Mettler-Toledo SAS METROLOGICAL QUALITY FOR A BALANCE

Article 1251 Weigh with an analytical balance

Chapter

22b
REFERENCE USP XXVIII

ARTICLE 1251 WEIGH WITH AN ANALYTICAL BALANCE

Weighing is a frequent step in analytical procedures, and the balance is an
essential piece of laboratory equipment in most analyses. In spite of this,
weighing is a common source of error that can be difficult to detect in the final
analytical results. The procedure described here applies directly to electronic
balances; therefore, certain portions of the procedure are not applicable to other
types of balance. The weighing procedure can be separated into three basic
steps: planning, checking the balance, and weighing the material.
Planning
The initial step is to assemble the proper equipment such as containers for
weighing, receiving vessels, forceps, pipets, spatulas of proper size, and so
forth. Use containers of such size that the loading capacity of the balance is not
exceeded. Make sure that the containers selected to receive the weighed mate-
rial are clean and dry. Assemble the necessary chemicals if solutions or rea-
gents are required.
Preparation of the material to be weighed is often necessary. The material may
require grinding or drying. Some materials may have been heated or stored in a re-
frigerator. Material must be brought to the temperature of the balance before they
are weighed. To avoid condensation of moisture, refrigerated materials must be al-
lowed to come to room temperature before the container is opened.
Checking the balance
In the next step it is important to remember that, unless the balance is
checked before each weighing operation is performed, errors can easily occur,
resulting in faulty analytical data. The balance user should check the Balance
environment, Calibration, and Balance Uncertainties. Do not assume that the
balance has been left in the proper operating condition by the previous user.
Balance Environment
The balance is placed in a suitable location with sufficiently low levels of vi-
bration and air current. It must have a constant electrical supply. The balance
and the surrounding work area have to be kept neat and tidy. It is good prac-
tice to use a camel's hair brush or its equivalent to dust the balance pan before
any weighing so as to remove any materials that may have been left by the
previous operator. [Note - Individuals must clean up debris, dispose of any
spilled materials or paper, and remove the vessels and apparatus used in
making the measurements.] When a balance is moved, it must be allowed to
adjust to the temperature of its new environment and be recalibrated.
Calibration
If necessary turn on the power, and allow the balance to equilibrate for at
least 1 hour before proceeding with the calibration. (Microbalances may re-
quire up to 24 hours reaching equilibrium.)
If the balance power has gone off and then came back on, as in a power out-
age, certain types of balance may display a message indicating that the balance
must be calibrated before a weighing is made. If the operator touches the balance
bar, the message may be cleared and the balance may display zeros; however,
the balance will not give the correct weighing until it has been calibrated.

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Reference USP XXVIII
Article 1251 Weigh with an analytical balance

Electronic analytical balances have an internal calibration system based on

an applied load. The calibration applies for the current ambient temperature.
Balance Uncertainties
Drift Reduction
Drift is one of the most common errors, and it is also one of the easiest to
reduce or eliminate. Balance drift can be present without the operator being
aware of the problem. Check the sample, the balance, and the laboratory envi-
ronment for the following causes of errors, and eliminate them:
(1) A balance door is open.
(2) Temperatures of the balance and the material to be weighed are not the
same.
(3) The sample is losing or gaining weight.
(4) The balance has been recently moved but has not been allowed to equil-
ibrate to its surroundings or has not been recalibrated.
(5) Air currents are present in the laboratory.
(6) Temperatures in the laboratory vary.
(7) The balance is not properly leveled.
(8) Laboratory operations are causing vibration.
(9) Hysteresis of the mechanical parts occurs during weighing.
Mechanical Hysteresis
Hysteresis in the balance is caused by excessive stretching of the springs,
and it is primarily due to overloading or to the accidental dropping of an object
onto the pan. Microbalances are very sensitive to overload and shock. When
using a microbalance, set the lever to the rest position when adding or remov-
ing material; turn the lever to the weigh position to register the weight. In some
cases, drift due to hysteresis can be eliminated by allowing the balance to
stand without weighing long enough for it to recover. If stretching of the springs
is excessive, an expensive balance overhaul may be needed. In the case of
electronic force restoration balances, springs are replaced by flexures and the
term creep is more appropriate than hysteresis.
Quality Assurance Procedure for Measurement of Balance Drift
Over an extended period of time, balance drift and other day-to-day varia-
tions are monitored by weighing a fixed check-weight on a regular basis; this
check should be performed after the balance has been calibrated at the ambi-
ent laboratory temperature. The check should be made before the first weighing
of the day or after any event that might disturb the balance's calibration (power
failure, moving the balance to a new location, etc.). The check-weight may be
any object whose mass remains constant and does not exceed the load limit of
the balance. A balance weight makes a reliable check-weight. Each balance
should be provided with a check-weight, which should be stored in a protective
container near the balance.
Perform the following procedures to reduce balance errors and the possibil-
ity of an incorrect reading because of drift:
(1) Make certain that the electrical power to the balance is on and that the
level bubble is in the center of the indicator.
(2) Calibrate the analytical balance or the microbalance, [Note: Some bal-
ances have a calibration lever, which must be returned fully to its original
weighing position. Do not depend upon any prior calibration.]

