MISCELLANEOUS TECHNIQUES AND IMPURITIES

MT 3 SPECIFIC GRAVITY, DENSITY, AND WEIGHT PER MILLILITRE

DEFINITIONS

Density (d). The density of a solid or liquid substance is defined as the mass of
the substance occupying unit volume at a stated temperature. When reporting the
density of a solid or liquid the units of mass and volume used must all be
explicitly stated, e.g., grams per millilitre at t °C. Unless otherwise stated,
density shall refer to mass (in grams) per millilitre at 20 °C.
t
Specific gravity (sp. gr.) 1 of solid, and liquid, is defined as the ratio of the mass
t2
of a given volume of substance at a temperature t1 to the mass of an equal
volume of pure water at a temperature t2. When reporting the specific gravity of
a solid or liquid the t1 and t2 must both be explicitly stated. Unless otherwise
stated t1 and t2 are both 20 °C.

3.1 Hydrometer method (Note 1)

OUTLINE OF METHOD

The sample is brought to the prescribed temperature and transferred to a

hydrometer cylinder at approximately the same temperature. The appropriate
hydrometer is lowered into the sample and allowed to settle. The hydrometer is
read and the temperature of the sample noted. If required, the cylinder and its
contents are placed in a constant temperature bath to avoid excessive
temperature variation during the test.

APPARATUS

Hydrometer graduated in g/ml at 20 °C. BS 718: 1979 Series L20 (± 0.0002) or

L50 (± 0.0005) or equivalent.
Constant temperature bath maintained at 20 °C
Cylinder BS 604 1000 ml, tall form or equivalent; internal diameter at least
25 mm greater than that of the hydrometer and height such that the
hydrometer floats freely in the sample with at least 25 mm clearance
between the bottom of the hydrometer and the bottom of the cylinder.
Thermometer range 0 to 100 °C; graduated in 0.2C.

PROCEDURE
Clean all apparatus before use. Allow the liquid to attain thermal equilibrium
with its surroundings and pour it into the cylinder. Avoid the formation of air
bubbles in the liquid by pouring it down the side of the vessel. Stir the liquid

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vertically with a loop stirrer, again avoiding the formation of bubbles. Measure
the temperature of the liquid to the nearest 0.2 °C.
Insert the hydrometer carefully into the liquid, holding it by the top of its stem.
Release the hydrometer when it is approximately in its position of equilibrium.
A little experience soon enables the user to appreciate when the hydrometer is
approaching equilibrium and to release it in such a position that the hydrometer
rises or falls by only a small amount when released. This is important with
viscous liquids for otherwise excess liquid will adhere to the stem and the
hydrometer will thereby be weighted down.
When the hydrometer is steady, press the top of the stem downwards a few
millimetres beyond the position of equilibrium or, if the liquid is viscous, only
one scale division, gripping the stem very lightly with a finger and thumb.
Withdraw the hand and observe the meniscus as the hydrometer oscillates to
equilibrium. If the stem and liquid surface are clean the meniscus shape will
remain unchanged as the hydrometer rises and falls. If the meniscus shape
changes, e.g., if it wrinkles or is distorted by the motion of the hydrometer, lack
of cleanliness is indicated and the hydrometer and cylinder should be cleaned
and the test repeated with a fresh sample. This precaution becomes increasingly
important with increasing surface tension of the liquid.
When the hydrometer, which must not be touching the side of the cylinder, has
again settled down to its equilibrium position (this may take some time with
viscous liquids) record the reading as follows:

(i) Transparent liquids. Record the scale reading corresponding to the plane of
intersection of the horizontal liquid surface and the stem. When taking the
reading, view the scale through the liquid, adjusting the line of sight so that it is
in the plane of the liquid surface.

