Name: Hazel Dawn B.

Patica Date Performed: September 8,2011 Date Finished: September 1, 2011

Experiment #9: Spectrophotometric Determinations Abstract The students conducted their ninth experiment which is the Spectrophotometric Determinations.Spectrophotometic Determination is an analytical technique which involves the determination of the concentration of solutes in a solution by measuring the amount of light absorbed or transmitted by the solution. The whole class was divided into three groups and were asked to prepare their standard solution using the serial dilution technique .The experiment has two parts namely the standardization and the analysis of unknown. I. Objectives

The objectives of this experiment is to make a regression analysis and generate the equation of the best fit line by plotting absorbance versus concentration and to form the equation of the best fit line for the unknown sample and determine its K2Cr2O7 concentration. II. Apparatus

The apparatuses used in this experiment are 100 mL volumetric flask, UV Visible Spectrophotometer, glass cell and pipette.

III.Chemicals The chemicals that were used in the experiment are: H2O It is a liquid, colorless, odorless. Its melting point is 0C and boiling point is 100C. It can burn the skin if it exceeds 100C. K2Cr2O7 It is orange-red crystalline solid . Its melting point is 398C and its boiling point is 500C. It is toxic if swallowed , inhaled or absorbed through the skin , corrosive and may produce eye damage. IV.Summary of Procedures Preparation of Standard Solutions

Prepare 1000 ppm K2Cr2O7 by dissolving 0.1 gram in 100 mL H2O. Prepare 100 ppm solution by diluting 25 mL of original solution. Prepare 80 ppm solution by diluting 200 mL of previous solution . Prepare 60 ppm solution diluting 15 mL of previous solution. Prepare 20 ppm solution by diluting 125 mL of previous solution. Identification of Wavelength of Maximum absorbance Fill a glass cell (cuvette) with the prepared solution. Measure absorbance at different wavelength over the range 400-800 nm. Identify the wavelength of maximum absorbance from the spectrum solution. Generation of the Standard Calibration curve and Analysis of an Unknown sample. Set the spectrophotometer to Photometric mode. Get the absorbance of each of the standard solution prepared . Plot

Data and Discussion Weight of crucible: 1st weighing 35.9515g 2nd weighing 35.9510g Wt. of crucible with precipitate #67 - 36.5448g # 61 36.0551g Run wt. Sample 0.5088 0.5059 Constant wt. crucible 36.4395 35.9510 Wt. residue 0.1053 0.1041 %FeO(OH) Ave. S RSD

1 2

23.03% 22.90%

22.97%

0.0919

4.0019

Sample Calculations:

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Interpretation: Based on the data obtained, the researcher had achieved an RSD which lies on the acceptable value. It indicates that the measurements obtained were precise. Error Analysis: The researcher cites the possible reasons on why encounter errors in the experiment performed. There are inevitable incidents wherein the crucible comes contact with moisture, thus making large gap between the measurements. Such incidents are the contact of the skin and the crucible and uncareful handling of the crucible after it was brought out the desiccator. The procedures were also a bit confusing thats why we cant proceed on our own. We did almost the entire experiment with our instructor behind us, instructing our every move. I. Conclusion:

The obtained % FeO(OH) values are 23.03% and 22.90%. The researcher did run 2 wherein she yielded 22.90% as her % FeO(OH). For the s and RSD, the obtained values are 0.0919 and 4.0019 respectively. This experiment entails accuracy and keen understanding of the nature of the whole experiment prior to its actual conduct on the laboratory so that errors are maximize and achieving accurate and precise measurements would be possible. II. Reference: p.34, Fundamentals of Analytical Chemistry 8th Edition by Skoog West, Holler and Crouch

Absorbance vs Concentration
0.45 0.4 0.35 0.3 0.25 0.2 0.15 0.1 0.05 0 0 20 40 60 80 100 120

20 40 60 80 100

0.11336 0.1971 0.2705 0.3555 0.3821

400 1600 3600 6400 10000

2.2672 7.884 16.23 28.44 38.21

0.124568 0.194144 0.26372 0.333296 0.402872

-0.011208 0.0030 0.0068 0.0222 -0.0208

-0.15036 -0.06662 0.00678 0.09178 0.11838

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