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ANALYSIS OF SAMPLES ABSORBANCES USING ULTRAVIOLET-VISIBLE (UV-VIS) SPECTROSCOPY

BY:

I PUTU RAIWATA MERTANJAYA

(0813031019)

CHEMISTRY EDUCATION DEPARTMENT FACULTY OF MATHEMATICS AND SCIENCES GANESHA UNIVERSITY OF EDUCATION SINGARAJA 2011

ANALYSIS OF SAMPLES ABSORBANCES USING ULTRAVIOLET-VISIBLE (UV-VIS) SPECTROSCOPY

I.

Experiment Objective 1. Determine the copper content in the metal ore. 2. Determine the absorbance of Ethyl-p-methoxycinnamate (EPMS). 3. Determine the absorbance of natural indicator in acidic and basic solutions.

II. Theory Many modern technologies depend on the metal. Therefore, it has become imperative for a chemist to analyze metal ore to determine its content and develop a method for the determination of metals that have commercial value. One of the important metal in technological and economic value is copper. Copper is widely used for conductors, water pipes, and a mixture of various other metals, known as the alliance (such as brass, bronze, and silver coins). Spectrophotometry is widely used in laboratory analysis. Most laboratories that require identification and determination of organic compounds and inorganic compounds (eg pharmaceuticals, fertilizer, mining, etc.) using a spectrophotometer. In this trial will be determined percentage of the mass of copper in copper ore using spectroscopic techniques. Spectroscopy is the study of interaction of light (electromagnetic radiation) with matter (atoms and molecules). If certain wavelengths of light by an adsorbed atom or molecule, then the resulting absorption spectrum. Electronic structure of a species or a critical molecule absorption of light by species or molecule. The color complex compounds depends on the metal involved and the number of d orbitals has, associated with the oxidation state. However, there are several compounds of transition group has no d orbitals but the compounds are colored. The color is caused by electronic transitions involving the valence electrons in the other. Physicochemical analysis method based on spectral data is known as spectrometry. Several spectrophotometric methods is very important is ultraviolet (UV), infrared (IR), nuclear magnetic resonance (NMR), and mass. Ultraviolet and visible spectrophotometry can provide information about the chromophore group, which covalently unsaturated group contained in the molecule. The main components of spectrophotometer tool shown in the following scheme.

Beam Source

Monochromator

Sample

Detector

Screen Here are the types of UV-Vis:

(c) Double beam (DB)-in-time Absorption of light by molecules in the ultraviolet and visible spectral regions depend on the electronic structure of molecules. Absorption of this energy is quantized, namely the elevation of the orbital electrons in the ground state (ground state) to the orbital with higher energy (excited state = excited state), causing changes in the electronic energy of molecules,

namely the transition of valence electrons in the molecule. Various electronic energy levels or electronic transition can be summarized as follows:

Figure 1. Electronic Energy Levels Transition of n * requires less energy than a transition * or * . Transition of n * (R band) of a single chromophore groups (such as carbonyl or nitro), the characteristic bands ( maks <100, 250, -350 nm). Transition of * (K band) for molecules with conjugated systems (such as butadiene, mesitil oxide, and aromatic molecules with substitutions:-styrene, benzaldehid, or asetofenon), the characteristic bands ( maks <104; 200-400 nm wavelength). Transition of

* (B band). Benzenoid is characteristic of aromatic

molecules or heteroaromatik, the characteristic bands at ( maks 102 - <5000; 230270nm). Transition of * (band E). Etilenic is typical for aromatic structure with substitution auksochrom, tape characteristics on ( maks > 104; 180-200nm). In analyzing the use of UV-Vis spektrofotrometer should note the following: a. Formation of colored compounds This step is conducted if the analyzed compounds not absorbing visible region. In this case the compound must be converted into other compounds that can do the absorption or reacted with reagent so as to absorb visible light. b. Selection of wavelength Wavelengths required in a quantitative analysis by spectrophotometry is the wavelength corresponding to maximum absorbance (peak absorption). This is

caused by changes in absorbance for each unit of concentration is greatest at the maximum wavelength, it will obtain the maximum sensitivity as well. c. Preparation of calibration curve For calibration curves, created a standard solution with various concentrations of the unknown. Absorbance of standard solution is measured, then plots the absorbance (A) against concentration (C), the curve formed is called the calibration curve.

