II. Spectrophotometry (Chapters 17, 19, 20)
|
|
- Garey Gibbs
- 6 years ago
- Views:
Transcription
1 II. Spectrophotometry (Chapters 17, 19, 20) FUNDAMENTALS (Chapter 17) Spectrophotometry: any technique that uses light to measure concentrations (here: U and visible - ~ nm) c = x 10 8 m/s (in vacuum) ν = frequency (s -1 ); λ = wavelength (m) h = Planck s ct. = x J/s (this is for 1 photon; for 1 mol of photons: x N) ν is the wavenumber = 1/λ E is inversely related to λ, but directly proportional to ν 1 Additive primary colours: red, green and blue The observed color is called the complementary color. A white object reflects all (visible) light 2
2 ? Airport body scanners Your microwave at home (2.45 GHz) 3 Interaction of molecules with light (EM radiation): Depends on the λ of the radiation: Microwave radiation: rotational transitions of molecule IR radiation: stretching and bending of bonds Irradiation of formaldehyde with the right λ increases the amplitude of the vibrations isible light and U radiation: Energetic enough to cause electronic transitions: electron moves from one MO to higher energy MO (e.g. n π*) Short wavelength U and X-rays: break bonds, ionize molecules All transitions are quantized! selection rules 4
3 Upon absorption of a photon, the entire molecule is in an excited state, but electronic transitions can usually be assigned to specific functional groups (e.g. C=O, C=C, NO 2, conjugated π system). These chromophores can undergo π π*, n π* and n σ* transitions (inorganic molecules: e.g. d d) With each electronic transition, there are numerous vibrational and rotational transitions broad peaks! E S 1 λ 3 λ 2 ν S 2 0 ν 1 0 (Rotational levels not shown) At room temperature, most transitions are from the lowest vibrational level of the ground state (S 0, ν 0 ). When irradiated with broadband EM radiation, those λ s corresponding with a particular transition can be absorbed. Because of numerous energy levels, numerous λ s are absorbed, giving the impression of a broad absorption peak. In addition, solution-phase spectra are broadened because of interaction of absorbing molecules with solvent molecules. For simple molecules in a dilute gas phase, individual rotational transitions can often be distinguished. There may be several chromophores in one molecule: broad and overlapping peaks 5 Spectra of atoms are line spectra, because they do not have vibrational and rotational transitions. Compare the width of these absorption peaks (notice the different scales) 6
4 What happens to the absorbed energy? Absorption of radiation increases energy of molecule; two ways to release that energy (besides taking part in a photochemical reaction): Radiationless energy transfer: vibrational relaxation and internal conversion (collisions with other molecules, e.g solvent) Emission of radiation: fluorescence, phosphorescence (= luminescence) 7 Fluorescence always from the lowest vibrational level of the excited state Emission at higher λ (lower frequency, lower E) Fluorescence: much more sensitive analysis technique then absorption spectrophotometry (~no background) 8
5 Absorption Spectrophotometry (Chapters 19, 20) Schematic of a single beam dispersive spectrophotometer: LIGHT SOURCE - Continuum source Produces a continuous band of λ s in visible and U region of spectrum Deuterium lamp ( nm): electric discharge causes D 2 to dissociate and emit U radiation (~ nm) + Tungsten lamp: W filament at 3000 K gives useful radiation in the range of nm (For atomic absorption, line sources are used see further) 9 Typically, the instrument switches automatically from the D 2 lamp to the W lamp when passing through 360 nm so that always the source with the highest intensity is used. MONOCHROMATOR -selects a narrow band of λ s from the continuum band. Historically, prisms were widely used, but they have been surpassed by gratings (optical components with closely spaced lines; different wavelengths of light are reflected at different angles from the grating = diffraction). 10
6 Polychromatic radiation is collimated The width of the exit slit can be adjusted to allow various bandwidths to reach the detector. A bandwidth of 1.0 nm through the exit slit is quite common, Rotates so that different λs can pass through exit slit A filter is often placed after the exit slit to prevent higher order diffractions of λ 2 /n to reach the detector e.g. 2 nd order of λ 2 /2; third order of λ 2 /3 11 CUETTE- places sample in path of light to be absorbed. P is the irradiance of the beam leaving the cuvette such that P P 0 The pathlength b is the distance the beam has travelled through the sample For U-is spectrophotometry cuvettes are made of quartz LIGHT DETECTOR - converts light to electric current e.g. photomultiplier tube, diode array detector (DAD), or charge coupled device (CCD) Transmittance T: fraction of original light that passes through the sample: P = irradiance (Js -1 m -2 ) % T P/P P 0 P 0 /P A %T = x 100% 100 % P 0 10% % Absorbance A: A is dimensionless, but you may see AU or mau as units 12
7 Beer-Lambert s law: Absorbance of a sample is linearly related to it s concentration: c = [analyte] (M) b = path length of cuvette (cm) ε = molar absorptivity or extinction coefficient (M -1 cm -1 ) ε is a characteristic of a compound for a particular λ, but can be influenced by intermolecular interactions Ideally as large as possible for good sensitivity Deviations from Beer s law: At high concentrations (>0.01 M), solute molecules are close enough to each other to interact and alter their light absorbing properties (i.e. ε value changes); high conc. of non-absorbing species can have this effect as well Strictly speaking only for truly monochromatic radiation In practice, deviations are not observed with the narrow range of λ s transmitted by spectrophotometers 13 Analytes that participate in a concentration dependent equilibrium (apparent deviation): e.g. weak acids (HA) are more dissociated at higher dilution. If ε of the undissociated species HA differs from that of the dissociated species A -, a series of dilutions of HA will appear not to obey Beer s law. (Solution: use a buffer to maintain a constant ph constant dissociation) Other apparent deviations: stray light, fluorescence, scattering by particles Application of Beer s law in chemical analysis: Select λ: usually λ of max. intensity (max. ε) to give best sensitivity, and to have the least change in A if drift in monochromator In case of interference with another compound, another λ may be necessary (note: with DAD, the whole spectrum can be recorded instantaneously) Record baseline spectrum of either pure solvent or reagent blank (alternatively, if solvent is used to obtain the baseline spectrum, the value of a reagent blank can be subtracted from the unknown) 14
