The Calibration of Weights and Balances Edwin C Morris Kitty MK Fen Monograph 4: NMI Technology Transfer Series Third Edition National Measurement InstituteThis monograph combines and updates two earlier CSIRO publications: The Calibration of Balances by David B Prowse, first published in 1985, and Balances and Weighing by Edwin C Morris, first published in 1992. Monographs ‘Monograph 1: Uncertainty in Measurement: The ISO Guide Monograph 2: Statistical Background to the ISO Guide to the Expression of ‘Uncertainty in Measurement ‘Traceable Measurements The Calibration of Weights and Balances ‘Thermocouples in Temperature Measurement : The Measurement of Electrical Quantities Pressure Measurement Humidity and its Measurement Liquid-in-Glass Thermometry ‘Monograph 10: Introduction to Radiometry Monograph 11: Platinum Resistance Thermometry Monograph 12: Radiation Thermometry Details of the monographs are given on NMI’s website ‘National Measurement Institute Bradfield Road, Lindfield, NSW 2070 PO Box 264, Lindfield, NSW 2070 (61 2) 8467 3796 (61 2) 8467 3849 hitp:/Awww.measurement.gov.att First edition — March 2002 Second edition — October 2002 Third edition — November 2003, June 2004, February 2005, June 2006, March 2007 © Commonwealth of Australia, 2002 Cartoons by Christophe Granet: Copyright Hagen Cartoons 2002Contents Chapter 1 Ll Chapter 2 21 2.2 2.3 24 25 Chapter 3 3.1 3.2 3.3 34 3.5 3.6 3.7 Chapter 4 4.1 4.2 43 44 4.5 Chapter 5 5.1 5.2 53 Chapter 6 6.1 6.2 63 64 6.5 66 Introduction Outline of the book.. Air buoyancy and conventional weighin; Air buoyancy Conventional weighing Definition of conventional mass. Buoyancy correction for conventional mass. Measurement of true mass for volume or density determination .. Mass calibration by direct comparison... Introduction . Substitution weighing. Extended substitution weighing Checking mass measurements Measuring balance sensitivity. Measuring the repeatability of mass comparison Examples Mass calibration using weighing schemes... Introductio1 Weighing schemes. Analysis of weighing schemes... Examples of weighing scheme analysis A simple scheme for a 5,3,2,1,1' decad Uncertainty estimation for mass calibration Introduction ... ‘Uncertainty of direct comparison ‘Uncertainties for weighing schemes. Calibration of electronic balances .... What is an electronic balance? The scope and purpose of the calibration . Balance calibratio Recording and reporting the results of an electronic balance calibration Using a calibrated balance... ‘Measuring corrections to balance reading when a full set of calibrated weights is not availabl 3 4. IS 5S 6 2 9 iiiChapter 7 Calibration of single-pan, two-knife-edge balances... 7.1 What is a single-pan two-knife-edge balance? 7.2 The scope and purpose of the calibration 73 Balance calibratior 7.4 Recording and reporting the resul 7.5 Using the calibrated balance... 7.6 Measuring corrections to dial readings using the comprehensive tolerance test .. 85 7.7 Measuring corrections to dial readings using a least-squares calibration Chapter 8 — Balance calibration uncertainties. 8.1 Electronic balances.. 8.2. Single-pan two-knife-edge balances. Definitions and Symbols... Appendix A. Use of balances AJ Environment. A2 Laboratory practic Appendix B. Use and handling of weights. Bl B2 B3 Care of weights.... B.4_ Estimation of the OIML class for old and/or special weight 119 120 120 121 Appendix C Traceability of Australian mass standards... Appendix D Least-squares analysis of weighing schemes. ‘Appendix E Least-squares calibration of weights installed in balances... El Numerical example... Appendix F_ Sample report for the calibration of weights .. Appendix G Statistical tests G.l_ The t-test... 141 G2 Anexample of the te 142 G3 The F-test... 142 G4 Examples of the F-test.Appendix H Air density measurement.. H.1 Air density equation... 2145 H.2 Measurements of temperature, humidity and pressu Appendix I Mass and density limits for the OIML classification of weights Appendix J. Buoyancy uncertainty in mass calibration... 153 Appendix K A brief outline of balance construction K.1 Electronic balances.. K2_ Single-pan, two-knife-edge balances. 153 154 157 157 159 AppendixL An introduction to uncertainty calculation . Ll Uncertainty calculatio: L.2 Rounding of results. Appendix M Resolution and the measurement of repeatabili Bibliography... Index.Acknowledgements ‘The authors received a good deal of useful input and suggestions from several members of the National Measurement Institute and the National Association of Testing Authorities. In particular, we would like to thank Robin Bentley, Ian Bentley and Max Purss. False scales are an abomination to the Lord, but a just weight is His delight. Proverbs 11:1 viChapter 1 Introduction In one form or another weighing is widely used in industry and commerce. For these measurements it is important to know the accuracy of the balances used, together perhaps with other information such as corrections to be applied to readings. Responding to this need, the CSIRO published Zhe Calibration of Balances by DB Prowse [1] in 1985 as a guide to good laboratory practice in this field. Standard weights with high precision calibrations must be available for the accurate and traceable calibration of balances as well as for legal metrology. A CSIRO technical memorandum Balances and Weighing by EC Morris [2] was published in 1992 to cover the techniques required for the calibration of standard weights. Since these two publications first appeared some major revisions have become necessary, and the present publication addresses this. Although mass metrology has its roots in quite ancient times, the development of balances proceeded’ slowly until the 1950s, At that time, two-pan beam balances were still most commonly used for analytic (moderate precision) and high precision measurement. Since then they have been progressively replaced, firstly by the single-pan two-knife-edge balance and more recently by electronic balances. The more accurate electronic balances use electromagnetic foree compensation (EFC), which balances part or all of the gravitational force on the object being weighed with an electromagnetic force. For lower accuracy requirements, balances using strain gauge transducers (load cells) are common and have the adventage of greater robustness. Over the last 30 years, single-pan two-knife-edge balances have in turn been largely replaced by the electronic kind (both EFC and strain gauge), which are now approaching total dominance of laboratory benches. Two-pan balances have become obsolete and, with very few exceptions, are relegated to dusty storerooms or displayed for purely aesthetic reasons. Other mechanical scales are still sometimes used for larger masses but are likewise being replaced. Over the same period, the quality of weights has also improved, though less dramatically. There are standards, most notably OIML R 111-1 [3], which specify every relevant characteristic (density, surface finish, magnetic susceptibility, shape, etc) so that a user can know what to expect from weights of a given class.2 THE CALIBRATION OF WEIGHTS AND BALANCES Recently, all branches of metrology have benefited greatly from the widely accepted ISO Guide to the Estimation of Uncertainty in Measurement [4]. At the same time, the development of quality systems has been greatly accelerated by the advent of the ISO 9000 series of standards [12], and the ISO/IEC 17025 [13] laboratory competence standard is now a reeognised guide to good laboratory practice, These developments have emphasised the need for proper uncertainty analysi This publication takes these developments into account while combining the two earlier publications referred to above. Most of the earlier material has been included here, a notable exception being the chapter on two-pan balances from The Calibration of Balances. Once again certain areas are not specifically mentioned, including the calibration and testing of weighing devices used for trade, large capacity weighing devices such as platform scales, weighbridges, some types of load-cell systems and some mechanical scales with an analog readout. However the techniques presented here should be applicable in some form to all these areas. There are two approaches to mass measurement, depending largely on the required accuracy. In the first approach, measurements of relatively high accuracy, such as those usually needed for the calibration of weights, are carried out using substitution weighing, This involves using a balance to measure only the very small mass difference between a reference weight and the weight to be calibrated. As a result, nothing needs to be known about the balance apart from its sensitivity and standard deviation (repeatability), both of which may vary with load. Tssues such as linearity, hysteresis, calibration of balance weights and even off-centre loading are normally irrelevant. Substitution weighing is not restricted to calibrating weights and may be used whenever a very accurate result is required. It is always necessary however for the combined mass of the reference weights to be nearly equal to that of the object being weighed to minimise dependence on balance characteristics, With the second approach, one notes the balance’s zero reading z with the pan empty, and the reading r with the object to be weighed on the pan. If these readings are in mass units, the mass of the object is then taken to be rz. This procedure is easier but generally less accurate than the first approach. As full use is now being made of the balance, it is necessary that it be calibrated if only to allow an estimate of uncertainty. A correction C, obtained from the balance calibration report, may be applied so that the measured mass becomes r—z+C. In this case, an accuracy approaching that of substitution weighing may be possible. As the first approach demands relatively little knowledge of the balance and is usually used for the calibration of weights, it is described in the chapters on mass calibration. Using the second approach, the mass measurement is relatively straightforward, but the characteristics of the balance are important. It is therefore discussed in the chapters on balance calibration.CHAPTER 1. INTRODUCTION 3 1.1 Outline of the book Chapter 2 deals with issues such as air buoyancy and conventional mass, which are important for all aspects of mass metrology. ‘The remaining chapters deal with mass calibration (Chapters 3 to 5) and balance calibration (Chapters 6 to 8) respectively. More detailed or more specialised material is given in appendices; Chapter 3 is concerned with mass calibration by direct comparison, which is the most widely used method. Note that the measurements of balance repeatability and sensitivity described here differ from those required for balance calibration. Chapter 4 desoribes the use of weighing schemes for mass calibration. For the same number of weights, the schemes require more measurements than direct comparison but give a more accurate and more consistent result, They also allow easier checks on errors in the readings or balance defects. Chapter 5 covers the estimation of uncertainty in mass calibration. Chapters 6 and 7 deal with the calibration of electronic balances and single-pan two-knife-edge balances respectively. Following the pattern of The Calibration of Balances, these chapters are very largely self-contained, though some cross-references to the other parts of the book are inevitable. Both chapters give a description of the tests, examples of the tests, a sample report form based on the examples, and a basic guide to using a calibrated balance. The calculation of uncertainties associated with balance calibration is summarised briefly in Chapters 6 and 7, and is dealt with in much greater detail in Chapter 8.THE CALIBRATION OF WEIGHTS AND BALANCES Sometimes buoyancy can be neglected, but sometimes large errors are introduced if it is overlooked.Chapter 2 Air buoyancy and conventional weighing 2.1. Air buoyancy Balances are normally thought of as instruments that compare masses, but balances of all kinds compare force rather than mass. Suppose, for instance, that the readings of a balance are exactly the same for a test weight J’ as they are for a reference weight 2. The common interpretation is that 7'and R have exactly the same mass, but strictly speaking we know only that the net downward force on the balance pan is the same for Yas it is for R. If the masses of the weights are my and me, then the equality of these forces means that: myg+X, =mgg +X, @1) where g is the acceleration due to gravity. Here mg and mag are the gravitational forces acting on the two weights, while X; and Xe are the sums of all other vertical forces acting on them. Only if these other forces are negligible or equal does equation (2.1) reduce to: My = My (22) Most of the other forces (e.g, stray magnetic forces, or forces resulting from air currents) can be made negligible by careful laboratory management or balance design. However the buoyancy force due to immersion in air can be removed only by weighing in a vacuum, and this is usually quite impractical. Moreover buoyancy is a relatively large force; for light materials such as wood it exceeds 0.1% of the gravitational force. Since air buoyancy cannot be eliminated, it must be taken into account somehow, even in weighings of quite modest accuracy. Assuming that air buoyancy alone contributes to Xp and Xp, we can calculate these quantities by applying Archimedes’ principle, which states that the buoyancy force on an object is equal to the weight of air displaced by the object: my mp 2 —— and Xp =—-P,V RB =—P, Pr * " Pr6 THE CALIBRATION OF WEIGHTS AND BALANCES where po is the density of air, pr and V;-are the density and volume of the test weight, and op and Vp are the density and volume of the reference weight, The minus signs indicate that buoyancy is an upward force. Substituting these equations in equation (2.1), we obtain: (23) Equation (2.3) is the basis of all buoyancy calculations associated with weighing. In very accurate weighings, such as a comparison of national secondary standards of mass with a platinum-iridium primary standard, the buoyancy corrections shown in brackets in equation (2.3) have to be determined as accurately as possible. This means that the densities of the weights must be measured if they are not already known. The density of the air in the balance case during the weighing also has to be measured either directly or indirectly. It is usually not too difficult to measure the densities of the weights with sufficient accuracy, but measuring the air density can pose severe problems. 2.2 Conventional weighing In well equipped laboratories, the densities required for buoyancy corrections can be measured if necessary. In the community at large however, such measurements are generally impractical. Fortunately, the accuracy required of mass comparisons in commerce, industry, and even most scientific research is not especially high so that buoyancy can be dealt with in a way that hardly ever requires the knowledge of densities. This is done by using a weighing convention that is known by several names, including © conventional weighing; © mass on the 8.0 basis; . apparent mass; © weighing in air; and © conventional value of the result of weighing-in-air For the sake of brevity, the convention is referred to in this book as conventional weighing, and the result of a conventional weighing is called the conventional mass. When discussing conventional weighing, mass as normally defined is sometimes called true mass in order to distinguish it from conventional mass'. The symbols m and Af are used here for true and conventional mass respectively. ‘Throughout the world, conventional weighing is used for almost all mass measurement. Event in national institutes of metrology such as the National Measurement Institute, it is used most of the time. From the point of view of most users, conventional weighing simply means that whether one is calibrating weights, calibrating balances or weighing machines, or weighing some commodity, one makes no allowance for air buoyancy, As will be scen below, this neglect of buoyancy is made possible by requiring all mass standards used in conventional ’ Hence true mass is a measure of an object’s resistance to acceleration, or equivalently, true mass determines the gravitational force experienced by an object.CHAPTER 2. AIR BUOYANCY AND CONVENTIONAL WEIGHING. 7 weighing to have densities that lie within prescribed limits. (Nevertheless a buoyancy correction may still be necessary at high altitudes or for mass measurements of unusually high accuracy: see section 2.4.) Conventional mass differs significantly from the corresponding true mass (see Table 2.1), but this does not matter, as most people are not interested in true mass. They want only a widely accepted convention that will yield consistent weighings without the need for difficult buoyancy corrections and that gives mass values reasonably close to true mass, Table 2.1: The difference (in parts per million) between conventional mass, M, and true mass, m, For an object with a density of 8000 kg.m™, conventional mass is equal to true mass. Material Density (kgm) [| (A¢—m/in (ppm) Platinum 21400 94 Lead 11300 “4 Brass 8400 7 ‘Aluminium 2700 295 Water 1.000 1050 Cork 250 -4700 2.3 Definition of conventional mass It follows from equation (2.3) that the relative error E that will result if buoyancy is ignored in a weighing is given (to a very good approximation) by E=p, ( -4) (2.4) Pr Pr Equation (2.4) shows that if the density of the test weight is equal to that of the reference weight, the buoyancy error is zero. The need for buoyancy corrections in the calibration of weights could therefore be eliminated by requiring all weights to have a certain standardised density such as 8000 kg.m™. Unfortunately it is not possible to ensure that all weights have a density of exactly 8000 kg.m°, or any other value, We can however require that the density be close enough to the standard value that the resulting buoyancy correction can be ignored in most weighings without significant error. Hence weights satisfying this condition can be treated as having a density exactly equal to the standard value. It is with these considerations in mind that conventional mass is defined as follows: The conventional mass of an object is equal to the true mass of a weight of density 8000 kg.m? which at a temperature of 20°C balances the object in air of density 1.2 kgm’.8 THE CALIBRATION OF WEIGHTS AND BALANCES Note that the definition applies to any object, not just weights. The specified air density of 1.2 kg.m™ was chosen because this value is typical for air-conditioned laboratories near sca evel and the temperature of 20°C takes account of thermal expansion, but for weights the temperature is not at all critical. Stainless steel and similar alloys have densities close to 8000 kg.m™, which explains the choice of this density in the definition. The OIML recommendation covering mass standards [3] gives tables showing how close to 8000 kg.m® the densities of weights must be (see Appendix I). In effect, if a weight used in conventional weighing has a relative maximum permissible error of ¢ parts per million, then it must have a density p in kg.m™ lying within the range: 8000, < 8000 es) wt = 60 60 (if 2 60, then only the lower limit is relevant). If the density lies in this range, then the weight can be considered to have a density of exactly 8000 kg.m", This in turn makes it possible for us to verify a hierarchy of mass standards according to the above definition of conventional mass”, For an object of density and true mass m, it follows from equation (2.3) that the conventional mass M is given by: (e-1.2)m M 0.99985 e9 2.4 Buoyancy correction for conventional mass For measurements of relatively high accuracy, one may still need to add a buoyancy correction to a measured conventional mass, particularly at higher altitudes where the air density is significantly less than 1.2 kgm". The need arises mostly in the calibration of weights, and seldom for other mass measurements. Even for weight calibration, a buoyancy correction is unlikely to be required at altitudes below 300m. Near sea level, the correction may be necessary only for weights with densities lying well outside the OIML limits or for very accurate mass measurements of light materials. 