Ultraviolet and visible spectra is a picture of the position and intensity of absorption. The position of absorption related to the radiation wavelength ( ), where the energy is equal to the energy required for electronic transitions, while the absorption intensity (transmittance or absorbance) depends on two factors: the ability of interaction between radiation energy and electronic systems, as well as differences between ground state state and excited state. The intensity of absorption quantitatively expressed as Lambert-Beer equation: A = b c = - log T = - log
I bC I0

I I = log 0 I I0

- log

Where, A is the absorbance. T is transmittance. I is the intensity of light emitted by the solution in the cell. I0 is the intensity of light emitted by the solvent in the cell at I the same. Log is logarithm to base 10.
is the coefficient of extinction of the absorbing species or constant comparison (cm-1

M-1). b is the length through which the light solution (typically 1 cm). C is the concentration of absorbing species in units of mol L -1 (M). Lambert-Beer law states the relationship between the intensity of light absorbed by the concentration and the thick solution through which the beam. If a beam of light with a certain length is passed in a solution containing absorbent material, where some rays will be absorbed and transmitted light sbagian. Simply put, Lambert-Beer law can be shown in the following scheme.

Beam source

P0

Sample
b

Figure 2. Light absorption by the solution with a concentration of C Intensity of light or radiation with P0 that passes through a medium-thick b containing a solution with concentration C, will result in reduced intensity of P so that P < P0. The relationship between transmission, heavy trailers and can be stated as follows:
Log

P0 kbC A P

Where P0 and P is the initial light intensity / beam fell and the light transmitted. A is the absorbance, b for kuvet thickness, C for concentration, and k is a constant which depends on the concentration used. If C in g / L, constant called absorptivity (a) and if C in mol / L, constant called the molar absorptivity (). Based on this, Lambert -Beer law can be written in two forms, namely: A = a, b C (g / L) or A = b C (mol / L) Transmittance is the fraction of the transmitted power falls by an example. If A = log (P0 / P) then A = log 1 / T, where T = (P0 / P). Absorption spectrum graph is most often described as the transmittance (T) or absorbance (A) against concentration (C). By changing the concentration, the absorbance will change at each wavelength (). Graph can be described as follows:

Slope = b

C (mg/L)

Graphic of relation between absobance and concenration

C (mg/L)

Graphic of relation between absobance and transmittance Information obtained from ultaviolet and visible spectra: 1. Maximum wavelength ( maks ) a. Quantitative analysis, all measurements are based on, but to compound that has been known to frequently used approach to Woodward-Fieser. b. Qualitative analasis: less informative. 2. Maximum molar Absorptivitas ( maks ); qualitative analysis, namely information type tape / electronic transitions (plays a role in elelusidasi structure). Copper Cu is one element of the transition period to the fourth element in the periodic system. Copper metal has the electron configuration Ar (3d 10 4s1) To achieve stability of copper metal releases electrons to form compounds. One of the properties of copper that can conduct electricity well but is less reactive. Cu in small amounts are essential for life, but would be toxic in large amounts, especially for bacteria, algae, and fungi. Among the many copper compounds used as pesticides are alkaline acetate, carbonate, chloride, hydroxide, and sulfate. Commercially important compounds that are CuSO 4. In addition in agriculture, CuSO4 also used for battery and plating, the manufacture of other copper salts petroleum, rubber and steel industries. Ethyl-p-methoxycinnamate (EPMS) is one of the active ingredients found in sunscreen lotions.
H O