8 Measure absorbances of (usually) 3 to 5 standard solutions containing accurately known concentrations of analyte, and the unknown (aim for an absorbance of for best accuracy) Construct a calibration curve: plot A vs. conc. or mass of analyte Use linear regression (least squares) to obtain: A = mc + b where m = slope of curve b = intercept with y-axis c = concentration of amount of analyte With the absorbance of the unknown, and the values of m and b from the calibration curve, the unknown concentration can be found 15 Example 1: The concentration of iron(iii) in an unknown was determined from a calibration curve of absorbance vs concentration of standard solutions. Calculate the concentration of iron (III) in the unknown in mol L 1. A unknown = 0.479; m = ppm -1 ; b = (A - b) unknown CA = mc = + b.. = = ppm unknown 1 m ppm = c c = 1.86 ppm mg C c = unknown L 3+ 1g 1mol Fe = 3.32 x mg g -5 mol Fe Example 2: Gaseous ozone has a molar absorptivity of 2700 M -1 cm -1 at 260 nm. Find the concentration of ozone in air with an absorbance of in a 10.0 cm cell if a blank of air has an absorbance of at this wavelength. A c = = -1-1 εb 2700M cm 10.0 cm -6 c = 8.62 x 10 M 3+ L -1 16
9 Double beam dispersive spectrophotometers: Advantages of double beam over single beam instrument: P 0 reflective surface Reference is left in instrument no switching around Better for following absorbance as a function of time (kinetics experiments) because corrects automatically for drift in both lamp intensity and detector response over time Easier to acquire whole spectrum of analyte by scanning λ-range P 0 17 The photomultiplier tube (PMT) as a sensitive detector: EM radiation hits photosensitive surface (at neg. potential), which emits electrons Emitted electrons strike a dynode (at less neg. potential than photosensitive surface); for each electron that hits the dynode, two or more other electrons are released These electrons hit a second dynode (at less neg. potential then first dynode), which releases even more electrons, which hit a third dynode Signal amplification leads to >10 6 electrons for each photon! (depends on kinetic energy of electrons, thus on potential difference btw photocathode and last dynode) 18
10 Photodiode array spectrophotometers: Entire spectrum recorded in fraction of a second (signal averaging!) = Type of spectrophotometer used in liquid chromatography Each diode receives a different λ; resolution depends on how closely spaced the diodes are, and the degree of dispersion by the polychromator. Best resolution currently available is ~ nm. Fig : Effect of signal averaging on a noisy spectrum 19 A reverse bias is applied to each diode, drawing electrons and holes away from the junction, creating a depletion region. Each photodiode can be thought of as a capacitor, with a fixed charge. When light hits a photodiode, free electrons and holes are created, partially discharging the photodiode. At the end of each measuring cycle, the current needed to recharge the capacitor is proportional to # photons it received (i.e. the irradiance). Charge coupled devices (CCDs) are also used as detectors, and are much more sensitive than photodiodes. They consist of a two-dimensional array of pixels and operate on a slightly different basis than DADs. 20
11 ATOMIC SPECTROSCOPY (Chapter 20) In atomic spectroscopy, samples are decomposed at high temperatures into atoms. Concentrations of atoms in the vapor are measured by absorption or emission of characteristic λs of radiation. μg/g to pg/g levels (sensitive!), with a precision of 1-2% Atomic Absorption Spectrometry (AAS) Nebulizer Liquid sample aspirated into flame Sample atomizes HCL emits light at λ that element can absorb Intensity of light that reaches detector (P) decreases as concentration of analyte increases (Beer s law applies flame = cuvette) 21 Energy level diagram of sodium (1s 2 2s 2 2p 6 3s 1 ): Modified from: 22
12 Hollow Cathode Lamp (HCL) Atomic absorption lines are very narrow (~ nm) Beer s law requires that linewidth of source << linewidth of absorbing sample Cannot use monochromator, instead use HCL with the cathode made from the same element that has to be analyzed P 0 HCL is filled with Ne or Ar (low pressure) applied: gas ionized and cations accelerated towards cathode, where they sputter metal atoms into gas phase. A certain fraction of these are in an excited state, and they fall back to the ground state by emission of photons of specific λs. 23 The λs of the emitted radiation are the same as those that can be absorbed by the analyte (not all λs will be useful) Note that the bandwidth of the emitted radiation (from cool atoms)< that of the absorption bandwidth of the atoms in the hot flame (Doppler linewidth ~ T) A different lamp is needed for each element, but some lamps are made with more than one element in the cathode Monochromator (see slide 8 same type) Selects one specific emission line Rejects as much emission from flame as possible Flame and Nebulizer Sample is aspirated in to the nebulization chamber by the rapid flow of oxidant, where it is turned into a mist (fine droplets) and mixed with fuel and oxidant. The mist flows past baffles which remove large droplets and promotes the formation of finer droplets, resulting in the aerosol, which eventually passes into the flame. (~5% of the solution originally aspirated 95% goes to waste!). 24
13 MX (solution) nebulization MX (solution aerosol) desolvation MX (solid aerosol) Desolvation: the liquid solvent is evaporated, and the dry sample remains aporization: the solid sample vaporizes to a gas Dissociation: the compounds making up the sample are broken into free atoms. vaporization MX(g) dissociation M 0 X 0 M + X - 25 The flame is long (~10 cm) and narrow; height is controlled by the flow of the fuel mixture The beam of light from the HCL is directed along the long axis and its height has to be optimized for each element because of different temperature regions within the flame (this affects formation of oxides, desolvation, vaporization etc.) Temperature of the flame depends on fuel/oxidant. Acetylene/air is most used ( K). Higher temperatures for refractory elements can be obtained with acetylene/oxygen (~3400 K) Detectors: PMT, DAD, CCD Interferences in AAS: Interference = any effect that changes the signal, while analyte conc. stays the same Spectral interference: overlap of spectral lines Chemical interference: e.g. decrease of extent of atomization Ionization interference: ion has different energy levels than atom 26
