRAPHY

Have a look at this diagram of a split/split less injector :

The injector can be used in one of two modes; split or splitless. The injector contains a heated chamber containing a glass liner into which the sample is injected through the septum. The carrier gas enters the chamber and can leave by three routes (when the injector is in split mode). The sample vapourises to form a mixture of carrier gas, vapourised solvent and vapourised solutes. A proportion of this mixture passes onto the column, but most exits through the split outlet. The septum purge outlet prevents septum bleed components from entering the column.

Columns There are two general types of column, packed and capillary (also known as open tubular). Packed columns contain a finely divided, inert, solid support material (commonly based on diatomaceous earth) coated with liquid stationary phase. Most packed columns are 1.5 - 10m in length and have an internal diameter of 2 - 4mm. Capillary columns have an internal diameter of a few tenths of a millimeter. They can be one of two types; wall-coated open tubular (WCOT) or support-coated open tubular (SCOT). Wall-coated columns consist of a capillary tube whose walls are coated with liquid stationary phase. In support-coated columns, the inner wall of the capillary is lined with a thin layer of support material such as diatomaceous earth, onto which the stationary phase has

Experiment Result GAS CHROMATOGRAPHY

been adsorbed. SCOT columns are generally less efficient than WCOT columns. Both types of capillary column are more efficient than packed columns. In 1979, a new type of WCOT column was devised - the Fused Silica Open Tubular (FSOT) column :

These have much thinner walls than the glass capillary columns, and are given strength by the polyimide coating. These columns are flexible and can be wound into coils. They have the advantages of physical strength, flexibility and low reactivity.

Column temperature For precise work, column temperature must be controlled to within tenths of a degree. The optimum column temperature is dependant upon the boiling point of the sample. As a rule of thumb, a temperature slightly above the average boiling point of the sample results in an elution time of 2 - 30 minutes. Minimal temperatures give good resolution, but increase elution times. If a sample has a wide boiling range, then temperature programming can be useful. The column temperature is increased (either continuously or in steps) as separation proceeds.

Detectors There are many detectors which can be used in gas chromatography. Different detectors will give different types of selectivity. A non-selective detector responds to all compounds except the carrier gas, a selective detector responds to a range of compounds with a common physical or chemical property and a specific detector responds to a single chemical compound. Detectors can also be grouped into concentration dependant detectors and mass flow dependant detectors. The signal from a concentration dependant detector is related to the

Experiment Result GAS CHROMATOGRAPHY

concentration of solute in the detector, and does not usually destroy the sample Dilution of with make-up gas will lower the detectors response. Mass flow dependant detectors usually destroy the sample, and the signal is related to the rate at which solute molecules enter the detector. The response of a mass flow dependant detector is unaffected by make-up gas. Have a look at this tabular summary of common GC detectors: Detector Flame ionization (FID) Thermal conductivity (TCD) Electron capture (ECD) Nitrogenphosphorus Flame photometric (FPD) Photoionization (PID) Hall electrolytic conductivity Type Support gases Hydrogen and air Selectivity Detectability Dynamic range 107

Mass flow

Most organic cpds.

100 pg

Concentration Reference

Universal Halides, nitrates, nitriles, peroxides, anhydrides, organometallics Nitrogen, phosphorus Sulphur, phosphorus, tin, boron, arsenic, germanium, selenium, chromium

1 ng

107

Concentration Make-up Mass flow Hydrogen and air Hydrogen and air possibly oxygen

50 fg 10 pg

105 106

Mass flow

100 pg

103

Concentration Make-up

Aliphatics, aromatics, ketones, esters, aldehydes, amines, heterocyclics, 2 pg organosulphurs, some organometallics Halide, nitrogen, nitrosamine, sulphur

107

Mass flow

Hydrogen, oxygen

The effluent from the column is mixed with hydrogen and air, and ignited. Organic compounds burning in the flame produce ions and electrons which can conduct electricity through the flame. A large electrical potential is applied at the burner tip, and a collector electrode is located above the flame. The current resulting from the pyrolysis of any organic compounds is measured. FIDs are mass sensitive rather than concentration sensitive; this gives the advantage that changes in mobile phase flow rate do not affect the detector's

Experiment Result GAS CHROMATOGRAPHY

response. The FID is a useful general detector for the analysis of organic compounds; it has high sensitivity, a large linear response range, and low noise. It is also robust and easy to use, but unfortunately, it destroys the sample.

