Environmental Express SimpleDist - Manual (Page 17)

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SimpleDist: Operation and Instruction Manual System Operation
5.0 Procedure
5.1 Pipette 50mL of sample or an aliquot diluted to 50mL with reagent water into the SimpleDist TM System boiling tube.
For solid samples weigh 1.0g or less to the nearest 0.01g, dilute to 50mL.
5.2 Insert inlet port liner into the green screw cap and thread assembly onto top of glassware. Be sure that the “step” on
the inlet port liner is flush with the top opening of the green cap.
5.3 Assemble inlet tube with funnel tip and insert into the smaller port on cap.
5.4 Pipette 25mL of 0.25N NaOH into the collection trap. If using the Snip & Pour concentrate pour the entire 5mL of the
1.25N NaOH into the trap and add enough DI Water to bring the volume up to a 22-23mL. The trap may be attached
to the glassware at this point or it may be filled off-line and then placed onto the glassware. Attach tubing/adaptor to
the collection trap.
5.5 Repeat 5.1 through 5.4 for all samples to be distilled.
5.6 Turn on the vacuum and slowly adjust each valve to provide an air flow bubble rate of 5-10 bubbles per second for
each position as viewed in collection trap. Vacuum should be sufficient to maintain slight negative pressure on the
assembly throughout the distillation.
5.7 If nitrate-nitrite is known to be present add 5.0mL of sulfamic acid reagent through the reagent inlet. Allow the air
flow to mix for several minutes.
5.8 If iron cyanide complexes are known to be present add 2.0mL of magnesium chloride reagent. If excess foaming
occurs, add an additional 2.0mL. Allow a few minutes to mix.
5.9 Slowly add 5.0mL of 18N sulfuric acid though the reagent inlet.
5.10 Turn the heat on and set the temperature of the heating block to 125°C. The block will achieve this temperature in
approximately 30 minutes. Heat for an additional 60 minutes after the block achieves this temperature.
5.11 Remove the collection trap from the assembly.
5.12 Turn air/vacuum valves to the off position. Repeat for each sample position.
5.13 The distilled cyanide in the cyanide trap is now ready for analysis. Pour contents into appropriate container. When
pouring position the vent tube of the cyanide trap up to prevent trapping of air.
5.14 After use clean exterior surfaces with a damp sponge. For acid spills sponge with a diluted solution of sodium
bicarbonate followed by distilled water.
Total Cyanide Distillation with the SimpleDist™ Continued:
1.0 Scope and Application
1.1 This method follows both Standard Methods 4500-NH3 titled Nitrogen (Ammonia) and US EPA Method 350.1
titled Determination of Ammonia Nitrogen by Semi-Automated Colorimetry. These methods are applicable to the
determination of ammonia nitrogen in drinking, ground, surface, and saline waters, domestic and industrial wastes,
and soils.
1.2 The standard applicable range is 0.01 – 2.0mg/L NH3 as N. Higher concentrations can be determined by sample
dilution.
2.0 Summary of Method
2.1 A sample is buffered at pH 9.5 with borate buffer to decrease hydrolysis of cyanates and organic nitrogen compounds.
It is then distilled into one of two catch solutions. Boric acid is used when nesslerization or titration are used for
analysis or into sulfuric acid when the phenate method or ion selective electrode method are used for analysis. The
distillate is then analyzed by one of the methods listed above.
2.2 Reduced volume versions of this method that use the same reagents and molar ratios are acceptable provided they
meet the quality control and performance requirements stated in the method.
2.3 Limited performance-based method modifications may be acceptable provided they are fully documented and meet
or exceed method requirements.
Ammonia Nitrogen Distillation with the SimpleDist™: