Lab Report Format CHEM 155 Instrumental Analysis Prof. Terrill Page 1 of 5 Reports will have 8 sections with the following weights: 1 – Cover page 02 2 – Abstract 13 3 – Introduction 15 4 – Experimental 15 5 – Analysis, Results and Discussion 15 6 – References 10 7 – Figures and Tables 15 8 – Appendix 15 Total 100 points 1. Cover page: 1.1. Title 1.2. Your name 1.3. Your partner’s name 1.4. Course 1.5. Professor Terrill 1.6. Date Submitted 2. Abstract: In a few short sentences convey (a) the general idea of the experiment, (b) what was done and how including important details such as the wavelengths used and (c) the final results, including errors (σ) and detection limits where appropriate. The boxes below contain some key points that I look at when scoring the reports! Idea, experiment, critical details, Zn results, errors, Fe results, errors, mg/pill units?, expected values, validations, detection limits, wavelength, stationary phase, mobile phase 3. Introduction: This is a summary of the analysis. 3.1. It should include a short description of the analytes – what they are why they are there and why it is important to know how much of these analytes are present in your sample. 3.2. A discussion of the instrumental method that you are using should also be included. Discuss how the instrument works and focus on the principles of the detection or separation e.g. the absorption of light by gas phase atomic analytes or the partitioning of analytes from a solution (mobile phase) to a stationary phase. 3.3. Mention the various experimental parameters that influence the performance of the instrument and why – e.g. flame stoichiometry or mobile phase composition, wavelength etc. C:\SJSU\Teaching\155\2005A spring\Report formats with comments saved.doc Page 1 of 5 Lab Report Format CHEM 155 Instrumental Analysis Prof. Terrill Page 2 of 5 4. Experimental 4.1. Instruments and Materials: (A) List the name and manufacturer of the instruments you used, e.g. “Unicam 929 AA spectrometer…” (B) Next, list the reagents that you used, including the water. It is acceptable to indicate that these were obtained from the SJSU Chemistry Service if more detailed information is not available. Indicate the manufacturer and the purity where available (e.g. with the concentrated acids since they contain trace metal impurities). Column type, flame type, stationary phase etc. 4.2. Procedure: In this section, Sample, standard, validation, & buffer describe what you did in such a preparations. way that another chemist could look at it and reproduce your UV-Vis experiment (HPLC) work. It is not a set of step-bystep instructions – but rather a Implementation of HPLC – flow rate, concise description of what you pressure, injection volume, injection actually did. For example: “The time, sample vials, injection order. calibration primary standard (1002.3 PPM) was prepared by dissolving 1.0023g of Co metal in yy mL of HNO3 (conc.), and diluting to 1.000 L with distilled water. Validation standards were similarly prepared to yield two, 500mL solutions of qq and zz PPM” “The working standards were prepared by serial dilution of the standards in the following way… The concentrations are listed in Table 1.” The standard concentrations and signals will be tabulated in the results section – see the below for details. Important experimental parameters used should be mentioned here. For example “For the FAAS analysis, an Air-acetylene flame source, hollow cathode lamp radiation source and a wavelength of xxx.x nm were employed ”. A common mistake is to claim that your standards are 10 ppm when they are actually 10.1 because the primary calibration standard was based on 101 mg instead of 100. I encourage you to make tables in this section – just state that a certain general procedure was used and then give the details in the table. This is much easier to real than a litany of repetitious sentences describing essentially the same thing but Tottering only in one or two numbers. C:\SJSU\Teaching\155\2005A spring\Report formats with comments saved.doc Page 2 of 5 Lab Report Format CHEM 155 Instrumental Analysis Prof. Terrill 5. Analysis, Results and Discussion: Describe the results of your measurements in words and figures. 