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Micro-mass standards to calibrate the sensitivity of mass comparators

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2007 Metrologia 44 266
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IOP PUBLISHING

METROLOGIA

Metrologia 44 (2007) 266274

doi:10.1088/0026-1394/44/5/002

Micro-mass standards to calibrate the


sensitivity of mass comparators
Tanguy Madec, Gaelle Mann, Paul-Andre Meury and
Thierry Rabault
LNE, 1 rue Gaston Boissier, 75724 Paris cedex 15, France
E-mail: tanguy.madec@lne.fr, gaelle.mann@lne.fr and paul-andre.meury@lne.fr

Received 23 February 2007


Published 31 August 2007
Online at stacks.iop.org/Met/44/266
Abstract
In mass metrology, the standards currently used are calibrated by a chain of
comparisons, performed using mass comparators, that extends ultimately
from the international prototype (which is the definition of the unit of mass)
to the standards in routine use. The differences measured in the course of
these comparisons become smaller and smaller as the standards approach
the definitions of their units, precisely because of how accurately they have
been adjusted.
One source of uncertainty in the determination of the difference of mass
between the mass compared and the reference mass is the sensitivity error of
the comparator used. Unfortunately, in the market there are no mass
standards small enough (of the order of a few hundreds of micrograms) for a
valid evaluation of this source of uncertainty. The users of these
comparators therefore have no choice but to rely on the characteristics
claimed by the makers of the comparators, or else to determine this
sensitivity error at higher values (at least 1 mg) and interpolate from this
result to smaller differences of mass.
For this reason, the LNE decided to produce and calibrate micro-mass
standards having nominal values between 100 g and 900 g. These
standards were developed, then tested in multiple comparisons on an A5
type automatic comparator. They have since been qualified and calibrated in
a weighing design, repeatedly and over an extended period of time, to
establish their stability with respect to oxidation and the harmlessness of the
handling and storage procedure associated with their use. Finally, the
micro-standards so qualified were used to characterize the sensitivity errors
of two of the LNEs mass comparators, including the one used to tie
Frances Platinum reference standard (Pt 35) to stainless steel and superalloy
standards.
(Some figures in this article are in colour only in the electronic version)

1. Creation of the micro-mass standards


1.1. Choice of material
Two characteristics prevailed in the choice of material:
a metal having a low density, in order to make the size of
the standard reasonablenot smaller than the resolving
power of the eye (so as not to have to use an optical
instrument to locate the micro-standards once made), and
0026-1394/07/050266+09$30.00

packaging of the material in the form of a coil of wire, to


allow adjustment by measurement of the length.
The metal chosen was an aluminium alloy containing
1% silicon and having a theoretical density of 2700 kg m3 .
A calibration was performed on a five metre sample by
hydrostatic weighing and confirmed the density to be (2692
14) kg m3 in
coils of wire 0.050 mm for 100 g, 200 g and 300 g
(length from 19 mm to 57 mm),

2007 BIPM and IOP Publishing Ltd

Printed in the UK

266

Micro-mass standards to calibrate the sensitivity of mass comparators

Figure 1. Examples of micro-mass standards.

coils of wire 0.120 mm for 400 g to 900 g (length from


12 mm to 27 mm).
1.2. Adjustment of the micro-mass standards
A sample 100 mm long was taken from each coil for the
determination by gravimetry of the mass per unit length of
each type of wire.
A clamping tool was used to hold the selected wire taut
between two jaws of which the spacing was adjusted using
a calliper to the length corresponding to the chosen nominal
mass. The wire was cut to length flush with the jaws, using
a well-sharpened cutter, thereby adjusting the masses of the
micro-standards to within 2 g and on average 0.8 g.
They were immediately checked by weighing on a UMX5
comparator having a capacity of 5 g and a resolution of 0.1 g.
1.3. Shape of the micro-mass standards
Various shapes were produced by bending to ensure
compatibility with the use of the A5 automatic comparator
and its robot. After a few trials, the most convenient shapes
were found to be
a lozenge open at the bottom,
an inverted vee (chevron) and
a triangle with double horizontal bar.
Duplicates were differentiated by beaks (folds towards the
exterior or the interior) on one of their bottom ends; this
was done without unbalancing the micro-standards, in order
to avoid problems when they are picked up by the robot of the
A5 (see figure 1).
1.4. Handling of the micro-mass standards
Given the fragility of the micro-standards, because of their
shape and the lack of hardness of the material of which they
are made, handling with tweezers was ruled out from the start.
Aluminium alloy rods ending in hooks were made for the
transfer to the support trolleys of the A5 comparator, with a
longer handle for loading on the M-one. A special tray for the
wire of the UMX5 comparator was also used for checking the
Metrologia, 44 (2007) 266274

