TABLE OF CONTENTS

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TITLE Abstract Introduction Objectives Theory Apparatus Procedure Results Calculation Discussion Conclusion & Recommendation References Appendix

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ABSTRACT

This experiment is conducted to achieve a few objectives, which are to determine the dissolved oxygen in water samples taken from different sources and to ascertain whether them comply with Malaysian Water Standard or not. In this experiment , manganese sulphate is added into the water sample.And then, water sample is titrated with sodium thiosulphate. After titrated, starch is added into the titrant. The titrant is titated again and amount of concentration dissolve oxygen is calculated. From this experiment, the concentration of dissolve oxygen in water sample that are tested for drain water is 0.18 mg/L , lake water is 2.20 mg/L , tap water is 2.52 mg/L and de-ionized water only is 0.7 mg/L dissolved oxygen. In conclusion, none of these four water samples are standardized with Malaysian Water Standard.

INTRODUCTION

Oxygen, (O) was initially discovered by Carl Wilhelm Scheele in the year of 1773 or earlier, and Joseph Priestly in1774. However, Priestly is often given priority because of his work was published first. The name oxygen was introduced by Antoine Lavoisier who discovered the phlogiston theory of combustion and corrosion. Oxygen, is the element in the group 16 (chalcogen group) and period 2 with atomic number of 8. The name was originated from the Greek oxys in which is sharp referring to the sour taste of the acids. At the standard temperature and pressure, two atoms of the element combine to form dioxygen with the formula of O2. This diatomic gas is a very pale blue in colour, odourless and tasteless. Oxygen is a highly reactive non metal element which can forms oxides with almost all other elements. Oxygen is also a strong oxidizing agent and has a high electronegativity of all elements after fluorine. On the other hand, oxygen is the third most abundant element in the universe only after hydrogen and helium. Oxygen saturation in the environment or environmental oxygenation refers to the amount of oxygen dissolved in the soil or the water bodies such as lakes and ponds. The environmental oxygenation is important to the sustainability of an ecosystem. Environmental hypoxia or insufficient oxygen in another term might occur in those water bodies tend to suppress the presence of aerobic organisms like fish. On the opposite site, anaerobic organisms in water, may lead to the fish killed and other adverse events. The method of water aeration was used to perform oxygenation. For instance, Chicagos Rivers South Branch or Bubbly Creek in Chicago, Illinois was deficient in oxygen because of an open sewer by the Chicagos meat packing industry. The water was oxygenated by introducing compressed air into its water, thus, increase the fish population. Dissolved Oxygen (DO) analysis was used to indicate the amount of oxygen dissolved in an aqueous solution,. Supersaturation occur if the concentrations of oxygen in water exceed 110%. Concentrations above this level are harmful to the aquatic life. Fish in water that contains excessive DO may suffer with gas bubble disease. However, this case happens very rarely. The bubbles of oxygen or emboli block the flow of blood through blood vessels causing death of fish. External bubbles or emphysema can also occur and be seen on fins, skins and other tissues. Moreover, aquatic invertebrates are also affected by gas bubble disease but at levels higher than those lethal to fish. Therefore, an adequate DO is necessary for good water quality.
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OBJECTIVES

The objectives of this experiment are : to determine the dissolved oxygen in water samples taken from different sources to ascertain whether them comply with Malaysian Water Standard or not

THEORY

The main objective of this experiment is to determine the dissolved oxygen (DO) level in a series of water samples and ascertain whether they comply with Malaysian Water Standards. In order to do so, the Winkler test is used to determine the concentrations of DO inside these water samples. The test was developed by Ludwig Wilhelm Winkler while working at Budapest University in the year of 1888. Through photosynthesis, phytoplankton and macroalgae present in the water produce oxygen. Meanwhile, bacteria and eukaryotic organisms such as zooplanktons, algae and fish consume this oxygen through cellular respiration. Therefore, the results of these two mechanisms will determine the concentration of DO inside the water. The first step in the Winkler test is adding an excess of manganese (II) salt and an iodide (I-). Therefore, 48% of the total volume of manganese (II) sulphate and potassium iodide (15% in potassium hydroxide 70%) is used to be added to create a brown precipitate. In this alkaline solution, DO will oxidize manganese (II) ions into a tetravalent state. The brown precipitate formed is the MnO(OH)2. 2 MnSO4(s) + O2(aq) 2 MnO(OH)2(s) Equation 1

