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DETERMINATION OF SULPHATE AS BARIUM SULPHATE

USING GRAVIMETRY WITH DRYING OF RESIDUE


Name: Eghan Kojo
Index N o : 6138811
Experiment N 0 : A 2.2.2
Graduate Assistant: Judith Odei
Date: 9 t h April, 2013

AIMS
1. To determine the amount of sulphate present in a sample by gravimetry.
2. To know how the digestion and other steps in gravimetric analysis is done.

INTRODUCTION
Gravimetry is the quantitative measurement of an analyte by weighing a pure, solid form of the analyte.
Obtaining pure solids from solutions containing an unknown amount of a metal ion is done by precipitation.
All Gravimetric analyses rely on some final determination of weight as a means of quantifying an analyte. Since
weight can be measured with greater accuracy than almost any other fundamental property, gravimetric analysis
is potentially one of the most accurate classes of analytical methods available. These methods are among the
oldest of analytical techniques, and they may be lengthy and tedious. Samples may have to be extensively
treated to remove interfering substances. As a result, only a very few gravimetric methods are currently used in
environmental analysis.
Gravimetric analysis describes a set of methods in analytical chemistry for the quantitative determination of an
analyte based on the mass of a solid. A simple example is the measurement of solids suspended in a water
sample: A known volume of water is filtered, and the collected solids are weighed.
In most cases, the analyte must first be converted to a solid by precipitation with an appropriate reagent. The
precipitate can then be collected by filtration, washed, dried to remove traces of moisture from the solution, and
weighed. The amount of analyte in the original sample can then be calculated from the mass of the precipitate
and its chemical composition.
In other cases, it may be easier to remove the analyte by vaporization. The analyte might be collectedperhaps
in a cryogenic trap or on some absorbent material such as activated carbon -- and measured directly. Or, the
sample can be weighed before and after it is dried; the difference between the two masses gives the mass of
analyte lost. This is especially useful in determining the water content of complex materials such as foodstuffs.
There are four fundamental types of gravimetric analysis: physical gravimetry, thermogravimetry, precipitative
gravimetric analysis, and electrodeposition. These differ in the preparation of the sample before weighing of the
analyte. Physical gravimetry is the most common type used in environmental engineering. It involves the

physical separation and classification of matter in environmental samples based on volatility and particle size
(e.g., total suspended solids). With thermogravimetry, samples are heated and changes in sample mass are
recorded. Volatile solids analysis is an important example of this type of gravimetric analysis. As the name
implies, precipitative gravimetry relies on the chemical precipitation of an analyte. Its most important
application in the environmental field is with the analysis of sulfite. Electrodeposition involves the
electrochemical reduction of metal ions at a cathode, and simultaneous deposition of the ions on the cathode.
Gravimetric analysis, if methods are followed carefully, provides for exceedingly precise analysis. In fact,
gravimetric analysis was used to determine the atomic masses of many elements to six figure accuracy.
Gravimetry provides very little room for instrumental error and does not require a series of standards for
calculation of an unknown. Also, methods often do not require expensive equipment. Gravimetric analysis, due
to its high degree of accuracy, when performed correctly, can also be used to calibrate other instruments in lieu
of reference standards.
Sulphate is widely distributed in nature and may be present in natural waters, soils and foods. Several methods
are available for the determination of sulphate. In this experiment, the sulphate in a sample is determined by
precipitation as barium sulphate. During the precipitation process the precipitant is added into the solution of
the analyte or generated insitu. The sulphate salt is precipitated in a dilute solution of hydrochloric acid as
barium sulphate by the addition of barium chloride slowly. The precipitation is carried out near the boiling
temperature.
The precipitate is digested, filtered; wash with water until free of chloride ions and dried before weighing
accurately as barium sulphate. To obtain high accuracy care should be taken that no precipitate is lost. Digestion
is a process of allowing the precipitate to be in contact with the mother liquor frequently at elevated
temperatures for sometimes before filtration. During the process of digestion the smaller particles of the
precipitate tend to dissolved and reprecipitate on the surfaces of the larger ones.
The method of choice for sulfate in waters and wastewaters is the precipitative gravimetric procedure
using barium. If Ba2+ is added in excess under acidic conditions, BaSO4 is precipitated quantitatively. The
reaction is allowed to continue for 2 hours or more at 80-90oC. This is to encourage the formation of BaSO4
crystals (non-filtrable) from the initially formed colloidal precipitate (partially filtrable). The precipitate is
washed, and then dried at 800`C for 1 hour. Low pH is needed to avoid the precipitation of BaCO3 and
Ba3(PO4)2. Positive bias may result from acid-resistant insoluble matter such as silica, sulfites which may
oxidize to sulfate, and nitrate and chloride which will associate with barium and co-precipitate to a small extent
with the barium sulfate. Negative bias may result from the presence of certain heavy metals (e.g., Cr, Fe) which
can form soluble complexes with sulfate.
Ba2+ + SO4-2 = BaSO4(ppt.)
Chloride may be determined by precipitation with silver. Interfering ions likely to form insoluble silver salts are
the other halogens (bromide, iodide), cyanide, and reduced sulfur species (sulfite, sulfide, and thiosulfate).
Fortunately, the reduced sulfur compounds can be pre-oxidized with hydrogen peroxide, and the others are
rarely present at high concentrations. Although AgCl can be determined gravimetrically, the recommended
procedure for water and wastewater is to use a volumetric procedure with chromate as an indicator.

CHEMICALS
1.
2.
3.
4.

0.05M Barium chloride solution


1:1 HCl
0.1M HNO3
Unknown sample

APPARATUS
1.
2.
3.
4.
5.
6.
7.

500ml beaker
200ml beaker
Stirring rod
Heating plate
Suction pump
Filter paper
Analytical balance

PROCEDURE

TABLE OF RESULTS
CALCULATIONS

DISCUSSION

PRECAUTIONS
1. The container that contained BaSO4 was washed with warm water to remove the Cl- salt present.
2. The filter paper and the precipitate were well dried to ensure accurate weight measurement.
3. HCl was added to the sample solution to prevent the precipitation of barium salts of weak acids such as
carbonates and phosphates etc., which will volatilize during ignition.
4. The precipitate was digested to increase the average particle size and reduce co-precipitation.
5. BaCl2 was added slowly amidst effective stirring to reduce relative supersaturation.

CONCLUSION

REFERENCES

1. Holler, F. James; Skoog, Douglas A.; West, Donald M. (1996). Fundamentals of analytical chemistry.
Philadelphia: Saunders College Pub.
2. APHA, AWWA, WPCF (1985) Standard Methods for the Examination of Water and Wastewater, APHA,
Washington, 16th edition, pp. 32-34, 76-80, 92-100.; or 15th edition, pp. 30-32, 70-73, 90-98.; or 14th
edition, pp. 34-36, 71-75, 89-98.
3. USEPA (1982) Handbook for Sampling and Sample Preservation of Water and Wastewater, US EPA,
EMSL, September, 1982; EPA-600/4-82-029 [Gov.Docs.: EP1.23/5:600/4-82-029].
4. Sawyer, C.N. & P.L. McCarty (1978) Chemistry for Environmental Engineers, McGraw Hill Publ,. pp.
65-69, 284-285, 454-462.
5. Snoeyink, V.L. & Jenkins, D. (1980) Water Chemistry, John Wiley & Sons, Publ., New York, pp. 74-82.