Chemistry Lab Report 3

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Linfield College *

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Chemistry

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Dec 6, 2023

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Chemistry Lab Report Name: Lydia Whyte Date: November 1 Experiment #: 3 Title: Quantitative and Qualitative Analysis Purpose: To measure the quantity of a substance, present in a chemical compound via quantitative analysis, along with determining the identity of chemical substances through qualitative analysis. Procedure: Quantitative analysis 1: 1. Place test tube inside the inside empty beaker and place on balance. 2. Tare balance. 3. Add one gram of metal carbonate and record weight. 4. Tare balance and add sulfuric acid to the test tube. 5. Observe fizzing reaction. 6. Mix until the fizzing settles. 7. Place beaker on the balance and record the new mass (which will be the mass lost). Quantitative analysis 2: 1. Place crucible container on balance. 2. Add hydrate to the crucible. 3. Measure the mass of the hydrate on balance. 4. Place lid on crucible with the unknown hydrate placed on the Bunsen burner. 5. Heat crucible for 10 minutes, and hydrate will lose water. 6. Place crucible in desiccator to cool for 10 minuets. 7. Place crucible on balance and record mass. Qualitative analysis 1: 1. Begin with stationary phase by placing a piece of porous filter paper, then the mobile phase will follow by a liquid moving by capillary action up the surface of the paper. 2. Prepare mixture of amino acids; Aspartic acid, Histidine, Leucine, Phenylalanine, Proline, and Aspartame 3. Place cylindrical pours paper in beaker where it does not touch the sides. 4. Cover the top with foil until the liquid climbs from the mobile phase to the stationary phase (about an hour). 5. After an hour, flatten the paper and mark the solvent front grown. 6. Once it has had the chance to dry spray the paper with Ninhydrin, which will visualize the spots for us. 7. After colors have developed mark them and measure the distance each compound has traveled from the starting line. 8. Calculate the Rf values from each compound. Qualitative analysis 2:
Chemistry Lab Report 1. Apply sample to carbon adhesive tape. 2. Place sample on the platform in the sputter coat chamber. 3. Mount the two carbon rods into the sputter coat chamber. 4. Create vacuum in sputter coat chamber by closing the top. Press the open button then push down the current button to check vacuum. 5. Remove the samples from sputter coater and insert samples into SEM/EDX. 6. Create vacuum in SEM/EDX by operating on a computer under vacuum and cluck pump. From here we will observe the column pressure being added. 7. Adjust the gross and fine positioning of sample 1 and magnify view of sample 2. Data/Results/Calculations: Quantitative analysis 1: % CO2 in the sample= (Weight loss / Sample Weight) x 100 % CO2 = (0.7033 / 1.1809) x 100= 59.56% Compound Molecular Weight % CO2 Calculation CaCO3 100.09 44.01/100.09= 43.97% K2CO3 138.21 44.01/138.21= 31.84% Na2CO3 105.99 44.01/105.99= 41.52% Li2CO3 73.892 44.01/73.892= 59.56% The experimental loss of CO2 matches Li2CO3 exactly so we know that the unknown carbonate must be Li2CO3. Quantitative analysis 2: % H2O in the sample = (Weight loss / Sample weight) x 100 %H2O= 0.3748 / 2.4406 x 100= 15.36% Compound Molecular Weight % H2O Calculation AlCl3x6H2O 241.43 108.096/241.43=44.77% MgCl2x6H2O 203.301 108.096/203.301=53.17% Na2CO3x10H2O 286.15 180.16/286.15=62.96% BaCl2x2H2O 244.462 36.032/244.462= 14.74% The experimental H2O loss best matches that of BaCl2x2H2O, so the unknown hydrate must be BaCl2x2H2O. Qualitative analysis 1: Calculation of amino acid Rf values= Rf= distance amino acid moved / distance mobile phase moved Rf (Asp)= 18mm/74mm= 0.243 Rf(His)=22mm/74mm=0.297 Rf(Leu)=55mm/74mm=0.743 Rf(Phe)=51mm/74mm=0.689 Rf(Pro)=33mm/74mm=0.446 Rf component 1: 21mm/74mm= 0.283 Best matches with Rf value and color of Asp (0.243) Rf component 2: 50mm/74mm= 0.676 Bests matches with Rf value and color of Phe (0.689) Aspartame= Aspartic acid and Phenylalanine Qualitative analysis 2: Unknown 1- The SEM/EDX spectrum demonstrates the presence of the following elements; C, N, and O.
Chemistry Lab Report The unknown must be C7H3NO, since it is the only compound containing C, N, and O. Unknown 2- The SEM/EDX spectrum demonstrates the presence of the following elements: C, O, and Br. The unknown must be C2H5OBr since it is the only compound containing C, O, and Br. Conclusions: Quantitative analysis 1: Carbonate analysis By comparing the % of CO2 with other carbonate compounds we were able to understand that CO2 was lost in the experiment. Since in this specific experiment 59.56% of CO2 was lost we could compare that to known values and with an exact match we were able to determine that the unknown carbonate was LiCO3. Quantitative analysis 2: Hydrate analysis By comparing the % of H2O lost in other compounds we were able to conclude that the value obtained, 15.36%, was a best match of BaCl2x2H20. Qualitative analysis 1: Paper chromatography We were able to conclude that the two unknown amino acids in Aspartame were Phenylamine and Aspartic acid. We were able to determine this from the two Rf values calculated in the Data/Results/Calculations section. Qualitative analysis 2: Scanned electron microscopy The SEM/EDX spectrum was able to detect C, N, and O in the first unknown sample. When presented with the possible molecules it could be we were able to infer that it was C7H7NO because it contained all the elements that were found by the SEM/EDX. In the second unknown sample the SEM/EDX found C, O, and Br. From this we were able to infer that it was C7H5OBr due to it being the only compound containing all the components found in the SEM/EDX. Notes: - The bubbling from the mixture containing sulfuric acid and carbonate was due to Carbon Dioxide being given off in the chemical reaction. - The hydrate lost water because it was holding several moles of water per compound, and the heat resulted in the water being boiled off. - The desiccator has material on the bottom that will prevent water from being picked up. - The crucible can withstand large amounts of heat and will not crack. - Paper chromatography is used for dividing mixtures into individual compounds to allow us to analyze the individual components. - Ninhydrin will react with amino acids to form compounds and color them differently to help us analyze said amino acids. - The SEM scans a sample with focused beams of electrons, that will interact with the sample and synthesize signals consisting of information related to surface topography and the compounds found in the sample. All elements from B to U (besides H) can be detected by the EDX combined with the SEM. Sputter coating is used to make a specimen conductive while preventing the electron beam to charge the specimen by covering it with a thin layer of conductive material. If the EDX is used with a sample that has a low atomic number, then carbon coatings can be used.
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