Astm E542 22 en Inglés
Astm E542 22 en Inglés
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E542 − 22
1. Sco
Scope
pe 1.4 This standard
standard may be used for the calibration
calibration of volu-
metric
metric ins
instru
trumen
ments
ts mad
madee fro
from
m mate
material
rialss of gla
glass,
ss, plas
plastic,
tic,
1.1 This practice covers procedures
procedures for use in the calibration
various stable metals, or any other stable materials provided
of volum
volumetric
etric instru
instruments
ments that includ
includee glassw
glassware,
are, plastic
plasticware,
ware,
appropriate volumetric coefficients of expansions are available.
and laboratory standards that are in common use in chemical,
analytical, clinical, and calibration laboratories. It is based on 1.5 This standar
standard d doe
doess not purport
purport to add
addre
ress
ss all of the
the gravimetric determination
determination of the quantity of pure water,
water, safety
safe ty co
conc
ncern
erns,
s, if an
anyy, as
asso
socia
ciated
ted wi
with
th its us
use.
e. It is th
thee
either contained or delivered at a calibration temperature, and responsibility of the user of this standard to establish appro-
the conversion of this value to a volume at a given reference priate safety, health, and environmental practices and deter-
temperature, normally 20 °C by means of suitable equations. mine the applicability of regulatory limitations prior to use.
Calibra
Cali bration
tion usi
using
ng mer
mercur
cury
y is exc
exclud
luded.
ed. Cali
Calibra
bratio
tion
n may be 1.6 This inte
interna
rnatio
tional
nal sta
standa
ndard
rd was dev
develo
eloped
ped in acc
accor
or--
performed using alternative gravimetric methodology, if it is dance with internationally recognized principles on standard-
izat
izatio
ionn est
estab
ablis
lishe
hed
d in th thee De
Deci
cisio
sionn on Pr
Prin
incip
ciples
les fo
forr th
thee
demonstrat
demons trated
ed and doc
docume
umente
ntedd tha
thatt the res
result
ultss obt
obtain
ained
ed are Development of International Standards, Guides and Recom-
equivalent to those obtained using the methodology described
herein. Alternative reference temperatures and associated equa-
equa- mendations issued by the World Trade Organization Technical
tions are provided. Barriers to Trad
Tradee (TBT) Committee.
2
For referenced ASTM standards, visit the ASTM website, [Link], or
1
This practice is under the jurisdiction of ASTM Committee E41 on Laboratory contact ASTM Customer Service at service@[Link]. For Annual Book of ASTM
Apparatus and is the direct responsibility of Subcommittee E41.01 on Laboratory Standards volume information, refer to the standard’s Document Summary page on
Ware and Supplies. the ASTM website.
3
Current
Current editio
edition
n approv
approved
ed Jan. 1, 2022. Published
Published Februa
February
ry 2022. Originally
Originally Availab
vailable
le from Intern
Internationa
ationall Organ
Organizatio
ization
n for Standa
Standardiza
rdization
tion (ISO), ISO
approved in 1979. Last previous edition approved in 2021 as E542 – 01(2021). DOI: Central
Centr al Secre
Secretariat
tariat,, Chemi
Cheminn de Bland
Blandonnet
onnet 8, CP 401, 1214 Vernier
Vernier,, Genev
Geneva,
a,
10.1520/E0542-22. Switzerland, [Link]
[Link]
[Link].
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
E542 − 22
NISTIR
NIST IR 737383
83 Sel
Select
ected
ed Pr
Proce
ocedu
dure
ress foforr Volu
olumet
metric
ric for periodic
ments shouldrecalibrations
recalibrations inspected
regularly be as needed
needed.. All tovolum
prior volumetric
use toetric instru-
ensure no
Calibrations, (2019)
SOP
SO P 2 Reco
Recomme
mmende
nded
d Sta
Standa
ndard
rd Ope
Operat
rating
ing Pro
Proced
cedure
ure for visible damage or contamination. Calibration intervals for all
Applyi
App lying
ng Air Buo
Buoyan
yancy
cy Cor
Correc
rectio
tions,
ns, NIS
NISTIR
TIR 696
6969,
9, volumetric instruments may be based on legal requirements,
(2019) manufacture
manuf acturer’s
r’s recomm
recommendati
endations,
ons, contro
controll charts of similar
SOP 14 Recomm
Recommended
ended Standa
Standard
rd Opera
Operating
ting Proced
Procedure
ure for types of volumetric instruments, analysis of history related to
Gravimetric Calibration of Volumetric Standards Using an similar models/types of instruments, use and storage frequency
Electronic Balance, NISTIR 7383, (2019) as well as the handling conditions and the content of materials
SOP 20 Standard Operating Procedure for Standard
Standard Devia- being used. References such as the NISTIR 7383, GMP 11, or
tion and Range Charts, NISTIR 7383, (2019) OIML
OIM L D 10 (ILAC
(ILAC G-G-2424)) ma
mayy be usused
ed to sesett an
andd ad
adju
just
st
SOP
SO P 29 Standard Operating Procedure
Procedure for the Assignment of calibration intervals.
