White Paper

Traceability with Microgram Weights

Mass Standards Down to 0.05 mg
Content

1. Introduction2

2. Difficulties with Low Force Measurement 2

3. Product Concept 3

3.1. Choice of Material 3

3.2. Ideal Shape 3

3.3. Storage and Handling 4

3.4. Production 6

4. Traceability and Ongoing Accuracy Via Calibration 6

4.1. Traceability to SI units 6

4.2. Proof of Concept (UKAS accreditation)  7

4.2.1 Mid-Term Stability 8

4.3. Challenges in Identifying Microgram Weights During Calibration 8

4.4. Common Calibration Procedures 9

4.4.1 Dissemination 9

4.4.2. Chosen Calibration Procedures at NMO 9

4.4.3. Duration of Calibration Process 11

4.5. Effect of Ambient Conditions / Air Buoyancy Correction 11

4.6. Cleaning of the Weights 12

4.7. Benefits of Automated Handling and Measurement 12

5. Worldwide Standards Adoption 13

6. Potential Applications 14

7. Summary 15

8. Appendix – Acronyms of National Metrology Institutes

and International Bodies 15

9. References 15
 This white paper will be of interest to National Metrology Institutes (NMI's) and National Measurement Institutes, private
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calibration laboratories, scientists in the field of nanotechnology, weight manufacturers, metrologists and anyone who
is who is interested in the latest developments in weighing technology and traceability of weights smaller than 1 mg.
Advances in nanotechnology and biotechnology are driving the need for traceable small-force measurement. Previ-
ously, there has been a lack of standards to guide the use of weights down to 50 microgram (µg), and a need for sta-
bility during calibration and transfer of micro-class reference weights. These factors have led to an evolution in weight
design, storage, and handling that has now created critical traceability in these tiny measurement ranges.
Calibrated microgram weights will allow National Metrology Institutes and clients with specialized nanotechnology
applications to use the direct comparison method to verify weight values below 1 milligram. Microgram weights are
now commercially available with a calibration certificate which assures full traceability to the International Prototype
Kilogram (IPK) and thus to the International System of Units (SI). Evidence shows that the weights are also very stable
over the mid-term.

1. Introduction
In the last several years, National Metrology Institutes (NMIs) around the world have begun fielding increasingly
frequent requests for a new, traceable weighing standard for weights below 1 milligram. Research laboratories
and NMI's in the United States, Asia and Europe have expressed strong interest in achieving traceable and com-
parable weighing standards in these minute ranges.

This increasing need for small-force measurement, particularly in nanotechnology applications, instigated re-
search on the part of the NMI, Beijing, China (1). In partnership with METTLER TOLEDO, Switzerland, they deter-
mined how to effectively lower basic-unit traceability to 50 µg, from the established 1 mg range. As a result of
this pioneering project, measurement authorities, such as NMIs, have changed their philosophy on microgram
weight calibration. Revisions to ASTM E617 – 13, “Standard Specification for Laboratory Weights and Precision
Mass Standards,” have been made which now introduce weight denominations down to 0.05 mg in ASTM ac-
curacy classes 0 – 000 (2).

New weight designs springing from public and private research, along with new manufacturing and handling
methods, have made the establishment of repeatable, traceable weighing using these standards a commercial
reality. These new designs and handling methods are helping to ensure uniformity in nanotechnology applica-
tions where object dimensions are less than 100 nanometers (smaller than one ten-millionth of a meter).
Evidence shows that the weights are also very stable over the mid-term.

This white paper will help increase understanding of the robust manufacturing process developed to produce ac-
curate and reproducible microgram weights, in conjunction with the effective calibration and handling methods
that has been developed for them by the British National Measurement Office (NMO) to the satisfaction of strin-
gent United Kingdom Accreditation Service (UKAS) requirements.

METTLER TOLEDO and the NMO work together to offer a combined supply-and-calibration service, with microgram
sets produced by METTLER TOLEDO in Switzerland and calibration/recalibration performed at the NMO in the UK.

This white paper will also reference several technical applications where these standards are currently proving
most useful.

2. Difficulties with Low Force Measurement

Traditionally, the traceability route for low force measurement has been the force generated by a known mass in
a known gravitational field. However, for forces below 10 µN (equivalent to a mass of 1 mg), the weighing uncer-
tainties are too high and masses are too small to be handled conveniently. Therefore, standards in use prior to the

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 development of the new weight class were calibrated using a chain of comparisons using mass comparators.
The primary source of uncertainty in the determination of a mass difference between compared mass and ref-
erenced mass is the repeatability and the air buoyancy correction influence. However, as this had been the only
way to estimate uncertainty in the absence of small enough mass standards, users had no choice but to rely on
manufacturers’ claims regarding each available comparator, or else determine sensitivity errors at higher values
— at least 1 mg — and then interpolate from these results to determine the accuracy of smaller mass differ-
ences. Clearly, this does not provide the surety of direct comparison.

3. Product Concept

National Metrology Institutes (NMI's) from around the world have undertaken research in the area of mass stan-
dards and micro-mass standards. These include: National Physical Laboratory (NPL), UK; Laboratoire National
de Metrologié (LNE), France; Korea Research Institute of Standards and Science (KRISS), Korea and NMI, China
(1, 3, 4, 5, 6). This work has demonstrated that many of the same challenges persist in the even smaller weight
classes.
Essentially, the primary challenges faced in the development of the new, smaller weight class include: choice of
material, shape, storage, handling and production.

