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  • Analysis of CA MG

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    Nafisa Meisa
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    Analysis of CA Mg removal by resin

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    Analysis of CA Mg

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    Analysis of CA Mg removal by resin

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    © All Rights Reserved
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    Sinalizar o conteúdo como inadequado
    74 visualizações14 páginas

    Analysis of CA MG

    Enviado por

    Nafisa Meisa
    Analysis of CA Mg removal by resin

    Direitos autorais:

    © All Rights Reserved
    Baixe no formato PDF ou leia online no Scribd
    Sinalizar o conteúdo como inadequado
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    lon-Exchange Resins: Analysis of a Calcium, Magnesium, or Zinc Salt ‘To become acquainted with the technique of ion-exchange chromatography and some ofits applications. Apparatus balance 250-ml. Erlenmeyer flasks (3) 100- and 250-mL beakers 50-mL burets 2) buret clamp and ring stand glass wool glass rod (long) polyethylene bottle PH paper ‘weighing paper Chemicals, cation-exchange resin distilled water (Dowex 50W-X-8) phenolphthalein 6MHCL indicator solution ~0.1 MNaOH potassium hydrogen unknown calcium, magnesium, phthalate (KHP) or zine salt 1. lon-Exchange Theory Chromatography is one ofthe more important and versatile techniques aval- able to separate the components of a mixture. Chromatography is a physical ‘means of separation in which the components of a mixture become distributed between two different phases. These two phases are commonly called the stationary phase and the mobile phase. The mobile phase is usually a liquid or a gas, whereas the stationary phase is usually a solid. Ifthe stationary phase is 2 polymer that possesses exchangeable ions, such as those illustrated in Figure 1, then the chromatographic technique is called ion-exchange chromatog- raphy. Polymers with exchangeable ionic functional groups have become known as ion-exchange resins. These ion-exchange resins are long-chain poly mers that contain polar functional groups and have no appreciable water sol- ubilty. They come in the form of spherical beads that swell when placed in contact with water, o thatthe water solution can enter the interior ofthe bead andl come into intimate contact with these functional groups. The polar func- tional groups are strong electrolytes and are thus completely ionized when in contact with water solutions. fons of like charge equilibrate between the solu- tion and the resin according to Equations (1] and [2} RH") + M*(aq) == R,M*(9) + Hag) 0 R*OH™(s) + X(aq) == R,*X(s) + OH(ag) 2 From Laturatory Experinents, Tenth Elion, Jon H. Nelson and Kenneth C. Kemp. Copyright ‘Sante by Pearson Education Ine Published by Prentice Hall ne All ights reserved, Experiment 1 | OByECTIVE APPARATUS AND CHEMICALS | DISCUSSION lon-Exchange Resins: Analysis of a Calcium, Magnesium, or Zinc Salt Experiment 1 To become acquainted with the technique of ion-exchange chromatography | OBJECTIVE and some of its applications, Apparatus sot Et APPARATUS balance mL Erlenmeyer flasks (3) 100- and 250-mL beakers 5o-mL burets @)” AND EMICALS buret clamp and ring stand glass wool glass od (long) polyethylene bottle pH paper weighing paper Chemicals cation-exchange resin distilled water (Dowex 50W-X-8) phenolphthalein 6MHCI indicator solution ~0.1MNaOH potassium hydrogen unknown calcium, magnesium, phthalate (KHP) or zine salt 1. lon-Exchange Theory Chromatography is one of the more important and versatile techniques avail-_| DISCUSSION able to separate the components of a mixture. Chromatography is a physical ‘means of separation in which the components of a mixture become distributed between two different phases. These two phases are commonly called the stationary phase and the mobile phase, The mobile phase is usually a liquid or a {gas, whereas the stationary phase is usually a solid. Ifthe stationary