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Article 1251 Weigh with an analytical balance

(3) The first person to use the balance each day should weigh the check-
weight and record the weight in the log book for comparison with previ-
ous readings. If a deviation greater than that indicated below for Analyti-
cal Balances and Microbalances is observed, the balance should be re-
ported for service. [Note - Check-weights tend to gain weight upon stand-
ing because of mishandling and exposure to contaminants in the atmos-
phere. These weights can be cleaned by wiping with a lint-free cloth
moistened with a small amount of an appropriate solvent such as diethyl
ether.]
Analytical balances - Select a check-weight of an appropriate mass to examine
an analytical balance. If possible, set the balance to read to 5 decimal places.
Follow the manufacturer's operating instructions. Pick up the check-weight with a
forceps, place it carefully on the balance pan, and weigh it. [Note Do not drop
the weight on the balance pan because damage to the balance could result.]
Place the weight in the center of the pan to eliminate corner weighing differences.
The accuracy of the weight is not important; the only factor of interest is whether
any drift has occurred. If no drift has taken place, the value should remain con-
stant. Periodic weighing of a fixed weight will determine if the boards (or knife
edges in the case of mechanical balances) in the instrument are defective. The
check for drift at the most sensitive position will show if a problem exists; the
variation in the observed weight does not exceed 0.2 mg. For example, with a
20 g weight, if the mean value of the readings were 19.9984, the tolerance
would be from 19.9982 to 19.9986 g. Thus, several readings must be taken
before one can establish a tolerance. [Note The check-weight need not be of
high accuracy, but it is essential that its mass remain constant. In addition, the
tolerance does not correspond to the value of 0.1%, specified under Weights
and Balances (41), for weighing material accurately. Rather, the tolerance is
purposefully tight to reveal possible drift or calibration errors: this tolerance is
readily achievable with modern electronic balances.
Microbalances - Proceed as directed for Analytical Balances, but use a check-
weight appropriate for the particular balance. For example, a 100-mg check-
weight might be selected for a balance that has a load limit of 150 mg; or a
10-mg check-weight might be used for an ultra-microbalance with a load limit
of 15 mg. (The operator must know the maximum capacity of the balance to
select the correct check-weight.) The balance indicates the weight in milli-
grams. Record the weight as soon as the reading is stable for a few seconds.
The variation in weighings ought to be within a range commensurate to the
specifications given by the balance manufacturer, but not greater than 0.1% of
the amount of material typically weighed on the particular balance. For exam-
ple, if 10-mg samples are routinely weighed, the variation in the weighings of
the check-weight cannot exceed 0.01 mg.
Weighing the material
In this final step, select the number of decimal places required for the analyt-
ical procedure. In most pharmaceutical analyses small quantities of material
are used, requiring the balance reading to be set to the fifth decimal place to
achieve the necessary accuracy. Weighing read with four decimal places is
preferred for weighing near-gram quantities. Do not allow the material to re-
main on the balance for an extended period of time because changes, caused
by interaction with atmospheric water or carbon dioxide, may take place.

