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TABLE OF CONTENTS 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 ABSTRACT.............................................................................................................. INTRODUCTION..................................................................................................... AIMS......................................................................................................................... THEORY................................................................................................................... APPARATUS AND MATERIALS.......................................................................... PROCEDURE........................................................................................................... RESULTS.................................................................................................................. CALCULATIONS..................................................................................................... DISCUSSIONS..........................................................................................................

10.0 CONCLUSION.......................................................................................................... 11.0 RECOMMENDATIONS............................................................................................ 12.0 REFERENCES.......................................................................................................... 13.0 APPENDIX...............................................................................................................

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1.0 ABSTRACT Spectroscopy is a technique that uses the interaction of energy with a sample to perform an analysis. The data that is obtained from spectroscopy is called a spectrum. A spectrum is a plot of the intensity of energy detected versus the wavelength of the energy. In this experiment, the spectrophotometer was used to determine the concentration of Chromium (VI) via the absorption. Chromium is a chemical element which has the symbol Cr and atomic number 24. It is the first element in Group 6. It is a steely-gray, lustrous, hard metal that takes a high polish and has a high melting point. It is also odorless, tasteless, and malleable. Chromium does not occur freely in nature. The main chromium mineral is chromite. As was mentioned earlier, chromium compounds can be found in waters only in trace amounts. The element and its compounds can be discharged in surface water through various industries. It is applied for example for metal surface refinery and in alloys. Stainless steel consists of 12-15% chromium. Chromium metal is applied worldwide in amounts of approximately 20,000 tons per year. It may be polished and it does not oxidize when it comes in contact with air. Chromium may be present in domestic waste from various synthetic materials. Through waste incineration it may spread to the environment when protection is insufficient. 2.0 INTRODUCTION In this experiment, the spectroscopy was used to determine the concentration of Chromium (VI) via the absorption. Spectroscopy is the study of the interaction between matter and radiated energy. Historically, spectroscopy originated through the study of visible light dispersed according to its wavelength. Later the concept was expanded greatly to comprise any interaction with radiative energy as a function of its wavelength or

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frequency. Spectroscopic data is often represented by a spectrum, a plot of the response of interest as a function of wavelength or frequency. Chromium metal is used in for a large variety of applications ranging from an additive in the manufacture of stainless steel to chromium plating. It is used for motorcycle exhausts and some older types of car bumpers to the colourisation of Rubies and Emeralds. Chromium metal has a more important use, it is a very hard transition metal and is normally amalgamated with titanium to make replacement hips in the USA and UK. Chromium compounds (such as Chromic acid) are used in the electroplating industry as both an additive and (in the case of Chromic acid) as a highly powerful oxidising agent. Chromic acid is roughly 3 times as powerful an oxidising agent as sulphuric acid due to the oxidising power of the Chromium (VI) it self. With all industrial processes, a waste product is inevitably formed. In the Chromium industries (plating and manufacturing), it is normally the Chromium (VI) compound (such as chromic acid and other high oxidizing Chromium (VI) cleaners). As was mentioned earlier, chromium compounds can be found in waters only in trace amounts. The element and its compounds can be discharged in surface water through various industries. It is applied for example for metal surface refinery and in alloys. Hexavalent chromium has been detected in groundwater across the United States due to industrial and military operations, including plating, painting, cooling-tower water, and chromate production. Because inhalation of Chromium (VI) can cause lung cancer in some persons exposed to a sufficient airborne concentration, questions have been raised about the possible hazards associated with exposure to Chromium (VI) in tap water via ingestion, inhalation, and dermal contact. Although ingested Chromium (VI) is generally known to be converted to Chromium (III) in the stomach following ingestion, prior to the

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mid-1980s a quantitative analysis of the reduction capacity of the human stomach had not been conducted. The water sample will be analyzed by the spectroscopy in order to get the absorbance value. From the result we can calculate the concentration of Chromium (VI) and know whether the water sample is suitable for drinking or other uses.

