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PURPOSE: The purposes of this experiment are to demonstrate that it is possible to precipitate an ionic substance in water by addition of another chemical and to analyze the precipitate formed using a gravimetric method. 2. PROCEDURE: 1. We measure 150 mL portion of the water sample provided to you and pour it in a 250 mL volumetric flask. 2. We add 3 mL HCl to the water sample to adjust the pH to between 4.5 and 5.0. At this point if pH meter is not available you can check the pH with methyl red indicator solution. 3. We heat the solution to boiling and, while stirring gently, add 10 mL warm barium chloride solution slowly until precipitation appears to be complete. 4. We digest the precipitate at 80-90C for not less than 2 hours. 5. We filter by using ashless filter paper and wash the precipitate with several portions of hot distilled water. 6. We dry and ignite the residue and the filter paper at 800C for at least 30 minutes. We do not allow the filter paper to flame. 3. THEORY: Sulfate (SO42-) can be found in almost all natural waters. There are several other sources of sulfate in water. Decaying plant and animal matter may release sulfate into water. Numerous chemical products including ammonium sulfate fertilizers contain sulfate in a variety of forms. The treatment of water with aluminum sulfate (alum) or copper sulfate also introduces sulfate into a water supply. Human activities such as the combustion of fossil fuels and sour gas processing release sulfur oxides to the atmosphere, some of which is converted to sulfate. (URL 1) Sulfate is generally considered to be non-toxic. The consumption of drinking water containing high amounts of magnesium or sodium sulfate may result in intestinal discomfort, diarrhea and consequently dehydration. This laxative effect is often observed when someone drinks water that contains greater than 500 milligrams per liter (mg/L) of sulfate. Over time, individuals appear to develop a tolerance to higher concentrations of sulfate. Diarrhea and dehydration are often observed when individuals accustomed to drinking water with low concentrations of sulfate consume water with high amounts of sulfate. It is not advisable to use water that contains high concentrations of sulfate for infant feeding. (URL 1) Sulfate is important in both public and industrial wastewater supplies because of tendency of waters containing appreciable amounts to form hard scales in boilers and heat exchangers. Sulfate is considerable concern because it is indirectly responsible for two serious problems. They are odor and sewer-corrosion problems. (Sawyer et al., 2003, p.670) Odor Problems: SO42- + organic matter S2- + H2O + CO2 (with anaerobic microorganisms)

H2S (g) HS- + H+ HS- S2- + H+

pKa1=6.91 pKa2=14.0

At pH values 9 and above, odor problem is minimal. At pH levels below 9, significant odor problem occurs if sulfate reduction yields significant amount of sulfide ion. Concentrations in air above 20 ppm should be avoided because of toxicity. (Sawyer et al., 2003, p.670) Corrosion of Sewers: When, wastewater temperatures are high, residence time in the sewers is long and sulfate concentrations are considerably high then, crown-corrosion of concrete sewer systems can be an important problem. Although the reduction of sulfate to H2S is hard to occur, the crown-corrosion is often linked to H2S. Actually, H2S is a weaker acid than carbonic acid and has little effect on good concrete. Nevertheless, crown-corrosion in gravity type sewers occur and H2S is indirectly responsible. (URL 2) (Sawyer et al., 2003, p.673)

Gravimetric Method of Determination of Sulfate: Gravimetric analysis is a four-step process: 1) Completely precipitate the desired component of a soluble compound as a compound of known composition. 2) Separate the precipitate from the solution by filtration.

3) Burn off the filter paper without a flame in a way which either does not change the composition of the precipitate or which changes it in a known way. 4) Weigh the precipitate and calculate the amount of the component in the original sample. Sulfates vary widely in their solubility in water, but barium sulfate is almost completely insoluble. Therefore, if a soluble barium compound, such as BaCl2 , is added to a solution containing a sulfate, essentially all the sulfate is removed from solution as a precipitate of barium sulfate: BaCl2 + SO42- BaSO4 + 2ClAlthough it is not a reactant, hydrochloric acid is added to the reaction mixture for two reasons: 1) It prevents the precipitation of other barium compounds which would have given interference in the determination. 2) It helps, along with heating, in the formation of larger crystals in the BaSO4 precipitate - which makes filtration easier. The precipitate is removed from the surrounding solution via an ashless filter paper -- the paper leaves no ash behind when it is burned off. (URL 3) Interference: The gravimetric determination of SO4 is subject to many errors, both positive and negative. In potable waters where the mineral concentration is low, these may be of minor importance. Interferences leading to high results suspended matter, silica, BaCl2 precipitant, NO3- . Interferences leading to low results alkali metal sulfates (URL 4)

4. DATA ANALYSIS AND CALCULATIONS: Sample: 150 mL tap water Table 1. Data table: Crucible Tare weight(gr) 19.1553 After ignition (gr) at 800C 19.1745

