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CHEMISTRY 311 - Mid Term ANSWER ALL QUESTIONS IN BOOKLETS PROVIDED. SHOW ALL WORK. TOTAL MARKS 40. 1. a) What volume of a 50.0 1g/L PO,* - P stock solution is required to prepare 250.0 mL ofa 1.00 pg/L PO,* - P standard solution? [2] | b) A researcher needs to analyze water samples for phosphorous down to levels of 0.050 uM. A supplier of an Ton Chromatograph (IC) reports a detection limit of 5 ppb PO.*. Does the IC meet the detection limit requirements of the researcher? [2] | | * _ (00 gh Ja02) 5g mb (50.049/- ) = es ee eG GF_9 Lreel Pep 10 49 0.050% 0 al mal PO FG (CHEM 311 Mid-term Oct 23, 2007 Page 1 b 2. A wastewater sample was volumetrically analyzed for ferrous iron according to; ClO; + 6 Fe* + 6H —-> Cr + 6Fe* +3H,0 a) Ifa 100, mL wastewater sample required 0.84 ml. of 0.100 N KCIOs titrant to reach the end point, what is the concentration of Fe” in units of mg/L Fe"? [2] ») If the titration was carried out in a class A, 50.0 mL burette (individual reading error 0.02 mL), what is the relative uncertainty in the final answer? [2] ©) What procedural modifications can you suggest to reduce the relative uncertainty in this determination? [2] @) What mass of potassium chlorate, KC/Os, (molar mass 122.5 g mot") is required to prepare 2.00 L of the titrant solution? [2] Ve, (2.100 M) (0.84 mt) (100, mL) oe ae Ni V, = Ne Ve N, > HW EW pee Kine a”) Enals e° trans ferrect pan male a 2 Limle 3, EW MW > SSESAN 7 ol ee Fest Cone, Fette Big x 10” Bll » SEBS guy ~ may Fer = 46.9 my, Rett or At my fe sz Ve = Vp-Vi Clos + (o.0a¥ ]* = 0.0288 poe 0.0339 (or aah) a ) m (0.0859 (abd) = I-58 ML ao ge Abg tly Yap RAZ M34. ie (CHEM 311 Mid-term Oct 23, 2007 Page 2 2 4) de lute febout Lovager sample volume small (more presse) bree (a0ot) (0-100 N) = 0.200 equiv of KD; mary KOO, = equiv. x EW Ews Mw hoy» CI Le ce v, 6 mela en tanshrack Ug ——- co Ko Tmo eta, cated Ewe 122-8 Val 6M Y/v0) 2 20. 42 VYequiv O.200 equiv x AY Yay > Foy J KAO, 3. A Standard Reference Material is certified to contain 94.6 ppm of an organic contaminant in soil. Your analysis gives values of 98.6, 98.4, 97.2, 94.6 and 96.2 ppm. Do your results differ from the expected result at the 95% confidence level? [3] Ao (bun voln= TAG pr ge b5 (uae cateutaster) Mas tO. Pe nS ds UE gy ab 19% Ww [eal = ts VN rearrange anol solve or Lele _ fw Lak - 1% al = @A)OE?) _ 525 165 Since tus > t (df= 4) ten reoully are signi treaty Lb ltat (CHEM 311 Mid-term Oct 23, 2007 Page 3 ‘4, Duting the field analysis of total hardness using a Hach Digital Titrator™ method a 100. mL sample is titrated with a 0.800 M ethylenediaminetetraacetate (EDTA), which forms a 1:1 complex with Ca®. A student inadvertently adds one drop (~50 uL) of titrant to the sample before carrying out the titration. Estimate the sign and the magnitude of the error introduced in ppm CaCOs. [4] # mols Ca? consumed. 