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Article 1251 Weigh with an analytical balance

Load limit
Select the appropriate balance for the quantity and accuracy needed. Each
balance has a load limit, which should not be exceeded. Each balance manu-
facturer supplies the maximum loading condition, and this limit varies with the
type of balance. The operator should know this limit so that the balance will not
be damaged. [NOTE - Electronic balances operate on a "load cell" principle
that produces an electrical output proportional to the movement of the strain
gauge and is linear over the range.
Receivers
The proper receiver for the material must be selected. The receiver's weight
plus the weight to be measured must not exceed the maximum load for the
balance: the size and shape of the receiver should be such that will permit it to
fit into the space and on the balance pan without interfering with any operation.
It is important that the receiver be clean and dry. Common receivers are weigh-
ing bottles, weighing funnels, flasks, and weighing paper. The correct receiver
depends upon the quantity and type of material (liquid. solid. or powder) to be
weighed. All other things being equal, a vessel of low mass should be chosen
when small amounts of material arc to be weighed. It is recommended that
gloves, forceps, or another type of gripping device be used when handling re-
ceivers, because oils from the hands will add weight.
The weighing funnel is often the most satisfactory receiver, because it can
function as both a weighing dish and a transfer funnel allowing easy transfer to
volumetric flasks. Weighing funnels come in various sizes: the size suitable for
the operation should be selected.
Weighing paper may be used for solids. Paper receivers must be handled
by hand, and great care must be used to prevent spills.
Weighing by Difference
Weighing is usually done by difference. The following methods are accepta-
ble for good analytical results.
Method 1
Tare the empty receiver as follows. Place the receiver on the balance in the
center of the pan and press the appropriate tare key on the balance. This op-
eration electrically sets the signal from the strain gauge to zero so that the
weight of the receiver is no longer indicated. Add the material to the receiver,
and record the weight. Transfer the weighed material to the final flask or receiv-
er; then reweigh the original weighing receiver by placing it in the same posi-
tion on the pan. [Note - Do not change the set tare of the balance between the-
se two weighings.] The second weight represents the un-transferred material
and is subtracted from the total material weight to determine the weight of the
transferred material.
Method 2
If the empty receiver is not going to be tared, add the material to the receiver,
and place the receiver on the balance in the center of the pan. Record the weight,
and transfer the weighed material to the final flask or receiver: then reweigh the
original weighing receiver by returning it to the same position on the pan. The
second weight represents the sum of the weights of the receiver and the un-
transferred material; subtract this sum from the sum of the total material weight
and the receiver weight to determine the weight of the transferred material.

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Method 3
This method may be described as quantitative transfer. The material is add-
ed to the tared receiver; the amount is determined by difference; and then the
whole amount is transferred quantitatively (e.g. by using a solvent) to the final
receiver.
Materials Handling Safety Procedures
The operator must be familiar with precautions described in the Material safety
Data Sheet for the substance before weighing it. Hazardous materials must be
handled in an enclosure having appropriate air filtration. Many substances are
extremely toxic, possibly allergenic, and may be liquids or finely divided parti-
cles. A mask that covers the nose and mouth should be used to prevent any in-
halation of chemical dust. Gloves should be used to prevent any contact with the
skin. [Note - The use of gloves is good practice for handling any chemical. If it is
necessary to handle the container that is being weighed, the operator should put
on gloves not only for self-protection but also to prevent moisture and oils from
being deposited on the weighed container.] During a weighing, the operator may
be exposed to high concentrations of the pure substance; therefore, the operator
must carefully consider these possibilities at all times.
Weighings are made on many different types of materials such as large sol-
ids, finely divided powders, and liquids (viscous or non-viscous, volatile or
nonvolatile). Each type of material requires its own special handling.
Weighing Solids
Solids come in two forms, large chunks, with or without powdery surface, and
finely divided powders or small crystals. If large chunks with a powdery surface
are to be weighed, at least a piece of weighing paper must be placed on the bal-
ance pan to protect it from damage. Large non-reactive chunks that have no
powdery surface may be placed directly on the pan (for example, a coated t tab-
let). [Note-Solid pieces must be handled with forceps, never by hand.]
Static charge
Fine powders have a tendency to pick up static charge which will cause the
particles to fly around. This static charge must be eliminated before a suitable
weighing can be made. An antistatic device may be used to minimize this
problem. [Note-Such devices may use piezoelectric components or a very
small amount of a radioactive element (typically polonium) to generate a
stream of ions that dissipate the static charge when passed over the powder to
be weighed.] The static charge depends upon the relative humidity of the la-
boratory, which in turn depends upon the atmospheric conditions. In certain
conditions, static charge is caused by the type of clothing worn by the operator;
this charge causes large errors in the weighing when discharged.
Weighing Procedure
Place the receiver on the balance pan, close the balance door, and weigh
as indicated for Weighing by Difference, with the following additions. Carefully
add the powdered material from a spatula until the desired amount is added.
Use care to avoid spilling. Close the balance door, and record the weight as
soon as the balance shows a stable reading.
Spills
If solids are spilled, remove the receiver, and sweep out all of the spilled mate-
rial from the balance. The spilled material must be properly disposed of and must