Uncertainty, NISTIR 6969, (2019) 4.2 The following examples are provided to assist end users:
2.4 OIML Standards: 5 4.2.1 Under ideal conditions,
conditions, borosilicate volumetric
volumetric glass-
OIML D 10 (ILAC G-24) Guidelin
Guidelines
es for the Determ
Determination
ination ware will hold its calibration indefinitely provided it is used
of Calibration Intervals of Measuring Instruments (2007) 6 with care and that it is not exposed to hydrofluoric acid, hot
OIML
OI ML D 28 Conventional Value of the Result of Weighing in phosphoric acid, or strong, hot alkalis, and that it is not heated
Air (2004
(2004)) above 150 °C when dry. dry. A frost
frosting
ing of the glass surface (viewed
(viewed
OIML R111 Weights of Classes E1, E2, F1, F2, M1, M1—2, when
whe n dry
dry)) ind
indicat
icates
es tha
thatt che
chemica
micall atta
attack
ck has occoccurr
urred,
ed, and
M2, M2—3 and M3 Part 1: Metrological and Technical recalib
rec alibrat
ration
ion may be in ord order
er.. As a pre
precau
cautio
tion,
n, it is rec
recom-
om-
Requirements (2004) mended
men ded that gla glassw
ssware
are always be ins inspec
pected
ted pri
prior
or to use to
ensure
ens ure no vis visibl
iblee dam
damage
age or cra cracks
cks.. Sig
Signifi
nifican
cantt dam
damageage to
2.5 BIPM Standards:7 glassware that impacts the calibration value is likely to be the
GUM: JCGM 100:2008 Evaluation of Measurement Data— result of breakage. Volumetric instruments with obvious breaks
Guide to the Expression of Uncertainty in Measurement or cracks should not be used. Glassware should be calibrated at
(Also: ISO/IEC Guide 98-3, same title) interv
intervals
als not to exc exceed
eed five yea years
rs unl
unless
ess doc
docume
umenta
ntatio
tion
n of
stabilit
stab ility
y ana
analys
lysis
is can be pro provid
vided
ed to supsuppor
portt ext
extens
ension
ion of
calibration intervals.
4
Available from National Institute of Standards and Technology (NIST), 100 4.2.2 Soda-
Soda-lime
lime volumetric glassware
glassware will become frost frosted
ed
Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, [Link] with time because of attack from moisture in the atmosphere as
5
Available from Organisation Internationale de Metrologie Legale (OIML), 11
well as from the chemicals mentioned above. In addition, it
Rue Turgot, 75009 Paris, France, [Link]
6
Also available from the International Laboratory Accreditation Cooperation, s ho
hou ld
ld n ot
ot b e hea
eate
ted
d ab
abo
ov e 9 0 ° C w hen
hen d ry
ry. I t is
ILAC Secretariat, PO Box 7507, Silverwater NSW 2128, Australia, [Link]
7 8
Available from Bureau International des Poids et Mesures (BIPM), Pavilion de Available from EURAMET, Bundesallee 100, 38116 Braunschweig, Germany,
Breteuil, F-92312, Sèvres Cedex, France, [Link] [Link]
2
E542 − 22
recommended, therefore, that it be inspected prior to use for or equivalent procedures such as EURAMET/cg-18/V. 4.0 (see
damage or cracks and calibrated at intervals not to exceed five Table 2 for resolution and uncertainties). Balances must be in
years. good operating condition with adequate capacity, sufficiently
4.2.3
4.2 .3 Stai
Stainles
nlesss stee
steell and oth
other
er meta
metals
ls use
used
d in vol
volume
umetri
tricc small
sma ll res
resolu
olutio
tion,
n, and suf
sufffici
icient
ently
ly sma
small
ll pr
proce
ocess
ss sta
stand
ndard
ard
instruments may be subject to corrosion over time and some deviation, as verified by a valid control chart or preliminary
may contain mixed materials, such as when they include glass repeatability
repeatability experiments using this proced
procedure.
ure.