O CH 3 O H

C 2H 5

EPMS Structure

Usually the ethyl-p-methoxycinnamate can be isolated from natural materials from Koempheria galanga (Kencur). These compounds can be isolated using solvent extraction using organic solvents. Sunscreen lotions are usually used to minimize ultraviolet radiation. The range of ultraviolet radiation is divided into two: UV A and UV B. UV-B which has a wavelength range 280-320 nm is responsible for the skin damage. Therefore, sunscreen lotion contains several active compounds that can absorb ultraviolet radiation rays. Ethy-p-methoxycinnamate crystal has a melting point of about 48 o-49oC. These crystals can be obtained by isolate it from the natural ingredients contained which in such as kencur. In isolation experiments EPMS can be used sokhlet extraction method. Separation principle is based on the distribution ratio of solute in two solvents that do not dissolve each other. Kencur-paste, put in sokhlet tool that has been wrapped with filter paper. Extraction sokhlet discontinued when the suspected substance in the circulation that will be extracted are exhausted, this is indicated by no color change of solvent after passing through the sample. The organic solvent used in isolation EPMS using soxhlet extraction method is solvent ether. Ethy-p-methoxycinnamate crystals obtained usually is mixed with impurities. Purification can be done by recrystallization using ethanol and proceed with the test crystal melting point EPMS. Erythrina crista galli or red dadap is a kind of tree tribe members Fabaceae (Leguminosae). Plants are often used as live fences and shade it has many other designations. Medium-sized tree, reaching 15-20 m tall and 50-60 cm. Sections of bark are still young and fine vertical stripes of green, gray, brown or whitish; stem usually with a small outboard spikes (1-2 mm) black. Similar umbrella or rounded canopy gap, abort leaves in the dry season. The compound leaves bear three leaves, green to light green, leaf axis with 10-40 cm long stalks. Child leaves inverted egg round, triangular, up to a rhombus shape with blunt tip; child leaves the tip of the largest in size, 9-25 10-30 cm. The flowers are arranged in cone-shaped bunches, in addition to or at the end of the bare twigs, usually appear when the leaves fall, attracts many birds coming to pollinate. The crown is red orange to dark red; flag from 5.5 to 8 8 cm, short nails, no white striped. Pod thick and dark, narrowed between seeds, 15-20 cm 1.5-2 cm, containing 50-10 eggs eggshaped seed, brown, red or purple shiny.

Erythrina crista galli often used as shade trees in coffee farms and cocoa, or the propagation of trees for black pepper, betel nut, vanilla, or yam tubers. Also good to use as a living fence poles. This plant produces a light wood (BJ 0.2 to 0.3), soft and white, good for making floats, packing crates, frame, and children's toys. The wood pulp is also an ingredient, but less well-used as a wood fire because a lot of smoke. The leaves of young Erythrina crista galli can be used as a vegetable. The leaves are nutritious augment maternal milk, making sleep more soundly, and together with interest thereon for the launch period. The fluid extract of leaves mixed with honey drink to cure worms; Erythrina crista galli leaf juice mixed with castor oil is used to cure dysentery. The leaves are heated Erythrina crista galli used as a poultice to relieve rheumatism. Bark Erythrina crista galli has efficacy as a laxative, laxative sputum urine and diluent. Has a protein content (and nitrogen) is high, the leaves Erythrina crista galli also used as feed for livestock or green manure. Erythrina crista galli tree of medium size, which trimmed 3-4 times a year, can produce 15-50 kg of green feed in a year. So far, the leaves are known Erythrina crista galli not toxic (toxic) for ruminants. Erythrina crista galli root symbiosis with Brady rhizobium bacteria bind nitrogen from the air, and improve soil fertility.

III. CHEMICAL AND CHEMICAL APPATARUS 3.1 Chemical Apparatus No 1 2 3 4 5 6 7 8 9 10 Chemical Apparatus Volumetric pipette Beaker glass Volumetric flask Pipette Analitical balance Spatula Funnel Stirring rod Filer Spectrofotometry UV-Vis Size Measure 5 mL 100 mL, 250 mL 50 mL, 100 mL Amount 1 2 1 2 1 1 1 1 1 1

3.2 Chemicals No Chemicals 1 CuSO4.5H2O 2 Aquades 3 Ethanol 95% Amount 2.4948 grams 500 mL 500 mL

4 5 6 7 8

Kelopak bunga dadap merah NaOH HCl Serbuk PP Kristal EPMS

100 grams 10 mL 10 mL 1 gram 1 gram

IV. PROCEDURES AND RESULTS a. Determinination of Cu content in sample No Procedures Part 1 1. A total of 2.495 grams CuSO4.5H2O weighed and then dissolved into a little distilled water. After it is inserted into a 100 mL volumetric flask and added distilled water until a limit (0.1 M CuSO4 solution). 2. A total of 100 mL of 0.1 M CuSO4 solution was diluted to a concentration of 0.02, 0.04, 0.06, 0.08 M added with distilled water. 3. Standard solution which has diluted the measured absorbance using UV-visible spectrophotometer. Results CuSO4.5H2O powder blue CuSO4.5H2O who weighed at 2.4948 g 0.1 M CuSO4 solution in the form of a solution of blue

Initial solution is diluted to a standard solution of 0.02, 0.04, 0.06, 0.08 M color is fading.