3.1 Choice of Materials

The metal chosen for the standards required a low enough density to make the size sufficiently large enough for
the newly-manufactured standards to be seen without magnification. A special aluminum alloy appeared to be
the most reliable solution. This material was chosen because of its non-magnetic quality, non-corrosion charac-
teristics and sufficient hardness, but primarily for its lower density. This theoretical density of 2700 kg/m3 pro-
vided a large volume for weights with the same nominal mass value. The lower density helps to make the size of
the standard reasonable, i.e. larger than the resolving power of the human eye — so that optical instruments are
not required to locate the standard after it is made. It is packaged in the form of a coil of wire with a diameter of
just 0.05 mm — equivalent to the width of a human hair.

3.2 Ideal Shape

Wire holds a distinct advantage over foil or ball shapes because it offers easier handling. A range of shapes
were investigated to allow for identification of the weight of each standard. The various shapes were produced
by bending the wire, and it was important to ensure compatibility of use on the a5 automatic mass comparator
from METTLER TOLEDO. The automated robotic handling eliminates the instability and potential for error that can
occur as a result of manual handling. A magnified graphic showing the shapes of each type of weight is shown
in Fig. 1.

Shapes of microgram weights

0.05 mg Inverted v-shape (chevron)

0.1 mg Inverted v-shape (chevron)

0.2 mg Triangle (with double horizontal bar)

0.5 mg Lozenge (open at the bottom)

Figure 1: Shapes of microgram weights

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 These shapes performed best according to the criteria, and proved robust enough to accommodate the required
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number of standards and ensure operators would not get them mixed up. They also allowed for easier manipula-
tion than alternative shapes.
Microgram weights are too small to be able to etch the nominal weight onto the surface. To address this is-
sue, the weights have been designed alternatively to OIML (Polygonal) such that each nominal weight has
different shape in order for proper handling with the a5 comparator and to uniquely identify them. Having
these different shapes with a centric load point on the hook of the carrier is a critical element
(see Figure 2).

Figure 2: Carrier from a5 automated mass comparator for weighing microgram weights

3.3 Storage and Handling

Storage and handling were also clear challenges to support the new standards. It was necessary to develop stor-
age and transfer methods that would not damage the delicate weights. The main criteria were to stabilize the en-
vironment and prevent losing the weights. It was also necessary to prevent oxidation occurring, which could alter
the weight of the standards beyond acceptable tolerances due to their small size. Consequently, an aluminum
box was designed which is easy to clean and protects the weights from electrostatic charges (pictured in Fig. 3).

Figure 3: Aluminum storage box for microgram weights

The full microgram weight set is supplied with an acclimatization chamber to assist with acclimatization prior to
use (shown in Fig. 4). It consists of a draft shield with 5 hooks to hang the weights on, and a special handling
tool consisting of an aluminum alloy handling tool with a hook on the end (see Fig. 5). This enables the weights
to be picked up and transferred to either a manual or automated comparator balance.

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Figure 4: Acclimatization chamber (draft shield) for hanging microgram weights

Figure 5: Aluminum handling tool with hook for transfer of microgram weights, showing second 0.2 mg weight. Shape is triangular with
double horizontal bar with one bent leg (to differentiate from the first 0.2 mg weight)

Standard tweezers, whilst helpful for picking up larger weights, are not sufficient for handling such small weights
on a consistent basis without damage or loss. It is simply too difficult to pick up a weight, which is only 0.05
mm diameter, with normal tweezers. Hence, specialized tweezers with ceramic tips have been designed for the
purpose of picking up the microgram weights. These tweezers are proven to be suitable for handling weights
from 0.05 mg – 500 mg (Fig. 6).

Figure 6: Tweezers with ceramic tips specifically designed for handling sub-milligram weights

All of the tools described above have been designed specifically to suit the material of the microgram weights, in
relation to minimizing electrostatic effects, the dimensions, construction and relative lack of hardness.

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 3.4 Production
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Manufacture of such small weights is not straightforward. One of the main challenges was to establish a pro-
cess robust enough to ensure precise and reproducible shapes for each nominal weight. The weight is adjusted
by automated cutting of the wire to a specific measured length. All microgram weights are bent into the desired
shape in a semi-automated process, perfected by a Swiss company who specializes in supplying precision
components to watch manufacturers.

4. Traceability and Ongoing Accuracy Via Calibration

These weight sets and handling procedures have helped to establish guidelines for direct-comparison weight
verification and maximum permissible errors in this range. To ensure ongoing accuracy, the NMO became the
world’s first mass calibration laboratory to be accredited according to ISO 17025 for mass calibration standards
down to 0.05 mg (50 µg) in September 2012.

Figure 7: John Pain, Calibration Lab Manager, NMO, UK

John Pain, Calibration Manager for the NMO who provided primary support for the ground-breaking project,
noted that while preliminary research had been done on weight design, little attention had been paid to cali-
bration of microgram weights. The main difficulty was that there was no blueprint to copy. It was necessary to
develop an effective method to calibrate these sub-milligram weights, along with new methods of calculating
uncertainty that would satisfy accreditation requirements.