14 Flameless methods: Generally better detection limits than flame AAS Graphite Furnace AAS: Sample is deposited (manually or automatically) into a graphite tube which is electrically heated Heating takes place in several steps to remove solvent, destroy organic matter etc. Sample is confined in the optical path for several seconds increases sensitivity (note: transient signal as opposed to continuous signal) Both liquid and solid samples Cold apor AAS: For Hg only (only metallic element with appreciable vapor pressure at ambient temperature) All Hg in a liquid sample is reduced to Hg 0, which is removed by bubbling inert gas through the sample, and introduced into the analysis chamber Hydride generation techniques: For As, Sb, Sn, Se, Bi and Pb: form volatile hydrides after reaction with NaBH 4 (to e.g. AsH 3 ). Most of analyte ends up in the instrument <> flame AAS where 95% of the sample goes to waste. 27 Inductively Coupled Plasma (ICP) Sample is introduced into a plasma (= partially ionized gas free ions and electrons) at a temperature of K Much of the interferences from AAS are lost (but not all!) At this high temperature, a higher fraction of atoms are in an excited state, and it is the radiation that is emitted by these atoms when they fall back to the ground state that is measured Multielement technique; 70+ elements can be determined at once! 28
15 Drinking water analysis (EPA certified method) GFAA for clinical use determination of trace elements in blood serum. Trace elements in food Trace element analysis of hair (forensics) For accurate quantitative analysis, multiply DL by 10 For analysis of elements at DL afforded by GFAAS and ICP-MS, a clean room with filtered air supply is necessary! 29 MATRIX EFFECTS (Chapter 5) Matrix: All non-analyte components of a sample Matrix effects: Influence of the matrix on the response of the instrument to the analyte Why are matrix effects a problem in analysis of real samples? If the response of the analyte in the unknown solution is different from the one in the standard solutions (because of matrix effects), then large errors can be introduced in the analysis. Methods used to minimize matrix effects: Separation of analyte from the matrix - Must be quantitative (e.g. chromatography, precipitation and filtration of interfering compound) Prepare standard solutions in the same matrix as the samples (e.g. standards in river water has to be free of analytes that are analyzed!) Standard addition: Allows the standard and analyte to be measured in same or nearly identical matrix. 30
16 Overcoming Matrix Effects using Standard Addition M. Bader, Journal of Chemical Education 57 (1980) 703 Known quantities of analyte are added to the unknown (small amounts of a concentrated standard are added, so that the matrix composition does not change a lot) From increase in signal, original amount or concentration is deduced Requires linear increase in response = conc. of analyte X in sample (volume 0 ); gives a signal intensity of I x I x = k A known conc. of a standard S (which is the same analyte as X) is added (conc. [S] i ; volume s ). The intensity of the signal is now I S+X I S+X = k ([X] f + [S] f ) [X] f = [X] 0 i [S] f = [S] s i ( = 0 + s ) 31 Dividing first equation by second equation: I X I S+X = [X] f + [S] f I X and I S+X are measured [X] f and [S] f are calculated can be determined There are a number of different ways in which standard addition can be performed. We will only discuss three cases: CASE 1: Same flask volume changes Accurately measure a certain volume of sample acquire signal Accurately add a known amount of standard into the sample solution acquire signal (e.g. ion selective electrode) EXAMPLE: A 50.0 ml sample of orange juice gave a signal of 1.78 μa using an electrochemical method. A standard addition of ml of M ascorbic acid increased the signal to 3.35 μa. Find the concentration of ascorbic acid in the orange juice. 32
17 I x = 1.78 μa I S+X = 3.35 μa 0 = 50.0 ml ; = 50.0 ml ml = 50.4 ml [X] f = 0 [S] f = [S] i = 50.0 ml 50.4 ml s = M ml 50.4 ml = = x 10-3 M 1.78 μa 3.35 μa = x 10-3 M = 2.49 x 10-3 M CASE 2: Sample in one flask Sample and standard in 2 nd flask both diluted to same final volume Usually done when reagents have to be added (e.g. colorimetric reaction) and/or when the measurement itself consumes the sample 33 Same volume of sample is added to both volumetric flasks; small volume of standard solution added to one of the flasks Reagents added to both volumetric flasks, which are then diluted to volume Signals for both solutions are acquired In the formula on slide 32, the numerator corresponds to the measurement of the undiluted sample. However, here the sample is diluted to its final volume when we measure it, so the formula we have to use changes to: I X I S+X [X] = f Standard addition at constant volume [X] f + [S] f EXAMPLE: Two 10.0 ml samples of run-off water are added to separate ml flasks. A ml aliquot of ppm iron(iii) is added to the second flask. Both flasks have reagents added to give a colored product and are then diluted to volume (25.00 ml). The absorbance of the two solutions in a 1.00 cm cell at 490 nm were and respectively. Calculate the concentration of iron (III) in the run-off water. 34
18 I x = I S+X = = ml ; = ml [X] f = 0 = ml ml = [S] f = [S] i s = ppm ml = 4.00 ppm ml = ppm = 13.0 ppm Case 3: Multiple Standard Addition at Constant Total olume Calibration Curves A series of solutions are prepared in volumetric flasks, each containing the same volume of unknown ( 0 ), and different volumes of standard ( s ) 35 (from slide 27) I S+X = k 0 + k [S] i s and add reagents, if any y = b + m x Plot I S+X vs. s from the equation of this curve, determine b and m: b = k m = k [S] i 0 b m = 0 [S] i = b m [S] i 0 36
19 I S+X s Alternatively, one can plot I S+X vs. [S] i s i.e. I S+X vs. conc. of standard in the flasks We now find: b = k m = k 0 b m = 0 = b m 0 Note that the factor / 0 takes into account the dilution of the sample in the volumetric flask. If we plot I S+X vs. [S] i s, the concentration of the 37 unknown in the volumetric flask is the neg. intercept with the x-axis: I S+X conc. (mm) - conc. of X in volumetric flask; has to be corrected with dilution factor to find 38
10/2/2008. hc λ. νλ =c. proportional to frequency. Energy is inversely proportional to wavelength And is directly proportional to wavenumber
CH217 Fundamentals of Analytical Chemistry Module Leader: Dr. Alison Willows Electromagnetic spectrum Properties of electromagnetic radiation Many properties of electromagnetic radiation can be described
More information2101 Atomic Spectroscopy
2101 Atomic Spectroscopy Atomic identification Atomic spectroscopy refers to the absorption and emission of ultraviolet to visible light by atoms and monoatomic ions. It is best used to analyze metals.
