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Arsen.01 Imprimir
Arsen.01 Imprimir
01-1
ARSENIC
PRINCIPLE
SCOPE
The method is applicable to corn sugar, corn syrup and corn starch.
SAFETY
Because of the use of hot concentrated acids and the extreme toxicity of arsine,
assemble all apparatus and perform reaction in a well-ventilated fume hood.
Operate behind a shield and wear protective gear in the handling and disposal of
reagents and reaction products according to Good Laboratory Practice. Consult
Manufacturer's Safety Data Sheets (MSDS) of all reagents.
SPECIAL APPARATUS
REAGENTS (Note 3)
Fill each scrubber tube with glass wool moistened with 10% lead acetate
solution, avoiding excess. Pipet 4.0 ml of silver diethyldithiocarbamate
solution into each absorber tube. When the 15-minute standing period has
elapsed, remove the generator flask from the bath, add 4 g of granular zinc
(Note 5), and immediately attach the scrubber tube and absorber tube.
Immerse the apparatus in the water bath at 25 °C for 30 mins. Repeat the
above with each assembly.
B. Analysis (Note 7): Weigh accurately 5.00 ± 0.01 g of sample (Note 8) into a
100-ml beaker and dissolve or dilute with 10 ml of distilled water (Note 9).
Transfer the solution to be analyzed quantitatively to a generator flask and
reserve an empty flask for a reagent blank. To each flask add 5 ml of
concentrated hydrochloric acid, 2 ml of 15% potassium iodide solution , and
0.5 ml of 40% stannous chloride solution. Dilute to 40 ml with distilled water,
mix, and allow to stand in a 25 °C water bath for 15 mins.
Fill a scrubber tube with glass wool moistened with 10% lead acetate solution,
avoiding excess. Pipet 4.0 ml of silver diethyldithiocarbamate solution into
the absorber tube. When the 15-minute standing period has elapsed, remove
the generator flask from the bath, add 4 g of granular zinc (Note 5), and
ARSEN.01-4
immediately attach the scrubber tube and absorber tube. Immerse the
apparatus in the water bath at 25 °C for 30 mins.
4. Small zinc granules adhering to the neck (24/40 Ts joint) of the generator
flask preclude a tight seal when attaching the scrubber tube and absorber.
Leaks cause low and erratic results. Avoid this problem by adding the zinc
granules through a small funnel, with a 0.5-inch I.D. by 2.5-inch long stem,
so that particles do not contact the neck.
In case of excessive foaming, repeat the entire series using less zinc;
however, the amount must be sufficient to provide adequate sweeping of
the solutions and assembly.
permitted to drain into a cloth or paper towel before introducing the next
solution.
METHOD HISTORY
Combined the Arsenic methods for Corn Starch (Unmodified) (B-6), Corn Syrup
(E-4) and Corn Sugar (F-4) on 4-15-2010.