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Cyanide

testing

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javeria.khalid.waada
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6 views2 pages

Cyanide

testing

Uploaded by

javeria.khalid.waada
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
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Cyanide

Apparatus

 Cyanide Distillation apparatus


 Boiling Flask, 1 L, with inlet tube and provision for water cooled condenser.
 Gas absorber, with gas-dispersion tube equipped with medium-porosity fritted outlet.
 Heating element, adjustable.
 Ground-glass ST joints, TFE-sleeved or with an appropriate lubricant for the boiling flask
and condenser. Neoprene stopper and plastic threaded joints also may be used.

Reagents

a. Sodium hydroxide solution

Dissolve 40 g NaOH in reagent water and dilute to 1 L.

b. Magnesium chloride reagent

Dissolve 510 g MgCl2 .6H2O in water and dilute to 1 L.

c. Sulfuric acid (H2SO4), 1+1


d. Lead carbonate (PbCO3), powdered
e. Sulfamic acid (NH2SO3H).

Procedure

Macro- Distillation Method

 Add 500 mL sample, containing not more than 10 mg CN – /L (diluted with reagent water,
if necessary), to the boiling flask. If a higher CN – content is anticipated, use the spot test
(4500-CN–. K) to approximate the required dilution.
 Add 10 mL NaOH solution to the gas scrubber and, if necessary, dilute with reagent
water to obtain an adequate liquid depth in the absorber. Do not use more than 225 mL
total volume of absorber solution.
 If the distilling flask is expected to generate S 2– that cannot be adequately mitigated by
pre-treatment, add 50 mg powdered PbCO3 (or more) to the absorber solution to
precipitate S2–. Connect the train, consisting of boiling flask air inlet, flask, condenser,
gas washer, suction flask trap, and aspirator.
 Adjust suction so at least 1 air bubble/s enters the boiling flask. This air rate will carry
HCN gas from flask to absorber and usually will prevent a reverse flow of HCN through
the air inlet.
 If this air rate does not prevent sample backup in the delivery tube, increase airflow rate
to 2 air bubbles.
 Observe air purge rate in the absorber, where the liquid level should not be raised more
than 6.5–10 mm. Maintain airflow throughout the reaction.
 Add 2 g sulfamic acid through the air inlet tube and wash down with reagent water.
 Add 50 mL 1+1 H2SO4 through the air inlet tube. Rinse tube with reagent water and let
air mix flask contents for 3 min. Optionally, add 20 mL MgCl 2 reagent through air inlet
and wash down with stream of reagent water. A precipitate may form that redissolves
when heated.
 Heat with rapid boiling, but do not flood condenser inlet or permit vapors to rise more
than halfway into condenser. Reflux for at least 1 h at a rate of 40 to 50 drops/min from
the condenser. Discontinue heating but continue airflow for 15 min.
 Cool and quantitatively transfer absorption solution to a 250-mL volumetric flask. Rinse
absorber and its connecting tubing sparingly with reagent water and add to flask. Dilute
to volume with reagent water and mix thoroughly.
 Distillation yields quantitative recovery of refractory cyanides, such as iron complexes.
To obtain complete recovery of cobalticyanide, use UV radiation pretreatment. If
incomplete recovery is suspected, distill again by refilling the gas washer with a fresh
charge of NaOH solution and refluxing 1 h more. The cyanide from the second reflux, if
any, will indicate completeness of recovery.

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