4.1 “Traceability to SI units”

The calibration method developed involves comparing the weights to the department’s mass standards using
a combination of subdivision and substitution weighing. The standards are then confirmed traceable to the na-
tional primary standard of mass, KG18, held at the British National Physical Laboratory.
Weights with a calibration certificate give the user assurance of full traceability to the International Prototype Kilo-
gram (IPK).

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 4.2 Proof of Concept (UKAS accreditation)
The latest accreditation schedule (scope) can be viewed on the UKAS website (7).

Schedule of Accreditation
issued by
United Kingdom Accreditation Service
21 - 47 High Street, Feltham, Middlesex, TW13 4UN, UK

National Measurement Office

Issue No: 031 Issue date: 04 November 2013

NMO Certification Services Contact: Mr M Panesar

Stanton Avenue Tel: +44 (0)20 8943 7246
Teddington Fax: +44 (0)20 8943 7270
0205
Middlesex E-Mail: mannie.panesar@nmo.gov.uk
TW11 0JZ Website: www.bis.gov.uk/nmo
Accredited to
ISO/IEC 17025:2005
Calibration performed at the above address only

DETAIL OF ACCREDITATION

Measured Quantity Range Calibration and Remarks

Instrument or Gauge Measurement Capability
(CMC) Expressed as an
Expanded Uncertainty
(k = 2)
MASS Nominal value (kg) (mg) NOTES
1000 3 000
500 250 1. Intermediate values can
250 125 be calibrated with an
100 50 uncertainty equal to that of the
60 10 next higher nominal value.
50 6.0
2. Calibrations can be given
Nominal value (g) (mg) in other units as required.
30 000 5.0
20 000 2.9
10 000 1.0
5 000 0.50
2 000 0.22
1 000 0.085
500 0.055
200 0.023
100 0.010
50 0.007 0
20 0.005 0
10 0.004 0
5 0.003 0
2 0.001 0
1 0.000 80
0.5 0.000 70
0.2 0.000 60
0.1 0.000 50
0.05 0.000 50
0.02 0.000 50
0.01 0.000 50
0.005 0.000 50
0.002 0.000 50
0.001 0.000 50
0.000 5 0.000 30
0.000 2 0.000 40
0.000 1 0.000 30
0,000 05 0.000 20

Figure 8: National Measurement Office (NMO) Accreditation Schedule from United Kingdom Accreditation Service (UKAS) demonstrating
their authority to calibrate weights down to 0.05 mg

The process was relatively straightforward: An application was made to UKAS and a calibration method was de-
Assessment Manager: NR2 Page 1 of 3

veloped starting from a blank page, which turned out to be only a minor obstacle in the course of achieving ac-
creditation, although it took some time. In fact, the main difficulty was the audit itself. Normally, after applying for
accreditation for a specific weight class, an audit has to be passed. This involves the national accreditation body
comparing two sets of results – one, a calibration of the weight set by an already accredited laboratory - with
two, a set of results from the laboratory who is applying for accreditation. This proved to be a major obstacle to
overcome, due to NMO being the first laboratory in the world to apply for this accreditation. Consequently, there
were no other accredited calibration laboratories results to compare to. Eventually, UKAS compared three sets
of results on a set of weights (see Table 1). Data generated by the supplier of the weights (Mettler-Toledo AG,
Switzerland), and data generated by the National Physical Laboratory (NPL, UK), were compared to the mea-
surements made by NMO at the request of UKAS. With these three sets of results and with every last detail of the
process closely scrutinized, the accreditation was awarded.
Intercomparison microgram weights
METTLER NPL NMO
TOLEDO
Mass ID No Result U95 = K 2 En Date Result U95 = K 2 En Date Result U95 = K 2 En Date Result U95 = K2 Date
0.05 mg 358931 0.05019 0.001 0.1 20/07/12 0.05156 0.0005 2.7 04/07/12 0.0501176 0.0002 0.0
0.1 mg 358931 0.0993 0.001 0.1 20/07/12 0.099169 0.0005 0.0 04/07/12 0.09915 0.0003 0.0
0.2 mg 358931 0.20068 0.001 0.2 20/07/12 0.200606 0.0005 0.3 04/07/12 0.20043 0.0004 0.0
0.2 mg* 358931 0.20183 0.001 0.0 20/07/12 0.201943 0.0005 0.1 04/07/12 0.20188 0.0004 0.0
0.5 mg 358931 0.49700 0.001 0.2 20/07/12 0.49724 0.0005 0.9 04/07/12 0.49674 0.0003 0.0
0.05 mg 358932 0.05132 0.001 0.4 20/07/12 0.05092555 0.0002 24/08/12 0.050928 19/06/12
0.1 mg 358932 0.10000 0.001 0.1 20/07/12 0.099921 0.0003 22/08/12 0.099915 12/06/12
0.2 mg 358932 0.20051 0.001 0.1 20/07/12 0.2004202 0.0004 22/08/12
0.2 mg* 358932 0.19773 0.001 0.1 20/07/12 0.19766437 0.0004 14/01/13
0.5 mg 358932 0.49825 0.001 0.1 20/07/12 0.498181 0.0003 20/08/12 0.498055 08/06/12
0.05 mg 358933 0.05354 0.001 0.2 13/08/12 0.05331555 0.0002 24/08/12
0.1 mg 358933 0.10526 0.001 0.2 13/08/12 0.1050611 0.0003 22/08/12
0.2 mg 358933 0.20555 0.001 0.1 13/08/12 0.2054302 0.0004 22/08/12
0.2 mg* 358933 0.20374 0.001 0.1 13/08/12 0.203656033 0.0004 14/01/13
0.5 mg 358933 0.50065 0.001 0.0 13/08/12 0.500601 0.0003 20/08/12

Table 1: Intercomparison results of microgram weight set from NMO, NPL and Mettler-Toledo AG

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 Normalized error values (“En”)- are all broadly lower than 1, which confirms both competence of the intercom-
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parison partners and stability of the weight piece during the time of the intercomparison.

