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AS/APR 2009/CHM256

UNIVERSITI TEKNOLOGI MARA FINAL EXAMINATION

COURSE COURSE CODE EXAMINATION TIME

BASIC ANALYTICAL CHEMISTRY CHM256 APRIL 2009 3 HOURS

INSTRUCTIONS TO CANDIDATES 1. 2. 3. 4. This question paper consists of five (5) questions. Answer ALL questions in the Answer Booklet. Start each answer on a new page. Do not bring any material into the examination room unless permission is given by the invigilator. Please check to make sure that this examination pack consists of: i) ii) iii) the Question Paper a two - page Appendix an Answer Booklet - provided by the Faculty

DO NOT TURN THIS PAGE UNTIL YOU ARE TOLD TO DO SO

This examination paper consists of 5 printed pages
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QUESTION 1 a) i) ii) Differentiate between qualitative analysis and quantitative analysis. For the following problems indicate whether its solution requires a qualitative analysis, or quantitative analysis or both: I - A hazardous-waste disposal site is believed to be leaking contaminants into the local groundwater. II - A more reliable method is needed by airport security for detecting the presence of explosive materials in luggage. III - A quick way is needed to screen an athlete's urine for the presence of performance-enhancing drug. (5 marks) b) i) A pipette is used to deliver a specified volume of solution. Which type of pipette would you use to transfer the following volume of: I - 25.0 mill - 7.5 mL III - 1.0 uL ii) Give any three precautions to minimise errors in measuring a mass of an object. Explain each answer. (9 marks) Show that the molarity of concentrated HCX purchased for laboratory use is approximately 12.1 M based on given information on the label on the bottle that it is 37.0% (w/w) and has a density of 1.19 g/mL Write the steps on the preparation of 1.000 L of 0.100 M HCi solution. (6 marks)

c)

i)

ii)

QUESTION 2 a) i) State whether the following errors are sources of determinate error or indeterminate error. I II III IV ii) wrong sample was collected insufficient samples collected several different readings reported by one same person reading the same instrument pH meter was incorrectly standardised

An empty 10-mL volumetric flask weighs 10.2634 g. When filled to the mark with distilled water and weighed again in the air at 20C, the mass is 20.2144 g. What is the true volume of the flask at 20C? [The volume of 1 g of water at 20C = 1.0029 mL] (6 marks) CONFIDENTIAL

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b)

A batch of nuclear fuel pellets was weighed to determine if they fell within control guidelines. The weights were 127.2, 128.4, 127.1, 129.0, and 128.1 g. Calculate the: i) ii) iii) iv) v) vi) mean median range standard deviation confidence limit at 90% confidence level value of Qcaicuiated if data 129.0 is suspected to be an outlier. Determine whether it is retained or rejected at 95% confidence level. (9 marks)

QUESTION 3 a) What is the difference between i) ii) b) titrant and titre value? acid-base titration and acid-base titration curve? (5 marks) Consider a titration between 25.0 mL of 0.100 M NaOH and 0.0500 M H C i i) ii) iii) iv) v) vi) vii) What is the pH of the base before titration begins? Determine the pH of the solution after 10.0 mL of acid has been added, Calculate the volume of acid added at the equivalence point, Show that the pH of solution is 2.23 after 60.0 mL acid has been added, Sketch the titration curve for the titration above Name the type of titration involved. What would be the colour change at the equivalence point if phenolphthalein is used as the indicator for this titration? (12 marks) Give one reason each why NaOH and HCi are secondary standard solutions, Suggest a reagent which you can use to determine the molarity of H C i H3NSO3 acid is a primary standard that can be used to standardise NaOH. H3NS03~ + OH - FW = 97.095
+

c)

i) ii) iii)

H2NSO3- + H 2 0

What is the molarity of a sodium hydroxide solution if 34.26 mL reacts with 0.3337 g of H3NSO3 acid? (6 marks)

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d)