The next step is to add a strong acid to acidify the solution. In this reaction, the precipitate will dissolve back into solution. The addition of sulphuric acid is shown as below: MnO(OH)2(s) + 2H2SO4 Mn(SO4)2 + 3H2O Equation 2

In this acidic medium, the Mn(SO4)2 will converts the iodide ion into an iodine. On the other hand, Mn(SO4)2 itself is reduced into manganese (II) ions. The reaction is shown below: Mn(SO4)2 + 2 I-(aq) Mn2+(aq) + I2 (aq) + 2 SO42-(aq) Equation 3

At the next stage, 2 mL of starch indicator was added to detect the presence of iodine. Addition of sodium thiosulphate must be done by titration method. The conical flask should be placed on top of a sheet of filter paper. The solution was titrated until the blue colour turned clear. This indicates that there is no iodine left inside the solution anymore. The equation that involved is as follow: 2 S2O32-(aq) + I2(aq) S4O62-(aq) + 2 I-(aq) Equation 4

Each 1ml of thiosulphate titre is equivalent to 0.1mg of oxygen in the 10ml subsample. Thus 1ml of thiosulphate is equivalent to 1mg oxygen per 100ml fresh water. The sample calculation is shown in the next page.

Sample calculation Range (mg/L)=volume of titrant(mL) 0.02 When volume of titrant is 9ml, Range (mg/L) = 9mL 0.02 = 0.18 (under range)

APPARATUS AND MATERIALS

Apparatus: 1. Conical flask 2. Water Sampling Bottle or BOD bottle 3. Direct reading titrator 4. Measuring cylinder 5. Beaker 6. Dropper Materials:
1. Drain, lake, tap and de-ionized water

2.

Alkaline Potassium Iodide Azide

3. Manganese (II) sulphate 4. Sodium thiosulphate 5. Starch indicator solution 6. Sulphuric acid

PROCEDURE

1. Lake water was fully filled into BOD bottle. It was ensured that there are no air bubbles present inside the bottle. This steps was better to be done at sink area to avoid spillages of the sample water. 2. Next, the manganese (II) sulphate and alkaline potassium iodide azide was added into the BOD bottle that contain lake water. 3. BOD bottle was closed with its cap and inverted twice.

4. The solution was inverted again after several seconds. 5. The precipitate formed that was collected at the bottom of the container was observed and the changes in colour are recorded. 6. Then, sulphuric acid was added into the solution. The BOD bottle was shook until the sulphuric acid was dissolved completely in the solution. 7. The colour of the solution was observed and recorded. 8. The solution was taken with the volume of 100 mL and placed in another conical flask by using measuring cylinder. 9. Starch indicator with the volume of 2 mL solution was added into the solution. The dark blue solution was form. 10. Next, by using direct reading titrator, the sodium thiosulphate solution was added into the solution. The volume of sodium thiosuphate needed to change the colour of the solution from dark blue to colourless was recorded. 11. The data was collected and recorded. 12. The step of 1 to 11 was repeated by using the different water sample which is drain water, tap water and de-ionized water.