More informationComplete the following. Clearly mark your answers. YOU MUST SHOW YOUR WORK TO RECEIVE CREDIT.
CHEM 322 Name Exam 3 Spring 2013 Complete the following. Clearly mark your answers. YOU MUST SHOW YOUR WORK TO RECEIVE CREDIT. Warm-up (3 points each). 1. In Raman Spectroscopy, molecules are promoted
More informationReference literature. (See: CHEM 2470 notes, Module 8 Textbook 6th ed., Chapters )
September 17, 2018 Reference literature (See: CHEM 2470 notes, Module 8 Textbook 6th ed., Chapters 13-14 ) Reference.: https://slideplayer.com/slide/8354408/ Spectroscopy Usual Wavelength Type of Quantum
More informationBecause light behaves like a wave, we can describe it in one of two ways by its wavelength or by its frequency.
Light We can use different terms to describe light: Color Wavelength Frequency Light is composed of electromagnetic waves that travel through some medium. The properties of the medium determine how light
More informationEmission spectrum of H
Atomic Spectroscopy Atomic spectroscopy measures the spectra of elements in their atomic/ionized states. Atomic spectrometry, exploits quantized electronic transitions characteristic of each individual
More information3 - Atomic Absorption Spectroscopy
3 - Atomic Absorption Spectroscopy Introduction Atomic-absorption (AA) spectroscopy uses the absorption of light to measure the concentration of gas-phase atoms. Since samples are usually liquids or solids,
More informationhigh temp ( K) Chapter 20: Atomic Spectroscopy
high temp (2000-6000K) Chapter 20: Atomic Spectroscopy 20-1. An Overview Most compounds Atoms in gas phase high temp (2000-6000K) (AES) (AAS) (AFS) sample Mass-to-charge (ICP-MS) Atomic Absorption experiment
More informationCh. 9 Atomic Absorption & Atomic Fluorescence Spectrometry
Ch. 9 Atomic Absorption & Atomic Fluorescence Spectrometry 9.1 9A. Atomization Most fundamental for both techniques. Typical types 1. flame - burner type 2. Electrothermal graphite furnace 3. Specialized
More informationOptical Atomic Spectroscopy
Optical Atomic Spectroscopy Methods to measure conentrations of primarily metallic elements at < ppm levels with high selectivity! Two main optical methodologies- -Atomic Absorption--need ground state
More informationCH. 21 Atomic Spectroscopy
CH. 21 Atomic Spectroscopy 21.1 Anthropology Puzzle? What did ancient people eat for a living? Laser Ablation-plasma ionization-mass spectrometry CH. 21 Atomic Spectroscopy 21.2 plasma In Atomic Spectroscopy
More informationAtomic Absorption Spectrophotometry. Presentation by, Mrs. Sangita J. Chandratre Department of Microbiology M. J. college, Jalgaon
Atomic Absorption Spectrophotometry Presentation by, Mrs. Sangita J. Chandratre Department of Microbiology M. J. college, Jalgaon Defination In analytical chemistry, Atomic absorption spectroscopy is a
More informationSpectroscopy. Page 1 of 8 L.Pillay (2012)
Spectroscopy Electromagnetic radiation is widely used in analytical chemistry. The identification and quantification of samples using electromagnetic radiation (light) is called spectroscopy. Light has
More informationChemistry Instrumental Analysis Lecture 18. Chem 4631
Chemistry 4631 Instrumental Analysis Lecture 18 Instrumentation Radiation sources Hollow cathode lamp Most common source Consist of W anode and a cathode sealed in a glass tube filled with Ne or Ar. Hollow
More informationInstrumental Analysis: Spectrophotometric Methods
Instrumental Analysis: Spectrophotometric Methods 2007 By the end of this part of the course, you should be able to: Understand interaction between light and matter (absorbance, excitation, emission, luminescence,fluorescence,
More informationSpectroscopy Problem Set February 22, 2018
Spectroscopy Problem Set February, 018 4 3 5 1 6 7 8 1. In the diagram above which of the following represent vibrational relaxations? 1. Which of the following represent an absorbance? 3. Which of following
More informationATOMIC SPECROSCOPY (AS)
ATOMIC ABSORPTION ANALYTICAL CHEMISTRY ATOMIC SPECROSCOPY (AS) Atomic Absorption Spectroscopy 1- Flame Atomic Absorption Spectreoscopy (FAAS) 2- Electrothermal ( Flame-less ) Atomic Absorption Spectroscopy
More informationSpectroscopy: Introduction. Required reading Chapter 18 (pages ) Chapter 20 (pages )
Spectroscopy: Introduction Required reading Chapter 18 (pages 378-397) Chapter 20 (pages 424-449) Spectrophotometry is any procedure that uses light to measure chemical concentrations Properties of Light
More informationLecture 7: Atomic Spectroscopy
Lecture 7: Atomic Spectroscopy 1 Atomic spectroscopy The wavelengths of absorbance and emission from atoms in the gas phase are characteristic of atomic orbitals. 2 In the lowest energy transition, the
More informationChem 310 rd. 3 Homework Set Answers