0.1005
Weight result (mg) 0.1
0.0995
0.099
0.0985
0.098
0.0975
0.097
NMO NPL METTLER TOLEDO
Figure 9: Calibrated values and uncertainties (k=2) for a specific 0.1 mg microgram weight. Intercomparison results of microgram weight
set from NMO, NPL and Mettler-Toledo AG.

An example of the intercomparison results for a specific 0.1 mg microgram weight is shown in Fig. 9. The graph
displays the calibrated weight value as measured by each of the organizations, with the measurement uncer-
tainty (k=2) in each result indicated.

4.2.1 Mid-Term Stability

Although the traceable calibration of microgram weights is a recent development, it is still possible during the
process of improving the calibration method to compare calibration results for the standards held at the NMO
with the data obtained at the beginning of the project in 2012. Recent evidence collected shows that the weights
are very stable, with all the weights showing very little change. In fact, the largest difference recorded over the 2
year period was 0.05 μg (see Fig. 10).

0.00006
0.00006  

0.00005  
0.00005
Measurement  Error  (mg)  
Measurement Error (mg)

0.00004
0.00004  

500 μg
500  µg  
0.00003
0.00003  
200 μg
200  µg  

50 μg
50  µg  
0.00002
0.00002  

0.00001
0.00001  

0
0  
Aug-12
Aug-­‐12   Dec-12
Dec-­‐12   Apr-13
Apr-­‐13   Aug-13
Aug-­‐13   Dec-13
Dec-­‐13   Apr-14
Apr-­‐14   Aug-14
Aug-­‐14  

Figure 10: Stability of microgram weights over the mid-term, showing the measurement error of the 50 μg, 200 μg and 500 μg weights
over a 2 year period. Uncertainty tolerances are displayed. Note: The 100 μg and 200a μg also fall within this range but are not displayed
for the purposes of clarity of the graph.

4.3 Challenges Associated with Identifying Microgram Weights During Calibration

Difficulty comes when differentiating between the standard weight and the test (unknown) weight of the same
nominal weight. During some processes two weights of the same nominal weight have to be weighed together.
This has the potential to cause confusion when the weights are taken off the comparator. How can you be abso-
lutely sure which weight is which?
For example, the process at NMO involves weighing two 50 μg weights together against two different 100 μg
weights.

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 Identifying which weight is which can only be done by weighing them. Therefore, an additional set of weights
that were outside tolerance was used. Hence, by weighing it becomes obvious which is the unknown and which
is the reference standard, because the reference is outside specified tolerance limits for these weights.

4.4 Common Calibration Procedures

A calibration of a set of weights is typically carried out using two established methods:
1) Direct Comparison: to compare the weights with a reference set using the one vs. one method, which requires
a full reference weight set with all required standard weights.
2) Dissemination (also known as subdivision/multiplication): to calibrate the unknown masses by only using
one reference weight and working downwards.

4.4.1 Dissemination

Dissemination can be very time-consuming and difficult to achieve with a manual or automatic comparator.
Often weights have to be stacked and specially designed weighing schemes have to be employed if using an
automatic or manual balance. For instance: the placement of several weights onto a hanging weighing pan of a
manual balance can be very challenging. Finding the center of gravity of a group of weights with different nomi-
nal values is practically impossible.

On the other hand, using a robotic system a flexible design of a weights dissemination scheme can be chosen,
where up to 3 weights can be loaded simultaneously onto the weighing pan.

The weights are automatically loaded symmetrically to avoid eccentric load errors.

For example: 500 μg vs. 200 μg + 100 μg + 200 μg

If an asymmetrical weighing scheme is chosen, for instance 5 g vs. 3 g + 2 g, an automatic correction to the
measured value is made according to the determined value of the eccentricity error. More information on this
topic was published in a paper at IMEKO in 2001 (8).

Required Minimum Weighing Cycles

Class 000,00,0 1 2&3 4&5 6&7
ABBA 3 2 1 1 1
ABA 5 3 2 1 1
AB .... BA 5 3 2 1 1
ASTM E61 7 (20 l 3) Table 1 2

• ABBA & ABA appropriate for weight classes 000, 00, 0, 1, 2, & 3
• AB ... BA may be used for weight classes 4, 5, 6, and & 7
• AB ... BA may be used for weight classes 000, 00, 0, 1, 2, & 3 if
a mass comparator with an automatic weight exchange
mechanism is used and if the system is installed in a protecting
housing.

Figure 11: Required minimum weighing cycles for various weight classes according to ASTM

4.4.2 Calibration Procedures at NMO

The NMO in the UK currently carry out two calibration procedures, which are:
• Direct calibration based on Borda's substitution method – which results in 0.7 µg uncertainty
• CMC (Calibration Measurements Capability) – which results in 0.2 µg uncertainty

The client decides which method they wish to use because the different methods have a different cost associated
with them. CMC method is more expensive than direct weighing because there is a lot more involved in this method.