phase is 2 polymer that possesses exchangeable ions, such as those illustrated in Figure 1, then the chromatographic technique is called ion-exchange chromatog ‘raphy, Polymers with exchangeable ionic functional groups have become known as ion-exchange resins. These ion-exchange resins are long-chain poly- mers that contain polar functional groups and have no appreciable water sol- ubility: They come in the form of spherical beads that swell when placed in contact with water, so thatthe water solution can enter the interior of the bead and come into intimate contact with these functional groups. The polar func- tional groups are strong electrolytes and are thus completely ionized when in contact with water solutions. Ions of like charge equilibrate between the solu- tion and the resin according to Equations [1] and (2} RH) + M*(aq) = R,-M*(s) + Haq) a R,"OH™(s) + X"(aq) ==R,*X"(s) + OH"(aq) 2 From Latorston Espernets, Tenth Eto, John H. Nelson and Kenn C. Kean. Copyright [© une by Pearson Education nc. Published by Prone Hal ine All rights reserved 10 on-Exchange Resins: Analysis of a Calcium, Magnesium, or Zinc Salt [—CH —CH, —CH —CH, —1, cH Cl J ao 99 SOcH? SO; NICH)" NICHs on on cation-exchange resin ‘Anion-exchange ren (RH) (R-OH) A FIGURE 1 lon-exchange chromatographic resins where R, symbolizes the resin, A resin that behaves according to Equation Ili called a cation-exchange resin, and one that behaves according to Equation [2] is called an anion-exchange resin. In general, the positions of these equilibria are influenced both by the nature and the concentrations of the ions in solution. Tons with a greater positive charge and a smaller size fond to have a greater affinity for the cation-exchange resin than do larger i ions with smaller charges. As shown in Equation [1], one H” ion s liberated i for each M* cation. Two H* ions would be liberated for each ‘M** cation, three H* ions for each M™* cation, and so forth. Thus, the extent ‘of exchange bf eations with H- on a resin would be expected to decrease in the orders: Thi > Alt > Ca®* > Na* and Cs* > Rb* > K* > Nav > Li*. In the latter series there appears to be a discrepancy because we expect the Cs" ion tobe larger than the Liv ion and thus to have a smaller charge density. How- fever, the Lit ion is hydrated and is tightly bound to six HzO molecules, SGhereas the Cs" ion is bound to only four H,O molecules, making the {Li(4;0).|* ion larger than the [Cs(H;0))" ion. Tn the same way, when small, highly negative anions come into contact swith an anion-exchange resin, they liberate one OH” for each negative Charge. Thus we would expect the position of equilibrium [2] to be influ ghee by the charge density ofthe anion aso. As. consequence, since anions gre not so tightly Bound to HO molecules as are cations, we expect the ex tent of exchange of anions in solutions with OF ions on the resin to de- crease in the orders: F> > CI” > Br’ > I” and PO, > SO > Cle, | for example. Because ion-exchange resins possess the ability to remove ‘ations and anions from water and replace them with H” or OH” ions, rex spectively, ion-exchange resins are commonly used to deionze water and to i soften water You may have a water softener in your home; if you do, you Should recognize that it is usta large container of cation-exchange resin IL. Hard Water ‘The term hard water has its origin in the fact that mineral impurities such as Ca, Mg2™, and Fe", which are frequently present in natural water, react with soap to form gummy precipitates. They also react with COs" and 50,2 in the water to leave what is called a biler sale (CaCOs, MgCOs, oF ‘CaS0,) on walls of the vessels in which hard water is boiled. Ordinary soap is 2 water-soluble sodium (solid soaps) or potassium (liquid soaps) salt of a on-Exchange Resins: Analysis of a Calcium, Magnesium, or Zinc Salt long;chain organic acid, RCO;H, such as sodium stearate, C;sHs¢CO:Na Sodium stearate reacts with Mg? or Ca? ions to form a sticky, insoluble precipitate according to Equation (3) 2CypHasCO3 (ag) + Ca?