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MT 181 Solubility in Organic Solvents: Miscellaneous Techniques

This document provides a method for determining the solubility of substances in organic solvents. It describes how to conduct a preliminary test to estimate solubility using 0.1g of test substance. Based on these results, the appropriate mass of test substance is selected for the main test. The main test involves adding incremental volumes of solvent to the test substance until complete dissolution is achieved to determine the solubility range. Duplicate determinations are performed for each solvent.

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2K views

MT 181 Solubility in Organic Solvents: Miscellaneous Techniques

This document provides a method for determining the solubility of substances in organic solvents. It describes how to conduct a preliminary test to estimate solubility using 0.1g of test substance. Based on these results, the appropriate mass of test substance is selected for the main test. The main test involves adding incremental volumes of solvent to the test substance until complete dissolution is achieved to determine the solubility range. Duplicate determinations are performed for each solvent.

Uploaded by

Felipe Navarrete
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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MISCELLANEOUS TECHNIQUES

*
MT 181 SOLUBILITY IN ORGANIC SOLVENTS

DEFINITION

The solubility of a substance is specified by the saturation concentration of


the substance in a given solvent at a given temperature. Solubility may be
specified in units of mass per volume of solvent or solution but the method is
intended to provide the former. Whilst the SI unit is kg m-3, other units such
as g/l or g/100 ml may also be requested.

SCOPE

The method is not suitable for the determination of solubilities below 10 g/l.
To determine lower solubilities, or when precision higher than the predefined
ranges described is required, MT157 (Water Solubility) may be adapted.

OUTLINE OF METHOD

The solubility - within predefined ranges - of a test substance in organic


solvents is determined by adding measured volumes of solvent to a known
mass of test substance until complete dissolution is observed.
A preliminary test is employed to determine the approximate solubility of the
test substance. The results of the preliminary test are used to select the most
appropriate mass of test substance for the test.

REAGENTS AND SUBSTANCES

Test substances. The method is applicable to substances of all purities.


However, it will determine the solubility of the least soluble component of
an impure test substance and caution is required when impurities of low
solubility are present. Solids must be thoroughly pulverised before use.
Test Solvents. The solubility of each test substance is determined in a series
of solvents. The solvents listed are recommended but alternatives may be
adopted where one or more of these is inappropriate to, or incompatible
with, the test substance.

*
Provisional CIPAC method 1997

314
MISCELLANEOUS TECHNIQUES

an aliphatic hydrocarbon - preferably n-heptane


an aromatic hydrocarbon - preferably p-xylene
a halogenated hydrocarbon - preferably 1,2-dichloroethane
an alcohol - preferably methanol or propan-2-ol
a ketone - preferably acetone
an ester - preferably ethyl acetate
The use of alternative solvents must be justified. If the test substance is
known to be incompatible with a solvent in the above list this must be
reported. The chosen solvents should be of high purity analytical grade.

APPARATUS
Water bath or spark-proof incubator thermostatically controlled to the test
temperature (20 or 25 (±1) °C).
Stoppered graduated cylinders 10ml.

PROCEDURE

(i)Preliminary test
To 0.1g of test substance in a graduated cylinder (10ml) add increasing
measured volumes of solvent according to the steps below.

Total volume 0.5 1.0 2.0 3.0 4.0 5.0 10.0


required for
complete dissolution
(ml)
Approximate >200 100- 50- 33-50 25- 20- 10-
solubility 200 100 33 25 20
(g/l)

After each addition of solvent, shake the mixture vigorously and then store at
the test temperature with intermittent shaking for 10 min. Check the contents
of the cylinder visually for undissolved test substance before making the next
addition of solvent.
For solvents which do not dissolve the test substance after 10 ml of solvent
has been added and the mixture shaken as described, the main test need not
be undertaken. Record the solubility as <10 g/l.

315
MISCELLANEOUS TECHNIQUES

(ii)Determination of solubility
Derive the quantity of test substance to be used from the estimate of
solubility generated in the preliminary test.

Preliminary >200 100- 50-100 <50


estimate of 200
solubility (g/l)
Mass of test 0.5 0.4 0.2 0.1
substance used (g)

Make duplicate determinations are for each solvent.


Weigh the test substance into a graduated cylinder (10 ml) and add
incremental measured volumes of solvent, as indicated below, until complete
dissolution is achieved.

Total volume Solubility (g/l)


required for
where the mass of test substance used is
complete
dissolution (ml)
0.5g 0.4g 0.2g 0.1g
2.0 >250 >200 >100 >50
2.5 200-250 160-200 80-100 40-50
ß 167-200 133-160 67-80 33-40
3.5 114-133 57-67 29-33
4.0 100-114 50-57 25-29
5.0 80-100 40-50 20-25
7.0 29-40 14-20
10.0 10-14

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MISCELLANEOUS TECHNIQUES

After each addition of solvent, shake the mixture vigorously and then store at
the test temperature with intermittent shaking for at least 30 minutes. Check
the contents of the cylinder visually for undissolved material before making
the next addition of solvent.

(iii)Notes

If the test substance dissolves with the first addition of solvent, or remains
undissolved after the last scheduled addition adjust the mass of test substance
accordingly and repeat the test.

Duplicate determinations should result in the same solubility range. If this is


not achieved repeat the test.

Extraneous material may result in particles remaining for more than two
additions of solvent after the bulk of the test substance has dissolved. When
testing technical grade materials low solubility impurities may also be
present. If this is observed, pulverise another portion of the test substance,
ensure the graduated cylinders are free from particulate matter and repeat the
test. Where similar results are produced the solubility of the test substance
should be considered to equate to the final addition of solvent that produced
an observable change in dissolution. Report the presence of lower solubility
extraneous matter as part of the results of the test.

If sufficient test substance is available, the test may be conducted on a larger


scale in a larger cylinder (e.g. 50.ml). Adjust the quantity of test substance
and volumes of solvent added accordingly.

317

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