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Universiti

Malaysia
Q PAHANG

Engineering . Technology Creativity

FACULTY OF CHEMICAL & NATURAL RESOURCES ENGINEERING
FINAL EXAMINATION
COURSE

: ANALYTICAL CHEMISTRY

COURSE CODE

: BKF1243

LECTURER

: EMAN N. AL!
FARHAN BINTI MOHD SAID

DATE

: 17 JUNE 2O15

DURATION

: 3 HOURS

SESSION/SEMESTER

: SESSION 2014/2015 SEMESTER II

PROGRAMME CODE : BKB/BKC/BKG

INSTRUCTIONS TO CANDIDATE:
I.
2.
3.
4.

This question paper consists of FOUR (4) questions. Answer ALL questions.
All answers to a new question should start on new page.
All the calculations and assumptions must be clearly stated.
Candidates are not allowed to bring any material other than those allowed by
the invigilator into the examination room.

EXAMINATION REQUIREMENTS:
1.

APPENDICES

DO NOT TURN THIS PAGE UNTIL YOU ARE TOLD TO DO SO
This examination paper consists of NINE (9) printed pages including front page.

6 15.8 13.0 13.3 5 15.2 3 14. Therefore.14 ml of 0. Determine the moiarity of HCl and identify the uncertainty of the value. Determine whether there is a significant difference in variance between the two methods. Table 1: Data of glucose content on two different methods No Glucose content (mg/ml) sample UV-VIS HPLC 1 13.05 M NaOH.10 ± 0.05 ml of HC1 is required for neutralization. data evaluation consider as a normal practice while doing research work or analysis of any product.6 14. a) The following data (Table 1) shows the content of the glucose content in a sample using ultraviolet-visible methods (UV-VIS) and high performance liquid chromatography (HPLC).0 4 13.00 ± 0. 20.CONFIDENTIAL BKB/BKC/BKG/1415111BKF1243 QUESTION 1 Analytical chemistry results need to be evaluated before writing the reports. (8 Marks) .50 ± 0.5 (17 Marks) b) In the titration of 10.5 13.0 2 13.

(4 Marks) c) Describe: i) Inclusion (1.00.00. (4 Marks) b) A 0.00 L of 0.CONFIDENTIAL BKB/BKCIBKG/1415111BKF1243 QUESTION 2 Gravimetric methods are one of oldest techniques in analytical chemistry which is considered the fundamental method. 50.100 M HCL. 10.500 g of CuSO4. Calculate the percentage of carbon in the sample if 0.2 121 g sample of an organic compound was burned in a stream of oxygen.00 mL of 0. and 60 mL of acid.00 M solution of the reagent. starting with a 6.100 M NaOH is titrated with 0.0750 M AgNO 3 from the solid reagent. a) Determine the mass of Cu (103) 2 can be formed from 0. (7 Marks) 3 .325 M HCL.6006 g of BaCO 3 was formed. Describe the preparation of: i) 500 mL of 0. and the CO2 produced was collected in a solution of barium hydroxide. (3 Marks) ii) 2. (2.51-120.00.5 Marks) iii) A 50.5 Marks) ii) Occlusion (3 Marks) d) Titration is a method of analysis using standard material as titrant to get the concentration of the analyte. Calculate the pH of the solution after addition of 0. and draw a titration curve from the data.

00 cm cell at 295 nm.34 ppm solution has atransmittance of 55. 4 . Calculate the molar absorptivity of the complex. express the range in wavenumbers.2glmol).im. (6 Marks) b) Express the following absorbance in terms of percent transmittance: i) 0.5% (1 Mark) d) A typical simple infrared spectrometer covers a wavelength range from 3 to 15 .7% when measured in a 1. given that a 1.013 (2 Marks) ii) 55.229 (1 Mark) c) Convert the following transmittance data to absorbance: i) 0.CONFIDENTIAL BKB/BKC/BKG/14151I1BKF1243 I QUESTION 3 Measurements based on light and other forms of electromagnetic radiation are widely used throughout analytical chemistry.494 (2 Marks) ii) 0. (4 Marks) e) Explain wave property that is measured by Fourier Transform JR and the units for this property? (2 Marks) f) Draw a simple spectrum using FTIR showing the following with naming x-y axis. The interactions of radiation and matter are the subject of science called spectroscopy. a) Beryllium (II) forms a complex with acetylacetone (166.