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 Normally, disseminations are performed downwards (or upwards) from one reference. The key difference of the
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method developed by NMO is that it is a dual system. This means that all comparisons are done twice, against
two different standards. The process is initiated with two different 1 mg reference weights and disseminated from
these. Therefore, two different sets are measured in parallel and the figures between each set are cross-checked,
followed by substitution from one set to the other, so the weights are crossed over.

There are two key benefits of performing two weighings in parallel:

1)  To maximize efficiency of the process
Another issue to consider, when devising the weighing sequence, is that it should be efficient, as well as accu-
rate. Systems used by other organizations may well be accurate but can involve 2-3 times more weighings per
decade (coming down from 1 kg). The streamlined method developed by John Pain at the British NMO, gives
reasonably good uncertainties but is continually being improved, with the aim of achieving an uncertainty of
lower than 0.2 µg for all weights.

2)  To cross-check the results during the process

This method involves performing a greater number of calculations than the single method. Instead of perform-
ing one weighing and getting a single answer, two weighing measurements are always performed, so that two
answers are obtained. This acts as a cross-check. Normally, the two results are extremely close, so this cross-
check provides a higher level of confidence in the result.

Calibration is achieved by simultaneously calibrating two sets of microgram weights, using a combination of
sub-division and Borda’s methods, against two 1 mg stainless steel reference standards, which in turn have
been calibrated by NPL mass section to their best measurement uncertainty. The balance used for the whole
process is an a5 robotic mass comparator from METTLER TOLEDO. By using a dual system, cross-referencing
the results and cross substituting various weights in each set, a very low uncertainty is achieved. Numerous
inter-comparisons are used in each calibration to achieve a good average value with a low standard deviation.

1 1 0.5 0.2 0.2a 0.1 0.05 0.5 0.2 0.2a 0.1 0.05
mg mg mg mg mg mg mg mg mg mg mg mg
1 A B
2 A B B
3 A B B
4 A B B B B
5 A B B B B
6 A B B B B
7 A B B B B
8 A A
9 A B B B
10 A B B B
11 A B B B B
12 B B B A B
13 A A A B B B
14 A A A B B B B
15 A B
16 A B
17 A B B B
18 A B B B
19 A B B
20 A B B
21 B A B
22 B A B
23 B A B B
24 B A B B
25 A B
26 A B B
27 B A B
28 A B

Table 2:Example of a design matrix for calibration of microgram weights on an a5 comparator. Used by John Pain at NMO (UK). "A" refers
to one weight (or weight set) and "B" refers to another weight (or weight set). Note: not every step in the dissemination scheme involves
weighing a standard against an unknown weight. For example, step 1 involves weighing two known standards against each other.

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 The process is as follows (see also Table 2):

1. Start with two 1 mg reference weights

2. Check these weights against each other
   – This step is important, as it ensures that there is nothing amiss with either of the standards, because
everything else in the sequence relies on this.
3. Check the 500 μg weights (there are two of them)
   – First, weigh against 1 mg standard
   – Next, weigh against a completely separate 1 mg standard
   – Then, the two results are averaged and should be very close
4. Weigh the two 500 μg weights against each other
5. Then, use one of them as the head weight for the next round of disseminations and the other for a second lot
of weighings
   – Perform two sets of weighings for the 200 μg weights
   – Continue sequence as above
   – Perform two sets of weighings for the 100 μg weights
   – Finally, with two of the 100 μg weights, check the 50 μg weights in the same way as the 500 μg were
checked

The current levels of uncertainty for nominal values from 0.5 mg to 0.05 mg are as low as 0.0002 mg (0.2 mi-
crograms) – see Table 3. However, the calibration method is being improved all the time, and thus uncertainties
are being minimized.

Nominal weight (mg) Nominal weight (μg) Uncertainty (μg)

0.5 mg 500 μg 0.3 μg
0.2 mg 200 μg 0.4 μg
0.2 mg 200 μg 0.4 μg
0.1 mg 100 μg 0.3 μg
0.05 mg 50 μg 0.2 μg

Table 3: Uncertainties relating to microgram weights calibrated with CMC method according to 2013 audit

4.4.3 Duration of Calibration Process

Calibration of a set of microgram weights typically takes 2-3 hours using Borda's method. However, calibration
of a set of weights with Calibration Measurement Capability can take more than a week of constant weighing.

The weights are usually set up at the end of the working day and the weighing steps are allowed to run through
the night to allow sufficient time. Two 500 μg weights can be weighed on the same carrier of the automated
mass comparator, allowing comparison of one against the other.

The optimum time to set the weights sequence running is through the night (and into the weekend, if necessary).
With no personnel in the building, everything is more stable. These seem like trivial small details, but with cali-
bration methods at the microgram level, this is imperative. Everything has to be applied to the extreme.