RESULTS

Water Sample

Concentration of dissolved oxygen

Observation

Conclusion

Drain water

9 0.02=0.18(under range)

white percipitate formed Orange brown colour

A little oxygen present

Lake water

110 0.02=2.20(between range)

turns into yellowish colour Orange brown colour

Oxygen present

Tap water

126 0.02=2.52(between range)

turns into dark yellow colour

Oxygen present

De-ionized water

70 0.01=0.70(under range)

White percipitate formed

A little oxygen present

Table 1: Shows the amount oxygen dissovled in water sample

CALCULATIONS

Range (mg/L) = volume of titrant(mL) 0.02 When volume of titrant is 9ml, Range (mg/L) = 9mL 0.02 = 0.18 (under range)

DISCUSSION

Oxygen saturation or dissolved oxygen (DO) is a relative measure of the amount of oxygen that is dissolved or carried in a given medium. There are three common methods for measuring DO. The first and most reliable is the Azide-Winkler titration method, against which the others are compared to test for accuracy. However, this method also requires the most training and the use of some strong chemicals. For these reasons, it is not often used in citizen monitoring programs. The second and probably most common method is the use of a DO probe and meter. DO can also be measures with field kits. The Winkler test is used to determine the concentration of dissolved oxygen in water samples. DO is widely used in water quality studies and routine operation of water reclamation facilities. An excess of manganese(II) salt, iodide (I) and hydroxide (OH) ions is added to a water sample causing a white precipitate of Mn(OH)2 to form. This precipitate is then oxidized by the dissolved oxygen in the water sample into a brown manganese precipitate. In the next step, a strong acid (either hydrochloric acid or sulfuric acid) is added to acidify the solution. The brown precipitate then converts the iodide ion (I) to iodine. The amount of dissolved oxygen is directly proportional to the titration of iodine with a thiosulfate solution. In the first step, manganese(II) sulfate is added to an environmental water sample. Next, alkali-iodide-azide is added. The floc is observed to appear in the water sample. The floc is in orange-brown colour, indicating the presence of dissolved oxygen. In the alkaline solution, dissolved oxygen will oxidize manganese(II) ions to the tetravalent state. 2 MnSO4(s) + O2(aq) 2 MnO(OH)2(s) There is some confusion about whether the oxidised manganese is tetravalent or trivalent. Some sources claim that Mn(OH)3 is the brown precipitate, but hydrated MnO2 may also give the brown colour. 4 Mn(OH)2(s) + O2(aq) + 2 H2O 4 Mn(OH)3(s) In the next step, a strong acid (either hydrochloric acid or sulfuric acid) is added to acidify the solution. The precipitate will dissolve back into solution. The brown precipitate

then converts the iodide ion (I) to iodine. The acid facilitates the conversion by the brown, Manganese-containing precipitate of the Iodide ion into elemental Iodine. Mn(SO4)2 + 2 I(aq) Mn2+(aq) + I2(aq) + 2 SO42(aq) The stabilized water sample is then titrated with sodium thiosulfate and turns pale yellow. When the starch solution is added, blue or purple coloration will be formed. We continue to the titration until the solution turns colourless or clear which indicates the endpoint of the titration process. 2 S2O32(aq) + I2 S4O62(aq) + 2 I(aq) From the experiment, the water sample is analyzed using Winkler method described above. The water sample was analyzed immediately as bacterial action may react with the dissolve oxygen content in water. As the reagents were added, the tip of the transfer pipettes was just kept below the surface of water to prevent penetration of more oxygen from the air into the sample. From the experiment we conduct, in drain water sample, it is observed that white precipitate is formed before sulphuric acid is added indicate no or little amount of oxygen is present. After titration with sodium thiosulfate, the amount of oxygen is 0.18 which fall under range of oxygen content which is from 2.00 to 10.00. For lake water sample, the floc of orange brown color turns yellowish color indicating the presence of oxygen. It is calculated that the amount of oxygen is 2.20 which fall between ranges of oxygen content. While for tap water, the floc of orange brown color turns dark yellow also indicating the presence of oxygen. It is calculated that the amount of oxygen is 2.52 which also fall between ranges of oxygen content. In de-ionized water, it is observed that white precipitate is formed which indicates no or a very little presence of oxygen. Based on calculation, we obtained the amount of oxygen to be 0.70 which fall under range of oxygen content. It can be considered that the water sample from the tape water and lake water obeyed the Malaysia standard of water quality. Hence the water sample is considered to have high concentration of dissolved oxygen and therefore, high productivity and less polluted.
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Nevertheless, there are some errors may be made during the experiment. In my opinion, the value of dissolved oxygen obtained from the water sample can become not precise due to the presence of air bubbles inside the water sample when it is filled in the BOD bottle. There is also little air bubbles present in the delivery tube, which results in the inaccuracy of the amount of dissolved oxygen. Other than that, the starch solution added may also not be of accurately 1 ml for each drop.

