University of Technology Petroleum Technology Department Analytical Chemistry Lab Guide For: First Stage suction A variety of apparatus used for bulb for accurate measuring liquid volumes and for for safe measuring Preparing end manipulating solutions ppetwne nd titrations @ ‘stopper fete ‘i 3) calibration 3) : i calibration measuring "mark burette ~calibrat . pipette efor Qo @ 100 cm? or ml 250 em? or ml @ @ © © A conical beaker flask graduated-volumetric flask By Dr. Najem Al-Rubaiey Lec. Rana A.Azeez Eng. Shahnaz Bassim Khazil Chem. Hayat Emad Hamdi Scanned with CamScanner_ eee Introduction:- This manu: q experiments for the first department which includ glassware with their nomenclatur Laboratory brief theoretical background and year student 0! les the most important ey Chemical Safety in the Conduct and also the experimental proc chemical Analytical Chemistry aot [vs se ef Ss O17 al describes Analytical hemistry laboratory f Petroleum Technology types of chemical edures with a equations Scanned with CamScannerLaboratory Report: 1. Cover Page: Title of the experiment, identify yourself and your partners and Date of Performing the experiment. 2. Purpose or Objective 3. Theoretical Basis. 4. Apparatus and materials required. 5, Results and calculation. 6. Discussion. 7. References. Scanned with CamScannerChemical Safety in the Laboratory:- There are a number of rules that must be followed in order to work safely in a chemical laboratory. Some of these rules are listed below. 1. Always wear your laboratory while working in the laboratory. 2. Always check the label on the bottle before using a chemical reagent. 3. Never taste a chemical or a solution, many laboratories chemical are poisonous 4. Keep your face at a safe distance if your experiment generates an objectionable gas. Work under the suction hood. 5. Don't pick hot objects with your bare hand. If your hand is bumed, use some burn ointment 6. Avoid using bare hand in the transfer of chemicals. 7. In the event of malfunction in any tool or device within the laboratory must inform the offices and not repaired by the student. 8. Wash your hands well before leaving the laboratory 9. To avoid spattering of acids which can cause burns, always add acid to water. Never add water to acid. 10. Before obtaining any reagents, carefully read the labels on the bottles twice. Many chemicals have similar names or concentrations may vary. 11. To avoid unnecessary waste, obtain only the amount of chemicals | called for in an experiment. Your instructor will tell you the proper procedure for dispensing liquids and solids. Never insert medicine droppers or scoops into reagent bottles, 12, Never return unused chemicals to the original dispensing bottle. Scanned with CamScannerAnalytical Chemistry ot Analytical chemist: z Analytical chemistry is often described as the area of chemistry responsible for characterizing the composition of matter, both qualitatively (Is there any lead in this sample) and \ quantitatively (How much lead is in this sample). As we shall see, this description is misleading. c Analytical chemistry: is the study of the separation, | identification, and quantification of the chemical components of L natural and artificial materials. 1-Qualitative analysis. determines the presence or absence of a particular compound, but not the mass or concentration. By definition, qualitative analyses do not measure quantity. gives an indication of the identity of the chemical species in the sample, 2- Instrumental methods use an apparatus to measure physical quantities of the analyst such as light absorption, fluorescence, or conductivity. The separation of materials is accomplished using chromatography, electrophoresis or field : flow fractionation methods. Analytical methods can be separated into classical and instrumental. Classical methods (also known as wet chemistry methods) use separations such as precipitation, extraction, and distillation and qualitative analysis by color, odor, or melting point. Classical quantitative analysis is achieved by measurement of weight or volume. 3-Quantit analysis 1-Gravimetric analysis Gravimetric ‘analysis involves determining the amount of material present by weighing the sample_ before and/or after some transformation. A common example used in undergraduate education is the determination of the amount of water in a hydrate by heating the sample to remove the water such that the difference in weighit is due to the loss of water. Scanned with CamScannerAnalytical Chemistry 2-Volumetric analysis Titration involves the addition of a reactant to a solution being analyzed until some equivalence point is reached. Often the amount of material in the solution being analyzed may be determined. A Titration is a method of analysis that will allow you to determine the precise endpoint of a reaction and therefore the Precise quantity of reactant in the titration