(ii) Opaque liquids. Record the scale reading where the meniscus merges into
the stem of the hydrometer.
Immediately after taking the reading, measure the temperature of the liquid to
the nearest 0.2 °C. The mean of this temperature and the initial temperature
should be used in the calculation of the corrections. (This procedure is
particularly important in the case of liquids having high values of coefficient of
thermal cubical expansion). The difference between the two temperatures should
not exceed 1 °C and if larger difference is found, lack of thermal equilibrium is
indicated and the test should be repeated.
If the hydrometer has been used in an opaque liquid it is necessary to correct the
reading for accurate results, since hydrometers are calibrated to be read at the
principal surface of the liquid (Note 2). For practical purposes this can be taken
as 0.0007 and 0.0014 for hydrometers L20 and L50 respectively.

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3.2 Pyknometer method

OUTLINE OF METHOD
In this method the weights of equal volumes or the material and water are
compared.

3.2.1 Capillary stoppered pyknometer

SCOPE
The method is suitable for the determination of the specific gravity or density of
liquids or solids. It is not suitable for these determinations on highly volatile liquids.

APPARATUS
Thermometer IP 39, BS 593: 1954 or equivalent
Constant temperature bath capable of being maintained within 0.05 °C (Note 3)
of the desired temperature
Capillary stopper gravity bottle available in three forms (Note 4)

(i) Capillary stopper gravity bottle BS 733: 1965 or equivalent; 10, 25, 50 and
100 ml sizes. It has no expansion chamber, so cannot be used accurately when
the temperature of the bath is lower than that of the laboratory (see Fig 5).

Figure 5 Capillary stopper specific gravity bottle

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Figure 6 Warden specific gravity bottle

(ii) "Warden" specific gravity bottle has a ground glass cap to eliminate expansion
and evaporation losses. It is available in 50 ml and 100 ml sizes and may be
used accurately at temperatures lower than that of the laboratory (see Fig 6).

(iii) Wide mouth, capillary stopper, specific gravity bottle BS 733: 1965 or
equivalent, suitable for viscous liquids and solids. It has no expansion
chamber so cannot be used accurately when the temperature of the bath is
below that of the laboratory (see Fig 7).

Figure 7 Wide mouth, specific gravity bottle

PROCEDURE

(i) Calibration of apparatus (Note 5). Clean the bottle and stopper (Note 6) dry,
and place side by side on the pan of a balance capable of weighing to an
accuracy of 0.1 mg. Clean and dry the counterpoise bottle and stopper, if used,
in a similar manner, and place on the other pan. If no counterpoise bottle is used,
immerse the density bottle up to its neck in the constant temperature bath,
withdraw, and wipe with the minimum of handling before placing on the
balance pan. This tends to establish the same surface conditions as will be
present for the second weighing.
Weigh the bottle (x g) after thermal equilibrium with the surroundings has been

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established and after any electrostatic charge caused by the drying has
disappeared. Fill the density bottle with pure water, which has been freshly boiled
and cooled to room temperature, and immerse to the top of its neck in a bath
maintained within ± 0.05 °C (Note 3) at a temperature slightly above room
temperature. Leave the bottle in the bath for at least 20 min. Insert the stopper,
which has been brought to the temperature of the bath, in the neck of the bottle,
taking care to avoid trapping air bubbles, and gently push home with a slight
twist. Remove the water on the neck of the bottle and the sides of the bottle with a
piece of dry filter paper. Finally dry the top of the stopper taking care not to
withdraw water from the capillary. Remove the bottle from the bath, determine
the temperature of the bath to 0.1 °C and record as the filling temperature.
Reweigh the bottle (y g). Plunge the counterpoise bottle into the bath as before,
and wipe both bottles free of adhering water before placing on their respective
balance pans. Carry out the second weighing after equilibrium conditions have
been reached.
Calculate the water equivalent (WE), i.e., (y - x) g or the capacity of the bottle
(v20), i.e. 1.0018 (y - x) ml at 20 °C.
If required, to correct for temperatures above 20 °C, add 0.003 ml/100 ml/1 °C
above 20 °C for soda glass and 0.001 ml/100 ml/1 °C for borosilicate bottles
(Note 5).