-1- Chem 310 rd 3 Homework Set Answers 1. A double line labeled S 0 represents the _ground electronic_ state and the _ground vibrational_ state of a molecule in an excitation state diagram. Light absorption
More informationCourse Details. Analytical Techniques Based on Optical Spectroscopy. Course Details. Textbook. SCCH 211: Analytical Chemistry I
SCCH 211: Analytical Chemistry I Analytical Techniques Based on Optical Spectroscopy Course Details September 22 October 10 September 22 November 7 November 17 December 1 Topic Period Introduction to Spectrometric
More informationAtomization. In Flame Emission
FLAME SPECTROSCOPY The concentration of an element in a solution is determined by measuring the absorption, emission or fluorescence of electromagnetic by its monatomic particles in gaseous state in the
More informationIntroduction to Spectroscopic methods
Introduction to Spectroscopic methods Spectroscopy: Study of interaction between light* and matter. Spectrometry: Implies a quantitative measurement of intensity. * More generally speaking electromagnetic
More informationChemistry 311: Instrumentation Analysis Topic 2: Atomic Spectroscopy. Chemistry 311: Instrumentation Analysis Topic 2: Atomic Spectroscopy
Atomic line widths: Narrow line widths reduce the possibility of spectral overlap and thus interferences. The band width at half height is used to indicate width. This is also sometimes called the effective
More informationChapter 13 An Introduction to Ultraviolet/Visible Molecular Absorption Spectrometry
Chapter 13 An Introduction to Ultraviolet/Visible Molecular Absorption Spectrometry 13A Measurement Of Transmittance and Absorbance Absorption measurements based upon ultraviolet and visible radiation
More informationR O Y G B V. Spin States. Outer Shell Electrons. Molecular Rotations. Inner Shell Electrons. Molecular Vibrations. Nuclear Transitions
Spin States Molecular Rotations Molecular Vibrations Outer Shell Electrons Inner Shell Electrons Nuclear Transitions NMR EPR Microwave Absorption Spectroscopy Infrared Absorption Spectroscopy UV-vis Absorption,
More informationChem 155 Midterm Exam Page 1 of 10 Spring 2010 Terrill
Chem 155 Midterm Exam Page 1 of 10 ame Signature 1. Mercury (Hg) is is believed to be hazardous to human neurological health at extremely low concentrations. Fortunately EPA Method 45.7 cold vapor atomic
More information9/13/10. Each spectral line is characteristic of an individual energy transition
Sensitive and selective determination of (primarily) metals at low concentrations Each spectral line is characteristic of an individual energy transition 1 Atomic Line Widths Why do atomic spectra have
More informationFLAME PHOTOMETRY AIM INTRODUCTION
FLAME PHOTOMETRY AIM INTRODUCTION Atomic spectroscopy is based on the absorption, emission or fluorescence process of light by atoms or elementary ions. Information for atomic scale is obtained in two
More informationSpectrophotometry. Dr. Shareef SHAIK ASST. PROFESSOR Pharmacology
Spectrophotometry Dr. Shareef SHAIK ASST. PROFESSOR Pharmacology Content Introduction Beer-Lambert law Instrument Applications Introduction 3 Body fluids such as blood, csf and urine contain organic and
More informationCHEM*3440. Photon Energy Units. Spectrum of Electromagnetic Radiation. Chemical Instrumentation. Spectroscopic Experimental Concept.
Spectrum of Electromagnetic Radiation Electromagnetic radiation is light. Different energy light interacts with different motions in molecules. CHEM*344 Chemical Instrumentation Topic 7 Spectrometry Radiofrequency
More information25 Instruments for Optical Spectrometry
25 Instruments for Optical Spectrometry 25A INSTRUMENT COMPONENTS (1) source of radiant energy (2) wavelength selector (3) sample container (4) detector (5) signal processor and readout (a) (b) (c) Fig.
More informationSpectrochemical methods
Spectrochemical methods G. Galbács The interactions of radiations and matter are the subject of spectroscopy py or spectrochemical methods (also called spectrometry). Spectrochemical methods usually measure
More informationChapter 4 Ultraviolet and visible spectroscopy Molecular Spectrophotometry
Chapter 4 Ultraviolet and visible spectroscopy Molecular Spectrophotometry Properties of light Electromagnetic radiation and electromagnetic spectrum Absorption of light Beer s law Limitation of Beer s
More informationAtomic Emission Spectroscopy
Atomic Emission Spectroscopy Ahmad Aqel Ifseisi Assistant Professor of Analytical Chemistry College of Science, Department of Chemistry King Saud University P.O. Box 2455 Riyadh 11451 Saudi Arabia Building:
More informationMOLECULAR AND ATOMIC SPECTROSCOPY
MOLECULAR AND ATOMIC SPECTROSCOPY 1. General Background on Molecular Spectroscopy 3 1.1. Introduction 3 1.2. Beer s Law 5 1.3. Instrumental Setup of a Spectrophotometer 12 1.3.1. Radiation Sources 13 1.3.2.
