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Application of Ion Exchange Resin

This document provides instructions for using ion exchange resins and gas chromatography to separate and analyze mixtures. Specifically, it describes: 1) Using anion exchange resin to separate nickel and zinc ions based on zinc forming anionic complexes that are retained on the resin while nickel passes through. Both are then titrated with EDTA. 2) A method to determine magnesium in milk of magnesia tablets by passing the sample through a cation exchange column where magnesium is retained and replaced by hydrogen, then titrating the acid in the eluate. 3) Gas chromatography can be used to separate ethanol from other components in beverages and determine the proof of alcoholic drinks based on their ethanol concentration.

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Edna Lip Aner
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134 views3 pages

Application of Ion Exchange Resin

This document provides instructions for using ion exchange resins and gas chromatography to separate and analyze mixtures. Specifically, it describes: 1) Using anion exchange resin to separate nickel and zinc ions based on zinc forming anionic complexes that are retained on the resin while nickel passes through. Both are then titrated with EDTA. 2) A method to determine magnesium in milk of magnesia tablets by passing the sample through a cation exchange column where magnesium is retained and replaced by hydrogen, then titrating the acid in the eluate. 3) Gas chromatography can be used to separate ethanol from other components in beverages and determine the proof of alcoholic drinks based on their ethanol concentration.

Uploaded by

Edna Lip Aner
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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1112 CHAPTER 37 Selected Methods of Analysis

working curve; then measure the emission intensity of the unknown. Correct the
data for background. Determine the cation concentration in the unknown by
comparison with the working curve.

37Q APPLICATION OF ION EXCHANGE RESINS


37Q-1 The Separation of Cations
The application of ion-exchange resins to the separation of ionic species of oppo-
site charge is discussed in Section 30D. Directions follow for the ion-exchange
separation of nickel(II) from zinc(II) based on converting the zinc ions to nega-
tively charged chloro complexes. After separation, each of the cations is deter-
mined by EDTA titration.

Discussion
The separation of the two cations is based on differences in their tendency to form
anionic complexes. Stable chlorozincate(II) complexes (such as ZnCl3 and ZnCl2 4 )
are formed in 2 M hydrochloric acid and retained on an anion-exchange resin. In
contrast, nickel(II) is not complexed appreciably in this medium and passes rapidly
through such a column. After separation is complete, elution with water effectively
decomposes the chloro complexes and permits removal of the zinc.
Both nickel and zinc are determined by titration with standard EDTA at pH 10.
Eriochrome Black T is the indicator for the zinc titration. Bromopyrogallol Red or
murexide is used for the nickel titration.

PREPARATION OF SOLUTIONS

1. Standard EDTA. See Section 37E-2.


2. pH-10 buffer. See Section 37E-1.
3. Eriochrome Black T indicator. See Section 37E-1.
4. Bromopyrogallol Red indicator (sufficient for 100 titrations). Dissolve 0.5 g of
the solid indicator in 100 mL of 50% (v/v) ethanol.
5. Murexide indicator. The solid is approximately 0.2% indicator by weight in
NaCl. Approximately 0.2 g is needed for each titration. The solid preparation is
used because solutions of the indicator are quite unstable.

PREPARATION OF ION-EXCHANGE COLUMNS

A typical ion-exchange column is a cylinder 25 to 40 cm in length and 1 to 1.5 cm


in diameter. A stopcock at the lower end permits adjustment of liquid flow through
the column. A buret makes a convenient column. It is recommended that two
columns be prepared to permit the simultaneous treatment of duplicate samples.
Insert a plug of glass wool to retain the resin particles. Then introduce sufficient
strong-base anion-exchange resin (Note) to give a 10- to 15-cm column. Wash the
column with about 50 mL of 6 M NH3, followed by 100 mL of water and 100 mL
of 2 M HCl. At the end of this cycle, the flow should be stopped so that the liquid
level remains about 1 cm above the resin column. At no time should the liquid level
be allowed to drop below the top of the resin.
37Q Application of Ion Exchange Resins 1113

Note
Amberlite CG 400 or its equivalent can be used.

PROCEDURE

Obtain the unknown, which should contain 2 to 4 mmol of Ni2 and Zn2, in a
clean 100-mL volumetric flask. Add 16 mL of 12 M HCl, dilute to the mark with
distilled water, and mix well. The resulting solution is approximately 2 M in acid.
Transfer 10.00 mL of the diluted unknown onto the column. Place a 250-mL
conical flask beneath the column, and slowly drain until the liquid level is barely
above the resin. Rinse the interior of the column with several 2- to 3-mL portions of
the 2 M HCl; lower the liquid level to just above the resin surface after each
washing. Elute the nickel with about 50 mL of 2 M HCl at a flow rate of 2 to 3
mL/min.
Elute the Zn(II) by passing about 100 mL of water through the column, using
the same flow rate; collect the liquid in a 500-mL conical flask.