(ii) Procedure for liquids. Repeat the whole process with the liquid being
examined, taking care to avoid air bubbles when filling.
y' − x
Specific gravity 20 °C/20 °C =
WE
y' - x
Density in g/ml =
v20
where:

WE = water equivalent at 20 °C
v20 ml = Capacity of the bottle at 20 °C
y' g = weight of bottle + liquid being examined

If required add a buoyancy to the result (Note 7)

Specific gravity Correction

0.60 - 1.04 + 0.0011
1.05 - 1.75 + 0.0010
1.76 - 2.00 + 0.0009

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(iii) Procedure for solids - insoluble in water but wetted by water. Weigh the
clean, dry pyknometer, which should be of the wide mouth type to the nearest
0.1 mg (w g). Introduce a suitable amount (about 1.5 ml), of the sample in the
form of small pieces, which should be as regular as possible in order to reduce
the possibility of trapping air bubbles. Bring the pyknometer and its contents to
room temperature and reweigh (x g).
Fill the pyknometer to about half its capacity with freshly boiled and cooled
distilled water. Place the pyknometer in a vacuum desiccator, without desiccant,
and reduce the pressure. Keep it under vacuum until all air bubbles have
escaped. Complete the filling of the pyknometer with freshly boiled and cooled
distilled water.
Bring the pyknometer and its contents to the test temperature, 20 °C by
immersing the pyknometer up to its neck in the constant temperature bath.
Leave the pyknometer in the bath for 20 min in order to stabilize the temperature
and to permit bubbles to rise to the surface. If, after this time, the liquid level is
still changing, keep the pyknometer in the bath until the liquid level becomes
stable. When the temperature is constant insert the capillary stopper, which has
been previously brought to the test temperature, taking care to avoid trapping air
bubbles below the stopper. Wipe excess water from the top of the stopper so that
the meniscus of water in the capillary is flush with the top of the stopper.
Remove the pyknometer from the bath and cool to a temperature slightly below
20 °C.
Dry the exterior surface of the pyknometer by wiping with a clean, lint-free
cloth, disperse any static charge, and weigh again (y g).
x−w
Specific gravity 20 °C/20 °C = (Note 7)
WE − (y − x)

0.9982 (x - w )
Density (g/ml at 20 °C) =
WE − (y − x)
where:
WE = water equivalent at 20 °C
(iv) Procedure for solids - either soluble in water or not wetted by water. If the
sample is soluble in water or is not wetted by water, choose a non-volatile liquid
in which the sample is insoluble, and/or which wets the sample, and carry out
the determination as under (iii) above, replacing water by the chosen liquid.
S ( x − w)
Specific gravity of the solid 20 °C/20 °C =
S ⋅ WE − (y − x)
0.9982 S (x - w )
Density of solid in g/ml at 20 °C/20 °C =
S ⋅ WE − (y − x)

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where:
S = specific gravity of the liquid used, determined by method (ii) above
WE = Water equivalent as determined by method (i) above.

3.2.2 Bicapillary pyknometer method.

The method is recommended for the accurate determination of the specific
gravity or density of all except the more viscous liquids, and is particularly
useful when only small amounts of sample are available.

APPARATUS As for 3.2.1 above except that the following should be substituted
for the gravity bottle:
Graduated pyknometer. May be used in any size from 0.25 ml to 10 ml. It is self
filling. By placing the hooked tip in the sample whilst keeping the
pyknometer upright, the liquid is drawn up by capillary attraction, and the
pyknometer then fills by siphoning. It is suitable for dealing with volatile
liquids, and for use at temperatures below that of the laboratory (see Fig 8).

Figure 8 Graduated pyknometer

PROCEDURE
Repeat the procedure 3.2.1 above, except that sufficient water should be used to
obtain a suitable reading on the graduated arms. The difference between the
weights of the filled and empty pyknometer gives the water equivalent at the
temperature used corresponding to the sum of the scale reading.
By removing successive quantities of water, repeat the determination in order to
obtain a series of at least three readings covering the greater part of the scale,
together with the corresponding weights. Plot the sum of the readings on the two
arms as abscissae, against the corresponding weights as ordinates to obtain a
standardization curve giving the water equivalent of the pyknometer for any
combined scale reading. This graph should be a straight line.