Figure 2. Handling tool and special wire tray of the UMX5


comparator.

adjustment (the micro-standard can be suspended from it) as


shown in figure 2.
1.5. Storage of the micro-mass standards
It was soon found that storing the micro-standards was a
problem that would have to be studied quickly. Indeed,
movement of the comparator door or heavy breathing on the
part of an operator could destroy them. They also had to be
stored in such a way that taking them out and putting them
back would not damage them.
A stainless steel box was accordingly designed and built.
Its back wall has two staggered rows of support hooks from
which the micro-standards can be suspended (1 standard per
hook) (figure 3). At the front, a guillotine door that displaces no
air when opened and closed gives access to the hooks, making
it easy to suspend and withdraw the micro-standards using the
handling hook. To make these operations more precise, the
top of the box is transparent.

2. Validation of the design of the micro-mass


standards
In order to validate the solutions chosen for the design of the
micro-standards from the viewpoint of handling, compatibility
with the comparator used for the calibration and preservation,
a first test set of micro-standards was made. This set comprises
six standards having the following nominal values:
2 500 g,
2 200 g,
2 100 g.
267

T Madec et al

2.2.2. Differences between the adjusted and observed values.


After the results had been processed by the generalized least
squares method, the differences between the values observed
in the course of the comparisons and the adjusted values
were determined. The absolute value of these differences
is, on average, 0.04 g. This demonstrates the quality of the
comparisons performed.

3. Micro-standards to determine the sensitivity


errors of comparators
3.1. Using 1.01 mg, 1.02 mg, 1.05 mg, 1.1 mg, 1.2 mg and
1.5 mg special mass standards
Figure 3. Main picture: the stainless steel box with a guillotine door
and a transparent top. Inset pictures: details of one of the eighteen
hooks.

2.1. Calibration of the micro-standard using weighing


designs
The least squares method using weighing designs was used to
calibrate the micro-standards. This method ensures that the
solution is overdetermined and, consequently, the quality of
the calibration can be checked. Moreover, the determination
of uncertainties can be made by matrix calculation, taking into
account variances and covariances directly (for more details
see [1, 2]).
The six micro-standards were calibrated several times,
at intervals of several weeks, in a weighing design (that is,
the programme of measurements) using two 1 mg reference
standards. Altogether, nine comparisons were performed to
weigh the micro-standards. These comparisons are defined in
the weighing matrix (table 1). The number of comparisons
was very large to allow for the defects of reproducibility
of the measurements and to ensure that the solution is
overdetermined.
The weighing plan takes the form of a matrix in which
each line represents a comparison, identified by a serial
number from 1 to 9, and
the standards appear in the columns; they are identified by
their nominal values, possibly completed by a prime for
the duplicates.
The table is read as follows. For the ith comparison, the
standard (or standards) having coefficient 1 of the ith line is
compared with the standard having coefficient 1 on the same
line as shown in table 1.
2.2. Calibration results
2.2.1. Repeatability. The comparison scheme is of the
ABBA type (A for the weighing of the standard and B for
the weighing of the mass). It was repeated six times per
comparison, and the first determination of the mass-standard
difference was systematically eliminated. The quadratic mean
of the standard deviations of repeatability calculated on the
nine comparisons is 0.11 g.
268

As described in the literature (cf [3]) the sensitivity/linearity


error of mass comparators can be determined in steps of 100 g
(and even 10 g) by special mass standards adjusted to 1.01 mg,
1.02 mg, 1.05 mg, 1.1 mg, 1.2 mg, 1.5 mg, etc. With this
method, the investigation of the sensitivity error determined in
steps of 100 g can be performed only from 3 mg as shown as
follows: 3.0 mg (2+1); 3.1 mg (2+2.1); 3.2 mg (2+1.2); 3.3 mg
(1.2 + 1.1 + 1); 3.4 mg (1.2 + 1.2 + 1); 3.5 mg (2 + 1.5); 3.6 mg
(1.5 + 1.1 + 1); 3.6 mg (1.5 + 1.2 + 1); 3.8 mg (1.5 + 1.2 + 1.1);
3.9 mg (1.5 + 1.2 + 1.2). Furthermore, using a difference of
mass standards is less flexible as you cannot simply modify the
tare value in order to check a particular part of the weighing
range (for example, from 0 mg up to 1 mg).
On a mass comparator, calibrations are performed using
a substitution between the mass standard and the unknown
weight. All weights are adjusted more or less close to the
nominal value in conventional mass metrology (it depends on
the class of the weight). So it is interesting to study this range
at 1 kg: 0.34 mg (0.500.16) for E1 and 1.1 mg (1.60.5)
for E2 .
In fact manufacturers, for practical reasons, prefer to
adjust weights with a positive correction rather than a
negative one.
Some of the advantages in using micro-standards for the
determination of the sensitivity are that
for each nominal value under study, it is convenient to use
a weight with the lightest correction and in that way to
access easily the high-heat range,
to explore the high-heat range only one micro-standard is
used at the same time and
in the uncertainty calculation of the sensitivity error, the
component of the mass standard to take into account is
only the uncertainty of one weight rather than four or
five in the example given before (without speaking about
covariances between weights).
3.2. Implementation
In order to cover the span of the domain to be explored, it was
decided to produce two sets of micro-standards from 100 g to
900 g in 100 g increments, as shown by table 2. They were
named SU 100 g to 900 g.
Metrologia, 44 (2007) 266274

Micro-mass standards to calibrate the sensitivity of mass comparators

Table 1. Weighing matrix of the micro-mass standards SN 100 g to 500 g.


Reference
r/kg m3
coefficients
1
2
3
4
5
6
7
8
9

1 mg
7960
1
1

1 mg
7960
1
1

500 g
2700
0.5
1
1
1
1

500 g
2700
0.5
1
1
1
1

200 g
2700
0.2

200 g
2700
0.2

1
1
1

1
1
1
1

100 g
2700
0.1

100 g
2700
0.1

1
1
1
1
1

1
1
1

Table 2. Shape of micro-mass standards SU 100 g to 900 g.

Identification

Shape

SU 100 g 1

SU 500 g 2

SU 100 g 2

SU 600 g 1

SU 200 g 1

SU 600 g 2

SU 200 g 2

SU 700 g 1

SU 300 g 1

SU 700 g 2

SU 300 g 2

SU 800 g 1

SU 400 g 1

SU 800 g 2

SU 400 g 2

SU 900 g 1

SU 500 g 1

SU 900 g 2

3.3. Choice of the method of calibration of the SU


micro-standards
Because of the large number of micro-standards (18 in
all), it was decided to calibrate them in four calibrations
using weighing plans, each comprising the same two 1 mg
references, 500 g micro-standards to check consistency
between weighing designs and two pairs of complementary
micro-standards, namely (100+900) g, (200+800) g, (300+
700) g or (400 + 600) g.
Unfortunately, it was quickly found that it was difficult to
create a weighing design having an invertible matrix. Since
the pivot is zero, the results of the matrix calculation became
aberrant (the complementary pairs always appear on the same
side in the equations linking them). In conventional weighing
designs the breakdown is of the 1-2-5 type and does not pose
this type of problem.
To resolve this difficulty, micro-standards were added to
each of the weighing designs to allow the addition of equations
to dissociate the complementary pairs as follows:
600 g in the series 200 + 800 200 + 600 = 800,
400 g in the series 300 + 700 300 + 400 = 700,
Metrologia, 44 (2007) 266274

Identification

Shape

200 g in the series 400 + 600 400 + 200 = 600,


2400 g in the series 100 + 900 100 + 2 400 = 900.
This solution, which made the matrix calculation solvable,
had the drawback of overly favouring certain standards that
appeared in many more equations than others and in more
weighing designs.
In the end, the choice was a weighing plan leading to
a single calibration using designs such that all the standards
appeared the same number of times and yielded a unique result
for each mass.
3.4. Weighing plan for the SU micro-standards
Altogether, 30 comparisons were performed to weigh the
18 micro-standards. These comparisons are defined in the
weighing design given below. Each micro-standard appears
in four comparisons (cf table 3 line n at the bottom of the
weighing matrix) and the two 1 mg reference standards are
used six times each.
269

T Madec et al

Table 3. Weighing matrix for the micro-mass standards SU 100 g to 900 g.