4 adldifien of Sal % EDTA ce = 16 = (50 x0 1) (0,826 a) = ox G Coe] eB antl is mols 4.0 xo 1 i Cet O.100L zc Conver ting Appi G02, 7 COs 0, 000m oxtok Th sp | nol Cals 100, 7 J vol @& 7 nol Cals = 40 "9 Cold, - 40 ppm Cele L Sine His 2 Je Cone. 9 Gt remove ye fa lArop addition (2 te eypecinanted repute wll suthr & negative bias — 40 ppm Ds (CHEM 311 Midterm Oct 23, 2007 Page 4 5. The following procedures may be included in a sampling and analysis programme. Indicate the rationale for THREE of the procedure. [3] a) The sample is filtered (0.45 pm) and 2 mL/L of HNOs is added b) A spike of isotopically labelled analyte is added prior to sample preparation steps c) Every 15" lab analysis is of a certified reference material 4) A deionized water blank is collected at the sampling site and transported to the lab for analysis a Lhd sample jv dessoluet anche /, mnibie aud addi presevve bisselvek bf -miaaue recover eae pr ntanol : : fol fb heck methool Q eg quality cortiel chart /s. fold lark A chick for corrtamin nan 4) shrage and fram sport gluning sameling (CHEM 311 Mid-term Oct 23, 2007 Page 5 ” 6, In'the determination of Calcium by flame atomic absorption spectroscopy, the following calibration curves were obtained. [3] ) Determine the concentration of Calcium for an unknown sample with an absorbance of 0.440 au. >) Comment on the relative precision and accuracy of results generated using these curves. Instructor Calton Curve Student Calibration Curve a ooo y= 005654 00078 ¥= 0.0500%- 0.0028 ae R? = 0.9992 R?= 0.9919 i dom oo 20 40 80 80 10 120 00 200 40 60 80 100 120 ene Cot oom) ane an pm 2) a) 4 -=mxrb a x= t Conc. = 0.440 — 0.0047 abs 0.0565 = #465 ppm @ by Ins tmeter colibratiin Urve 4A amare precise a2 Com be sean, vi sual sy cata (also R™ closer 4e b000 Does mine worth, cok Comet termine aueurate 140 al fe can HE 311 Migtem 0425, 2007 Pages breton Cure wll withot 7. A Dlood serum sample was analyzed for potassium by flame atomic emission spectrometry (FAES) using the method of standard additions. In FABS, the signal obtained is directly proportional to analyte concentration. A 0.500 mL aliquot of serum, was placed in each of two 5.00 mL volumetric flasks. In one flask, a 20.0 uL spike of 0.0500 M KCI was added. Both flasks were then filled and mixed by inversion. The signal for the unspiked flask was 32.1 a.u. and for the spiked flask 58.6 a.u. respectively. ‘What is the potassium concentration in the original sample? [4] Ae AU ate ad ball He 7. Lers. ‘heck anol sprbeat Ares Dd ESI CO an dilitedl [x]; - Vea 0. S00 mL : B00 mb ae 5 VE CS]¢ = CS]; _ Co sca Mi a0,0x10 L) Vp C G00 x /0FL ) Cc 4 a R00 xo 11 = 200M x] Se) £ 58.6 Cxlp + (a 00 mM) 0. 5YFE LX p+ 061095 mt = cxdy OX g (1 = 0.8498) = 0.1095 0/4 [x], = 2:1075 nlf att | o.a493 0M (j- 0.5478) Ox = 4a, 0/4 CHEM 311 Mid-term Oct 23, 2007 Page 7 8, An HPLC analysis of combined standard of 25.0 #M Valium™ (MW = 284.5 g/mol) and 10.0 uM nitro-diazepam (internal standard) gave signal areas of 4322 a.u. and 1458 a.u,, respectively. When a 100. mg hair sample was digested (dissolved), and analyzed for Valium, the digest (15.00 mL) was spiked with 100.0 jiL of 20.0 mM nitro-diazepam, and subjected to HPLC analysis. The signal areas obtained for Valium and nitro- diazepam were 152 a.u. and 110 a.u., respectively. Determine the Valium concentration in the digest sample (\iM) and the original hair sample (mg/g). [5] 432ry | fe Bon, 1.1%, fom combined 14 58 ig ult standard ln, frm spied sample} 152 /exdy 110 /¢SJp whos (Sp = (000 xt t)Cz00 0M) C158 x 107 L) = 0.1333 7/1 JAS, BR e(/. 1%,) (110) . aa Exly © 02/333" afd So £XIp= 0-185 mM th ipa 53, fait = 0.1550 x lo? a84 59» 1§.0X10% nan Vaktam

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