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If it is desired to determine the specific gravity referred to water at some

temperature other than 20 °C, standardize at the desired temperature.
Re-standardize pyknometers at intervals as directed by experience.
Introduce sufficient sample to obtain readings any where on the graduated arms
but, when the sample is volatile, low scale readings should be aimed at in order
to minimize evaporation and expansion losses. Bring the pyknometer and
content to the test temperature as indicated by constancy of reading, take
readings on the two arms, remove the pyknometer from the bath, dry the exterior
surface as before, allow to come to equilibrium conditions and weigh.
From the standardization curve, read off the water equivalent corresponding to
the sum of the two pyknometer scale readings. Divide the difference between
the weights of the empty pyknometer and the pyknometer filled with the sample
by the water equivalent of the pyknometer to obtain the specific gravity in air of
the sample at 20 °C/20 °C (Note 7).

3.3 Density of suspension concentrates

3.3.1 Hydrometer method

OUTLINE OF METHOD
Direct determination of density by hydrometer, density bottle or liquid
displacement method has been shown to be unsuccessful because of aeration and
viscosity effects. The density at 20 °C of a 1 : 1 aqueous dilution can be readily
determined using a hydrometer and hence the actual density of the suspension
concentrate can be calculated.

APPARATUS

Hydrometer, to BS 718:1979, usual range 1.000 - 1.100 g/ml

PROCEDURE
Weigh (to the nearest 0.1 mg) 100 g of distilled water into a 250 ml beaker.
Carefully add, causing minimum aeration, an equal mass of the suspension
concentrate. Mix by slowly pouring the liquid into another beaker and repeat until
a homogeneous suspension is obtained. Transfer the 1 : 1 dilution to a 250 ml
cylinder and allow to stand for 10-15 minutes. Remove any remaining air
bubbles from the liquid surface using a pipette. The suspension should now be
homogeneous. Adjust the temperature to 20 ± 0.5 °C.

Gently place the hydrometer into the suspension and allow to sink under its own
weight. If the hydrometer is pushed below its natural level, the graduations on
the stem are obscured.

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Record the density after about 5 minutes when the equilibrium conditions
should be attained.
In extremes of ambient temperature it may be necessary to use a water bath to
maintain the suspension at 20 °C.

Calculation
a
Density of suspension concentrate = g/ml
2−a

Where
a is the density of the 50% m/m dilution and the density of water is taken to
be 1.0.

3.3.2 Density bottle method

OUTLINE OF METHOD

A portion of the sample is weighed into a density bottle and diluted with water
containing an anti-foam agent, using vacuum, if necessary to remove occluded
air. The volume of sample taken is then found by making up to capacity with the
anti-foam solution and weighing.

REAGENT
Anti-foam solution 1% m/v aqueous solution of a silicone anti-foaming agent.
A very dilute solution of "Silcolapse 5000" has been found to be satisfactory
at a dilution of 4 drops in 2.5 l of water.

PROCEDURE
Measure about 20 ml of well-mixed sample, previously adjusted to 20 ± 0.5 °C by
standing in a water bath, into a suitable 100 ml density bottle (Note 8), previously
weighed and calibrated with water at 20 °C, and weigh. Add about 20 ml of anti-
foam solution, previously brought to 20 ± 0.5 °C, and mix by swirling. Fill the
bottle to just below the mark with anti-foam solution, without mixing, and place
in a water bath held at 20 ± 0.5 °C for 10 minutes. Ensure that no air bubbles
remain (Note 9) then, without delay (to avoid temperature changes), adjust the
volume to the 100 ml mark with anti-foam solution. Dry the outside of the bottle
and weigh. To obtain the density of the anti-foam solution, determine the mass
of the density bottle filled with anti-foam solution at 20 ± 0.5 °C.