flask. A burette is used to deliver the second reactant to the flask and an indicator Volumetric methods may be based on I- Neutralization (Acid/ Base) reactions. The organic compounds containing the acidic group are analyzed by this titration. This is based on the neutralization reaction between acid and base. An acid-base indicator is used to detect the end point which indicates the completion of reaction between acid and base by changing the color of the mixed solution, [The Types of acid /base rea 1. a- Strong Acid Against a Strong Base ‘ For example, titration of HCl and NaOH b-Strong Acid against Weak Base For example titration of HCI and Na,CO; c-Strong acid against mixture of strong and weak base For example titration of HCI and( NaOH, Na,CO;) d-Strong base against weak acid For example titration of NaOH and CH;COOH e-Back titration = Scanned with CamScannerAnalytical Chemistry 2-Precipitation Reactions. Precipitative volumetric analysis relies on the formation of solid phase with a very low solubility product constant. In _ environmental analysis, it may be used. for chloride determination. Specific indicators are used to detect excess silver or mercury 3-Complexation Reactions. Complexometric titrations often employ _ethylenediaminetetraacetic acid or EDTA [HOOCCH,),NHCH,CH;NH(CH,COOH),]. This is a hexadentate ligand which binds very strongly to many metals. For calcium and total hardness determination, a couple of specific dyes are used to determine the presence of excess cation. 4-Redox Reactions. Many _oxidation/reduction based volumetric methods employ the iodometric method. This involves the oxidation of iodide to iodine and subsequent titration with sodium thiosulfate using starch as an indicator. Many of these employ a series of redox reactions. *The selection of indicator is very important in acid- base titration because the equivalence point is determined by the stoichiometric of the reaction whereas the endpoint is measured by changing the color from indicator. The reaction is neutralized but it is not necessary to come to theend point at pH = 7. The completion of the reaction depends on the strength of acid and base. Scanned with CamScannerAnalytical Chemis, ny Methods to Determine the Endpoint S w . pH indicator - This is a substance which shows the chemical change by changing the color. A Stiaan ieee This is used to measure the electrode potential of the solution. These are used for redox titration. They show the end point with changing potential of the working electrode. pH meter - It is a ion-selective electrode. In pH meter the potential of electrode depends on the amount of H+ ion present in the solution. The pH of the solution can be measured in the whole titration. This gives more correct result than indicators. Conductance -The conductivity of solutions is also changed in titration and it depends on the ions present in the solution, mobility of ions and ions concentration. . Color change- In the redox reactions, the color of solution changes without use of indicator. This is due to different oxidation states of the product. Scanned with CamScanner Poly \Analytical Chemistry Volumetric (Titrimetric) analysis:- Volumetric analysis Titration is the slow (or Quantitative chemical analysis): addition of one solution of a known Concentration (called a titrant or titrator) to a known volume of another solution of unknown Concentration (called a titrand or analyte) until the reaction reaches neutralization, which is often indicated by a color change. 1- The process of adding the standard solution until the reaction is just complete is termed a titration, _ 2- The solution of accurately known strength is called the standard solution. > 3° The standard solution i’ usually added from a’ graduated vessel called a burette. 4- The reagent of known concentration is called thetitrant, and the substance being titrated is termed the titrand. 5- Equivalent point is the point,in a-titration where'the amount of standard titrant added is chemically equivalent to the amount of analyte in sample. 6- End ‘point is the-point in a’ titration whet an observable change.that signals of the titrant’s aniount_added is chemically equivalent to the amount of analyte in sample. 7- Indicator is a reagent used to indicate when the end point has been reached 8- A primary standard is a highly purified compound that serves as a reference material in all volumetric titrimetric methods. r Scanned with CamSc: annerof the Motaity oF Base Solution Total volurie of petermination ‘an Acid oF the 4. Select TYPE 2. Lich with ! select Pere (one 6 Odd ostengaadve.sronanese ‘oweatatdys. 