3.0 AIMS I. II. To determine the concentrations of Chromium (VI) by absorption of spectroscopy. To determine the quantity of Chromium (VI) present in water sample by using spectroscopy. III. To determine whether the water sample is suitable for drinking or agricultural purposes. IV. To demonstrate the proper method of preparing a stock solutions in the range of 15 to 300 parts per million (p.p.m) to be used in the calibration of the spectroscopy.

4.0 THEORY Chromium occurs naturally as a trace component of most crude oils, and the concentrations of chromium found in residual and distillate oils have been measured. Available information suggests that the chromium is emitted in the trivalent state from oil combustion, sewer sludge incineration, cement production, municipal waste incinerators, and refractories. Chromium is used for corrosion resistance, steel production, and as protective coating for automotive and equipment accessories. It is a permanent and stable inorganic pigment used for paints, rubber, and plastic products. Chromium has also been detected but not quantified in motor vehicle exhaust by the Air Resources Board (ARB).

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Chrome plating is a source of Chromium (VI) emissions in the state. Chrome electroplating operations are conducted in baths containing chromic acid and during the plating process, bubbles of gas are emitted through the surface of the bath. These bubbles carry entrained Chromium (VI) into the air. Chromium emissions can occur from Chromium (VI) firebrick lining of glass furnaces. Although it is a minor source of emissions, the most commonly seen hexavalent chromium is lead chromate. Lead chromate is the pigment in the yellow paint used to mark traffic lanes. In addition, hexavalent chromium in water solution is converted through electroplating (decorative chrome plating) to the bright metallic chromium coating seen on plastic or metal products such as shower heads or car bumpers. Although not commonly seen by the general public, one of the most important uses of chrome plating is to apply a hard, smooth surface to machine parts such as crankshafts and printing rollers. This process is known as "hard" chrome plating. Chromic acid anodizing is another industrial metal finishing process which uses hexavalent chromium. Chromium that is deposited on highroads originated from brake and dusts and exhaust of automobile engine can unfavourably permeate into any water straems nearby via flowing rainwater. Lakes and water streams which is nearer a typical congested with automobiles areas are the most susceptible areas to be contaminated by such chromium. Due to its cancer-risk character and toxicity even at mere concentrations, a lot of federal environmental agencies are doing researches to determine its presence in many environmental samples. Thus, in this experiment absorption spectroscopy will be used to detect the concentrations of Chromium (VI) in a water sample. As a matter of fact, colored aqueous solutions have chemical species contents which absorb significant wavelengths of light. Similarly, heavy metals can be identified via absorptions of wavelengths of light. The amount of light absorbed is linearly proportional to the concentration of metal ions.

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Absorption spectroscopy operates on the measuring principle of light. Absorption spectroscopy refers to spectroscopic techniques that measure the absorption of radiation, as a function of frequency or wavelength, due to its interaction with a sample. The sample absorbs energy, i.e., photons, from the radiating field. The intensity of the absorption varies as a function of frequency, and this variation is the absorption spectrum. Absorption spectroscopy is performed across the electromagnetic spectrum. Absorption spectroscopy measuring priciple of light before and after it passes through an aqueous metal solution. The amount of light absorbed by the chemical species in the sample is equivalent to the difference in the amount of light before it enters the sample and after it exits the sample. For the purpose of light to be absorbed by chemical species, the light must be set to a specific wavelength. Every chemical species absorbs distinct wavelengths of light. In absorption spectroscopy, the wavelengths of light absorbed by the in solution are detected. In this experiment, standard stock solutions are prepared by diluting 300 parts per million (p.p.m) of Chromium (VI) standard solution Five standard stock solutions being prepared from the concentrated Chromium (VI) standard solution with range from 15 p.p.m to 300 p.p.m. To calculate the dilute solutions volume needed, the solution dilution formula can be used: M1V1 = M2V2 M 1 : is a concentration of standard Chromium (VI) solutions, which is 300 p.p.m. V1 : is volume of distilled water needed to dilute Chromium (VI) solutions M2 : is a concentration of stock solution of Chromium (VI) solutions, which are 15, 45, 75, 150 and 300 p.p.m.