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mass of sample in g X−W

Then density at 20 ° C in g/ml = =
volume of sample in ml 100 − Y − X
D
Where:
W = mass of bottle only (g)
X = mass of bottle with sample (g)
Y = mass of bottle with sample and anti-foam solution to capacity (g)
Z = mass of bottle with anti-foam solution only to capacity (g)
Z −W
D = density at 20 °C of anti - foam solution in g/ml =
100

Note 1 This method is based on method BS 718:1979 or IP 160/64 but does

not include all the precautions necessary for precision determinations
since it has been adapted for use with methods of analysis for
pesticides. For more accurate determinations method BS 718 or IP 160
should be followed.
Note 2 See method BS 718 or IP 160 for methods and tables of correction to be
applied for more accurate determinations.
Note 3 Unless otherwise directed for routine work, ± 0.5 °C can be used.
Note 4 The 'Warden' form (Figure 6) is recommended for all except viscous or
solid products and should always be used for volatile products.
Note 5 It is recommended that new pyknometers should be re-calibrated after
one year, and thereafter at intervals depending upon the magnitude of
any changes found.
Note 6 Clean the pyknometer and stopper with chromic acid cleaning solution,
rinse well with distilled water, and dry. Ensure that all traces of water
are removed, using a current of filtered air if necessary. Cleaning
should be carried out in this manner whenever the pyknometer is to be
calibrated, or whenever the liquid fails to drain cleanly from the
internal walls of the pyknometer or the capillary of the stopper.
Normally the pyknometer may be cleaned between determinations by
washing with light petroleum spirit, followed by vacuum drying.
Note 7 Specific gravities (relative densities) as calculated in the text are
apparent values in air.
Hence
Apparent density = apparent SG × 0.99700 g × cm-3
True density = (apparent SG × 0.99700) + 0.0012 g × cm-3
true density
True specific gravity =
0.99820

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Note 8 A suitable density bottle consists of a 100 ml volumetric flask, with the
neck cut down to approximately 12 mm above the graduation mark.
Note 9 If bubbles persist, place the bottle in a vacuum desiccator, evacuate
cautiously, leave under vacuum for 5 min., then replace the bottle in the
20 °C water bath.

MT 5 MATERIAL SOLUBLE IN ACETONE

SCOPE

These methods are intended for materials which are freely soluble in acetone.

5.1 Hot solution

OUTLINE OF METHOD

The sample is refluxed with acetone, the acetone is evaporated, and the residue
is dried and weighed.

REAGENT

Acetone (CH3COCH3) anhydrous; RE 34

APPARATUS

Soxhlet extraction apparatus or straight through extractor

Round bottom flasks 250 ml with ground joint to fit the extractor; containing
2 glass beads and tared
Distillation set to fit the flask
Soxhlet thimble previously extracted with acetone then dried
Flameproof oven at 60 to 70 °C

PROCEDURE

Weigh (to the nearest mg) the specified amount (w g) of sample, transfer to the
thimble, and extract completely with acetone for about 4 h into the tared flask
(x g). Remove the flask from the extraction apparatus, distil off the acetone and
dry the flask and residue in the oven to constant weight at 60 to 70 °C. Cool and
reweigh (y g).
100 ( y − x )
Content of material soluble in acetone = % m/m
w

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5.2 Solution at room temperature

OUTLINE OF METHOD

The material is shaken with acetone, the insoluble material is filtered off, dried
and weighed.

REAGENT

Acetone (CH3COCH3) anhydrous; RE 34

APPARATUS

Conical flask 250 ml 29/32 neck with stopper

Sintered glass crucible porosity P16 (pore size 10-16 µm); tared
Oven 60 to 70 °C
Magnetic stirrer

PROCEDURE

Weigh (to the nearest mg) the specified amount (w g) of the dried material and
transfer to the flask.
Add acetone (100 ml at a temperature of 20 °C), stopper the flask and stir for 30 min
at 20 °C, then filter the solution through the tared crucible (x g).
Wash out the flask and the residue in the crucible with acetone (5 or 6 small
portions) and allow the crucible to dry under suction for 5 min. Finally dry in the
oven, cool, and reweigh to constant weight (y g).
100 [ w - (y - x)]
Content of material soluble in acetone = % m/m
w

MT 6 MATERIAL SOLUBLE IN HEXANE

SCOPE
These methods are intended for materials which are freely soluble in hexane.

OUTLINE OF METHOD
The sample is refluxed with hexane, the hexane is evaporated and the residue
dried and weighed.

