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“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 1448-32 (1992): Methods of test for petroleum and its

products, Part 32: Density and relative density [PCD 1:
Methods of Measurement and Test for Petroleum, Petroleum
Products and Lubricants]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 ,IS144S[P:32]:1992
.
( Reaffirmed 2003 )

Indian Standard
PETROLEUM AND ITSPRODUCTS-
METHODS OF TEST
[P:32]

DENSITY AND, RELATIVE DENSITY

(Second Revision )

UDC 665-61-7: 531.756

@ BIS 1992

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

November 1992 Price Group 8

Methods .of Test for Petroleum ‘Products and Lubricants Sectional Committee, PCD 1

FOREWORD
This Indian Standard [ P : 32 ] ( Second Revision ) was adopted by the Bureau of Indian Standards,
after the draft finalized by the Methods of Test for Petroleum, Petroleum Products and Lubri-
cants Sectional Committee had been approved by the Petroleum, Coal and Related Products
Division Council.
While preparing the standard considerable assistance has been derived from the standards
IP 59/82, IP 189/86 and IP 190/86, issued by the Institute of Petroleum, London ( U. K. ).
Provisions have been made in this standard for the conversion of density and relative density
from the test temperature to 15°C or 20°C by using the ASTM/IP Petroleum Measurement Tables
( Clause 3.4.1 ). Accordingly, use of various tables viz. Tables 23A, 23B, 23D. 24A, 24B,
24D, 53A, 53B, 53D, 54A, 54B, and 54D of IP 200 and Table A and Table B of IP 250 referred
to in API-ASTM-IP Petroleum Measurement Tables ( API 2540; ASTM D 125O/IP 200 and IP
250 ) has been felt necessary for the purpose of corrections for thermal expansion of the
pyknometer in the calculation of density from measurements made at a temperature at which
the pyknometer has been calibrated ( Clauses 9.3 and 17.3 ). The Tables mentioned above have,
however, not been included in the standard as the same are widely known and in use since long
by the various testing laboratories.
In reporting the results of a test or analysis made in accordance with this standard, if the final
value, observed or calculated, is to be rounded off, it shall be done in accordance with
IS 2 : 1960 ‘Rules for rounding off numerical values ( revised )‘.
 IS1448[P:32]:1992

Indian Standard
PETROLEUM AND ITSPRODUCTS-
METHODS OF TEST
[P:32]

DENSITY AND RELATIVE DENSITY

( Second Revision)
1 SCOPE reference temperature t, is 4X!, relative density
and density are numerically equal since the
1.1 Four methods are described to determine density of water at 40~ is unity.
the density and relative density of solid and
liquid petroleum products and similar materials. 3 METHOD A ( RELATIVE DENSITY
BALANCE METHOD )
1.1.1 The application of these methods is 3-L Outline of the Method
indicated in the following tabIe: A plummet suspended from the graduated

Product RecommendedMethods
a) Mobile liquids with Reid vapour A. Density Balance method
pressure up to l-3 kg/cm*, e. g., Bicapillary pyknometer method
Stabilized crude oil c”: Capillary stoppered pyknometer method
Stabilized Gasoline
Naphthas
Kerosine
Gas oils
Lubricating oils
Non-waxy fuel oils
b) Viscous liquids and semi-solids, C. Capillary stoppered pyknometer method
e. g., Waxy fuel oils
Slack waxes
Soft bitumen
c) Solids, e. g., Bitumen C. (9 Capillary stoppered pyknometer method
D. (ii) Displacement method

2 TEBMINOLOGY beam of a density or relative density balance

2.1 Density of Solids and Liquids ( Rig. 1 ), such as the Westphal balance, is
immersed in the liquid which is held at the test
The density o a solid or liquid substance at a temperature. Four rider weights are then dis-
temperature t is defined as the mass of the posed on the beam in such a way as to return
substance occupying unit volume at a temper- the latter to its original position. The positions
ature t. When reporting the density the units of the tiders on the beam gives a direct indi-
of mass and volume used together with the cation of the relative density of the liquid. The
temperature shall be explicitly stated, for density of the material is calculated from its
example, grams per millilitre at t”C. relative density. The amount of sample
required is small ( 15 ml ), and practically all
2.2 Relative Density of Solids and Liquids of it is recoverable.
Relative density t,/t* of solid and liquid sub-
stance is defined as the ratio of the density of
the substance at a temperature t, to the den- 3.1.1 This method is suitable for determining
sity of water at a temperature t2. When the quickly and accurately the density or relative

1
IS 1448 [ P : 32 ] : 1992

density of petroleum products, such as gaso- 20°C may be done by using the ASTM/IP
line, kerosine, and gas oil, particularly when Petroleum Measurement Tables.
the quantities available for test are small.
3.4.1.1 For the. measurement. of temperature,
3.2 Apparatus suitable thermometer graduated in tenths of a
degree shall be used.
3.2.1 Balance - Westphal or equivalent bala-
nce, capable of determining relative density or 3.5 General Precautions
density to the forth decimal place, and equipped 3.5.1 All apparatus shall be absolutely clean
with a plummet for use at the test temperature. and dry before use. When drying and filtering
3.2.2 Sample Gntainer - A jacketed container the liquid samples for the removal of water
in which the sample temperature, may be kept and suspended impurities, precautions shall be
constant at the test temperature, and from taken to minimize loss of volatile constituents.
which the sample may be run off at the conclu- 3.5.2 When the products are heated to facili-
sion of the test. tate pouring, changes due to evaporation of
3.2.3 Balance Case - To protect the balance volatile constituents shall be avoided.
from draughts and dust. 3.6 Standardization
3.2.4 Support for the Sample Container - -A 3.6.1 Assemble the apparatus as shown in
device for supporting the sample container in Fig. 1 and, using a suitable pump, circulate
a vertical position within the balance case. water from the bath through the annulus of
the sample container ( 1 in Fig. 1 ) so as to r
3.2.5 Water-Circulating Pump
keep the temperature, as measured by the
3.2.6 Constant-Temperature Bath - A water- thermometer ( 2 in Fig. 1 ) in the container,
bath capable of maintaining the sample at the at the test temperature f 0~05C.
test temperature to within f 0*05”C. 3.6.2 Standardize theinstrument in the follow-
3.2.1 Thermometer -- See 3.4.1.1. ing way:
Adjust the balance to equilibrium in air,
3.3 Buoyancy Corrections and then fill the container with freshly
3.3.1 To obtain the true relative density, that boiled distilled water. When the latter
is the relative density in vacuum, of a substance has reached test temperature ( 10 to 15
from its relative density in air as determined minutes ) adjust the riders of the beam ( 3
by comparing the mass in air of equal volumes in Fig. 1 ) until equilibrium is obtained
of the substance and water, a correction shall and read the result to the fourth decimal
be applied for buoyancy of the air. This cor- place. All subsequent results obtained
rection for the temperature of 15°C is given from the balance shall be divided by this
by the following formula: figure.
3.6.3 Empty the container by opening the tap
The true relative density, B ( 4 in Fig. 1 ) at the bottom; clean it with
= A - 0.001 2 ( A - 1 ) acetone, drain it, and dry it with a current
of air.
where
A = relative density in air. 3.7 Procedure
For ready reference, buoyancy corrections 3.7.1 Pour the sample to be tested into the
for various values of [ 0*0012 ( A - 1 ) ] are clean sample container without splashing, so
given in Table 1. as to avoid the formation of air bubbles and
to reduce to a minimum the evaporation of the
3.4 Temperature Corrections for Liquid Substances lower-boiling constituents of the lighter oils.
In the case of reference determinations, errors
3.4.1 Whenever possible the substance whose arising from changes in the volatility may be
density or relative density is being determined avoided by transferring the sample to the
should be brought to the reporting tempera- sample container by water displacement or by
ture. When this is not practicable the siphoning. If air bubbles are formed, remove
deviation from the reporting temperature them after they have collected on the surface
should not exceed 10°C for obtaining good by touching them with a piece of clean blot-
results. The conversion of density and relative ting paper or filter paper before placing the
density from the test temperature to 15°C or plummet in the sample.

