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Experiment_2a.docx

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Department
Chemistry
Course
CHM4354
Professor
Don't Know
Semester
Winter

Description
Advanced InstrumentalAnalysis Laboratory CHM4116 Laboratory#2a ElementalAnalysis of Minerals by Inductively Coupled Plasma Optical Emission Spectrometry Nicholas Beach Abstract: Inductively Couple Plasma Optical Emission (ICP-OES) and Mass Spectrometry (ICP-MS) are continuously used for instrumental analysis. Here we attempt to undergo analysis of Chalcopyrite (CuFeS 2, Pyrite (Fe2 ), and a mineral mixture to determine their compositions using the ICP 2500 instrument. Portions of varying quantities are made for each of the three analytes of interest: 15 different mineral mixture samples, 4 different Chalcopyrite samples, and 4 different Pyrite samples. ICP takes the measured intensity, of the ejected photons from the excited analytes as they go to ground state, and calculates the concentration of the analyte present. Difference in response of the two elements to instrumental parameters such as RF power, nebulizer flow, and potential spectral interferences were also analyzed. %Chalcopyrite composition in the mineral mixture was found to be: 3.0mg portions (24.43%), 10.0mg portions (29.67%), and 50mg portions (27.52%). Variance increases as the inverse of the sample mass increases. Experimental: For method and procedure please refer CHM4116: Advanced Instrumental Analysis Laboratory manual. Pages 23-25 Instruments:  Mineral Mixture was heated using DigiPrep heat block  ICP 2500 was used to conduct spectral analysis of all samples  Samples were prepared using analytical balances for weight, and when necessary micropipettes Table.1: Mineral mixture Portion Mass of Mineral Mix Mass of Final solution Number (mg) (g) 1 3.0mg 50.13 2 3.0mg 50.74 3 3.0mg 50.73 4 3.0mg 50.45 5 3.0mg 50.10 6 10.0mg 50.49 7 10.0mg 50.75 8 10.0mg 50.33 9 10.0mg 50.46 10 10.0mg 50.43 11 50.0mg 50.10 12 50.0mg 50.72 13 50.0mg 50.35 14 50.0mg 50.28 15 50.0mg 50.29 **Please note: Prior to heating each digestion tube had 2mL and conc H3O and HCl added to them, and after heating they were brought to 50.0g with addition of necessa2y dH O Table.2: Cu Standard solution Portion Volume of 1000 ppm Mass of Final Solution Concentration (ug/g) number (g) (g) 1 0 50.88 0.00 2 0.1278 50.12 2.55 3 0.2699 51.1 5.28 4 0.49 50.03 9.79 **Please note: to each solution 1mL of conc HNO3& HCl and diluted to final concentration with necessary dH2O Table.3: Fe Standard Solution Portion Volume of 1000 ppm Mass of Final Solution Concentration (ug/g) number (g) (g) 1 0 49.95 0.00 2 1.32 50.43 26.17 3 2.68 50.25 53.33 4 5.24 50.37 104.03 **Please note: to each solution 1mL of conc HNO 3 HCl and diluted to final concentration with necessary dH2O Results: For Raw intensity data, please refer to “Raw Int” in the spreadsheet available to you in your inbox. Table.4: Calculated concentrations of samples Calculated Concentration Cu1 Fe1 Fe2 Cu2 1 0.212 ± 0.0125 1.042 ±0.9511 0.103 ± 0.2309 0.202 ± 0.0311 2 0.210 ± 0.0125 -0.010 ±0.9511 -0.210 ± 0.2309 0.211 ± 0.0311 3 0.225 ± 0.0125 0.906 ±0.9511 0.439 ± 0.2309 0.210 ± 0.0311 4 0.235 ± 0.0125 -1.071 ±0.9511 -0.263 ± 0.2309 0.170 ± 0.0311 5 0.233 ± 0.0125 1.051 ±0.9511 0.311 ± 0.2309 0.223 ± 0.0311 6 0.225 ± 0.0125 1.450 ±0.9511 0.162 ± 0.2309 0.290 ± 0.0311 7 0.195 ± 0.0125 1.913 ±0.9511 -0.113 ± 0.2309 0.199 ± 0.0311 8 0.225 ± 0.0125 -0.572 ±0.9511 0.073 ± 0.2309 0.237 ± 0.0311 9 0.221 ± 0.0125 1.042 ±0.9511 0.303 ± 0.2309 0.229 ± 0.0311 10 0.207 ± 0.0125 -0.092 ±0.9511 0.042 ± 0.2309 0.218 ± 0.0311 11 0.156± 0.0125 -0.455± 0.9511 -0.502± 0.2309 0.216 ±0.0311 12 0.138± 0.0125 0.716± 0.9511 -0.219± 0.2309 0.128 ±0.0311 13 0.127± 0.0125 1.387± 0.9511 -0.491± 0.2309 0.163 ±0.0311 14 0.113± 0.0125 0.217± 0.9511 -0.712± 0.2309 0.146 ±0.0311 **Please note: this is only a fraction of the original data set of 125 measurements Percent composition of chalcopyrite: Sample %Chalcopyrite S02 S m2 Ss2 X cp 3.0mg Portions 24.43% ± 1.15% 1.42 0.100
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