A mixture of the three compounds shown below is separated, using a 2.1x150 mm C8 column in 10-30% acetonitrile/water, and at a flow rate of 1mL/min. Three peaks are seen in the resulting chromatogram at 6.12, 6.25 and 6.98 minutes. Void time = 1.2 minutes. но. NH -Ph 4-methylpentanoic acid (R)-4-benzyloxazolidin-2-one N. Ph (R)-4-benzyl-3-(4-methylpentanoyl)oxazolidin-2-one
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What would the elution order of these compounds be? Why?
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- These chromatograms were recorded using reverse phase HPLC. |1,2,3 Peaks: 1. Benzyl alcohol 2. Phenol 5. Ethyl benzoate 6. Toluene 7. 2,6-Dimethoxytoluene 8. o-Methoxybiphenyl 8 3. 3,4-Dimethoxyacetophenone 4. Benzoin 6,7 |2,3 51 5 8 5 5 10 15 20 25 Time (min) Time (min) → a) Give an example of a mobile phase for this type of separation. b) Give an example of a detector that might be used for these compounds. c) Give an example of a stationary phase that might be used for these separations. Chromatogram A Chromatogram BThe following data were obtained by gas-liquid chromatography on a 40-cm packed column: Compound tr, min W, min Air 1.9 Methylcyclohexane 10.0 0.76 Methylcyclohexene 10.9 0.82 Toluene 13.4 1.06 If a resolution of 1.75 is desired in separating methylcyclohexane and methylcyclohexene (Use a spreadsheet to complete this question.) a. how many plates are required? 2798 plates b. how long must the column be if the same packing is used? Length = cm c. what is the retention time for methylcyclohexene on the column of part (b)? Retention time = minA mixture of three compounds was chromatographed using a silica gel column with diethyl ether/hexanes (10:90) as the eluting solvent. Fractions were collected and TLC analysis of each fraction was performed, with the results shown here: A 3 4 7 8 Mixture before separation Which fractions should be combined to give pure samples of A, B and C?
- 1a) Hexane, CH3(CH2)4CH3, is found to have a long retention time when separated from a mixture. A column with a C18 (18-carbon chain) stationary phase and a methanol-water modal phase is used for the separation. Explain why hexane has a long retention time. 1b)You wish to chromatographically seperate a mixtureof the follwing compunds. Which of the two compounds will be most difficult to seperatate from one another? Why?2. A Tlc plate was run on the fractions (#1-4) collected from a silica gravity column chromatography that was done. The Tlc plate was developed in 20% ethyl acetate/80% hexanes and is shown below. -------- Fraction # 1234 The compounds that were isolated in each fraction are shown below. Label each compound with the number of the fraction that it was likely found in, based on the TLC results. For example, was compound A found in fraction #2? If so, write A = #2 fraction. Do the same for all 4 compounds. CH₂CH3 .CH3 OH og OH D B CH₂6. A certain mixture contains the following compounds: propionic acid, 2-hexanol, isoamyl acetate, and 3,4-dimethylheptane. Rank the compounds in the order of decreasing rate of elution using normal phase liquid chromatography. Explain your answer.
- In an experiment of Reverse Phase chromatography using C-18 stationary phase and a mixture of methanol/ethyl acetate/acetic acid, a researcher tried to separate the 3 compounds shown below. Which compound would have the lowest Rf and which the highest Rf in this experiment? Explain your answer and show any relevant structures.Describe the procedural steps to achieve adequate separation of a homogeneous, liquid mixture containing benzoic acid, n-propylbenzene, and phenol, provided a 4:1 hexane to ethyl acetate solution as the eluent, using Thin Layer Chromatography (TLC).1) Study the chromatograph (below) of a mixture of Compounds A and B, run on the GCs in the teaching labs at CU Boulder. Compound A has the shorter retention time. STAAT 61 1.11 227 RT TYPE AREA XXXX XXXX XXXX AREAS 0.009 55874 44.117 ARIHT 0.61 XX XX XX 1.11 2.27 XX XX XX TOTAL AREA=XX MUL FACTOR=XX 1. What is the retention time of compound A? Compound B? 2. Which compound is present in a larger amount? 3. Which compound has the lower boiling point? 4. What would happen to the retention times of compounds A and B if the column temperature were raised? 5. You suspect that compound B is octane. What can you do to provide supporting evidence for this hypothesis?
- separate a mixture containing acetone, acetamide and 1,2-dichloroethane using a high- performance liquid chromatography (HPLC) technique. The instrument was equipped with a 40-cm column packed with cyano propyl bonded to the siloxane backbone material. i) List THREE (3) examples of mobile phase solvent/solvent systems that can be used with the column above. ii) Determine the sequence in which the three analytes eluted from the column and explain the underlying principle applied. iii) Sketch the chromatogram that would be produced if the column was replaced with a column filled with C18 hydrocarbon bound to the siloxane backbone material and acetonitrile was employed as the mobile phase. Label the peaks observed.Look up the boiling point for each of the following compounds then determine the order that they will elute from the column. Use this elution order to identify the compound in each of the 6 standard chromatograms. Once you have identified the compound in each chromatogram, record its retention time. Compound Structure Compound Name Elution Order (1-6) Non polar → Polar Boiling Retention Time (From Chromatograms) Point Propyl acetate H H. H. Butyl acetate H. H. H H. H H. H. H. Methanol H O- Ethanol 2-butanone H H H. H. 4-methyl-2- pentanone H. H. HH H.5. A mixture was analyzed using TLC and it was doubted to contain three components: R, T, and Y. A non polar solvent was used with a polar stationary phase. Answer the following questions: cm 9. solvent front origin line R T Yrple Y mpte before lofter Which of the doubted components (R, T or Y) are present in the sample? Are there other components in the sample? What are the Rr values ofR and T?