2
 IS 1448 [P:32]:19!82

FIG. 1 RELATIVEDENSITYBALANCE

3.7.2 Make the determination on the material 3.9 Precision

under test using the technique described
in 3.6.2 and divide the result by the value Results of duplicate tests shall not differ by
obtained for distilled water. This gives the more than the following amounts:
relative density in air of the product at the
test temperature. Size of Phment Repeatability Reproducibility
5 ml 0~000 4 O-000 4
3.8 Calculation and Reporting

relative density in vacua. 4 METHOD B ( GRADUATED BICAPILLARY

3.8.1 To obtain PYKNOMETER METHOD )
correct the relative density 15°~150C in air
by applying the buoyancy correction from 4.1 General
Table 1. Report the value to the forth decimal
place as relative density 15O/15°C. 4.1.1 This method covers the determination of
the density of crude petroleum and of petro-
3.8.2 To obtain the value of density in vacua, leum products or mixtures of petroleum and
for example at 15°C correct the relative density non-petroleum products normally handled as
15”/15”C by applying the buoyancy correction liquids. The method is restricted to liquids
from Table 1, then multiply the figure so having Reid vapour pressures of l-25 bar
obtained by the density of water at 15°C which ( 1.25 x lo5 Pa ) or less and having viizosities
is O-999 1 g/mI. Report the result to the fourth less than 50 centistokes at test
decimal place. temperature.

3
IS 1448 [ P : 32 ] : 1992

Table 1 Buoyancy Corrections

( &use 3.3.1 )

[ Coriections to be added are shown with ( + ) mark and those to be subtracted with (- ) mark J

Relative
Density
at

0 40 +omO7 +owO7 +omO7 +omO7 +0+007 +O+IOO7 $0.0006 + OTNIO6 to.0066 +0~0006
0.50 +0.0006 +0.0006 +0.0006 +-OWO6 -;-OGIO6 +0.0005 +oxmO5 +0+005 +oGOO5 + 0~0005
0.60 +oGOO5 +0@005 +oQOo5 +0*0004 -+ 0.0004 -1.omO4 +0~@004 +0*0004 -+oGOO4 +0.0004
0.70 +oGLO4 +.0*0003 +owO3 +0.0003 +omO3 $-0+003 +odOO3 +oGOO3 +- 0.0003 +omO3
0.80 $0~0002 +0+002 +omO2 + omO2 +omlO2 +0~0002 +oGOO2 +omO2 +0@002 $OmOl
0.90 -1.OmOl +o~OOol +omot +0xmO1 $-OmOl -+0+KlO1 0*0000 0.0000 0mOO owOo
l@O O+@OO o*ooOO 0mOO 0~0000 0~0000 -0+001 -0wO 1 -0dIOO1 AmOO -oQOOi
1.10 -0wO1 -0GOO1 -OT@Ol -0mO1 -0mO2 -0wO2 -0QOO2 -0.0002 -0mO2 -0~0002

4.1.2 Special precautions are described for

determining the density of highly volatile r- 26-30 _I
liquids.
4.1.3 The method is recommended for the
accurate determination of the density of all
except the more viscous products, and is parti-
cularly useful when only small amounts of
sample are available.

4.2 Outline of the Method

127
‘The liquid sample is drawn into the pykno-
meter and after it has reached equilibrium at
the test temperature the liquid levels are noted
and the pyknometer is weighed. The density of
the sample is then calculated from its weight,
a calibration factor proportional to an equal
volume of water and a term which corrects
for the buoyancy of air.

o
5 APPARATUS

5.1 Pyknometer - capacity 2 !o 10 ml con-

forming to the dimensions given in Fig. 2
constructed of boros%cate or soda-lime glass,
annealed after manufacture, and having a total
I
?*0444

- A4
weight not exceeding 30 g. Any bicapillary
pyknometer conforming to these requirements
may be used.

5.2 Constant Temperature Bath - water bath

having a depth of at least 300 mm, capable
of being maintained within f 0.05°C of the
desired temperature.

5.3 Bath Thermometer - See 3.4.1.1. Other total

x/ 6-12

immersion thermometers of suitable range and All dimensions in millimetres.

equal or greater accuracy may also be used. FIG. 2 GRADUATEDBICAPILLARYPYKNOMETER

4
 IS 1448 [ P : 32 ] : 1992

5.4 Pyknometer Holder ( Optional) - to allow NOTE - If the balance is not fitted with a static
the pyknometer to be mounted vertically at eliminator, static charges may be dissipated by
breathing on the pyknometer. In such cases ensure
the correct depth in the constant temperature that the pyknometer has regained constant mass
bath. A suitable design is shown in Fig. 3; it before recording the weight.
shall be constructed of metal which will not
corr\)de in the water bath. A series of pykno- 7.2 Fill the pyknometer with sufficient freshly
meter holders may be supported in the boiled, cooled, distilled water to obtain read-
constant-temperature bath by the use of a non- ings near the top of the graduated capillaries.
corrodible rectangular metal bar of sufficient Filling is readily achieved by placing the hook-
length to lie across the rim of the bath. A ed tip in the liquid while keeping the pykno-
series of holes of sufficient diameter to accom- meter upright, thus allowing the liquid to be
modate the 6.5 mm rod of the pyknometer drawn over the bend in the capillary attraction.
holder is drilled in the bar at about 45 mm
apart. Each rod is secured in its hole by
locking the bar between the hexagon nut and 19
the wing nut and washer. SPRING CLIP
0.3 THICK SHEET
, (METAL BRASS)
Alternatively any other form of pyknometer
mounting may be employed which allows the SECTION A-A
pyknometer to be held vertically in the cons-
tant temperature bath at the correct depth of
immersion. QIQ- W’NG NUT
clcF--- WASHER
5.5 Balance - capable of weighing to the near-
est 0.1 mg. w HEX
NUT
+ :$;;6xD; EQUIVALENT)
6 PREPARATION OF APPARATUS
rl
6.1 Thoroughly clean the pyknometer with
surfactant cleaning fluid, rinse well with SOLDER
distilled water, then with acetone and dry.
Ensure that all traces of moisture are removed
by drying with a current of filtered air passing
slowly through the pyknometer. Wipe the
outside of the pyknometer with a clean, lint-
free cloth. Cleaning should be carried out in
this manner whenever the pyknometer is to be
calibrated or whenever liquid fails to drain
cleanly from the internal walls of the pykno-
meter. Normally the pyknometer may be
cleaned between determinations by washing
with a suitable light petroleum solvent, follow-
ed by vacuum drying.
NOTE - If sufficient cleauing fluids do not give
adequate cleaning, chromic acid cleaning solution
may be used. 0.3 THICKSHEET
METAL TRAY
CAUTION : Chromic acid is potentially ( BRASS)
hazardous in contact with organic materials / 3 HOLES 03.2
and is toxic and highly corrosive. If used
wear approved face-shield and full-length
protecting clothing including gloves.

7 CALIBRATION OF APPARATUS
SECTION B-B
7.1 After drying allow the pyknometer to All dimensions in millimetres.
reach room temperature. Dissipate any static
charge which may have formed and weigh to FIG. 3 A SUITABLE DESIGN OF PYKNOMETBR
the nearest O-1 mg. HOLDER