4.5 Effect of Ambient Conditions / Air Buoyancy Correction

In fact, with NMO's experience in handling the microgram weights, it has been observed that the ambient condi-
tions are not so critical. This parameter is less important when handling microgram weights than it is for the
higher weight ranges. Considering the uncertainty as a ratio of the nominal weight, this factor is larger for micro-
gram weights. With microgram weights using a direct weighing method, the uncertainty is 0.7 μg. For a 50 μg
weight, that equates to 1.4%. For this reason, the air buoyancy correction is also not an important factor. Calcu-
lations have demonstrated that the only buoyancy correction of concern is going from the 1 mg stainless steel

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 standard weight to the aluminum microgram weights. The density of the stainless steel is 8000 kg/m3 compared
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to the density of the aluminum of 2700 kg/m3. The largest effect that has been observed is 10 ng (0.01 μg), un-
der extreme conditions (i.e. air density effects), which are very rare. So, typically the air buoyancy correction is in
the order of 0.00x μg, which effectively means that this effect can be ignored for microgram weights. From that
point of view it is easier than normal weighing.

4.6 Cleaning of the Weights

Cleaning of the microgram weights is a straightforward process. Typically, they are brushed over with a very
fine brush. Visual inspection also plays an important role and very high power lenses are used to look at the
weights before handling. However, to date only brand new weight sets have been calibrated at NMO, which are
clean. No recalibrations of used customer weight sets have been performed to date.

4.7 Benefits of Automated Handling and Measurement

The weighing sequences for the calibration of microgram weights at NMO in the UK are performed on the a5
automated robotic mass comparator [METTLER TOLEDO]. This method provides the capability to achieve lower
uncertainties that it would be possible to achieve with manual weighing. The a5 has a maximum load of 6.1 g
and a readability of 0.1 μg.

Figure 12: a5 series automated mass comparator from METTLER TOLEDO

Many of the weighing steps performed by NMO are based on the CMC capability – so it is necessary to have a
robotic automated system to make this possible. This could involve performing 25 inter-comparisons of just one
weight. This task even takes several hours on a robotic system, which can simply be set up and left to run the
weighing sequence. It is almost inconceivable to consider undertaking this task manually.

Additionally, the robotic system has greater accuracy when it comes to timing, and this is critical in achieving the
lowest possible uncertainties in the measurement.

Another advantage of the automated approach is that it avoids anyone breathing on the weights. When weighing
manually, breathing on the weight is hard to avoid. This has the effect of increasing the carbon dioxide (CO2) content
around the vicinity of the balance. The carbon dioxide content has an effect on the air density, which in turn affects
the measurement uncertainty. Clearly, there is a benefit in eliminating any additional contributions to the uncertainty.
A key benefit of the automated comparator is that it can be set up with a time delay, so that it performs the
weighing processes overnight. The balance is always more repeatable at night, because all the external influ-
ences are stable. There is less risk of vibration or interference or other influencing factors. From the user perspec-
tive, you simply come in to the calibration laboratory the following morning and everything is done for you, with
all results recorded automatically.

12 White Paper
METTLER TOLEDO
 More information on the benefits of robotic mass comparators is available in a white paper entitled "Mass cali-
bration with robotic mass comparators" (9). Technical specifications are available in the comparator balances
brochure (10).

Note: John Pain is now a senior technical adviser offering consultancy services as an Independent Consultant
Metrologist (11).

5. Worldwide Standards Adoption

The three major weight specifications used in the United States are:

ASTM E617 Standard Specification for Labora- Industry & Laboratory Standard
tory Weights and Precision Mass
Standards

OIML R111 Metrological & Technical Require- Legal Metrology, Industry & Labo-
ments for Classes E1 to M3 used ratory Standard
for verification of weighing instru-
ments and calibration of weights of
a lower accuracy class

NIST Handbook 105-1 Specification and Tolerances for Legal Metrology & commercial
Reference Standards and Field weighing instruments
Standard Weights & Measures

Table 4: United States organizations which define weight specifications

ASTM E617-13, Standard Specification for Laboratory Weights and Precision Mass Standards, was updated
in August 2013 (2). The changes introduce two new weight classes 00 and 000, and recognize the progress
which has recently been made in the field of microgram-weights, by defining sub-milligram weight specifica-
tions. These ASTM regulation changes are now in full force and effect.