1009 889° opase 6. After Titration, ‘calculate and Enter Molarity of 4, Select the Indleator ‘Ovetny orange (Phenotphinateln Molarity of. Volume of How can calculate Equivalent weight (1)Equivalent weight in neutralization reaction: - The equivalent weight of the acid is equal to the molecular weight of the acid divided by the number of hydrogen atoms Replaced acid into a draw reaction Hil—» Ht + CL So ihe weight equivalent of hydrochloric acid = 1/36.5= 36.5 gm/ eq ~ The equivalent weight of the base equal to the equivalent weight of the base dividedThe number of substituted hydroxyl groups in a draw reaction NaOH ——*Na* + OH” Scanned with CamScannerAnalytical Chemistry So equivalent weight of sodium hy i ! i ydroxide= 1/40 = ; ne ete weight of salt is equal to the sess watts e salt divided by multiplying the numb i RECO BN COL er of cations a weight sodium carbonate equal = 2*23 + 3*16+12= So equivalent weight= 106/2 = 53 gm/eq (2) Equivalent weight in Oxidation —Reduction: The equivalent weight of an oxidant or a reducing is the number of electrons which 1mol of the substance gains or losses in the reaction. Calculate the equivalent weight of the worker oxiding agent reducing agent That divides the molecular weight of the material on the overall change in the number of oxidation of the elements or the number of electrons transmitted through the half or interaction r207-+6 Fe *** 14H"... ace + +6Fe ** + 7H 20 This change in the interaction of a number of oxidation of the chromium atoms to so the equivalent weight of a substance second potassium chromate is equal to the molecular weight : divided by the Overall equivalent weight in these interactions is equal to the molecular weight of the material divided by the product of ‘the change in rewards given cation in the number of the cation Scanned with CamScannerAnalytical Chemiays Contents Exp.No.1 Preparation of Standard Solution Exp.No.2 Preparation of Secondary Solution Exp.No.3 Titration of Hydrochloric Acid with Sodium Carbonate Exp.No.4 | Titration of Hydrochloric Acid with Sodium Hydroxide Exp.No.5 Titration of Mixture (base strong and base weak) with Acid Strong Exp.No.6 Acidity of Vinegar Exp.No.7 Oxidation - Reduction Reaction Exp.No.8 Identification of First Positive Group (Silver Group) cn NE LET Scanned with CamScannerner TmaRTcms rere ansnninnanins Analytical Chemistry Experiment(1) Preparation of Standard Solution” e Primary standard solution: ~~ The primary standard is a highly purified compound that serves as a reference material in volumetric and mass titrimetric methods. The accuracy of a method is critically dependent on on the properties of this compound. Important req requirements for . Primary standard are the following Standard materials are classified into:- 1- Standard materials primary 2- Standard materials secondary Important requirements for primary standard compounds are: ¢ Extremely pure ( high purity .e.g/ 99.9% by weight). ¢ Highly stable( Atmospheric stability). i ¢ Anhydrous ( Absent of hydrate water), i ° Less hygroscopic a ¢ High molecular weight relatively. ° Can be weighed easily. Should be ready to use and available. Should be preferably non toxic . ° Should not be expensive (modest cost). Interaction with the substance to be a quick appointment with a clear end point Scanned with CamScannerSB ic s Analytical Chemis i J In practice, it is difficult to get a typical standard tule applies all the conditions that were mentioned, but it is necessary to take account of these conditions when choosing a primary standard ~~ example: one of such compounds is sodium carbonate (Na 2C03) Procedure: To prepare 250ml of 0.1N Sodium carbonate (Na 2Co;). 1- We find the Weight of sodium carbonate of normally law and weighed by the delicate balance, 2- Movement quantity weighted to Baker glass is then added to baker of distilled water and sodium carbonate solution is transferred to a Volumetric flask capacity 250ml and uses glass road Therefore, and wash the baker and Blass road several times added material Washing the volumetric flask , 3- Add water to the Volumetric flask to the extent mark and then Shake solution, : Calculation: + 2NaHCO;+ NaCL NaHCO;+ HCL—» NaCL+CO,+H,0 In this reaction one mole of hydrochloric acid equivalent with sodium carbonate and converted into sodium bicarbonate. The second mole of hydrochloric acid converts the produced sodium bicarbonate into sodium chloride, water and carbon dioxide gas which evolves to the atmosphere. The two equations can be assumed and re-written into the following reaction Na ,CO;+HCL—+ NaCL+ H,0 + CO, Scanned with CamScannerAnalytical Chemistry Procedure: Atocedure; 1- Transfer 10 mi of 0.1 N Na Ci i I . ‘0. omisitae: iy pipes 2\-V3 Solutions to the 250mi 2- Add 2-3drops of methyl Orange as indicator, 3- Full the burette with hydrochloric acid solution (unknown normality), 4- Titrate the solution drop wise uni til the pale yellow colored solution converts to orange colored s olution. 5- Record the volume of hydrochloric acid Calculation: (Na COs) (HCL) N*V = M*y, Discussion: 1- Why is used Na 2CO; with HCL in this Titration? 2- Why use methyl orange M.O indicator in this Titration? 