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not be swept out onto the balance table where other operators may come in con-
tact with the chemical. Then either start the process over or reweigh the remaining
material. [Note Never returns any excess material to the original container. Any
excess material must be disposed of in a proper manner.]
Weighing Liquids
Liquids may be volatile or nonvolatile and viscous or no viscous. Each type
requires special attention.
Weighing procedure
Weigh as directed for Weighing by Difference, with the following conditions.
Liquids should always be weighed into a container that can be closed so that
none of the material is lost. It is best if the liquid can be added to its receiving
container outside of the balance because of the possibility of a spill. [Note-
Liquids spilled within the balance housing can cause serious damage to the
balance, and they may be difficult to remove.)
Non-viscous liquids can be handled with a Pasteur capillary pipette
equipped with a small rubber bulb such as a medicine dropper bulb. The liquid
is discharged into its receiver, the top is closed or stoppered, and the receiver
and contents are weighed. Small quantities of viscous liquids can be handled
by touching a glass stirring rod to the surface of the liquid and then carefully
touching the rod to the side of the receiving vessel, which allows some of the
material to be transferred.
Weighing Corrosive Materials
Many chemical such as salts, are corrosive, and materials of his nature
should not be spilled on the balance pan or inside the balance housing. Ex-
treme care is essential when materials of this nature are being weighed.
CONCLUSION
By carefully following the procedures outlined above, laboratory personnel will
eliminate many errors that might be introduced into weighing procedures. How-
ever, it is important for each balance to be serviced and calibrated regularly by a
specially trained internal or external service person. The balance should he tested
using weights traceable to standardization by NIST. No repairs should be made
to any balance by anyone other than a qualified maintenance person.

ARTICLE 1251 WEIGHING ON AN ANALYTICAL BALANCES RE-

VISION DRAFT

Weighing is a frequent step in analytical procedures, and the balance is an es-

sential piece of laboratory equipment. The general information described here
applies directly to electronic balances used in analytical procedures. Although
many portions of the chapter are applicable to all balances, some are applica-
ble only to this type of balance. This chapter should not be considered all-
inclusive, and other sources of information (e.g., the US National Institute for
Science and Technology and balance manufacturers) may be useful and appli-
cable when analysts perform a weighing operation or implement a weighing
procedure.
The information given in this chapter is applicable not only to balances used
for materials that must be accurately weighed (see Balances <41> but also to
balances used in all analytical procedures.

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QUALIFICATION
Users should consult Analytical Instrument Qualification <1058>, standard op-
erating procedures, and recommendations from manufacturers when they de-
vise qualification plans.
Installation
Users should consult Analytical Instrument Qualification 1058, standard oper-
ating procedures, and recommendations from manufacturers when they devise
qualification plans.
Support surface: The balance should be installed on a solid, level, nonmagnet-
ic surface that minimizes the transmission of vibration (e.g., a floor-mounted,
granite weigh bench). If a metallic support surface is used, the surface should
be grounded in order to prevent the buildup of static electricity.
Location: If possible, the balance should be located in a room that is tempera-
ture and humidity controlled. The location should have a clean, consistent elec-
trical power supply. The location should be free of drafts and should not be
near ovens, furnaces, air conditioner ducts, or cooling fans from equipment or
computers. The balance should be positioned away from outside windows so
that direct sunlight does not strike the balance. The balance should not be in-
stalled near sources of electromagnetic radiation such as radio-frequency gen-
erators, electric motors, or hand-held communication devices (including cord-
less telephones, cellular telephones, and walkie-talkies). The balance should
not be located near magnetic fields induced by laboratory instrumentation or
other equipment.
The performance of the balance should be assessed following installation and
before use in order to demonstrate adequate performance. In some situations, it
may not be possible to position the balance in an optimum environment. Ex-
amples of potential facility issues include the following:
1. Air currents sometimes are present in the laboratory.
2. Temperatures in the laboratory vary excessively (check the manufacturers
literature about temperature sensitivity).
3. Humidity is either very low or very high. Either condition may increase the
rate at which the sample weight varies because pickup or loss of water. Low
humidity increases the buildup of static electricity.
4. Adjacent operations are causing vibration.
5. Corrosive materials are used nearby or are routinely weighed.
6. The balance is located within a fume hood because it is used to weigh cor-
rosive or hazardous materials.
7. The balance is adjacent to equipment producing a magnetic field (e.g., a
magnetic stirrer).
8. Direct sunlight strikes the balance.
In situations when the balance is located near equipment or systems that in-
duce vibration, drafts, electromagnetic radiation, magnetic fields, or changes in
temperature or humidity, the assessment should be conducted with those sys-
tems operating in order to duplicate a worst-case scenario.
Operational Qualification
An operational qualification should be performed either by the user or by the
balance manufacturer after the equipment has been installed. As a minimum,
the power should be turned on and the balance should be allowed to equili-