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V2 : is a volume of volumetric flask which is 50mL Quantitative analysis using spectroscopy is based on Beer-Lambert Law. Beer-lambert Law states that absorbance value depends on total quantity of the absorbing compound in the light path through the cuvette. Thus, if we plot a graph of absorbance versus concentration of the compound solution, we get a straight line passing throught the origin. A compound w ith high molar absorbance is very effective at absorbing light. Hence, low concentrations of a compound and high molar absorbance can be easily detected by the spectroscopy.The Beer-Lamberts Law A = LC A : is absorbance value from the spectroscopy : molar absorbance (L/mol.cm) L : path length of the cuvette in which the sample is contained C : Concentration of the compound in solution (mol/L)

5.0 APPARATUS : 1. Spectrometer. 2. 10 mL of cuvette. 3. Pipette. 4. Dropper. 5. Measuring cylinder. 6. 50 mL volumetric flask. 7. Stopper. 8. Beaker.

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5.0 REAGENT: 1. Distilled water. 2. Stock solution of chromium (VI) solution (300ppm) 3. 5 set of diluted chromium (VI) solutions which are 300 ppm, 150 ppm, 75 ppm, 45 ppm and 15 ppm. 4. Lake Sample. 6.0 METHADOLOGY/ PROCEDURES: 1. All the materials and apparatus are setup. 2. The standard solutions of chromium are prepared with the different concentrations which are 300 ppm, 150 ppm, 75 ppm, 45 ppm and 15 ppm. 3. By using the pipette, 25 mL, 12.5 mL, 7.5 mL and 2.5 mL of chromium (VI) solution is taken and placed in the different volumetric flask and it labeled. All the preparations are conducted in the fume hood. 4. The volumetric flask is filled with the distilled water until it reaches the mark on the volumetric flask. 5. The volumetric flask is closed with the stopper and then shake 2 times or more to make the solution mix well. 6. The spectrometer is switched on. 7. 10 mL of distilled water is filled into the square cuvette and the placed in the spectrometer slot. Before that, make sure there are no bubbles in the cuvette because it can affect the reading of the absorbance. 8. To ensure the all data obtained are accurate, the zeroing step is done first. 9. The diluted solution which known as standard solution, is transferred into the square cuvette.

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10. After that, the cuvette is placed in the spectrometer slot. Before that, make sure the cuvette is cleaned from dirt and also fingerprint to avoid from error reading of absorbance of the solution. 11. The reading of absorbance is recorded and tabulated into a data. 12. After that, the water sample is filled into the cuvette and placed in the spectrometer slot to get the reading of absorbance. 13. All the data is recorded and analyzed.

7.0 RESULT: To dilute 50 mililiters standard solution of 300 p.p.m, the solution dilution formula is used in order to calculate the volume of Chromium (VI) solution. (M1)(V1) = (M2)(V2) (1) (300)V1 = (300)(50) V1 = 500 mL

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To dilute 50 mililiters standard solution of 150 p.p.m, the solution dilution formula is used in order to calculate the volume of Chromium (VI) solution. (M1)(V1) = (M2)(V2) (1) (300)V1 = (150)(50) V1 = 250 mL

To dilute 50 mililiters standard solution of 75 p.p.m, the solution dilution formula is used in order to calculate the volume of Chromium (VI) solution. (M1)(V1) = (M2)(V2) (1) (300)V1 = (75)(50) V1 = 12.5 Ml

To dilute 50 mililiters standard solution of 45 p.p.m, the solution dilution formula is used in order to calculate the volume of Chromium (VI) solution. (M1)(V1) = (M2)(V2) (1) (300)V1 = (45)(50) V1 = 7.5 mL

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To dilute 50 mililiters standard solution of 15 p.p.m, the solution dilution formula is used in order to calculate the volume of Chromium (VI) solution. (M1)(V1) = (M2)(V2) (1) (300)V1 = (15)(50) V1 = 2.5 mL