White Paper
METTLER TOLEDO
13
White Paper
E617 − 13
TABLE 1 Maximum Permissible Errors
NOTE 1—Maximum Permissible Errors are reported in SI units, typically milligrams.
NOTE 2—The “grain” is the same in avoirdupois, troy and apothecaries units of mass.
NOTE 3—See NIST SP 811 and NIST SP 1038 for conversion and units of measure.
Denomination ±mg except as noted
Metric Class 000 Class 00 Class 0 Class 1 Class 2 Class 3 Class 4 Class 5 Class 6 Class 7
5000 kg 25 g 50 g 100 g 250 g 500 g 750 g
3000 kg 15 g 30 g 60 g 150 g 300 g 450 g
2000 kg 10 g 20 g 40 g 100 g 200 g 300 g
1000 kg 5g 10 g 20 g 50 g 100 g 150 g
500 kg 2.5 g 5g 10 g 25 g 50 g 75 g
300 kg 1.5 g 3g 6.0 g 15 g 30 g 45 g
200 kg 1g 2g 4.0 g 10 g 20 g 30 g
100 kg 500 mg 1g 2.0 g 5g 10 g 15 g
50 kg 13 mg 25 mg 63 mg 125 mg 250 500 mg 1.0 g 2.5 g 5g 7.5 g
30 kg 7.5 15 38 75 150 300 600 mg 1.5 g 3g 4.5 g
25 kg 6.25 12.5 31 62 125 250 500 1.2 g 2.5 g 4.5 g
20 kg 5.0 10 25 50 100 200 400 1.0 g 2g 3.8 g
10 kg 2.5 5.0 13 25 50 100 200 500 mg 1g 2.2 g
5 kg 1.3 2.5 6.0 12 25 50 100 250 500 mg 1.4 g
3 kg 0.75 1.5 3.8 7.5 15 30 60 150 300 1.0 g
2 kg 0.5 1.0 2.5 5.0 10 20 40 100 200 750 mg
1 kg 0.25 0.5 1.3 2.5 5.0 10 20 50 100 470
500 g 0.13 0.25 0.60 1.2 2.5 5.0 10 30 50 300
300 g 0.075 0.15 0.38 0.75 1.5 3.0 6.0 20 30 210
200 g 0.05 0.10 0.25 0.50 1.0 2.0 4.0 15 20 160
100 g 0.025 0.05 0.13 0.25 0.50 1.0 2.0 9 10 100
50 g 0.015 0.030 0.060 0.12 0.25 0.60 1.2 5.6 7 62
30 g 0.014 0.026 0.037 0.074 0.15 0.45 0.90 4.0 5 44
20 g 0.013 0.025 0.037 0.074 0.10 0.35 0.70 3.0 3 33
10 g 0.010 0.020 0.025 0.050 0.074 0.25 0.50 2.0 2 21
5g 0.005 0.010 0.017 0.034 0.054 0.18 0.36 1.3 2 13
3g 0.005 0.010 0.017 0.034 0.054 0.15 0.30 0.95 2.0 9.4
2g 0.005 0.010 0.017 0.034 0.054 0.13 0.26 0.75 2.0 7.0
1g 0.005 0.010 0.017 0.034 0.054 0.10 0.20 0.50 2.0 4.5
500 mg 0.002 0.003 0.005 0.010 0.025 0.080 0.16 0.38 1.0 3.0
300 mg 0.002 0.003 0.005 0.010 0.025 0.070 0.14 0.30 1.0 2.2
200 mg 0.002 0.003 0.005 0.010 0.025 0.060 0.12 0.26 1.0 1.8
100 mg 0.002 0.003 0.005 0.010 0.025 0.050 0.10 0.20 1.0 1.2
50 mg 0.002 0.003 0.005 0.010 0.014 0.042 0.085 0.16 0.50 0.88
30 mg 0.002 0.003 0.005 0.010 0.014 0.038 0.075 0.14 0.50 0.68
20 mg 0.002 0.003 0.005 0.010 0.014 0.035 0.070 0.12 0.50 0.56
10 mg 0.002 0.003 0.005 0.010 0.014 0.030 0.060 0.10 0.50 0.40
5 mg 0.002 0.003 0.005 0.010 0.014 0.028 0.055 0.080 0.20
3 mg 0.002 0.003 0.005 0.010 0.014 0.026 0.052 0.070 0.20
2 mg 0.002 0.003 0.005 0.010 0.014 0.025 0.050 0.060 0.20
1 mg 0.002 0.003 0.005 0.010 0.014 0.025 0.050 0.050 0.10
0.5 mg 0.002 0.003 0.005 0.010 0.014 0.025 0.050 0.050 0.10
0.3 mg 0.002 0.003 0.005 0.010 0.014 0.025
0.2 mg 0.002 0.003 0.005 0.010 0.014
0.1 mg 0.002 0.003 0.005 0.010
0.05 mg 0.002 0.003 0.005
Avoirdupois Class 0 Class 1 Class 2 Class 3 Class 4 Class 5 Class 6 Class 7
Pound
Table 5: ASTM guidance for MPE of mg
weights down mgmilligrams
to 0.05 g & mg g & mg g & mg g & mg g & mg g & mg
10000 lb 23 g 45 g 90 g 227 g 454 g 680 g
5000 lb 11 g 22 g 44 g 113 g 227 g 340 g
3000 lb 7g 14 g 28 g 68 g 136 g 204 g
With regards to OIML, there is currently no standard defined for micro-weights. The scope of nominal values goes
2500 lb
2000 lb
6g
4.5 g
12 g
9g
24 g
18 g
57 g
45 g
113 g
91 g
170 g
136 g
down to 1 mg as the lowest value. Therefore, OIML issue no guidance in relation to tolerances and maximum
1000 lb
500 lb
2.3 g
1.7 g
4.5 g
2.3 g
9g
4.6 g
23 g
11 g
45 g
23 g
68 g
34 g
permissible errors, and no recommendations
100 lb
50 lb
57 mg
29 in57terms of shapes or raw materials for weights below 1 mg (12).
110 mg 230 mg
110
460 mg
220
920 mg
440
2.3 g
1.1 g
4.5 g
2.3 g
6.8 g
4.1 g
30 lb 17 34 68 140 260 680 mg 1.4 g 3g
25 lb 14 28 56 110 220 570 1.1 g 2.5 g

6. Potential Applications
20 lb 12 23 46 92 180 450 910 mg 2g
10 lb 5.5 11 22 44 88 230 450 1.3 g
5 lb 2.7 5.4 11 22 43 110 230 760 mg
3 lb 1.7 3.4 6.8 14 27 68 140 510
2 lb 1.2 2.3 4.6 9.2 18 45 91 430
1 lb 0.55 1.1 2.2 4.4 8.8 27 45 270
0.5 lb 0.27 0.54 1.1 2.2 4.3 15 23 160
Potential uses of microgram weights currently include many nanotechnology applications, such as:
0.3 lb 0.17 0.34 0.68 1.4 2.7 10 14 110
0.2 lb 0.12 0.23 0.46 0.92 1.8 8.1 9.7 91