More informationCh. 8 Introduction to Optical Atomic Spectroscopy
Ch. 8 Introduction to Optical Atomic Spectroscopy 8.1 3 major types of Spectrometry elemental Optical Spectrometry Ch 9, 10 Mass Spectrometry Ch 11 X-ray Spectrometry Ch 12 In this chapter theories on
More informationINTRODUCTION Atomic fluorescence spectroscopy ( AFS ) depends on the measurement of the emission ( fluorescence ) emitted from gasphase analyte atoms
INTRODUCTION Atomic fluorescence spectroscopy ( AFS ) depends on the measurement of the emission ( fluorescence ) emitted from gasphase analyte atoms that have been excited to higher energy levels by absorption
More informationatomic absorption spectroscopy general can be portable and used in-situ preserves sample simpler and less expensive
Chapter 9: End-of-Chapter Solutions 1. The following comparison provides general trends, but both atomic absorption spectroscopy (AAS) and atomic absorption spectroscopy (AES) will have analyte-specific
More informationAN INTRODUCTION TO ATOMIC SPECTROSCOPY
AN INTRODUCTION TO ATOMIC SPECTROSCOPY Atomic spectroscopy deals with the absorption, emission, or fluorescence by atom or elementary ions. Two regions of the spectrum yield atomic information- the UV-visible
More informationChapter 17: Fundamentals of Spectrophotometry
Chapter 17: Fundamentals of Spectrophotometry Spectroscopy: the science that deals with interactions of matter with electromagnetic radiation or other forms energy acoustic waves, beams of particles such
More informationChemistry 311: Instrumentation Analysis Topic 2: Atomic Spectroscopy. Chemistry 311: Instrumentation Analysis Topic 2: Atomic Spectroscopy
Topic 1: Atomic Spectroscopy Text: Chapter 12,13 & 14 Rouessac (~2 weeks) 1.0 Review basic concepts in Spectroscopy 2.0 Atomic Absorption and Graphite Furnace Instruments 3.0 Inductively Coupled Plasmas
More informationChapter 17: Fundamentals of Spectrophotometry
Chapter 17: Fundamentals of Spectrophotometry Spectroscopy: the science that deals with interactions of matter with electromagnetic radiation or other forms energy acoustic waves, beams of particles such
More informationANALYSIS OF ZINC IN HAIR USING FLAME ATOMIC ABSORPTION SPECTROSCOPY
ANALYSIS OF ZINC IN HAIR USING FLAME ATOMIC ABSORPTION SPECTROSCOPY Introduction The purpose of this experiment is to determine the concentration of zinc in a sample of hair. You will use both the calibration
More informationChem 321 Lecture 18 - Spectrophotometry 10/31/13
Student Learning Objectives Chem 321 Lecture 18 - Spectrophotometry 10/31/13 In the lab you will use spectrophotometric techniques to determine the amount of iron, calcium and magnesium in unknowns. Although
More informationSkoog Chapter 6 Introduction to Spectrometric Methods
Skoog Chapter 6 Introduction to Spectrometric Methods General Properties of Electromagnetic Radiation (EM) Wave Properties of EM Quantum Mechanical Properties of EM Quantitative Aspects of Spectrochemical
More informationAnalytical Spectroscopy Review
Analytical Spectroscopy Review λ = wavelength ν = frequency V = velocity = ν x λ = 2.998 x 10 8 m/sec = c (in a vacuum) ν is determined by source and does not change as wave propogates, but V can change
More informationChemistry 311: Instrumentation Analysis Topic 2: Atomic Spectroscopy. Chemistry 311: Instrumentation Analysis Topic 2: Atomic Spectroscopy
Topic 2b: X-ray Fluorescence Spectrometry Text: Chapter 12 Rouessac (1 week) 4.0 X-ray Fluorescence Download, read and understand EPA method 6010C ICP-OES Winter 2009 Page 1 Atomic X-ray Spectrometry Fundamental
More informationvery high temperature for excitation not necessary generally no plasma/arc/spark AAS
Atomic Absorption Spectrometry (Chapter 9) AAS intrinsically more sensitive than AES similar atomization techniques to AES addition of radiation source high temperature for atomization necessary flame
More informationCompact Knowledge: Absorbance Spectrophotometry. Flexible. Reliable. Personal.
L A B O R A T O R Y C O M P E T E N C E Compact Knowledge: Absorbance Spectrophotometry Flexible. Reliable. Personal. The interaction of light with molecules is an essential and well accepted technique
More informationReflection = EM strikes a boundary between two media differing in η and bounces back
Reflection = EM strikes a boundary between two media differing in η and bounces back Incident ray θ 1 θ 2 Reflected ray Medium 1 (air) η = 1.00 Medium 2 (glass) η = 1.50 Specular reflection = situation
More informationUltraviolet-Visible and Infrared Spectrophotometry
Ultraviolet-Visible and Infrared Spectrophotometry Ahmad Aqel Ifseisi Assistant Professor of Analytical Chemistry College of Science, Department of Chemistry King Saud University P.O. Box 2455 Riyadh 11451
More informationATOMIC ABSORPTION SPECTROSCOPY (AAS) is an analytical technique that measures the concentrations of elements. It makes use of the absorption of light
ATOMIC ABSORPTION SPECTROSCOPY (AAS) is an analytical technique that measures the concentrations of elements. It makes use of the absorption of light by these elements in order to measure their concentration.