Sulfate ion concentration can be found the equation below. SO4= mg/L= (mg BaSO4*411.5)/mL sample BaSO4 mg= 19.1745-19.1553=0.0192 g *1000=19.2 mg SO4= mg/L= (19.2 mg*411.5)/150 mL=52.672 mg/L 5. DISCUSSION AND CONCLUSION: 1. Gravimetric analysis means using the special laboratory scales to find out the gross weight (sample + tare) and the tare weight. It is very important to know how to use the

scales correctly, and not to think that it is simple. We should remember, once again, that weighing is the starting point in analytical chemistry for all other operations and so it is obviously vital not to let error creep in at this stage. To use the scales you should do as follows: put the scales on a flat, non-vibratory surface in a room where the temperature and humidity levels are constant, away from direct sources of heat, taps or anything else that could interfere with the weighing process; keep the scales level i.e. the platform need to be parallel to your work surface (adjust the micrometric screws at the bottom); keep the pan and the rest of the scales clean; check frequently that the tare weight is the same as that certified by the manufacturers; never weigh things directly in the pan, but always use containers like beakers etc. as a tare; never weigh objects or substances while hot but always cool them down in a nonhumid environment (dessicator); correct weight for air current affecting light but voluminous objects.(URL 5)

2. Sulfates are considerable concern because they are indirectly responsible for two serious problems often associated with the handling and treatment of wastewater. They are odor and sewer corrosion problem result from the reduction of sulfates to hydrogen sulfide under anaerobic conditions. The amount of sulfates in wastewater is a factor of concern in determining the magnitude of problems that can arise from reduction of sulfates to hydrogen sulfide. For example knowledge of sulfates content of the sludge or waste fed to digestion units provides a means of estimating the hydrogen sulfide content of the gas produced. From this information, the design engineer can determine whether scrubbing facilities will be needed to remove hydrogen sulfide and size of the units required. (URL 6) 3. Acid rain is the wet or dry deposition of acidic substances and their precursors on the Earth's surface. Wet deposition refers to RAIN, SNOW, HAIL, drizzle and other familiar forms of visible precipitation. Dry deposition, mostly invisible, occurs through gravitational settling of large particles and uptake of gases and small particles at the Earth's surface. Rain and other precipitation may be defined as acidic or alkaline (basic) depending on chemical composition. The degree of acidity is usually measured on the pH scale, a logarithmic measure of the concentration of hydrogen ions (H+) in precipitation. A neutral solution has a pH of 7. Acidic solutions have values below 7 and basic solutions have values above 7. For each change of one pH unit, the hydrogen ion content changes by a factor of 10. A clean water sample in equilibrium with atmospheric carbon dioxide will have a value of 5.6 and this is often used as a definition of "clean" rain. When values are different from this, it means that other substances, either natural or man-made, are present in the rain. Current annual measurements of the average pH of precipitation in the northern hemisphere range from about 4.0 to 7.0. The lower, highly acidic values occur primarily over and immediately downwind of urban and industrialized areas in North America, Europe and Asia. Higher pH values in precipitation are found over less industrialized regions where the atmosphere contains larger amounts of alkaline dust. The primary cause

of low pH in precipitation over northeastern North America is sulfuric acid (H2SO4) resulting from industrial and urban emissions of sulfur dioxide (SO2). (URL 7) 4. Suda slfat genellikle yksek konsantrasyonlarda bulunabilir, nk kayalardan zeltiye geen katyonlar genellikle slfatla, znebilen bileikler verirler. Yurdumuzda TS 266 da ime suyu standardnda 200 mg / lt msaade edilebilen deer, 400 mg / lt maksimum deer olarak limitlendirilmitir. Birok Avrupa devletinde. Kanada 'da ve Dou Amerika'daki sularda slfat konsantrasyonu 20 - 50 mg / lt dir. Avrupa'nn 23 byk kentinde kullanma sularndaki ortalama slfat konsantrasyonu 64 mg / lt dir. ngiltere sularnda ki SO4 miktar ise 4 - 303 mg / lt arasnda bulunmutur. Su tasfiyesinde flokulant olarak kullanlan alminyum slfat k suyunda litrede 25 - 50 mg slfat ihtiva ederler. Normal su tasfiyesi ile giderilemez. Avrupa'daki ie sularnda ortalama slfat konsantrasyonu 223 mg / lt dir. (URL 8) Therefore, our sample is good for drinking because max level for sulfate concentration for drinking water 400 mg/L but our samples sulfate concentration is 52.672 mg/L. 6. REFERENCES: 1. URL 1. Sulfate, retrieved 23 December 2012 from,

2. URL 2. Sulfate, retrieved 23 December 2012 from, 4c57a69edd.pdf 3. URL 3. Quantitative Analysis of a Sulfate, retrieved 23 December 2012 from, 4. URL 4. Standard Methods for the Examination of Water and Wastewater, retrieved 23 December 2012 from, 5. URL 5. Retrieved Dec,24,2012 from 6. URL 6. Retrieved Dec,24,2012 from 7. URL 7. Retrieved Dec, 24, 2012 from 8. URL 8. Retrieved 24, Dec, 2012 from 9. Sawyer ,C.N., McCarty, P.L., Parkin , G.F., Chemistry for Environmental Engineering and Science 5th edition, The McGraw Hill Companies, New York, 2003 pp. 670-676