• Support of mass calibration for low force or small force measurements. Applications including manu-
Copyright by ASTM Int'l (all rights reserved); Thu Dec 5 06:58:30 EST 2013
4
facturing of objects
Downloaded/printed by with dimensions of < 100 nm, e.g. micro-electromechanical systems such as computer
Roger Marti (Mettler-Toledo Ag) pursuant to License Agreement. No further reproductions authorized.
chips and microscopic devices. Also, mechanical testing of nano- and bio-material sensors.
•  Calibration of mass comparators. The weights can help with evaluation or calibration of the sensitivity of
mass comparators, providing high accuracy.
•  Calibration of atomic force microscopes (AFM). Micro-weights can be used to calibrate the very fine canti-
lever of an atomic force microscope, which is drawn over an uneven object to reveal the surface contours at
sub-nanometer level. The weights are used for measuring the spring constant of atomic-force microscopes.
Typical AFM force is also very small — or about 10nN, corresponding to about 1 µg in mass unit.
•  Development of thrust balances for space propulsion systems operating in the range of 0.1 µN to several
millinewtons.
•  Second-generation nano-science battery technology also requires weight of nanowire to estimate its theo-
retical capacity.

14 White Paper
METTLER TOLEDO
 7. Summary

Traceable microgram weights in the range of 0.05 – 0.5 mg are now commercially available worldwide with a
calibration certificate. The micro weights are manufactured by Mettler Toledo in Switzerland. Evidence shows that
the weights are very stable over the mid-term.

The National Measurement Office (NMO) in the UK performs the calibration and re-calibration of these micro-
gram weights. NMO is the world's first mass calibration laboratory to be accredited according to ISO 17025 for
the calibration of mass standards down to 0.05 mg. Accreditation was from United Kingdom Accreditation Ser-
vice (UKAS).

As a result, revisions to ASTM E617 – 13, “Standard Specification for Laboratory Weights and Precision Mass
Standards,” have been made which now introduce weight denominations down to 0.05 mg in ASTM accuracy
classes 0 – 000.

8. Appendix – Acronyms of National Metrology Institutes and

International Bodies

National Metrology Institutes (NMI's) around the world have contributed significant research and/or support to the
development of micro standards. A partial list of these organizations and their corresponding acronyms follows.

ASTM American Society for Testing and Materials, now known as ASTM International
BIPM Bureau International des Poids et Measures (International Bureau of Weights and Measures)
EURAMET European Association of National Metrology Institutes
KRISS Korea Research Institute of Standards and Science
LNE Laboratoire National de Metrologié, France
NCSLI National Conference of Standards Laboratories International
NIM National Institute of Metrology, China
NIST National Institute of Standards and Technology, U.S. Department of Commerce
NMO National Measurement Office, United Kingdom
NPL National Physical Laboratory, United Kingdom
OIML Organisation International de Métrologie Légale (International Organisation of Legal Metrology)
PTB Physikalisch-Technische Bundesanstalt, National Metrology Institute of Germany
UKAS United Kingdom Accreditation Service

9. References

1.  “ Research on Micro-Gram Weight Standards below 1 mg in NIM.” XX IMEKO World Congress, Metrology for
Green Growth. Busan, Republic of Korea, September 9-14, 2012.
2.  “ASTM E617 – 13.” American Society for Testing and Materials. 2013. Downloaded by permission.
3.  http://www.npl.co.uk/science-technology/dimensional/research/low-force-measurement
4.  “Micro-mass standards to calibrate the sensitivity of mass comparators.” Madec et al. Metrologia 44 (2007)
266-274.
5. “Establishment of Mass Standards from 1 mg to 50 µg.” Chung et al. Proceedings of Asia-Pacific Symposium
on Measurement of Mass, Force and Torque (APMF2009). Tokyo, Japan, June 1-4, 2009.
6. “Report on EURAMET. M.M-S2: Supplementary comparison of 100 gram, 10 gram, 500 microgram, 200 mi-
crogram and 100 microgram weights.” EURAMET project number 1054.
7.  United Kingdom Accreditation Service (UKAS) website,
http://www.ukas.com/about-accreditation/accredited-bodies/Calibration-laboratories-schedules.asp

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METTLER TOLEDO
15
 (National Measurement Office, Laboratory number 0205). Direct link:
http://www.ukas.org/calibration/schedules/Actual/0205Calibration%20Single.pdf
8.  “A new Mass Comparator Generation for the Automatic Calibration of weights sets.” Arthur Reichmuth,
IMEKO, 2001.
9.  "Mass calibration with robotic mass comparators". White paper 30112582, Mettler-Toledo AG, 2013.
http://glo.mt.com/global/en/home/supportive_content/White_Papers/Mass_Calibration_Robotic.html
10. "Comparator balances brochure". 11795840A, Mettler-Toledo AG, 2012.
http://glo.mt.com/global/en/home/supportive_content/product_documentation/product_brochures/Mass_
Comparators/_jcr_content/download/file/file.res/Bro_Comparator_Balances_en.pdf
11.  J Pain Consultancy Ltd. http://www.jpain.eu
12.  International Recommendation OIML R111-1, OIML, 2004.

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