2 Strictly speaking, if the density of a test weight satisfies equation (2.5), then when the weight is compared with 2 standard of density 8000 kg.m™, a variation in the air density of 10% above or below the value of 1.2 kgm” does not lead to a variation in the result of the comparison exceeding 4/4 ppm. It follows that if we simply ignore the buoyancy correction in this comparison (equivalent to taking the density of the test weight to be 8000 kg.m’), then the measured conventional mass of the test weight will be in error by no more than 2/4 ppm.CHAPTER 2. AIR BUOYANCY AND CONVENTIONAL WEIGHING 9 For substitution weighing (in which a test weight or other object is directly compared with a reference weight 2 of the same nominal mass, see Chapter 3), the buoyancy correction is given by: aM =(p, taf a Qn Pa where 2, is the air density at the time of the weighing, pis the density of the test weight (or other object), px is the density of the reference weight, and dM is to be added to the measured conventional mass M of the test weight (or other object) in order to obtain the correct conventional mass, Notice that the buoyancy error in substitution weighing is zero if the air density is equal to 1.2 kg.m™ or if the test and reference weights have the same density. For mass_measurement with a calibrated single-pan_two-knife-edge balance, the buoyancy correction is again given by equation (2.7), where pp is the density of the inbuilt weights of the balance. In most cases, ag can be taken to be 8000 kg.m° if it is not known. For mass measurement with a calibrated electronic balance, the buoyancy correction is given by: om [2512 eae es) 2 Pe where p, is the air density when M is measured, p,(cal) is the air density at the time the balance was calibrated and pp is the density of the reference weights used to calibrate the balance. In most eases, e can be taken to be 8000 kg.m’ if it is not known, If in doubt about the need for a buoyancy correction, substitute likely values of the densities into equation (2.7) or (2.8) to estimate the likely correction. For both 9, and p,(cal), use the mean value of air density for the altitude of the laboratory, see Table J.1, and if pp is not known, assume a value of 8000 kg.m™. If the estimated correction is significant compared with the desired uncértainty, then an accurately determined correction will need to be applied. To calculate dM accurately, p must be known (by measurement, from reference tables, or as information supplied by a manufacturer) while both g, and ,(cal) may need to be measured (see Appendix H). For the more accurate substitution weighings pr should be known, but otherwise it may be taken as 8000 kg.m™. None of these densities needs to be known particularly accurately; an expanded uncertainty of 1% would almost always be quite adequate.10 THE CALIBRATION OF WEIGHTS AND BALANCES 2.5 Measurement of true mass for volume or density determination Sometimes it is necessary to measure the true mass of an object or liquid sample. Since density is defined as the true (not conventional) mass per unit volume, this mostly occurs in measurements involving the density of relatively light materials such as water. Two common instances are: . measurement of the density of a liquid or the volume of a container; and . using Archimedes” principle (hydrostatic weighing) to measure the density of a liquid or a solid sample. If Archimedes’ principle is not used, one can simply make conventional mass measurements (corrected for buoyancy if necessary) and use equation (2.6) to obtain the true mass from the conventional mass. When using Archimedes’ principle, the measurements are usually analysed using a variant of equation (2.3): 2. mp) 1-2 |e mg| 12 22 2.9) ( é] ( Pr } where p, is the density of the liquid in which the test object is immersed when it is balanced against reference weight(s) of conventional mass Mz. The quantity My is the apparent mass of the immersed object and it may be obtained from substitution weighing or simply read off a calibrated balance. (In either case, a buoyancy correction may needed.) Therefore the densities Pr, and pz must be known, as must the true mass mr of the test object, the true mass mp corresponding to Mp and either , or pr. Fortunately, no significant difficulty is raised by this, except for very accurate (£0.002%) density or volume measurements, First of all, ar may be taken as 8000 kg.m’® and hence the true mass mg will be equal to the conventional mass Mp. Secondly, p can be calculated from a well known formula (see Appendix H) using air temperature and pressure measurements of quite modest accuracy (41K and +500 Pa) with the relative humidity taken as 50%. (For measurements of modest accuracy, 2, can be obtained from Table J.1.) Usually pp will be known or easily calcutated with sufficient accuracy, but on rare occasions it may be necessary to obtain it by iteration. Having measured Mr separately, one then calculates ‘my from equation (2.6). Finally, as either p, or pr is known, the other may be calculated.Chapter 3 Mass calibration by direct comparison 3.1 Introduction This chapter deals with the calibration of weights. For this task, substitution weighing is strongly recommended, as it is for the very accurate mass measurement of any object. The principal advantage of substitution weighing is that one need not be concemed with balance characteristics such as linearity, corrections to readings, masses of in-built weights, hysteresis, etc. Therefore one need not calibrate the balance for these characteristics nor worry that they may be drifting with time. The only quantities that must be known are the balance sensitivity and repeatability of mass comparison, both of which may vary with load, Another important advantage is a much clearer line of traceability for mass standards. A requirement of substitution weighing is that the test weight or object must be compared with a mass standard or group of standards of nearly the same mass, For weights this means that the test and reference weights should be nominally equal. For other objects, mass equality to within approximately 0.02% is recommended where possible. ‘Throughout this chapter and the next, the buoyancy correction (see section 2.4) will not be mentioned; it will be assumed that the observer makes the correction where necessary. The observer should also be familiar with the basic rules for handling balances and weights, which are detailed in Appendices A and B. Techniques for minimising the effects of a drift in balance readings are mentioned several times in what follows, but the observer should nevertheless do whatever is possible to minimise the drift itself. The causes are often linked to temperature, for instance a large variation in laboratory temperature, using a balance during its warm-up period, or using weights that are not in thermal equilibrium with the balance. See Appendix A for further information.12 THE CALIBRATION OF WEIGHTS AND BALANCES 3.2 Substitution weighing Simple substitution weighing consists of the following three steps and is the minimum that is required to determine the mass Mr of the test weight in terms of the mass Mr of the reference. The quantities r, t) etc. are balance readings to be noted at the indicated point of the procedure, Some balances need to be arrested except when taking readings. @ Place the reference weight R on the pan of the balance, 7). Gi) Remove R from the pan and place the test weight Ton the pan, f;. (iii) Remove 7 from the pan, ‘Two extra weighings in reversed order are often added, leading to the five steps shown below. This group of four weighings is called double substitution weighing or just double weighing. Provided the time intervals between the readings are approximately equal, double weighing will largely eliminate the effect of drift in the readings. (The weighing sequence 7, R, R, Tis equally acceptable.) (i) Place the reference weight X on the pan of the balance, 7). (i) Remove & from the pan and place the test weight F'on the pan, f7. Gil) Move T well off the pan and then place it back on the pan, f. (iv) Remove 7’from the pan and place R on the pan, r2. (¥) Remove R from the pan. Notice that it is not necessary to zero the balance before one commences the weighings, though one may do so. Indeed, for single-pan two-knife-edge balances it is often necessary to offset the zero slightly before one starts (to give a small positive reading with the pan empty) to avoid the pointer running off the scale. Once the reading 7, has been taken, the balance must not be tared or zeroed, nor should any tare weights or built-in weights be moved. Some balances have a high resolution range (with ten times the normal resolution) covering perhaps one-fifth the total range of the balance, and sometimes the high resolution range can, by retaring, be moved anywhere throughout the load range of the balance. In such cases one may take advantage of the higher resolution by retaring the balance after placing weight R on the pan in step (i). ‘The first two weighings give: My, =My+S(t,-7) G1) and from the last two: M, =M,+S(t,-) (3.2) where S is the sensitivity reciprocal, defined as the mass of a small weight added to the pan of the balance divided by the resulting change in the balance reading (see section 3.5). (For a well adjusted balance, S should be very nearly equal to 1.) From these equations, the mean value of ‘Mr obiained from double weighing is: M,=M, +S +t, B.3)CHAPTER 3. MASS CALIBRATION BY DIRECT COMPARISON 13 3.3 Extended substitution weighing Extended substitution weighing consists of repeating a double weighing two or more times to give the readings: a 2 G4) where 7 is an even number”. The measured mass of T is: My = My +3940) = Mgt 65) > where (fr) is the mean value of the measured mass differences (1, r)). Once again, weights should be lifted well off the pan between readings and the time intervals between readings should be approximately equal within each group of four. Extended weighing reduces the uncertainty of the mass comparison and also allows the repeatability of mass comparison 5, of the balance (see section 3.6) to be determined (see Example 3.7.2). The value of sq, so obtained can be compared with previous determinations of Sn (see section 3.4) as a check on the measurement. 3.4 Checking mass measurements A measurement of M; using simple substitution or double weighing may be sufficient to give the mass value with the desired uncertainty, but it is advisable to check measurements to ensure that no error has been introduced. This is particularly so for simple substitution as a single measurement can easily contain an undetected operator error. For this reason, simple substitution is not recommended for direct comparison calibration and should be used only in weighing schemes (see Chapter 4) that include a measurement check. ‘The simplest check is to compare the results from each half of a double weighing; in other words, to compare S(t, —r,) with S(¢—72). These two quantities should differ by no more than 3.25», where Sn is the repeatability of mass comparison for the balance (see section 3.6). For the more critical calibrations, some kind of check weighing is recommended. Two approaches to check weighing are mentioned here: (a) The mass of a check weight C is measured at regular intervals using the same balance and reference weight as the measurements to be checked. A record of the measured mass values Mc is kept, and ideally the record should contain at least 5 previous measurements. ‘The results are analysed using a t-test (see Appendix G, where the quantity Q in section G.1 becomes Mc). An example is given in section G.2. * In the absence of significant drift, n could be odd.14 THE CALIBRATION OF WEIGHTS AND BALANCES (b) The repeatability of mass comparison sy for the balance (at one or more loads) is determined in the course of mass measurements by carrying out extended substitution weighing. Alternatively s, could be measured separately from the measurements to be checked, as described in section 3.6. For the purpose of the check, at least one previous sy measurement is needed, though a record of several recent measurements is better. If the latest value obtained for s,, is significantly greater than the earlier ones, the operator is alerted to a possible problem, To determine whether an increase in balance repeatability is significant, the F-test is used. See Appendix G for details. Sec also the first example in section G.4. Should check (a) or (b) fail (ie. the value of ¢ or’F is too large), then a potential problem is indicated and must be investigated. Points to consider are: * The balance. Has it been allowed to warm up properly? Has its performance deteriorated? * Laboratory conditions. Ate there large temperature variations or air-conditioning problems? Is the relative humidity reasonably steady in the range 40 to 60% relative humidity? * The weights, including the reference. Are they free of dust etc and at the same temperature as the balance? For check (a), itis possible that weight C has drifted and there may be nothing wrong with the measurements being checked. ©) The operator. Is the operator new to this work? Has something been overlooked or a reading taken incorrectly? ‘None of these checking procedures is perfect. False positive and false negative indications are both possible. 3.5 Measuring balance sensitivity Once the balance has been adjusted at the location where it is to be used, the sensitivity reciprocal § of a modern balance usually remains close to unity. Any variation with time or with load is normally insignificant for substitution weighing. For such balances § need not be measured very frequently; once per year should be sufficient. Some balances may need to be checked more often, and it is up to the operator to choose a frequency based on the history of the instrument. Where there is no history, the sensitivity should be measured on the first three occasions that the balance is used. The sensitivity reciprocal can be measured by adding a small weight of mass Mjeys to the balance pan after the last weighing of a sequence. Alternatively, separate weighings may be carried out in the following way: (i) place weight 4 of mass Mj on the pan, r1; (ii) add the sensitivity weight Ming 72CHAPTER 3. MASS CALIBRATION BY DIRECT COMPARISON 15 Weight 4 must not be touched between the weighings, nor should any built-in or tare weights be moved after reading 7, has been taken. The balance may need to be arrested while placing A on the pan, but do not arrest the balance when the sensitivity weight is added. The sensitivity reciprocal at load M, is given by: G.6) where 4, =[44— Ideally Mune should be at least 20 times larger than the largest mass difference AM likely to be measured on the balance (see section 5.2.1). (Example: If a 1 kg balance is used to calibrate F; and F; weights, then Mens should be at least 20 times the maximum permissible error of 15 mg for a Fy kilogram, i.e. Myx, should be at least 300 mg.) A mass in the range 20 to 200 times AM is probably best. For single-pan two-knife-edge balances however, Myns cannot exceed the range of the optical scale. Since S does not have to be accurately known, variations with load of a few percent are often permissible for the calibration of standard weights. Modern balances usually show much less variation than this, so S will normally have to be measured at only one load, such as half maximum load. 3.6 Measuring the repeatability of mass comparison For substitution weighing, the repeatability of mass comparison 5», is the standard uncertainty associated with a single mass comparison S(t, —7;}, see equations (3.1), (3.3) and (3.5). Note that a different expression of balance standard deviation, called the repeatability of measurement 5, is used in Chapters 6, 7 and 8. Normally the repeatability of mass comparison s, is measured every six months, but the balance history and usage may lead an operator to choose a period as Jong as a year or as short as a week. The need for a measurement is indicated whenever odd or inconsistent results are obtained. The repeatability must be measured and recorded as it contributes to the overall uncertainty of mass measurements. One can obtain a value of s» from a set of measurements, such as an extended substitution weighing (see the example in section 3.7.2), or it can be measured separately from any mass measurement. The latter course is recommended unless the balance is used very infrequently (less than once in six months). Whichever approach is used, s» should be based on at least ten measurements of mass difference unless the accuracy required for mass measurement is very easily obtained from the balance. Five measurements are recommended as a minimum.16 THE CALIBRATION OF WEIGHTS AND BALANCES To measure s» separately, place a weight on the pan, note the reading, and then remove the weight (arresting the balance as required). Do this 20 times to obtain the readings r1, r2, rs, watz Calculate the 10 mass differences: =SMrr-r2), = SMes~ 7), = SMrs— 10), + 5a = S19 720) and find the standard deviation s of these quantities. If the time intervals between the readings are the same, s will not be affected by a moderate drift. ‘The measured standard deviation s usually provides a good value for the standard uncertainty and hence the repeatability, in which case one could simply equate s,, to s. However, balances are sometimes resolution-limited — they give the same reading many times when the same weight is placed on the pan — and for such balances s may not be a good value fors, ‘As a consequence of this, proceed as follows: If a is the resolution semi-range of the balance, then 5,, is equal to s (with nine degrees of freedom), or equal to 0.82a (with 1000 degrees of freedom), whichever is the greater. (See Appendix M for a brief discussion of resolution and its effect on the measurement of balance repeatability.) The example in Section 3.7.3 below illustrates this procedure. Note: The standard deviation s of m quantities 5), 5, ... 