os (nents ERIMENT 13: PLOTTING A STANDARD CURVE EXPE XCEL SPREADSHEET SOFTWARE (VERSION 2009) ° “ ice plotting a standard ct i tical data to practice plotting ‘urve with the Exc rh ve POAT Later experiments will refer you back to this proced wr ne eerexperiments Launch Excel (or click “file” then “new” if alreadh apr el spreadsheet soft. lure to plot standard ly launched) to begin. data for the standard curve in the A and B spreadsheet columns. Use the “A” 1, Type n for the concentrations and the “B” column for the Corresponding instrument read- rales For the unknown, type in the instrument readout value in the “B" column cell cr the standards, but leave the corresponding concentration cell blank. When finished, etal B columns should appear as in Table 6.1 in which there are four standards with is of 1, 2, 3, and 4 ppm and one unknown. dards data in the A and B columns. 9, click “Scatter,” and then select the upper left icon. The graph should in theAnal alytiCa Chery "Vb eh 180 _——_——_—_ TABLE 6.1 Example of the A-B Columns in the Spreadsheet in Step 1 a 8 1 1 3 2 2 59 3 3 94 4 4 2 5 2 cere 4. setct he “Layout tab and click “Axis Tiles.” Enter the ties vec ans tor ma of 9 forthe horizontal axis and ear Po re tty anh Forever ile, Se Rote ie at rate ine 12 Eeprmnt 20° or ater descriptive ile above the graph so add "ent 5. Weal on the “aye” ab ick “Tending” Selec "More THe pe ely iia Equcrion Chart,” and "Display rquared ne Op s. oe a a cepinee hesope et her me ae oe 6 Gis Be creat te enkrown a gn eye ang sepia igang oma Peeler cris et formula fer cat te sing he values that yb, and m are “type og See Should row bein thea" kooin eheen 10 location directly below the data, lr emccefticien ee UIE tet coe! Ene unknowns and cor Olan sr" Intro, xpfRIMENT 15: COLORIMETRIC ANALYSIS OF [EXPERINID/OR REAL WATER SAMPLES FOR IRON Re? swear safety glasses rv fan 20.30 bao = Sr pnk(no iro) real water samples are being analyzed and you expect the iron oe ea pare two atonal standard that are 0: and 0. pp : pepe ie eal water samples by pipeting 25.00 mL of each into SO-mL volume fas Pete standards, do not dite to the mar unl Step 6. an instructor prepared ‘eronn s provided, do not dilute it to the mark until as directed in Step 6 forall asks. ‘er astvctor may also provide you with a control sample. Prepare the contol asifit were ‘rel water sample by pipetting 25.00 mL of it into a S0-ml flask, pattern of absorption a2 Analytical Che, "my flasks (standards, samples, blank, and contro} istry toy, (2) 0.5 mL of 10% hydroxylamine hydrochloride ada {0 2.5 ml of 0.1% o-phenanthroline solution fe) 4.0 ml of 10% sodium acetate ‘These reagents are required for proper color development, 44 ide hea reducing agent, which is required to keep the iron in the Ys"*Vlaming ee isa igand that reacts with the Fe to form the orange-colone They compe? lex {s the “absorbing species.” In addition, since the reaction 'S BH depender! pm Stun, ty To each of the ‘\ if «needed for buffering at the optimum pH. nie each to the mark with distilled water and shake wel in i Cuing one of your standards and the Spectronic 20, or others meter, obtain an absorption (or transmittance) spectrum ngle-beam yj Pole ion (instructor will demonstrate use of instrument Deet® Feloph es, from the spectrum and use this wavelength ne seas obtain maximum absorbance readings ofall the solutions. (Use the blank for 100% T setting) Plot the standard curve using the spreadsheet procedure