5
IS 1448 [ P : 32 1 : 1992

The pyknometer then fills by syphoning. Place approximately the test temperature by the
the pyknometer in the constant temperature method described in 7.2, so that the liquid
bath so that the whole of the liquid in the levels are in the graduated portions of the
pyknometer is below the level of the .bath capillaries. When the test temperature is lower
liquid. Maintain the temperature of the bath than the laboratory temperature low scale
at 15” f 0*0X or within f 0.05”C of the requ- readings should be aimed at in order to
ired calibration temperature. Keep the minimize any losses due to evaporation during
pyknometer in the bath for 20 min then read weighing. Bring the pyknometer and contents
the scale to the nearest small division at the to the test temperature t, by immersion for 20
liquid level in each arm. minutes in the constant temperature both as
described in 7.2 and obtain readings of the
7.3 Remove the pyknometer from the bath, liquid level in the two graduated arms. In
allow the water on the exterior to drain off the case of the more viscous and/or opaque
and wipe with a clean, dry, lint-free cloth. samples no readings must be taken until ample
Allow to come to room temperature, dissipate time for draining has been allowed after any
any static charge, and weigh to the nearest disturbance of the pyknometer. The 20 min-
071 mg. utes immersion time is normally sufficient,
provided that the pyknometer has not been
7.4 The difference between the weights of the
disturbed during this period.
filled and empty pyknometer gives the weight
of water contained by the pyknometer at the NOTE - For mixtures of non-petroleum products
test temperature, corresponding to the some it is essential to ensure that the test temperature
of the two scale readings. By removing is the same as the final reporting temperature
successive quantities of water repeat the deter- unless an approximate value is acceptable and the
volumetric compression of the mixture is known
mination so as to obtain a series of at least together with the volumetric correction coefficient
three pairs of readings, together wi’th the of the components in the mixture.
corresponding weights, with the water level at
different scale points on the graduated arms. 8.3 Remove the pyknometer from the bath,
One pair of readings should be at the upper allow the water on the exterior to drain off‘
end of the scale and another at the lower end. and wipe with a clean, dry, lint-free cloth.
Plot the sums of the scale readings on the two Allow to come to room temperature, dissipate
arms against the corresponding weights. The any static charge, and weigh to the nearest
points should lie on a straight line which gives 0.1 mg.
the weight of water contained by the pykno-
meter for any combined scale reading. If the 8.4 When carrying out the determination on
points show a scatter of more than two small highly volatile samples containing appreciable
scale divisions as marked on the pyknometer amounts of material boiling below 20X!, or for
arms on either side of a straight line drawn any sample where there is uncertainty concern-
through the array of points and subsequent ing loss which might result from evaporation
test do not correct this, discard the pyknometer during the determination, cool the sample and
as imperfect. pyknometer to a temperature of 0” to 5°C
before filling. If the dew point is sufficiently
7.5 If it is desired to determine density at a high to cause condensation of moisture in the
temperature other than 15oC calibrate the pyknometer during the cooling operation,
pyknometer at the desired temperature. attach a drying tube to the arm of the pykno-
meter in order to avoid this. With samples
7.6 Re-calibrate pyknometer at intervals as of this type it is essential to restrict the filling
dictated by experience. of the pyknometer to obtain a low scale
NOTE - It is reeommended that pyknometer be reading thus minimizing losses due to evapora-
calibrated at the test temperature at which densities tion. If the total length of unfilled capillary
are to be determined, s&e this greatly simplifies is over 10 cm the rate of diffusion is so low
the calculation of densities and eliminates any that even with highly volatile compounds such
uncertainty as to the coefficient of cubical expansion
of the glass used in the manufacture of the iso-pentane losses during the
pyknomcter. iitermination are ‘n”.$bly low.
8 PROCEDZJRE 9 CALCULATION AND REPORTING
8.1 Weigh the clean, dry pyknometer to the 9.1 Symbols
nearest O-1 mg, dissipating any static charge The following symbols are used in the calcula-
if necessary ( see Note under 7.1 ). tions:
8.2 Fill the pyknometer with the sampIe at ta - any reference temperature, e.g. 15°C;

6
 IS 1448[P : 32 1: 1992

tc - the temperature at which the pykno- Table 2 Buoyancy Corrections*

meter is calibrated by water filling ( see 7.2
and 7.5 ); ( Clause 9.1 )
tt - the temperature at which the pykno-
meter is filled with the liquid under test w-mm, Correction, mt - m, Correction
( see 9.2.2 ); m, - m, g/ml m-m, g/ml
m, - the apparent mass in air ( weight in 060 OWO 48 0.80 O@OO 24
air ) ( g ) of the empty pyknometer; 0.61 OmO 47 0.81 OX)00 23
- the apparent mass in air ( g ) of the 0.62 OQOO46 0.82 0*000 22
Fiknometer filled with water at the cali- 0.63 oxlOO 44 0.83 OaOO 20
bration temperature t, ; 064 0aOO 43 O-84 0GOO 19
mt - the apparent mass in air ( g ) of the 0.65 OGJO 42 0.85 O-000 18
pyknometer filled with the liquid under test 0.66 oaOO 41 O-86 0-000 17
at the temperature tt ; 0.67 0mO 40 O-87 OGIO 16
0.68 O+OO 38 0.88 o*oOO 14
C - the correction for air buoyancy, in g/ 0.69 0aOO 37 0.89 0*000 13
ml ( see Table 1 ); OGOO 36
0.70 0.90 oaOO 12
the density of water, in kg/m”, at the 0.71 OaOO 35 0.91 oao 11
fgcpcrature of calibration tt ( see Table 2 ); 0.72 0.000 34 0.92 OaOO 10
aI - the coefficient of cubical expansion of 0.73 O+XIO32 0.93 OXJO 08
borosilicate glass ( see 9.3.2 ); 0.74 0aOo 31 0.94 owe 07
0.75 o*OOo 30 0.95 0.000 06
as - the coefficient of cubical expansion of 0.76 oaOo 29 0.96 OaOO 05
soda-lime glass ( see’ 9.3.3 );
0.77 0.000 28 o-97 OaOO 04
it - the density of the sample, in g/ml, at 0.78 0.000 26 0.98 oaOO 02
the test temperature tt ; o-99
0.79 0*000 25 0*000 01
Ps- the density of the sample in g/ml, at
any reference temperature ts ; *Calculated for standard air of density O*OOl222 g/ml
at 1556°C and at a pressure of 1.013 bar.
pls - the density of the sample, in g/ml, at
the reference temperature of 15OC; These corrections are applicable for air density
values between O*OOl 1 and OJMll 3 g/ml.
pz,,- the density of the sample, in g/ml, at
the reference temperature of 20°C;
@ - the apparent density, in g/ml, at the 9.3 Corrections for the Thermal Expansion of
test temperature tt as determined in soda- the Pykuometer
lime glass apparatus calibrated at the refe-
rence temperature ts = 15” or 20°C, i.e. the 9.3.1 General
observed density uncorrected for glass
expansion - required for entering the API- The calculation of density from measurements
ASTM - IP Petroleum Measurement made at the temperature tt which differs from
Tables. the temperature tt at which the pyknometer
was calibrated, involves a correction for cubical
NOTE -The conventional unit g/ml has been expansion or contraction of the glass from
retained for this calibration although the API- which the pyknometer is made.
ASTM-IP Petroleum Measurement -Tables for
density are given in kg/ems.
If the calculation is based on the density
9.2 Reference, Calibration and Test correction tables given in the API - ASTM - IP
Temperatures Petroleum Measurement Tables or TP 250,
a similar correction may also be required
9.2.1 The pyknometer may be calibrated at any ( see 9.3.4 ).
convenient temperature and this may corres-
pond with the reference or test temperatures. 9.3.2 Pyknometer Made of Borosilicate Glass
It is recomended that pyknometers be calibra-
ted at the test temperature at which densities 9.3.2.1 The coefficient of cubical expansion of
are to be determined since this greatly simpli- borosilicate glasses are known to depend on
fies the calculation of density and only the the glass to fall three main categories having
calculations given in 9.4.1.1, 9.4.2.1 and 9.4.2.2 coefficient of cubical expansion of 10x 10S6,
then apply. 14 x IO-6 and 19 x 10m6per 1°C respectively.

7
IS 1448 [ P : 32 1 : 1992

For determination of the highest accuracy using Tables 53A, 53B, 53D or Table A when
when borosilicate pyknometers are used, there- tc = 15” or 20°C as appropriate to the table
fore, either entered.
a) ensure that tt = tc’ or If te does not correspond to the reference
b) use a pyknometer for which the coefficient temperature ts for which the table used is cons-
of cubical expansion is known. When the tructed, an adjustment is required for the
foregoing is not possible and a lower pre- expansion of the pyknometer over the tempera-
cision is acceptable, the use of 10x 10S6 ture range tc-+ts.
per 1°C is recommended.
9.3.3 Pyknometers, Made of Soda-lime Glass 9.3.4.5 Alternatively, the corresponding volume
correction Tables 54A, 54B, or 54D may be
9.3.3.1 For pyknometers made of soda-lime used. These tables do not include any correc-
glass, the coefficient of cubical expansion may tion for the expansion of glass but must be
be assumed to be 25 x 10e6 per 1°C. entered with a density at the appropriate
reference temperature. Consequently the use
9.3.4 API-ASTM-IP Petroleum Measurement of these tables requires a tedious repetitive
Tables ( ASTM D 1250 IP and IP 250 ) calculation. This procedure is not therefore
recommended and is not covered in 9.4
9.3.4.1 The following tables referred to in API- and 9.5.
ASTM-IP Petroleum Measurement Tables are
relevant only for determinations of petroleum 9.4 Calculation of Density
and petroleum products. The tables must not
be used for non-petroleum products for which 9.4.1 Density at any Temperature tt
it must always be ensured that tt = I* ps is
required. 9.4.1.1 When tt = rc,

IP 200 Table 53 Correction

to Density at 15°C.
IP 250 Table A
of Observed Density

Correction of Observed
pt =

9.4.1.2
c ( mt -
(MC--mo)

When tt -: tc.
m. 1
1000 I
+c

Density to Density at 20°C.

