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Cyanide Chemistry and Analysis
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Contents
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Distribution of the Industrial Uses of CN
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Who is measuring cyanide?
• NPDES
• Pretreatment
• SDWA
• Industrial hygiene
• foods
• beverages
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A generalized summary of cyanide and it’s metal
– cyanide species
• Transition metals - strong bonds
• Alkali metals - ionic bonds :C≡N
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Free Cyanide is the CN ion and HCN, generate
HCN at pH 6
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Metal Complexes require acid to generate HCN
Zn, Cd, Cu, Ni, Ag
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Strong Metal Complexes are stable in acid
solution
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Iron Cyanide Complexes are very stable in the
environment
[Fe(CN)6]-3 + H+
6 HCN + Fe+3
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Toxicity of Cyanide Complexes is related to its
ability to produce HCN
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Cyanide methods measure the various cyanide
“species”
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Holding Time Study – Sulfide Bearing Samples
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Cannot use Cadmium to Treat Sulfide
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Headspace to Treat Sulfide
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Bismuth to Treat Sulfide then distillation
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On-line Sulfide Abatement - ASTM
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Oxidizer Removal
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Manual “distillation” is used to dissociate as HCN
Macro Distillation MIDI
Distillations
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Distillation can be automated on a continuous
flow analyzer
Distillate
Distillation and
condenser
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Cyanide methods that utilize distillation have
significant disadvantages
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Many cyanide interferences result from
distillation
• Destroy CN • Create CN • UV distillation colorimetry - worst
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These compounds are in almost every sample
and interfere significantly
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Interferences –
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Interferences – Thiocyanate
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Interferences – Thiocyanate and Nitrate
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Interferences – Thiosulfate
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Interferences – Sulfite
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Interferences – Sulfur Compounds
• No Spot Tests
• Dechlorination
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How do you solve interference problems caused
by distillation?
?
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Replace distillation with gas diffusion
HCN
CN-
Membrane
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Interferences with Determinative
Step
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Titration by silver ion
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Ion Selective Electrode (ISE)
S-2
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Colorimetric methods
Turbidity
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Gas diffusion - Amperometry
HCN
CN-
Membrane
Sulfide > 50 ppm
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Free Cyanide Analysis
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ASTM D7237-06
Buffer
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Obtain accurate, cost effective free cyanide results
in minutes, not hours
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Available Cyanide Analysis
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Amenable Cyanide—CATC methods measure
“available cyanide”
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WAD Cyanide methods measure “available
cyanide”
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Ligand Exchange methods measure available
cyanide
GD-amperometry methods do not require
distillation
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Ligand Exchange GD-amperometry methods get
better recovery
OIA 1677 CATC WAD
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OIA 1677 or ASTM D6888 flow diagram
Acid Reagent
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Ligand Exchange GD-amperometry methods have
fewer interferences
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Ligand Exchange GD-amperometry methods give
you results in minutes
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Total Cyanide Analysis
Manual Distillation Methods
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Total cyanide methods using manual distillation
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Most total cyanide analyses are by EPA 335.4 or
similar
• Prolonged heating
• strong acid (pH <2)
• Purging into base
• Colorimetry
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Semi-automated colorimetric cyanide analysis flow
diagram
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Semi-Automated GD-amperometric by ASTM
D7284
Acid Reagent
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Automated total cyanide methods use UV to
liberate HCN from Fe
[Fe(CN)6]-3 + H+
6 HCN + Fe+3 hv
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A sample diagram of the Kelada 01 automated
cyanide method
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A sample diagram of the EPA 335.3 automated
cyanide method
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A sample diagram of ASTM D7511
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Comparison of Kelada and ASTM D7511
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Comparison of Total CN methods
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ASTM D7511-09 has fewer interferences than
distillation
* Cyanide added at 0.200 mg/L (EPA MCL SDWA)
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Interferences – Thiocyanate and Nitrate
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Thank You
Questions?
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