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brate according to the manufacturer's instructions (124 h, depending on the

type of balance) before use. Depending on the balance, analysts should in-
clude the following procedures in the operational qualification:
1. Mechanical mobility of all moveable parts
2. Control of stable indication
3. Manually triggered or automatic adjustment by means of built-in weights
4. Operation of ancillary equipment
5. Tare function
6. Initial calibration.
Several types of electronic analytical balances use built-in weights for manually
triggered or automatic adjustment. This adjustment usually is applied to reduce
the drift of the balance over time and to compensate for drifts caused by varia-
tions in the ambient temperature. Calibration normally is performed as part of
the operational qualification, but it also can be performed periodically thereaf-
ter. Calibration should be performed at the location where the balance is used
in normal operation.
Performance Qualification
Table 1 provides a list of the most important balance properties that should be
assessed during performance qualification. Depending on the risk of the appli-
cation and the required weighing process tolerance, some of these tests may
be omitted. Tests also can be omitted if there is evidence that the property in
question has only minimal effect on the weighing performance. Any procedures
used should be consistent with in-house standard operating procedures, appli-
cable for the specific balance, and adequately justified. Performance qualifica-
tion should be performed periodically as described in standard operating pro-
cedures, and the frequency of each of the individual tests can vary depending
on the criticality of the property.
The weights that are used to perform the tests should be stored and handled in
a manner that minimizes contamination. Before executing the tests, the analyst
should place the weights in the vicinity of the balance for an appropriate time to
reach sufficient thermal equilibrium. If possible, all tests should be carried out
with only one test weight in order to minimize handling errors. The tests should
be recorded in such a manner that the data can be used to easily track balance
performance and to assist in laboratory investigations as needed. Meaningful
acceptance criteria can be set depending on the required weighing tolerance,
i.e., the maximum allowed deviation permitted by specifications, regulations,
etc., of a quantity to be weighed from its target value. Procedures should be in
place to address test results that are outside acceptable ranges and to provide
assurance that balance cleanliness and environment have not affected the re-
sult. Also, a procedure should be in place for removing a balance from opera-
tion when observed results fall outside acceptable ranges.

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Table 1. Suggested Performance Qualification Tests

Test Definition Example Acceptance Criteria
Change in weighing
value divided by the
change in load, usu-
NMT 0.05% devia-
ally measured be-
The test load at or tion where <41> is
tween zero and the
sufficiently close to applicable. For other
Sensitivity nominal capacity of
the nominal capacity uses, respective tol-
the balance. Sensitivi-
of the balance. erance requirement
ty usually is ex-
divided by 2.
pressed as deviation
from the correct value
at nominal capacity.
Ability of a balance to
follow the linear rela-
tionship between a
NMT 0.05% devia-
load and the indicat-
tion where <41> is
ed weighing value. From 3 to 6 points
applicable. For other
Linearity Nonlinearity usually over the range of the
uses, respective tol-
is expressed as the balance
erance requirement
largest magnitude of
divided by 2.
any linearity deviation
within the test inter-
val.
Deviation in the
measurement value
caused by eccentric
Performed in the
loading in other
center of gravity and
words, the asymmet-
the four quadrants
rical placement of the
(for rectangular plat- NMT 0.05% devia-
center of gravity of the
ter shapes) or at tion where 41 is ap-
load relative to the
analogous locations plicable. For other
Eccentricity load receiver.
for other platter uses, respective tol-
Eccentricity usually is
shapes. Test load erance requirement
expressed as the
usually is between divided by 2.
largest magnitude of
50% and 100% of
any of the deviations
the nominal capacity
between an off-center
of the balance.
reading and the cen-
ter reading for a given
test load.