Concentration of Chromium (VI) solution (p.p.m) M1V1 = M2V2 (300)V1 = (300)(50) V1 = 50 mL

Absorbance value

0.763

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M1V1 = M2V2 (300)V1 = (150)(50) V1 = 25 mL M1V1 = M2V2 (300)V1 = (75)(50) V1 = 12.5 mL M1V1 = M2V2 (300)V1 = (45)(50) V1 = 7.5 mL M1V1 = M2V2 (300)V1 = (15)(50) V1 = 2.5 mL 0.074 0.127 0.185 0.396

Absorbance of lake water sample = 0.144

8.0 CALCULATIONS: For 300 p.p.m

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300 ppm = 300

= 0.300

50 mL Chromium solution n = MV = 0.30 (0.05 L)

= 0.05 L Chromium solution

= 0.015 g.mol Chromium

Mass = no of moles

molar mass = 0.780 g of Chromium

0.015 g.mol Chromium

Percentage of chromium = = =52% Actual Concentration = 300ppm x15% = 4500 x100

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For 150 p.p.m 150 ppm = 150 = 0.150

50 mL Chromium solution

= 0.05 L Chromium solution

n = MV = 0.15 (0.05 L)

= 0.0075 g.mol Chromium

Mass = no of moles

molar mass = 0.390 g of Chromium

0.0075 g.mol Chromium

Percentage of chromium = = =52% Actual Concentration = 150ppm x15% = 2250 x100

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For 75 p.p.m 75 ppm = 75 = 0.075

50 mL Chromium solution n = MV = 0.075 (0.05 L)

= 0.05 L Chromium solution

= 0.0038 g.mol Chromium Mass = no of moles molar mass = 0.198 g of Chromium

0.0038 g.mol Chromium

Percentage of chromium = = =52% Actual Concentration = 75ppm x15% = 1125 x100

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For 45 p.p.m

45 ppm = 45

= 0.045

50 mL Chromium solution

= 0.05 L Chromium solution

n = MV = 0.045 (0.05 L)

= 0.0023 g.mol Chromium

Mass = no of moles

molar mass

0.0023 g.mol Chromium Percentage of chromium =

= 1.196 g of Chromium

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= =52% Actual Concentration = 45ppm x15% = 675

x100

For 15 p.p.m

15 ppm = 15

= 0.015

50 mL Chromium solution

= 0.05 L Chromium solution

n = MV = 0.015 (0.05 L)

= 0.008 g.mol Chromium

Mass = no of moles

molar mass = 0.416 g of Chromium

0.008 g.mol Chromium

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Percentage of chromium = = =52% Actual Concentration = 15ppm x15% = 225 x100

A=lc 0.144 =( 435 10-9)(4.5)(c)

c = 73563.218 m c = 73.563

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Absorbance value againts concentration of Chromium solution

0.9 0.8 0.7 absorbance value 0.6 0.5 0.4 0.3 0.2 0.1 0 0 100 200 300 400 500 600 concentartion of Chromium solution (M)

Based on the graph, the value of the gradient is : m=

= =

= 0.0014 By interpolating graph, the equation of the linear line was given by as : Y = mX + C The y-intercept in the graph is 0.043, so, the value of C = 0.043. by substituting the value of , the equation is given as :

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Y = 0.0014X + 0.043 X=

By substituting the value of Y with the value of the absorbance of water sample, which is 0.144 abs, the equation is given as : X=

X = 72.14 X is equivalent to the concentration of Chromium (VI) contains in the water sample, which is 72.14 parts per million (p.p.m).