sed in Exper erimer rao derelation coefficient and the concentrations of the unk nt ni 3 Irceal water samples and a control were analyzed, remember thereon. Oo diluted by a factor of 2. Multiply the concentrations found in Step 7 by il Behe sy answers in that case. ‘Maintain the logbook for the instrument used in this experiment. Rec - Record the erenet), the experiment name or number, the R? value, and sample. Also, if directed by your instructor, plot the control ame os oe for this experiment posted in the laboratory. Ui on acon SA nn a ens mpeg rnrnorrren ney eng ren aeraee | experiment in % EXPERIMENT 17: CONCENTRATION AT WHICH A BI that the Beer's law plot constructed in Experiment 15 isi i ite You should have noticed toe snow nventrations of 1 ppm Fe and 4 ppm Fe. At some poi ah ° int wil bea deviation from Beer lav. Design an experiment that wll pee Lisle’ ‘concentration a which this occurs. Write a step-by-step procedure asin eis cies ‘soa for rearing needed solutions Brdssing the spectrophotometero maa ances of each. After your instructor approves your procedure, perform the cae the laboratory. DESIGN AN EXPERIMENT: DETERMINING THE |EER’S LAW PLOT BECOMES NONLINEAR,samples is determined by visible specton=) le with potassium antimony! tartate nn hould be washed in phosphate-fee deter smber to wear safety glasses. EXPERIMENT 18: THE DETERMINATION OF PHOSPHORUS IN ENVIRONMENTAL WATE Note: In this experim following a reaif veo, 02500 Chern ene et Ot ea Sat geal O45 of - 'ewirl to make homogeneous, Prepare until dissolved, Jaa a re 6 gol anmeniom maybe ea 0 ge solu ‘molybdate in Brac cin get HO wih aa ae ee Fee teat — rea jo go ascorbic aid it a 250. jt weigh 278 ‘0-mL Erlenmeyer las, dite weil make HOARE Prep led 99 mt of 2.52 MHSSO. tom concentrated sue wi Maes ne 100 aL efthe color predic reagent min es sete ero Sting gently after each addition: SO mi ofthe eee A a solution, 15 mt ofthe ammonium reba eer en sla. 82 TS apap ester sa 125. Eermeyer fase is 1 nt te psp contains nada Bi soe ree “iis combined reagent is stable for afew hours. ww perakaTion OF STANDARD SOLUTIONS seta s-ppn goss ck hon by cig ccc ca sit. mien 6g POH dards that are 0 0.5 1.0, and 1.5 ppm Pf ecto voumev is ot sn nts MEGAN 0 RES sion standard, unknown, contol ‘sample and distilled w ten sat hn neers ABO he cn i tough. Ate Teast 10 min, but no more than 30 min, measure the ‘each at 660 0M. eta. of ay curve, using te procedure practiced in Experiment 13, by ploting 4, eat evs. concentration ‘and obtain the concentration ofthe unknowns and control. 0th logbook for the ‘strument used in this experiment. Record the date, your oN he experiment name OF ‘number, the R? value, and the results for the control atthe conrol sale results On ‘a control chart for this experiment posted inns EXPERIMEN JECTROPHOTOMETRIC ANALYSIS ¥ EXPERIMEN pane ‘SAMPLE FOR TOLUENE ‘ other solvent wil est in sce sigtesomainsion wih Wate B05 err > wear ety ase ; coumetic sk and five 25m volume asks These ag eee my be epred by westng with copy water pg be clean and dy. Tre water wit several ses with acetone, ang ath i wa tht allane soe Be wed ey hey ee acetone wi : cyclohexane) sock standard solution of toluene in an alkane solvent 2 Fer 1 tte fs ad dingo the mark wth the akan ae 1 kof ee pI Shake wel Ths solution has a concentration of Osmo OM eer earaten standards with concentrations of 0.0435, 00870, Orn ngo Tithe alkane solvent by ing te eck scton prepared in ep. Us et ‘elumetic sks prepared in Step 1. 