Dissemination of South African Mass Standards from the National Prototype

R.T. Mautjana NMISA Private Bag x 34, Lynwood Ridge, 0040, South Africa Email:tmautjana@nmisa.org Phone: +27 12 841 4798 Fax: +27 12 841 2131 Abstract The South African national standard for mass, prototype No.56 of the Kilogram is a cylinder of platinum-iridium alloy maintained by NMISA and is calibrated once in ten years at the BIPM. It is traceable to the international prototype in BIPM and it is currently serving as a national primary standard of mass. The mandate of the NMISA Mass laboratory is to maintain and disseminate the value of the kilogram. To ensure this NMISA utilises two high quality (Class E1) weights as transfer standards calibrated against the prototype using an automated system and a double substitution method of measurements. Other working standards, ranging from 1mg to 20kg, are also utilised. The working standards are calibrated by sub-division and multiplication methods using a single reference standard. This paper presents the multiple and sub-multiple methods used at the NMISA to disseminate the value of the kilogram and provide traceability of customer standards. 1. Introduction National Metrology Institute of South Africa (NMISA) Mass laboratorys mandate is to maintain and disseminate the value of kilogram. To ensure this NMISA possess copy No 56, a platinum-iridium alloy cylinder traceable to the international prototype maintained by Bureau International des Poids et Mesures (BIPM). The prototype is calibrated once in 10 years at the BIPM and it is currently serving as the national primary mass standard for South Africa. To disseminate the kilogram NMISA utilise two 1kg stainless steel E1 weights which are used as transfer standards. The transfer standards are calibrated directly against the prototype on an automated system and are used for dissemination of traceability to the SI unit of mass. In addition there are a number of stainless steel working standards ranging from 1mg to 20kg, which are calibrated by sub-division and multiplication methods against one of the transfer standards. The working standards are used to calibrate the customer reference weights. All measurements are carried out using substitution method on digital electronic balances or comparators. In the substitution weighing the test weight is compared against the standard weight of a similar nominal value, by placing them on the balance pan in turns. 2. Calibration Methodology The accurate mass determination of multiples of a unit may be attained by employing weighing designs that lead to an orthogonal system of normal equations i.e. a system which produces no variances or covariances [5]. Weighing designs are used to calibrate a set of weights (particularly E class weights) using one reference weight. The weighing designs have the following advantages: a) Less use of reference weights

b) New calibration values for the check weights every time they are used in the decade c) Calibration is consistent for a set of weights d) More measurements than unknowns. However sometimes they require placing of several weights on the balance pan and more comparisons to be performed. The evaluation of the results and associated uncertainties may become complicated [2, 3]. Normally weights for calibration are grouped in series of weights, called decades. The calibration of a decade of 5,2,2,1 structure (where 5 may refers to 5kg, 500g....to 5mg) is carried out through comparisons between a head weight standard and combinations of weights which sum gives the same nominal value of the head weight standard. A head weight of a decade becomes the closure weight for the next decade going up. For example, 10g is the head weight for 5g, 2g, 2g*, 1g but it is the closure for 50g, 20g, 20*, 10g decade with a head weight of 100g. A decade usually includes a check weight a reference standard weight used to verify the values assigned to the test weights [3]. In the 5,2,2*,1 decade structure the check weight is (1)*. Note: The use of * - indicates a check weight standard or a replica of another standard weight with same nominal value. The normal equations associated with the calibration of a set of weights from 5kg to 1mg using 1 kg as a standard weight are presented in Table 1.
Table 1. Normal system of equations

(10) (10) (5) (5) (2)+(1) (2)+(1)* (2) (2)*

= = = = = = = =

(5) + (5) +

(2) + (2) + (2) + (2) +

(2)* + (2)* + (2)* + (2)* + (2)* + (2)* +

(1) (1)* (1) + (1)* + (1)* + (1) + (1) + (1) + (1)* + (1)* +

a1 a2 a3 a4 a5 a6 a7 a8

Note: a1 to a8 refers to the differences observed from the balance display. To determine the values of all the unknown weights the normal equations would have to be orthogonal (i.e. without variances). To ensure orthogonality some of the equations may be omitted and some used more than once [1]. The system in Table 2 below is orthogonal [1,4,6].

Table 2. Orthogonal system of equations

(10) (10) (10) (5) (5) (2+1) (2+1)

= = = = = = =

M (5) + (5) + (2) + (2) + (2) + (2) + (2)* + (2)* + (2)* + (2)* + (2)* + (2)* + (2)* + (2)* + (1) + (1) + (1) + (1) + (1) + (1) + (1)* + (1)* + (1)* + (1)* + (1) + (1)* + (1)* + (1)* + (1) (1)* a1 a2 a3 a4 a5 a9 a6 a10 a7 a11 a8 a12

(2)+(1)* = (2)+(1)* = (2) (2) (2)* (2)* = = = =

The use of the orthogonal system in the calibration of weights leads to higher accuracies. The system was first introduced in 1935 by B Lenk and later popularised by M Grabe in 1978 [1]. A natural system can only be transformed into an orthogonal system only under the condition that the highest mass of the set is to be considered the defining mass [1]. Hence in Table 2, (10) is taken to be the defining mass with a nominal of 10kg. 2.1 Sub-division method of calibration In the subdivision method, weights are sub-multiples of 1kg and the reference weight is 1kg. Determining the values for 500g to 1mg, as depicted in Table 2, will require the following five equations:
1

Where (10) is the certificate value of the 1kg and (1)* is the check weight. The 500g weight is calculated from the sum of the first four equations from Table 2 which contains (5). Similarly, the 200g weight is calculated from the first seven equations which contain (2).