3.5. Matrix calculation


All comparisons performed and included in the weighing
design underwent a single analysis in a weighing programme
by the generalized least squares method, using the software
developed by the LNE. Given the size of the matrix to be
inverted (32 lines 20 columns, including the equations of
the standards), the results were analysed again to ensure the
validity of the matrix calculation. Mathlab software was
used for this independent calculation using the MoorePenrose
method for the matrix inversion.
The differences found between the two calculation
methods, whether they concern the masses or their associated
uncertainty, are less than 0.01 g for the all 18 micro-standards.
This tends to confirm the results of the first analysis.
3.6. Calibration results
It must be acknowledged that in the five successive calibrations
of the 18 micro-standards, the quadratic mean of the standard
deviations obtained in the 30 comparisons made in the course
of the weighing designs is always smaller than the resolution of
the comparator used, namely, 0.1 g (except for two aberrant
values that were discarded out of the 150 values collected).
270

The typical value of the difference, for a comparison


of a combination of micro-standards, between the adjusted
value derived from the analysis of the weighing designs and
the measured value, calculated on these same five weighing
designs, is 0.028 g (cf table 4). The mean uncertainties
resulting from the analyses of the weighing designs are as
stated in table 5.
3.7. Stability of the standards
Before they were used, the micro-standards were calibrated
twice in succession in order to judge their stability in the
very short term. They were then used to determine the
sensitivity errors on the A5 comparator, the same one used for
their calibration. At the end of these measurements, another
weighing design was performed to judge the impact of using
them on their stability. Subsequently, the micro-standards
were used again, this time to determine the sensitivity errors
on the M-one comparator. Finally, to confirm their stability,
two more weighing designs were successfully performed in
succession.
Among the 18 micro-standards used, the standard
deviation found in the five determinations of their masses,
Metrologia, 44 (2007) 266274

Micro-mass standards to calibrate the sensitivity of mass comparators

Table 4. Quadratic means of the standard deviations and of the difference of adjusted and measured values in the five successive and
identical calibrations weighing designs.
Quadratic mean/g

W.D. No.1

W.D. No.2

W.D. No.3

W.D. No.4

W.D. No. 5

Mean

Standard deviation
Residue

0.075
0.027

0.075
0.028

0.092
0.024

0.091
0.041

0.073
0.017

0.081
0.028

Correction of mass of micro-standard/g

Table 5. Standard uncertainty of calibration of the micro-standards.


Standard uncertainty/g

100
200
300
400
500
600
700
800
900

0.065
0.065
0.075
0.085
0.090
0.11
0.13
0.14
0.16

Standard deviation
of sensitivity/g
Nominal values of
micro-standard

Nominal value/g

Table 6. Standard deviations obtained on the four sensitivity error


values.
Nominal values studied
1 mg 10 mg 100 mg 1 g 5 g
100 g
200 g
300 g
400 g
500 g
600 g
700 g
800 g
900 g

0.07
0.05
0.07
0.09
0.04
0.02
0.09
0.03
0.04

0.02
0.03
0.01
0.04
0.03
0.02
0.08
0.00
0.05

0.02
0.03
0.04
0.08
0.03
0.01
0.03
0.03
0.05

0.02
0.02
0.07
0.06
0.04
0.03
0.10
0.04
0.03

0.11
0.07
0.06
0.12
0.18
0.15
0.08
0.04
0.13

1.0

4. Determination of sensitivity errors on the A5


automatic comparator

0.8

0.6

4.1. A5 automatic comparator

0.4

0.2
(standard uncertainty)

0.0
0

The A5 automatic mass comparator was used at LNE to


perform the mass dissemination from 5 g to 1 mg. It was used
also to perform this study on micro-standards (for more details
about this mass comparator see [4]).