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Test Definition Example Acceptance Criteria

Ability of a weighing
instrument to display
identical measure-
ment values for re-
peated weighings of
the same objects un-
der the same condi-
10 replicate weigh-
tions, e.g., the same Requirement from
ings (using a test
measurement proce- where <41> is ap-
weight that is a few
Repeatability dure, same operator, plicable. For other
percent of the nomi-
same measuring sys- uses, respective tol-
nal capacity of the
tem, same operating erance requirement.
balance).
conditions, and same
location over a short
period of time. Re-
peatability usually is
expressed as the
standard deviation of
multiple weighings.
Sensitivity, linearity, and eccentricity all account for systematic deviations; i.e.
they limit the accuracy of the balance (based on the definition of accuracy in
Validation of Compendial Procedures 1225 and ICH Q2). In the International
Vocabulary of Metrology (VIM) and documents of the International Organization
for Standardization, this concept is referred to as trueness. Because deviations
are largely independent from each other, it is not likely that all deviations occur
simultaneously and have the same algebraic sign. Therefore the arithmetic ad-
dition of all individual deviations to assess the balance accuracy would consti-
tute a rather conservative approach. A quadratic addition of the individual devi-
ations is a more realistic approach. By allocating 50% of the weighing toler-
ance budget to the acceptance criteria of the individual properties, analysts en-
sure adherence to the required weighing tolerance. These properties or a sub-
set of them also can be taken to fulfill the accuracy requirement described in
<41>.
In this case the acceptance criteria thus allow a maximum deviation of 0.05%
for sensitivity, linearity, and eccentricity. Repeatability preferably is tested with a
test weight of a few percent of the balance capacity. At the lower end of its
measurement range, the performance of laboratory balances is limited by the
finite repeatability, and limitations induced by systematic deviations normally
can be neglected. Therefore, the whole weighing tolerance budget can be allo-
cated to the acceptance criterion of the repeatability test.
For the sensitivity and linearity tests as described above, the analyst should
use certified weights with an appropriate weight class (e.g., according to Inter-
national Organization of Legal Metrology R111 or American Society for Testing
and Materials E617, available from and , respectively). [NOTE If a differential
method is used for the linearity test, certified weights may not be required.] De-
pending on the acceptance criterion, it may be sufficient to consider only the
nominal weight value of the test weights. If the nominal value of the test weight
is considered, analysts should ensure that the maximum permissible error

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does not exceed one-third of the acceptance criterion. Alternatively, if the certi-
fied value of the test weight is considered, its calibration uncertainty should not
exceed one-third of the acceptance criterion. For tests such as eccentricity or
repeatability, the use of certified weights is optional, but analysts must ensure
that the mass of the weight does not change during the test.
The tests described above also can be included in formal periodic calibration in
order to fulfill applicable cGMP requirements.
Balance Checks
A balance check using an external weight helps ensuring that the balance
meets weighing tolerance requirements. The balance check is performed at ap-
propriate intervals based on applicable standard operating procedures. The fre-
quency of the balance check depends on the risk of the application and the re-
quired weighing tolerance. Checks with external weights can be replaced par-
tially using automatic or manually triggered adjustment by means of built-in
weights. When analysts perform the balance check with an external weight, the
same acceptance criteria may apply as described in the sensitivity test above.
Minimum Weight
The minimum net sample weight, mmin, of a balance can be expressed by the
equation:
mmin = k s/required weighing tolerance
where k is the coverage factor (usually 2 or larger) and s is the standard de-
viation (in a mass unit, e.g., in mg) of not fewer than 10 replicate measure-
ments of a test weight. The minimum weight describes the lower limit of the
balance below which the required weighing tolerance is not adhered to. The
equation above takes into account that the performance of laboratory balances
at the lower end of the measurement range is limited by the finite repeatability.
For materials that must be accurately weighed, <41> stipulates that repeatabil-
ity is satisfactory if two times the standard deviation of the weighed value, di-
vided by the nominal value of the weight used, does not exceed 0.10%. For
this criterion the equation above simplifies to:
mmin = 2000 s
If not subject to the requirements of <41>, the minimum weight value may
vary depending on the required weighing tolerance and the specific use of the
balance. To facilitate handling, the test weight that is used for the repeatability
test does not need to be at the minimum weight value but can be larger be-
cause the standard deviation of repeatability is only a weak function of the test
weight value. In order to satisfy the required weighing tolerance, when samples
are weighed the amount of sample mass (i.e., the net weight) must be equal to
or larger than the minimum weight. The minimum weight applies to the sample
weight, not to the tare or gross weight.
Factors that can influence repeatability while the balance is in use include:
1. The performance of the balance and thus the minimum weight can vary over
time because of changing environmental conditions.
2. Different operators may weigh differently on the balance i.e., the minimum
weight determined by different operators may be different.
3. The standard deviation of a finite number of replicate weighings is only an
estimation of the true standard deviation, which is unknown.
4. The determination of the minimum weight with a test weight may not be
completely representative for the weighing application.

