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This document describes a redox titration method to determine the calcium content in limestone. Calcium is precipitated from the limestone sample as calcium oxalate by reacting it with oxalate ions. The calcium oxalate precipitate is dissolved in acid and then titrated with potassium permanganate. The titration results are used to calculate the percentage of calcium oxide in the original limestone sample. The average percentage of calcium oxide found in the limestone samples tested was 38.14% with a percent error of 16.48%, likely due to errors in precipitate formation and loss.
This document describes a redox titration method to determine the calcium content in limestone. Calcium is precipitated from the limestone sample as calcium oxalate by reacting it with oxalate ions. The calcium oxalate precipitate is dissolved in acid and then titrated with potassium permanganate. The titration results are used to calculate the percentage of calcium oxide in the original limestone sample. The average percentage of calcium oxide found in the limestone samples tested was 38.14% with a percent error of 16.48%, likely due to errors in precipitate formation and loss.
This document describes a redox titration method to determine the calcium content in limestone. Calcium is precipitated from the limestone sample as calcium oxalate by reacting it with oxalate ions. The calcium oxalate precipitate is dissolved in acid and then titrated with potassium permanganate. The titration results are used to calculate the percentage of calcium oxide in the original limestone sample. The average percentage of calcium oxide found in the limestone samples tested was 38.14% with a percent error of 16.48%, likely due to errors in precipitate formation and loss.
School of Chemistry and Chemical Engineering, MAPUA Institute of Technology
Abstract A redox titration is based on oxidation-reduction reaction between analyte
(Na2C2O4) and titrant (KMnO4). It determines the concentration of an analyte containing either an oxidizing or a reducing agent by measuring it against a standardized titrant. Potassium permanganate is a powerful oxidizing agent and serves as a self-indicator in the titration with reducing agent. The analyte in a redox titration must be in a single oxidation state at the outset. The steps that precede the titration the sample preparation and elimination of interferences which usually involve converting the analyte to a mixture of oxidation states. Prereduction is done to ensure that the analyte is present in a single oxidation state. Limestone usually contains a mixture of calcium carbonate and magnesium carbonate, which is called dolomitic limestone. Calcium is conveniently determined by precipitation with oxalate ion and it was found out that its average percent weight is 38.14% while its percent error is 16.48%. Errors in coprecipitation and loss of precipitate are just some of the few errors that account for this experiment discuss in the conclusion part.
Keywords: redox titration, calcium, limestone, oxidation states
INTRODUCTION can donate an electron. Consider, for
example, a titration in which a titrant in a An oxidation/reduction (redox) reduced state, Ared, reacts with a titrant in an reaction is one in which electrons are oxidized state, Box. transferred from one reactant to another. It can be analogous to the Brönsted-Lowry Ared+Box⇌Bred+Aox concept of acid/base reactions. Both involve the transfer of one or more charged particles Limestone is usually described as from a donor to an acceptor – the particles rock made from calcium carbonate, CaCO3 , being electrons in a redox reaction and but in fact most limestone rock contains protons in an acid-base reaction. significant amounts of magnesium, silicates, manganese, iron, titanium, aluminum, sodium, potassium, sulphur (as sulphides or A substance that has a strong affinity sulphates) and phosphorus. In this to electrons is called oxidizing agent, or an experiment, a sample of limestone is be to oxidant. A reducing agent, or reductant, is a analyzed to determine how much calcium it specie that easily donates electrons to contains. another specie. When a reducing agent donates an electron, it becomes an oxidizing In common with a number of other agent that can accept an electron. cations, calcium is conveniently determined Conversely, when an oxidizing agent gains by precipitation with oxalate ion. The solid an electron, it becomes a reducing agent that calcium oxalate is filtered, washed free of
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excess precipitating agent, and dissolved in Continue adding ammonia until the dilute acid. The oxalic acid liberated in this solution becomes an intermediate to yellow- step is then titrated with standard orange indicator. Let the solution stand for permanganate or some other oxidizing awhile to allow the precipitate to settle down reagent. This method is applicable to and filter. Wash the precipitate to samples that contain magnesium and alkali remove(𝑁𝐻2 )4 𝐶2 𝑂2 , by several portions of metals. Most other cations must be absent 10mL cold water. since they either precipitator coprecipitate and cause positive errors in the analysis. After separating the precipitate, a 50- Consider the reaction below: mL of 3M sulfuric acid is added to each flask and was titrated using 0.1687mmoles/mL of potassium permanganate solution while maintaining its temperature to about 55-90℃ using thermometer and placed a magnetic stirrer to each flask for continuous swirling of the These are the equations for the redox sample to avoid over titration. results are analysis of Ca in the unknown limestone reported in % CaO in the sample. sample that are used in calculating the %weight of CaO in the unknown RESULTS/ DISCUSSIONS
