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Sample questions Test 3 1. Circle the correct response. a. A three electrode potentiostat is used to apply two voltages simultaneously to the same working electrode to measure both the current and the resistance simultaneously to eliminate the voltage measurement error that can occur at high currents to eliminate errors in measuring currents in solutions of low resistance b. Measurement with an ion selective electrode is an example of potentiometry voltametry conductometry c. coulometry In ICP-AES the species detected is an unexcited neutral atom, a neutral atom or ion in an exited electronic state, an ion in the ground state, an atom or ion in the ground electronic state d. Which of the following techniques has the lowest detection limits? flame AA flame emission electrothermal AA ICP AES e. Which of the following techniques is NOT routinely used for simultaneous mutli-element analysis? arc emission ICP-MS ICP-AES AA spectroscopy f. In which of the following methods is the concentration of the analyte is determined from the Nernst Equation. potentiometry coulometry voltametry conductometry g. Which technique is most useful for determining the chemical nature of a molecule on a surface Auger electron XPS X-ray lectron spectroscopy fluorescence microprobe h. Chemical interference is not a serious problem in a plasma as compared to a flame because a plasma has more ions than a flame a plasma has fewer ions than a flame a plasma is much hotter than a flame a plasma is much cooler than a flame i. Mercury is commonly used as an electrode because mercury has a high overpotential for the reduction of hydrogen ions in the solvent mercury has a high density mercury is the least reactive metal mercury is easily reduced j. This technique is generally only used for the analysis of alkali metals ICP-MS differential pulse flame emission polarography k. Beam (or source) modulation is used in flame AA and flame AE to reduce the effects chemical interferences eliminate interferences caused by emissions from the flame eliminate ionization interferences 1 flame absortion Sample questions Test 3 increase the intensity of the source l. Which of the following techniques would be least useful for determining a trace amount of tin in a sample of a metal? x-ray differential pulse ICP-AES AA fluorescence polarography m. For which of the following surface techniques is it sometimes possible to detect adsorbates at part per billion levels XPS SIMS Auger electron microprobe n. What is detected in ICP-MS ions in the plasma radiation from ions in the plasma atoms in the plasma radiation from atoms in the plasma o. In which of the following methods is the voltage scan preceded by a concentration phase polarography anodic differential pulse cyclic stripping polarography voltametry p. Which of the following types of probe beams can be used for high resolution surface imaging with little surface damage He ion Ar ion electron X-ray q. In which techniques are electrons used as a probe and X-rays are detected x-ray fluorescence XPS electron microprobe Auger r. Which of the following is NOT a type of voltametry (differential pulse polarography, anodic stripping, pH measurement, square wave polarography) s. Which tecnique tends to be more sensitive to high molecular weight atoms. XRF spectroscopy Auger electron ESCA spectroscopy t. In which of the following techniques is the sample completely destroyed ? differential pulse coulometry potentiometry polarography SIMS polarography u. In which of the following electrochemical methods is the determination of concentration based on diffusion controlled migration of analyte conductometry polarography pH measurement coulometry v. The charging current in polarograhy is due to undesired ions in solution, the electrical double layer around the electrode, concentration polarization, overpotential 2 Sample questions Test 3 w. In which one of the following the sample is probed with X-rays and the electron emitted are analyzed. XPS Auger the electron XRF spectroscopy microprobe x. Which technique is used for simultaneous analysis and identification of multiple ions potentiometry coulometry voltametry conductometry y. A(n) (auger, photo-, thermal, free) electron is created in a two electron process in an atom. An upper level electron in an atom that is missing a core electron drops to a lower level to fill the hole and simultaneously a valance electron is ejected. z. Which of the following techniques is not used for simultaneous multielement analysis? flame AA ICP-MS ICP-AES arc emisson aa. Which is FALSE about Atomic Absorption Spectroscopy? The sensitivity for various atoms differs significantly Hollow cathode lamps are used as sources Flame AA has lower detection limits than electrochemical furnace AA The energies of the transitions are in the UV-visible region bb. Give the following two half reactions and reduction potentials, what is the spontaneous reaction and what is the cell voltage 2+ Zn + 2e- → Zn(s) Eo = -0.763 Ni2+ + 2e- → Ni(s) Eo = -0.250 2+ Zn + Ni(s) → Ni2+ + Zn(s) Eo = 0.513 V Zn2+ + Ni(s) → Ni2+ + Zn(s) Eo = -0.513 V Ni2+ + Zn(s) → Zn2+ + Ni(s) Eo = 0.513 V Ni2+ + Zn(s) → Zn2+ + Ni(s) Eo = -0.513 V cc. Which of the following is most useful for determining the chemical structure of an unknown molecule ? Auger electron spectroscopy X-ray diffraction electron microprobe Atomic force microscope dd. Which of the following is most useful for determining the atomic composition of a surface with micrometer resolution? X-ray flourescence X-ray diffraction electron microprobe Scanning tunelling microscope 2 Briefly answer the following questions. a. Why is the surface concentration of an electroactive species often different from the bulk concentration? 3 Sample questions Test 3 b. Why is ultra high vacuum needed for most surface analysis techniques. c. What is overpotential and what is its source? d. How are electrons analyzed and detected? e. How are X-rays analyzed and detected? 3. For each technique indicate what is measured (current, voltage, current vs. voltage, current vs. time, etc.). Also give an example of an application of each technique. measured application coulometry differential pulse polarography potentiometry 4. Describe briefly how you could analyze the following samples. Indicate the instrumental technique or techniques that you will use and what information you expect from each technique. Indicate if any sample preparation or separation is likely to be needed. Assume that all instrumental techniques are available to you. a. Test for Pb in a soil sample. These are expected to be present at the ppb level. b. Quickly determine the composition of a metal ore with a precision of 10 %. c. Determine the Ca and Mg content of some grains. 4 Sample questions Test 3 d. Determine the thickness of a thin diamond film that has been deposited on a metal surface.. e. Test a cleaning solution for several metals and non metals simultaneously. 5 (6 ) Give a typical application for each of the following X-ray fluorescence XPS SIMS scanning tunneling microscopy 5