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5. The tare vessel also may influence minimum weight because of the interac-
tion of the environment with the surface of the tare vessel.

For these reasons, when possible, weighings should be made at larger values
than the minimum weight.
OPERATION OF THE ANALYTICAL BALANCE
Select the appropriate balance for the quantity and performance needed. Gen-
eral chapter <41> provides requirements for balances used for materials that
must be accurately weighed. The balance user should check the balance envi-
ronment (vibration, air currents, and cleanliness) and status of calibration be-
fore use.
Receivers
To ensure suitable performance in measuring the weight of a specimen, ana-
lysts should consider selection of a proper receiver for the material.
General characteristics: All receivers must be clean, dry, and inert. The total
weight of the receiver plus the specimen must not exceed the maximum ca-
pacity of the balance. With a properly maintained and adjusted laboratory bal-
ance, weighing uncertainty for small samples, i.e., net weights with a mass not
exceeding typically a few percent of the capacity of the balance, essentially is
determined by the repeatability. However, repeatability depends on the size and
surface area of the weighed object. For this reason large or heavy receivers in-
troduce a deviation from the conditions under which the repeatability was de-
termined without considering the receivers. Therefore, either receivers of a low
mass and small surface should be used (especially in cases when specimens
of low weight are being measured) or the repeatability test should be performed
with the receiver placed on the weighing pan as a preload. Receivers should be
constructed from nonmagnetic materials in order to prevent magnetic interfer-
ence with electronic balance components. Receivers should be used at ambient
temperature in order to prevent the formation of air currents within the weighing
chamber.

Solid samples: Receivers for weighing solid materials include weighing paper,
weighing dishes, weighing funnels, or enclosed vessels, including bottles, vi-
als, and flasks. Hygroscopic papers are not recommended for weighing be-
cause they may have a detrimental effect on the observed results. Weighing
dishes typically are constructed from a polymer or from aluminum. Antistatic
weighing dishes are available for measuring materials that retain static elec-
tricity. Weighing funnels typically are constructed from glass or from a polymer.
The design of this type of receiver combines attributes of a weighing dish and a
transfer funnel, which can simplify the analytical transfer of a weighed powder
to a narrow-necked vessel such as a volumetric flask. For solid samples that
are volatile or deliquescent, analysts must weigh the material into an enclosed
vessel. Where practical, analysts should use an enclosed vessel with a small
opening in order to reduce sample weight loss from volatilization or weight
gain from the adsorption and absorption of atmospheric water.
Liquid samples: Receivers for liquid samples typically are inert, enclosed ves-
sels. For liquid samples that are volatile or deliquescent, analysts should use
an enclosed vessel with a small opening, and the enclosure should be re-
placed rapidly following material transfer. Special precautions should be taken

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Article 1251 Weighing on an Analytical Balances revision draft