5, can be calculated from either of the two formulae: [G-a -5} G.Ta) (3.70) where 7 is the number of measurements of 5(10 in the above example), and 5 is the mean value of the §. For most modem balances, it would be sufficient to measure the repeatability of mass comparison at maximum load only. Even if a consistent variation were discovered, it should seldom be necessary to measure s,, at more than half load and maximum load. (In this case adopt the half-load value up to half load, and the full-load value beyond that.) When obtaining s,, from an extended substitution weighing, it is very desirable that drift be eliminated from the balance readings or twice as many weighings will be required to achieve nine degrees of freedom. * Inthe absence of noticeable drift, complete 10 mass comparisons (7 = 10 in equation 3.5) and calculate the standard deviation s of the mass differences S(t, — 7).CHAPTER 3. MASS CALIBRATION BY DIRECT COMPARISON 7 . If drift is an unavoidable problem, carry out 20 mass comparisons and combine the differences in pairs to give 10 quantities such as the second term on the right-hand side of equation (3.3). Take s to be the standard deviation of these quantities multiplied by 2. This value of s will have nine degrees of freedom. For the reason given above, 5, is then calculated as follows: If @ is the resolution semi-range of the balance, then as above, s,, is equal to s (with nine degrees of freedom), or equal to 0.82a (with 1000 degrees of freedom), whichever is the greater. 3.7. Examples 3.7.1 Double substitution weighing and sensitivity check An E, reference weight R has a mass of 1000.001 1 g. It is used to calibrate a F; test weight 7 and the following balance readings are obtained (after taring at 1000 g): 7 0.0009 g ty 0.0003 g & ~0,0002g vr 0.0010g Since the sensitivity of the balance has not been checked for some time, a sensitivity weight having a mass of 0.019 955 g is then placed on the balance (without moving the reference after noting reading r) to give the reading 0.020 9 g. From equation (3.6), the sensitivity reciprocal is given by: 0.019955 0.0209 — 0.0010 = 1.0028 and since the permissible uncertainty for a sensitivity reciprocal is a few percent when calibrating standard weights, S will be taken as exactly 1.0, From equation (3.3) one then finds: M,, =1000.0011 + (—0,0003 — 0.0002 — 0,0009 — 0,0010)/2 =1000.001 1 -0.0012 = 999.9999 g 3.7.2 Extended substitution weighing and a calculation of repeatability of mass comparison A weight 7 is calibrated against a reference R having a mass of 19.999 94 g. Extended substitution weighing is used with the following results, in grams: Fy 199.999 89 rs 199,999 87 ts 199.999 90 t 200,000 25 ts 200.000 25 & 200.000 27 t; 200.000 27 t, 200.000 22 % 200.000 27 rz 199,999 92 Tx 199.999 89 % 199.999 9018 THE CALIBRATION OF WEIGHTS AND BALANCES From equation (3.5), taking S'to be 1: M,, =199.99994 +£(0.00036 +0.000 35 + 0.000 38 + 0.000 33 + 0.00037 + 0.00037) = 199.999 94 + 199.999 94 +0.000 36 = 200.000 30 ¢ 0.00216 6 Since the drift in the readings is very small, one can calculate the repeatability of mass comparison from the six mass differences 0.000 36, 0.000 35, 0.000 38, 0.000 33, 0.000 37 and 0.000 37 g, The mean mass difference has already been found to be 0.000 36 g, so the six quantities (5, —5) to be substituted into equation (3.7a) are: 0.0 0.000 01 0.000 02 0.000 03 0.000 01 0,000 01 g ‘The resulting standard deviation s is 0.000 018 g, Since this is greater than 0.82a (which is 0.000 004 1 g), we take s,, = s = 0.000 018 g, with five degrees of freedom. 3.7.3 Repeatability of mass comparison (s») The repeatability of mass comparison for a 1 kg balance (with S'= 1) is measured at full load by placing the same weight on the pan 20 times. The readings, in grams, obtained after taring at 1 kg are: 0.0006 0.0007 0.0006 0.0004 0.0007 0.0006 0.0006 0.0008 0.0008 0.0008 0,0007 0.0008 0.0009 0.0008 0.0008 0.0010 0.0009 0.0008 0.0009 0.0009 There seems to be a slight drift in the results, but provided the readings are taken at equally spaced intervals, this does not matter when the standard deviation is measured by using the mass differences 4}, 6, ete shown in section 3.6. The mass differences are: 0.0001 0.0002 0.0001 -0.0002 0.0000 -0.0001 0.0001 -0.0002 0.0001 0.000 0 The mean is -0.000 01 and the standard deviation calculated from equation (3.7a) is 0.000 14 g. Since this is greater than 0.82c (which is 0.000 041 g), we take 5» = 0.000 14 g, with nine degrees of freedom.Chapter 4 Mass calibration using weighing schemes 41 Introduction A weighing scheme consists of several mass comparisons carried out using the techniques of Chapter 3. Three or more weights are involved, at least one of which must be a reference while one (or more) may be a check weight. The rest will be test weights. Weighing schemes are the norm for class E; calibrations, optional for E2 and F, calibrations, but are not normally used for class F) and below. In general, schemes have several advantages: (a) @) © @ For a set of weights, a more consistent calibration will result. Some schemes make very little use of reference weights, thereby giving them some protection from mass changes due to usage. Indced it is possible to calibrate ah entire set of weights using just one reference, Checking the measurements is easier. It is normal, for instance, to incorporate a check weight (see section 3.4) in the scheme. This may allow the use of single substitution weighing, at least halving the number of readings per mass comparison. Some schemes give a value for a quantity such as the balance repeatability of mass comparison 5, Which can be used to check the weighings using a statistical test (see section 3.4 and Appendix G). However there are also some potential disadvantages: @ ) ©) It is sometimes necessary to place several weights on the balance pan. This may be tricky and the operator may have to be careful to avoid error due to off-centre loading, More mass comparisons may be necessary (compared with direct comparison) to calibrate the same number of test weights. The analysis of a weighing scheme to obtain the test masses and their uncertainties is generally quite complicated and must be done by computer. However modern spreadsheet programs can perform this task quickly and easily. Such a program can be prepared using instructions given later in this chapter. In most circumstances, one may choose between schemes and direct comparison, but for two situations weighing schemes must be used:20 THE CALIBRATION OF WEIGHTS AND BALANCES (@) calibrating the masses of the in-built weights of most single-pan two knife-edge balances (see Appendix E); (&) calibrating a set of weights when one has only one reference weight. 4.2 Weighing schemes Over the years, a large number of schemes have been proposed by many authors, but only three are described in detail here. The Closed Cycle is mostly used for calibrating two test weights (or one test and one check weight) in terms of a single reference, where all three weights have the same nominal mass. The Simple Decade and the Extended Decade schemes are for calibrating weights belonging to a weight set. ‘The mass comparisons that make up the schemes are listed below using equations such as: A+B=C+Dt+E+a @p This equation indicates that weights A and B (as a group) are compared with weights C, D and E (asa group) to obtain the mass difference a. To measure a, one uses substitution weighing as desoribed in sections 3.2 and 3.3, where R now stands for the group C+ D + E, while T stands for the group A + B. Thus, equation (3.5) may be rewritten: = Muy ~Mesnes =S0-7) @2) 4.2.1 Closed cycle The closed cycle belongs to a family of weighing schemes designed for weights of nominally equal mass. The version given in equations (4.3) shows a single reference and two test weights. However weight 7; could be a check weight. R=T +a T=T+a (43) Th=Rt+a; Ideally, 2a = a; + a) + a; would be zero, so the magnitude of this quantity, referred to as “Sum a’, provides an immediate check on the measurements (see Chapter 5 for further details).CHAPTER 4. MASS CALIBRATION USING WEIGHING SCHEMES 21 The simplicity of the closed cycle allows the masses Adr; and Mrp of the test weights to be calculated from reasonably simple equations: Mp = Mp* (2ay + a2 + a3)/3 (4:4a) Mrz = My (-ay— a2 + 2ayy3 (4.40) (cf. equations D.7), Alternatively the spreadsheet described in section 4.3 could be used to calculate the test masses. If 7; is a check weight, the mass Mrz would be used to check the outcome of the cycle as described in section 3.4. 4.2.2. Simple decade and extended decade In weight sets, the weights are grouped into decades, such as 5,2,2',1; 5,2,1,1'; 5,3,2,1 ete, where 5, for instance, may stand for a 5 kg, 500 g, 50 g, ... or 5 mg weight depending on the decade in question. The following discussion applies to the 5,2,2',1 and 5,2,1,1' structures as ‘these are by far the most common. Note: A prime’ is used to indicate a second weight having the same nominal mass as another weight of the decade. Thus a 5,2,2',1 decade contains two weights of nominal mass 2. Tn decade weighing, the test weights are not compared directly with weights from a reference set. Instead, a weight from the test set called the head weight acts as the reference weight. ‘Apart from the head weight and test weights, a decade normally includes a cheek weight. The head weight of a decade is the smallest weight of the next decade up; thus 100 g is the head weight of the 50 g to 10 g decade. The check weight is an additional weight that is added to make the decade up to 5,2,2'1,1’. For the 5,2,2',1 structure, the check weight would be a 1’ weight. The head weight normally belongs to the same set as the weights being calibrated, while the check weight is from some other set. The mass of the head weight must be known in advance, as it is effectively the reference weight for the decade. To see how decade weighing may be used to calibrate a complete set of weights, it is best to consider an example. Suppose a set of test weights has the 5,2,2',1 structure and extends from 20 kg to 1 mg. Since the 20 kg and 10 kg weights do not form a complete decade they must be measured by direct comparison or by a closed-cycle scheme. In either case they are compared with weights from a reference set. The 10 kg test weight then becomes the head weight for the calibration of the 5 kg to 1 kg decade. The check weight for this decade is any suitable 1 kg weight. After the 5 kg to 1 kg calibration is complete, the 1 kg test weight becomes the head weight for the next decade, and 80 on. Notice that, once the 10 kg test weight has been calibrated, the reference set is no longer needed (unless the check weights are taken from it).22 THE CALIBRATION OF WEIGHTS AND BALANCES ‘The simple and extended decades are given by equations (4.5) and (4.6) respectively: 10 =5+24+2'+1 tay 5 +2741" ta 2 tay (45) a o=1d) +4 1 =r tas 10 =54+2+2'+1 +a 10° =5+24+24+1 +a 5 =242'+1 tay $ =24241 tay 46) 241 21 +as 240 =2 41 +45 2 =1t1 tay vo sit tag where 10 is the head weight and either 2’ or 1’ is the check weight. Mass values for the test weights are obtained by analysing the available data, which consist of the quantities a, to a, or a; to ag, plus the mass value of the head weight. For the simple decade, this gives five equations in five unknowns, so mass values for the test and check weights may be obtained from the solution of simultaneous equations. For the extended decade, there are eight equations in five unknowns (i.c. three degrees of freedom). In such cases, the mass values that best fit the data must be determined. 43 Analysis of weighing schemes Weighing schemes are best analysed using a spreadsheet program, and this section gives instructions for writing such a program, These instructions are for EXCEL, so some formulae may need modification for other spreadsheet programs. No attempt is made to justify or explain the mathematics except to the very limited extent that is necessary for writing the program. The instructions are thus intended for the reader with a reasonable understanding of spreadsheet programming, but not necessarily any understanding of matrix algebra or linear regression. For readers wishing to know more, the mathematical background to what follows is given in Appendix D. Figure 4.1 shows how the lefi-hand side of the spreadsheet could be set out. (Readers may choose their own lay-out, but if it is not the same as that shown in Figures 4.1 and 4.2, some of the cell addresses used in formulas given below may need to be modified.) The closed cycleCHAPTER 4. MASS CALIBRATION USING WEIGHING SCHEMES 23 scheme is used in this illustration in order to fit it conveniently on to a page, but similar lay- outs are easily devised for decade schemes, see section 4.3.1 for details. Cells C19, C20, D19, D20, E19, £20, C23 and C25 contain formulas (given below) and the indications ‘0’ and “#NUM!" are due to the fact that no input data has been entered. The entries in cells B25 and C25 are not relevant for closed cycles and should be omitted. (They are shown in Figure 4.1 because they are required for the extended decade scheme described later.) x z c Seis Rains Vans oeoronce nase Qf Siar aneariyofreerence ses (nh of eedon or reference mass wneerah Mass sonpareors ‘Comparison esol (value ofa] —| Standard oncertany | Baprens of Tesdon na) Ta a Tretasaz =Arat Dee st dew Gag) Figure 4.1: The left-hand side of a spreadsheet for analysing closed cycle weighing schemes. The input data are entered into the shaded cells of Figure 4.1. The mass of the reference weight Rwill be entered at E4 while the results of the three mass comparisons will be placed in D11, Di2 and D13. The standard uncertainties and corresponding degrees of freedom to be entered in E5, E6 and cells E11 to F13 will be discussed in Chapter 5. Here we are interested only in calculating the values of the test masses, not their uncertainties. This can be done by simply putting all the input uncertainties equal to 0,01 mg and all the degrees of freedom equal to 10. (Any reasonable values will do.) The right-hand side of the spreadsheet, shown in Figure 4.2, shows the arrays in which miost of the calculations are carried out. The array labelled X (shown in cells H3 to J6) is known as the design matrix as it describes the structure of the weighing scheme. The design matrix for a closed cycle is shown in Figure 4.2, while those for decade schemes are given in Tables 4.1 and 4.2.24 THE CALIBRATION OF WEIGHTS AND BALANCES This array should be named X. To do this, highlight cells H3 to J6, move the cursor into the name box (at the far left of the formula bar) and click, type the letter X, then press [Enter]. ‘The array Va has the same number of rows as columns, namely. the number of mass comparisons plus one. So Va is a4 x 4* array for a closed cycle. The quantity in cell L3 is the square of the standard uncertainty (i.e. the variance) of the reference mass, so enter the formula =E5/2 jin this cell. The other ceils down the diagonal of the array contain the variances of the mass comparisons, so enter =E11“2 in Md, =B12%2 in NS and =E13“2 in 06. Enter zero in every other cell of Va, Highlight the array and name it Va, using the procedure of the previous paragraph. The first quantity in array a is the mass of the reference weight in grams, so enter =E4 in cell HL. The lower cells contain the results of the mass comparisons in grams, so enter =D11/1000 in H12, =D12/1000 in H13 and =D13/1000 in H14, Name this array a. ea a ee = eu FeeaNUME >} @NOMI =| - aM “ENUM SND | Figure 4.2: The right-hand side of a spreadsheet for analysing closed cycle weighing schemes. ‘Array VM has 3 rows and 3 columns (for a closed cycle), and the formula to be entered in this array is: =MINVERSE(MMULT(TRANSPOSE(X), MMULT(MINVERSE(Va),X))) + Ay xz amay has y rows and z columnsCHAPTER 4. MASS CALIBRATION USING WEIGHING SCHEMES 25 but a special formula entry procedure is required: Firstly highlight the cells where the array is to be located (cells J11:L13 in this example). Then type the formula and press [Control] + [Shift] + [Enter]. (That is, press [Enter] while holding down [Control] and [Shift].) Name this array VM. Array V has 3 rows and 4 columns. The formula to be entered is: =MMULT(VM,MMULT(TRANSPOSE(X),(MINVERSE(Va))) and this is entered using the special procedure of the previous paragraph, Name this array V. Array M has 3 rows and the formula to be entered (using the special procedure) is: =MMULT(V,a).. Name this array M. Arrays Rs and SSR are not needed for @ closed eycle scheme. The remaining arrays are needed for calculating degrees of freedom using the Welch- Satterthwaite formula (see Chapter 5). Array Vu has the same number of rows and columns as V, and special care is required for entering this array as each column requires a different formula. Each column of Vu is found by multiplying the corresponding column of V by one of the input standard uncertainties and then raising this product to the fourth power. For the first column, the multiplying factor is the standard uncertainty of the reference mass; for the second column, it is the standard uncertainty of the first mass comparison; for the third column, it is the standard uncertainty of the second mass comparison, and so on. For the first column of Vu the formula is therefore =(E5*N11:N13)4 and it is entered using the special procedure, i.e. highlight the first column of Vu, type in the formula and press [Control] + [Shift] + [Enter]. For the remaining columns, formulas are =(E11*011:013)4, =(E12*PLI:P13)“4 and =(E13*QU1:Q13)4. Highlight all of Vu and name it Vu. Asray N has 4 rows and contains the reciprocals of the input degrees of freedom with =1/E6 entered in the first row, and =1/F1 1, =1/F12 and =1/F13 in the subsequent rows. Do not use the special procedure for entering these formulas. Name this array N. Array D has 3 rows and the formula to be entered (using the special procedure) is =MMULT(VuN). Array DF has 3 rows and each row is found by dividing the’ square of a diagonal element of VM by the corresponding row of D. Thus the formulas for DF, starting with the first row, are =J11/2/026, =K12°2/027 and =L13“2/028. Do not use the special procedure for entering these formulas. It is now possible to write the formulas required on the left-hand side of the spreadsheet. The first cell of array M (i.e, H19) gives the mass of the reference and hence should be equal to cell E4, The lower cells give the masses of the test weights. So enter the formula =H20 in cell C19, and =H21 in C20. The standard uncertainties of the masses of the test weights are the square~ roots of the diagonal elements of array VM, starting with the second. So enter the formula =SQRT(K12) in cell D19 and =SQRT(L13) in cell D20. The degrees of freedom for these standard uncertainties are in array DF, starting at the second row. So enter the formula =Q27 in cell B19 and =Q28 in cell E20. Finally, the formula for cell C23 is =SUM(D11:D13)..26 THE CALIBRATION OF WEIGHTS AND BALANCES Cells C19 and C20 should be formatted to show six figures after the decimal point, while cells D19 and D20 show four and cells E19 and £20 show none. The other cells in Figure 4.1 may be left unformatted. There is no need to format any cell in Figure 4.2, but the programmer may like to do so. 4.3.1. Adapting the spreadsheet to particular weighing schemes The spreadsheet described in section 4.3 is suitable for the closed cycle scheme, but may be readily adapted to any scheme with only one reference weight. For the decade schemes given in this chapter, the following modifications are needed. (This list should be read in conjunction with the instructions in section 4.3.) * The ‘Reference’ becomes the ‘Head weight’. * The ‘Mass Comparisons’ section is extended to show either five (simple scheme) or eight (extended scheme) comparisons. The entries in the ‘Comparison’ column would be taken from equation (4,5) or (4.6).. . The ‘Results’ section is extended to show five test masses (5, 2, 2', | and 1’) instead of Tland 12. . The ‘Sum a’ section is not required. The ‘Decade Std Devn’ section is required for the extended decade scheme only. © Amay Xisas given in Table 4.1 or Table 4.2. * Array Va is 6 x 6 cells (simple scheme) or 9 x 9 cells (extended scheme). The top left hand cell is the variance of the head weight. As for the closed cycle scheme, the other cells on the diagonal of Va are the variances of the mass comparisons, All other cells, in the array are zero. * Array a has six rows (simple scheme) or nine rows (extended scheme). The first row contains the mass of the head weight in grams while the other rows contain the results of the mass comparisons in grams. ‘Table 4.1: Design matrix X for the simple decade scheme. TiololTotoyo if -afpay-i yao oft a} 8 oj; o}il-ailolo ololotli fala ofofolfofif-—7 Table 4.2: Design matrix X for the extended decade scheme. 