The protein in a 1.2846-g sample of an oat cereal is determined by the Kjeldahl procedure for organic nitrogen. The sample is digested with H 2 S0 4 , the resulting solution made basic with NaOH, and the NH3 distilled into 50.00 mL of 0.09552 M HCI The excess HCi is then back titrated using 37.84 mL of 0.05992 M NaOH. Calculate the %(w/w) of N in the sample. (5 marks)

QUESTION 4 a) Define the following terms: i) precipitant ii) digestion iii) coagulation iv) supernatant (6 marks) b) i) ii) iii) Give any two ways to encourage the formation of larger particles of precipitate. Suggest a precipitant and the final product formed in a determination of S042" content in Shah Alam Lake. To determine the amount of iron in a dietary supplement, a random sample of 15 tablets weighing a total of 20.505 g was ground into fine powder. A 3.116 g sample was dissolved and treated to precipitate the iron as Fe(OH)3. The precipitate was collected, rinsed, and ignited to a constant weight as Fe 2 0 3 , yielding 0.355 g. Report the iron content of the dietary supplement as g FeS0 4 .7H 2 0 per tablet. (10 marks)

c)

The water content of a 875.4-mg sample of cheese was determined with a moisture analyser. What is the %(w/w) H 2 0 in the cheese if the final mass was found to be 545.8 mg? (2 marks)

QUESTION 5 a) i) ii) iii) What is the basic principle of chromatography with reference to stationary phase and mobile phase? Give two classifications of chromatographic method based on mobile phase, Column chromatography and planar chromatography are the two basic types of chromatographic methods. Explain the differences between the two chromatographic methods. (7 marks)

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b)

A substance X is suspected to contain either A, B, or C. Figure 1.1 below shows the chromatogram obtained when thin layer chromatography was carried out in water as the mobile phase and Figure 1.2 shows the chromatogram obtained when the same experiment was repeated in ethanol.

Figure 1.1 i) ii)

Figure 1.2

By comparing the two chromatograms obtained, suggest the most likely identity of X. Justify your answer, What can you deduce about the solubility of standard B in both mobile phases used in the experiment above? (5 marks)

c)

Name two applications of thin layer chromatography. (2 marks)

END OF QUESTION PAPER

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APPENDIX 1

AS/APR 2009/CHM256

ATOMIC MASSES OF THE ELEMENTS 1999 - IUPAC

Name Actinium
Aluminium

Americhim Antimony Argon Arsenic Astatine Barium Berkelium Beryllium Bismuth Bohrium Boron Bromine Cadmium Caesium Calcium Californium Carbon Cerium Chlorine Chromium Cobalt Copper Curium Dubnium Dysprosium Einsteinium Erbium Europium Fermium Fluorine Francium Gadolinium Gallium Germanium Gold Hafioium Hasaium Helium Holmium Hydrogen
Tral-iiim

Sym. Ac Al Am Sb Ar Aa At Ba Bk Be Bi Bh B Br Cd Cs Ca Of C Ce

a Or
Co Cu Cm Db Dy Es Er Eu Fm F Fr Gd G* Ge Au Hf Hs He Ho H In I Ir Fe Kr La Lr Pb Li Lu Mg Mn Mt Md Hg Mo Nd Ne Np Ni Nb N

Iodine Iridium Iron Krypton Lan&ianum Lawrencium Lead

1 Jthium

Lutetium Magnesium Manganese Meitnerium Mendelevium Mercury Molybdenum Neodymium Neon Neptunium Nickel Niobium Nitrogen

No. 89 13 95 51 18 33 85 56 97 4 83 107 5 35 48 55 20 98 6 58 17 24 27 29 96 105 66 99 68 63 100 9 87 64 31 32 79 72 108 2 67 1 49 53 77 26 36 57 103 82 3 71 12 25 109 101 80 42 60 10 93 28 41 7

