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UMass Amherst CHEM 242 - Part 1 - Lab 4 lecture

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Part 1 (Lab 4 lecture)Lab report writingAcademic integrityWhy keep a laboratory notebook?Slide 5Laboratory notebookTitle / Abstract / IntroductionTitle: Specifies system and what is interestingSpring 2007 Vanadium titlesPart 2 (prior to lab 9)Slide 11Data analysisDiscussionGroup exercise #1Revision exercise #2Group exercise #2Part 1 (Lab 4 lecture)Lab report writing•Scientists read for content, not for pleasure–Content should be accessible, not obscured•People estimate quality of science from quality of writing–If you want your work to be read, make sure you are writing well•No work achieves its full potential without major revising–Generally needs external inputAcademic integrity•Copying of work is not permitted–Material cannot be copy verbatim from any source–No class materials may be shared electronically–You cannot share or use photocopies of the work of others•Violations will result in all parties involved being disciplinedWhy keep a laboratory notebook?•In scientific research (industry)The lab notebook is like a notarized document. If your work is not recorded in a signed lab notebook, it DID NOT HAPPEN, from a legal point of view.This has important legal ramifications when patents are issued, especially when priority is at stake and billions of dollars are on the line.Since many synthetic procedures are not out of a book, it will also provide a record of the steps necessary to make a product and to verify its nature, both for yourself and for your colleagues (should your actions ever be questioned).Why keep a laboratory notebook?•In this labUseful data is kept handy (MWs, mp’s/bp’s, hazards, etc.)Chance to envision the experiment in advance–Should have a schematic flow chart, not a 50-step procedure–Chance to consider what variables are crucial to successRecord of work actually performed–Value of your observations may only be obvious in hindsight–This way we know that you are not changing results to fit modelLaboratory notebook•Should be clear on tense–Flow chart: Add 350mg of Co complex and 140L of en to MeOH soln.–Record: 352 mg of CoCl3.6H2O (green powder, Aldrich, 98% purity) were added…•Should include variables crucial to success/failure–352 mg of CoCl3.6H2O (green powder, Aldrich, 98% purity) were added en masse to 5.0 ml of MeOH in a 25ml RB flask. 140. L of en (Sigma, 99.5%) were added dropwise over ~ 2 minutes, causing a little bubbling, and turning the solution from dark green to a medium purple. 4 chunks of a dull gray mossy zinc (TW: 117 mg, Alfa, 98%) were cleaned by swirling in 6N HCl for ~1 min, followed by three water rinses, one MeOH rinse, and air jet drying. No change in the color of the Zn was observed during the cleaning process. The Zn and a stirbar were added to the reaction mixture. The solution was refluxed over a sand bath (setting: 40) with the RB flask in contact with the sand with slow stirring (unable to create stable vortex at higher spin settings). A yellow solid began to appear at the top of the RB flask (outside of the liquid) after 40 min. After a total of 65 minutes of heating, the solution was directly quenched into an ice bath, allowed to cool for 7 min, and filtered through a 12 mm piece of filter paper (Fisher brand, pore size 6). A fine purple powder was obtained – no yellow solid was found in the filtrate, even after washing with cold 100% EtOH. The Zn chunks had a pitted look and a duller luster after the reaction.Title / Abstract / Introduction•Used to judge if full article will be read or not•Title: –Specifies system and what is interesting–Should make people want to read your article / report•Introduction:–Should answer question of why work was done–Should discuss the question being posed, and value of answer–May need to provide background information•Abstract:–Needs to be comprehensive in scope–Should only include the most essential results and conclusions–You have been asked to write an Introduction, not an AbstractTitle: Specifies system and what is interesting•Homochiral Coordination Polymer with Infinite Double-Stranded Helices •Photochemical Production of a Highly Reactive Porphyrin-Iron-Oxo Species •An Unusual 1D Manganese Azido Complex with Novel EO/EO/EO/EE Coordination Mode: Synthesis, Structure, and Magnetic Properties •Low-Temperature Spectral Observation of the First Six-Coordinate Nitrosyl Complexes of Cobalt(II) meso-Tetratolylporphyrin with Trans Nitrogen Base Ligands •Cyanide-Bridged WV-CoII Double-Zigzag Chain Based on an Octacoordinated W Precursor: Metamagnetism and Spin Canting •Deliberate Design of a 3D Homochiral CuII/L-met/AgI Coordination Network Based on the Distinct Soft-Hard Recognition PrincipleSpring 2007 Vanadium titlesA. Separation and Spectroscopic Characterization of the Four Common Oxidation States of VanadiumB. Contributions to the visible spectrum as a result vanadiums various oxidation statesC. Reduction of Vanadium and the separation of its oxidation states through ion exchange chromatographyD. Using Column Chromatography and UV-vis to separate and analyze oxidation states of VanadiumE. Separation of the multicolored oxidation states of Vanadium using a resin packed chromatographic columnF. separation of vandium’s oxidation states through ion exchange chromatographyG. Generation and separation of four oxidation states of Vanadium via ion exchange chromatographyPart 2 (prior to lab 9)Academic integrity•Copying of work is not permitted–Material cannot be copy verbatim from any source–No class materials may be shared electronically–You cannot share or use photocopies of the work of others•Violations will result in ALL parties involved being disciplinedData analysis•Convert primary (raw) data to a more useful form–Product mass (g) → Percent yield (%)–UV-vis max (nm) → crystal field gap (eV, kJ/mol, cm-1)–Absorbance (dimensionless) → concentration (M) or  (L mol-1 cm-1)–Diffraction peak position (°) → cubic lattice parameter (Å)–Chemical formula → inner sphere coordination environment–E° (V) → equilibrium constant (dimensionless)–Mass change (g) → effective magnetic moment (B)•Answer question: How far can my results be trusted?–What is the error for weighing samples?–What is the error in an IR measurement?–What is the error in a uv-vis measurement?–What is the error in an x-ray diffraction experiment?Discussion•Answer: What


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