1 9 o 0 oO 0 fi falalat-ato slololo|-|—CHAPTER 4. MASS CALIBRATION USING WEIGHING SCHEMES 27 * For both schemes, array VM is 6 x 6 and contains the same formula as given in section 4.3. * Array V is 6x6 (simple scheme) or 6x9 (extended scheme) and contains the same formula as given in section 4.3. * For both schemes, M has six rows and contains the same formula as given in section 4.3, * The array Rs is not required for the simple scheme. For the extended scheme, it has nine rows and contains the formula: =MMULT(X,M)-a which is entered using the special procedure described in section 4.3 for array VM. Name this array Rs. * The quatity SSR is not required for the simple scheme. For the extended scheme, SSR is a single cell containing the formula: -MMULT(TRANSPOSE(RS),Rs) which is also entered using the special procedure described in section 4.3. * Array Vu is 6x6 (simple scheme) or 6x9 (extended scheme). For each column, the array formula to be entered is as described in section 4.3. However most cell addresses will inevitably be different to those given for the closed cycle scheme. If, for instance, the standard uncertainty of the second mass comparison is in cell B12 while the third column of V is in cells Q14:Q19, then the formula to be entered in the third column of ‘Vu is =(E12"Q14:Q19)4. * Array N has 6 rows (simple scheme) or 9 rows (extended scheme). As in section 4.3, the first row contains the reciprocal of the degrees of freedom for the head weight standard uncertainty, while the following rows contain the reciprocals of the degrees of freedom for each mass comparison in turn. * Forboth schemes, array D has 6 rows and contains the same formula as given in section 4.3. © Forboth schemes, array DF has 6 rows where each row is found by dividing the square of a diagonal element of VM by the corresponding row of array D (as in section 4.3, though most cell addresses will be different). . As for the closed cycle, array M contains the masses of the test weights, starting at the second row. Thus the second row shows the mass of the 5 weight, the third row shows the mass of the 2 weight, and so on. As in section 4.3, carry these five masses into the second column of the ‘Results’ section. . As for the closed cycle, the diagonal elements of array VM are the variances of the test weights, starting at the second diagonal element. So the second diagonal clement is the variance of the 5 weight, etc. As in section 4.3, carry the square-roots of these five diagonal elements into the third column of the ‘Results’ section. © Asfor the closed cycle, array DF (starting at the second row) contains the degrees of freedom required in the fourth column of the ‘Results? section. © Forthe extended scheme, the formula for the decade standard deviation is =SQRT(CA/3)*1000, where CA is the cell address of the quantity SSR (L19 in Figure 4.2, for example).28 THE CALIBRATION OF WEIGHTS AND BALANCES 4.4 Examples of weighing scheme analysis The following examples can be used to check spreadsheet programs written to analyse weighing schemes. 44.1 Closed-cycle example An E, reference is used to calibrate two F, test weights. The reference mass is 500.000 45 ¢ and the results of the mass comparisons are —1.1 mg, 1.4 mg and -0.1 mg. As uncertainties are not to be calculated, put the standard uncertainties of the reference mass and mass comparisons all equal to 0.01 mg. Put the degrees of freedom equal to 15 for the reference mass and equal to 10 for the three mass comparisons. The spreadsheet should give 500.001 62 g for the mass of 7; and 500.000 28 g for the mass of 7, while Sum a should be 0.2 mg (see Chapter 5 for the significance of Sum a). The standard uncertainties shown for both test masses should be 0.0129 mg with 31 degrees of freedom, and although these figures have no significance (as the input uncertainties and degrees of freedom were chosen arbitrarily) they can be used to check the spreadsheet. 4.4.2 Simple-decade example The F, head mass is 100.000 29 g, and the results of the mass comparisons (in mg) are: 0.455 0.125 0.170 ~0.060 0.270 As uncertainties are not to be calculated, put the standard uncertainties of the reference mass and mass comparisons all equal to 0.01 mg, Put the degrees of freedom equal to 15 for the reference mass and equal to 10 for the five mass comparisons. The spreadsheet should give 49,999 72 g for the mass of the 50 g weight, 19.999 88 g for the 20 g weight, 20.000 05 g for the 20’ g weight, 10.000 19 g for the 10 g weight, and 9.999 92 g for the 10' g weight. The standard uncertainties shown for the test masses should be 0.01 mg with 44 degrees of freedom for 50 g, 0.0072 mg with 20 degrees of freedom for 20g, 0.0057 mg with 33 degrees of freedom for 20’ g, and 0.0069 mg with 26 degrees of freedom for both 10 g and 10” g. Although these standard uncertainties and degrees of freedom have no significance (as the input uncertainties and degrees of freedom were chosen arbitrarily) they can be used to check the spreadsheet. 443 Extended-decade example ‘The F; head mass is 100.000 29 g, and the results of the mass comparisons (in mg) are: 0.455 0.750 0.370 0.125 0.105 0.415 0.195 0.060CHAPTER 4. MASS CALIBRATION USING WEIGHING SCHEMES 29 As uncertainties are not to be calculated, put the standard uncertainties of the reference mass and mass comparisons all equal to 0.01 mg, Put the degrees of freedom equal to 15 for the reference mass and equal to 10 for the eight mass comparisons. The spreadsheet should give 49.999 72 g for the mass of the 50 g weight, 19.999 886 g for the 20g weight, 20,000 037g for the 20’ g weight, 10.000 175g for the 10g weight, and 9.999 914 g for the 10’ g weight. The decade standard deviation should be 0.0168 mg (see Chapter 5 for the significance of this quantity). The standard uncertainties shown for the test masses should be 0.0071 mg with 44 degrees of freedom for 50 g, 0.0045 mg with 64 degrees of freedom for 20 g and 20’ g, and 0.0043 mg with 62 degrees of freedom for 10 g and 10’ g. Although these standard uncertainties and degrees of freedom have no significance (as the input uncertainties and degrees of freedom were chosen arbitrarily), they can be used to check the spreadsheet. 4.5 Asimple scheme for a 5,3,2,1,1' decade For a simple 5,3,2,1,1' decade scheme, the mass comparisons and design matrix are: 10=54+34+2 +a +14 +a +1 tas +1 tay tas lololofo}—|— sjolo|=|Llo! A spreadsheet very similar to that described in section 4.3.1 for the simple 5,2,2',1,1' decade scheme can be used for the analysis of this scheme. Placing several weights on a balance can be tricky30 THE CALIBRATION OF WEIGHTS AND BALANCESChapter 5 Uncertainty estimation for mass calibration 5.1 Introduction This chapter shows how to calculate the uncertainties of masses that have been measured using the techniques described in Chapters 3 and 4, The reader is referred to Appendix L for a brief introduction to uncertainty calculation and to other sources [4, 5] for a more complete treatment, As far as possible, symbols and terminology in this chapter follow references [4, 5]. Uncertainty calculations for direct comparison calibrations are shown first. The application to weighing schemes is then discussed. 5.2 Uncertainty of direct comparison 5.2.1 The model For the purpose of calculating uncertainties, we need an equation, called the model, which expresses the measurand as a function of the parameters used in its determination. For direct comparison the measurand is Mr, the mass of the test weight being determined, and the equation that best serves as a model is obtained by combining equations (3.5) and (3.6): M,, — MyM, += 0-7) : (1) where Me is the mass of the reference weight, Mens is the mass of the small weight that was used to measure the sensitivity reciprocal of the balance (see section 3.5), Aru: is the change in the balance reading that occurred during the measurement of sensitivity reciprocal (see section 3.5), and (¢—r) is the mean value of the measured mass differences (¢;~ 7). Note that equations (3.1), (3.2) and (3.3) are just special cases of equation (3.5) with n = 1 or n= 2. Notice also, that Mies is approximately equal to Arsen; because the sensitivity reciprocal is approximately equal to one. 3132 HE CALIBRATION OF WEIGHTS AND BALANCES ‘An examination of equation (5.1) shows that the sources of uncertainty that affect the measurement of Mp are: 1 ‘The calibration uncertainties in Mg and Meens 2. The uncertainties due to the instability of Me and Moons 3. ‘The repeatability of mass comparison for the balance, affecting both Arsen: and (fr) 4, The buoyancy uncertainty, since the buoyancy correction of equation (2.7) is not included in equation (5.1) 3. _ The rounding of My in the final statement of results ‘These are the uncertainty contributions most likely to occur in practice. A more comprehensive listing is found in reference [6], though the vast majority on this list are significant only under ‘unusual circumstances. Equation (5.1) is also used to obtain the sensitivity coefficients c; needed to calculate the effect on the measurand My of the above uncertainties in the quantities on the right of that equation: For Me co For Moons. (5.2) For Ar sens For (f=r) #1 Note: These sensitivity coefficients are found by taking the partial derivative of My with respect to the relevant quantity. To find the sensitivity coefficient for Arson, for OM, instance, one must evaluate From equation (5.1), Me. Maw GF wv LED, since Mt. * Ange, a5 mentioned above. BAroes Ms M soos For the calibration of standard weights, the sensitivity mass Moy: should be at least twenty times larger than the mass difference (f—) (see section 3.5), and hence the sensitivity coefficients for Mune and Arsns should be smailer than 0.05. When this condition is met, the uncertainties in these quantities are insignificant and can be ignored. When calibrating non- standard weights, such as weights for a pressure balance, however, the c; values may be greater than 0.05 and consequently uncertainties in Mex: and Avs may be significant (see section 5.2.3.2). Each of the above sources of uncertainty will now be examined in turn.CHAPTER 5. UNCERTAINTY ESTIMATION FOR MASS CALIBRATION 33 5.2.2 Uncertainty contributions for direct comparison (1) Calibration uncertainties of the reference weights Calibration reports will normally give the expanded uncertainty U and the value of coverage factor & used. In this case U; = U, k:= k and the number of degrees of freedom v; equivalent to kcan be found from Table L.1. (See Appendix L for an explanation of the quantities U; and ki.) Sometimes a report may give a standard uncertainty u and the degrees of freedom v. Then, U; =u, k= land y= v. It is sometimes necessary to use more than one reference weight. To calibrate a 300 g weight from a set with the 5, 3, 2, 1 structure for instance, the reference may be a 100g weight together with a 200 g weight. The uncertainty of a combination of N reference weights may be found by simple addition of their standard uncertainties — a simplification based on the seasonable assumption that they are highly correlated (see Note below). Thus, if each calibration uncertainty is converted to a standard uncertainty, with that for the j* reference mass being 1, we have for the reference weight combination: u Y= Qu, 63) a Since U; is a standard uncertainty, &; = 1 and one should take vj to be equal to the degrees of freedom ¥; for the largest of the contributions, (max). Asan example, consider the calibration of a 300 g weight requiring reference weights of 100 g and 200 g, The former has a reported (expanded) uncertainty of 0.15 mg with a coverage factor of 2.0 and the latter 0.25 mg with a coverage factor of 2.1. Thus, the standard uncertainties for the individual reference weights are: © forthe 100 g weight: woo . for the 200 g weight: — wa99 ).15/2.0 = 0.075 mg; and ).25/2.1 = 0.119 mg. and from equation (5.3), the combined reference uncertainty is therefore U; = 0.075 + 0.119 = 0.194 mg. The larger standard uncertainty, which is for the 200 g weight, has 19 degrees of freedom (since the coverage factor is 2.1). Hence, we have U; = 0.194 mg, & = 1 and y= 19. Note: The covariances cy between the N reference weights are not normally known, but if they are, then a better estimate of U; is obtained from equation (5.4). Once again, put ¥; equal to the degrees of freedom y, for the largest of the contributions, u(max): we up +2) Dew (54) Fl k= Equation (5.4) becomes identical with equation (5.3) as the covariances approach their maximum values, the condition known as full, or 100%, correlation. In practice, reference weights will be highly correlated, particularly if they are from the same set. Hence equation (5.3) is a reasonable approximation.34 THE CALIBRATION OF WEIGHTS AND BALANCES 2) Instability of the reference weights The mass of a weight will invariably change somewhat after calibration. Such changes are largely unpredictable and will affect the uncertainty of reference mass values. In what follows, it is assumed that the uncertainties quoted in the reports for reference weights do not include a contribution to account for these changes. This contribution must therefore be included in the calculations presented here. If it is clear from the report on the reference weights that quoted uncertainties do include the effect of mass instability, then the uncertainty contribution discussed in this subsection should be omitted from the calculations. ‘The estimation of this uncertainty component is obviously very difficult miles a long calibration history or other data, such as a history for similar weights, is available (see Note below). In most cases the calibrator has litle option but to use a rule devised by someone who has studied mass variations in similar weights under similar conditions of use and storage. Such a rule may, for instance, relate the standard uncertainty due to mass instability to the OIML maximum permissible error (see Appendix 1). Experience at the National Measurement Institute has shown that this contribution can be surprisingly large even for properly handled weights from a reputable manufacturer. It is therefore recommended that, in the absence of other information and under reasonably good laboratory conditions, the standard uncertainty be taken as 8% of the maximum permissible error for the relevant OIML class, with 4 degrees of freedom (corresponding to an estimated 35% relative uncertainty for this estimate). For weights used in relatively poor conditions or by inexperienced personnel, this estimate may have to be increased by a factor of 2 or more. As Uj is a standard uncertainty, k; If there is doubt about the effective class of reference weights (which can often be the case for older weights), then the laboratory that calibrated the weights may be able to offer advice. When using two or more reference weights in combination, one can take the instability contributions for the various weights to be uncorrelated (unless a calibration history suggests otherwise). They can therefore be added in quadrature (equation L.4). Note: Obtaining an estimate of the instability uncertainty from a calibration history is clearly more satisfactory than merely adopting a certain pereentage of the OJML maximum permissible error, but it must be approached with caution. ‘The history should contain at least five calibrations, preferably carried out at the same laboratory and hhaving similar uncertainties. Provided the mass values from these calibrations show no consistent trend, ‘one finds their standard deviation syy and compares it with the mean standard uncertainty tig of the calibrations (obtained by dividing cach reported calibration uncertainty by its coverage factor and averaging the results). ‘The correlations between the calibration uncertainties complicate the analysis, but it is reasonable to take the instability standard uncertainty to be equal to sy4 if ny is greater than ue /2, and zero otherwise. If 2 trend is evident in the mass values (¢g. they tend to rise with time) then the trend should be eliminated from the data before proceeding as above. One must then decide whether to correct reported ‘mass value for the trend or to treat the trend as an extra component of uncertainty. The later is safer. For this estimate of U,, k= I and ¥; is equal to one less than the number of calibrations analysed.CHAPTER 5. UNCERTAINTY ESTIMATION FOR MASS CALIBRATION 35 (3) __ Repeatability of mass comparison for the balance The repeatability of mass comparison s» (section 3.6) is the repeatability of a mass difference (4-1) obtained in substitution weighing. Although the circumstances of balance sensitivity measurement are somewhat different, the repeatability of Aix; can also be taken as Sy. Since (f=) is the mean of 7 differences, the standard uncertainty of this quantity will be: . Sal if Sp > Spe and © Sy if'S9 = Ses (Se Appendix M). These estimates of U; are standard uncertainties so ki = 1, and y; is the number of degrees of freedom of s,,, which is usually nine. (4) Buoyancy In conventional weighing, the buoyancy correction given in equation (2.7) is not normally made, particularly in laboratories at altitudes within 300m of sea level. The buoyancy uncertainty is therefore the uncertainty that results from ignoring the correction, and it is given (see Appendix J) by: u, =4.5x10 4p, RM mg (5.5) where App is the total width (in kg.m’*) of the OIML density limits (see Appendix I) for the class of the test weight 7, R is given for various altitudes in Table J.1, and Mis the nominal mass of the test weight in grams. Since all the quantities in equation (5.5) are well defined, the degrees of freedom are very high; the exact figure is not important so one may take it to be 1000. So U; =u, and since u is a standard uncertainty, k= 1. Note: If the corveetion given in equation (2.7) is made and a similar correction was made when the reference weight was calibrated, then provided gp, ge and py are known with uncertainties of 1% or less, us will be negligible except in some extreme cases. To check that this is so, us may be calculated from equation (5.6) [3]: #-f ayer 2, =1.2Xp. ~ Par) Mp, Pel PF 42 wv 5.6) 7 Wen ¢ Where tga Upr and gg are the uncertainties of ., Or and pg respectively and py is the air density when the reference mass was calibrated, The degrees of freedom are not easily calculated and it is recommended that it be equated to the degrees of freedom £0F tn Ur OF Upa depending on which of these makes the largest contribution to 1s. @) Rounding Numbers are rounded to remove unwarranted detail in the least significant digits and the rounding process begins by considering the magnitude of the expanded uncertainty U [5}. It should be done only once, when the final measurement result is expressed. Briefly, express U to only one significant figure when the most significant digit (the first non-zero digit from the360 THE CALIBRATION OF WEIGHTS AND BALANCES left) is 5 or more and to two significant figures otherwise, and the values should be rounded up except where rounding down involves a change of less than a few percent. Finally, the value of the measurand should be rounded to match the rounding of the uncertainty. To caloulate the uncertainty component due to rounding, proceed as in the following example. Suppose that the measured mass values are rounded to the nearest 0.001 mg, then the rounding uncertainty is +0.0005 mg with a rectangular probability distribution, Thus, we would put U;= 0.0005 mg, = 1.73, as the distribution is rectangular, and v; = 1000. 5.2.3. Examples in caleulating the uncertainties for a direct comparison The two following examples make use of summary tables (such as Table 5.1) that are easily adapted to a spreadsheet program. The shaded columns show the location of the input data Ui, k, ¢, and y, In the spreadsheet, the u(x,) column contains the formula given by equation (L.2), the combined uncertainty 1, is calculated from equation (L.4), vy fiom equation (L.5), & from equation (L.7) and U from equation (L.6). 5.2.3.1 Calibration of a 10 kg Fi weight In this first example, a 10 ke F, weight is calibrated in terms of an E, reference using double substitution weighing on a 30 kg balance having a repeatability of mass comparison 5 of 715 mg (with 9 degrees of freedom). The laboratory is within 20 metres of sea level and the reference has a history of only 3 calibrations. We first calculate the various sensitivity coefficients. The difference (f—r) between reference and test masses is approximately 27 mg, whereas the weight used to measure the balance sensitivity reciprocal had a mass (Mie) of 5 g. From equations (5.2) we have: efor; = 1 for Mens = 27/5000 = efor Arun = 27/5000 ~-0.0054 efor @=7) = 1 ‘Next, we evaluate the component uncertainties that result from the five sources listed in the above section. w ‘The calibration uncertainties In the calibration report, the expanded uncertainty of the reference mass Mz is given as 5 mg with a coverage factor of 2.1, From Table L.1 we see that this coverage factor implies 19 degrees of freedom, Hence U, = 5 mg, k= 2.1 and y= 19. The calibration uncertainty for Mens is ignored, as the sensitivity coefficient for this quantity is less than 0,05 (see section 5.2.1), @) The instability in Mf As a satisfactory calibration history for the reference does not exist, the instability standard uncertainty is taken as 8% of the maximum permissible error for a 10 kg Eo weight, with 4 degrees of freedom. Hence U; = 0:08 x 16 mg = 1.28 mg, k= 1 and y= 4. The instability of Mun: is ignored, as the sensitivity coefficient is less than 0.05.CHAPTER 5. UNCERTAINTY ESTIMATION FOR MASS CALIBRATION 37 8 4) Balance repeatability The balance has a repeatability sq of 7.5 mg with 9 degrees of freedom. As n = 2 for double substitution weighing, U;=7.5/V2 = 5.30 mg, ki = 1 and 4 =9 (division by ¥2 is allowable as sy > Sy — see Appendix M). The uncertainty in Arg due to repeatability is ignored, as the sensitivity coefficient is less than 0.05. Buoyancy Since the laboratory is near sea level, the buoyancy uncertainty will be negligible compared with the OIML maximum permissible uncertainty for an F, weight. However it may be significant compared with the uncertainty actually achieved. The OIML density band 4p; is 1340 kg.m for an Fy weight and R is 0.02 kgm? (Table J.1). So, from equation (5.5): 4, = 4.5 x 10 x 1340 x 0.02 x 10000 = 1.206 mg giving U;= 1.206 mg, k= 1 and y= 1000. Rounding The data for the above five uncertainty components are entered into the spreadsheet (Table 5.1). As the resulting expanded uncertainty is about 13 mg, both Mp and its expanded uncertainty U will be rounded to the nearest 1 mg, i.e. to + 0.5 mg. So, for the rounding component U;= 0.5 mg, k= 1.73 and v,= 1000. All the above data are shown in the uncertainty summary table, Table 5.1. The report for this weight would quote an unceriainty of £0.013 g with a coverage factor of 2.14. ‘Table 5.1; Summary table for calculating the calibration uncertainty for a 10 kg F: weight calibrated by direct comparison using double substitution weighing. Component (= 1, 2, 6) Component values ve | foams | lvauts'/y, U;(mg) |__| led | leur) 1. Calibration of Mie {| 2.381 5.669 1.7E+00 2. Instability in Mg 1.280 1.638 | 6.7E-O1 3. Balance repeatability on @—>) 5.300 28.090 | 8.8E+01 4, Buoyancy 1.206 1.454 | 2.1E-03 5. Rounding of Mp 0289 0.084 | 7-05-06 Combined standard uncertainty u,(mg) 6.08 Degrees of freedom vay 1s Coverage factor k 2.14 Expanded uncertainty U (mg) 12.98 = 13 mg when rounded 5.2.3.2 Calibration of non-standard weights In this example we consider the calibration of six brass weights that are to be used on a pressure balance. Their quality is roughly equivalent to class F; and they have masses of approximately 55.065 g, the largest mass being 55,070 g, Four substitution weighings are38 THE CALIBRATION OF WEIGHTS AND BALANCES made on a 100 g balance having a repeatability of mass comparison of 0.19 mg (with 9 degrees of freedom). The reference weight set has only been calibrated once. The reference could be a 50 g+ 5 g+ 50 mg + 10 mg +5 mg group or perhaps a 50 g+5g+ 100 mg group. However to simplify the weighings, just the first two weights are used. Thus the maximum mass difference (7-7) is 55.070— 55 = 0.070 g. The sensitivity reciprocal of the balance was measured with a 100 mg weight with an uncertainty of 40.012 mg and a coverage factor of 2.0. The sensitivity coefcints, from equations (5.2), are as follows: fore = for Maen = fon100 efor Ariens = —70/100 efor (=r) = 1 0.7 -0.7 Since the sensitivity coefficients for Mrns and Arsen: are greater than 0.05, the uncertainties involving these quantities cannot be ignored (see section 5.2.1) as in the last example. Indeed, it will be seen, in Table 5.2, that the quantity A7.,; is responsible for the largest contribution to ‘the uncertainty of My. The component uncertainties are now evaluated. (1) The calibration uncertainties The calibration uncertainties of the 50 g and 5 g weights are =+0.09 mg and +0.035 mg respectively with a coverage factor of 2.0, implying 60 degrees of freedom. As described in section 5.2.2 (I), the standard uncertainty of this group must be found by simple addition of the standard uncertainties of the two weights: U,= 0.09/2 + 0.035/2 = 0.045 + 0.0175 = 0.0625 mg, with k= 1 (as this U; is a standard uncertainty) and y= For Mens U;= 0.012 mg, k= 2.0 and y= Q) The instability in Mg and Mens As calibration histories for these weights do not exist, the instability standard uncertainty is taken as 8% of the F maximum permissible error. For the 50 gweight: U;= 0.08 x 0.30 mg = 0.024 mg For 5 g: j= 0.08 x 0.16 mg = 0.013 mg For 100 mg: U,= 0.08 x 0.05 mg = 0.004 mg In each case, ki aaa wind. @) _ Balance repeatal The balance repeatability i is 0.19 mg with 9 degrees of freedom. As four weighings were made when measuring @=r), U; = 0.19/V4 = 0.095 mg (division by V4 is allowable as Sn > Sps — sce Appendix M). When measuring Ars, only a single weighing was made, so Uj=0.19 mg. In both cases, k= I and y= 9. (@ — Buoyancy The buoyancy uncertainty is seldom significant for F, test weights and in this case it is sure to be negligible, even if the laboratory were located at high altitude, as both the test and reference weights are made of brass and hence will have very nearly the same density.CHAPTER 5, UNCERTAINTY ESTIMATION FOR MASS CALIBRATION 39 © — Rounding . Both My and its expanded uncertainty U will be rounded to the nearest 0.01 mg, ie. to £0,005 mg. So, U;= 0.005 mg, k= 1.73 and = 1000. ‘The above data are shown in the uncertainty summary table, Table 5.2. The relatively large contributions due to Arse; (0.133 and 0.029 mg) highlight the need to use reference weights with a combined mass very close to that of any non-standard object when making accurate mass measurements by substitution weighing. It follows from equations (5.2) that the smaller the difference between reference and test objects, the smaller (/—r) will be, and hence the smaller the ¢; values for Mens and Arsons. Small c; values in turn reduce the effect of Mis and Arsens uncertainties. The report for the weights would quote an uncertainty of +£0.37 mg with a coverage factor of 2.08. Table 5.2: Summary table for calculating the calibration uncertainty for 55.065 g weights calibrated by direct comparison using four substitution weighings. . ‘Component values > “ Component (= 1, 2,11) =>} >], | exuded? | JonnGeyl'7v, Ucmgy | | lel_| levwtd) ea =| 0.063 |: 0.004 0.024 0013 0.003 0.095 | 398-03 | 2.5E-07 1.8E-05 | 528-12 S.8E-04 83E-08 1.66-04 | 6.7E-09 788-06 | 1.5E-11 9.05-03 | 9.1B-06 1. Calibration of My. 2. Calibration of Mis 3. Instability in 50 g 4. Instability in 5 g 3. Instability in Moy 6. Balance repeatability on =) 0.133 0,000 0.003 1.8E-02 | 3.SE-0S 0.0E+00 | 0,06+00 8.48-06 | 7.0E-14 7. Balance repeatability on Sse 8. Buoyancy 9. Rounding of Mr iene Combined standard uncertainty u.(mg) 0.177 Degrees of freedom vig 22 Coverage factor k 2.08 Expanded uncertainty U (mg) 0.368 = 0.37 mg when rounded 5.3 Uncertainties for weighing schemes For weighing schemes, the model is more complicated than equation (5.1). However the model for each individual measurement of mass difference a; is very similar to equation (5.1), since from equation (4.2): M.,. — a, = 5.7) 7. @-r) 6.7)40 THE CALIBRATION OF WEIGHTS AND BALANCES Although the mass of the reference, Mg, does not appear in this equation, it enters via the analysis of the weighing scheme. Hence the five uncertainty sources and the sensitivity coefficients listed in section 5.2.1 still apply, as does the discussion of section 5.2.2. Equations (L.4) and (L.5) are not applicable in the simple forms shown, Instead, w- and ver must be calculated with the aid of the spreadsheets introduced in Chapter 4, as will be described below. To minimise the complexity of the examples given below, it will be assumed that the sensitivity coefficients for Mun: and Armas are less than 0,05 so that uncertainty contributions involving these terms can be ignored. This will always be the case for the calibration of standard weights if Manis large enough (section 3.5). To illustrate the approach to calculating the uncertainties of mass values obtained in weighing schemes, reference will be made to the spreadsheet for the closed cycle scheme shown in Figure 4.1. However, the following discussion is easily adapted to any weighing scheme. Firstly one must combine the uncertainty components involving Mg. Remember that the head weight is the reference weight for a decade scheme. The resulting combined standard uncertainty 1(R) of the reference mass and the corresponding degrees of freedom v,,(R) are then entered into the spreadsheet at cells ES and B6 respectively. The next step is to calculate the standard uncertainties of the mass differences a, that is, of the quantities(t—r) for each mass comparison, The standard uncertainty u(4M)} of the first mass difference a; and the associated degrees of freedom (4M) are then entered into the spreadsheet at cells El] and FI respectively. The corresponding quantities for the other mass differences are entered in the cells below El] and Fil, For each measured mass value, the scheme gives a standard uncertainty and corresponding degrees of freedom (for instance: cells D19 and E19 for the first test weight T1). For this uncertainty, k= 1 and c= 1, and it must be combined with the buoyancy uncertainty (if significant) and the rounding uncertainty to obtain the combined uncertainty of the measured mass value. For decade weighing, the head and test weights normally come from the same set and hence will have very similar densities. Consequently the buoyancy uncertainty will very likely be negligible for the test weights of a decade scheme, even at high altitudes. It may be significant for the check weight, but the uncertainty of this weight does not need to be calculated. Examples are now given for a closed cycle and a decade scheme. 5.3.1 Uncertainty estimation for a closed-cycle weighing scheme This example. calculates the uncertainties for the closed cycle weighing scheme shown in section 4.4.1, where a 500 g Ez reference is used to calibrate two F, test weights.CHAPTER 5. UNCERTAINTY ESTIMATION FOR MASS CALIBRATION 41 The uncertainty of the reference mass is +0.18 mg with 30 degrees of freedom, so Uj = 0.18 mg, k= 2.04 (from Table L.1) and = 30. The instability uncertainty is taken to be 8% of the OIML maximum permissible error of 0.8 mg with 4 degrees of freedom, so U; = 0.8 x 0.08 = 0.064 mg, k= I and vj = 4. These contributions are combined as shown in the top section of Table 5.3 to give values for u(R) and veg(R). The mass differences are determined using single substitution weighing, so the standard uncertainties of the a; are all simply equal to the repeatability of mass comparison s, of the balance. For this 1 kg balance, s» is 0.11 mg with 9 degrees of freedom, so for each aj, 1AM) = 0.11 mg and (4M) = 9. When u(R), v%zq(R), (AM) and 4AM) are entered (as described in section 5.3) into the closed cycle spreadsheet, one obtains for both test masses a scheme standard uncertainty of 0.140 mg with 43 degrees of freedom (see Figure 5.1). x = = Gest eana Basses "Valo of ference ass (gh SESE SOO ONDA ‘Slade unenariy of waronco mass) [ese aPRONOT Degrees of fede or referonco st. Une: |e oS ‘Rosulvaive ofall] Standard uncerainy Toa ia Reta iS zB Teresa t a [sanreo=O ‘Standard ancora | Dogrese of Hesdom™ H Bag 2.140 Figure 5.1: The appearance of the closed cycle spreadsheet after entering (into the shaded cells) the data relevant to the example of section 4.4.1. ‘The laboratory is within 100 m of sea-level, hence R = 0.02 kg.m” in equation (5.5), while the OIML density range Apr is 1340 kg.m™. So, for the buoyancy component: U;=4.5 x 10° x 1340 x 0.02 x 500 ~ 0.0603 mg, k= I and y= 1000. The result will be rounded to the nearest 0.01 mg, i. to + 0.005 mg. So. U = 0.005 mg, ky = 1.73 and ¥;= 1000. ‘The scheme, buoyancy and rounding uncertainties are combined as shown in the second part of Table 5.3 to give a combined uncertainty of 0.31 mg with a coverage factor of 2.00. This analysis applies equally to both test weights.42 . "THE CALIBRATION OF WEIGHTS AND BALANCES Table 5.3: The summary table for the calculation of combined expanded uncertainty for two 500 g F; weights calibrated by means of a closed eyele scheme. Shaded cells show input data. ‘Component values 2 Component wi | leeuGen? | jevaeyly U;Gmg) |__| led | lene) Calibration of Me ag 4:fcts | 0.088 7.8E-03 | 2.0E-06 Instability in Me [0,064 0.064 | 41e-03 | 428-06 ‘Combined standard uncertainty u(R) (mg) _ 0.109 Degrees of freedom vy) 23 ‘Component values > “ ‘Component ve | levuGedl | lester, Ui(ng) | ki} led_| levaeespl 0.140 0.060 0.003 2.0E-02 | 8.9E-06 3.6E-03 | 135-08 8.4E-06 | 7.0E--14 From weighing scheme Buoyancy Rounding of result Combined standard uncertainty 1, (mg) 0,152 Degrees of freedom vey 60 Coverage factork 2.00 Expanded uncertainty U (mg) 0.305 = 0.31 mg when rounded ‘As a check on the measurements, the quantity Sum a should be less than 2¥3u(AM) = 0.38 mg, In fact it is only 0.20 mg, so we can be reasonably confident in the results of the scheme. (f Suma exceeds 2V3u(AM), then this is a warning of a potential problem that should be investigated. See section 3.4, At the very least, the measurements should be repeated.) 5.3.2 Uncertainty estimation for a decade weighing scheme ‘The uncertainties of the five F; test masses calibrated using the extended decade weighing scheme of example 4.4.3 are estimated here. The first four mass comparisons were made on a 160g balance and the last four on a 30g balance. Double substitution weighing was used throughout. The 100 g head weight (also class F,) is from the same set and was calibrated the previous day as part of the 1 kg to 100 g decade. The result of that calibration was a mass of 100.000 29 with a standard uncertainty of 0.055 mg having 42 degrees of freedom. The head weight instability uncertainty is taken as zero since the calibration was so recent and the weight was not even moved to another laboratory. There is therefore no need for a section of the summary table for combining the Me uncertainties and we ‘can just take u(R) = 0.055 mg and vag(R) = a2.CHAPTER 5. UNCERTAINTY ESTIMATION FOR MASS CALIBRATION 43 First four mass comparisons: The balance repeatability sis 0.022 mg with 9 degrees of freedom. Since sy > Sy. we can divide by-V/2 to find the standard deviation of the mean mass difference (see Appendix M). Thus 1(AM) = 0.022//2 = 0.0156 mg and (AM) =9. Last four mass comparisons: The repeatability is 0.006 mg, again with 9 degrees of freedom. Once again, 5», > res $0 u(AM) = 0.006//2 = 0.00424 mg and (AM) = 9. ‘When the uncertainties and degrees of freedom for the reference mass and the comparisons are entered into the decade scheme spreadsheet in a manner similar to that desoribed in section 5.3, one obtains the standard uncertainties: 0.0286, 0.0115 and 0.0060 mg for the 50 g, 20 g, and 10 g weights, respectively. The degrees of freedom are 49, 50 and 59, respectively. Since all the weights are from the same set, it is assumed that the densities are very similar, and hence the buoyancy uncertainty can be ignored. (The 10 g check weight is from another set, but the uncertainty of its measured mass does not need to be calculated.) Mass values will be rounded to the nearest 0.01 mg (for the 50 g weight) and to the nearest 0.001 mg (for the 20 and 10 g weights). So U; is equal to 0.005 mg for 50 g and 0,005 mg for 20 and 10 g, with & = 1.73 and y= 1000. The effect of this rounding uncertainty is negligible as can be seen from the final combination of uncertainties shown in Table 5.4 for the 50 g weight. Spreadsheets for the 20 and 10 g weights are similar. The expanded uncertainties are therefore 0.06, 0.024 and 0.012 mg, for the 50 g, 20g, and 10 g weights, respectively. Table 5.4: The calculation of the combined expanded uncertainty of the 50 g mass value calibrated by means of an extended decade scheme. Shaded cells show input data. Component Component values ve | teawt| Jone wicmg) [| tel | enuta) From weighing scheme 0.02862]: <1, "|-1%] 0.029 "| 8.2E-04 | 145-08 Buoyancy pac | 0.000 | 0.08+00 | 0.08+00 Rounding of result Le [i731] 0.003 8.4E-06 | 7.0B-14 ‘Combined standard uncertainty w. (mg) 0.028 Degrees of freedom vy 50 Coverage factor k 2.01 Expanded uncertainty U (mg) 0.0578 = 0.06 mg when rounded The mass obtained for the check weight can be used in a consistency check based on the t-test described in Appendix G. (See the example of section G.2.) This check is available for both simple and extended decade schemes.44 THE CALIBRATION OF WEIGHTS AND BALANCES The decade standard deviation shown on the decade scheme spreadsheet is 0.0171 mg. As a further check on the measurements, the square of this quantity should be less than four times the avorage value of u(AM)?. This rule is obtained from an F-test similar to those discussed in ‘Appendix G. In this case we require 0.0171? to be less than 4- (0.0156? + 0.004247)/2, where the values for u (AM) are given above. That is, we require 0.000292 to be less than 0.000554, which it is. If this check fails, the decade should be repeated. This check is not possible for the simple decade scheme.Chapter 6 Calibration of electronic balances 6.1 What is an electronic balance? ‘An electronic balance is essentially one that uses an electric sensor, the output of which is processed electronically to generate a reading shown on a digital display. However many balances that do not fit this simple description may also be calibrated by the procedures described here. In particular, * A balance may have tare weights, but preferably not more than two or three. This allows the electronic range (ie. the range of the display for a given selection of tare weights) to be less than the full range of the balance. * Instead of being displayed directly, the reading may be transmitted to a computer, data logger or printer. This does not matter provided the present reading can be observed when required. * Some balances have two or more ranges with different characteristics. These ranges may have to be calibrated separately as described below. * The balance may be top-loading or have a suspended pan. See Appendix K for more details of the construction of electronic balances. 