Konsentrasi larutan standar Cu2+ (M) 0,02 0,04 0,06 0,08 4. From these data the standard calibration curve is made of copper which states the relationship between concentration and absorbance.
Absorbantion

Absorbansi 0,224 0,470 0,724 0,969

Standard Calibration Curve of Copper


1.5 1 0.5 0 0 0.05 Concentration 0.1 Linear (Series1) y = 12.44x - 0.025 R = 1 Series1

Part 2 1. Copper ore weighed about - about The mass of copper that weighed 1.0150 1.01 grams and was placed in 100 grams. mL beaker and add 10 mL of Copper after the soluble form of the blue concentrated nitric acid and 6 drops solution. of concentrated sulfuric acid. Reaction expected until the copper dissolves completely in concentrated nitric acid. 2. The mixture is inserted into a 250 After the solution becomes diluted color is fading. mL volumetric flask and then added distilled water to mark the limit. After that, 25 mL samples were taken and diluted to 50 mL. 3. The samples were diluted in the measured absorbance using UVKonsentrasi larutan Absorbansi 2+ visible spectrophotometer. Molar standar Cu (M) concentration of samples was Sample 0,371 determined through a calibration curve in part I. b. Determination of EPMS and nattural indicator absorbances No 1 Procedures Sedikit kristal EPMS dilarutkan dalam pelarut etanol. Rekam spectrum larutan EPMS berikut dengan menggunakan etanol 95% sebagai sampel referensi dan ukur absorbansinya. Results Kristal EPMS berupa kristal berwarna putih Larutan EPMS berupa larutan bening tidak berwarna Larutan EPMS 1,834

Absorbansi pada maks

c. Determination of indicators absorbance No Procedures Bagian 1 1 Serbuk PP dilarutkan dalam pelarut air. 2 Results Serbuk PP berupa serbuk berwarna putih Larutan PP berupa larutan bening tidak berwarna

Rekam spectrum masing masing larutan berikut dengan Larutan Larutan Larutan menggunakan air sebagai sampel E F G referensi Absorbansi 0,130 0,407 0,079 Larutan E : Larutan PP pada maks Larutan F : Larutan PP + NaOH Larutan G : Larutan PP + HCl Bagian 2 Kelopak bunga dari bunga Dadap Kelopak bunga Dadap Merah berwarna Merah digerus kemudian hasil merah padam

gerusan disaring. Ekstrak bunga Dadap Merah dilarutkan dengan etanol 95% Rekam spectrum masing masing larutan berikut dengan menggunakan etanol 95% sebagai sampel referensi dan ukur absorbansinya. Larutan H : Ekstrak bunga Dadap Merah Larutan I : Ekstrak bunga Dadap Merah + NaOH Larutan J : Ekstrak bunga Dadap Merah + HCl

Ekstrak bunga Dadap Merah berupa larutan berwarna merah kecoklatan

Absorbansi pada maks

Larutan Larutan Larutan H I J 0,036 0,444 0,008

V. ANALYSIS AND DISCUSSIONS a. Analysis of copper content in sample In these experiments used UV-Vis spectrophotometer to determine the amount of absorption wavelength of a colored complex compounds. UV-Vis spectrophotometer uses two light sources are deuterium lamp (D) for ultraviolet light and tungsten light (W) for visible light. The sample to be measured absorbance is inserted into the sample container (kuvet). Sample container or kuvet is made of material which could continue to absorb light and no light. Kuvet usually is made of glass or silica. Then the light source is passed through an existing gap in the monochromatic, where the light is directed separately through reference and sample with a rotating mirror that allows the first light in one direction, then in the other direction. Both light and then turn to change direction with a continuous rotation mirror and see the light detector and then the other one repeatedly. Electrical signals that change is processed, converted to digital, and compared and programmable calculations performed. Monochromatic wavelength is set to transfer a motor driven or for the measurement wavelength is determined by the operator. In this lab analysis of copper metal content of the sample solution CuSO4. Copper Content Analysis of Solvent Samples CuSO4 First of all done recording the spectra distilled water in a reference cell and a solution of A to D in the sample cell. Solvent A to D is a solution containing cupri ion Cu (H2O)42+, where the data is obtained as follows: Concentration (C) Absorbance Wavelength (nm) A 0.02 0.224 800 B 0.04 0.470 800 C 0.06 0.724 800 D 0.08 0.969 800

From the table above can be made to the absorbance relationship against concentration as follows:

Standard Calibration Curve of Copper


1.2 1 Absorbance 0.8 0.6 0.4 0.2 0 0 0.02 0.04 0.06 0.08 0.1 Series1 Linear (Series1) y = 12.44x - 0.025 R = 1