IP 200 Table 54 Correction of Observed Volume
to Volume at a reference temperature
of 15°C.
lJt =c ( mc-m.
( mt - m0 ) pc
) 1000 [ l-al-t-)]

where a1 = a1 or aa as appropriate
1 +’
to the
IP 250 Table B Correction of Observed Volume pyknometer used.
to Volume at a reference temperature
of 20°C.
9.4.2 Density at Reference Temperature, ta
9.3.4.2 Enter Tables 53 A, 53B, 53D or Table A
( according to the type of sample under test ) 9.4.2.1 When tt = tc = ts,
with densities determined in glass apparatus
calibrated at 15” or 20°C as appropriate. (mt - m0 1 pc
Ps = Pt -
( mc - m. ) 1000 +’
The tables include a correction for the expan-
sion of the glass apparatus used (assumed to be
soda-lime glass ) for which the conventional 9.4.2.2 When tt = tc # ts ( ts = 15” or 20°C )
value of 23 x 10-e per 1°C applies. The density determined at the test temperature
tt as in 9.4.1.1 is the true density at tt in soda-
9.3.4.3 When entering Tables 53A, 53B, 53D or lime glass apparatus calibrated at ts before
Table A with the results of determinations made entering Tables 53A, 53B, 53D .or Table A as
with pyknometers constructed from borosilicate appropriate. This always applies irrespective
glass, a correction will be required for the of the glass from which the pyknometer is
difference between the coefficient of cubical made, i.e. enter Tables 53A, 53B, 53D or
expansion of the borosilicate glass and the
Table A with Ptl and against tt extract pr5 or pa,,
conventional value for soda-lime glass incor-
respectively, interpolating as necessary, where
porated in the tables.
9.3.4.4 When the pyknometer used is made of ( mt - m. ) PC
ptl = +c ] [l+% ( ts--tt)]
soda-lime glass no correction is necessary when [ ( m,--m, ) 1000
 IS 1448 [ P : 32 ] : 1992

9.4.2.3 When ic = ts # tt ( t8 = 15” or 20°C ) 10 PRECISION

a) Pyknometer made of soda-lime glass - 10.1 The following criteria should be used for
Tables 53A, 53B, 53D or Table A may be judging the acceptability of results ( 95 percent
entered directly with ptl and against tt the confidence ).
corresponding plo or pzO is extracted,
interpolating as necessary, where 10.1.1 Repeatability

( mt - m. 1 pc Duplicate results by the same operator should

ptl = be considered suspect if they differ by more
( mc-mm,) 1000 +’
than the following amounts:
b) Pyknometer made of borosilicate glass -
Range, g/ml Repeatability
Tables 53A, 53B, 53D or Table A must be
entered with ptl adjusted for the differen- 0.777 0 to O-892 0 0~000 7
tial expansion of the pyknometer glass
and against tt the corresponding pls or
p.. is extracted 10.1.2 Reproducibility
The results obtained by each of two laborato-
( mt - m, 1 pc
ptl =
C (m,-mm,)1000 + C
I
[I+(%--cc1)
( ts - tt ) ]
ries should not be considered suspect unless
they differ by more than the following
amounts:
Second-order terms, which are not significant, Range, g/ml Reproducibility
are ignored.
0.777 0 to 0.892 0 0~001 0
9.4.2.4 When tt f tc # ts
The above values were obtained when using
The density determined at the test temperature 5 ml pyknometers. The use of larger ( e.g.
tt as in 9.4.1.2 is the true density at tt. The 10 ml ) pyknometers should give equal or better
result obtained must, therefore, be adjusted to accuracy.
give the apparent density at tt in soda-lime
glass apparatus calibrated at tB before entering The method is not restricted to samples having
Tables 53A, 53B, 53D or Table A as appropriate. densities within the range O-777-0.892 g/ml
This always applies, irrespective of the glass but precision figures are not available for values
from which the pyknometer is made, i.e. enter outside this range.
Tables 53A, 53B, 53D or Table A with ptl and
against tt extract p15or peaas appropriate, inter- 11 METHOD C ( CAPILLARY-STOPPERED
polating as necessary. The expression for ptl may PYKNOMETER METHOD )
be rearranged as follows, ignoring second-order
11.1 General
terms which are not significant.
11.1.1 This method covers the determination
a) Pyknometers made of soda-lime glass - of the density or relative density of crude
ptl =

I:mtt--m.
(
( mc-m0
1 pc
) 1000
+c 3
[ l+a* (h--tc)l
petroleum and of petroleum products handled
as liquids or solids. The method may also be
used for coal tar products, including road tars,
creosote and tar pitches, or for mixtures of

ct
b) Pyknometers made of borosilicate glass -
these with petroleum products.
m--m, ) pc
Ptl = ( mc_m, ) 1

3
ooo+ C [ l+&+adt
( &,+a8 1 tc1
- 11.1.2 The method is not suitable for the
determination of the density or relative density
of highly volatile liquids having Reid vapour
pressure greater than 0.5 bar (5x 10’ Pa ) or
9.4.2.5 When ts = tt # tc having initial boiling points below 40°C.
Use the expression in 9.4.1.2.
11.2 Summary of Method
9.4.3 Rounding-08 of Calculations and Reporting
11.2.1 The weights of equal volumes of the
Carry out all calculations to five figures and sample and of water are compared. Equal
report the final result to the nearest 0.000 1 as volumes are ensured by placing the filled
density giving the units of mass and volume pyknometer in a bath at the test temperature
and the temperature. until equilibrium is reached.

9
IS 1448 1 P : 32 1: 1992

12 APPARATUS 12.2 Constant-temperatore Bath - a water bath

having a depth greater than that of the pykno-
12.1 Pyknometer - One of the four types shown meter, capable of being maintained within
in Fig. 4 and 5 ( see 15.1 and 16.1 ), construc- fO.OZX ( O.l°F ) of the desired temperature.
ted of borosilicate glass or soda-lime glass and
annealed after manufacture. 12.3 Bath Thermometer - See 3.4.1.1. Other
The ‘warden’ form [ Fig. 4 ( b ) ] is determined total immersion thermometers of suitable range
for all except viscous or solid products and and equal or greater accuracy may also be
should always be used for volatile products. used.
The ground-glass cap, or ‘warden’, almost
eliminates expansion and evaporation losses 12.4 Pyknometer Holder ( Optional ) - to hold
and this form of pyknometer may be used when pyknometer vertically and at the correct depth
the test temperature is lower than that of the in the constant-temperature bath, a metal
laboratory. holder is desirable. It may be constructed of
any suitable metal which will not corrode in
The conical ( Fig. 5 ) is recommended for waxy the water bath.
oils and semi-solids.
12.5 Balance - capable of weighing to the
The form of pyknometer shown in Fig. 4 ( a ) nearest O-1 mg.
is suitable for non-volatile liquids except those
of high viscosity. 13 PREPARATION OF APPARATUS
The wide-mouth ( Hubbard ) form of pykno-
meter [ Fig. 4 ( c ) ] is used for very viscous 13.1 Thoroughly clean the pyknometer and
liquids and solids. stopper with a surfactant cleaning fluid, rinse
well with distilled water, then with acetone and
As the forms of pyknometer shown in Fig. 4 dry. Ensure that all traces of moisture are
(a)and(c)h ave no ‘warden’ or expansion removed by drying with a current of filtered air
chamber, they cannot be used when the tempe- passing slowly through the pyknometer and
rature of the test is so far below that of the stopper capillary. Wipe the outside of the
laboratory as to cause loss of sample by expan- pyknometer and stopper with a clean, lint-free
sion through the capillary. cloth.

4A CAPILLARY-STOPPER 48 WARDEN 4C WIDE MOUTH HUBBARD

FIG. 4 PYKNOMETER FORMS

10
 IS 1448 [ P : 32 ] : 1992

IQ 0 s APPROI

FIG. 5
ui
z

CONICAL CAPILLARY-STOPPER
WElour Of 6oRoslucA~
Ouss
COWLEE
PIKNOYETER
EXCEPT FOR
RESERVOIR CAP SHOULD
PREFERIILY
1tlAN 660

PYKNOMBTBR
BE US

NOTE - If sufficient cleaning fluids do not give distilled water, cooled to slightly below 15C,
adequate cleaning, chromic acid cleaning solution and firmly’ insert the stopper, taking care to
may be used.
avoid the inclusion of any air bubbles. Immerse
CAUTION - Chromic acid is potentially the pyknometer to the neck in the constant-
hazardous in contact with organic materials temperature bath. When using the conical form
and is toxic and highly corrosive. If used, of pyknometer, place the reservior cap in the
wear approved full face-shield and full-length constant-temperature bath. Maintain the bath
protective clothing including gloves. within f 0*05X! ( f 0~1°F ) of the calibration
temperature for not less than one hour.
Cleaning should be carried out in this manner
whenever the pyknomtter is to be calibrated or 14.3 With the pyknometer and its contents at
whenever liquid fails to drain cleanly from the this temperature wipe the top of the stopper
internal walls of the pyknometer or the capil- so that it is dry and the meniscus of the water
lary of the stopper. Normally the pyknometer in the capillary is flush with the top of the
may be cleaned between determinations by stopper. Care is necessary during this opera-
washing with a suitable light petroleum solvent, tion, since capillary action of the cloth can
followed by vacuum drying. draw liquid out of the stopper. Place the
warden firmly on the stopper ( if the pykno-
14 CALIBRATION OF PYKNOMETER meter is of this type ). When using the conical
14.1 After drying allow the pyknometer to form, raise the pyknometer in the water bath
reach room temperature. Dissipate any static until the smaller cone is clear of the water.
charge which may have formed on it and then Remove the reservoir cap and wipe the cone
weigh, complete with warden if of form 4 ( b ) so that it is dry and the meniscus of the water
or form 5, to the nearest O-1 mg. in the capillary is flush with the top of the
stopper, then place the warden firmly on the
NOTE - If the balance is not fitted with a static stopper.
eliminator, static charges may be dissipated by
breathing on the pyknometer. In such cases ensure 14.4 Remove the pyknometer from the bath.
that the pyknometer has regained constant mass Ifnot of the ‘warden’ form, cool the pykno-
before recording the weight.
meter and its contents to a temperature slightly
14.2 Fill the pyknometer with freshly-boiled below the temperature of the bath.