6.2 The scope and purpose of the calibration The main purpose of a balance calibration is an estimation of the accuracy of measurements ‘made on the balance, However balance calibrations have three other important functions: (a) A table of corrections to the balance readings is provided. (6) The user is given information on limitations of the balance, principally the effects of off-centre loading and hysteresis. This information can act as a diagnostic indicating that repairs may be required. (©) The balance report contains information that allows the user to carry out effective checks on the balance between calibrations (see section 6.5.2 for details of user checks). 4546 THE CALIBRATION OF WEIGHTS AND BALANCES The balance is adjusted, using the sensitivity adjustment (see section 6.3.1) present in almost all electronic balances, before calibration and before user checks (and at any other time deemed necessary). In this way, sensitivity drift is eliminated, which is essential if the user checks are to detect other changes in the balance performance. 6.3. Balance calibration The following general considerations should be noted: 1. Unlike most other measuring instruments, balances must be calibrated in the position - where they are to be used. They cannot be sent to a calibrating laboratory for calibration, If it becomes necessary to move a balance after calibration, even to another position in the same room, the user checks of section 6.5.2 should be carried out to see whether a recalibration is necessary. 2. Some balances have a high-resolution range (with ten times the normal resolution) covering perhaps one-fifth the total range of the balance. Sometimes the high- resolution range is permanently restricted to the first 20% (say) of the load range, while sometimes it can, by taring, be moved anywhere throughout the load range. The moveability of @ high-resolution range is useful for substitution weighing (see Chapter 3), but is of limited value when calibrating a balance. Nevertheless, one can take some advantage of a movable high-resolution range when calibrating a balance. While the repeatability and the corrections to the balance readings must be measured without retaring, off-centre loading errors and hysteresis may be measured after retaring in order to make use of the higher resolution, 3. The last digit of a reading will sometimes flick continually between two successive numbers. When this happens the reading used should be the mean of the two digits. 4. ‘Where calibrated weights are called for (sections 6.3.3 and 6.6), the density of the weights should be in the vicinity of 8000kgm™. The accuracy of the balance determines how close the density must be to this value. This is usually not a problem provided the weights are made of stainless steel, brass or bronze, but to be quite sure that the density of the weight is acceptable, use weights conforming to a standard, such as the OIML classification [3]. For example, to calibrate a 1 kilogram balance to have an uncertainty of weighing of £75 mg, an OIML My weight set could be used since the maximum mass uncertainty of the weights used is +17 mg and they have an acceptable density for this level of uncertainty. 5. A client may request that a balance be calibrated over a restricted range. This is acceptable provided the range restriction is made clear in the report and on the balance.CHAPTER 6. CALIBRATION OF ELECTRONIC BALANCES 47 6. Some balances have a zero-tracking facility whereby the balance automatically tares out small departures from a zero reading. This facility should be tumed off during balance calibration and user checking. 7. When weights are transported to a laboratory for the purpose of calibrating a balance, care must be taken that they do not become excessively warm or cool relative to the likely temperature of the balance. For instance, if the vehicle used is not air- conditioned, one should consider putting the weights in a thermally insulated container. Table B.2 in Appendix B shows how long one may have to wait if the weights do become cool or warm, 6.3.1 Adjustment Almost all electronic balances are adjustable as it is necessary to set the scale to the local gravity (the local value of g). Balance manuals often refer to this procedure as ‘calibration’, but, as it is really just a sensitivity adjustment, the term ‘adjustment’ is used here. This avoids confusion with the far more comprehensive calibration of balances described in this chapter. The adjustment may be automatic, semi-automatic or manual. It may be activated whenever the balance is switched on, or only when triggered by the user. It involves a weight usually referred to in balance manuals as the calibration weight, which may be a built-in or a designated separate weight. The manual should give instructions for carrying out the adjustment. Before adjusting the balance, make sure that it has been switched on for the warm-up period recommended by the manufacturer, or at least 30 minutes if this period is not known. It is also recommended that the balance be ‘exercised’ by placing a weight, of mass approximately equal to full load, on the pan once or twice. It is strongly recommended that a pre-adjustment check of the balance be made in order to gauge its stability and because a large adjustment may have consequences for recent measurements made with the balance. The check is performed by using a calibrated weight to measure the correction of the balance near full scale before the adjustment is made. Adjust the balance following the manufacturer’s instructions. In the absence of instructions: zero the balance with the pan empty; place a weight of known mass (preferably close to the maximum capacity) on the pan; adjust the balance until it displays the known mass value; then remove the weight and check that the balance zero has not changed significantly (by not more than 1 or 2 counts in most cases). If the balance zero has changed, then repeat the adjustment. Between successive calibrations, the validity of the most recent calibration depends on the mass stability of the calibration weight. If a separate weight is used, it must therefore be handled with great care. It should remain with the balance user (not the calibrator), be used for this purpose only, and be stored separately from other weights in a suitably lined dust-tight container.48 THE CALIBRATION OF WEIGHTS AND BALANCES Many adjustment procedures assume that the mass of the calibration weight is close to its nominal value. For instance, a balance with a 10g calibration weight may automatically display 10.0000 g after adjustment. if it is found that the corrections to the balance reading (see section 6.3.3) and hence the Limit of Performance (see section 8.1.3) are unexpectedly large, it is possible that a calibration weight with a large departure from nominal mass is to blame. For smail balances, obtaining a calibration weight with a sufficiently small departure from nominal mass may not be easy as even the E; tolerance may well be too large. The user may have to approach a manufacturer to obtain a weight with an unusually low tolerance. For built-in calibration weights, this problem should arise rarely, unless the balance is used in an adverse environment. 6.3.2 Repeatability of measurement The repeatability of measurement s, of a balance is the standard uncertainty associated with a single mass measurement. When using a calibrated balance, a single mass measurement consists of two readings — a zero reading z, and a reading r with the object whose mass is to be measured on the pan. If drift is a problem, a second zero reading is recommended, see section 6.5.1. To measure s,, one therefore starts by calculating the standard deviation s of 2 mass measurements, the /* such measurement being: 6.1) Thus, if the average value of M, is M: (62) The recommended minimum number of measurements (je. the minimum value of 7 in equation 6,2) is 10, in which case s has nine degrees of freedom. ‘The measured standard deviation s usually provides a good value for the standard uncertainty and hence the repeatability, in which case one could simply equate s, to s. However balances are often resolution-limited ~ they give the same reading many times when the same weight is placed on the pan — and for such balances s may not be a good value for s, As a consequence of this, the repeatability should always be determined as follows: If a is the resolution semi-range of the balance, then s, is equal to s (with nine degrees of freedom), or equal to 0.82a (with 1000 degrees of freedom), whichever is the greater. (See Appendix M for a brief discussion of resolution and its effect on the measurement of balance repeatability.) Since electronic balances do not weigh at constant load, s, may vary significantly over the range of the balance, and consequently this procedure should be carried out near halfCHAPTER 6. CALIBRATION OF ELECTRONIC BALANCES 49 maximum and maximum load. However, one may measure 5, at loads other than exactly full scale and half full scale, provided that the difference is not greater than 20%, Standard weights are not required; any clean and reasonably smooth piece of turned brass or stainless steel is adequate, One ot two weights can be used to make up the load for s, measurement, though one weight is preferable. When using two weights, care should be taken to get the centre of gravity of the weights as close as possible to the centre of the pan (by placing both weights off-centre but with the larger one closer to the centre). For multi-range balances: (@) __ if the balance’s measuring system changes from range to range, the repeatability should be measured near the mid-point and near the top of each range; (b) _ if the balance’s measuring system does not change, a measurement near the top of each range is sufficient. 6.3.3 Corrections to balance reading Even though a balance has been adjusted to read correctly at a certain load (usually close to the maximum), it may still be necessary to apply corrections to the readings, for two reasons: (a) the mass of the calibration weight may differ significantly from its nominal value; (6) the balance reading as a function of load may be significantly non-linear. ‘The corrections to balance reading should be measured at sufficient equally-spaced points over the range to ensure that one may safely interpolate between points. This usually means a minimum of 10 points. The following procedure assumes that the balance calibrator has a set of calibrated weights (see section 6.6 if this is not the case). As far as practicable, the calibrated masses should have uncertainties less than the resolution of the balance, in order to minimise the uncertainty of the measured corrections. The corrections to balance reading are determined by successively placing calibrated masses on the pan and observing the readings. The steps are: @) __ Read the zero. (ii) Place weight(s) of known mass Mon the pan, where Mis approximately one-tenth the range of the balance. Note the reading. (iii) Remove the weight(s) momentarily, then replace them on the pan and note the new reading, This reading is averaged with the one in (ii) to give 1; (iv) Remove the weight(s) and read the zero. This reading is averaged with the reading in (i) to give the zero value, z). (v) Place weight(s) of mass 244, on the pan and note the reading. (vi) Remove the weight(s) momentarily then replace them on the pan and note the new reading. This reading is averaged with the one in (v) to give r>. (vii) Remove the weight(s) and read the zero. This reading is averaged with the reading in (iv) to give the zero value, z2. (viii) Repeat with weights of mass 3M, 4M, etc, until the capacity of the balance is reached.50 THE CALIBRATION OF WEIGHTS AND BALANCES If readings ry and z; correspond to weight(s) of total calibrated mass Mj on the pan, then the correction to balance reading for this toad is given by: C,=M,-(-2)) (6.3) The correction is the amount that should be added to a measurement (e.g. equation 6.1) to give the correct mass. It should be small and not change significantly with load (within the manufacturer’s tolerance). The negative of the correction (— C)) is known as the departure from nominal value. For balances with more than two ranges, the correction to balance reading may be measured at fewer than 10 points per range, provided there are at least 20 points covering the full balance range. If the only change between ranges is the manual loading or unloading of tare weights, then measure the correction for at least 10 points over the full balance range, and for at least 4 points on cach range. 6.3.4 Effect of off-centre loading When the centre of mass of the object being weighed is off-centre on the pan, off-centre loading error (also called shift or corner-load error) may occur. It is difficult to comect accurately for this because the effect is not always linear with respect to either load or position. This test is designed to enable the user to decide how accurately objects must be positioned on the pan for this effect to be negligible. If the measured errors are large compared with the manufacturer's specification, the balance is probably in need of repair. The error is most easily measured by placing a weight on the centre of the pan and then lifting and placing it successively to front, rear, left and right positions on the pan, noting the reading cach time. Standard weights are not required; any clean and reasonably smooth piece of turned brass or stainless steel is adequate, provided it has roughly the same shape as a standard weight. The test should be carried out at the load recommended by the manufacturer or, if this is not known, at a load between one-third and half the maximum capacity of the balance. Most balance manufacturers recommend a one-third load or quote performance figures at this load. Placing a much larger weight near the edge of the pan could possibly damage the linkages between pan and sensor, and will not necessarily give a larger reading. A single weight should be used for this test, and this restricts the choice to values of 1, 2, 5 and perhaps 3, unless special weights or objects are available. For example, a balance of 1200 g capacity should be tested with a 500 g weight, because 200 g is too small. When moving the weight to the front, back, left or right, lift and place it so that the outer edge of the weight is approximately aligned with the edge of the pan, without tilting the weight. If this is not possible (if, for example, the pan curves upwards near the edge) move the weight as far from the pan centre as possible without tilting it.CHAPTER 6. CALIBRATION OF ELECTRONIC BALANCES SL The measurement of the off-centre loading error will be subject to the uncertainty arising from balance non-repeatability. If the repeatability of measurement s, is similar to or larger than the off-centre loading error, then the latter will be difficult to measure accurately but its exact value will be of small importance anyway. For dual or multi-range balances, this test should likewise be carried out at the load recommended by the manufacturer or at a load between one-third and half the maximum capacity of the balance. If the balance has a high-resolution range then this range should, if possible, be moved to include the load at which this test is carried out. This is normally done by re-taring the balance. 6.3.5 Hysteresis One should test for hysteresis when a balance is calibrated for the first time or after a major repair. Aficr that, it normally need be measured only a few times during the life of the balance. A properly adjusted balance in good condition should show no more hysteresis than | count. If the balance shows more hysteresis than this, then the user should consult the manufacturer. Testing at one point, about mid-range, is adequate. Proceed as follows: (i) place weight(s) of mass MM, equal to approximately half the balance range, on the pan and note the reading, p); (i) add extra weight(s) of mass M’to bring the balance reading close to full scale; (ii) remove the weight(s) M’and read the balance with the weight(s) M still on the pan, 91; (iv) remove all weights from the pan, and then replace weights Mand M% (v) _ remove the weight(s) M’ and read the balance with the weight(s) M still on the pan, 2; (vi) remove all weights from the pan, replace weight(s) Mand note the reading, py; (vii) remove all weights from the pan Repeat these steps to obtain a second set of readings ps, gz, qu and ps. The hysteresis is then given by: (> +2 + Ps + Pa)~(1 +42 +45 +44) hysteresis = ¥ ry 64) Note that if the readings are approximately equally spaced in time, the effects of any drift in the balance readings will be largely eliminated. If the balance has a high-resolution range then it should be used, if possible, when carrying out this test (by retaring the balance at load M if necessary). In the absence of drift, a simpler approach to measuring hysteresis is possible [1]: () zero the balance, 2/3 place a weight M, equal to half the balance range, on the pan, 75 (iii) add extra weight Mf to bring the balance reading close to full scale; (iv) remove the extra weight M and road the balance with A/still on the pan, 725 (v) remove Mand read the zero, 22.52 THE CALIBRATION OF WEIGHTS AND BALANCES Carry out the above procedure three times and calculate the average differences: (ry — 72) and (é1— 22). Take the hysteresis to be (r) — r2) provided it is numerically at least twice as large as the drift (2) —2). For dual or multi-range balances where the measuring system changes from range to range, the hysteresis should be measured for each range. For a given range, mass M now corresponds to the mid-point of the range, while mass M + M’is now close to the top of the range. 