Concentration

Curve 1. Curve relation to the concentration of the sample solution absorbance

From the above curve can be obtained straight line equation: y = 12.44x - 0025, where the value 12.44 represents the slope of the curve. A = mC + a A = 12.44 C - 0.025 0.371 = 12.44 C - 0.025 12.44 C = 0.371 + 0.025 C = 0.0318 M for 50 mL (after the sample was diluted from 25 mL to 50 mL) Solution concentration before dilution is: V1.M1 = V2.M2

50 mL x 0.0318 M= 25 mL x M2 M2 = 0.0637 M So the initial molarity (in volume 250 mL) is 0.0637 M. So the number of moles in the initial solution is: Mol Cu = MxV = 0.0637 M x 0.25 L = 0,015925 mol Mass Cu in sample = mole x molar mass

= 0.015925 mol x 63,5 = 1,0112 grams % Cu in sample = =


1,0112 1,0150

100%

100%

= 99,63 %

b. Analysis of EPMS absorbance EPMS is an active compound in a sunscreen lotion. Uptake EPMS can be measured by using UV-Vis. The results show two peaks at a wavelength of 307 nm and 228.5 nm. EPMS absorption at a wavelength of 228.5 nm is 0.770 and for a wavelength of 307 nm absorbance is 1.834. EPMS can absorb at a wavelength of 307 nm. This suggests that EPMS can absorb UV-B so that used as a sunscreen lotion. For the data can be seen in this following image.

c.

Analysis of natural indicator absorbance PP indicator absorption in the atmosphere of acids and bases can be determined by using UV-Vis. Uptake of PP without the addition of acid indicator or base can be seen in the picture below.

From this picture can be seen there are three peaks at a wavelength of 229, 276, and 342.5 nm with absorption, respectively, 0.396, 0.163, and 0.130. Addition of acid in the PP is not too much change summit, but the uptake of PP changed. This does not provide color changes in the solution of PP. PP acid absorption in the atmosphere can be seen in the following figure.

Uptake of PP at 228.5, 276, and 342 nm respectively are 0.329, 0.108, and 0.079. Addition of base change in the indicator PP peak. Originally there were three peaks, but with the addition of alkali to make 2 pieces of the peak. This shows the changes in the structure of PP under alkaline conditions. These structural changes cause the PP red under alkaline conditions. PP absorption in alkaline conditions can be seen in the following figure.

PP uptake was detected in two peaks at a wavelength of 370 and 553 nm. Uptake of each peak was 0.082 and 0.407. In this experiment also tested the absorption of red dadap flower extract as a natural indicator sample. Absorption of red dadap extract without the addition of acid or base brownish red in color, shows 3 pieces of the peak at a wavelength of 230, 283, and 663 nm. Uptake of each peak is 2.003, 1.166, 0.036. Figure absorption red dadap extract attached. Addition of acid to extract red dadap provide 4 pieces of the peak at a wavelength of 225, 284, 532, and 665 with respective absorption peaks are 1.316, 0.635, 0.077, and 0.008. The addition of these top causes dadap extract red color changed from red to brownish red. Figure absorption dadap extract of red in acidic form. Addition of bases in extracts of red dadap provide 2 pieces of the peak at a wavelength of 244 and 579 with respective absorption peaks are 2.458 and 0.444. This peak reduction causes red dadap extract color changes from red brown to greenish brown. Figure absorption red dadap extract under alkaline conditions attached.

VI. CONCLUSION 1. Standard curve absorbance relationship with concentration can be made from data obtained using UV-Vis spectroscopy and copper metal content can be searched, which acquired levels of copper in copper ore at 99.63%. 2. EPMS can absorb UV-B at wavelengths of 307 with the uptake of 1.834. 3. Dadap red flower extract may be used as a natural indicator because it can change color in acidic and alkaline.

REFFERENCES Ismono. 1978. Cara-cara Optik Dalam Analisis Kimia. Diktat. Bandung: Jurusan Kimia ITB Fessenden, Ralph dan Joan Fesseanden. 1982. Kimia Organik Jilid 1. Jakarta : Erlangga. Khopkar, S.M. 1990. Basic Concepts of Analytical Chemistry. Terj. Saptoraharjo, A. Konsep Dasar Kimia Analitk. Jakarta: UI-Press. Petrucci. 1985. Kimia Dasar Prinsip dan Terapan Modern. Jakarta : Erlangga. Diakses tanggal 24 April 2008 dari http://www.Kebonkembang.com/neo. Tim Pembina Ilmu Kimia. 2004. Modul Pembinaan Pembelajaran Kimia Bidang Ilmu Kimia Fisika. Bali : Jurusan Kimia FMIPA Universitas Udayana.

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