to be certain that the receiver and the enclosure are constructed from a material
that is compatible with the liquid sample. The receiver and enclosure must
have a seal that is sufficient to prevent leaks from a liquid that is of low vis-
cosity or has low surface tension or a low boiling point.
Types of Weighing
Weighing for quantitative analysis: The initial step for many quantitative anal-
yses is to accurately weigh a specified amount of a sample. Section 6.50.20
in the General Notices stipulates that solutions for quantitative measures must
be prepared using accurately weighed analytes: i.e., analysts must follow
<41>. Errors introduced during the weighing of a sample can affect the accu-
racy of all subsequent analytical measurements.
Addition weighing: Addition weighings typically are used for solid samples or
liquid samples for which volatility is not an issue. The receiver is placed on the
balance. After the balance display stabilizes, the analyst should tare the bal-
ance; add the desired amount of material to the receiver; allow the balance
display to stabilize; record the weight; and quantitatively transfer the material to
an appropriate vessel or, if it cannot be guaranteed that the entire amount has
been transferred, weigh the receiver again and note the weight difference.
Dispense weighing: Dispense weighing typically is used for weighing emul-
sions or viscous liquids such as topical ointments. In these situations it is not
practical to weigh the material into a typical receiver. Accordingly, the analyst
should tare the balance; place the sample on the balance in a suitable con-
tainer (e.g., a bottle, tube, transfer pipette, or syringe) that has been wiped
clean on the outside; record the weight after the balance display stabilizes;
transfer the desired amount of sample to an appropriate receiving vessel, such
as a volumetric flask; and place the pipette or syringe back onto the balance.
The difference in the two weighings is equal to the weight of the transferred
specimen.
Gravimetric dosing: Gravimetric dosing typically is used for sample and
standard preparations or capsule filling. For such weighing the analyst places
the volumetric flask, vial, or capsule shell on the balance; tares the balance af-
ter the balance display stabilizes; adds the solid or liquid components into the
receiver by means of dosing units; and records the respective weights.
Problem Samples
Electrically charged samples and receivers: Dry, finely divided powders may
be charged with static electricity that can make the powder either attracted to or
repelled by the receiver or the balance, causing inaccurate weight measure-
ments and specimen loss during transfer. A drift in the balance readings should
alert the operator to the possibility that the material has a static charge. Com-
mercially available balances with a built-in antistatic device can be used to
remedy the problem. Such devices may use piezoelectric components or a very
small amount of a radioactive element (typically polonium) to generate a
stream of ions that dissipate the static charge when passed over the powder
being weighed. Antistatic weigh boats, antistatic guns, and antistatic screens
also are commercially available. The static charge depends also on the relative
humidity of the laboratory, which in turn depends on atmospheric conditions.
Under certain conditions, static charge is caused by the type of clothing worn
by the operator and this charge can cause large errors in the weighing. Borosil-
icate glassware and plastic receivers have a well-known propensity for picking

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Article 1251 Weighing on an Analytical Balances revision draft

up static charge, especially at low relative humidity. The gloves used to protect
the operator also may increase the potential for a static charge problem. Plac-
ing the container in a metal holder may help to shield the static charge, and
antistatic gloves also can help to alleviate the problem.
Volatile samples: When weighing a liquid that has a low boiling point, ana-
lysts must receive the specimen in a vessel with a gas-tight enclosure of small
diameter. The analyst then tares the vessel and enclosure, adds the desired
amount of sample, and replaces the enclosure. After the balance display stabi-
lizes, the analyst records the specimen weight.
Warm or cool samples: Samples that are warm or cool should be equilibrated
in the laboratory, or the weight readings may be erroneous. With regard to
warm samples, the apparent weight is smaller than the true weight because of
heat convection. For example, a flask that is warmer than ambient air warms
up this air, which then flows upward along the flask and reduces the apparent
weight of the contents by viscous friction.
Hygroscopic samples: Hygroscopic materials readily absorb moisture from the
atmosphere and steadily gain weight if left exposed. Therefore, hygroscopic
samples must be either weighed promptly or placed in a vessel with a gas-tight
enclosure. For a gas-tight vessel, analysts should tare the vessel and enclo-
sure, add the desired amount of sample, and replace the enclosure. After the
balance display stabilizes, the analyst can record the specimen weight.
Aseptic or biohazardous samples: The weighing of sterile or biohazardous
samples should take place within the confines of a clean bench, biosafety cab-
inet, isolator, or similar containment device. Air flow within the hood potentially
can cause balance instability, so after a balance has been installed under a
hood, analysts should perform a rigorous qualification study with suitable
weight artifacts (see <41>) in order to determine the acceptability of the bal-
ance performance in this environment.
Weighing corrosive materials: Many chemicals, such as salts, are corrosive,
and materials of this nature should not be spilled on the balance pan or inside
the balance housing. Extra care is essential when materials of this nature are
weighed. Analysts should consider the use of sealed containers such as weigh-
ing bottles or syringes. In the event of a spill, requalification of balance may be
necessary, depending on the nature of the spill.
Safety Considerations When Weighing
During a weighing, the analyst may be exposed to high concentrations of a
pure substance. The analyst must carefully consider this possibility at all times
and should be familiar with the precautions described in the substance s Mate-
rial Safety Data Sheet before weighing it. Hazardous materials should be han-
dled in an enclosure that has appropriate air filtration. Many toxic and possi-
bly allergenic substances present as liquids or finely divided particles. When
weighing these substances, analysts should use a mask that covers the nose
and mouth to prevent any inhalation of the substance, and they should use
gloves to prevent any contact with the skin. [NOTE The use of gloves is good
practice for handling any chemical. If it is necessary to handle the container
being weighed, the analyst should wear gloves not only for self-protection but
also to prevent moisture and oils from being deposited on the weighed con-
tainer.]

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