gauge tubes with associa
associated
ted fasteners, where contact point
pointss
impact the long-term stability. Storage and transport methods NOTE 1—Standard deviations obtained from mass calibrations or other
may be critical because a minor dent might not be visible on a weighings often do not reflect the process repeatability of gravimetric
calibrations; additional factors such as setting and adjusting the meniscus
met
metal
al in
inst
Materials stru
rumen
ment,
other t, ye
than yett may(for
water impact
imp act th
thee petroleum,
example, calib
calibra
rated
ted metered
volu
volume
me.. and process repeatability
repeatability are normally obtained using this procedure
procedure and
not those for mass calibrations. The accuracy of the balance and weighing
chem
chemica
icals)
ls) ma
mayy als
also
o cau
cause
se a ch
chemi
emical
cal rereact
actio
ion
n wit
with
h th
thee procedures should be evaluated to minimize potential bias in the mea-
material and impact the stability of the volumetric instrument surement process.
overr time
ove time.. Sta
Stainle
inlessss stee
steell vol
volume
umetric
tric ins
instru
trumen
mentsts sho
should
uld be
6.2 Mass stan
standar
dards
ds mus
mustt be ava
availab
ilable
le in nom
nomina
inall val
values
ues
inspected prior to each use for damage and contamination and
slight
slightly
ly la
larg
rger
er th
than
an th
thee no
nomin
minal
al vo
volu
lume
me plplus
us ma
massss of ththee
be calibrated at intervals not to exceed one year.
container and calibrated with adequate accuracy. Specification
5. Unit
Unitss of Measu
Measurem
rement
ent E617 prov
provide
idess spe
specific
cificatio
ations
ns and tol
tolera
erance
ncess for mas
masss stan
stan--
dard
da rds.
s. Ma
Mass
ss st
stan
anda
dard
rdss ar
aree us
used
ed as an ininteg
tegra
rall pa
part
rt of th
this
is
5.1 Volume—Th Thee ba
basi
sicc SI un
unit
it fo
forr vo
volu
lume
me is th
thee cu
cubi
bicc
procedure. They may also be used to calibrate or verify the
meter, m3. Due to its large size, the cubic meter is rarely used
balance prior to use to ensure accurate mass values are used in
in reporting glassware volumetric calibration results but may
be appro
appropriate
priate for metallic standards.
standards. The cubic centimeter,
centimeter, the calibration. Ordinarily, weights with Class 3 (OIML F1) or
cm3, is most often used and is employed in this practice. The better tolerances are required. Uncertainty limits are specified
unit,
uni t, mill
millilit
iliter
er,, mL, may be conconsid
sidered
ered as equ
equiva
ivalen
lentt to the by Specification E617 E617..
cu
cubi
bicc ce
cent
regardingntim
imet
eter
er.. Se
Seee and
conversions NIST
NI ST SP 81
8111 methods
presentation and
and NI
NIST
ST SP 10
1038
for units 38
and 6.3 Thermometer, for mea measusuri
ring
ng th
thee tem
tempe
pera
ratu
ture
re of th
thee
water and air. Thermometers are used for determining the water
symbols. density, the air density, and the volumetric temperature correc-
5.2 Refer
Reference
ence Temperatur
emperature— e—Volum
olumetric
etric instr
instrumen
umentsts for tions. The accuracy of the gravimetric volume measurement
measuring aqueous solutions or liquids other than fuels, and depends on the accuracy of the temperature standards used (see
those referenced in Specification E694 are usually calibrated at Table 2 for resolution and uncertainties).
20 °C. The procedures described provide for such a calibration.
When it is necessary to work at other reference temperatures, 6.4 Barometer, capable of providing atmospheric pressure
such
such as 27 °C in tr trop
opica
icall co
coun
untr
tries
ies,, or fo
forr no
non
n-laboratory measurements
measur ements used in determ
determining
ining air densi
density
ty,, consis
consistent
tent with
applica
app licatio
tions,
ns, gen
generi
ericc equ
equatio
ations
ns are pro
provid
vided
ed in Section 15 15.. the resolution and uncertainty given in Table 2. 2. If barometric
Possible
Possib le altern
alternative
ative refer
reference
ence temper
temperatures
atures and applic
applications
ations pressure is obtained from the local weather service, suitable
are provided in Table 1. 1. assurance must be provided to document that the pressures are
provided at “station elevations” and not “sea level” corrections;
6. Equi
Equipment
pment and Standards
Standards adjustments may be needed for laboratories not at applicable
6.1 Analytical Balance—Balances must have enough capac- elevations.
ity to weigh the loaded vessel or transfer vessel plus a full 6.5 Timing Device, for timing delivery and drain times.
quantity of water. The physical dimensions of the balance must
also accept the size of the vessels which need to be weighed. 6.6 Distilled or Deionized Water, suitable for general labo-
The resolution of the balance may be a limiting factor in the ratory purposes,
purposes, accord
according
ing to Specifi
Specification
cation D1193 T Type
ype III,
accurac
accu racy
y of the meas
measure
uremen
ments.
ts. Cali
Calibra
bration
tion and unc
uncert
ertain
ainty
ty ISO 3696, Class 3, equivalent or better, measured or calculated
analysis of the balance may be conducted using Practice E898 to the nearest 0.000001 g/cm3.