4. Suan uiwown fom you nstuctr and dilute othe mark with he aan se * Rinse the remaining 25-mL lk from Step 1 with the control sample several tines tess fig the flask neal othe mark with this sample. 5. Obtain an absorption spectrum ofeach of your standards, the unknown, ante cs sample on a scanning UV/Vis spctrophotometer interfaced toa compute irda ens, fon, Follow the istructon provided for your instrument and software 6. Oban the maximum absorbance value for each spectrum and prepare the andadane (Beer's law plot) as in Experiment 13. Obtain the concentration of the unknown andi ‘contro sample, 7. Mai 1, Prepare oe 100-m instrument used in this experiment. Record the dt yt imber, the correlation coefficient, and the results forte |sample results on a control chart for this experi instructor.121: DETERMINATION OF Ni pXPERIMEN ITRATE IN Dj WATER BY UV SPECTROPHOTOMETRY NING 3 over ty se tas prepared a 50-ppm stock solution of rit 1h KN I {000 ml. of solution. on of mitogen in water by dssohing 1918 ation standards that a 0.5, 1.0, 3.0, 5.0, and 10.0 rapt ey ing te stock standard wt tld water Ae tio ent vole eyo mL of 1N Ha into each flask and shake well. + diluting to the mark, or amples if aecesary. Then, prepare them se gsm ofeach “This ean be done by ling nse frst) SoseLec ee ine ee 30m mak and then pipeting 1.0 lof the HCl tse fades aie ol sample anda blank stile vate in he sameway sates aI sgecrepotomete wih he Dark at 20 nn. Mee sons ‘alto hoon, and con) 3 lows Sing quarts covets, Messe tea _ Sind at 275 rm foreach sotion, Since dssohed organic mater may ako se iis necessary cret for nerleenc, obi votes se: sears the absorbance t 220s a sui corecton procedure forse sr adc two times the absorbance at 275 from the absorbance t 20 foreach, Fens are outside the range ofthe standards hgh dive them by an amour hat feel xing them into range and measure them again. «Pe hsandad conve as practiced in Experiment 13 by plating the esting absorbances fenand obtain the concentration ofthe samples andthe contro any water samoles prt the measurement, appl the dion actor bore eporing he es 0 the instrument used inthis experiment. Record the date, your number, the correlation coefcient andthe results forthe sample results ona contol car posted inthe aboEXPERIMENT 25: QUANTITATIVE FLAME ATOMIC ABSORPTION ANALYSIS OF A PREPARED SAMPLE Note: Your instructor will select the metal to be the analyte inthis experiment Remember to wear safety glasses 1. Prepare calibration standards of the selected metal, with concentrations suppeng, instrictor. rom a 1000-ppm stock solution. Dilute each to the mark with ds yg)” shake well 4 2. Obiain an unknown from your instructor and dilute to the mark with distill yy, shake well ™ 3. Select the hollow cathode lamp to be used and instal it inthe instrument. You in, may wish to demonstrate the lamp installation first. Also check the mixing chaniy 4” system to be sue it is ready. “ 4. A oumber of instrument variables need to be set prior to making measurements include sit, wavelength, lamp current, lamp alignment, amplifier gain, arin ‘burner head position, acetylene pressure, air pressure, acetylene flow rat, ane rate, Some instruments ae rather automated in the set up process whereas ths wp Your instructor will provide detailed instructions forthe particular instrument you ae ya. Be sure to turn on the fume hood above the flame. % 5. The blank for this experiment is distilled water. Follow the instruction provi yy, instrument for zeroing with the blank and reading the standards, the unknown, andcagy 6. Follow the instructions provided for instrument shutdown. 