11
IS 1448 [ P : 32 ] : 1992

14.5 Dry the exterior surface of the pykno- NOTE - For mixtures containing non-petroleum
meter by wiping with a clean, lint-free cloth, products it is essential to ensure that the test
temnerature is the same as the final renortina
paying particular attention to the joint between temberature unless an appropriate value isoafcc;;t
the stopper and pyknometer, dissipate any able and the volumetric composition
static charge and weigh to the nearest O-1 mg. mixture is known, together with the volumetric
correction coefficients of the components in the
14.6 The difference between the weights of the mixture.
filled and empty pyknometer gives the mass of
When the temperature is constant, firmly insert
water contained by the pyknometer at the cali-
the dry capillary stopper, which has also been
bration temperature.
brought to the test temperature, taking care
14.7 If it is required to determine density at to avoid trapping air bubbles below the
a temperature other than 15% or to determine stopper.
relative density referred to water at a tempera- NOTE- It is essential to ensure that no air
ture other than ( 60°F ) 15*6”C, calibrate the bubbles are left trapped in the liquid and adequate
pyknometer at the required temperature. It is time must be allowed for air bubbles to rise to the
recommended that pyknometer be calibrated at surface before inserting the stopper.
the test temperature at which the densities are
to be determined, since this greatly simplifies Wipe excess liquid from the top of the stopper
the calculation of densities and relative den- so that the meniscus of the liquid in the
sities and eliminates any uncertainty as to the capillary is flush with the top of the stopper.
type of glass used in the construction of the Place the ‘warden’ over the stopper ( if the
pyknometer. pyknometer is of this type ).

14.8 Re-calibrate pyknometers at intervals as 15.4 Remove the pyknometer from the bath
dictated by experience. and, if not of the ‘warden’ type cool to a
temperature slightly below ft. Cool the pykno-
NOTE - It is recommended that new pyknometers meter and contents to room temperature if the
should be re-calibrated after one year and there- test temperature is high.
after at intervals dependent upon the magnitude
of any changes found. Soda-lime glass pykno-
meters may require calibration more frequently 15.5 Remqve all traces of sample and water
than borosilicate glass pyknometers. from the exterior surface of the pyknometer
by wiping with a clean, lint-free cloth, disperse
15 PROCEDURE FOR LIQUIDS any static charge and weigh to the precision
given in 15.2.
15.1 Choose an appropriate form and size
of pyknometer for the sample to be tested 16 PROCEDURE FOR SOLID OR
( see 12.1 ). The 75 ml and 50 ml sizes are SEMISOLID SAMPLES
normally the most suitable.
16.1 Weigh the clean, dry pyknometer which
15.2 Weigh the clean, dry pyknometer with should be of the wide-mouth type [ Fig 4 ( c ) ]
warden [ if of form 4 ( b ) or 5 ] and if neces- or the conical type ( Pig. 5 ) complete with
sary, disperse any static charge ( see Note warden to the nearest 0.5 mg.
given under 14.1 ), Pyknometers of 25 ml or
greater capacity should be weighed to the 16.2 Introduce a suitable amount of the sample
nearest 0.5 mg, and those of smaller capacity in the form of small pieces, which should
to the nearest 0.1 mg. be as regular in order to reduce the possibility
of trapping air bubbles. Alternatively, pour
15.3 Fill the pyknometer with the sample, if the molten sample in to the warmed pykno-
necessary warming both sample and pykno- meter, taking care to avoid the inclusion of
meter to assist filling and separation of air air bubbles. Fill the conical pyknometer up
bubbles. Bring the pyknometer and its con- to the 20 ml graduation mark. Allow the test
tents to the test temperature ( tt ) by immersing portion and pyknometer to cool slowly to
pyknometer up to its neck in the constant- ambient temperature. Check that no voids
temperature bath. Keep the pyknometer in have formed between the test portion suffi-
the bath for 20 minutes in order to stabilize ciently to remove the voids and again allow to
the temperature and to permit air bubbles to cool.
rise to the surface. If after this time the
liquid level is still changing, keep the pykno- 16.3 Bring the pyknometer and its contents
meter in the bath until the liquid level becomes to room temperature and weigh to the nearest
stable. 0.5 mg.

12
 IS 1448 [ P : 32 ] : 1992

16.4 In cases of sample having very high wax 17 CALCULATION AND REPORTING
contents it may be necessary to weigh the
cooled test portion and pyknometer before 17.1 Symbols - The following symbols are
overcoming the problem of voids. The weighed used in the calculations :
test portion and pyknometer are then reheated
until the voids disappear and allowed to cool. ts - any reference temperature, e. g. 15°C;
As soon as the melted test portion has set, tc - the temperature at which the pykno-
the surface should be covered with freshly meter is calibrated by water filling
boiled and cooled distilled water to prevent ( see 16.5 and 17.2 );
the ingress of air into any voids which may
form later at the bottom of the pyknometer. tt - the temperature at which the pykno-
meter is filled with liquid under test
( see 17.2.2 );
16.5 Fill the pyknometer with freshly-boiled,
cooled distilled water, removing all air bubbles. m. - the apparent mass in air ( weight. in
A fine wire may be used to facilitate the remo- air ) ( g ) of the empty pyknometer;
val of bubbles. Bring the pyknometer and its - the apparent mass in air ( g ) of the
contents to the test temperature, which must F;knometer filled with water at the calibra-
be the same as the calibration temperature of tion temperature tc;
the pyknometer, by immersing the pyknometer mt - the apparent mass in air ( g ) of the
up to its neck in the constant-temperature pyknometer filled with the liquid under test
bath. When using the conical form of pykno- at the temperature tt;
meter, place the reservoir cap on the capillary
stopper and firmly insert it, taking care to m, - the apparent mass in air ( g ) of the
avoid trapping air bubbles below the stopper, pyknometer plus solid or semi-solid
and immerse to half-way up the reservoir. cap ( see 16.3 );
in the constant-temperature bath. m2 - the apparent mass in air ( g ) of the
pyknometer plus solid or semi-solid plus
Keep the pyknometer in the bath for 20 water ( see 16.7 );
minutes in order to stabilize the temperature C - the correction of air buoyancy, in
and to permit bubbles to rise to the surface. g/ml ( see Table 4 );
If after this time the liquid level is still chang-
ing, keep the pyknometer in the bath until the PC- the density of water, in kg/ma, at the
liquid level becomes stable. temperature of calibration;
a1 - the coefficient of cubical expansion of
When the temperature is constant, firmly insert borosilicate glass ( see 17.3.2 );
the capillary stopper, which has also been aa - the coefficient of cubical expansion of
brought to the test temperature, taking care soda-lime glass ( see 17.3.3 );
to avoid trapping air bubbles below the ,~t- the density of the sample, in g/ml, at
stopper. When using the conical pyknometer it the test temperature tt;
is only necessary to raise the pyknometer until
the smaller cone is clear of the water and ps - the density of sample in g/ml, at any
remove the reservoir cap. Wipe excess water reference temperature ts;
from the top of the stopper so that the - the density of the sample, in g/ml, at
meniscus of the water in the capillary is flush Fe reference temperature of 15°C;
with the top of the stopper. Place the warden - the density of the sample, in g/ml, at
firmly on the stopper if the pyknometer is of ,“l?e reference temperature of 20°C;
the conical form.
ptl - the apparent density, in g/ml, at the
test temperature tt as determined in soda-
16.6 Remove the pyknometer from the bath lime glass apparatus calibrated at the refe-
and if the pyknometer is of the wide-mouth rence temperature t. = 15” or 2O”C, i. e.,
form, cool to a temperature slightly below the the observed density uncorrected for
tests/calibration temperature. Cool the pykno- glass expansion - required for entering the
meter and contents to room temperature if API-ASTM-IP Petroleum Measurement
the test temperature is above ambient. Tables.
16.7 Dry the exterior surface of the pykno- dt - the relevant density at the test tem-
meter by wiping with a clean, lint-free cloth, perature tt;
disperse any static charge and weigh to the $ - the relevant density at reference tem-
nearest O-5 mg. perature ts;

