Calculate: Retention factor (k), Separation factor (α), and Resolution (R) for slide 29. Comment on how these may be adjusted to give optimum values.
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- h) i) j) Ph + НО OSI(CH3)3 Br PPH3 1) "BuLi /THF/rt / 1.5 h H CH3 homo /rt / 1 h 2) -Si(CH3)3 OCH3 TiCl4 CH₂Cl₂/-78°C / 15 min PPh3/1₂ (1 eq) imidazole / THE 0°C-itA solution of volume 1 mL, containing an equal parts mixture (by weight) of aspirin and paracetamol (acetaminophen), was analysed by HPLC, displaying peaks at retention times 1.5 mins (area integration 1500) and 2.0 mins (area integration 2500). An unknown solution, also volume 1 mL, was analysed under the same conditions and, among a number of other peaks, there was one at 2.0 mins (area integration 4000). (i) How can the 2.0 min peak in the unknown sample be confirmed as paracetamol? (ii) In a subsequent analysis, 5.0 mg of aspirin was dissolved in the unknown solution and an extra peak appeared in the HPLC at 1.5 mins (area integration 2000). Assuming the 2.0 min peak confirmed as paracetamol, determine its concentration (g L-¹) in the unknown sample and estimate the error in the determination.A 5.00 mL sample of white vinegar is diluted in acetone and analyzed by GC-TCD using 1-propanol as internal standard and a ZB-Wax20 M Column. The most retained component in the analysis is: а. Acetone O b. Methanol с. 1-propanol d. Formic Acid О е. Асetic Acid
- A student researcher performed a chromatographic separation of caffeine and aspartame. The retention time for caffeine, tc, was found to be 209.6 s with a baseline peak width, w., of 14.4 s. The retention time for aspartame, ta, was 260.0 s with a baseline peak width, wa, of 21.2 s. The retention time for the unretained solvent methanol was 49.2 s. Calculate the average plate height, H, in micrometers for this separation, given that it was performed on a 22.1 cm long column. H = um %3D Calculate the resolution, R, for this separation using the widths of the peaks. R = Calculate the resolution if the number of theoretical plates were to increase by a factor of 2. R2N =A 5.00 ml sample of white vinegar is diluted in acetone and analyzed by GC-TCD using 1-propanol as internal standard and a ZB-Wax20 M Column. The most retained component in the analysis is: O a. Methanol Ob. Acetic Acid Oc Formic Acid Od. Acetone O e. 1-propanolThe method of internal standard was used to analyze and measure the concentration of chemical X by GC A known mixture of compounds X and Y (internal standard) gave the following chromatographic results: Compound X Y a) 2.0 x 106 M b) 8.4 x 10-7 M c) 6.6 x 10-7 M Concentration (M) 6.3 x 10-8 2.0 x 10-7 d) 4.1 x 10-7 M e) 2.9 x 10-7 M Peak Area Then, an unknown was analyzed as follows. 3.0 mL of unknown X was treated with 0.100 mL of 1.6 x 10-5 MY and the mixture diluted to 10.0 mL final volume. Peak areas were 633 (for X) and 520 (for Y). What is the concentration of X in the unknown. (The original 3.00 sample?) 395 787
- The data in the following table were extracted from a gas chromatographic analysis of a two- component mixture. Air nonane decane Retention time (s) 5 26 32 Peak width, baseline (s) 5 4 (i) Calculate the capacity factor, k, for the two compounds. (ii) Calculate the selectivity factor, a, for the two compounds.Tim is interested in analyzing for Pyraclostrobin (pesticide) in strawberries using QuECHers method for extraction and clean up before analysis with HPLC-uv. The concentration of the Pyraclostrobin in the fruits that he sampled is thought to be between 1-10 ng pesticide per g fruit fresh weight. The HPLC-uv instrument he is using has a LoQ of 5 ppb for Pyraclostrobin. Tim is starting out with 500 mg of the sliced fruitResearchers used gas chromatography to determine the % v/v methyl salicylate in rubbing alcohol [Van Atta, R. E.; Van Atta, R. L. J. Chem. Educ. 1980, 57, 230-231]. A set of standard additions was prepared by transferring 20.00 mL of rubbing alcohol to separate 25 - mL volumetric flasks and pipeting 0.00 mL, 0.20 mL, and 0.50 mL of methyl salicylate to the flasks. All three flasks were diluted to volume using isopropanol. Analysis of the three samples gave peak heights for methyl salicylate of 57.00 mm, 88.5 mm, and 132.5 mm, respectively. Determine the % v/v methyl salicylate in the rubbing alcohol.
- The concentration of acetylsalicylic acid in an antipyretic tablet was determined by HPLC using a normal calibration curve. Standard solutions of acetylsalicylic acid were prepared and analysed using a 10µL loop. The results obtained for the standards are tabulated below: Conc. of Acetylsalicylic Acid (ppm); Signal (arbitrary units) 50; 6352 100; 12869 150; 19175 200; 25536 250; 31936 To determine the concentration of acetylsalicylic acid in an antipyretic tablet, 10 tablets were weighed (6.500 g total) and crushed to a fine powder using a mortar and pestle. A quantity of powder equal the mass of one tablet was added to a 100 mL volumetric flask. The tablet powder was dissolved with 20 mL of methanol and the flask was made to volume using water. The solution was filtered. A 1.000 ml aliquot was transferred to a 10 ml volumetric flask, which was then made to volume with water. Analysis was conducted using a Bio Sil HL C18, 250mm x 4.6mm column; 5um, with a mobile phase of acetonitrile:…3. This is the standard procedure for determination of nicotine in urine. A 1.00mL sample was placed in a 12mL vial 5-aminoquinoline was added as the internal standard (5 ug). The sample was monitored using mass spectrometry at m/z values for nicotine (84) and the internal standard (144). Given the following data determine the concentration of the two unknown samples Nicotine (ug/L) Area Area 12 0.056 0.059 51 0.402 0.391 102 0.684 0.669 157 1.011 205 Unknown 1 Unknown 2 1.278 0.51 1.18 1.063 1.355 0.53 1.32(4.113+1 5. A monoprotic acid (HA) with K, of 8.76 x 10 has a partition coefficient of 3.9 (favoring octanol) when distributed between water and octanol, An aqueous solution (100.0 ml, pH 4.50) initially containing a 0.200 M formal concentration of HA is extracted once using 30.0 mL of octanol. a) What is the extraction efficiency? b) Calculate the formal concentration of the acid in both the water phase and the octanol phase after performing the extraction. Fwater = Foctanol = c) Would the extraction efficiency increase, decrease, or not change if the pH of the aqueous phase is adjusted to 7.00 prior to performing the extraction? no change Circle one: increase decrease Briefly explain: