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Gravimetric Determination of Copper

Gravimetric Determination of Copper

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Analytical Chemistry Laboratory 2
Electrogravimetric Determination of Copper
 Mr. ***** 
 Department of Chemical Engineering and Chemistry, Mapua Institute of Technology
 Electrogravimetric analysis is an easy and accurate method for determining metalconcentrations using electrochemistry. The element copper that was determined was deposited asa solid on a pre-weighed electrode throughout the reduction process, and was measured by theweight gained by the electrode. The experiment was performed in two trials using sample # 2.The average percentage of copper in the solution was 17.72%.
Objective
The main purpose of thisexperiment is to determine the percentage of copper in the solution by electrogravimetricanalysis.
Discussion
Overview
In electrogravimetry, a metal ion isquantitatively (>99.9%) electroplated onto a preweighed “working” electrode almostalways as the solid metal. This takes place atthe negative electrode or cathode, which isdefined as that electrode at which reductiontakes place. From the gain in mass of theelectrode, the amount of metal in the samplecan be calculated – assuming no interferantsare also electroplated onto the electrode. Afew metal ions can be deposited in somechemical form onto the anode, the electrodeat which oxidation takes place.The unknown sample containingcopper was prepared by weighing (to thenearest 0.1 mg) 1-g samples into a 250-mL beaker. 25 mL of water was added, followed by 4 mL H
2
SO
4
and 1 mL HNO
3
. It was thenheated below boiling until solution iscomplete. After the solution was heated, itwas then cooled and diluted to 100 mL. This procedure was repeated again for the secondtrial.Copper (Cu) is a heavy metal whoseunbound ions are toxic. Copper salts areirritants to the skin, eyes, and mucousmembranes. Ingestion of copper salts maycause vomiting, diarrhoea, hemorragicgastritis, and excessive salivation. Toxicityis primarily due to accidental and suicidalattempts, and results in intravasculahemolysis, methemogloninemia, renalfailure and often death. Vineyard sprayersusing a solution containing aqueous copper sulphate developed granulomatous andfibrotic lung lesions. Inhalation of copper dust and fume results in irritation of therespiratory tract, ulceration and perforationof nasal septum, metallic or sweet taste, andin some instances, discoloration of the skinand hair. The inhalation of metal fumes produced at high temperature, such aswelding, may cause "metal fume fever", aninfluenza-like (benign) illness. High copper content in drinking water and food maycontribute to the development of severe liver damage in infants.As with all of the other industrialactivities, copper production is highlysubject to environmental regulation related
 
to air quality. The main pollutant of concernthat results from the copper smelting processis sulfur dioxide. Uncontrolled copper smelting processes emit large quantities of this, which can have major impacts onhuman health. Because of the consequencesevolving from these processes, The CleanAir Act was established, setting standards toregulate the “criteria pollutants”. In additionto the air quality concern with the miningand mineral processing of copper, there arealso many impacts on the environmentdealing with the water quality and wastedisposal. These adverse water qualityimpacts are caused primarily by landdisposal practices that fail to contain wastes, by run-on and run-off controls that areinadequate to prevent surface water fromflowing through impoundments, or bygroundwater infiltrating surfaceimpoundments. These open-pit miningmethods also can cause disturbances that canlower the water table in an area, causingwater shortages, land subsidence, andfracturing. In response to these effects, theEPA administered four major programs tohelp control the water quality and wastedisposal practices at domestic copper miningoperations. The first program was The CleanWater Act, which imposes limitations on point sources and requires permits from the National Pollutant Discharge EliminationSystem for any discharge of pollutants. Thenext program was the ResourceConservation and Recovery Act, regulatingthe generation, transport, and disposal of hazardous and solid wastes. Anothe program was the Superfund, which designs priorities for and oversees the clean up of these polluted sites. The fourth program wasthe Safe Drinking Water Act, designed to protect the quality of public drinking water supplies. As for the adverse impacts oncopper wastes, waste management practiceshave been established to set acceptablelevels to control areas such as theminimization, collection, and treatment of mine drainage, mill process water, andcontaminated surface damage. These areasof control are also for handling, storage,ultimate disposal of tailings and waste rock,and reclamation of the site to minimize longterm environmental effects once activemining has ceased.
Methodology
Preparation of Electrodes.The platinum electrodes wereimmersed in hot 6 M HNO
3
for about 5minutes. It was then washed with distilledwater and rinsed with several small portionsof ethanol, and was dried in an oven at110ºC for 2 to 3 minutes. It was then cooled.Electrolysis.The cathode was attached to thenegative terminal and the anode to the positive terminal of the electrolysisapparatus. The samples were placed in the beaker and the electrode was immersed in it.The electrolysis was then commencedmaintaining a current of 0.5 A (2 V) withstirring operating for about 30 minutes.After the duration, the completeness of theelectrolysis was tested by removing onedrop of the solution with a medicinedropper, and was mixed with a few drops of  NH
3
(aq) in a small test tube. The mixturedid’t turned blue therefore electrolysis wascomplete. The cathodes were dried for about3 minutes at 110ºC, and were cooled in air  before weighing them.
 Instrumentation
With this electrolysis apparatus, thecathode absorbs the copper ions in thesolution.
Interpretation

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