7. Create the standard curve, using the procedure practiced in Experiment 13, by absorbance vs, concentration and determine the concentration of the unknown andi, 8, Maintain the logbook for the instrument used in this experiment. Record the ey, name(s) the experiment name or number, the cortelation Coefficient and theres iy Contr sample. Also plot the control sample results on a control chart for his eine, posted in the laboratory. EXPERIMENT 26: THE ANALYSIS OF SOIL SAMPLES FOR IRON USING ATOMIC ABSORPTION Note: Soil samples may be dried and crushed ahead of time. If not, you may report theres an “as-received” basis. Its presumed that you have previously performed Experiment 25 or other introduc ep ment on the AA equipment. If you have not done this, carefully read through the Eset 25 procedure so that you are aware of certain precautions and instrument set-up reutee, Remember to wear safety glasses. 1. Prepare 500 ml of one extracting solution with two solutes. Diluting 25 mL of 1 NHlad 12.5 mL of 1 N H,5O, to 500 mL with distilled water. 2. Weigh 5.00 g of each soil sample to be tested into dry 50-ml. Erlenmeyer fats. Ft i of extracting solution into each flask. Stopper and shake on a shaker frat lest, 3. Filter ll samples simuitaneously into small dry beakers using dry Whatman #2 ep, transfercing only the supernatant. Do not rinse the soil samples in the fies, ste ba would dilute the sample extracts by an inexact amount. 4. While waiting forthe samples to be shaken and/or filtered, prepare standard that ae, 1.0, 30, and 5.0 ppm iron. Use a 1000-ppm iron solution, and prepare one 1ipe intermediate stock solution, Use 50-m. volumetric flasks, and use the extracting sions400 f Iso be i i control may al so be provided. Dilute it also to the m i ark with the extracti acting ition atomic absorption instrument and obtain absorb: Bs ‘ ant i sa, extracting solution for the blank. Follow the instru ‘on feacia Hr al epluone ictions provided for instrument oo ; curve, using the procedure practiced in Experiment 1 ‘periment 13, by plottin rd iB , 8 6 concentration and determine th i nce VS i ¢ je concentrati ete the ppm Fe in the soil by the following iia the unknown and con- ppm Fe (extractable) = ppm (in solution) x 4 - yintain the logbook for the instrument used i ‘ - Maintain ‘ used in this experimen It, the experiment name or number, the correlation Toaiiant andthe ire SE your . results for the conrol sample. Also plot the control sample resul posed inthe laboratory. P Its on a control chart for this experimentSY fo EXPERIMENT 23: DESIGN AN EXPERIMENT ne Meyy THE STANDARD ADDITIONS meron SOD “Ny in speriment 28, you determined the ppm Nain Soda POP sng the norma) Inperiment 2 ean be dane sig the sand ado fn gare: Te ara acd nt chp an then wit sop Ret, “ED proved asin bok x prpaig the needed 2 ig eres he nk Oa hal ome athe fe ee eet ge, Pree OW sock ang Pperetor approves your procedure, perform the experiment inthe Tabovnn nec m EXPERIMENT 30: DESIGN AN EXPERIMENT: ANALYSIS OF FERTILIZER Fog POT ‘he potassium in solid fertilizer granules can be extracted using a simp The a nie et dered yar Wie Proce vation given below, design an experiment for this ana Tah a ey on imatadure asin ater experiment