EXTRACTION : DETERMINATION OF ITS EFFICIENCY AND CALCULATION OF DISTRIBUTION COEFFICIENT

Natasha Pauline Go Marvin Marqueta Bachelor of Science Degree in Chemistry De La Salle University

Abstract To effectively utilize chemicals, they must be pure. With this being said, there arises a need for an extraction. This is done by dissolving solutes of importance in different solvents like water and organic solvents to separate them into another simpler more workable phase. In the process of extraction, there is always an error that comes up because different methods have varying rates of efficiency. The efficiency of an extraction method is determined by the distribution coefficient which is simply the ratio of the concentrations of the solute in the organic and aqueous solvents. This will determine which method is more efficient and effective. In this experiment, dimethyl ether was used to extract glacial acetic acid from an acetic acid solution. Two methods were used and analyzed in this experiment one step addition and double portions. The distribution coefficient of the first method is 0.1356 and the other method had a distribution coefficient of 0.1184. This clearly shows that the single step addition of the ether was more efficient than the other method but the difference is very small that it eventually becomes negligible in the end. It is recommended that another trial be performed to verify or nullify the results of this experiment.

I.

Introduction

Chemicals have different and distinct characteristics which are indeed helpful in many ways. These are remarked as their trademarks but to access these traits, they must be pure of impurities. This is when the role of extraction takes into account. Extraction is the process of sorting out an individual chemical from a mixture or a chemical. This process is done to come up with a product that is inside a chemical. It is

also called as the liquid liquid extraction; wherein, the chemical being extracted is dissolved in a solvent that is immiscible with its current solvent. Usually, water and organic solvents are used in this process. The substance in liquid phase A must also be soluble in liquid phase B for the extraction to occur. Once these two phases separate from each other, the separatory funnel is utilized to fully separate these two and transfer them into different containers to avoid recontamination.

Extractions can be done in a single step process, wherein the solvent is added once and the wanted substance is extracted once, and a multi step process, wherein the solvent is added and the substance is extracted multiple times. In this experiment, the efficiency of these two methods were determined, compared and analyzed to determine which method is more efficient in terms of extracting the substance of importance. This process can be rated according to its efficiency. There are many ways and means to express the efficiency of the extraction process namely, the distribution ratio, separation factors, decontamination factor, and slopes of graph. The most commonly used way to express this is through the distribution ratio or the distribution coefficient. This is given by the formula: (1) wherein, K is the coefficient and C is the concentration of the substance in the given solvent. This formula will be used in the discussion of this experiment. The distribution coefficient is used to express how well-extracted a substance is from its source, hence, the fraction in the formula resulting to a ratio. In this experiment, glacial acetic acid dissolved in water was extracted using an ether. Acetic acid is a colourless chemical that is famous for being the main component of vinegar. It is a simple carboxylic acid which implies that it is soluble in water and other organic solvents as most acids are. It is

also hydrophilic which means it is polar and can dissolve polar solutes like water and alcohols can. It also has properties that make it soluble in nopolar solvents as well. The extraction of this acid is very crucial since it is used in numerous ways like in production. Photographic films are manufactured using cellulose acetate, a derivative of acetic acid, and polyvinyl acetate is the main component of wood glue.

II.

Experimental Procedure

An acetic acid solution was prepared for utilization in the analysis. First, the sample was tested to determine the number of grams of glacial acetic acid that is present in 20mL of the sample solution. This was done using titration against 0.2M sodium hydroxide. Exactly 20mL of the sample solution was transferred to a 125mL Erlenmeyer flask and 2 drops of phenolphthalein was added to it to act as the indicator. The sample was titrated with the titrant until the distinct pink hue from the phenolphthalein becomes evident. The volume of the titrant used was noted and this was then used in the computation. Second, the glacial acetic acid was extracted using a single step addition of dimethyl ether. Another 20mL aliquot of the sample solution was transferred to a separatory funnel and 20mL of dimethyl ether was added to it. The funnel was sealed and it was shook back and forth carefully to
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bring about a reaction through their solubilities. The ether will dissolve the acetic acid and separate it from water. The acetic acid enters the organic phase through the ether added. As pressure builds up, the stopcock was opened and closed repeatedly to release it. When the sound from the pressure release was negligible already, the separatory funnel was left to stand cradled in the iron ring. Once the two phases were already distinguished, the separation began. The lower layer is the water with the acetic acid and the upper layer is the ether with the acetic acid. The amount of acetic acid extracted by the ether was determined by subtracting the amount of acetic acid in the plain solution and the one from the separation process. The difference is the amount of glacial acetic acid that the dimethyl ether extracted from the aqueous acetic acid solution. Lastly, the glacial acetic acid was extracted from the aqueous solution using two portions of the same ether. Instead of a single 20mL addition, the process was divided into two. Two batches of 10mL ether addition-extraction was performed and the same procedure as the first extraction was applied.

III.

Results and Discussion

The table below summarizes the data gathered and calculated from the experiment. PreExtracti on Volume (mL) of the sample Volume (mL) of titrant used Number of grams (g) of acetic acid left Number of moles (mol) of acetic acid left Number of grams (g) of acetic acid extracted Number of moles (mol) of acetic acid extracted Distributio n Coefficient 20 Single Step Extracti on 20 Double Step Extractio n 20

8.45

7.48

7.59

0.102

0.0898

0.0912

0.00169

0.00150

0.00152

0.0122

0.0108

0.000020

0.000018

0.1356

0.1184

Table1. This table summarizes the data from the experiment done.

Based on the given data, it can be concluded that the two methods do not have a significant difference in their efficiency in small scale experiments. Their difference is very negligible. Although it is negligible, the single step addition seems more efficient
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than the double step extraction in terms of their distribution coefficients. It is recommended that another trial be performed to verify these inherent results.

        

IV.

Appendix

4. number of grams extracted using first method 

A. Sample Calculations

   

    

 

1. number of grams of glacial acetic acid in sample solution (preextraction)             

5. number of grams extracted using second method

     

 

2. number of grams of glacial acetic acid in sample solution (single ether addition)        

6. concentration of acetic acid in water (first method)      

3. number of grams of glacial acetic acid in sample solution (double portioned ether addition)

7. concentration of acetic acid in ether (first method)       B. Set-Up Used in the Experiment 8. concentration of acetic acid in water (second method)       9. concentration of acetic acid in ether (second method)       V.
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11. Distribution Coefficient of Second Method

1. Separatory Funnel for Extraction1

References

10. Distribution Coefficient of First Method

LBYCH37 Experiments, Chemistry Department, De La Salle University 2 Acetic Acid Wikepedia http://en.wikipedia.org/wiki/Acetic_acid 3 Liquid Liquid Extraction Wikipedia http://en.wikipedia.org/wiki/Liquidliquid_extraction

I hereby certify that I have given a substantial contribution to this report and I did not copy and/or quote from any resource material unless being cited as reference. I am made known that failure to accomplish the second clause would be grounds for plagiarism and a failing grade in this final laboratory report.

Marvin Marqueta

Natasha Pauline Go