*(ag) = CalCy7H3=CO3)2(8) BI ‘This results in waste ofthe soap and the formation of an undesirable film on items that the soap is used to clean. You may have observed the formation of such a precipitate and the fact that soap does not form much of a foam or lather in hard water. Suppose, then, that a solution containing calcium chloride, CaCl, were slowly passed through a bed of cation-exchange resin contained in a column, In this case equilibrium [4] would occur 2RH*G) + Ca?(ag) + 2C aq) [Re )2Ca* Js) + 2H"(aq) + 2c) — ta) The eluate, or solution, coming out ofthe column (Figure 2) would contain HT and Cl" ions, and the Ca** ions would be retained by the column because their affinity for the resin is greater than that of the H1* ions. If this eluate = oe Fresh vet Dp 2 Column packing ‘Statonay pas) rai totvent be ass 8 8 Seven fo cutie o ‘FIGURE 2 (a) lon-exchange chromatography: ths is an example of an anion-ex- ‘change resin, since only anions can be atracted to it. (b) Schematic epresentaton of ‘2 chromatographic separation. The salute witha greater affinity fr the stationary Phase remains on the columa longer. " cry lon-Exchange Resins: Analysis of a Calcium, Magnesium, or Zinc Salt were then passed through an anion-exchange resin in the OH™ form, then tquilibrium [5] would oecur on the column: 2H" (ag) + 2CI"(ag) + 2RLOH) 2RACI(6) + 2H"(aq) + 20H"@q) “Thus, passing a CaCl; solution successively through a cation- and then an sae Eishange resin would produce a solution containing neither Ca"” nor aaeorrne in the eluate. Since OH ions react with H” ions according to Equa- tion (6), the eluate would be pure water: HY(@q) + OH" (aq) — 1200) (6) ‘Water treated in this way is said to be deionized. Tr onder to carry out such a process in actuality it is necessary to have a large volume of resin with respect to the volume of solution, because fone raechange resins typically have an exchange capacity of only about 5 mmol/s sna diy basis. Also, it is necessary to have a long contac time between the sation and the resin so that all the ionic sites on the resin may contact the se im solution. Thus we generally use a column such as illustrated in i Figure 2 and slowly pass through it the solution tobe exchange Tenexchange resins are useful not only for separation and purification purposes, but also for analytical purposes. Suppose you passed a solution PeMaining a known mass of pure soluble calcium salt (which contained an coknowrramount of calcium) through a cation-exchange resin. Equilibrium [7] would occur on the column: IR,-H*) + CaP(aq) — [Re 2Ca* Ils) + 2H") am “The liberated H1 inthe eluate from the column could be determined by 2 sinle aches tation witha standard NaOH solution. Assuring that all the Ca? was captured by the column, the caleium content of the sample can be easily calculated. Exampte 1 TR 204g sample ofa soluble calcium salt was passed through 2 cation, ‘cchange column in the H” form, The H” i the elute required 2622 ml of oias RY NaOH to reach a phenolphthaein end point. Calculate the percentage calcium inthe origina sample. SOLUTION: The acid-base reaction is H"(aq) + OH"(as) — H010. iL Vo cxsan( aie) 688 « 19°? mol ‘smal H* (see Equation (7) 22.688 x 10 mol moles HY moles C3 34 10 mol 1.344 x 107 mel} $0.08 g/mol) 53.87 x 107g 5387 X 107 gC scat (Siege = 18.32% Ca Record all data directly onto the report sheets. x9 | 13 Ion-Exchange Resins: Analysis of a Calcium, Magnesium, of Zinc Salt In this experiment, you are to determine the percent calcium, magnesium, | PROCEDURE ‘or zinc in an unknown by performing a cation exchange followed by an acid base titration of the eluate. Your instructor will tell you which cation you are determining. You will first standardize your base sofution (NaOH, the titrant). Preparation of Approximately 0.100 M Sodium Hydroxide (NaOH) Heat 500 ml. of distilled water to boiling in a 600-mL flask,* and after cooling under the. | PROCEDURE toater tap, transfer to a. I-pint bottle fitted with a rubber stopper” (CAUTION: Concentrated NaOH can cause severe burns. Ifyou come in contact with itim- ‘mediately wash the area with copious amounts of water) Add 3 mL of stock Solution of carbonate-free NaOH (approximately 19 M) and shake vigorously fora last 1 min, Preparation of a Buret for Use Clean a 50-mL buret with soap solution and. a buret brush and thoroughly rinse with tap water. Then rinse with at least five 10-mL portions of distilled water. The water must run freely from the buret without leaving any drops adhering to the sides. Make sure that the buret does not leak and that the stopcock turns freely. Reading a Buret All liquids, when placed in a buret, form a curved menis- ‘cus at their upper surfaces. In the case of water or water solutions, this ‘meniscus is concave (Figure 3), and the most accurate buret readings are ob- tained by observing the position of the lowest point on the meniscus on the graduated scales, “To avoid parallax errors when taking readings, the eye must be on a level with the meniscus, Wrap a strip of paper around the buret and hold the top edges of the strip evenly together. Adjust the strip so that the front and back a White paper Meniscus A FIGURE 3 Reading a buret “The water fs boiled to remove carbon dioxide (CO), which would react with the NAOH and change ts molarity "A rabber stopper shouldbe use ora bottle containing NaOH solution A strongly aaline soliton fence To cement» glass topper so ful that is felt o remove iaeonnisniee soos alienate a 4 on Eachange Resins: Analysis of Calcium, Magnes, or Zin Salt edges are in line withthe lowest part of the menisc and take the reading by edges ing to the nearest tenth of a marked division (O° ‘mL.).A simple way Sf doing this for repeated readings on a buret is illustrated in Figure 3 A. Standardization of Sodium Hydroxide (NaOH) Solution Prepare about 400 to 450 mL-of COs-ree water By Dot for about 5 min. To Prepare pena an additional 400 mL of COr-free water or st ‘Cy boiling, see agh from a weighing bot (your lab instructs) show you how sec raging bottle if you don’t already know) Wipes ‘samples of be- toe and 0 g each of pure potassium hydrogen prAn=IS (KHP) into Three separate 250-ml. Erlenmeyer asks: accurately ‘weigh to four signifi- ais figures." Do not weigh the flasks, Record the masses ‘and label the three cant jer to distinguish among them, Add to cach samp about 100 mL. sae iled water that has been freed from CO? by Boling ‘and warm gently of ising unt the salt is completely dissolved, Add fo each flask two “rops of phenolphthalein indicator solution, OP ot Pe previously cleaned buret with atleast four Sn PTO, of the: approximately 0.100 M_ NaOH salution that YO hhave prepared. Discard SEEN portion into the designated receptacle. Do oy is At ofthe washings «2c Pe, Completely fil the burt with the solution and SN the air ttn he tip By running out some ofthe liquid info an PY. ‘beaker. Make from re he Tower part ofthe meniscus is at the Zero mark OF slightly lower. Se the ict to stand for at Teast 30 sec before reading the ar position aoe Meniscus. Remove any hanging drop from the Eure AF by touching it on rity of the beaker used forthe washings. Recard the in ial buret read- jing on your report sheet Ey add the NaOH solution to one of your Maske of KHP solution wile gently swirling the contents ofthe flask, a8 illustrated in Figure 4. AS ‘evel of meiscus rullthe stopeockin against Teler enc sime you ri Ashetof wt apes Genet ro sw he ask onto help in reer P sn col Sint one drop of HErant cases changeattheend pont at one tru he ‘A FIGURE 4 Titration procedure. sa cas where te ase of sample flange than LE S6 Se to weigh only to the FS A rE ean he ne ngs er a 10 mL epi oN ‘ages. lon-Exchange R the NaOH solution is added, a pink color appears where the drops of the base come in contact with the solution. This coloration disappears with swirling. As the end point is approached, the color disappears more slowly, at which time the NaOH should be added drop by drop. Itis most important that the flask be swirled constantly throughout the entire titration. The end point is reached when one drop of the NaOH solution tuens the entite solu- tion in the flask from colorless to pink. The solution should remain pink ‘when it is swirled, Allow the titrated solution to stand for at least 1 min so