E. Tool and Materials Tools

Gas chromatography instrument is completed with N2 gas (Ultra High Pressure), O2 gas as compress air (High Pressure), H2 gas (Ultra High Pressure) ADC as connector between GC and computer Computer

Experiment Result GAS CHROMATOGRAPHY

F. Procedure -

Preparation of Gas chromatography instrument This observation only doing in preparation.

O2 gas N2 gas
is opened by using spanner is opened directly is opened by using spanner

H2 gas

Pressure of each gas in psi or bar

GC, ADC, and computer is turned on

PREPARATI ON AND CONDITIONI NG INSTRUMEN T

GC, ADC, and computer is ready

G. Data of experiment

Pressure of gases in Gas chromatography Gas N2 O2 as compress air H2 Pressure (bar) 100 120 110 Pressure (psi) 1500 1700 1550 Properties Ultra High Pressure (UHP) High Pressure (HP) Ultra High Pressure (UHP)

Experiment Result GAS CHROMATOGRAPHY

H. Analysis

This experiment has objective to understand preparation of Gas Chromatography (GC) only. In Firstly, we have to open gases that used for gas chromatography, there are N2 gas, O2 gas as compress air and H2 gas, all of the gas must be openned begin. N2 and H2 has UHP (Ultra High Pressure). For open that gases, we need different way for each gases. For N2 gas, we can open it directly. But for O2 gas and H2 gas we have to use spinner, spinner number 6 for O2 gas and number 8 for H2 gas. After we open the gases, we also record the gases pressure, it can be in psi or in bar unit. Its for knowing flowing of the gases. The steps are start from open gas N2 ,O2 and the last is H2. O2 should be opened before H2 gas to prevent flame exploded in GC instrument. After gas opened we should turn on instrument GC, ADC as a connector because we use instrument GC that old type and the computer as output data . After all of tools is turned on, we have to do conditioning to GC instrument before we can use it. Conditioning need a time around 1 hour. When conditioning, gas N2 should not turned off because it can broke GC column. There are occur several mistake when prepare GC instrument, this instrument is occur condensation. In this condition, instrument will be moist. The other indication shows that the instrument contain noise is too high in detector temperature. Normal temperature detector is 200 C. in this observation the tempeture is more than 200 C. Beside that, output of computer can also shows that our GC instrument is in unwell condition. The spectrum that in computer shown there are many pick that cery crowded, it means that the detector contain noise. So, it is positive if GC instrument is condensed and the detector in bad condition. To solve this problem, we make temperature of detector higher, it is about 250C to remove the noise. But it is doesnt work. So, we have to do destruction for the detector. Before we do destruction for the detector. We have to turn off all of the instrument first. Before to do it, it must be attention to switch off the instrument the N2 gas must be still, it for to protect the GC instrument not broken. Temperature of detector, injector and the oven must be down before, minimum 100C as a safety temperature when switch off instrument. After to do it, we can switch off the instrument. Then we can do destruction. The destruction is done by upper part of GC instrument. Next is releasing the detector in this instrument, rinse with methabol and drying with dry and

Experiment Result GAS CHROMATOGRAPHY

celan fabric. Before releasing the detector, must be attetntion that the detector must be cold, because in this part there is fire and the process of combustion.

The part that must be release

To minimalize this problem, we can do destruction from the beginning. So before swith on the instrument, we can take the detector and rinse with methanol then dry and clean with fabric. So we can make sure that the detector is clean and not wet. And we must do conditioning of instrument, so we can do efficient of time with well.

I. Conclusion -

Condensation problem in Gas Chromatography (GC) instrument can be solved by elevating the temperature of detector until reach 250C, and next do destruction of detector.

J. Reference Anonynomous. (online).

: http://en.wikipedia.org/Gas_chromatography. Access on

Tuesday, December 18, 2012 Anonynomous. (online). http://www.teaching.shu.ac.uk . Access on Tuesday, December 18, 2012 Monica, Maria SBW, dkk.2012.Panduan Praktikum Kimia Analitik III Spektroskopi dan Kromatografi.Surabaya: UNESA Unipress.

Experiment Result GAS CHROMATOGRAPHY

ATTACHEMNT Picture Explanation Gases used in Gas Chromatography (GC) Red : H2 Blue : O2 Yellow : N2 gas

Gas Chromatography Instrument

Experiment Result GAS CHROMATOGRAPHY

Signal of detector shown: 75, 9 It is lower than 100. It is mean that detector is dirty. It can be caused by condensation or other noise

This spectrum shows that the detector contain noise, if it is free from noise the spectrum is straight line.

Inside part of Gas Chromatography Instrument

Experiment Result GAS CHROMATOGRAPHY