3
E542 − 22
TABLE 2 Measuring Instrument Recommendations
Measurement Parameter and Range Resolution Uncertainty (k = 2)A,B
Balance (Nominal capacity > 2000 mL to 10 000 mL) 10 mg (0.01 g) 40 mg (0.04 g)
Balance (Nominal capacity > 1000 mL to 2000 mL) 1 mg 4 mg
Balance (Nominal capacity 10 mL to 1000 mL) 0.1 mg 0.4 mg
Balance (Nominal capacity < 10 mL) 0.01 mg 0.04 mg
Mass standards (See Specification E617 or OIML ASTM Class 3 < 1/3 of specified tolerances
R111) OIML Class F1
Relative humidity (40 % to 60 %) 1% 5%
Air temperature (17 °C to 23 °C) 0.1 °C 0.2 °C
Water temperature (17 °C to 23 °C) 0.01 °C 0.1 °C
Barometric pressure 0.13 hPa 0.67 hPa
(0.1 mmHg) (0.5 mmHg)
Timing Device (calibration not required) 1s 1 s / 24 h
A
Uncertainties for balances are recommended for the maximum capacity of the balance but may be reduced proportionally according to the applicable range of actual
use.
B
Uncertaintie
Uncertainties
s for other measur
measuring
ing instruments
instruments are determined based on the calibration
calibration and range of use as required.
6.7 Recomm
Recommended
ended tolerances
tolerances and uncer
uncertainties
tainties for measur- the labor
laboratory
atory conditions.
conditions. Referen
References
ces provi
provide
de guida
guidance
nce for
ing instruments used in this procedure and for the calculation equilibration times between 2 h and 24 h and depend on the
of V 20 are provided in Table 2.
2. starting temperatures of each item used in the calibration. The
recommended difference between laboratory instruments and
7. Laborato
Laboratory
ry Condi
Condition
tions,
s, Clea
Cleaning,
ning, Setting and water is less than 0.5 °C.
Adjusting the Meniscus, Timing Considerations
7.3 Cleanliness of Volumetric Instruments:
7.1 This section describes
describes laboratory
laboratory and instru
instrument
ment condi-
7.3.1 The volume contained in, or delivered by,
by, a volumetric
tions and techniq
techniques
ues required to obtain accurate and repro
reproduc-
duc-
instrument depends on the cleanliness of the internal surface. It
ible volum
volumetric
etric measur
measurements
ements..
7.2 Environmental Conditions Needed for Performing Gra- is import
imp
cleaned ortant
ant tha
thattstandard
following volum
volumetr
etric
ic ins
instru
laboratorytrumen
mentsts are ortho
procedures thorou
roughl
ghly
manufac-y
vimetric Volume Calibrations: turer’
turer’ss ins
instru
tructio
ctions
ns bef
before
ore bei
being
ng cali
calibra
brated
ted or use used.
d. Saf
Safee
7.2.1 Stable laboratory
laboratory environments
environments are essential for ob- clean
cle anin
ingg ma
mater
teria
ials
ls sh
shou
ould
ld be us used
ed tak
takin
ing
g ca care
re no
nott to us
usee
taining accurate measurement results. Balances have manufac- cleaning materials that can damage the instrument. Glass and
turer’s normal operating ranges and mass standard and volu- metall vol
meta volume
umetric
tric ins
instru
trumen
ments ts mus
mustt be suf
suffficie
iciently
ntly clea
clean
n to
metric
metr ic ins
instru
trumen
ments ts hav
havee app
applica
licable
ble ref
refere
erence
nce con
conditi
ditions
ons as permit uniform wetting of the surface. When clean, the walls
well. The following temperature and relative humidity condi- willl be uni
wil unifor
formly
mly wetted,
wetted, and the wat water
er will adhere
adhere to the
tions are recom
recommended
mended.. Deviati
Deviations
ons from recommendations
recommendations surface in a continuous film with no obvious air bubbles. The
require assessment of the impact on measurement results. clean
clea n walls of some plastic instruments, however, will not be
7.2.2 T Tempera
emperatur turee of the labor atory sho
laboratory should
uld be betw
between
een wetted. Lack of cleanliness causes irregularities in capacity by
17 °C anand d 23 °C°C,, sta
stabl
blee to 6 1 °C per hour (or during during the distorting the water at the surface of the instrument, appearance
calibra
calibration
tion).