6.4 Recording and reporting the results of an electronic balance calibration Examples of the tests described in section 6.3 are given below, along with a sample report form. Alll examples are for a single-range balance with a maximum capacity of 1200 g and a resolution of 0.01 g. The procedures are easily extended to multi-range balances. ‘A class F, weight set is used to determine the corrections to balance reading. A calibration report gives the masses and corresponding uncertainties of these weights to be those shown in ‘Table 6.1, with a coverage factor of 2.04 for the uncertainties. The calculations could be made using either a calculator or a spreadsheet program. However a properly checked and protected spreadsheet is less susceptible to error. Table 6.1: The masses and corresponding uncertainties of the weights used in the example of an electronic balance calibration. The uncertainty coverage factor is 2.04. (200 indicates a second weight having a nominal mass of 200 g.) Nominal mass Mass Calibration uncertainty @ (g) 100 100.000 1 0.000 5 200 199.9977 0.000 9 200° 200.002 2 0,000 9 500 500.003 9 0,002 2 1000 1000.005 0 0.003 0CHAPTER 6. CALIBRATION OF ELECTRONIC BALANCES 33 64.1 Pre-adjustment check This consists of a measurement of the balance correction at a load of 1200 g. Pan load Reading Means Diterenes | onesies 0 0.00 1200.007 1200.00 1200.007 1199.99 1199,995 1199.995 0.012 0 0.00 0.00 6.4.2 Repeatability of measurement (example) The repeatability would normally be measured at full and half maximum capacity (1200 g and 600 g). However it is more conveniently measured at 1000 g and 500 g and this is acceptable as the load difference is only 17%. In the table of measurements below, M is nominally 1000 ¢ and all data are in grams. Number | Pan toad | Reading Measurement f= m2 1 0 0.00 (2) M 1000.03 (7) 1000.03 2 0 0.00 M 3000.03 1000.03 3 0 0.00 M 1000.03 1000.03 4 0 0.00 M 1000.04 1000.04. 5 0 0.00 M 1000.03 1000.03 6 0 0.00 M__| 100003 1000.03 7 0 0.00 M 1000.03 1000.03 g 0 0.00 M 1000.03 1000.03. 9 0 0.01 M 1000.03 1000.04 10 0 0.00 M 1000.03 1000.03 Using equation (6.2), the standard deviation s is found to be 0.0042 g, and since this is greater than 0.82a (which is 0.0041 g), s, is taken as 0.0042 g with nine degrees of freedom. The maximum’ difference between successive measurements is 0.01 g. A similar set of measurements is made at a nominal load of 500 g, and for the purpose of these examples it is assumed that the repeatability obtained at that load is 0.0041 g (based on the resolution).34 THE CALIBRATION OF WEIGHTS AND BALANCES 6.4.3 Corrections to balance reading (example) an load Reading Means Difference | oneton 0 0.00 100.000 (M;) 100.00 100.000 100.00 100.00 (r;) 100.00 0.000 oO 0.00 0.00 (z;) 199.998 200.01 199.998 200.01 200.01 200.01 0.012 0 0.00 0.00 299.998 300.01 299.998 300.01 300.01 300.01 0.012 0 0.00 0.00 400.000 400.02 400.000 400.02 400.02 400.02 0.020 0 0.00 0.00 500.004 500.03 500.004 500.03 500.03 500.03 0.026 0 0.00 0.00 600.004 600.03 600.004 600.04 600.035 600.03 0.026 0 0.01 0.005 700.002 700.05 700.002 700.04 700.045 700.035, 0,033 0 0.01 0.01 300.002, 800.05 800.002, 800.05 800.05 800.04 0.038 0 0.01 0.01 900.004 900.05 900.004 900.05 900.05 900.04 0.036 oO 0.01 0.01 1000.005 1000.04 1000.005 1000.04 1000.04 1000.03 0.025 oO 0.01 0.01 1100.005 1100.03 1100.005 1100.03 1100.03 1100.02 0.015 0 0.01 0.01 1200.007 1200.02 1200.007 1200.02 1200.02 1200.015 0.008 oO 0.00 0.005 All data in the table are in grams. The uncertainties of these corrections are calculated in section 8.1.CHAPTER 6. CALIBRATION OF ELECTRONIC BALANCES 55 6.4.4 Effect of off-centre loading (example) As a single weight should be used for this test, its nominal mass must be 500 g as 200 g is too small. However a suitable piece of metal of approximate mass 400 g could be used (see section 6.3.4), The readings are in grams. Back: 501.17 Left: 501.18 Centre: 501.18 Right: 501.19 Front: 501.20 Maximum difference = 0.03 g 6.4.5 Hysteresis (example) Two weights of mass M and M’ are used, where both masses are nominally 500g. The headings 1 and 2 refer to the first and second set of readings, and all data are in grams. The readings shown in brackets need not be recorded. Pan load 1 2 M1, Ps) 500.03 500.03 M+M! (1000.04) (1000.05) M (qn a9) $00.03 00.03 Zero (0.02) (0.02) M+M (1000.04) (1000.04) MG» 9), 500.03 500.02 Zero (0.02) (0.02) M(p2,pa) 500.03 500.03 (500.03 + 500.03 + 500.03 + 500.03) - (500.03 + 500.03 +500.03+500.02) _ 0.01 ; = = 0.0025 6.4.6 Sample report for an electronic balance Apart from the balance parameters described above, a calibration report for an electronic balance should quote the following: (a) the uncertainties of the corrections; (b) the Limit of Performance; and (c) the uncertainty of weighing (if requested by the user). ‘A sample report for the above balance appears on the following pages. Full details of the calculation of the uncertainty of correction and the uncertainty of weighing are given in sections 8.1.1 and 8,1.2, and the Limit of Performance is determined in section 8.1.3.56 THE CALIBRATION OF WEIGHTS AND BALANCES Page | of 3 National Measurement Institute Bradfield Road, Lindfield, NSW 2070, Australia Tel: (61 2) 8467 3600 Fax: (61 2) 8467 3610 REPORT ON An Electronic Balance Report no. RN 12344 Maker Mettler += Model_— 1200 Serial no. 13254 Capacity 1200 g Resolution (least digit) 0.01 g Type —Top-loading Client Examined at Examined by Calibration date National Measurement Institute, Bradfield Road, Lindfield, NSW 2070 Room C20E, National Measurement Institute EC Morris 28 November 2005 Date of issue of report 4 December 2005 ‘Temperature during test 20.4°C Pre-adjustment check Adjustment The correction to balance reading at 1200 g load before adjustment was found to be 0.012 g. Before calibration, the balance was adjusted according to the manufacturer’s instructions. Repeatability of measurement Corrections to balance reading Ref RN 12344 Load Repeatability of | Maximum difference between © measurement (g)_| _ successive measurements (g) _| 300 0.0041 0.00 1000 0.0042 0.01 Load Comection Uncertainty @) @® ) (gs) 100 0.000) 0.008 200 0.012 0.009 300 0.012 0.009) 400 =0.020 0.009) 500 0.026 0.009, 600 0.026 0.008. 700 0.033 0.008 800 0.038 0.008, 900 0.036 0.008) 1000 0.025 0.008 1100 0.015 0.008. 1200 ~0.008 0.008. Fite: CB/05/0835 Checked: x5 Date: 4 December 2005CHAPTER 6. CALIBRATION OF ELECTRONIC BALANCES 37 Poge 2 of 3 Off-centre loading A weight of mass 500 g was moved to various positions on the pan. Except for the Centre position, the weight was placed as close as possible to the edge of the pan without passing beyond the edge. The balance readings (in grams) at each position, relative to the centre reading, are given in the table below Centre Front Back Left Right | Maximum difference 0.00 +0.02 =0.01 0.00 40.01 0.03 Hysteresis Load Hysteresis @) 500 <0.01 Uncertainty of weighing of the balance ‘Load ‘Uncertainty (4) Load Uncertainty () @ @ @ © 100 0.012 700 0.012 200 0.012 800 0,012 300 0.012 900 0.012 400 0.012 1000 0.012 500 0.012 1100 0.032 600 0.012 1200 0.012 Limit of Performance for the balance: 0.055 g Notes 1. The balance has been tested according to procedures detailed in The calibration of weights and balances by EC Mortis and K Fen, National Measurement Institute, Lindfield, NSW, Australia . 2. When the sign of the correction is positive (+) the amount should be added to the balance reading to give the correct mass value and when negative (-) subtracted from it. 3. Any corrections for air buoyancy should be calculated by assuming that the object being weighed is balanced against hypothetical weights of density 8000 kgm”? in air of measured density. Ref RN 12344 File: CB/05/0835 Checked: xj Date: 4 December 200538 THE CALIBRATION OF WEIGHTS AND BALANCES Page 3 of 3 4, The Limit of Performance is the upper limit of the measurement error that may be expected when no corrections are made to the balance readings. 5. The uncertainty of weighing is the uncertainty of a single measurement of mass that is obtained after applying the corrections given in this report to the balance readings. 6. The uncertainty stated in this report has been calculated in accordance with principles in the ISO Guide to the Expression of Uncertainty in Measurement, and gives an interval estimated to have a level of confidence of 95%. The coverage factor for the interval is 2.0. The uncertainty applies at the time of measurement only and takes no account of any drift or other effects that may apply afterwards. When estimating the uncertainty at any later time, other relevant information should also be considered, including, where possible, the history of the performance of the instrument and the manufactures’s specifications. Ms K Fen for Dr B D Inglis Chief Metrologist t Ref RN 12344 File: CB/05/0835 Checked: x) Date: 4 December 2005CHAPTER 6, CALIBRATION OF ELECTRONIC BALANCES 59 6.5 Using a calibrated balance . 6.5.1 The normal procedure for measuring mass with a calibrated electronic balance There are various ways of using a calibrated balance, but in essence they all reduce to the following: * Allow the balance to warm up for the period recommended by the manufacturer, or at least 30 minutes if the recommended warm-up period is not known. Exercising the balance by placing a weight, of mass approximately equal to full load, on the pan is recomrfiended. * The object or material to be weighed should be placed close to the balance until approximate temperature equality with the balance is attained (see Table B.2 for the times required for weights). However close thermal equality is not very important for low precision (>30 ppm) weighing. * With the balance pan empty, note the zero reading, z). (The balance may be tared before this reading.) © With the object to be weighed on the pan, note the reading, 7). + One may make a second reading after lifting the object off the pan and replacing it, rz * Remove the object from the pan. If the balance readings are drifting, note the zero reading again, z2. * Take the zero reading z to be 2; unless a second zero reading is made, in which case calculate the average zero reading: z = (2; + 2,)/2. * Take the reading r to be r; unless a second reading is made, in which case calculate the average reading: r = (7 + 1r2V/2. +" If the balance Limit of Performance F is less than the maximum allowable uncertainty for the measurement, then the measured mass may be simply taken as: M=r-z (65) * Alternatively, the measured mass is obtained from equation (6.6) where Cy, is the correction to balance reading at load M. In this case, the uncertainty of the measurement may be quoted as + U, where U is the uncertainty of weighing of the balance at load M: M=r-z+Cy (66) The mass value obtained from a calibrated balance is the conventional mass. The value of the true mass is needed only in relatively rare circumstances (see section 2.5) and it can be obtained from the measured conventional mass using equation (2.6). The difference between true and conventional mass is explained in Chapter 2.60 THE CALIBRATION OF WEIGHTS AND BALANCES 6.5.2 User adjustment and tests on balances 6.5.2.1 Adjustment A balance should be adjusted at least monthly when in regular use (sce section 6.3.1). This ensures that the corrections to balance reading will be as close as possible to those obtained when the balance was calibrated. It is recommended that a pre-adjustment check be carried out by measuring the correction at the full scale of the balance. 6.5.2.2 Repeatability test The repeatability of measurement s, should be determined every six months (see section 6.3.2) to ensure that the balance has not developed a defect that will affect mass measurements. A single measurement near the top of the usual weighing range is sufficient for single-range balances, For multi-range balances, one determination in each range is recommended, The values obtained should be recorded so that the latest result s,(latest) can be compared with the previous result s,(previous). Ideally, this test should always be carried out by the same ‘operator. Assuming that the repeatability is always measured with nine degrees of freedom, then 5,(latest) should not exceed 1.78s,(previous). Furthermore, s,(latest) should not be greater than twice the repeatability given in the most recent calibration report for the balance. If these requirements are not met, then there is a fairly strong indication that the performance of the balance has deteriorated. The user should consult the calibrating laboratory to see if calibration, servicing or some other action is required. ‘A more sophisticated version of this test is possible, in which the previously measured values of the repeatability are pooled. See Appendix G for details, and note that it may not be advisable to include measurements made before the most recent balance calibration in the pool. This version of the test gives a better indication of any problem arising with the balance. 6.5.2.3 A check on the correction to reading Using a suitable calibrated weight of mass M, the correction to reading at load M should be measured following the procedure of section 6.3.3 and using equation (6.3). Ideally M will be at least one-third the full balance range and its uncertainty Uj, will be small compared with the unceriainty of correction. This check should be carried out monthly at a single point, though multi-range balances should be checked at one point in each range. ‘The difference AC between the correction given in the latest calibration report and the value obtained in this test should be numerically less than the combined uncertainty of its measurement. Using an approximation that is good enough for the purposes of this check, it is required that:CHAPTER 6, CALIBRATION OF ELECTRONIC BALANCES 61 lac] < fu? +25? +03, (6.7) where U is the uncertainty of the correction at load M. If this condition is not satisfied, then there is a fairly strong indication that the balance needs recalibration. 6.5.3 Air buoyancy and weighing All objects exposed to the atmosphere are subject to buoyancy, an upwards force equal to the gravitational attraction acting on the mass of air displaced by the object. Thus the buoyancy varies with the volume of an object and hence, for objects of the same mass, inversely as their density. Since the corrections to balance reading given in a report were obtained using standard weights with a density of approximately 8000 kg.m™, they will be in error when weighing materials of different density, because of the different buoyancy. This buoyancy error will be small for dense materials (e.g. brass, steel, lead) and greatest for materials with a density of 1000 kg.m” or less (e.g. water, oil, wood, cork). Errors are also introduced by variations in air density. Fortunately the accuracy required when weighing light materials is usually low enough to allow these errors to be ignored. If an object of mass M having a density p is weighed in air of density g, on an electronic balance that was calibrated at a time when the air density was (cal), then the correction 5M that must be added to the measured mass to account for the buoyancy error is: (68) (Generally the density of ait need only be determined with an uncertainty of 1%, which is achieved by measuring the air temperature, pressure and humidity with instruments of modest accuracy, See Appendix H for further details. If the required uncertainty of mass measurement is not very demanding, then the air density can be obtained from Table J.1) For a laboratory with reasonable temperature control, the air density typically varies over a total range of + 0.04kg.m® from the average value, due largely to changes in atmospheric pressure. The magnitude of the buoyancy correction is best seen by considering the examples in Table 6.2. The shaded rows show worst-case scenarios, while the unshaded rows show situations that could easily occur in practice. Notice that for a dense material such as brass, the correction is relatively small and varies only moderately with altitude. For water on the other hand, the correction is much larger and can increase rapidly with altitude. When weighing water on a calibrated electronic balance at an altitude of 700m, the buoyancy correction will usually be in the order of 0.01%. Lighter materials such as wood will require even greater corrections. If it is necessary to weigh light materials with 2 mass uncertainty in the order of 40.05% or less, estimate the likely size buoyancy correction as follows: for the altitude of the laboratory, find the mean value of p, (Table J.1 may be used for this purpose). Then substitute this value62 ‘THE CALIBRATION OF WEIGHTS AND BALANCES into equation (6.8) for both p, and p,(cal), while putting p equal to the density of the material being weighed. For instance, Table J.1 indicates that the mean laboratory air density at 700 m is 1.099 kg.m’°, Substituting this value into the equation for p, and p.(cal), and putting p equal to 1000 kg.m™, one obtains 0.009% for the estimate of the buoyancy correction when weighing water. Table 6.2: Examples of the buoyancy correction for an electronic balance, calculated from equation (6.8). All symbols have the same meaning as in that equation. ‘The shaded rows show worst-case scenarios. Altimde | Material (my weighed OMIM: peal) (ppm) e (gin) (kgm) —106 If the correction calculated in the previous paragraph represents a serious error if ignored, then corrections determined from equation (6.8) will have to be applied. Consequently the air density at the time of the balance calibration (as well as at the time of mass measurement) should be known; preferably it will be stated on the balance calibration report. 6.5.4 Minimum mass for a calibrated balance In some industries, such as the pharmaceutical industry, users sometimes need to achieve a certain relative uncertainty such as 0.1%. When the quantities become smaller and smaller, a poiat will be reached below which the required relative uncertainty can no longer be achieved. This point is the minimum mass. The minimum mass My», can be calculated from the equation: F M,,, =——> “™ U(rel) where F is the Limit of Performance or the uncertainty of weighing of the balance and U(rel) is the required relative uncertainty. Some balances have a facility, which warns the user when the mass being weighed is less than the minimum mass.CHAPTER 6. CALIBRATION OF ELECTRONIC BALANCES 63 6.6 Measuring corrections to balance reading when a full set of calibrated weights is not available When using the procedures described in this section, one should continue to use an adjustment weight with a mass approximately equal to the full range of the balance. In theory one could use the procedure of section 6.6.1 to adjust the balance, but this is not recommended, partly because it is prone to error and partly because it means that a full calibration of the balance corrections would be required whenever one wanted to check the adjustment. When using the procedure of section 6.6.2, one must use a calibrated adjustment weight in order to measure the full-scale correction. A sot of uncalibrated weights, called tare weights, are also needed to make up sub-multiples of the balance’s full range. Ideally, these weights would all have masses nominally equal to one- tenth the range of the balance. 