More informationA Spectrophotometric Analysis of Calcium in Cereal
CHEM 311L Quantitative Analysis Laboratory Revision 1.2 A Spectrophotometric Analysis of Calcium in Cereal In this laboratory exercise, we will determine the amount of Calium in a serving of cereal. We
More informationThe Fundamentals of Spectroscopy: Theory BUILDING BETTER SCIENCE AGILENT AND YOU
The Fundamentals of Spectroscopy: Theory BUILDING BETTER SCIENCE AGILENT AND YOU 1 Agilent is committed to the educational community and is willing to provide access to company-owned material. This slide
More information1901 Application of Spectrophotometry
1901 Application of Spectrophotometry Chemical Analysis Problem: 1 Application of Spectroscopy Organic Compounds Organic compounds with single bonds absorb in the UV region because electrons from single
More informationClinical Chemistry (CHE221) Professor Hicks Week 1. Statistics Made Slightly Less Boring and Introduction to Spectrophotometry. Accuracy vs Precision
Clinical Chemistry (CHE221) Professor Hicks Week 1 Statistics Made Slightly Less Boring and Introduction to Spectrophotometry 3 Accuracy vs Precision Precision is the consistency of a measurement made
More informationtwo slits and 5 slits
Electronic Spectroscopy 2015January19 1 1. UV-vis spectrometer 1.1. Grating spectrometer 1.2. Single slit: 1.2.1. I diffracted intensity at relative to un-diffracted beam 1.2.2. I - intensity of light
More informationPRINCIPLE OF ICP- AES
INTRODUCTION Non- flame atomic emission techniques, which use electrothermal means to atomize and excite the analyte, include inductively coupled plasma and arc spark. It has been 30 years since Inductively
More information2001 Spectrometers. Instrument Machinery. Movies from this presentation can be access at
2001 Spectrometers Instrument Machinery Movies from this presentation can be access at http://www.shsu.edu/~chm_tgc/sounds/sound.html Chp20: 1 Optical Instruments Instrument Components Components of various
More informationChem 321 Name Answer Key D. Miller
1. For a reversed-phase chromatography experiment, it is noted that the retention time of an analyte decreases as the percent of acetonitrile (CH 3 CN) increases in a CH 3 CN/H 2 O mobile phase. Explain
More informationa. An emission line as close as possible to the analyte resonance line
Practice Problem Set 5 Atomic Emission Spectroscopy 10-1 What is an internal standard and why is it used? An internal standard is a substance added to samples, blank, and standards. The ratio of the signal
More informationAtomic Absorption Spectroscopy and Atomic Emission Spectroscopy
Atomic Absorption Spectroscopy and Atomic Emission Spectroscopy A. Evaluation of Analytical Parameters in Atomic Absorption Spectroscopy Objective The single feature that contributes most to making atomic
More informationlevels. The signal is either absorbance vibrational and rotational energy levels or percent transmittance of the analyte
1 In this chapter, absorption by molecules, rather than atoms, is considered. Absorption in the ultraviolet and visible regions occurs due to electronic transitions from the ground state to excited state.
More informationAtomic Absorption & Atomic Fluorescence Spectrometry
Atomic Absorption & Atomic Fluorescence Spectrometry Sample Atomization Atomic Absorption (AA) Atomic Fluorescence (AF) - Both AA and AF require a light source - Like Molecular Absorption & Fluorescence,
More informationUltraviolet-Visible and Infrared Spectrophotometry
Ultraviolet-Visible and Infrared Spectrophotometry Ahmad Aqel Ifseisi Assistant Professor of Analytical Chemistry College of Science, Department of Chemistry King Saud University P.O. Box 2455 Riyadh 11451
More informationPRINCIPLES OF AAS atomization flame furnace atomization absorption
INTRODUCTION Atomic absorption spectroscopy (AAS) currently is the most widely used of atomic spectroscopic techniques. AAS is a quantitative method of elemental analysis that is applicable to many metals
More informationINTRODUCTION TO OPTICAL ATOMIC SPECTROSCOPY (Chapter 8)
INTRODUCTION TO OPTICAL ATOMIC SPECTROSCOPY (Chapter 8) Atomic spectroscopy techniques: Optical spectrometry Mass spectrometry X-Ray spectrometry Optical spectrometry: Elements in the sample are atomized
More informationAtomic Absorption Spectroscopy
CH 2252 Instrumental Methods of Analysis Unit IV Atomic Absorption Spectroscopy Dr. M. Subramanian Associate Professor Department of Chemical Engineering Sri Sivasubramaniya Nadar College of Engineering
More information24 Introduction to Spectrochemical Methods
24 Introduction to Spectrochemical Methods Spectroscopic method: based on measurement of the electromagnetic radiation produced or absorbed by analytes. electromagnetic radiation: include γ-ray, X-ray,
More informationCourse: M.Sc (Chemistry) Analytical Chemistry Unit: III
Course: M.Sc (Chemistry) Analytical Chemistry Unit: III Syllabus: Principle of spectrophotometry Types of spectrophotometer Applications - Dissociation constants of an indicator simultaneous spectrophotometric
More informationChapter 15 Molecular Luminescence Spectrometry
Chapter 15 Molecular Luminescence Spectrometry Two types of Luminescence methods are: 1) Photoluminescence, Light is directed onto a sample, where it is absorbed and imparts excess energy into the material
More informationAbsorption spectrometry summary
Absorption spectrometry summary Rehearsal: Properties of light (electromagnetic radiation), dual nature light matter interactions (reflection, transmission, absorption, scattering) Absorption phenomena,
More informationChemistry 524--Final Exam--Keiderling May 4, :30 -?? pm SES
Chemistry 524--Final Exam--Keiderling May 4, 2011 3:30 -?? pm -- 4286 SES Please answer all questions in the answer book provided. Calculators, rulers, pens and pencils are permitted. No open books or
More informationCOMPARISON OF ATOMIZERS
COMPARISON OF ATOMIZERS FOR ATOMIC ABSORPTION SPECTROSCOPY Introduction Atomic spectroscopic methods are all based on the interaction of light and analyte atoms in the gas phase. Thus, a common component
More informationCh 313 FINAL EXAM OUTLINE Spring 2010
Ch 313 FINAL EXAM OUTLINE Spring 2010 NOTE: Use this outline at your own risk sometimes a topic is omitted that you are still responsible for. It is meant to be a study aid and is not meant to be a replacement
More informationQuestions on Instrumental Methods of Analysis
Questions on Instrumental Methods of Analysis 1. Which one of the following techniques can be used for the detection in a liquid chromatograph? a. Ultraviolet absorbance or refractive index measurement.