5.1. Refer to the various numbered figures (spectra, chromatograms or graphs) and tables in turn and discuss the results. Where possible, you explain (a) why the results are what they are and (b) what they mean and (c) how you used them. Don’t forget to mention relevant measurements such as the UV-Vis absorbance spectra and retention times for the HPLC experiment. Page 3 of 5 UV-vis results, Calibration, linear regression and error calculations, problems in chromatogram or with spectrometer. Sample-sample variation versus standard deviation estimate based on calibration curve. Agreement with expectation – is difference between expected value and measured value larger than the standard deviation. This question applies to both the validations and the samples. What does this mean? Comments on chromatogram – elution order, resolution etc. 5.2. Make a table of absorbance and concentration values including the appropriate uncertainties for all of your samples, calibration and validation standards. I include an example for the FAAS experiment below: Table 1. Absorbance Data Sample 1 2 3 4 Validation 1 Validation 2 Spinach • • C [PPM] 1.23 4.45 10.2 20.2 12.2 9.23 ---------- Absorbance Note in this section if any of the calibration data were thrown out! Note whether the validation data were in agreement with the calibration or not. According to the validation standards, how accurate are the results? 5.3. Make a calibration graph from your analyte absorbance values as illustrated below. It can be on a separate page. All the points are shown, including the regression line, validations, and the sample absorbance is indicated with a horizontal line intersecting the calibration line. The uncertainty of the sample absorbance (if known) is indicated by two parallel lines drawn at the sample absorbance plus and minus the C:\SJSU\Teaching\155\2005A spring\Report formats with comments saved.doc Page 3 of 5 Lab Report Format CHEM 155 Instrumental Analysis Prof. Terrill Page 4 of 5 standard deviation in the sample absorbance. Your experimental uncertainty may be too small to do this graphically, but it illustrates nicely the way that the uncertainty in the sample absorbance propagates into an uncertainty in the sample concentration. You may be able to address the question of whether this instrumental method is suitable in terms of detection limit for the given analysis 5.4. Finally, discuss the least-squares (linear regression) analysis. Note that this implies that you are fitting the data to a model, e.g. A = m*C[PPM] + Sb. Report the best-fit sensitivity, m, and blank signal, Sb and their respective uncertainties. Put the actual regression and propagation of error calculations in the appendix. 5.5. Do not forget to list the final results of the analysis here. This means the amount of the analyte that is in a meaningful amount (e.g. a serving) of the original sample, e.g. 4 grams of spinach or 12 ounces of diet coke. Compare this value to what is expected for this product. 5.6. Make it clear that you understand the results. Discuss the relative value of the validation versus random errors. Do sample-to-sample variations swamp the calculated standard deviations and if so, what does this mean? 6. References: List the references here that correspond to the numbered citations in the text. Please cite at least one source relating to the analytical method used other than the textbook for the class and one relating to either a. the general importance of analyzing for the particular analyte(s), or b. the particular problem of measuring, e.g. Fe using FAAS. All references included should be cited in the paper. Web URL’s do not count. 7. Tables and Figures: Put the titled and numbered tables and figures together, in order immediately following the references. Mainly, this is a place to summarize the results. Please only put here the figures and tables that you produce, not the ones that the instrument makes. Finally, every figure that you put here should be referred to in the text. All figures must be clearly labeled. Avoid dark backgrounds and unnecessary information. Neat hand work on figures is perfectly acceptable. 8. Appendix: Put your calculations here. Neat handwork is fine – but I expect to see samples of all the important calculations that you performed. If you used a computer program (e.g. Microsoft Excel) please print out a report from the program illustrating the results. I do not expect anyone to do the linear regression by hand! Your legible notebook carbons may suffice for the experimental parts here. C:\SJSU\Teaching\155\2005A spring\Report formats with comments saved.doc Page 4 of 5 Lab Report Format CHEM 155 Instrumental Analysis Prof. Terrill Page 5 of 5 9. An example of a calibration curve showing the sample absorbance (and confidence intervals or standard deviations) along with validation points is below. Your graph does not need to look identical to this one. Primary Calibration Standards First Validation Standard Second Validation Standard Digested Spinach Sample 0.5 Absorbance 0.4 0.3 0.2 0.1 0.0 0 2 4 6 8 10 12 14 16 18 20 Mg Concentration [PPM] C:\SJSU\Teaching\155\2005A spring\Report formats with comments saved.doc Page 5 of 5