Making Physical Measurements Terry A. Ring Department of Chemical Engineering University of Utah 22 August 2005 OVERVIEW • Course experiments – general approach to making physical measurements • Terminology • Calibration • Types of Instruments • Class Participation Experiments • Preparation for an experiment - organization – teamwork - time management • Equipment/apparatus - keep detailed list of equipment/chemicals - know your equipment/capabilities - most equipment expensive, do not abuse or neglect Important Terms • Error – the difference between the “true value” and the observed (measured) value • Random error – fluctuations in the measured value due to repeated measurements • Systematic error – all measured values are off by the same amount due to a) incorrect calibration b) faulty equipment c) other causes • Illegitimate error – erroneous method/technique, goofs Random Error Sources • Judgement errors, estimate errors, parallax • Fluctuating Conditions • Digitization • Disturbances such as mechanical vibrations or static electricty caused by solar activity • Sampling Systematic Error Sources • Calibration of instrument • Environmental conditions different from • • calibration Technique – not at equilibrium or at steady state. Sampling 2 2 Total sampling measuremen t Important Terms • Accuracy - a measure of how close the result • • comes to the “true value” (correctness). An indication of how well we control systemic errors. Precision – a measure of how exactly the result is determined (reproducibility) – no relation to “true value”. An indication of how well we overcome or analyze random errors Limit of detection – smallest value which can be detected. Important Terms • Discrepancy – the difference between values for the same measurement • Uncertainty – an estimate of the range in the error. Always determined for a particular confidence level, i.e. y y y (95% confidence level ) Experiments • Literature work • - understand theory/principles/concepts from textbooks and references References - textbook - Perry’s chemical engineers handbook - CRC handbook of chemistry/physics - Instrument Engineers’ Handbook- process measurement and analysis – B.G. Liptak, ed. - Web sites Potential Problems • Paralax • Scale Interpretation • Appropriate Scale • Appropriate Instrument – Appropriate detection limits – Signal to Noise ratio – Appropriate Accuracy and Precision • Significant Figures WHAT PRECISION IS REQUIRED? • Overall Precision • Impact on Calculation • Difficulty of Measurement Calibration • • Should use primary standards if possible Calibrate as close to measuring conditions as possible Sometimes performed at • • • • – – the factory Professional laboratories Laboratory standards ice bath, constant temp bath Tabulated properties and relationships boiling water at barometric pressure triple point of water Linear vs Non-linear Calibration curves Types of Instruments • Off-line Process Instrumentation • Density Measurement • Weight and Misc. Sensors • Analytical Instrumentation – Issues • Sampling Quantitative – Grab sample – Statistical Sampling • Sample Preparation – Splitting, extraction, decomposition • On–line Instrumentation – – – – – Flow Measurement Level Measurement Temperature Measurement Pressure Measurement Safety Liquid Density Measurement • Hydrometers (based upon buoyancy) • Pycnometer (based on weight) • Weighing a fixed volume • Oscillating Coriolis Densitometers • Hydrostatic Densitometers • Radiation Densitometers – liquid/sludge • Vibrating Densitometers – Liq/sludge/gas Analytical Instrumentation • Viscometers • Spectrophotometers • • • • • – IR – UV-Visible Chromatographs Ion-selective Electrodes Mass Spectrometers Inductively Coupled Plasma Spectrometer Many, many more Types of Analysis • Content Analysis – What is in it? – Qualitative – Semi-Quantitative – Quantitative • Distribution Analysis – Where is it? • Process Analysis – When does it occur? • Structural Analysis –What is its structure? Analytical Strategies • • • • Sampling Sample Preparation Analytical Principle Analytical Procedure – Decomposition Methods – Separation Methods – Enrichment Methods • Measurement Methodology • Measurement Results – Accuracy – Precision CONCLUSIONS KNOW YOUR EQUIPMENT Know its limitations and strengths CHOOSE THE RIGHT PRECISION CALIBRATE AS MUCH AS POSSIBLE UNDERSTAND THE LIMITATIONS OF YOUR EQUIPMENT LEARN THE TERMINOLOGY Audience Participation