). The closcloserer mea
measur
suremen
ements ts are to the ref refere
erence
nce of air bubbles
bubbles on the inteinterio
riorr sur
surfac
faces,
es, and can impact the
temperature and standard conditions, errors due to coefficients meniscus reading and setting as well as the uniform filling or
of cubical expansion uncertainty, and buoyancy errors associ- delivery of water. Regardless of the type of vessel, if chemicals
ated with usi using
ng bal
balanc
anceses and mass stan standar
dards
ds may be min mini-i- other than water are used for cleaning, always rinse thoroughly,
mized. Balances must be within the manufacturer’s operating first with tap water and then with distilled water and let dry
specifications. fully for “to contain” calibrations.
7.2.3 Relative humidity of the laboratory should be between 7.3.2
7.3 .2 Exa
Exampl
mplee clea
cleanin
ningg met
method
hodss are ava
availab
ilable
le in NIS
NISTIR
TIR
40 % and 60 %, stable to 6 5 % per 4 h to meet most balance 7383, GMP 6 and 7, and GLP 13, ISO 4787, Annex A, and
manufacturer operating conditions. While relative humidity is EURAMET/cg-21/V. 2.0 (for metal volumetric instruments).
used and corrected in the calculation of air density, it does not
correct for potential errors due to evaporation or condensation. 7.4 Reading and Setting a Liquid Meniscus:
Stable
Stab le rel
relativ
ativee hum
humidit
idityy may alsalso
o min
minimiz
imizee the imp
impact
act of 7.4.1 Reading the Meniscus—For all volumetric instruments
evaporation or condensation on the volumetric instruments and calibrated by this procedure, the reading must be made on a
can min
minimiz
imizee the imp impactact of sta
static
tic elec
electric
tricity
ity on vol
volume
umetri
tricc level surface or with the instrument level and the reading made
instruments, mass standards, and balances during the measure- on the lowest point of the meniscus. For the lowest point to be
ments. observed, it is necessary to place a shade of some dark material
7.2.4 WWater
ater and Volume olumetric
tric Instr
Instrument
ument Equilib ration,, to
Equilibration immediately below and behind the meniscus, which renders the
laboratory conditions will minimize potential uncertainties in profile of the meniscus dark and clearly visible against a light
the cali
calibra
bratio
tion
n res
result
ultss due to uncuncert
ertain
ainties
ties ass
associ
ociated
ated with background. A convenient device for this purpose is a collar-
temperature changes during the measurements, water density shaped section of thick black rubber tubing, cut open at one
calculations, and corrections associated with the coefficients of side and of such size as to clasp the tube firmly. Alternatively,
cubical expansion. The length of time required for equilibra- black paper may be used. “Short line” gradu
graduated
ated vessels where
tion is dependent on the starting temperature of the water and the lines are less than one half of the circumference may be
4
E542 − 22
of
of the
the meniscus
upper edgeis obtained by havingline.
of the graduation the eye in the same plane tion line, using the burette stopcock to lower the liquid level,
and touch the tip with the wetted wall of a beaker to remove
7.4.2.
[Link]
2 The position
position of the low
lowest
est poi
point
nt of the meniscus
meniscus any excess water. A weighing flask (transfer vessel) that has
with reference to the graduation line is such that it is in the been tightly stoppered and weighed empty is placed with the
plane of the middle of the graduation line. This position of the inside of the neck in contact with the tip of the burette (the flask
meniscus is obtained by making the setting in the center of the will be at a slight angle).
ellipse formed by the graduation line on the front and the back
8.2 Ful
Fully
ly open the stopcock
stopcock until
until the water
water is only a few
of the tube as observed by having the eye slightly below the
millimeters
millimeters above the graduation
graduation being calibrated
calibrated and then the
plane of the graduation line. The setting is accurate if, as the
stream is slowed to make an accurate setting. When the setting
eye is raised and the ellipse narrows, the lowest point of the
has been completed, move the flask horizontally, breaking the
meniscuss remain
meniscu remainss midway between the fron
frontt and rear porti
portions
ons
contact with the burette. Recheck the setting.
of the graduation line. By this method, it is possible to observe
the approach of the meniscus from either above or below the 8.3 The
Then n sto
stoppe
pperr and weigh
weigh the flas
flask
k a seco
second
nd time, after
line to its proper setting. which re
which refill
fill th
thee th
ther
ermo
mome
meter
ter tu
tube
be an
andd cal
calib
ibra
rate
te th
thee ne
next
xt
NOTE 2—The difference between meniscus positions resulting from the
interval in the same manner as the first one—from the zero
alternative methods of adjustment is the volume equivalent of one half the graduation line to the next graduation line needed.