Moreover, the 100g weight is calculated from the first six equations containing (1) from Table 2. In a second decade of 50g, 20g, 20g* and 10g, the value of the 100g weight calculated from the 1st decade would be the reference (head weight) standard. Similarly, the 10g weight would be the reference for the 5g, 2g, 2g* and 1g decade etc.
2.2 Multiplication method of calibration In this case the test weights to be calibrated are multiples of 1kg, for example 10kg, 5kg, 2kg and 2kg*. The weighing design is the same as for the sub-multiplication and therefore (10) would refer to 10kg, (5) to 5kg and (1) to 1kg. However the mass of 10kg is not known, therefore it is assumed to define an arbitrary internal unit u. In terms of Table 2, (10) = M = 10u, which implies u = (1), therefore the mass of (10) = 10(1). Equation 4 & 5 are used to compare the results of (10). Knowing the value of the 10kg, equations 1 to 5 are used to calculate the values of 5kg, 2kg, 2kg*, 1kg and 1*kg respectively. It should be noted that the method presented covers the range 1mg to 10kg. Larger weights are compared directly with a collection of calibrated smaller weights which add to the same nominal value. For example a 20kg is compared directly against two calibrated 10kg weights.

2.3 Calculation of uncertainty The uncertainty of the test weights (5), (2), (2)* and (1) is composed of uncertainties associated with the following: mass of the reference standard, air buoyancy correction, the instrument used, drift of the reference weight, densities of the reference & test weights and the uncertainty due to the weighing process. They are added together and multiplied with cover factor (k=2) to get the expanded uncertainty [4]. 3. Traceability of mass standards to the SI unit The primary mass standard of South Africa is copy number 56 of the international prototype. It is kept under two bell jars in a safe at NMISA. Since it was purchased in 1954 it has been calibrated seven times at the BIPM. The uncertainty of the last calibration in 2005 is 5 g. The Table 3 below indicates the recent dates of calibration and the measurements obtained. Table 3. Mass of Prototype No. 56 carried out at BIPM Date 1986 1993 1998 2005 Mass (g) 1000,000 237 1000,000 240 1000,000 241 1000,000 255 Uncertainty ( g) 8 2,3 4 5

Currently NMISA utilises two high quality (Class E1) 1kg stainless steel weights, which are calibrated by direct comparison against number 56 every five years, on an automated 1kg comparator. The automated system has a resolution of 1 g with a repeatability of 2 g. The automated system can inter-compares four weights at a time. The measurements are carried

out by double substitution method (ABBA). Double substitution is when a test weight (B) is compared with a standard (A) of similar nominal value by placing them in turns on the balance pan, following the order A1B1B2A2. It is important that B1 and B2 measurements are independent of each other. The expanded uncertainty of the transfer standards at about 95% confidence level is 50 g, mainly due to the effect of buoyancy because of differences in densities, for example prototype 56 =21542 kg/m3 while stainless steel =7950 kg/m3. Traceability of the mass standard is given by figure 1 below indicating how customer weights are linked to the national prototype:

Prototype No. 56

Stainless Steel (SS) 1kg Transfer Standards

E1 SS 10kg-1mg Working Standards

E2 SS 20kg-1mg Working Standards

E2 Customer Standards

F1 SS 20kg-1mg Working Standards

F1 Customer Standards

Figure 1. Traceability of mass standards

4. Conclusion Weighing designs which leads to orthogonality of normal equations are very significant in calibration as they results in zero variances and least usage of the standard weights. They are the most accurate method to use in calibration of weights of high quality. They also results in new calibration values for the check weights every time they are used in decades. 5. References 1. G. Mihailov, and M. Romanowski, Calibration of the Multiples of the Unit of Mass, Metrologia, 1990, 27, 17 to18. 2. E.C. Morris, and K.M. Fen, Calibration of Weights and Balances, 2004, National Measurements Laboratory CSIRO, ISBN 0-9750744-3-1 3. S. Davidson, M. Perkin, and M. Buckley, Measurement Good Practice Guide No.71, The measurement of Mass and Weight, 2004, National Physical Laboratory, UK, ISSN 1368-6550 4. M. Goutaman, and L. Tripurari, Calibration Technique of a Set of Weights using one Reference Standard, Journal of Metrology Society of India, 2008, 23 (1), 55 to58 5. W.G. Lee, Calibration designs for mass standards for two comparators in a decade, Metrologia, 2002, 39, 337 to 341. 6. G. Chapman, Weighing Designs and Weight Scales, Mass course notes, NMISA, South Africa, May 2001, 1 to 20.