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APPARATUS
1. Beaker—500 mL.
REAGENTS
1. Silver nitrate (AgNO3) solution, 0.1 M—accurately standardized.
2. Sulfuric acid solution—about 0.5 M (see AOCS Laboratory Safety).
3. Potassium chromate indicator solution—dissolve 5 g of K2CrO4 (see AOCS Laboratory Safety) in distilled water
and add AgNO3 solution in distilled water until a slight red precipitate is formed. Filter and dilute to 100 mL with
distilled water.
4. Phenolphthalein indicator solution—1% in 95% alcohol.
5. Magnesium nitrate solution—20% Mg(NO3)2 · 6H2O in distilled water. Solution must be neutral and chloride
free.
All rights reserved. No part of this method may be reproduced or transmitted in any form or by any means without written permission of the publisher.
PROCEDURE
1. Accurately weigh 5 g (2–3 g for samples containing more than 5% NaCl) of the test sample into a 500 mL beaker
and add 300 mL of chloride-free distilled water. Boil if necessary to effect solution.
2. Add an excess of Mg(NO3)2 solution (usually about 25 mL of the 20% solution), filter, and wash thoroughly with
chloride-free distilled water to remove all chlorides.
3. Cool to room temperature (20–25°C). If the solution is alkaline, add a little phenolphthalein and then 0.5 M
H2SO4 until just colorless, avoiding an excess of more than 1 drop of acid. Add 1 mL of K2CrO4 indicator for every
100 mL of solution and titrate with 0.1 M AgNO3 to the first permanent reddish tinge.
4. Prepare a blank in a 500 mL beaker containing the same volume of distilled water, Mg(NO3)2 solution and indica-
tor. Add sufficient CaCO3 to the blank to make the turbidity equivalent to that of the test portion when both are
swirled.
5. Using the blank for comparison, continue the titration of the sample until a faint, but distinct color change occurs.
At the end point, the color of the sample solution should not be dark, but just distinctly different from that of the
blank.
6. Add sufficient 0.1 M AgNO3 to the blank so that the color of the blank and sample match.
CALCULATIONS
1. Chlorides, as NaCl, % =
(S − B) × M × 5.85
mass of test portion, g
Where—
S = volume of titrant, mL of test portion
B = volume of titrant, mL of blank
M = molarity of AgNO3
(S − B) × M × 7.46
2. Chlorides as KCl, % =
mass of test portion, g
Tetrachloroethylene (perchloroethylene) is a colorless, volatile, nonflammable liquid stances. Perform manipulations under a properly operating fume hood. Take partic-
chlorinated hydrocarbon that will emit toxic fumes of phosgene when exposed to ular precautions, such as the use of a glove box, when toxins are in dry form, because
sunlight or flames. It is an irritant to eyes and skin. The TLV is 50 ppm in air. of their electrostatic nature and resulting tendency to disperse in working areas. Swab
accidental spills of toxin with 5% NaOCl bleach. Rinse all glassware exposed to tox-
Tetrahydrofuran is a highly flammable liquid and a dangerous fire risk. The flammable ins with 1% NaOCl bleach solution and then wash thoroughly with warm water.
limits in air are 2–11%. It is toxic by ingestion and inhalation. The TLV in air is 200
ppm. It tends to form peroxides upon storage in air.
REFERENCES
Toluene is a highly flammable liquid and a dangerous fire risk. Explosive limits in air
are 1.27–7%. It is toxic by ingestion, inhalation, and skin absorption. The TLV is Official Methods of Analysis, Association of Official Analytical Chemists, 14th edn.,
100 ppm in air. A fume hood should be used at all times when using toluene. 1984, pp. 1010–1015.
Trichloroethane is a synthetic, light-sensitive, volatile, colorless, liquid miscible with Standard Methods for the Analysis of Oils, Fats and Derivatives, 7th edn., Blackwell
many nonpolar organic solvents. It is an irritant to eyes and skin. The TLV is 350 Scientific Publications, 1987.
ppm in air.
Hawley’s Condensed Chemical Dictionary, 11th edn., revised by N. I. Sax and R. J.
Xylene is flammable and a dangerous fire risk. The TLV is 100 ppm in air. Lewis, Jr., 1987.