thickness of the graduation line. In the case of volumetric instruments
where
whe re the cap
capaci
acity
ty is rea
read
d as the dif
differ
ferenc
encee bet
betwee
weenn two menmenisc
iscus
us 8.4
8.4 Fo
Forr bu
bure
rette
ttess wi
with
th a sp
spec
ecifie
ified
d wa
waiti
iting
ng tim
time,
e, us
usee th
thee
readings (for example, on a burette), then no error results if the article is following procedure: after adjustment to the zero graduation
manufactured using one method of adjustment and is later used by the line, fully open the stopcock until the meniscus has reached a
other method. Bias and the impact of visual acuity and lighting when posi
po sitio
tion
n a fefew
w mimilli
llimet
meter
erss ab
abov
ovee th
thee gr
grad
adua
uatio
tion
n lin
linee fo
forr
reading the meniscus should be studied by the laboratory to determine
calibration. After the specified waiting time (for example, 30
differences among operators and may be captured as a component of the
calibra
calibratio
tion
n unc
uncert
ertain
ainty
ty.. Dif
Differ
ferenc
ences
es in rea
readin
dingg the men
menisc
iscus
us may be s), adjust the meniscus to the graduation line, remove the flask,
apparent in the results of interlaboratory comparisons, especially when and weigh.
different procedures are selected for use in each laboratory. Calculation
C alculation of
the uncertainty associated with reading and setting the meniscus
meniscus may be 8.5 Repeat the procedure
8.5 procedure to obtain replicate
replicate values. Report
Report
perfor
per formed
med ususing
ing cal
calcul
culati
ations
ons pro
provid
vided
ed in NINISTI
STIR
R 737383,
83, GM
GMP P 3, the mean of the calibrated values as the calibrated measure-
EURAMET/cg-
EURAM ET/cg-19/V
19/V.. 3.0, or ISO 4787, Annex B as noted in Sectio
Sectionn 17
17.. mentt res
men result.
ult. Use the repeatabi
repeatability
lity of the runs to ensensure
ure the
7.5 Delivery and Drain Times—For volumetric instruments validity of the measurements according to Section 16 and to
used for delivery of a liquid, the volume delivered is always determ
determine
ine the unc
uncert
ertain
ainty
ty com
compon
ponent
ent ass
associ
ociated
ated with the
less than the volume contained, due to the film of liquid left on measurement
measur ement repeat
repeatability
ability according to Section 1717..
5
E542 − 22
10. Cali
Calibrati
bration
on Pro
Procedu
cedure
re of Flas
Flasks
ks (to Contain) 12. Calibration Procedure
Procedure of Other Volumetric
Volumetric
10.1 After
10.1 After cle
clean
anin
ingg an
and
d dr
dryi
ying
ng,, we
weig
igh
h th
thee em
empt
pty
y fla
flask
sk Glassware
including the stopper. Place an appropriately sized funnel in the 12.1 Measuring Pipettes (and Multi-Graduation Pipettes)—
flask to discharge the water below the stopper. Fill from beaker Measuring pipettes may be calibrated by a similar procedure as
or supply line, below the reference line so that the walls of the described in Section 8, except that the tip must be in contact
volumetric instrument considerably above the ring mark are with the wet wall of a beaker or other vessel when the setting
not wetted. is made on the zero line of a measuring pipette. This includes
10.1.1
10.1. 1 Place the flask under a burette and complete filling pipette
pip ettess tha
thatt hav
havee mul
multip
tiple
le gra
gradua
duation
tionss rath
rather
er tha
than
n sin
single
gle
and setting the meniscus, taking care not to splash water on the graduations (one-mark pipettes).
walls, after which place stopper in neck to lessen evaporation
12.2 Graduated Cylinders—Volumetric instruments of this
and weigh. A pipette
pipette or drop
dropper
per with a finely drawn tip may be
kind may be calibrated by the procedures described in Sections
used to adjust the meniscus instead of the burette. Determine
10 or 11
11,, dep
depen
endi
ding
ng on whwhet
ethe
herr th
they
ey ar
aree id
iden
entifi
tified
ed as to
the temperature by placing a thermometer in the filling beaker Contain or to Deliver (often designated as TC or TD).
or in one which has been filled from the water supply. The
temperature may be taken after final weighing by placing a 13. We
Weighing
ighing Measurements
Measurements
ther
th ermo
momemeter
ter di
dire
rect
ctly
ly in ththee fla
flask
sk,, pr
prov
ovidided
ed th
thee fla
flasksk is of
13.1 The analytical
analytical balance that is used should
should meet manu-
sufficient
suff icient size to accommodate it. Alternatively, after weighing,
thee wa
th wate
terr may be po pourured
ed in
into
to a flaflask
sk of su sufffic
icien
ientt siz
sizee to facturer’s
factur er’s specifications
specifications and resoluresolution
tion requi
requirements
rements for the
measurement. Balances may be calibrated following Practice
accommodate the thermometer.