Titration of Nickel
Evaporate the solution containing the nickel to dryness to eliminate excess HCl.
Avoid overheating; the residual NiCl2 must not be permitted to decompose to NiO.
Dissolve the residue in 100 mL of distilled water, and add 10 to 20 mL of pH-10
buffer. Add 15 drops of Bromopyrogallol Red indicator or 0.2 g of murexide.
Titrate to the color change (blue to purple for Bromopyrogallol Red, yellow to
purple for murexide).
Calculate the number of milligrams of nickel in the unknown.

Titration of Zinc
Add 10 to 20 mL of pH-10 buffer and 1 to 2 drops of Eriochrome Black T to the
eluate. Titrate with standard EDTA solution to a color change from red to blue.
Calculate the mass of zinc in the unknown in milligrams.

37Q-2 Determination of Magnesium by


Ion-Exchange Chromatography
Discussion
Magnesium hydroxide in milk of magnesia tablets can be determined by dissolving
the sample in a minimum of acid and diluting to a known volume. The excess acid
is established by titrating several aliquots of the diluted sample with standard base.
Other aliquots are passed through a cation exchange column, where magnesium
ion is retained and replaced in solution by a chemically equivalent quantity of
hydrogen ion:

Mg2  2Hres 
res  2H

S Mg2

The acid in the eluate is then titrated; the difference between the volumes of base
needed for the two series of titrations is proportional to the magnesium ion in the
sample. Thus,

net mmol H  2  mmol Mg2


1114 CHAPTER 37 Selected Methods of Analysis

PROCEDURE

Step 1. Prepare approximately 1 L of 0.05 M NaOH. Standardize this solution


against weighed portions of dried primary-standard potassium hydrogen
phthalate (KHP); use about 0.4-g (to the nearest 0.1 mg) samples of KHP
for each standardization.
Step 2. Record the number of tablets in your sample. Transfer the tablets to a
clean 500-mL volumetric flask (Note 1). Dissolve them in a minimum
volume of 3 M HCl (4 to 5 mL/tablet should be sufficient). Then dilute to
the mark with distilled water.
Step 3. Titrate the free acid in several 15.00-mL aliquots of the dissolved sample;
phenolphthalein is a satisfactory indicator.
Step 4. Condition the column with about 15 mL of 3 M HCl (Note 2), followed by
three 15-mL portions of distilled water. Never permit the liquid level to
drop below the top of the column packing.
Step 5. Charge each column with a 15.00-mL aliquot of the sample. Elute at a rate
of about 2 to 3 mL/min. Wash the column with three 15-mL portions of
water. Collect eluate and washings in a conical flask. Repeat this step with
additional aliquots of the sample (Note 3).
Step 6. Titrate the eluted samples (and washings) with standard base. Correct the
total volume for that needed to titrate the free acid, and calculate the mass
of Mg(OH)2 in milligrams in each tablet.

Notes
1. The sample will dissolve more quickly if the tablets are first ground in a mortar.
If you choose this alternative, you will need to know (a) the total mass of your
tablets and (b) the mass of ground sample that you transfer to the volumetric
flask.
2. The volume of the sample aliquots and the volume of base used in the several
titrations must be measured carefully (to the nearest 0.01 mL). All other vol-
umes can and should be approximations only.
3. A 25-mL buret packed to a depth of about 15 cm with Dowex-50 cation
exchange resin makes a satisfactory column. Reconditioning after 4 or 5 elu-
tions is recommended.

37R GAS-LIQUID CHROMATOGRAPHY


As noted in Chapter 31, gas-liquid chromatography permits the analyst to separate
the components of complex mixtures. The accompanying directions are for the
determination of ethanol in beverages.

37R-1 The Gas-Chromatographic Determination of


Ethanol in Beverages15
Discussion
Ethanol is conveniently determined in aqueous solutions by means of gas chro-
matography. The method is readily extended to measurement of the proof of
alcoholic beverages. By definition, the proof of a beverage is two times its volume
percent of ethanol at 60°F.

15Adapted from J. J. Leary, J. Chem. Educ., 1983, 60, 675.

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