inthis book for preparing the Teele) ai sep Brocetrophotomte t measure the absorbance ofeach. After your ins lations andi A re: pero he experiment nthe laboratory ce apt ‘Sample: Dry multicolored granules Samet: Pace 2.5 gna 250-mk volume atk Ad 150m | rr or 30 min, Coo), ute to volume with dated water and shake of seg, Seo 3c pa ra osm conor dey What quot 1 8 100-m. fas, ate 1 volume, and sake Henig | samples containing more than 20% KO, use smaller aliquot. ‘thoroughly fy nae aa mT ia secondny, less esitve, fe. Misused eo, ‘centration of potassium. iiss sta reparation: Prepare a stock standard with a concentration naa Be par tion of 1000 ppm rg Linear range: Up to 600 ppm.FACULTAD DE CIENCIAS BASICAS EINGENIERIAS ‘PROGRAMA DE QUIMICA (QUIMICA ANALITICA, Eldorado por: Edineld Las Cells Msc, Maui Lora Aganer Qo PRACTICA Nex ANALISIS DE HIERRO CON‘ VANTROLINA EN UN FERTILIZANTE 1. omErivo CCuaatar por esecrfconeris de absace molec en la replén vise allan ina mods de alain pz alr el cone de Neto en ‘ela. 2. FUNDAMENTOTEORICO Para les anaes, po mis imparane de abso par especies niles ela sor pr vase de ag ‘Una epaie que no abate ral vise puede converting en ot que bbs sometindola' un rescind frmain de comple oe son eompuesos eat ‘sorbate yg per amo pete tala tans ones meas en Rss. Para lanl de oes mets Js frmein decompo tne a wena de que gent scomplisne es genes seta yarn ones forma compe smo agente acompleje, cad on se pa malar povecndo ls oases ‘specs del comple deers. La enc ene Fe (Uy 1 10fenanoin par frmar un compl de colo sun ‘ndodo apopids pore determin et hlero. La ascividal mola dl cpl {(GaHlFe" es 10003 $08 nm. a eka color ex inspec tp ene Tze de 2 8. El complejo es muy esl ys abotani propa 21 ‘concern que que cpl ey de Ber ‘cama heme debe ere exo de cdc +2 2 debe agregar a mae un gente edict antes del sample, Se sa clonaodeolamin ca on elie (0) ene a uence ~ Bee N+ AO 2Fe" + 2NOH + 208" Pao mi PéginaFACULTAD DE CIENCIAS BASICAS E INGENIERIAS. PROGRAMA DE QUIMICA QUIMICAANALITICA laborado por Eaineldo Lans Ceballos. Mc, Mauro Lora Agamez Q.co Para tener pl ente 6 9 se empleaelaxato de sdio 0 amonlac, 3. MATERIALES YREACTIVOS frascoslavador ‘Agua Destlada 0 éesonizada Especrofotémetro (Cel de cuar2o 12 vasos de precptaos de 150 ml ina de enmascarar Papel secame ode cocina pipes de 5, 10,15 y 25m para de succin | {balonesaforados de $0 mL. 1 balon aforado de 200m. Balanzaanalitca Bbeacker 25 y 100 ml Pancha de clenamiento (1 pra todo el grupo) Solucén de oro-fenantoina Solucién pan de hero Solucién de clorure de hidoxamina Solucén de aceato de sodio ‘acido sulfirco concentado Solucién problema | 4. PROCEDIMIENTO reparacin de solucones: A. Diss ge 130 esa (sno sed 2, Dislver 10 de loo . Disolver 10 g de aces Pégina 2——t— FACULTAD DE CIENCIAS BASICAS E INGENIERIAS PROGRAMA DE QUIMICA. QUIMICAANALITICA Etaborado por: Edineldo Lans Ceballos. M.sc, Mauricio Lora Agamez.Q.co D, Preparacién de a muestra: Pesar 0,3 g de frilizante en un beacker de 100 mL, agregar agua y 3 mL de acido lothiieo concentrado, calentar un poco con el recpientetapad,filrar y hacer lavados ‘on agua deslaa ria hata aproximadamente 80 ml recoglendo el agua dels lavados en ‘un balon de 200 ml completa a volume con agua destilada. De la slucién anterior tomar 10 ml. en un balén de 200 mL, agregaleen el orden que se da: 1.5 mL de solucén de hidroxilamina, 12 mL de acetato de sodio y 15 ml. de ‘ortofenanroina, completar a volumen con agua, agitary