EXPERIMENTAL In common with a number of other
cations, calcium is conveniently determined This experiment is divided into two by precipitation with oxalate ion. The solid parts. First is the preaparation of the sample calcium oxalate is filtered, washed free of and second is the precipitation of the oxale excess precipitating reagent, and dissolved to determine the calciumcontent in the in dilute acid. The oxalic acid liberated in limestone. this step is then titrated with standard permanganate or some other oxidizing The unknown sample is dried for 2 reagent. This method is applicable to hours and cooled after in the desiccator and pthealkali metals. Most other cations must duplicate samples of the unknown are be absent since they either precipitate or weighed from 0.25-0.30g. This is done for coprecipitate as oxalates and cause positive two trials. To each sample placed in a 500- errors in the analysis. mL Erlenmeyer flask, 10mL water is added and 10mL HCl is added. For example, the calcium oxalate Second, is the preparation or th formed in a neutral or an ammoniacal precipitation of the oxalate ion. A 5 drop of solution is likely to be contaminated with Bromine solution added in the solution and calcium hydroxide or a basic calcium heat after for 5 minutes inside the fume oxalate, either of which will cause low hood; note: Bromine is highly toxic. Dilute results. The formation of these compounds each sample to 50 mL water and add 100 is prevented by adding the oxalate to an mL of hot 6% (w/v)(𝑁𝐻2 )4 𝐶2 𝑂2 , 3-4 drops acidic solution of the sample and slowly of methyl red. PRecipitae calcium oxalate forming the desired precipitate by the by adding 6M Ammonia. dropwise addition of ammonia. The coarsely crystalline calcium oxalate that is produced
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under these conditions is readily filtered. interference through the formation of Losses resulting from the solubility of soluble oxalate complexes of magnesium. calcium oxalate are negligible above pH 4, Prompt filtration of the can also help provided that washing is limited to freeing prevent interference because of the the precipitate of excess oxalate. pronounced tendency of magnesium oxalate to form supersaturated solutions from which Table-1 precipitate formation occurs only after an TRIAL e.1 TRIAL 1 hour or more. These measures do not suffice Wt of 0.2161 02638 for samples that contain more magnesium sample,g than calcium. Here, reprecipitation of the Volume of 9.9 9.3 calcium oxalate becomes necessary. 𝑲𝑴𝒏𝑶𝟒 used,mL Limestones are composed principally Volume of 0.1 of calcium carbonate; dolomitic limestones 𝑲𝑴𝒏𝑶𝟒 in blank det’n contain large amounts of magnesium used,mL carbonate as well. Calcium and magnesium Net volume 9.8 9.2 silicates are also present in smaller amounts, of 𝑲𝑴𝒏𝑶𝟒 along with the carbonates and silicates of ,mL iron, aluminum, manganese, titanium, % CaO in 42.92 33.36 sodium, and other metals. Hydrochloric acid the sample is an effective solvent for most limestones. Wt of CaO in 0.2116 0.2008 Only silica, which does not interfere with the the analysis, remains undissolved. Some sample,mg limestones are more readily decomposed Average % 38.14 after they have been ignited; a few yield weight of only to a carbonate fusion. CaO The method that follows is The data above shows the tabulated remarkably effective for determining results gathered from this experiment which calcium inmost limestones. Iron and shows that the weight percent of CaO is aluminum, in amounts equivalent to that of 38.14% while its true value is 45.67%.It is calcium, do not interfere. Small amounts of essential that the mole ratio between calcium manganese and titanium can also be and oxalate be exactly unity in the tolerated precipitate and thus in solution at the time of titration. A number of precautions needed to CONCLUSION/RECOMMENDATION ensure this condition. Redox titration is important in Coprecipitation of sodium oxalate determination of the mass of calcium in a becomes a source of positive error in the sample and then determination of the determination of calcium whenever the percent of mass in limestone is by titrating it concentration of sodium in the sample with KMnO4. The result is 38.14% and it exceeds that of calcium. The error from this shows that there are many sources of errors source can be eliminated by reprecipitation. in this experiment as it has obtained a Magnesium, if present in high concentration, 16.48% experimental error. may also be a source of contamination. An excess of oxalate ion helps prevent this
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Co-precipitate of the other cations with the calcium oxalate and incomplete precipitation of CaC2O4 when adding NH3, standardization process of KMnO4, impurities of the chemical, wrong determination of the end point, errors in reading the burette, errors in the analytical balance and the glassware used, incomplete heating at a specific temperature and doing the titration when the media is cool, loss of precipitate during filtration and loss of precipitate during transferring are errors that are encountered durng this experiment.