for each compound. (2 Marks) Absorbance (2 Marks) g) List the names of three equipments in applying spectroscopy technology. (3 Marks) 5 .1 3.5 3. k.CONFIDENTIAL i) BKB/BKCIBKG/141511jB1cy1243 Transmittance and.0 Caffeine 86 8. (3 Marks) QUESTION 4 a) An HPLC separation of two components pharmaceutical product yielded the following results (Table 2). R. Table 2: Retention time and peak width of caffeine and aspirin on HPLC Compound Retention time Peak width at base Peak width at V2 (mm) (mm) height (mm) Solvent 30 Aspirin 75 6.25 Determine the following items: i) The capacity factor. (4 Marks) ii) The plat number of each compound using base widths. (5 Marks) iii) The resolution of the two compounds.

determine the height of the theoretical plate? (4 Marks) b) The separation of two compounds on a packed and capillary column gave the following data in Table 3: Table 3: Data of two compounds on a packed and capillary column Component Packed column Capillary column Dead time (s) 15 30 Retention time of Component A (s) 160 75 Retention time of Component B (s) 170 86 Number of theoretical plates 6400 1967 Identify which column is giving the better resolution and.CONFIDENTIAL BKB/BKCIBKG/1415111BKJ1243 iv) Given the column used in this analysis is 25 cm long. (9 Marks) END OF QUESTION PAPER 6 . justify your answer.

CONFIDENTIAL BKB/BKC/BKG/1415111BKF1243 APPENDICES hc E = h V = .= abC = sbC po R = 2Z WA PT (x 2[(tR)B—(tR)A] + WB i=1 = WA+WB N—i tRtM k' F°2 exp a ( t R)B tM ( t R)A tM u — Xx -J exp N = 16(t/w)2 S pX = .= log-.= hcv ±xi N A = —logT = —log. r(L 7 )2 .Jog [X] H R S _1JSA +SB 2 R) = SR .