Percentage error = = = 98.06 % 100 %

100 %

Discussion A solution of Cr3+ is deep violet for example, and a trace of Cr3+ in the Al2O3 crystal structure gives ruby its beautiful red hue. Chromium readily forms a thin, adherent, transparent

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coating of Cr2O3 in air, making the metal extremely useful as an attractive protective coating on easily corroded metals. Chromium metal and the Cr2+ ion are potent reducing agents. The metal displaces hydrogen from dilute acids to form blue Cr2+ (aq), which reduces O2 in air within minutes to form the violet Cr3+ ion: 4Cr2+ (aq) + O2 (g) + 4H+ (aq) 4Cr3+ (aq) + 2H2O (l) Eooverall = 1.64V

Chromium (VI) compounds in acid solution are strong oxidizing agents (concentrated solutions are extremely corrosive), the chromium (VI) being readily reduced to chromium (III): Cr2O72- (aq) + 14H+ (aq) + 6e- 2Cr3+ (aq) + 7H2O (l) Eo = 1.33V

This reaction is often used to determine the iron content of a water or soil sample by oxidizing Fe2+ to Fe3+ ion. In basic solution, the CrO42- ion, which is a much weaker oxidizing agent, predominates: CrO42- (aq) + 4H2O (l) + 3e- Cr(OH)3 (s) + 5OH- (aq) Eo = -0.13V

The experiment was conducted to achieve a few of main objective in this experiment such as to determine the Chromium(1V)content which present in the water sample by using the spectrometer,to demonstrate the proper method of diluting solution to prepare of standard solution in the range 10 to 300 p.p.m and lastly to analyse wheter the water sample is suitable for drinking water and agriculture purpose. In chemistry,spectrophotometry is the quantitative measurement of the reflection or transmission properties of a material as a function of wavelength and the water sample.The water sample is used to examine the presence of chromium is assumed that to be contaminant,the source of the water sample is the source of water sample is located near a roadway where road users with automobiles use it every day. This is due to rivers, lakes and any water

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streams which are near to congested areas have the highest risk or most susceptible to contain heavy metals such as chromium itself and is then classified as contaminated water source. The first step in this experiment is to prepare 5 standard solution Cr(VI) standard solutions using serial method as mentioned in the theory section. The concentrations for standard 1, standard 2,standard 3, standard and standard 5 is 300 ppm, 150 ppm, 75 ppm, 45 ppm and 15 ppm respectively. The absorbance for each five standard solutions and the lake water sample is taken by using the spectrophotometer. The average absorbance is then calculated. A graph of the absorbance is plotted against the concentration of standard solutions. ( R e f e r s Graph 1.1 at results: Graph of absorbance Value versus Concentration of Chromium (IV) in p.p.m) . Linear regression analysis is performed in order to determine the linear best fit for the absorbance versus concentration data. The R2 value indicates how well the regression analysis fits the absorbance-concentration data. The closer the R2 value is to 1.00, the better the linear regression analysis has fit the data. Graph 1.1 in results show a graph of absorbance versus concentration of five standard solutions. The line determined from the regression analysis will be in the form of y = mx + b, where y is the absorbance value and x is the concentration of the solution. Algebraic substitution of the absorbance value (y) for the unknown metal solution into the linear regression equation for the line permits the determination of the concentration (x) of the unknown solution. For the lake water sample of a = 0.144.From the graph, the

concentration of chromium (IV) in water sample is 72.14 parts per million. The state and federal regulatory agencies consider that the chromium, chromium (VI) to be toxic at concentration levels > 0.0300 ppm. Natural waters whose chromium (VI) concentrations exceed 0.300 ppm may not be used for drinking water or for agricultural

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purposes. After doing some calculations based on the graph, the concentration of the simulated lake water sample is determined to be at 72.14 ppm which is not suitable for drinking water and for agricultural purposes. CONCLUSION From this experiment, it can be concluded that chromium (VI) are present in the sample water. By using the spectrophotometer, the concentration of chromium (VI) in the sample water is 72.14 ppm. Since it is above the level of standard allowed by the Malaysian Environmental Quality (Sewage and Industrial Effluents) Regulations of 1979 which is 0.01 ppm. Therefore, the water is concluded as contaminated and does not suitable for drinking or agricultural purposes. The experiment was successfully conducted. RECOMMENDATIONS A few recommendations are suggested on the techniques employed during the experiment. The techniques applied to measure a small volume of chromium (VI) might not be suitable. The most accurate apparatus to be used is a pipette. The volume inserted inside the pipette can be controlled more accurately rather than using measuring cylinders. Next, the square cuvette bottles must be cleansed and dried properly with a distilled water in order to avoid inaccurate contents of either standard solutions or the chromium solution. On the other hand, the square cuvette bottles must be held properly as any fingerprints or smudge imprinted on the outer surface of the cuvette can become unfavourably interference for the solutions to absorb wavelengths of light in the spectrophotometer. Also, for future studies, it is recommended to use a different approach such as the reading might not be accurate. Therefore, the person that handling the bottles must wear a pair of gloves throughout the experiment. In addition, this experiment must be repeated thrice to increase the accuracy of the reading. The average value can be obtained and much more convincing rather than doing an experiment without an average.