the buret will drain properly. Remove any hanging drop from the bueet tip bby touching it to the side of the flask and wash down the sides of the flask with a stream of water from the wash bottle. Record the buret reading on your report sheet. Repeat this procedure with the other two samples. Dis- ‘pose of the neutralized solutions as instructed, From the data you obtain in the three titrations, calculate the molarity of the NaOH solution to four significant figures as in Example 2. ‘The three determinations should agree within 1.0%. If they do not, the standardization should be repeated until agreement is reached. The average of the three acceptable determinations is taken as the molarity of the NaOH. Calculate the standard deviation of your results. SAVE your standardized solution for the unknown determination Part B. kee KHP is a monoprotic acid with the acidic hydrogen bonded to oxygen and. has a molar mass of 204.2 ‘The balanced equation for the neutralization of KHP is given in Equation [8} KHCgH,Og(aq) + NaOH(0q) —+ H;0(0) + KNaC3HOs(aq) [8] In the titration of the base NaOH against KHP, an equal number of moles of KHP and NaOH are present at the equivalence point. In other words, at the equivalence point moles NaOH = moles KHP °) The point at which stoichiometrically equivalent quantities are brought together is known as the eguizalence point ofthe titration. It should be noted that the equivalence point ina titration isa theoretical point. It can be estimated by observing some physical change associated ‘with the condition of equivalence, such as the change in color of an indicator, which is termed the end point, 3s: Analysis of a Calcium, Magnesium, or Zinc Salt 18 canner 16 lon-Exchange Resins: Analysis ofa Calcium, Magnesium, or Zinc Salt EXAMPLE 2 Whats the molanty of a NaOH solution i 35.78 mL of if required vo neutral ize 1070 g of KHP? SOLUTION: Recall from Equation [9] that at the equivalence point the numer SPmmoles of NaOH equals the number of moles of KHP, 1 mol KP, 3042.3 KAP. because this is exactly the mmber of mols f NAOH thas contained in 3875 ‘mL of solution, its molarity is: 240 x 10° mol KHP 5.240 x 10"? mol NOH 91455 M NaOH Ce 008575 B. Preparation of the Ion-Exchange Column and Determination of Cation ‘Weigh out about 7 to8 g ofthe cation ion-exchange resin to the Nene Ee Weigh ont ot be inthe acid form. In order to ensure that itis slurry Pe The i rn Erlenmeyer flask with a mixture of 30 ml of 6M HC and. resin 2 polled disilled water Allow the surry to stand, with ocasionsl tng, for 15 min. Then decant the acd solution and wash he Fatt with: FaeepeaL portions of boiled dstiled water, decanting the wash guid after es washing, Finally add 50 mi. of boiled distilled water to thé re Dane Tong wire or glass od, push a small plug of cotton to Whe bot of saben buree Then put 5 mLof boiled distilled water on top of he <4, oa rct clamp the buret vertically ina buret clamp on a ring 804 and. aera esti resin slury to the buret, with the aid of more boiled distilled transfer the tee Drain off excess water occasionally from the bottom of vat i Nover allow the liquid level n the buret to fall below the evel of the burt ee this usually causes channels to develop in the resin co Mew and greatly reduces its efficiency. Wash the resin by allowing boiled dis: aon so flow through it unl the pH of the effluent is the same 95 pH ofthe boiled distilled water (use pH paper to check the ‘pH of the boiled Peo Sater andthe eluate). Then drain water from the Puret until he water level is just barely above the top of the resin. ee aca sample ofa soluble calcium, magnesium, oF 2ine sat from Your lntopnury instructor. With the aid of weighing paper, weigh out © he eas, aaporttigvarn approximately 0.15 gof this salt. Transfer the weighed S210 ae rn Brakerand diolve it in about 20 ml.of oiled distilled wate, Tere: soo eit latin to the ton-exchange column. rine the beaker twice Wh Sinl portions of deionized water, and add the sinsings to he ion-exchange er porte liquid level begins to reach the top ofthe column, drain

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