Hydrogen

I invite suggestions for estimation of chloride content in organics?

I have an Organic compound comprising of Hydrogen chloride in dissolved form. There is a presence of another halogenated compound as well. My first task is to accurately determine HCl; and second task equally important is to determine total chloride content.

Quantitative Estimation of Chlorides and Sulphates in Expressed Plant Tissue Fluids
Ross Aiken Gortner, Walter F. Hoffman
Botanical Gazette, Vol. 77, No. 1 (Mar., 1924), pp. 96-102

Methods have been described for the rapid and accurate determinations of chlorine and sulphates in plant saps. These methods are essentially as described by Wetmore for chlorides in blood and by Benedict for sulphur in urine. The manipulations are simple, and neither elaborate apparatus nor exceptional skill is required.

II:Oxidation of organically bound chlorine is effected by heating with specially prepared silver dichromate in the presence of concentrated sulphuric acid. Inorganic chloride may be determined after its oxidation in the cold by an acid permanganate mixture (Conway, 1935), organically bound chlorine not being attacked under these conditions. The latter
methodmay be used for the specific determination of DDTsince 1 mol.ofhydrochloricacidisliberated/mol. of DDT by the action of alcoholic alkali (Gunther, 1945). Chlorine volatilized bythe oxidation is carried
CHLORINE IN ORGANIC COMPOUNDS
by a stream of nitrogen into potassium iodide solution contained in an absorbing vessel. The problem then becomes one of micro-iodometry. For amounts down to 1 ,ug. chlorine a direct determination of the liberated iodine is possible. For amounts below lug. a technique has been devised for the separation of the free iodine and its conversion to iodate. In studies of the distribution and fate of DDT in the body, these methods may be applied to the
analysis oftissue extracts. Bycarrying out determinations
of total chlorine, inorganic chlorine before and after incubation with alcoholic alkali and of alkali-soluble organically bound chlorine, it is possible to establish the presence of DDT, other organic compounds containing neutral chlorine and alkali-soluble compounds containing chlorine.
Apparatus
Description. The apparatus is constructed ofpyrex
glass. Oxidation is carried out in the reaction vessel A,
connected by means of combined still head and dropping
funnel Bto the absorbing vessel Cwhich consists ofa delivery
tube contained in an outer vessel, the walls of which fit
closely to the spiral rod wound round the delivery tube.
C is connected with the absorber D of similar construction.
The central absorbertube Cis required onlyforthe determinationof Cl in tissues. Its purpose is to remove SO2 which may be evolved during the reaction and it contains a mixture of saturated KMnO4 (2 vol.) and 50% (v/v) H2SO4 (1 vol.).
A spiral of glass rod is wound round the stem of the
dropping funnel B; its purpose is made plain in the section
on the determination of DDT. The gas inlet E is connected
by pressure tubing to a N2 cylinder fitted with a reducing
valve, and the gas rate is adjusted by the bubble rate in
a wash bottle. The gas inlet consists of a tube fitting by a
standard joint into the neck of the dropping funnel B. The
latter holds H,S04, which is run into the flask after the
apparatus has been assembled.
The purpose of a fine capillary in C and D just below the
level of the joint socket will be made clear in the section on
gas flow.
Gasflou. Because of the dimensions of the apparatus, the
passage of gas at the rates required leads to irregular flow
owing to fluctuations of pressure within the assembly.
Regularity was achieved by introducing constrictions just
below the joints of the delivery tubes .
Reagents
Sulphuric acid. The concentrated acid (A.R. grade) has
been found to give a zero blank. It should be stored away
from direct light and should be shaken before use with
a small amount of silver dichromate to remove reducing
substances.
Silver dichromate. The commercial salt yields a large blank,
owing to traces of nitrate. The following method of preparation
yields a product giving zero blank values. Silver
oxide is prepared from AgNO3 by precipitation with 40%
(w/v) NaOH. The precipitate is washed with water 12 times
by decantation. The moist oxide is then dissolved in the
minimum volume of70% (v/v) H2504 and an excess ofCrO8,
dissolved in the minimum volume of water, is added. A dark
red precipitate of the dichromate separates at once. The
flask is now placed in a boiling water bath, and air drawn
rapidly through the mixture for about 3 hr. Nitrate and
chloridearethus completelyremoved. Asoda-limetubeshould
be attachedto theairintake. The contents ofthe flaskare then
diluted and allowed to stand overnight. The precipitate is
washed by decantation at least 10 times. At the end of the
washing, the water should be bright yellow in colour from
dissolved dichromate. The flask and contents are now dried
at 900 and the silver dichromate stored in a dark bottle. The
yield is almost quantitative.

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