6.6.1 One calibrated weight is available The calibrated weight should have a mass M that is approximately one-tenth the range of the balance, though a smaller fraction such as 1/12 or 1/15 is acceptable. The uncertainty associated with M should be less than the resolution of the balance. The procedure is as follows: @ Read the zero. (ii) Place the calibrated weight on the pan and note the reading. Remove the weight momentarily, then replace it and note the new reading. Average the two readings to obtain 7). Remove the weight and read the zero — this reading is averaged with the reading in (j) to give the zero value, z). iv) Place tare weights on the pan until a reading close to r, is displayed. This effectively becomes a ‘zero’ reading, like that in (j). () Add the calibrated weight to the pan and note the reading. Remove the calibrated weight only, then replace it and note the new reading, Average these readings to obtain rn (vi) Remove the calibrated weight and read the ‘zero’ — this reading is averaged with the reading in (iv) to give the zero value, 22. Place additional tare weights on the pan until a reading close to r2 is displayed. Add the calibrated weight to the pan and take two readings as in (v) above. Average the readings to obtain rs. (ix) Remove the calibrated weight and read the ‘zero’ — this reading is averaged with the reading in (vii) to give the zero value, 2). (%) Continue in this way until the capacity of the balance is reached. ‘The additional balance correction for each step is given by: ¢,=M-(7,-2,) 69)64 THE CALIBRATION OF WEIGHTS AND BALANCES and the total correction for the Joad iM is found by adding the first i additional corrections: C= tet = te = M-Y,-z,) (6.10) a Multi-range balances should be treated in the manner described at the end of section 6.3.3. An example of this test as far as the fourth correction is given in the table below. The calibrated weight has a mass of 100.001 g, and the quantities Mj, M;, etc. refer to the tare weights. Ail data in the table are in grams. The uncertainties of the corrections C; are calculated in section 8.1.1.3.1. a Additional - is Difference , ‘Cumulative Pan load Reading Means on correction orreetion M= (7-2) 0 0.00 100.001 100.00 100.001 100.00 100.00 (ri) |" 100.000 0.001 0.001 0 0.00 0.00 (z,) Mi 100.02 ‘M,+100.001 | 200.03 ‘M,+100.001 | 200.03 200.03 100.010 0.009 0.008 M, 100.02 100.02 M; 200.05 ‘M;+100.001 | 300.05 M,+100.001 | 300.06 300.055 100.005 -0.004 0.012 M, 200.05 200.05 A 300.01 ‘Ms+100.001 | 400.01 ‘Ms+100.001 | 400.01 400.01 100.000, 0.001 0.011 My 300.01 300.01 6.6.2 No calibrated weight (apart from the adjustment weight) is available ‘The designated tare weight referred to below should have a mass that is approximately one- tenth the range of the balance, though a smaller fraction such as 1/12 or 1/15 is acceptable. When adjusting the balance, the correction S at full scale must be measured. For an adjustment process which sets the balance reading to exactly the nominal full scale value, S is given by: S=nominal full scale mass — calibrated mass of the adjustment weight Altematively, S could be measured by double weighing using the adjustment weight. Normally, Swill be very small.CHAPTER 6, CALIBRATION OF ELECTRONIC BALANCES 65 The procedure is as follows: @ Read the zero. (i) Place'a designated tare weight (call it weight a) on the pan and note the reading. Remove weight a momentarily, then replace it and note the new reading. Average the two readings to obtain 7). (iii) Remove weight a and read the zero — this reading is averaged with the reading in (i) to give the zero value, 27. (iv) Place tare weights on the pan until a reading close to r; is displayed. This effectively becomes a ‘zero’ reading, like that in (i). (v) Add weight a to the pan and note the reading. Remove weight a only then replace it and note the new reading. Average these readings to obtain 73. (vi) Remove weight a and read the ‘zero’— this reading is averaged with the reading in (iv) to give the zero value, 22. (vii) Place additional tare weights on the pan until a reading close to r» is displayed. (viii) Add weight a to the pan and take two readings as in (v) above. Average the readings to obtain 75, (ix) Remove weight a and read the ‘zero’— this reading is averaged with the reading in (vii) to give the zero value, 25, (x) Continue in this way until the capacity of the balance is reached. Supposing the mass of weight A to be M, then equations (6.9) and (6.10) will still be valid. Therefore, from equation (6.10): Cc, = mM->(,-2z,) = 8 (6.11) a where 7 is the number of points at which the balance correction is measured. Hence: M UseXb, -«)} (6.12) Sat and using this value of M, the ? correction can be found from equation (6.10). An example of the calculation of the uncertainty of the correction C; is given in section 8.1.1.3.2. Multi-range balances should be treated in the manner described at the end of section 6.3.3.THE CALIBRATION OF WEIGHTS AND BALANCES 1,0743857323856347 kg anceChapter 7 Calibration of single-pan, two-knife-edge balances 7.1 What is a single-pan two-knife-edge balance? A Single-pan two-knife-edge balance is one that compares the mass of the object on the balance pan with the mass of built-in weights. The dials move the built-in weights off the pan support to restore balance. An optical scale displays the small mass difference between the object and these weights. The mass of the object being weighed can be read directly from the dial readings and the optical scale. Sometimes the optical scale is replaced with an electronic readout, Although there may be a digital readout, it is not an electronic balance as described in Chapter 6. The optical scale or the electronic display is normally less than 1% of the full range of the balance. See Appendix K for more details of the construction of single-pan two-knife- edge balances. 7.2 The scope and purpose of the calibration The main purpose of a balance calibration is an estimation of the accuracy of measurements made on the balance. However balance calibrations have three other important functions: (a) _A table of corrections to the balance readings is provided. (b) The user should have information on the limitations of the balance, principally the effects of off-centre loading and hysteresis. This information sometimes acts as a diagnostic indicating that repairs may be required, (©) The balance report should contain information that allows the user to carry out effective checks on the balance between calibrations. The repeatability of reading is important in this regard. 7.3 Balance calibration Because this type of balance usually has built-in weights and compares gravitational forces, moving from one place to another should have little effect on the balance reading. Nevertheless, it should be calibrated in the position where it is to be used to account for environmental changes. It should not be sent to a calibrating laboratory for calibration. If a 6768 THE CALIBRATION OF WEIGHTS AND BALANCES balance is moved after calibration, the user checks of section 7.5.2 should be carried out to see whether a recalibration is necessary. Where calibrated weights are used in the calibration, the density of the weights should be in the vicinity of 8000 ke’, The accuracy of the balance determines how close the density must be to this value. This is usually not a problem provided the weights are made of stainless steel, brass or bronze, but to be quite sure that the weight density is acceptable, use weights conforming to a standard, such as the OIML classification [3]. For example, to calibrate a L kilogram balance to have an uncertainty of weighing of £75 mg, an OIML M, weight set could be used since the maximum mass uncertainty of the weights used is #17 mg and they have an acceptable density for this level of uncertainty. When weights are transported to a laboratory for the purpose of calibrating a balance, care must be taken that they do not become excessively watm or cool relative to the likely temperature of the balance. For instance, if the vehicle used is not air-conditioned, one should consider putting the weights in a thermally insulated container. Table B.2 in Appendix B shows how long one may have to weight if the weights do become cool or warm. 7.3.1 Optical (or digital) scale check Check the optical (or digital) scale of the balance. This process is usually manual and should be done monthly if the balance is in regular use. It is done by zeroing the balance, placing a weight equal to the full optical scale value on the pan and checking that the optical scale displays the correct mass for this weight. This can be done at any load and zero load is chosen for convenience. If the optical scale is significantly in error, the balance will need to be adjusted, though such adjustment is rarely needed for a balance in good condition. To adjust the balance, use the sensitivity adjustment screw (see Figure K.2) located under the cover of the balance. 7.3.2 Repeatability of measurement The repeatability of measurement s, of a balance is the standard uncertainty associated with a single mass measurement. When using a calibrated balance, a single mass measurement consists of two readings — a zero reading z, and a reading r with the object whose mass is to be measured on the pan. The readings for repeatability measurement must be obtained in a way that realistically reflects how a balance is used in practice. These balances weigh at approximately constant load so there is no need to perform repeatability tests with weights over the full range of the balance, The repeatability should be measured with weights near half the capacity of the balance and at both ends of the optical scale. This is to account for the change in effective shape of the knife edges. The most realistic way to assess the repeatability is to remove and replace the weight on the pan for each load tested. This causes a greater disturbance to the balance than merely releasing and arresting it.CHAPTER 7. CALIBRATION OF SINGLE-PAN, TWO-KNIFE-EDGE BALANCES 69 To measures,, one therefore starts by calculating the standard deviation s of m mass measurements, the difference between the zero optical scale reading of the balance (z,) and the reading with a weight on the pan (7;), the i” such measurement 6M; being: 6M, = 7; Ql) ‘Thus, if the average value of 5M is OM. s 72) The recommended minimum number of measurements (ie. the minimum value of » in equation 7.2) is 10, in which case, s has nine degrees of freedom. ‘The measured standard deviation s usually provides a good value for the standard uncertainty and hence the repeatability, in which case one could simply equate s, to s. Single-pan balances are not normally resohtition-limited — they don’t normally give the same reading many times when the same weight is placed on the pan — but if they are then 5 may not be a good value for s,.. Asa consequence of this, the repeatability should always be determined as follows: If a is the resolution semi-range of the optical scale, then s, is equal to s (with nine degrees of freedom), or equal to 0.82a (with 1000 degrees of freedom), whichever is the greater. (See Appendix M for a brief discussion of resolution and its effect on the measurement of balance repeatability.) 7.3.3 Corrections to balance reading Corrections may need to be applied to the balance readings, which are the combination of the dial readings and the optical scale readings. Even though a single-pan two-knife-edge balance has been adjusted to read correctly close to the full optical scale, it may still be necessary to apply corrections to the readings, for two reasons: (a) The optical scale reading as function of load may be significantly non-linear. (b) The mass of the built-in weights may differ significantly from their nominal values. (The corrections to the dial readings are actually the departure of the mass of the built- in weights from their nominal values.) When corrections are not needed, one should know whether the balance readings conform to the tolerances claimed by the manufacturer, or whether the balance is accurate enough for its intended use.70 THE CALIBRATION OF WEIGHTS AND BALANCES 7.3.3.1 Optical (or digital) scale The purpose of calibration is to measure the correction that needs to be applied to the balance reading, Readings at 5 points on the optical scale are adequate. A set of calibrated weights with an uncertainty less than the resolution of the balance is required for the calibration. The corrections should be determined at a number of points, say 5, over the range of the optical scale by successively placing small calibrated weights on the pan and observing the optical scale readings. Ideally, the calibrated weights will have nominal mass values equal to multiples of one fifth of the full optical range. The steps are: (® With all dials set to zero, release the balance and note the first zero reading. (i) Place the weight(s) of mass M; (where M; is approximately one fifth of the full optical range for the first step) on the pan and note the reading. - (iii) Remove the weight(s) momentarily, then replace them on the pan and note the new reading. This reading is averaged with the one in (ii) to give, r7. (iv), Remove the weight(s) and re-read the zero — this reading is averaged with the reading ~~ in (@ to give the zero reading for the calculation, z). (¥) Repeat steps (ii) and (iv) to cover the whole optical scale. If reading 7, and 2) correspond to weight(s) of total calibrated mass M; on the pan, then the correction to the optical scale reading for this load is given by: C,=M,-(,~-2,) (73) ‘The correction is the mass value that should be added to the optical scale reading to give the correct mass when a reading is made at that point of the optical scale, 7.3.3.2 Dial readings Alll single-pan, two-knife-edge balances have weights installed in the balance. Some balances have three or even four decades of weights and a full calibration can be very time consuming. Removing the built-in weights from the balance for calibration is generally not recommended as it will risk scratching the weights during replacement. ‘There are a number of possible methods of performing a calibration on these built-in weights in situ. These will be described in the following sections, @ Simple tolerance test — check the conformance to manufacturer’s tolerance, simpler than comprehensive tolerance test. In use, no correction is applied during mass measurement. (i) Comprehensive tolerance test —check the conformance to manufacturer’s tolerance, using the method proposed in ASTM standard E319 [7]. In use, no correction is applied during mass measurement.CHAPTER ?. CALIBRATION OF SINGLE-PAN, TWO-KNIFE-EDGE BALANCES n (iii) Direct calibration — easy and straightforward method. Corrections are applied to the balance readings during mass measurement. (iv) Least-squares calibration — most accurate method. Corrections are applied to the balance readings during mass measurement. In the following sections, the simple tolerance test and the direct calibration method will be described. For the user who requires more accurate mass measurement, corrections should be applied to the balance readings and least-squares calibration should be used for balance calibration. Comprehensive tolerance test and least-squares calibration will be discussed at the end of this chapter and in Appendix E respectively. The calibration requires that the combination of weights used for a particular load must have an uncertainty not greater than the standard deviation of the balance. Note that when calibrating a balance with built-in weights it is very important to distinguish between the value indicated by the balance (or the value of the built-in weights), and the reading obtained when a standard weight is placed on the pan. An example will help make this clear. . Consider a dial setting of 20 g. During calibration, a 20 g standard is placed on the pan and the balance reads 20.01 g. If. standard of mass 19.99 g were placed on the pan the balance would read 20.00 g, Therefore the true value associated with the 20 g dial setting is 19.99 g, not 20.01 g. In other words, the balance has a correction of ~0.01 g at 20 g. The actual value of the built- in weight (or weights) is also 19.99 g. This is apparent because placing 19.99 g on the pan and lifting the *20 g” built-in weight off the pan leaves the reading unchanged. In reporting the result of the calibration of the built-in weights, it is important to give the mass valué for the dial setting, or the corresponding correction, Here the correction: value of the standard — balance reading 20.00 ~ 20.01 =-0.01 g. In either case the user has merely to add up the true values for the dial settings or the corrections used to obtain the correct mass of the object being weighed. In the above example the reading of 20.01 g should nor be given in the Report as this will almost certainly result in the wrong value being used in calculating the mass. When more than one dial setting is used, which is the usual case in practice, the corrections or mass values for each dial reading are added together to give the total correction or value, respectively. (a) Simple tolerance test In general, there are very few balance users who actually apply corrections for the dial readings. Most want to know whether the corrections to the dial readings conform to the tolerances laid down by the manufacturer, or whether the balance is sufficiently accurate for their purpose without applying corrections.R THE CALIBRATION OF WEIGHTS AND BALANCES The quickest way to check the tolerances is to set the dial reading so that all the built-in weights from one decade are lifted from the beam (eg. position 9 or 90, etc.), place standards of equivalent value on the pan and read the difference. In some combinations not all the weights from the same decade are lifted off at position 9 and a'second dial setting is required to ensure that this happens. It is possible (although unlikely) to have two large errors that cancel. This method only gives one correction for each decade of the built-in weights. The maximum correction fiom the measurements of all decades is reported. Therefore it is used for checking the conformance of the balance rather than applying corrections. If corrections are applied, the methods outlined in 7.3.3.2.2 or Appendix E should be used. (b) Calibration of each dial setting by direct calibration ‘This involves measuring the correction for each dial setting by using appropriate weights from a calibrated set. The method is described in the following steps: (®__withall dials set to zero and no load on the pan, release the balance and note the reading, 27; (ii) “sot the “I” on the dial to be tested, place a calibrated weight of equivalent value on the pan, release the balance and note the reading, r; (iii) arrest the balance, remove the weight and replace it, release the balance and note the reading r»; (iv) __ return the dial to zero, remove the weight from the pan and read the zero, 22, this becomes the first zero reading for the next dial setting, R, to be calibrated; (v) repeat steps (ii) to (iv) for all the dial settings of the balance. The correction C to the dial setting R is calculated by means of the following formula: C=M-[6 +7)/2-(,+2,)/2]-R (14) where Mis the value of the calibrating weight. ‘This formula yields the amount that must be added to the balance reading to give the correct value whenever this dial setting is used. The value of C may be positive or negative. Usually the mass value of the calibrated weight is close to that of the dial setting and it is not necessary to apply any corrections, This method does not provide any safeguards against misreading the balance’ or arithmetical errors, but it has the advantage of being relatively easy and straightforward to use. 7.3.4 Effect of off-centre loading When the centre of mass of the object being weighed is off-centre on the pan, shift or comer- load error may occur. It is difficult to produce figures that can be used to correct the balance readings because the effect is not always linear with respect to either load ot position. This test is designed to enable the user to decide how accurately objects must be positioned on the pan for this effect to be negligible. If the measured errors are large compared with the manufacturer’ specification, the balance is probably in need of repair.