More informationAnalytical Technologies in Biotechnology Prof. Dr. Ashwani K Sharma Department of Biotechnology Indian Institute of Technology, Roorkee
Analytical Technologies in Biotechnology Prof. Dr. Ashwani K Sharma Department of Biotechnology Indian Institute of Technology, Roorkee Module - 6 Spectroscopic Techniques Lecture - 2 UV-Visible Spectroscopy
More informationSpectrophotometry. Introduction
Spectrophotometry Spectrophotometry is a method to measure how much a chemical substance absorbs light by measuring the intensity of light as a beam of light passes through sample solution. The basic principle
More informationAnalytical Chemistry II
Analytical Chemistry II L4: Signal processing (selected slides) Computers in analytical chemistry Data acquisition Printing final results Data processing Data storage Graphical display https://www.creativecontrast.com/formal-revolution-of-computer.html
More informationAtomic absorption spectroscopy
Atomic absorption spectroscopy Modern atomic absorption spectrometers Atomic absorption spectroscopy (AAS) is a spectroanalytical procedure for the quantitative determination of chemical elements using
More informationSkill Building Activity 2 Determining the Concentration of a Species using a Vernier Spectrometer
Skill Building Activity 2 Determining the Concentration of a Species using a Vernier Spectrometer Purpose To use spectroscopy to prepare a Beer s Law plot of known dilutions of copper(ii) sulfate so that
More informationChapter 4 Scintillation Detectors
Med Phys 4RA3, 4RB3/6R03 Radioisotopes and Radiation Methodology 4-1 4.1. Basic principle of the scintillator Chapter 4 Scintillation Detectors Scintillator Light sensor Ionizing radiation Light (visible,
More informationFinal Exam. Physical Constants and Conversion Factors. Equations
Final Exam Instructions: This exam is worth 100 points. Some questions allow a choice as to which parts are answered. Do not answer more parts than are requested. velocity of light in a vacuum: 3.0x10
More informationOverview of Spectroscopy
Overview of Spectroscopy A. Definition: Interaction of EM Radiation with Matter We see objects because they remit some part of the light falling on them from a source. We function as reflection/ transmission
More informationChem 434 Instrumental Analysis Test 1
Chem 434 Instrumental Analysis Test 1 Name: 1. (15 points) In Chapter 5 we discussed four sources of instrumental noise: Thermal Noise, Shot Noise, Flicker Noise, and Environmental noise. Discuss the differences
More informationChemistry 311: Topic 2 - Atomic Spectroscopy Topic 2: Spectroscopy:
Topic 2: Spectroscopy: Introductory Theory Basic Components Qualitative and Quantitative applications Atomic Spectroscopy Molecular Spectroscopy Electromagnetic Radiation : Wave-Particle Duality Light
More informationDesign and Development of a Smartphone Based Visible Spectrophotometer for Analytical Applications
Design and Development of a Smartphone Based Visible Spectrophotometer for Analytical Applications Bedanta Kr. Deka, D. Thakuria, H. Bora and S. Banerjee # Department of Physicis, B. Borooah College, Ulubari,
More informationModel Answer (Paper code: AR-7112) M. Sc. (Physics) IV Semester Paper I: Laser Physics and Spectroscopy
Model Answer (Paper code: AR-7112) M. Sc. (Physics) IV Semester Paper I: Laser Physics and Spectroscopy Section I Q1. Answer (i) (b) (ii) (d) (iii) (c) (iv) (c) (v) (a) (vi) (b) (vii) (b) (viii) (a) (ix)
More informationChapter 8: An Introduction to Optical Atomic Spectrometry
Chapter 8: An Introduction to Optical Atomic Spectrometry Sample is atomized (gaseous atoms/ions) absorption or emission measured Optical Atomic Spectra Atomization Methods Sample Introduction Methods
More informationAtomic Absorption Spectroscopy (AAS)
Atomic Absorption Spectroscopy (AAS) Alex Miller ABC s of Electrochemistry 3/8/2012 Contents What is Atomic Absorption Spectroscopy? Basic Anatomy of an AAS system Theory of Operation Practical Operation
More informationSpectrophotometric Determination of Iron
Spectrophotometric Determination of Iron INTRODUCTION Many investigations of chemical species involve the interaction between light and matter. One class of these investigations, called absorbance spectrophotometry,
More informationMolecular Luminescence Spectroscopy
Molecular Luminescence Spectroscopy In Molecular Luminescence Spectrometry ( MLS ), molecules of the analyte in solution are excited to give a species whose emission spectrum provides information for qualitative
More informationBeer's Law and Data Analysis *
OpenStax-CNX module: m15131 1 Beer's Law and Data Analysis * Mary McHale This work is produced by OpenStax-CNX and licensed under the Creative Commons Attribution License 2.0 1 Beer's Law and Data Analysis
More informationChem Homework Set Answers
Chem 310 th 4 Homework Set Answers 1. Cyclohexanone has a strong infrared absorption peak at a wavelength of 5.86 µm. (a) Convert the wavelength to wavenumber.!6!1 8* = 1/8 = (1/5.86 µm)(1 µm/10 m)(1 m/100
More informationLecture 0. NC State University
Chemistry 736 Lecture 0 Overview NC State University Overview of Spectroscopy Electronic states and energies Transitions between states Absorption and emission Electronic spectroscopy Instrumentation Concepts
More information09/05/40 MOLECULAR ABSORPTION METHODS
MOLECULAR ABSORPTION METHODS Absorption spectroscopy refers to spectroscopic techniques that measure the absorption of radiation, as a function of wavelength ( absorption spectrum ), due to its interaction
More informationUNIT I COLORIMETER AND SPECTROPHOTOMETERS PART A
UNIT I COLORIMETER AND SPECTROPHOTOMETERS PART A 1. List any four elements used in spectrophotometers. 1.Radiant source 2.wavelength selector 3.photodetector 4.sample 2. What is meant by flame emission
More informationMASTERING THE VCE 2014 UNIT 3 CHEMISTRY STUDENT SOLUTIONS
MASTERING THE VCE 2014 UNIT 3 CHEMISTRY STUDENT SOLUTIONS FOR ERRORS AND UPDATES, PLEASE VISIT WWW.TSFX.COM.AU/VCE-UPDATES QUESTION 45 QUESTION 46 Answer is A QUESTION 47 The number of protons in the element.
More informationSpectroscopy of Atoms and Molecules
CHEM 121L General Chemistry Laboratory Revision 2.1 Spectroscopy of Atoms and Molecules Learn about the Interaction of Photons with Atoms and Molecules. Learn about the Electronic Structure of Atoms. Learn
More information