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manual of methods of analysis of foods - Ministry of Health and ...

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METALS<br />

Convert Cd <strong>and</strong> Zn dithizonates in third separator to chlorides by adding 40<br />

ml <strong>of</strong> 0.2N HCl <strong>and</strong> shaking vigorously for one minute. Carefully drain CCl 4<br />

layer <strong>and</strong> discard. Remove droplets <strong>of</strong> dithizone from aqueous phase by<br />

rinsing with 1 to 2 ml <strong>of</strong> CCl 4 <strong>and</strong> drain <strong>of</strong>f CCl 4 as completely as possible<br />

without allowing acid layer to pass bore <strong>of</strong> separator. Again adjust alkalinity<br />

to 5% by adding 10 ml NaOH solution. Add exactly 25 ml <strong>of</strong> dithizone<br />

solution <strong>and</strong> shake vigorously exactly for 1 min. Allow layers to separate<br />

exactly for 3 min. Wipe separator stems dry with cotton. Filter organic layer<br />

through pledget <strong>of</strong> cotton, discarding first 5 ml. Read the absorbance <strong>of</strong> the<br />

cadmium dithizone complex solution at 510 nm. Calculate cadmium in µg<br />

from st<strong>and</strong>ard curve or by substituting absorbance in linear equation.<br />

Preparation <strong>of</strong> St<strong>and</strong>ard Curve:<br />

Prepare in duplicate 6 st<strong>and</strong>ards containing 0, 5, 10, 15, 20, 25 µg <strong>of</strong><br />

cadmium as follows:<br />

Add appropriate volumes <strong>of</strong> st<strong>and</strong>ard solution to separator, adjust to 40 ml<br />

with 0.2N HCl, <strong>and</strong> 10 ml <strong>of</strong> NaOH solution <strong>and</strong> 25 ml <strong>of</strong> dithizone<br />

solution. Shake exactly for 1 min. let st<strong>and</strong> exactly for 3 min <strong>and</strong> filter<br />

organic layer through a pledged <strong>of</strong> adsorbent cotton, discarding first 5 ml.<br />

Determine absorbance ‘A’ at 510 nm <strong>and</strong> plot st<strong>and</strong>ard curve.<br />

(Ref :- A.O.A.C 15 th edn Official Method 945.58 Cadmium in Food ,<br />

Dithiozone Method / Manual Methods <strong>of</strong> Analysis for Adulterants <strong>and</strong><br />

Contaminants in Foods I.C.M.R,1990 Page 148)<br />

34

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