Chapter 1

1 What was done by the classical method of gravimetric analysis? In gravimetric measurements, the mass of the analyte or some compound produced from the analyte was determined 2 What was done by the classical method of volumetric analysis? In volumetric, also called titrimetric, procedures, the volume or mass of a standard reagent required to react completely with the analyte was measured 3 What are instrumental methods? Newer methods than classical methods for separating and determining chemical species such as chromatographic and electrophoretic techniques, light absorption or emission, mass-tocharge ratio, fluorescence, conductivity, and electrode potential 4 In an instrument for analysis, what is the stimulus? The stimulus is usually in the form of electromagnetic, electrical, mechanical, or nuclear energy that elicits a response from the system under study. 5 In an instrument for analysis, what is the system under study? The system under study is the unknown variable or sample being analyzed 6 In an instrument for analysis, what is the response? The response is the analytical information 7 What are data domains? Data domains are the various modes of encoding information, data domains may be broadly classified into nonelectrical domains and electrical domains 8 What are nonelectrical domains? Measurement process that begin and end in nonelectrical domains. The physical and chemical information that is of interest in a particular instrument does not use electrical devices to obtain a result 9 What are electrical domains? Modes of encoding information as electrical quantities that can be subdivided into analog domains, time domains, and the digital domain. 10 What are some examples of output transducers? Voltmeters, alphanumeric displays, electric motors, computer screens, and many other devices that serve to convert data from electrical to nonelectrical domains 11 What are analog-domain signals? Information in the analog domain is encoded as the magnitude of one of the electrical quantities - voltage, current, charge, or power 12 What are time-domain signals? Information that is stored in the time domain as the time relationship of signal fluctuations
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13 What is digital-domain signal? Data encoded in the digital domain in a two-level scheme. The information can be represented by the state of a lightbulb, a light-emitting diode, a toggle switch, or a logical-level signal. The characteristic that these devices share is that each of them must be in one of only two states (ON or OFF) 14 What is a detector? A detector is a mechanical, electrical, or chemical device that identifies, records, or indicates a change in one of the variables in its environment such as pressure, temperature, electrical charge, electromagnetic radiation, nuclear radiation, particulates, or molecules. 15 What is a transducer? Devices that convert information in nonelectrical domains to information in electrical domains and the converse. Examples include photodiodes, photomultipliers, and other electronic photodetectors 16 What is a sensor? A sensor is an analytical device that is capable of monitoring specific chemical species continuously and reversibly. Examples are glass electrode, ion-selective electrodes, oxygen electrodes, and fiber-optic sensors 17 What is a readout device? A readout device is a transducer that converts information from an electrical domain to a form that is understandable by a human observer: a series of numbers on a digital display, the position of a pointer on a meter scale, etc 18 What are the two types of comparison with standards? Direct comparison Titrations 19 Describe direct comparison of standards Direct comparison of standards involves comparing a property of the analyte (or the product of a reaction with the analyte) with standards such that the property being tested matches or nearly matches that of the standard 20 Describe titration comparison of standards Titrations are among the most accurate of all analytical procedures. In a titration, the analyte reacts with a standardized reagent (the titrant) in a reaction of known stoichiometry. The amount of standardized reagent needed to achieve chemical equivalence can then be related to the amount of analyte present 21 Describe external-standard calibration An external standard is prepared separately from the sample. External standards are used to calibrate instruments and procedures when there are no interference effects from matrix components in the analyte solution. External standards allow for the creation of a calibration curve 22
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What are some errors in external-standard calibration? Blank, ideal blank, reagent blank, solvent blank, standards prepared incorrectly, chemical form of standard incorrect, decomposition of standards 23 Describe standard-addition methods One of the most common standard addition methods involves adding a standard solution to sample aliquots containing identical volumes. Measurements then can be made on the original sample and on the sample plus the standard after each addition. Standard addition methods are useful for analyzing complex samples in which matrix effects are likely 24 Describe the internal-standard method A substance is added in a constant amount to all samples, blanks, and calibration standards in an analysis. The ratio of the signals of the analyte and the internal standard are used. The internal standard should provide a signal that is similar to the analyte signal in most ways but sufficiently different so that the two signals are distinguishable by the instrument 25 Defining the problem To select an analytical method intelligently, it is essential to define clearly the nature of the analytical problem 26 What are the questions to be answered when defining a problem? 1. What accuracy is required? 2. How much sample is available? 3. What is the concentration range of the analyte? 4. What components of the sample might cause interference? 5. What are the physical and chemical properties of the sample matrix? 6. How many samples are to be analyzed? 7. Speed? 8. Ease and convenience? 9. Cost and availability of equipment? 10. Cost per sample? 27 What are the numerical criteria for selecting analytical methods? 1. Precision 2. Bias 3. Sensitivity 4. Detection limit 5. Dynamic range 6. Selectivity 28 What are the criteria to be considered for precision? The precision of analytical data is the degree of mutual agreement among data that have been obtained in the same way. Precision provides a measure of the random, or indeterminate, error of analysis. Absolute standard deviation, relative standard deviation, coefficient of variation, variance 29 What are the criteria to be considered for bias?
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Bias provides a measure of the systematic, or determinate, error of an analytical method. Determining bias involves analyzing one or more standard reference materials whose analyte concentration is known. Absolute systematic error, relative systematic error 30 What are the criteria to be considered for sensitivity? A measure of its ability to discriminate between small differences in analyte concentration. Calibration sensitivity, analytical sensitivity 31 What is calibration sensitivity? Calibration sensitivity is the slope of the calibration curve at the concentration of interest. The calibration sensitivity as a figure of merit suffers from its failure to take into account the precision of individual measurements 32 What is analytical sensitivity? Analytical sensitivity takes into account the precision of individual measurements. The analytical sensitivity offers the advantage of being relatively insensitive to amplification factors 33 What is the detection limit? Minimum concentration or amount that can be detected at a known confidence level: Sm = Sbl + ksbl where Sm is the minimal distinguishable analytical signal, Sbl is the mean blank signal, sbl is the standard deviation of the blank, and k is the arbitrary multiple. The figure of merit is blank plus three times standard deviation of the blank 34 What is the dynamic range? The applicable range in which we plot concentration vs response. extends from the lowest concentration (LOQ) limit to the highest concentration (LOL) limit 35 What is LOQ? Limit of quantitation which is the lowest concentration at which quantitative measurements can be made 36 What is LOL? Limit of linearity at which the calibration curve departs from linearity by a specified amount 37 What is selectivity? Selectivity of an analytical method refers to the degree to which the method is free from interference by other species contained in the sample matrix. Coefficient of selectivity 38 What is a figure of merit? Quantitative instrument performance criteria that can be used to decide whether a given instrumental method is suitable for attacking an analytical problem