number of weighing design

4.2. Procedure

Correction of mass of micro-standard/g

Figure 4. Example 1: correction of mass of micro-standard SU


300 g in the course of the five successive calibrations.
1.5

1.3

1.1

0.9
0.2 g
0.7
(standard uncertainty)
0.5
0

number of weighing design

Figure 5. Example 2: correction of mass of micro-standard SU


800 g in the course of the five successive calibrations with a
perceptible jump of 0.2 g.

performed over a period of nearly 3 months, is not more than


0.04 g for 16 of them. The remaining two micro-standards
exhibited accidental jumps of 0.1 g and 0.2 g.
Two examples of the evolution of the mass (data correcting
the nominal value) are presented in figures 4 and 5.
The micro-mass standards so developed turn out to be fit
for the purpose for which they were developed. As the above
results show, they are more than adequately stable when used
and stored in a manner appropriate to their small size and their
fragility.
Metrologia, 44 (2007) 266274

The sensitivity errors of the A5 automatic comparator were


determined by successive comparisons of several standards
with themselves (the tare value) plus a micro-standard.
The weighing procedure followed was of the 5ABBA
type (A = Standard, B = Standard + Micro-Standard). For
each nominal value chosen, two procedures were executed
using each of the 18 micro-standards, which means that the
nine sensitivity errors, from 100 g to 900 g, of each of the
nominal values studied were determined four times, by two
different micro-standards.
The measurement range of the comparator is from 0 g to
5.1 g. The nominal values used were 1 mg, 10 mg, 100 mg, 1 g
and 5 g.
4.3. Measurement results
On average, the standard deviation of the four values of each
of the nine sensitivity error determinations made for the five
nominal values chosen is less than 0.06 g (the readability of
the comparator is 0.1 g) as shown in table 6.
In addition, the difference between the sensitivity error
results obtained with one set of micro-standards and the other
is on average 0.06 g, and at most 0.12 g.
4.4. Remarks
It can be seen that at three nominal values the sensitivity errors
remain non-significant (of the order of the quantification step
271

T Madec et al
1.0
1 mg

0.5
Sensitivity error/g

10 mg

100 mg

1g

5g

Curves of sensitivity error of 5 nominal values studied (from 1 mg up to 5 g)

0.0
0

10

-0.5

-1.0
Nominal value of micro standard/g x10-2

Figure 6. Evolution of the sensitivity error versus the difference of


mass of the standards compared at five nominal values: 1 mg, 10 mg,
100 mg, 1 g and 5 g.

of the comparator, at most). On the other hand, at two nominal


values, 1 mg and 1 g, beyond 200 g, the error exceeds 0.2 g,
reaching 0.3 g to 0.4 g at 900 g (see figure 6). Nevertheless,
this is still very small given that no pair of class E1 or E2
masses in the range of the comparator can differ by more
than 200 g.

5. Determination of the sensitivity errors of the


M-one automatic comparator
5.1. M-one automatic comparator
The M-one automatic mass comparator was used at LNE to
perform the mass dissemination from 1 kg to 50 g, including the
one used to tie Frances Platinum reference standard (Pt 35) to
stainless steel and superalloy standards. An airtight enclosure
ensures a constant environment, from atmospheric pressure to
a moderate vacuum (102 Pa). So it is appropriate to study
during vacuumair transfer the evolution of mass standards
used, for example, in the watt balance experiment (for more
details about this comparator see [5]).
5.2. Procedure
To determine the sensitivity errors on the M-one comparator,
the fixed objectives were the following.
To operate as close as possible to the effective working
zone (nominal value of 1 kg).
To use the four stations to reduce the number of placements
and the total time required for the study.
To minimize the effect of air buoyancy difference between
the mass standards (used as tares) of each comparator
station.
To have a frame from which to suspend the microstandards to avoid the risk of handling damage.
To define a method of loading and unloading the
micro-standards without opening the enclosure of the
comparator.
To satisfy these requirements, it was decided to proceed as
follows.
Four mass standards were chosen, having a nominal value
of 500 g, made side by side from the same bar so as not
to differ in density. When they were calibrated, their
272

Figure 7. Assemblies [500 g mass + trolley] on the mass holder of


the M-one comparator with, in the foreground, an 800 g
micro-standard. The tares are placed above it, on the upper tray,
completing the load on the weighing cell to 1 kg.

