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Analysis II UV and IR Assignment Lideta Stud

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79 views13 pages

Analysis II UV and IR Assignment Lideta Stud

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fuadf5915
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St.

Lideta Health Science and Business Collage


Department of Pharmacy
Pharmaceutical Analysis II
Assignment I By: D. A (MSc, AAU)
UV Visible Spectroscopy

1. What is the frequency and energy of a photon with a wavelength of the following:
(a) 650 nm (b) 1,700 µm (c) 195 nm (d) 0.5 µm

2. Calculate the energy, in kilo Joules per mole of radiation, of a wave with wavelength
2.50 mm.What type of radiant energy is this? Ans = 47.7 kJ/mol

3. Diphenyl Ketone have three peaks in the UV-vis spectrum with λ max values of 238 nm,
270 nm and 354 nm.

a. indicate the type of transitions in each λ max of the compound


b calculate the energy (in Joules) associated with each of these transitions
c. calculate the frequency (in Hz) of the photon absorbed for each of these transitions

4. Based on the compound given below in the UV-Visible Spectroscopy?

a. Write all the possible transitions of the compound in The UV


b. What is the baseline of the compound?
c. Predict λmax of the compound

1
5 In the reaction blow on increasing pH, what will be the effect of the PH
(Bathochromic, Hypsochromic, hperchromic or hypochromic shift))

6. Given below are two cyclic enones A and B. What happens to the UV-Visible spectra
when A is converted into B? (red shift/Blue shift/Hpochromic/hperchromic)

7. Diphenyl ketone given below λ max 270 nm peak shift to longer wavelengths, 340nm when
Placed in a more polar solvent. Explain the effect of the solvent to shift the λ max

8. What is the percent transmittance if the absorbance of a compound is

a. 0.5 b. 1.0 c. 2.5 d. 0.001

9. If the molar absorptivity for the compound above is 3500 M -1cm -1, calculate the
Concentration of each solution

10. What is the absorbance if the percent transmittance is

a. 3% b. 90% c. 0.5% d. 50%

11. What are the two most common sources used in a UV-vis spectrophotometer

2
12. We have been discussed two basic classes of monochromators: prism and grating.
Discuss the advantages and disadvantages of both types?
13. Explain the main difference between double beam and Single beam UV-Visible spectroscopy

14. What are the advantages of Derivative Spectroscopy over zero order (normal) spectroscopy?

15. Compare and contrast UV-Visible and IR detectors?

16. Rank each of the following molecules from highest to lowest λmax. for the π- π* transition.

17. Which one of the following compounds is expected to have the longest wavelength?
Absorbance (λmax)? Justify your answer

18. What are the concentrations of the following solutions of drugs in g/100 ml?

a. Carbimazole, A (1%, 1 cm) value=557 at 291 nm, measured absorbance=0.557


at 291 nm (Ans.= 0.001 g/100 ml)

b. Hydrocortisone sodium phosphate, A (1%, 1 cm) value=333 at 248 nm,


measured Absorbance =0.666 at 248 nm Ans.= 0.002g/100 ml

c. Isoprenaline, A (1%, 1 cm) value=100 at 280 nm, measured absorbance= 44


0.5 at 280 nm (Ans.= 0.005 g/100 ml

3
19. Two samples each containing same analyte at equal concentration are irradiated with
different intensities of radiation as shown below..

Select the CORRECT statement regarding the absorption

a. A2=4 A1 b. A 2 = 2 A 1 c. A 2 = A 1 d. A2=1/2 A1

20. predict λmax of The following Compounds (use Woodward rule)

a b c

d e f
21. Predict λmax of the compound by using no of conjugated double bonds (Kuhn & Haussler rule)

b b
22. Calculate the concentration of the drug in an aqueous solution in which the absorbance in 4
cm cell at its λmax , 261nm, was found to be 0.87. the A (1%, 1 cm) value of the drug is
given as 520 at 261 nm. Ans= 0.0668 mg/ml

4
23. Assay of Furosemide Tablet

Tablet powder containing 0.258 g of furosemide is shaken with 300 ml of 0.1 M NaOH to extract
the acidic furosemide. The extract is then made up to 500 ml with 0.1 M NaOH. A portion of the
extract is filtered and 5 ml of the filtrate is made up to 250 ml with 0.1 M NaOH. The absorbance
of the diluted extract is measured at 271 nm and the following results were obtained.
– Stated content per tablet: 40 mg of furosemide
– Weight of 20 tablets: 1.656 g
– Weight of tablet powder taken for assay: 0.53406 g
– Absorbance reading: 0.596
– A (1%, 1 cm) value at 271= 580

a. Calculate the % of stated content in a sample of furosemide tablets: 99.6%


b. Calculate the content of furosemide in a tablet of average weight 39.84mg
c. Does the product comply with pharmacopeial specifications? (BP limit: 95- 105%)