E898 (or use EURAMEURAMET/cg-1
ET/cg-18/V8/V.. 4.0). Follow the balance
10.1.2
10. 1.2 To perperfor
form
m reprepeat
eated
ed cali
calibra
bratio
tions,
ns, two opt option
ionss are
manufacture
manuf acturer’s
r’s instru
instructions
ctions and good laboratory
laboratory practi
practice
ce in
allowed:
making the requis
requisite
ite weigh
weighings.
ings. Weighing
Weighingss shoul
shouldd be made
(1) The flask must be dried between each run. Obtaining Obtaining an
with
wit h car
caree and exp
expedi
editio
tiousl
usly
y to min
minimiz
imizee eva
evapor
poratio
ation
n los
losses
ses
initial dry weight will allow the operator to determine when the
which can constitute a source of error. Care must be taken to
flask is sufficiently dry.
gently place the vessel in the center of the balance pan to avoid
(2) Remo
Remove ve a suf
suffficie
icient
nt amo
amount
unt of liqliquid
uid,, mea
measursuree the
off-cent
of f-center
er loadin
loading g error
errors.
s. Vessels should not be filled while
temperature of the liquid inside the flask, clean the entire neck
so tha
thatt the wal
walls
ls of the volvolume
umetric
tric ins
instru
trumen
mentt con
consid
sidera
erably
bly sitti
sitting
ng on th thee ba
bala
lanc
ncee pa
pann as ththat
at pr
prac
actic
ticee can inintr
trod
oduc
ucee
hysteresis errors. The vessels that are weighed should be clean
above the graduatio
above graduation n lin
linee are not wet
wetted,
ted, set the meniscus
meniscus externally and handled carefully to avoid contamination and
again taking care not to splash water on the walls and weigh the
flask
flask.. Th
Thee in
init
itia
iall va
valu
luee of th
thee dr
drie
ied
d fla
flask
sk is usused
ed in al
alll heat or static transfer. Vessels may be wiped with a clean cotton
cloth as required and covered or stoppered whenever possible
repetitions.
to minimize evaporation. Handling volumetric instruments and
10.2 Repeat the procedure
procedure to obtain replicate
replicate values. Report mass standards with clean cotton gloves is a good practice,
the mean of the calibrated values as the calibrated measure- taking care to prevent wetting or other contamination of the
mentt res
men result
ult.. Use the rep
repeat
eatabil
ability
ity of the runs to ensensure
ure the gloves. See NISTIR 6969, GMP 10 to better understand factors
validity of the measurements according to Section 16 and to affecting weighing operations.
determi
determine
ne the unc
uncerta
ertaint
inty
y com
compon
ponent
ent ass
associa
ociated
ted wit
with
h the
measurement
measur ement repeat
repeatability
ability according to Section 1717.. NOTE 3—Balance indications are conventional mass values and based
on cali
calibra
bratio
tion
n wit
with
h kno
known
wn mas
masss sta
standa
ndards
rds cal
calibr
ibrated
ated to a ref
refere
erence
nce
temp
temper
erat
atur
uree of 20 °C
°C,, a re
refe
fere
renc
ncee ma
mass
ss de
dens
nsit
ity
y of 8.8.0
0 g ⁄cm3, an
⁄cm and
d
11. Calibration Procedure
Procedure of Flasks (to Deliver)
refere
reference
nce air den
densit
sity
y of 0.0
0.0012
012 g/c
g/cmm3 per OIML D 28. The rec record
orded
ed
11.1
11 .1 Do not dry flasks that are calibrated to deliver
deliver prior to balance indications provide conventional mass values and are uncorrected
the tes
the test.
t. Fil
Filll th
thee fla
flask
sk to ap
appr
prox
oxim
imate
ately
ly th
thee in
inde
dex
x lin
linee an
and
d for air buoyancy under the conditions of calibration.
empty rapidly by gradually inclining the flask to avoid splash- 13.2 One weighing
weighing is required of the mass standard
standard used in
ing on the walls as much as possible. When the main drainage this procedure
procedure (one-point
(one-point balanc
balancee calibra
calibration).
tion). A mass standard
stream has ceased, the flask will be nearly vertical.
vertical. Hold in this is selected to be slightly larger than the loaded capacity of the
position for 30 s and touch off the drop of water adhering to the volumetric instrument to provide a calibration correction factor
top of the flask. Place a watch glass or plastic cap on the flask between zero and the full mass of the vessel loaded with water
6
E542 − 22
being weighed. First zero the balance and then gently place the same time and location as the measur
measurements
ements of the calibr
calibration.
ation.
mass standard in the center of the balance pan and record the Measur
Mea suremen
ements
ts imm
immedi
ediatel
ately
y bef
before
ore and aft
after
er the cali
calibra
bratio
tion
n
reading as IM. may
ma y be us
used
ed to dedeter
termin
minee av
aver
erag
agee co
cond
nditi
ition
onss as we
well
ll as
NOTE 4—For large volumes, and longer time intervals, mass standards
verification of environmental stability during the calibration.