dejaren eposo durante 10 minutos ants de hacer el andlss 4.1 METDO DEL ESTANDAR EXTERNO reparacin de las solucionespatré "Nota: Para la solucién made de hierro deben hacer los cileulos correspondientes de los gramos a tomar del reactivo que contenga hierro, adicionar ests gramos en un Dalin aforado de 200 mL, adiionar 50 mL de agua destilada y eguidamente 25 ml de acid sulfrico concentrado y afore. ‘A paride una soluein madre de 10 mg FL, tomar en balones de 50 mL 135,10, 15 mL, ‘agregar a cada ban en el orden que se da: 0.5 mL de soluci dehidroxlamina, 4 mL. de ‘acetato de sodioy 5 mL. de ontofenantrolina, completar a volumen con agua, agit dejar fen epoco durante 10 minutos anes de hacer el anlisis. De igual forma prepara un blanco tomando 10 ml. de agua destilads, y reper el procedimiento anterior ‘Tome una de las soluciones ptrén preparadas ancerirment,realice un barrio entre 400 y 600 nm haciendo lecturas cada 10 nm. Regs las absorbancia en cada lecturay relic el espero de absorcin, CCon base en el espectro anterior, seleccionar la ongitud de onda de- maxima absorbancia Esta constuye I longitu de onda de abajo. ~ de ig Pei, de Pagina 3 isFACULTAD DE CIENCIAS BASICAS F INGENIERIAS PROGRAMA DE QUIMICA QUIMICAANALITICA "laborado por: Field Lans Cellos. Msc, Mauricio Lora Agamez Qc Realce lectus de absoebanica tes veces minimo de cada uno de os patranes preparatos neler Haga el mismo procelimint con muest. 4.11 Cuestionario 1. Hallar Is concenracin de Fe en% pip_yen mg ques encuentra en el eriizante repore Ia inceridumbre dela medi. 2. Halle 4) pndiente de a recta y su esa standar ») eoeticeme de deteriancién «)iterept ys desvacdn estan los resiusles ©) Bractud del medida 42 METODO DELAADICION ESTANDAR 421 Método grafic ‘Tomar 5 balones de 50 mL, adicionar 3 cada uno 10 mL de moesray sepuidamente 0.0; $50,100; 1500) 20.0 ml. dea solcion made. Agregar a cada balén en el orden que sed OSL de solveién de hidroxlamina, dma. de acetao de sod y $m de oofenanoli completar a volumen con agu, agar y dear en reposo durante 10 minutos antes de hacet {als de igual forma preparar un blanco tomand 10 mL de agua desis, y repel procedimiento anterior 4214 Cuestionario 4) Responda ls mismas preguntas el custontio 4.1.1 422Método por célculo ‘Tomat 2 balones de 50 mL adiionar a cada uno 15 mL. de muestra y seguldamente 0.0 y 1200 mia de a solucién madre de 10 mg Fe/L, ademas agregar a cada balén en el orden Pagina 4labora por: aid Lans Cellos. Mac Mauricio Lora Agamez Qo 'FACULTAD DE CIENCIAS BASICAS E INGENIERIAS [PROGRAMADE QUIMICA Quimica ANaLimica, {que sed 05m de solu de Moulin, 4 mi 6 aeatoe sdioy 5m de ‘ofenanolina, complear a volamen con ap, agar y dar eh repos durame 10 ros ares de hace el ais, de gual frma prepara un blanco remand 10m. de ‘gun desing, yepetielproedintoatri, 422, Cuestionario 2) ls concentra de Fe en 6 en ppm. by Hara exact 2} Cl eas tes modo de cuauitiecin es mis exaco { cCusndoy por qe stu el co de con estan y pa cen? . 10) Sis soon de su moesza problema ene una absrtacl por eina 0 por dao de fs abate de 1s slucines patton gt ‘eta pede tener ean en el eilado el ais y como se slusona S.mmLIORAFIA 1 Pésina aris DC. Amal quinio camiavo. 2 el, Bacon: Revere S.A: Raymond PW. Sct. reples nd practice of ehromatorahy, Crom ‘ook Series, COPYRIGHT 2003. indar Methods for he examination of wate and wastewater ead por “Aad E Greenery oes 1882 Publsdo pr Pubaton ice Amerian Pubic Heat Associaton ec, US.A