24. In a spectrophotometric determination of a drug in an aqueous solution, the absorbance of 4.5


x 10-5 mg/ml of a standard solution of drug at 273 nm was found to be 0.454 with a path
length of 1 cm. The absorbance reading of the sample solution was 0.367 at 273 nm, with
the path length of 1 cm. Determine the concentration of a drug in mg/ml?
( Hint: use Absorbance ratio method)
C= 0.00364 mg/ml
25 The molar absorptivities of drug X and Y were measured with pure samples of each

Mixture of drug X and Y in a 1.000 cm cell has an absorbance of 0.957 at 272 and 0.559 at
327 nm Find the concentrations of X and Y in the mixture (Simultaneous equation)

5
St. Lideta Health Science and Business Collage
Department of Pharmacy
Pharmaceutical Analysis II
Assignment I By: D. A (MSc, AAU)
IR Spectroscopy

1. Arrange the following radiation from smaller to larger wavelength?


A. infrared B. Visible C. X-ray D. ultra violet E. Gamma rays
2. Write the type of transitions mainly occur in IR?
3. What type of materials used to made Beam splitters in IR spectroscopy
4. Identify the basic components of IR spectroscopy and write their functions
5. Write main differences between Dispersive IR and FTIR spectroscopy
6. Caffeine molecules absorb infrared radiation at 1656 cm−1. Calculate the following:
(i) Wavelength of this radiation; ans λ 6.039 μm
(ii) Frequency of this radiation; ans: ν = = 4.964 × 1013 Hz
(iii) Energy change associated with this absorption ans _E = 3.107 × 10−20 J
7. How many vibrational modes would you expect in the molecule given blew
Identify active and inactive in the IR and why?

a. hydrazine (H2NNH2)? b. chloroform (CHCl3)? c. CO2 (symmetric and asymmetric)


8. The highest energy band in the IR of H2NNH2 occurs at about 3350 cm-1;
What vibration is this likely to be due to?

A: N-N stretch B: (sym /asym) N-H stretch C. N-N bond rotation

9. Hydrogen bonding is one of the factors that affect the position of absorption band in IR.
Alcohol O–H stretching mode be expected to change the vibrational frequency when
Hydrogen bonded. If so, would it decrease or increase? Why?

10. The Infrared spectrum of compound “A”, C3H6O, shows strong absorption band at 1730
cm-1 and no absorption band at 2700-2800 cm-1. Suggest a structure for this compound.

11.. A compound with a molecular formula C2H6O has an Infrared spectrum which shows,
amongst others, a broad absorption between 3200 - 3400 cm-1 and a band at 1100-1380 cm-1
Propose a structure for this compound

6
12. The IR spectrum of a compound of molecular formula C6H15N is given below:

a. Using The spectra Identify The functional group of the compound

b. Using the Formula and IR Spectra predict the structure of the compound

13. Which structure is most consistent with the following infrared spectrum?
Identify each vibrational mode indicated on The IR spectrum of the compound

7
14. A compound X has a formula C3H3NO2 gives the IR spectra given below
a. Identify the vibrational mode of the indicated position on the IR
b. what is the Principal Functional group of the compound and
C. Determine the structure of the compound

15. Compound Y has the formulaC14H12O and given the IR spectrum below
a. Identify the vibrational mode of the indicated position on the IR spectrum
b. What does the IR spectrum tell you about the aromatic ring substitution?

(mono substituted, Disubstituted: (ortho, meta, para) or no aromatic ring)

C. predict the structure of the compound

8
16. Quantitative analysis of tablets containing aspirin, phenacetin and caffeine is to be carried
out. Each of these components show distinct carbonyl bands in chloroform solution and
calibration data for known concentrations are listed below table 1 . Each of the standards
was studied byusing a 0.1 mm pathlength NaCl transmission cell. Given that the absorbance
values for an unknown tablet produced under the same conditions are given below in Table 2,
estimate the concentrations of aspirin, phenacetin and caffeine in the unknown tablet.

Hint: First calculate the ℇ value of each drug from the given standard (known conc) of each
Drug. Then calculate the unknown con of each drug From Given absorbance

Ans Asprin 85 mg ml−1 , phenacetin = 71 mg ml-1 , and caffeine 22 mg ml-

Table 1 Calibration data for a standard drug mixture

Table 2 Absorbance values for an unknown drug mixture

9
17. Match the following IR spectra to the proper compounds given below

C.

10
18. Match the following IR spectrum to the proper Drugs given below

Vanillin ASA (Aspirin) Ibuprofen

Diclofenac Acetaminophen (Paracetamol) Salicylic Acid

11
B

12
D

E.

13

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