Scribd
Upload
495 views

Barium

This document contains procedures for the quantitative chemical determination of barium and sulfates. The barium determination involves titrating a barium ion solution with EDTA at pH 12, indicated by a color change of methyl thymol blue/potassium nitrate mixture from blue to gray. The sulfate determination involves precipitating sulfate as barium sulfate, dissolving the precipitate in excess EDTA, and back-titrating the excess EDTA with magnesium chloride using solochrome black indicator. Proper amounts of 30-50 mg of indicator are recommended to get satisfactory color change without the color becoming too intense.

Uploaded by

R Fadhilah Lubis
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
495 views

Barium

This document contains procedures for the quantitative chemical determination of barium and sulfates. The barium determination involves titrating a barium ion solution with EDTA at pH 12, indicated by a color change of methyl thymol blue/potassium nitrate mixture from blue to gray. The sulfate determination involves precipitating sulfate as barium sulfate, dissolving the precipitate in excess EDTA, and back-titrating the excess EDTA with magnesium chloride using solochrome black indicator. Proper amounts of 30-50 mg of indicator are recommended to get satisfactory color change without the color becoming too intense.

Uploaded by

R Fadhilah Lubis
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
You are on page 1/ 2

Vogel

TEXTBOOK OF
QUANTITATIVE
CHEMICAL
10.52 DETERMINATION OF BARIUM: DIRECT TlTRATlON
Pipette 25 mL barium ion solution (CU 0.01 M) into a 250 mL conical flask and
dilute to about 100 mL with de-ionised water. Adjust the pH of the solution to
12 by the addition of 3-6 mL of 1 M sodium hydroxide solution; the pH must
be checked with a pH meter as it must lie between 11.5 and 12.7. Add 50 mg
of methyl thymol blue/potassium nitrate mixture [see Section 10.50(C)] and
titrate with standard (0.01 M) EDTA solution until the colour changes from
blue to grey.
1 mole EDTA = 1 mole Ba2+

C. Amount of indicator. The addition of too much indicator is a fault which


must be guarded against: in many cases the colour due to the indicator intensifies
considerably during the course of the titration, and further, many indicators
exhibit dichroism, i.e. there is an intermediate colour change one to two drops
before the real end-point. Thus, for example, in the titration of lead using xylenol
orange as indicator at pH = 6, the initial reddish-purple colour becomes
orange-red, and then with the addition of one or two further drops of reagent,
the solution acquires the final lemon yellow colour. This end point anticipation,
which is of great practical value, may be virtually lost if too much of the indicator
is added so that the colour is too intense. In general, a satisfactory colour is
achieved by the use of 30-50 mg of a 1 per cent solid mixture of the indicator
in potassium nitrate.

10.73 DETERMINATION OF SULPHATES


The sulphate is precipitated as barium sulphate from acid solution, the
precipitate is filtered off and dissolved in a measured excess of standard EDTA
solution in the presence of aqueous ammonia. The excess of EDTA is then
titrated with standard magnesium chloride solution using solochrome black as
indicator.
Procedure. Prepare a standard magnesium chloride solution (0.05M) and a
buffer solution (pH 10); see Section 10.72. Standard EDTA (0.05M) will also
be required.
Pipette 25.0 mL of the sulphate solution (0.02-0.03 M) into a 250 mL beaker,
dilute to 50 mL, and adjust the pH to 1 with 2M hydrochloric acid; heat nearly
to boiling. Add 15 mL of a nearly boiling barium chloride solution (CU 0.05 M)
fairly rapidly and with vigorous stirring: heat on a steam bath for 1 hour. Filter
with suction through a filter-paper disc (Whatman filter paper No. 42) supported
upon a porcelain filter disc or a Gooch crucible, wash the precipitate thoroughly
with cold water, and drain. Transfer the filter-paper disc and precipitate
quantitatively to the original beaker, add 35.0 mL standard 0.05 M EDTA
solution and 5 mL concentrated ammonia solution and boil gently for 15-20
minutes; add a further 2 mL concentrated ammonia solution after 10-15 minutes
to facilitate the dissolution of the precipitate. Cool the resulting clear solution,
add 10 mL of the buffer solution (pH = IO), a few drops of solochrome black
indicator, and titrate the excess of EDTA with the standard magnesium chloride
solution to a clear red colour.
Sulphate can also be determined by an exactly similar procedure by
precipitation as lead sulphate from a solution containing 50 per cent (by volume)
of propan-2-01 (to reduce the solubility of the lead sulphate), separation of the
precipitate, dissolution in excess of standard EDTA solution, and back-titration
of the excess EDTA with a standard zinc solution using solochrome black as
indicator.

You might also like