S10. DETERMINATION OF SODIUM AND POTASSIUM IN BEER BY FLAME PHOTOMETRY. PURPOSE To analyse samples of beer for their sodium and potassium content, using a flame photometer. INTRODUCTION Flame photometry is a technique that uses the measurement of emitted light from a sample in a flame as a measure of how much analyte is present. This is the reverse of what happens in AAS, where the amount of light absorbed is measured. Flame photometry needs no lamps. It only needs town gas and a supply of compressed air, plus a simple power point. Its disadvantage is that it can be used for only a very few metals. The internal standard method may be of use in overcoming variations in flame conditions. The internal standard chosen should have properties similar to the element being analysed but should not be present in the sample. When graphing the results using the internal standard the ratio of the analyte to the internal standard is plotted against the concentration of the analyte PREWORK Calculate the concentration of an intermediate standard which would be used to prepare the following standard series and how it could be prepared from a stock solution of 1000mg/L . The formula C1V1= C2V2 will be of use for this calculation 1. 100 mL of calibration standards containing 1, 5, 10 and 20 mg/L Na using dilutions of 1, 5, 10 and 20 mL of the intermediate solution. 2. 100 mL of calibration standards containing 5, 10, 20 and 50 mg/L K using dilutions of 2.5, 5, 10 and 25 mL of the intermediate solution. PROCEDURE I. Sample and standard preparation 1. Prepare the Na and K intermediate standards as per Prework 1 and 2 2. Obtain about 50 mL of beer. De-gas this by pouring from one beaker to another a number of times and then place the beaker in an ultrasonic bath for 5 minutes 3. Prepare 100 mL of Na calibration standards as per Prework 1, and label them Flasks A, B, C and D. 4. Prepare 100 mL of each of the following MIXED sodium/potassium/ lithium standards. Aliquots of each metal are pipetted into ONE flask! Use the intermediate sodium and potassium standards and the 1000mg/L lithium standards Solution Blank Flask 1 Flask 2 Flask 3 Flask 4 Volumes (mL) Na intermediate 0 1 5 10 20 K intermediate 0 2.5 5 10 25 1000 mg/L 5 5 5 5 5 5. Pipette 5 mL of the 1000mg/L Li stock solution and 10 mL of degassed beer into a 100 mL volumetric flask, and make up to the mark with de-ionised water. General instrument set-up for flame photometry • Turn on the compressed air and then the gas. Light the flame using the ignition switch on the instrument. • While aspirating water through the capillary tube, adjust the gas/fuel mixture so that sharp blue cones are formed at the burner holes. • Insert the correct filter for the element you are reading • Aspirate the most concentrated standard, and set the instrument to give a convenient reading by selection of the appropriate range (100 is a useful number but it does not matter where you start). Wipe the capillary with a tissue then rinse with water before placing in another solution. • Aspirate the blank and set the zero with the zero or blank control. Recheck the top standard, then the blank again until the readings are steady. • Read and record all solutions, rinsing well with water and the next solution between each reading. • Aspirate water to rinse out the instrument before turning if off. • Turn off the gas first followed by the air. II. Direct intensity method for determination of sodium 6. The teacher will demonstrate the method of set up for the flame photometer available in your laboratory. Use the blank to set the zero value and the 20 mg/L Na standard to set the 100 (or an appropriate) emission value. 7. Aspirate standards A-D and the diluted sample and record the sodium emission value. Between each sample, ensure that you aspirate some deionised water to flush the system. III. Internal standard method for determination of Na and K 8. Set the zero with the blank 9. Using flask 4, set the sodium emission to 100 (or an appropriate value) 10. Aspirate each standard and sample, reading the emission intensities for Na and Li by moving the filter selector. Do not adjust the sensitivity dials for lithium, simple record the number. 11. Repeat steps 8-10 for K (and also Li) in place of Na IV. Evaluation of matrix effects on emission intensity 12. Record the emission intensities for sodium of the following solutions, which will be provided: 10 mg/L Na, 10 mg/L Na + 10 mg/L K; 10 mg/L Na + 100 mg/L K. Use the 10 mg/L sodium solution to set the instrument to 100. CALCULATIONS Graphing emission intensities against concentration will often result in curves not straight line plots. To overcome this problem it may be necessary to plot the log of the intensity against the concentration. If this does not ‘straighten’ the curve you may need to consult your teacher. 1. For the direct intensity set of results, plot the emission intensity against the concentration of Na in the standards. 2. If the line is not linear, you will need to plot the log of the intensity against concentration. 3. Read the Na value for the sample from the graph. 4. Correct the Na value by the dilution factor. 5. For the internal standard method calculate the following ratios: 6. Plot the ratio against the concentration 7. If the line is not linear, you will need to plot the log of the ratio against concentration 8. Read the values for Na and K of the appropriate graph 9. Correct the value for the dilution factor. DISCUSSION • compare the Na results to each other • evaluate which method (direct intensity or internal standard) should be more accurate • comment on preparing a mixed standard with both Na and K as compared to separate standards • comment on the reason for the different intensity values for the sodium solution in Part IV QUESTIONS 1. Why are flame photometers only built for analysis of Na, K, Li and occasionally Ca? 2. Flame photometers are relatively inexpensive because they do not contain a monochromator to separate the radiation into its different wavelengths. How does the photometer distinguish between the light emitted by Na, K and Li (ie what does the switch between the three elements do)? 3. Explain why flame temperature variations cause problems in flame emission instruments, but not in AAS. S10. RESULTS SHEET Date of analysis II. Direct intensity for determination of sodium Conc Na Emission intensity log emission intensity 0 1 5 10 20 Beer III. Internal standard method for determination of Na and K Na Conc Na Int Li Int Na Int/ Li Int K Int Li Int K Int/ Li Int 0 1 5 10 20 Beer K Conc 0 5 10 20 50 Beer IV. Evaluation of matrix effects on emission intensity Solution Na intensity 10 mg/L Na 10 mg/L Na + 10 mg/L K 10 mg/L Na + 100 mg/L K Have you? Date Signature Completed the instrument log Completed the sample register Completed the standard register Teachers signature