difference of mass was reduced to a minimum by adding


stainless steel wires, weighed and cut to length.
Four A5 comparator trolleys were also used. They were
chosen from among the 27 available to have masses
as close as possible to one another. Since they are
made mainly of aluminium, the differences found were
corrected by adding aluminium wires cut to length.
The M-one comparator was tared using a 1 kg mass
standard adjusted to the target value. The complement
to 1 kg of the assembly [500 g mass + trolley] was
determined and placed on the tare tray of the M-one. The
assemblies were calibrated against one another to refine
their adjustment to within a few micrograms.
A hook of the same type as the handling tool (cf
section 1.4) but with a longer handle (50 cm) was
made so that the micro-standards could be introduced
and withdrawn through the porthole in the front panel
without opening the enclosure and without the thermal
perturbation that would have resulted.
Figure 7 shows the mass holder of the M-one with microstandards, trolleys and 500 g weights.
5.3. Execution of the weighings
To determine the sensitivity errors of the M-one comparator,
from 1 kg up to 1 kg + 900 g in conventional mass in steps
of 100 g, 17 weighing designs were performed (denoted
WD Nr.1 to 17). Station 1 was used as reference and was
therefore always left empty of a micro-standard. Stations 2,
3 and 4 each held a micro-standard. Three placements were
needed to determine the sensitivity errors at the nine nominal
values. For each weighing design, all the stations are compared
against each other in order to get the best adjusted value of
the differences. But only S2 versus S1 , S3 versus S1 and S4
Metrologia, 44 (2007) 266274

Micro-mass standards to calibrate the sensitivity of mass comparators

Table 7. Chronological list of the comparisons performed in weighing designs to determine the sensitivity errors of the M-one comparator
from 100 g to 900 g.
Identification of the station

Cycle

Weighing
designs
WD

S1
S2
S3
S4
Identification of tare (+ micro-standard) on each station

A
A
A
A
A/B
B
B
B
B/C
C
C
C
C/D
D
D
D
D

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17

M1
M1
M1
M1
M1
M1
M1
M1
M1
M1
M1
M1
M1
M1
M1
M1
M1

M2
M2 + 100 g
M2 + 400 g
M2 + 700 g
M2
M2 + 100 g
M2 + 400 g
M2 + 700 g
M2
M2 + 100 g
M2 + 400 g
M2 + 700 g
M2
M2 + 100 g
M2 + 400 g
M2 + 700 g
M2

versus S1 are used to calculate the sensitivity error. The cycle


sequence of measurement composed by six weighing designs
is as follows.

Four successive determinations (cycles A to D) of the nine


nominal values of the micro-standards were made, with an
alternation between the standards with primes (SU ) and the
standards without (SU), as shown in table 7. The sensitivity
error for each of the nine values is the mean of these four
determinations. Between two cycles, the empty weighing
designs are common for these cycles (WD Nr. 5, 9 and 13).

M4
M4 + 300 g
M4 + 600 g
M4 + 900 g
M4
M4 + 300 g
M4 + 600 g
M4 + 900 g
M4
M4 + 300 g
M4 + 600 g
M4 + 900 g
M4
M4 + 300 g
M4 + 600 g
M4 + 900 g
M4

3.0
2.0
Sensitivity error/g

WD Nr.1without micro-standard, determination of the


adjusted value S2 versus S1 , S3 versus S1 and S4 versus S1 .
WD Nr.2placement of SU 100 g on S2 , SU 200 g on
S3 and SU 300 g on S4 then a new determination of the
adjusted value S2 versus S1 , S3 versus S1 and S4 versus S1 .
WD Nr.3placement of SU 400 g on S2 , SU 500 g on
S3 and SU 600 g on S4 , etc.
WD Nr.4placement of SU 700 g on S2 , SU 800 g on
S3 and SU 900 g on S4 , etc.
WD Nr.5new determination of the adjusted value S2
versus S1 , S3 versus S1 and S4 versus S1 without microstandard.

M3
M3 + 200 g
M3 + 500 g
M3 + 800 g
M3
M3 + 200 g
M3 + 500 g
M3 + 800 g
M3
M3 + 200 g
M3 + 500 g
M3 + 800 g
M3
M3 + 200 g
M3 + 500 g
M3 + 800 g
M3

1.0
0.0
-1.0
-2.0
(standard uncertainty)
-3.0
100

200

300
400
500
600
700
Nominal value of micro-standard/g

800

900

Figure 8. Sensitivity error of the M-one comparator from 100 g to


900 g.