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CONCLUSIONS & RECOMMENDATIONS

The amount of dissolved oxygen in water sample drain and deionized water is 0.18 and 0.70 which both fall under range of oxygen content. While tap and lake water samples 2.20 and 2.52 which fall in range of oxygen content. So, dissolved oxygen level in a series of water sample in tap and lake water obeyed the Malaysia Water Standards because it fall between ranges. Hence the water sample is considered to have high concentration of dissolved oxygen and therefore, high productivity and less polluted. A few recommendations is suggested on the techniques employed during the experiment. First, during the step of filling the sample water into the conical flask, we must make sure that there is no bubble present inside the container. The present of air bubble which contain oxygen can make our results to be not accurate. This problem can be overcome by letting the sample water to be flow for a few second to make sure the container are fully filled by the sample water. Second, after the sample water was mixed with manganese (II) sulphate and potassium iodide azide, the solution must be inverted many times until the solute was surely dissolved and form a certain precipitate. This important step also needed to apply during the mixing of the solution with sulphuric acid. After that, during the titration step, the colour changes of the solution must be observes carefully to avoid excess addition of sodium thiosulphate into the solution. This problem can be preventing by using filter paper for easier to detect the colour changes of the solution. Also, for future studies, it is recommended for student must be used latex glove and goggle to avoid the harmful chemical substances to be contact with eye or skin.

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REFERENCES

Brown, T. L., LeMay, H. E., Bursten, B. E., & Murphy, C. J. (2009). Chemistry The Central Science. NJ: Pearson Education, Inc.

Chang, R. (2010). Chemistry Tenth Edition (10th Edition ed.). Singapore: McGraw-Hill

Thierry Labasque, Christian Chaumery, Alain Aminot, Gilles Kergoat, Spectrophotometric Winkler determination of dissolved oxygen: re-examination of critical factors and reliability, Marine Chemistry, Volume 88, Issues 1-2, August 2004, Pages 53-60, ISSN 0304-4203, 10.1016/j.marchem.2004.03.004.

Roberto DAutilia, Margherita Falcucci, Vincent Hull, Luisa Parrella, Short time dissolved oxygen dynamics in shallow water ecosystems, Ecological Modelling, Volume 179, Issue 3, 30 November 2004, Pages 297-306, ISSN 0304-3800, 10.1016/j.ecolmodel.2004.02.009.

M.B. Lakin, Chemical catalyst interference in the winkler titration determination of dissolved oxygena method for correction, Water Research, Volume 10, Issue 11, 1976, Pages 961966, ISSN 0043-1354, 10.1016/0043-1354(76)90073-7.

Irja Helm, Lauri Jalukse, Martin Vilbaste, Ivo Leito, Micro-Winkler titration method for dissolved oxygen concentration measurement, Analytica Chimica Acta, Volume 648, Issue 2, 26 August 2009, Pages 167-173, ISSN 0003-2670, 10.1016/j.aca.2009.06.067.

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APPENDICES

Sample calculation Range (mg/L)=volume of titrant(mL) 0.02 When volume of titrant is 9ml, Range (mg/L) = 9mL 0.02 = 0.18 (under range)

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EXPERIMENT 4: BASIC WATER PROPERTIES 1

Oxygen saturation or dissolved oxygen (DO) is a relative measure of the amount of oxygen dissolved in a medium. DO is naturally present in water and tends to be manipulated in order to suit spesific applications; in drinking water a higher DO level improves the taste, but at the expense of higher rates of pipe corrosion, consequently industry tends to minimise the DO level to reduce maintenance costs.

You are required to determine the DO level in a series of water samples and ascertain whether they comply with Malaysian Water Standards.

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