13
IS 1448 [ P : 32 ] : 1992

the relevant density at the reference source of the glass and to fall into three main
$gpLature of ( 60°F ) 15.6%; categories having coefficients of cubical expan-
sion of 10 x 10’6, 14 x 10-e and 19 x 10m8
dtl- the apparent relative density at the per 1°C respectively.
test temperature tt as determined in glass
apparatus calibrated at the reference tem- For determination of the highest accuracy
perature ts = ( 60°F ) 15*6”C, i. e. the when borosilicate pyknometers are used, there-
observed relative density uncorrected for fore, either
glass expansion required for entering the
API-ASTM-IP Petroleum Measurement
a) ensure that tt = tc or
Tables.
b) use a pyknometer for which the coeffi-
17.2 Reference, Calibration and Test Tempera- cient of cubical expansion is known.
tnres
When the foregoing is not possible and a lower
17.2.1 The pyknometer may be calibrated at
precision is acceptable, the use of 10 x 10’6
any convenient temperature and this may
per 1°C is recommended.
correspond with the reference or test tempera-
tures. The calculation of density is greatly
17.3.3 Pyknometers Made of Soda-Lime Glass
simplified when the pyknometer is calibrated
at the test temperature since only the cacula- 17.3.3.1 For pyknometers made of soda-lime
tions given in 17.4.1.1, 17.4.2.1 and 17.4.2.2 glass, the coefficient of cubical expansion
then apply. may be assumed to be 25 x 10”’ per 1°C.
17.2.2 For qualitative purposes, the test tem-
perature is usually chosen to correspond with 17.3.4 The API-ASTM-IP Petroleum Measure-
the required reference temperature, but for ment Tables ( API 2540 ! ASTM D 25OjIP 200
quantitative purposes involving the calculation and IP 250
of the mass or of the apparent mass in air of a
given quantity of oil, the density or relative 17.3.4.1 The following tables referred to in the
density should be determined within 3% of API-ASTM-IP Petroleum Measurement Tables
the temperature at which the oil is measured are relevant only for determinations non-
by the selected dynamic or static method. petroleum and petroleum products. The tables
However, in the case of very volatile products must not be used for non-petroleum products
having a Reid vapour pressure above 0.5 bar, for which it must always be ensured that tt =
the test should be carried out at a temperature ts when ps or d, is required:
of 15°C or below to minimize the loss of light
fractions. IP 200 Tables Correction of Observed
53A, 53B and P,eFity to Density at
53D 0
17.3 Correction for tbe Thermal Expansion of
the Pyknometer IP 250 Table A Correction of. Observed
Density to Density at
17.3.1 General
20°C
The calculation of density or of relative IP 200 Tables Correction of observed
density from measurements made at a tem- 23A, 23B and Relative Density (60”/6O”F)
perature tt which differs from the temperature 23D 15*6”/15*6”C to Relative
tc at which the pyknometer was calibrated, p5e;s-Ey ( 60”/60”F ) 15*6”/
involves a correction for cubical expansion or . 0
contraction of the glass from which the pykno- IP 200 Tables Correction of Observed
meter is made. 54A, 54B and Volume to Volume at a
54D reference temperature of
If the calculation is based on the density or
15°C
relative density correction tables given in the
API-ASTM-IP Petroleum Measurement Tables, IP 250 Table B Correction of Observed
a similar correction may also be required Volume to Volume at a
( see 17.3.4 ). reference temperature of
20°C
17.3.2 Pyknometers Made of Borosilicate Glass
IP 200 Tables Correction of Observed
17.3.2.1 The coefficient of cubical expansion of 24A, 24R and Volume to Volume at a
borosilicate glass are known to depend on the 24D reference temperature

14
 IS 1448 [ P : 32 ] : 1992

17.3.4.2 Tables 53A, 53B, A, 53D, 23A, 23B and 17.4.2 Density at Reference Temperature ts
23D are entered with densities or relative den-
sities determined in glass apparatus calibrated 17.4.2.1 When tt = tc = t8
at a temperature tc in “C ( Tables 53A, 53B
53D or A ) or “F ( Tables 23A, 23B or 23D ). a) for liquids
ps = Pt = ( mt - m. ) PC + c
The tables include a correction for the expan-
sion of the glass apparatus used ( assumed to
( me- m, ) 1 000
be soda-lime glass ) for which the conventional b) for solids or semi-solids
value of ( 25 f 2 ) x 10msper 1°C applies. ( ml -
ps = pt =
17.3.4.3 When entering Tables 53A, 53B, 53D, ( mc-mO- mlmp:p; 1000+ c
A, 23A, 23B, 23D with the results of determi-
nations made with pyknometers constructed 17.4.2.2 When tt = tc#ts = 15” or 20°C
from borosilicate glass, a correction will be The density determined at the test temperature
required for the difference between the coeffi- tt as in 17.4.1.1, is the true density at tr. The
cient of cubical expansion of the borosilicate result obtained must, therefore, be adjusted
glass and the conventional value for soda-lime to give the apparent density at tt in soda-lime
glass incorporated in the tables. glass apparatus calibrated at ts, before eate:;tt
Table 53 or Table A as appropriate. ’
17.3.4.4 When the pyknometer used is made always applies irrespective of the glass from
of soda-lime glass no correction is necessary which the pyknometer is made, i. e., enter
when using Tables 53A, 53B, 53D, A, 23A or Table 53 or Table A with ptl and against tt
23B, when t,=15”C, 20°C or ( 60°F ) 15.6”C as extract pr5 or pzOrespectively, interpolating as
appropriate to the table entered. necessary, where
If t, does not correspond to the reference a) for liquids
temperature tp for which the table used is
(mt -
~,‘,~oo+C]
constructed, an
expansion of the
ture range tc-+ts.
adjustment is required for the
pyknometer over the tempera-
ptl=
(m-1: o

b) for solids or semi-solids

[l+a2 (ts-tdl

cl
17.3.4.5 Alternatively, the corresponding (mt - m. ) PC
volume correction Tables 54A, 54B, 54D, 24A, Ptl = [ (m,-mo-mm,+m, ) 1000 +
24B or 24D may be used. These tables do not
include any correction for the expansion of [ 1 + a2 ( ts - tt > 1
glass, but must be entered with a density at
the appropriate reference temperature. Con- 17.4.2.3 When t, = t, # tt ( tg = 15” or 20°C)
sequently the use of these tables requires a
tedious repetitive calculation. This procedure a) Pyknometer made of soda-lime glass -
is not, therefore, recommended and is not Tables 53A, 53B, 53D or A may be
covered in 17.4 and 17.5. entered directly with pi1 and against tt
the corresponding pIs or pa,,is extracted,
17.4 Calculation of Density interpolating as necessary, where
(mt - mO)pc
17.4.1 Density at any Temperature tc Pt’ =
(m, - m, ) 1000 +’
17.4.1.1 When tt = tc
b) Pyknometers made of borosilicate glass -
a) for liquids Tables 53A, 53B, 53D or Table A must
ml-mo)pc be entered with ptr adjusted for the
pt =
(ril
c-m,) 1000
I c
differential expansion of the pyknometer
glass, and against tt the corresponding
b) for solids or semi-solids pls or pea is extracted, interpolating as
(m,-mo)pc necessary, where
) 1000 +C
Pt = ( mc-mm,-m,+ml
Ptl = (m-
trnt 0
+ c]
,m;;;oo
17.4.1.2 When tt f tc [
( mt--m, 1 PC [ 1 + ( aa - al ) ( 63 - tt ) 1
pt =
lOOO[ l-a’(
( m,-mm,) tc--t)l +C
where a1 = a I or a3 as appropriate to the Second-order terms, which are not again
pyknometer used. significant, are ignored.

15
IS 1448 [ P : 32 ] : 1992

17.4.2.4 When tt # to # te 17.5.3 Carry out all calcu!ations to five decimal

places and report the final results to the near-
The density determined at the test temperature est O*OOO 1 as Relative Density giving test and
tt as in 17.4.1.2 is the true density at tt. The reference temperatures.
result obtained must, therefore, be adjusted to
give the apparent density at tt in soda-lime NOTE - Since the densities in Table 3 are given in
kg/m*, it is essential that these values be divided by
glass apparatus calibrated at ts before entering 1 000 to convert them to g/ml ( kg/l ).
Tables 53A, 53B, 53D, or Table A as appropri-
ate. This always applies, irrespective of the 18 PRECISION
glass from which the pyknometer is made, i. e.
enter Tables 53A, 53B, 53D, or Table A with ptr 18.1 With samples which are neither very vola-
and against tt extract pi5 or ps,, respectively, tile nor very viscous, and using a pyknometer
interpolating as appropriate. The expression of at least 25 ml capacity, results of duplicate
for ptl may be rearranged as follows, ignoring test should not differ by more than the follow-
second-order terms which are not significant: ing amounts:

a) Pyknometers made of soda-lime glass Repeatability Reproducibility

Density 0.000 6 g/ml 0.000 6 g/ml
pt’ =
C ( mt -
(m, -m,)
m0 1 PC
1000
+ c
1 Relative density O*OOO 6 g/ml O-000 6 g/ml

These values are based on estimates of normal

[l+ct, (&-&)I good practice and are not derived by statistical
analysis.

c -
b) Pynometers made of borosilicate glass For volatile or very viscous sampIes and for

1
(mt m. ) pc solids no specific figures for precision can be
ptl = +C given.
( m,^L m, ) 1000

19 METHOD D ( DENSITY OR RELATIVE

11 + a1 t8 + a8 tt - ( a1 + aI ) tc ]
DENSITY OF SOLIDS - DISPLACEMENT
METHOD
17.4.2.5 When tB = it # tc
19.1 Outline of the Method
Use the expression in 17.4.1.2.
When a solid is weighed first in air and then in
water, the difference between the two weigh-
17.4.3 Rounding-ofl of Calculations and Reporting
ings is equal to the weight of water displaced.
Carry out all calculations to five decimal places The rel. d t/t of the solid may, therefore, be
and report the final result to the nearest 0.000 1 calulated, where t is the temperature of the
as Density, giving the units of mass and volume water. If the solid has a relative density greater
and the temperature. than unity a piece of it may be weighed directly
in the water. If the relative density is less than
17.5 Calculation of Relative Density unity the solid must be made to sink in the
water in some suitable way, for example, by
securing it to a metal crucible.
17.5.1 In accordance with the definition, the
appropriate values for dt, dtl and d, can be The method may be used for the determination
derived by dividing the corresponding values of the relative density of bitumen and similar
for density in 17.4.1 and 17.4.2 by the density products which are sufficiently solid to be hand-
of water in the same units at the required refer- led in pieces. The pyknometer method is,
ence temperature ( see Note under 17.5.3 ). however, more precise.
20 APPARATUS
17.5.2 When the correction of relative density
t/( 60°F ) 15.6% of petroleum and petroleum 20.1 Thermometer - See 3.4.1.1.
products is required to the reference tempera- 20.2 Balance Straddle - a pan straddle of con-
ture of ( 60°F ) 15.6”C ( see 17.4.2.2, 17.4.2.3 venient size to support a beaker and permit
and 17.4.2.4 ), use Tables 23A, 23B or 23D or determination of the weight of the specimen
IP 200 ts, tt and lc wilI be in “F and the coeffi- in water.
cient of cubical expansion a, and a2 shouId
be stated per 1°F for a, the value of 14 x 10’6 20.3 Waxed Thread - a length of fine, waxed
per 1°F may be taken. silk thread.

16
 IS 1448 [ P : 32 ] : 1992

20.4 Nickel Crucible - in a modification of the temperature so that the crucible and wire sus-
method a thin nickel crucible of 5-25 ml pension are completely immersed; remove
capacity may be used. It should be provided any air bubbles adhering to the crucible and
with a three-wire suspension which permits the determine the weight in water.
complete immersion of wire and crucible when
determining the weight in water. 23.3 Dry the crucible and pour in some of the
molten sample, taking care to avoid inclusion
21 PROCEDURE FOR SOLIDS OF RELATIVE of air bubbles, after which allow the crucible
DENSITY GREATER THAN UNITY and contents to cool, preferably under vacuum
to room temperature. Determine the weight
21.1 Suspend a piece of the material, as in air.
smooth as possible, free from cracks and dust,
and weighing at least 5 g, from the hook on 23.4 Place the crucible and content in a beaker
one side of a balance, using a suitable length of of freshly boiled distilled water maintained at
waxed silk thread so that the bottom of the the desired temperature and leave until the
specimen is about 25.4 m ( 1 in ) above the crucible and contents attain that temperature.
straddle. Tare the thread previously by a
length of thread on the other pan. Weigh the 23.5 Place the beaker containing distilled water
sample to the nearest mg. Place the sample in on the pan straddle and suspend the crucible
a beaker of freshly boiled distilled water main- from the hook on one side of the balance.
tained at the desired temperature, e. g. 15’C, Remove with a fine wire any air bubbIes adher-
and allow to remain for sufficient time to ensure ing to the crucible or sample, and determine
that the sample has attained that temperature. the weight in water of the crucible and
Then place the beaker containing distilled contents.
water on the pan straddle and suspend the 24 CALCULATION AND REPORTING
sample from the hook on one side of the
balance. Remove with a fine wire any adher- 24.1 Let W, = weight of crucible in air;
ing air bubbles and determine the weight of the WC, = weight of crucible in water
sample in water. at t;
NOTE - The main source of error is air bubbles Wf = weight of crucible + sample
either occluded in the sample or adhering to its in air;
outer surface during weighing in water. Errors Wfw = weight of crucible + sample
caused by weighing qr by temperature variation are in water at t;
usually small in comparison.
then Wf - W, = weight of sample in air;
22 CALCULATION AND REPORTING
and ( Wr - W,, ) - ( Wf, - W,, )
22.1 If a is the weight of the specimen in air, = loss in weight of sample when
and b is the weight of the specimen in water at weighed in water at t.
t, then therefore,
a
relative dt/t in air = ~ relative density dt”C/t”C in air
U- b
Wf - WC
22.2 Report the value so obtained, to the
= ( wf- WC ) - ( Wrw - WC,
nearest O*OOl,as Relative Density dt/t, Method
D. The buoyancy correction in this case is 24.2 Report the result as Relative Density,
negligible. Method D. The buoyancy correction in this
22.3 To obtain density multiply the rel d t/t case is negligible.
by the density of water at t, obtained from 24.3 To obtain density multiply the relative
Table 3. density dt/t by the density of water at t, obta-
ined from Table 3.
23 PROCEDURE FOR SOLIDS OF
RELATIVE DENSITY LESS THAN UNITY 25 PRECISION
In using the crucible method: Results of duplicate tests should not differ by
more than the following amounts:
23.1 Suspend the crucible from the hook on
one side of the balance by means of a tared Size of Sample Repeatability Reproducibility
length of waxed thread, and determine its
weight to the nearest mg. 5 g or larger 0.004 0.008
Less than 5 g No specific permissible varia-
23.2 Suspend the crucible in a beaker contain- tions can be given
ing freshly boiled distilled water at the desired ._-. __ .._._._._ ~~__._~~~~._~. ~~~--------

17
IS 1448 [ P : 32 J : 1992

Table 3 Density of Water in kg/ms Against “C of the International Practical Scale of Temperature ( 1968 )
( czause 9.1 )