The sensitivity error at the nominal value of the microstandard j is calculated by the relationship
sj = Cj Cj (0),
where Cj is the result of equation (1) and Cj (0) is
the conventional mass of the micro-standard j calibrated
previously (see section 3.4).

5.4. Calculation of sensitivity error


The weighing of the micro-standard j is calculated by the
relationship
Cj = [(CMi + Cj ) CM1 ] [CMi CM1 ],

(1)

where i = 2, 3 or 4 and j = 1 to 18, CM1 , CM2 , CM3 and


CM4 are the weights on stations 1, 2, 3 and 4 of the M-one
handler, respectively.
In equation 1, the term [(CMi + Cj ) CM1 ] is the
weighing of CMi + Cj versus CM1 , and the term [CMi
CM1 ] is the mean value of the weighing of CMi versus CM1 ,
before and after the weighing with the micro-standard.
Metrologia, 44 (2007) 266274

5.5. Measurement results


After zero adjustment of the position of the electrical Mone range, by switching it on with a mass standard very
close to 1 kg in conventional mass, the sensitivity errors of
the first milligram of the M-one weighing range (i.e. 1 kg to
1 kg + 1.5 g) were determined from 100 g to 900 g in steps
of 100 g. They have a mean value of zero (see figure 8
and table 8). Modelling them by a least squares straight
line gives a slope of practically zero and a typical residue
of 0.15 g. The uncertainty of the determination of each
value, given the uncertainty on the masses of the microstandards (calibrated before and after the measurements), on
273

T Madec et al

Table 8. Sensitivity errors and associated standard uncertainty of


the M-one comparator from 100 g to 900 g.
Nominal
value/g

Sensitivity
error/g

Standard
uncertainty/g

100
200
300
400
500
600
700
800
900
Mean
Residue1

0.12
0.14
0.02
0.13
0.06
0.12
0.32
0.05
0.18
0.02
0.15

0.38
0.43
0.48
0.38
0.34
0.41
0.46
0.33
0.32

1
Typical absolute difference between
observed and adjusted values.

the quantification step (which appears four times) and on the


repeatability and reproducibility of the measurements, gives a
standard uncertainty of the order of 0.40 g (cf table 9).
It can therefore be concluded that in a range of
approximately 1 mg explored around the nominal value of 1 kg,
the M-one comparator is free of any significant sensitivity error.

6. Conclusion
The production and calibration of micro-standards turns out
to be a realistic venture provided that suitable precautions are
taken for their handling and preservation. Recourse to an A5
type automatic comparator proves to be one way of achieving
this, by limiting human intervention, which is the main threat
to the survival of the micro-standards even if the speed of

274

Table 9. Example of standard uncertainty calculation of M-one


comparator sensitivity error at 100 g.
Component

u-type/g

Micro-standard
Resolution (four times)
Reproducibility
Repeatability
Least square error
Combined standard uncertainty

0.06
0.16
0.27
0.14
0.14
0.38

displacement of its robot, for this type of use, could be reduced.


It is reassuring to find that the sensitivity errors observed
on two comparators, including the one used in the chain that
extends from platinumiridium references to stainless steel
and superalloy standards, confirm the general belief in the
excellence of their characteristics as regards the linearity of
their sensitivity curves.

References
[1] Bich W 1990 Variances, covariances and restraints in mass
metrology Metrologia 27 1116
[2] Bich W and Cox M G 1993 Uncertainty modelling in mass
comparisons Metrologia 30 495502
[3] Glaser M and Firlus M 1993 Erweiterung der Masseskala fur
den Bereich unter 1 mg PTB-Mitteilungen 103 1315
[4] Reichmuth A 2001 A new mass comparator generation for the
automatic calibration of weight sets Proc. 17th Int. Conf.
Force, Mass, Torque and Pressure Measurement: IMEKO
TC3 (Istanbul, Turkey, 1721 September 2001) pp 31019
[5] Reichmuth A and Richard P 2003 Density determination using
the MettlerToledo M one Mass Comparator Weighing 2003,
South Yorkshire Int. Weighing Conf. (1718 June 2003,
Barnsley, UK) pp 15-115-13

Metrologia, 44 (2007) 266274

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