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REFERENCES 1. P. Religa, A. Kowalik, P. Gierycz, Application of nanofiltration for chromium concentration in the tannery wastewater, Journal of Hazardous Materials, Volume 186, Issue 1, 15 February 2011, Pages 288-292, ISSN 0304-3894,

10.1016/j.jhazmat.2010.10.112. 2. Brown, T. L., LeMay, H. E., Bursten, B. E., & Murphy, C. J. (2009). Chemistry The Central Science. NJ: Pearson Education, Inc. 3. S. Silberberg Martin, McGraw. Hill International Edition, Fifth Edition Chemistry The Molecular Nature of Matter and Change, 1221 Avenue of the Americas, New York, NY, 2009, pg 783-808 4. Wensheng Yao, Robert H Byrne, Determination of trace chromium(VI) and molybdenum(VI) in natural and bottled mineral waters using long pathlength absorbance spectroscopy (LPAS), Talanta, Volume 48, Issue 2, February 1999, Pages 277-282, ISSN 0039-9140, 10.1016/S0039-9140(98)00243-4. 5. Y.C. Sun, C.Y. Lin, S.F. Wu, Y.T. Chung, Evaluation of on-line desalter-inductively coupled plasma-mass spectrometry system for determination of Cr(III), Cr(VI), and total chromium concentrations in natural water and urine samples, Spectrochimica Acta Part B: Atomic Spectroscopy, Volume 61, Issue 2, February 2006, Pages 230-234, ISSN 0584-8547, 10.1016/j.sab.2006.01.007. 6. http://chemistry.about.com/od/analyticalchemistry/a/spectroscopy.htm 7. http://www.scribd.com/doc/39166236/Determination-of-Chromium-VI-Concentrationvia-Absorption-Spectroscopy-Experiment

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APPENDIX SAMPLE CALCULATION To dilute 10mL standard solution of 5.6 p.p.m, the solution dilution formula is used to calculate the volume of chromium(VI) solution. M1V1 = M2V2 Equation 3-3

M1 = concentration of the Chromium (IV) given = 156 p.p.m V1 = volume of Chromium (IV) required ti perform serial dilution M2 = concentration of serial dilution wanted V2 = standard volume for a volumetric flask used =50Ml

For concentration of 20ppm M1V1 = M2V2 ( 156 ppm ) V1 = ( 5.6 ppm ) ( 50 mL ) V1 = 0.32 mL

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Graph of Absorbance Value versus concentration of Cr(IV) in ppm

1.400 1.200 Absorbance Value 1.000 0.800 0.600 0.400 0.200 y = 0.0098x + 0.2009 R = 0.9971

1.180 0.999

0.762

0.375] 0.237
20.000 40.000 60.000 80.000 100.000 120.000 Concentration of Cr(IV) in ppm

0.000 0.000

Graph 3-2:Graph of absorbance value versus concentration of Cr(IV) in ppm From the graph 1.1, the equation of linear equation is given: Y=0.098X + 0.2009 Equation 3-4

The average absorbance value of water sample,0.389 is substituted to Y , therefore we will get the value of x, concentration of chromium(IV) contains in water sample: x = y 0.2009 0.098 = 0.389 0.2009 0.0098 = 19.19 Thus, the concentration of chromium(IV) solution in water sample is 19.19 parts per million.