764 8.160 2.832 2767 2.902 14.772 5.191 2.42 14.053 2.269 4.0 236.669 3.576 3.786 7.628 2.544 1296 2.206 2.259 3.849 1796 2.239 3.838 3.938 1.725 3.9 18.328 2.641 2588 2.256 6.484 4.558 4365 3.965 6.40 10.308 1. 238.62 14.988 6.534 4387 4284 4.803 4.5 39.414 3.05 (95% Confidence Level) i 2 4 5 6 8 9 10 ii 12 13 14 15 16 17 18 19 20 00 1 2 3 4 5 6 10 9 .858 5.127 2.501 3.256 6.347 4.226 4.01 5.007 2.699 4.05 (95% Confidence Level) V31V11 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 1 2 3 4 5 7 6 8 9 10 15 20 984.544 2477 2.938 3.630 5.347 3.098 2.8.209 3.764 2.63-3 3482 3374 3.538 2.599 7.607 3.73 15.096 6.285 1209 3.163 6.891 4.544 2.813 4.112 1958 2.719 2.876 4818 4.150 2.43 39.352 2.602 2.380 3.9 2405 241.13 91552 9.965 4.510 4.950 3.852 2.591 4.857 6.179 3.044 3.04 17.715 7.544 4.214 2.39 39.737 4.146 7.434 10.117 9013 8 8.197 4.467 4.197 2.534 3 682 3.999 4.CONFIDENTIAL BKB/BKC/BKG/1415111BKF1243 Table 1: F-table for one-tailed test at 95% confidence level i:TabIe for One-Tailed Test at cc= 0.54 14.853 7.878 2.717 4.724 3.196 2.596 3.072 3.30 39.759 3.494 3.765 6.242 4.44 9.124 1.708 3.155 1.905 8.269 2134 2.773 2661 2.419 3.982 3.203 1.411 3.236 4.890 5.066 3.571 4.16 1925 1930 1933 1935 19.433 4.928 2.522 3.494 2.388 7.298 2.617 2.996 4.3 968.881 4275 4.020 2.895 2.587 3.00 19.935 2307 3.207 4.320 4.22 6.8 -161 4 1993 215.740 2.526 2283 3.500 3438 3.483 3.10 14.494 4.199 3.854 4.741 2.996 2.660 8.078 5.514 2.88 15.50 S.2 956.095 3.866 2.456 2.913 2.978 6.474 5.948 3.844 3.364 9.326 3.147 4.511 1218 3.917 2.577 2.552 3.605 2.416 6.38 19.826 5.995 5.6 647.823 4.587 3.374 3.599 2.---- 7 .329 6.849 5.073 4.066 2403 2.7 2244 2302 234.073 2.010 1.318 4.179 1137 4.456 6.493 3.769 1667 3.060 2.862 2.786 6.381 -3.33 39.937 3.072 3.767 3.40 39-45 39498 39.663 3.080 4.533 2.463 2.257 9.845 2 646 2.664 3330 3.37 -19.227 6.591 2.728 3.546 2.964 3.892 4.423 2.099 2.735 4.37' 39.447 2.250 3.293 3.634 3.600 3.714 2671 4.357 3204 3.757 4.529 4.200 Ov.965 2.17 13.949 2.950 4.143 4.779 3.101 1670 4.010 L831 1.461 5.372 2.197 9.820 5..761 4.099 4.978 4.718 5.451 3.478 3.2 899.756 3.1 1018 963.351 3.436 3.600 5.790 2707 2.667 3.47 14.806 3.619 6.588 3.6 921.619 4.276 2.51 39.592 3.863 3.880 15 co 20 2459 248.074 8.915 2.378 4.874 3.006 2374 2338 2.843 2.487 3.899 5.44 16.388 3.605 9.36 39.333 4.555 3.848 2.287 3056 2.51 19.357 4.293 3.121 4.060 5.652 3.277 9.901 2.987 5.855 3.015 6.703 5628 5.388 2.142 4.25 38.944 5.0 2543 19.117 4256 3.1 948.526 8.666 1570 1000 'e degrees of freedom in numerator v2 = degrees of freedom in denominator Table 2: F-table for two-tailed test at 95% confidence level F-Table for Two-Tailed Test at a = 0.468 4.65 12.608 5.094 6.739 3.230 3.147 2.637 5.523 5.709 6.120 3.9 993.053 5.996 2.972 3.00 14.415 3.119 4.285 5.512 3.412 2.230 2.459 2.295 4.604 3.980 8.135 3.747 3885 1490 3.842 2.657 2.8 799.344 3.358 5.168 5.25 14.999 5964 5.787 1726 3677 3.131 2.699 3614 2.695 5.523 6.568 4.012 1948 2896 2.428 6.845 8.804 4.17 39.43 19.414 3.450 2.-.817 5.459 4.347 4.31-2 3.711 2.123 3.753 - 4.103 3.059 7.591 6388 6.46 19.026 3.960 2.445 3230 3.404 2.153 4.657 8.560 8.844 8.348 2.542 8.812 8.102 4. =degrees of freedom In numerator v3 degrees of freedom in denominator 8 .844 2.810 2.681 6.177 3.8 937.395 3.393 3.581 3.217 3.548 4.7 864.041 5.666 3.409 5 192 5050 4.260 .025 2.757 6.979 10.928 2.

634 0.493 0.765 (o.926 0. 5% ConiIdence 99% Confidence 0.829 0.970 0.507 O46 0.526 9 JO 0.710 0.821 0.437 0.568 3 4 5 6 7 0.560 0.740 0.68() 0.466 Table 4: Periodic Table The Periodic Table of the Elements 9 .oi 0.412 0.625 0L56 04994 0.941 0.ci ii Q Ntmber of Obsrvation 90% Confidence > Q.CONFIDENTIAL BKB/BKC/BKG/1415111BKF1243 Table 3: Table of critical value of Q test (Rtji.598 0.