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Atomic Spectroscopy
(a) In terms of spectral shape, how are atomic spectra different from molecular spectra? What is the source of this difference?
(b) Describe the decision-making process for picking a line for atomic emission analysis of a given analyte.
(c) For quality assurance, spike recovery is not sufficient to establish confidence in an analytical procedure. Explain this statement. What should be done instead to demonstrate satisfactory performance of an instrumental method (including elemental analysis).
(d) Find a literature example of atomic spectroscopy used for elemental analysis. State the operating conditions with sufficient detail to reproduce the analysis;
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- As a forensic toxicologist, you have been given a task on determining amount of cadmium, mercury, chromium, copper and lead metal contents in medicinal herbs using flame atomic absorption spectroscopy (AAS). Hollow cathode lamp (HCL) was selected as radiation source for this analysis. The highest concentration came from lead element followed by chromium and copper, however cadmium and mercury were not detected in the sample. a) Based on your knowledge, conclude whether the above result is valid or not. b) If you are given an option of electrothermal or flame atomizer for above case study, determine which one is suitable and justify your answer.Exactly 5.00 mL aliquots of a solution containing analyte X were transferred into 50.00-mL volumetric flasks and the pH of the solution is adjusted to 9.0. The following volumes of a standard solution containing 2.00 µg/mL of X were then added into each flask and the mixture was diluted to volume: 0.000, 0.500, 1.00, 1.50 and 2.00 mL. The fluorescence of each of these solutions was measured with a fluorometer, and the following values were obtained: 3.26, 4.80, 6.42, 8.02 and 9.56, respectively. ii. Using relevant functions in Excel, derive a least-squares equation for the data, and use the parameters of this equation to find the concentration of the phenobarbital in the unknown solution.The determination of iron in wines was carried out by atomic absorption spectrophotometry, using the standard addition method. To do this, 10 mL of wine were placed in five 50 mL volumetric flasks; then 0, 5, 10, 15 and 20 mL of a 10 ppm iron standard solution were added to each of them. Next, they were gauged with distilled water and the absorbance was measured, obtaining the values of 0.040, 0.062, 0.081, 0.102 and 0.125 respectively. Calculate the regression parameters and obtain the iron concentration in the wine, in µg / mL.
- 0.1120 g of a solid sample containing copper was dissolved by acid and transferred to a 250.00 mL volumetric flask and volume was made up with distilled water. The solution was then diluted by a factor of 25. The final solution was analyzed by atomic absorption spectrophotometry and the concentration was found be 2.982 ppm, What is the weight percentage of copper in the original solid sample? Keep four significant figures in your final answer.To quantify the Cadmium content in a water sample, 5 aliquots of 10 mL were taken, adding to each one of them a volume of a standard solution of Cd (2 mg / mL); after the addition the final volume for all solutions was 50 mL. The absorbance reading was taken in an Atomic Absorption spectrophotometer, the data recorded were: Aliquot 1 2 3 4 5 Cd solution (mL) 0 1 2 3 4 Absorbance 0.163 0.240 0.319 0.402 0.478 Calculate the ppm of Cd.The validation process comprises four main steps that are : hardware validation, software validation, method validation and system suitability. To evaluate a spectrophotometer’s accuracy by measuring absorbance, a solution of 60.06 mg/L K2Cr2O7 in 0.0050M H2SO4 was carefully prepared together with a 0.0050 M H2SO4 as a reagent blank. If the spectrometer’s signal is properly calibrated, it has been reported that this solution should provide an absorbance of 0.640 +- 0.010 at wavelength 350 nm. Which one of the validations mentioned above had been involved in this process? Explain your choice
- Quinine in a 1.553-g antimalarial tablet was dissolved in sufficient 0.10 M HCl to give 250 mL of solution.A 10.00-mL aliquot was then diluted to 50.00 mL with the acid. The fluorescence intensity for the dilutedsample at 347.5 nm provided a reading of 196 on an arbitrary scale. A standard 100-ppm quinine solutionregistered 125 when measured under conditions identical to those for the diluted sample. Calculate the massin milligrams of quinine in the tablet.Assume for the following situations that Beer’s law remains linear. For (a) and (b), indicate whether the extinction coefficient ε, path length b, or concentration C is changing, and how it will change the absorbance of the solution. (a) A sample is moved from a test tube that is 1.0cm wide to a test tube that is 1.5cm wide. (b) A sample is diluted by adding enough solvent to double its volume. (c) A solution of iron (III) chloride appears brown when in high enough concentrations. In a 1.0 cm cuvet, the absorbance of 334 nm light by a 5.4 × 10−4 M solution of FeCl3 is measured to be 1.05. What is the extinction coefficient of the FeCl3 complex at this wavelength? (d) A sample containing an unknown concentration of FeCl3 is measured to have an ab- sorbance of 0.43 at 334 nm in a 1.0 cm cuvet. What is the molar concentration of the solution?A 10.00-g sample containing an analyte was transferred to a 250-mL volumetric flask and diluted to volume. When a 10.00-mL aliquot of the resulting solution was diluted to 25.00 mL it was found to give a signal of o.235 (arbitrary units). A second 10.00-mL aliquot was spiked with 10.00 mL of a 1.00- ppm standard solution of the analyte and diluted to 25.0o mL. The signal for the spiked sample was found to be o.502. Calculate the weight percent of analyte in the original sample.
- Quinine in a 1.939-g tablet was to be analyzed by dissolving it with 0.10 M HCl to a final volume of exactly 500 mL. This solution was diluted by adding 50.00 mL to a 100.0 mL flask and diluting to the mark. Afterwards the fluorescence intensity was found to be 394 in arbitrary units. Under identical experimental conditions, a standard 150.0-ppm had an intensity of 184.Quinine in a 1.939-g tablet was to be analyzed by dissolving it with 0.10 M HCl to a final volume of exactly 500 mL. This solution was diluted by adding 50.00 mL to a 100.0 mL flask and diluting to the mark. Afterwards the fluorescence intensity was found to be 394 in arbitrary units. Under identical experimental conditions, a standard 150.0-ppm had an intensity of 184. Calculate the number of milligrams in the original sample.(5) A sample of sodium phosphate is dissolved in water to give 100.00 mL of solution (Solution A). Then this solution is diluted 5 times to give the final solution (Solution B). Solution B is Known to contain 3.920 x 1022 number of PO43- ions, which has an absorption peak at 460 nm and absorbance value of 0.355 in a 1.000 cm cuvette. (i) Calculate the molar absorptivity of Solution B. (ii) What mass of sodium phosphate (MM 163.94 g/mol) dissolved in Solution A.Quantitative Analysis by External Standard Method Calcium in a juice sample is determined by atomic absorption spectrophotometry. A stock solution of calcium is prepared by dissolving 1.834 g of CaCl, 2H20 in water and diluting to 1000.0 mL. A substock calcium solution was prepared by transferring 10.00 mL of the stock to a 100.00 mL volumetric flask and diluting to the mark. Three standard solutions of calcium were prepared by transferring 2.500 mL. 5.00 mL and 10.00 mL of substock to 50.00 mL volumetric flasks and diluting to the mark. The sample is prepared by transferring 1.000 mL of fruit juice from the original bottle to a 25.00 mL flask and diluting to the mark. Strontium chloride is added to all solutions before dilution to avoid phosphate interference. Instrumental response of the standards is measured against the blank, and the following readings are recorded: 9.10, 18.6 and 37.0. The sampie reading is 28.1. Using the multipoint method, find the concentration of calcium in…