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 MISCELLANEOUS TECHNIQUES AND IMPURITIES

REAGENT
Hexane fraction boiling range 68 - 70 °C; RE 76
APPARATUS
Soxhlet extraction apparatus or straight through extractor
Round bottom flasks 250 ml with ground joint to fit the extractor; containing
2 glass beads and tared
Distillation set to fit the flask
Soxhlet thimble previously extracted with hexane then dried
Flameproof oven at 60 to 70 °C
PROCEDURE
Weigh (to the nearest mg) the specified amount (w g) of sample, transfer to
the thimble, and extract completely with hexane for about 4 h into the tared
flask (x g). Remove the flask from the extraction apparatus, distil off the
hexane and dry the flask and residue in the oven to constant weight at 60 to
70 °C. Cool and reweigh (y g).
100 (y - x)
Content of material soluble in hexane = % m/m
w

MT 7 MATERIAL SOLUBLE IN ETHANOL

SCOPE
These methods are intended for materials which are freely soluble in ethanol.
7.1 Hot solution
OUTLINE OF METHOD
The sample is refluxed with ethanol, the insoluble material is filtered off, dried
and weighed.
REAGENT
Ethanol (CH3CH2OH) 95% or Industrial Methylated Spirit
APPARATUS
Round bottom flask 250 ml reflux condenser to fit
Sintered glass crucible porosity P40 (pore size 16 - 40 µm); tared
Flameproof oven at 80 to 85 °C

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 MISCELLANEOUS TECHNIQUES AND IMPURITIES

PROCEDURE

Weigh (to the nearest 10 mg) about 10 g of sample (w g) and transfer to the
flask. Add ethanol (100 ml), and reflux for 30 min. Cool, filter the solution
through the tared crucible (y g), and wash the flask and the crucible with small
portions of cold ethanol (to remove any adhering solids). Dry the crucible, cool
and reweigh to constant weight (x g).
100 [ w - (x - y)]
Content of material soluble in ethanol = % m/m
w

7.2 Solution at room temperature

OUTLINE OF METHOD

The material is shaken with ethanol, the insoluble material is filtered off, dried
and weighed.

REAGENT

Ethanol (CH3CH2OH) 95% or Industrial Methylated Spirit

APPARATUS

Conical flask 250 ml 29/32 neck fitted with stopper

Sintered glass crucible porosity P16 (pore size 10 - 16 µm); tared
Mechanical shaker
Flameproof oven at 80 to 85 °C

PROCEDURE

Weigh (to the nearest mg) about 1 g of sample, transfer to the flask, add ethanol
(50 ml at 20 °C), and shake mechanically for 30 min at 20 °C, then filter the
solution through the tared crucible (y g). Wash out the flask and the residue on
the crucible with ethanol (5 or 6 × 5 ml) and dry under suction for 5 to 10 min.
Dry the crucible at 80 to 85 °C, cool and reweigh to constant weight (x g).

100 [ w - (x - y)]
Content of material soluble in ethanol = % m/m
w

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MT 8 MATERIAL INSOLUBLE IN KEROSENE

OUTLINE OF METHOD

The sample, dissolved in kerosene, is exposed to daylight at room temperature

for 10 days. It is examined at intervals for any turbidity and sediment.

REAGENT

Kerosene deodorized; RE 73

APPARATUS

Nessler cylinder or stoppered cylinder 100 ml

PROCEDURE

Dissolve the sample (20 g) in sufficient kerosene to make 100 ml of solution, and
transfer to the cylinder. Stopper, place the stoppered tube in an upright position,
and expose at room temperature to normal daylight for a period of 10 days. At the
end of the third and seventh days, examine the solution for the appearance of
turbidity or sediment. After the examination, invert the tube through 5 cycles
(Note 1) and replace it in its original upright position. At the end of the tenth
day, again examine the solution for turbidity or sediment on the wall or bottom
of the tube. Report the absence or presence of any turbidity and/or sediment.

Note 1 The expression 'invert the tube' as used above, implies that the
stoppered tube is tipped by hand through 180 degrees, and is then
brought back to its original position, each cycle being completed in
approximately 2 sec.

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