Atomic Mass [227] 26.981538(2} [243] 121.760(1) 39.948(1) 74.92160(2) [210] 137.327(7) [247] 9.012182(3) 208.98038(2) [264] 10311(7) 79.904(1) 112.411(8) 132.90545(2) 40.078(4) [251] 12.0107(8) 140.116(1) 35.453(2) 51.9961(6) 58.933200(9) 63.546(3) [247] [262] 162.50(3) [252] 167.259(3) 151.964(1) [257] 18.9984032(5) [223] 157.25(3) 69.723(1) 72.64(1) 196.96655(2) 178.49(2) [277] 4.002602(2) 164.93032(2) 1.00794(7) 114.818(3) 126.90447(3} 192.217(3) 55345(2) 8330(1) 138.9055(2) [262] 207.2(1} [6.941(2)] 174.967(1) 243050(6) 54.938049(9) [268] [258] 200.59(2) 95.94(1) 144.24(3) 20.1797(6) [237] 58.6934(2) 92.90638(2) 14.0067(2)

I Name
KTobelium Osmium Oxygen Palladium Phosphorus Platinum Plutonium Polonium Potassium Praseodymium Promettaium Protactinium Radium Radon Rhenium Rhodium Rubidium Ruthenium Rutherfordium Samarium Scandium Seaborgium Selenium Silicon Silver Sodium Strontium Sulfur Tantalum Technethun Tellurium Terbium Thallium Thorium Thulium Tin Titanium Tungsten Ununbium UnunniHum Ununquadium Unununium Uranium Vanadium Xenon Ytterbium Yttrium Zinc Zirconium

Sym. No Os Pd P Pt Pu Po K Pr Pm Pa Ra Rn Re Rh Rb Ru Rf Sm Sc Sg Se Si Ag Na Sr S Ta Tc Te Tb Tl Th Tm Sn Ti W Uub Uun Ouq Uun U V Xe Yb Y Zn Zr

No. 102 76 8 46 15 78 94 84 19 59 61 91 88 86 75 45 37 44 104 62 21 106 34 14 47 11 38 16 73 43 52 65 81 90 69 50 22 74 112 110 114 111 92 23 54 70 39 30 40

Atomic Mass [259] 190.23(3) 15.9994(3) 106.42(1) 30.973761(2) 195.078(2) C244] [209] 39.0983(1} 140.90765(2) [145] 231.03588(2) [226] [222] 186.207(1) 102.90550(2) 85.4678(3) 101.07(2) [261] 150.36(3) 44.955910(8) [266] 78.96(3) 28.0855(3} 1073682(2) 22389770(2) 87.62(1) 32.065(5) 180.9479(1) [98] 127.60(3) 158.92534(2) 204.3833(2) 232.0381(1) 168.93421(2) 118.710(7) 47.867(1) 18334(1) [285] [281] C389] C272] 23832891(3) 50.9415(1) 131.293(6} 173.04(3) 88.90585(2) 65.39(2) 91.224(2)

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APPENDIX 2

AS/APR 2009/CHM256

Table 1 Values of t for Various Levels of Probability Factor for Confidence Interval Degrees of freedom 1 2 3 4 5 6 7 8 9 10 11 12 13 14
00

90% 6.31 2.92 2.35 2.13 2.02 1.94 1.90 1.86 1.83 1.81 1.80 1.78 1.77 1.76 1.64

95% 12.7 4.30 3.18 2.78 2.57 2.45 2.36 2.31 2.26 2.23 2.20 2.18 2.16 2.14 1.96

99% 63.7 9.92 5.84 4.60 4.03 3.71 3.50 3.36 3.25 3.17 3.11 3.06 3.01 2.98 2.58

Table 2 Critical Values for the Rejection Quotient Q Critical Values Number of Observations 3 4 5 6 7 8 9 10 90% Confidence 0.941 0.765 0.642 0.560 0.507 0.468 0.437 0.412 95% Confidence 0.970 0.829 0.710 0.625 0.568 0.526 0.493 0.466 99% Confidence 0.994 0.926 0.821 0.740 0.680 0.634 0.598 0.568

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