at the loaded and at the empty mass of the volumetric instrument, and
14.2 Measu
Measurement
rementss of water temperature
temperature must be made to
buoyancy conditions for filled and empty instruments, may be needed with
appropriate modifications in the procedure and associated equations. See dete
determ
rmin
inee th
thee tem
tempe
pera
ratu
turere of th
thee wa
wate
terr us
used
ed du
duri
ring
ng th
thee
NISTIR
NISTI R 7383, SOP 14 for alternative
alternative proced
procedures
ures and equati
equations
ons for larg
largee calibration as close to the time of calibration as possible, taking
volumes. Alternatively, use Practice E898 or EURAMET/cg-18/V
EURAMET/cg-18/V.. 4.0 and into consideration that the insertion of a thermometer into a
calibrate the balance prior to use and use a factor of 1 in lieu of the value volumetric instrument where possible will remove the mass of
Ms/IM. water being weighed when done prior to the weighing. Care
13.3 Two weighings
weighings are required of the volum volumetric
etric instru- must also be taken to minimize possible gradients in the neck
mentt or tran
men transfe
sferr ves
vessel,
sel, nam
namely
ely IL refreferr
erring
ing to the loaloaded
ded of flasks or volumetric instruments due to handling methods
vessel, and IE referring to the empty vessel. Normally, I E and and or due to lack of water equilibration with the laboratory
IL are ob
obseserv
rved
ed ununde
derr th
thee sa
same
me co cond
nditi
ition
ons,
s, an
andd araree be
best
st environment. Volumetric instruments will gradually equilibrate
obse
ob serv
rved
ed by ze zero
roin
ingg th
thee ele
electr
ctron
onicic ba
balan
lancece pr
prio
iorr to eaeach
ch with the lab
labora
orator
tory
y env
enviro
ironme
nment
nt dep
depend
ending
ing on the mas
masss of
measurement. Both required weighings must be completed in water
wat er pre
presen
sentt and can inflinfluen
uence
ce meas
measure
uremen
mentt res
results
ults if not
as short a time interval as convenient to ensure that weighings
made as quickly as possible.
are being made under similar environmental conditions. The
air temp
tempera
eratur
ture,
e, rel
relativ
ativee hum
humidi
idity
ty,, and bar
barome
ometric
tric pre
pressu
ssure
re
15. Calc
Calculat
ulations
ions
should be recorded within or as near to the balance as possible
for use in air dendensity
sity calculatio
calculations.
ns. The masmasss of volvolume
umetri
tricc 15.1 Calc
15.1 Calcula
ulate
te the volume
volume frofrom
m the weight
weight of the wate
water,
r,
instrument or transfer vessel is weighed with both loaded and contained or delivered, as follows:
empty conditions, thus cancelling any corrections associated
with the density and buoyancy of the vessel/instrument itself. V 20 5 ~ I L 2 I E ! S DS
MS
IM
12
ρa
ρS
DS 1
ρw 2 ρa
D@ 1 2 γ ~ t 2 20! # (1 )
14. Temperatur
emperaturee and Environme
Environmental
ntal Measurements 15.2 Water Densit
Densityy Calcul
Calculations—Calculate water density
ations—
14.1 Measur
14.1 Measureme
ements
nts of the air tem
temper
peratu
ature,
re, bar
barom
ometr
etric
ic using the following equations. Sample calculation results are
pressure, and relative humidity must be made at nearly the provided in Table X1.2 for use in verifying calculations.
S D
MS
IM
The mass divide
divided
d by the balanc
balancee indica
indication
tion produc
produces
es a “cali
“calibratio
brationn correc
correction
factor” for the balance at the maximum point of use. This value becomes 1 when
tion
S 1
ρ w2 ρ a
D A density term which requires the calculation of air density, ρ a, and water density,
ρw, and corrects for buoyancy differences between the conventional mass value
reported at reference conditions of 20 °C and mass density of 8.0 g/cm 3 and the
density of water, which is slightly less than 1 g/cm 3 (see Eq 4).
[1 – γ (t – 20)] The thermal expansion factor used to convert the volume from the temperature
of the measurement in degrees Celsius, to the reference temperature of 20 °C.
The symbol γ represent
representss the coefficient
coefficient of cubica
cubicall expans
expansion
ion of the volumetric
instrument or transfer vessel. Table X1.1 provides a short table of possible coeffi-
cient of cubical expansion values. Specific data may be provided by the volumet-
ric instrument manufacturer as well.
[1 – γ (t – t ref)] The thermal expansion factor used to convert the volume from the temperature
of measurement in degree
degrees s Celsiu
Celsius,
s, to an alternative reference
reference temperature.
temperature. The
symbol γ represents the coefficient of cubical expansion of the volumetric instru-
ment or transfer vessel.