Minus
ta*OC o-o 0.1 o-2 o-3 04 0.5 0.6 0.7 0.8 o-9 F/P; Air-Free

0 999.839 6 999.846 3 999.852 8 999.859 l 999.865 3 999.871 3 999.877 1 999.882 7 999.888 2 999.893 4 om5 9 -0.002 6
1 999.898 5 999.903 5 999.908 2 999.912 8 999.917 2 999.921 4 999.925 4 999.929 3 999.933 0 999.936 5 o+m4 1 -0*002 7
2 999.939 9 999.943 1 999.946 1 999948 9 999.951 6 999.954 1 999.956 5 999.958 7 999.960 7 999.962 5 0*002 4 -0*002 8
3 999.964 2 999.965 7 999.967 0 999.968 2 999.969 2 999.970 1 999.970 a 999.971 3 999.971 7 999.971 9 O@OOa -0*003 0
4 999.972 0 999.971 8 999.971 6 999.971 1 999.970 5 999.969 8 999.968 9 999.967 8 999.966 6 999.965 2 -o*OOO a -0dIO3 1
5 999.963 7 999.962 0 999.960 2 999.958 2 999.956 0 999.953 7 999.951 3 999.948 7 999.945 9 999.943 0 -0.002 4 -0*003 3
6 999.939 9 999.936 7 999.933 4 999.929 9 999.926 2 999.922 4 999‘918 4 999.914 3 999.910 1 999.905 7 -0m3 9 -0+03 4
7 999.901 1 999.896 4 999.891 6 999.886 6 999.881 5 999.876 2 999.870 8 999.865 2 999.859 5 999.853 7 --0+05 3 -0m3 5
8 999.847 7 999&tl 6 999.835 3 999.828 9 999.822 3 999.815 7 999.808 8 999.801 9 999.794 7 999.787 5 -00068 -0w3 5
9 999,780 1 999.772 6 999.764 9 999.757 1 999.749 2 999.741 1 999.732 9 999.724 6 999.716 1 999.707 5 -0QOa 1 -0*003 4
10 999.698 7 999.689 8 999.680 8 999.671 7 999.662 4 999.653 0 999643 4 999.633 7 999.623 9 999.614 0 -0GO9 5 -MO3 3
11 999.603 9 999.593 7 999.583 4 999.512 9 999,562 3 999.551 6 999.540 a 999.529 a 999.518 7 999.507 4 -0.010 8 -0+03 1
12 999.496 1 999.484 6 999.473 0 999.461 2 999.4494 999.437 4 999.425 3 999.413 0 999400 7 999.388 2 -0*012 1 -0.002 9
13 999.575 6 999.362 8 999.350 0 999.337 0 999.323 9 999.310 6 999.297 3 999.283 8 999.270 2 999.256 5 -0*013 3 -0~002 6
14 999.242 7 999.228 7 999,214 6 999.200 4 999.186 J 999.171 7 999.157 I 999.1424 999.127 6 999.112 7 -0.014 5 -0~~02 3
15 999.097 7 999.082 6 999.067 3 999.051 9 990.036 4. 999.020 8 999.005 1 998.989 2 998.973 3 998.957 2 -0.015 7 -0*002 0
16 998.941 0 998.924 7 998908 3 998.891 7 998.875 l 998.858 3 998.841 4 998.824 4 998.807 3 998.790 1 -0.016 8 -0‘001 7
17 998.772 a 998.755 3 998.737 8 998.720 1 998.702 3 998.684 5 998.666 5 998.648 3 998.630 1 998.611 8 -0.017 9 -0~0014
18 998.593 4 998.574 a 998.556 2 998.537 4 998.518 5 998.499 5 998.4804 998.461 2 998441 9 998.422 5 -0.019 0 -0~001 1
19 998403 0 998.383 3 998.363 6 998.343 8 998.323 3 998.303 7 998.283 6 998.263 3 998.242 9 998.222 4 -0.020 1 -o.ooo 9

20 998.201 9 998.181 2 998.160 4 998.139 5 998.118 5 998.097 3 998.076 1 998.054 8 998.033 4 998.011 9 -0.021 2 -0.000 6
21 997+90 2 997.968 5 997.946 7 997.924 7 997.902 7 997.880 5 997.858 3 997.836 0 997.813 5 997.791 0 -0.022 2 -0.000 4
22 997.768 3 997.745 6 997.722 7 997.699 8 997.676 7 997.653 6 997.630 3 997.607 0 997.583 5 997.560 0 -0.023 2 -0.000 2
23 997.536 3 997.512 6 997.488 7 997.464 a 997440 a 997.416 6 997.392 4 997.368 0 997.343 6 997.319 1 -0.024 2 -0.000 1
24 997.294 4 997.269 7 997.244 9 997.220 0 997.195 0 997.169 9 997.144 6 997.119 3 997.093 9 997.068 5 -0.025 2 wO.000 0
25 997.042 9 997.017 2 996.991 4 996.965 5 996.939 6 996.913 5 996.887 3 996.861 1 996.834 7 996.808 3 -0.026 1 -0.0000
26 996.781 8 996.755 1 996.728 4 996.701 6 9%.674 7 996.647 7 996.620 6 996.593 4 996.566 1 996.538 8 -0.027 0 -0.000 0
27 996.511 3 996.483 7 996.456 1 996.428 4 996400 5 996.372 6 9%.344 6 996.316 5 996.288 3 996.260 0 -0.028 0 -0.0000
28 996.231 6 996.203 2 996.174 6 996.146 0 996.117 2 996 088 4 996,059 5 996 030 5 996.001 4 995.972 2 -0.028 9 -_o~~ 0
29 995943 0 995.913 6 995.884 2 995.854 6 995.825 0 995.795 3 995.765 5 995.735 6 995.705 6 995.675 6 -0 029 a -0.000 0

30 995.645 4 995.615 2 995.584 8 995 554 4 995.523 9 995.493 4 995.462 7 995.431 9 995.401 1 995.370 1 -0.030 6 0400 0
31 995.339 1 995.308 0 995.276 8 995.245 6 995.214 2 995.182 8 995.151 2 995.119 6 995.087 9 995.056 1 -0.031 5 0900 0
32 995.024 3 994.992 3 994.960 3 99fl.928 2 994.896 0 994.863 7 994.831 3 994.798 3 994.766 3 994,733 7 -0.032 3 oxQoo
33 994.701 0 994.668 2 994.635 3 994.602 1 994.569 3 994.536 2 994.503 0 994.469 7 994.436 4 994402 9 -0.033 2 oaocl 0
34 994.369 4 994.335 8 994.302 1 994.268 3 994.234 5 994.200 5 994.166 5 994.132 4 994.098 2 994.064 0 -0.0340 0300 0
35 994.029 6 993.995 2 993.960 7 993.926 1 993.891 5 993.856 7 990.821 9 993.787 0 993.752 l 993.717 0 -0.034 8 oaoo0
36 993.681 9 993.646 7 993.611 4 993 576 0 993.540 6 993.505 0 993.469 4 993.433 8 993.398 0 993.362 2 -0.035 6 0300 0
37 993.326 3 993.290 3 993.254 2 993.218 1 993.181 8 993.145 5 993.109 2 993.072 7 993.036 2 993.999 6 -0.036 3 omo 0
38 992.962 9 992.926 1 992.889 a 992.852 4 992.815 4 992.778 4 992.741 2 992.704 0 992.666 8 992.629 4 -0.037 1 omo 0
39 992.592 0 992,554 5 992.516 9 992.479 2 992441 5 992.403 7 992.365 8 992.327 9 992.289 9 992.251 8 -0.037 8 0Goo 0

40 992.213 6

18
 IS1448(P:32]:1992

Table 4 Buoyancy Corrections*

( CZause17.1 )

mi- m, Correction, m-m Correction, m-m Correction,

M fdmf M g/ml M g/ml

0.60 O@OO48 0.80 oaOO 24 la0 0*000 00

0.61 OaOO47 0.81 OGOO23 1.01 - 0.000 01
0.62 OGIO 46 0.82 0*000 22 1.02 - o*OOO 02
0.63 o*OOO 44 0.83 0.000 20 1.03 - o*OOO 04
0.64 00IO 43 0.84 0.000 19 1.04 - o@OO05
0.65 OWO 42 0.85 0.000 18 1.05 -0@0006
066 o*OOO 41 0.86 0.000 17 1.06 -0~00007
0.67 OGJO40 0.87 O*OOO 16 1.07 - OWO 08
0.68 ONKI 38 0.88 0.000 14 1.08 - OGOO10
0.69 0.000 37 0.89 o*oOO13 1.09 - 0.000 11
0.70 O@OO36 0% 0.000 12 1.10 -0.00012
0.71 0xrOO35 0.91 ONIO II 1.11 - OGMI13
0.72 o+OO 34 0.92 OWO 10 1.12 - OGOO14
0.73 OGOO32 0.93 o*OOO 08 1.13 - 0.000 16
0.74 o*OOO 31 0.94 o@OO07 1.14 - 0*000 17
0.75 ox@0 30 0.95 0.000 06 1.15 - oGOO18
0.76 o@OO 29 0.96 o@OO05 1.16 - o*OOO 19
0.77 0.000 28 0.97 o*OOO 04 1.17 - 0*000 20
0.78 0.000 26 0.98 0.000 02 1.18 - 0*000 22
0.79 OX)0025 0.99 OXKKI 01 1.19 - OGOO23

*Calculated for standard air of density OGOl 222 g/ml at 15~56OCi 60°F ) and at a pressure of 1 : 013 bar
( 760 mm mercury ).
These corrections are applicable for air density values between OGOl 1 and OGOl 3 g/ml,
NOTE - M = Weight in air water contained by the pyknometer at temperature t.

19
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