18 Scanned with CamScannerey iment? Exp! : lorie Acid with Sodium Titration of Hydroc”. Hydroxide i issolve after ide] ‘1 stals quickly disso! ium hydroxide is a white cry’ I eed ag ie atmosphere, and even uring wee standard not be used as a solution first record with on dvoid ca solution of diluted hydrochloric acid and so a Secon be standardized calculation according to the following L + H.0 NaOH + HCL—* NaC Procedure: 1+ Transfer 10ml of sodium hydroxide solution into a 250ml conical flask by pipette. 2. Add 2-3 drops (ph.ph) indicator. 3+ Full the burette with hydrochloric acid standardized solution 4- Titrate drop wise with continuous shaking until one drop of the acid converts the pink color base solution into a colorless solution. Calculation: Determine the normality of sodium hydroxide solution using the formula: (NaOH) (HCL) NM * VW = Nm * WV N=? NaOH Scanned with CamScanner #1— = 1- Why standard; : normality dardize the HCL before determination the NaOH 2- Defined the indicators, 3- What are the colors of solutio: indicator (M. ns when using methyl orange : 0.) and Phenolphthalein indicator (phph), > i NaCO,, and why? amount of more than one directory in the 4- What kind of solution is: HCl, NaOH, 5- Do you use affects the Process Titration? why? 6- Why it is used HCL? ph.ph as indicator in the Titration process NaOH and 7- Why is washed walls of the concail flask during Titration Process from time to time? 20 —— Scanned with CamScanner a ee| | ” Volumetric titration very useful t Exper ase Titration of Mixture (base strong and b weak) with Acid Strong 0 determine the quantities of ities of the carbonate and i determine the quant é ° eee aero tric titration with two hydroxide in mixture, we will use volumet i different acid-base indicators in the same solution. Sodium hydroxide is strong base in will be the first react with HCI with ph.ph as indicator worked pH (10.0-8.3), then sodium carbonate reacts with HCl according to the following equation: NaOH + Na,CO;+2HCL > NaCL+H,0+ NaHCO; NaHCO; + HCL_,NaCL+H,0 +CO, In other words, to neutralize all the carbonate, two equivalent of HCI should be used and as such the equivalent weight of sodium carbonate = M.wt/2 =53 When one equivalent of HCl is added to the carbonate it is transformed into bicarbonates Na,CO;+HCL- NaHCO; +NaCL and the pH of the solution changes form alkaline about 12 to 8.3. When phenolphthalein is used, it changes to colorless at the end of this stage as its color range falls within the same zone. ph.ph (8.3-10). When another equivalent of HCl is added to the . . solution of bicarbonate, complete neutralization takes place and - it is transformed into sodium chloride and CO; gas is evolved. NaHCO3+ HCL=NaCL +H,0 +CO, Scanned with CamScanner 7L Analytical Chemistry / The pH of solution changes from 8, of HCI will change the pH to about 3.8 which is in range of methyl orange M.O worked pH (3.1-4,4), Procedure: 3 to 7.0, and only one drop 1- The mixture is transferred( 10 ml) to the conical flask by a pipette and then add two drops of the indicator ph.ph. 2- Decanter against a standard acid HCL found in burette and tecord previously that the color of the solution changed from dark pink to colorless, 3-it records the size of the consumer (Vx) , which represents the amount of acid that interacted with (NaOH+1/2 Na 2COs). 4-In addition to the same beaker and the above solution is colorless ( 2-3) drop of orange instance indicator becomes yellow and the color of the solution and titrate with acid (HCL) to the color of the solution changed from yellow to pink and record the size of sour consumer burette represents(vy) the size of the acid equivalent of the tastiest (1/2 Na 2C03). 1- Calculate the concentration Na »CO3 To calculate the size of the acid (HCL) equivalent of sodium carbonate Vi=2Vy =2* 1/2 Na,CO; Nucy * Vict = Nicos * Vxa2co3 2-- Calculate the concentration NaOH Scanned with CamScanner‘ch is equivalent of Calculate the size of the acid(HCL) which is eq sodium hydroxide V.= Vx- VY =(1/2Na2CO3* NaOH)- ( 1/2Na 203) =NaOH Nuct * Vcr =Nwaon* nao 0.1*V,= 2*10 Discussion: 1- How much indicator used in the experiment? and why? 2- Explain any mix of vehicles (NaOH, Na 2COs)—reacts first when adding indicator (ph.ph) them reacts when adding indicator (m.o) ? and remember how the equations for clarification? 3. what other methods used to titrate mixture (NaOH, Na 2 CO) 23 /... Scanned with CamScannerAnalytica Chemistry Experiment(6) Acidity of Vinegar standard solu ia tao by volumetric titration with On of sodium h droxid Fi : \_ Phenolphthalein indicator. Miroxide solution using CH;COOH+NaOH _> CH3COONa+H,0 Procedure: Titration of weak acid CH;COOH with strong calibrated base 1-. Put Sm sample of vinegar into 25ml weighted clean beaker, Then determine the wei r ight of net vinegar. Transfer the sample quantitatively to 100ml clean volumetric flask then dilute to the mark, 2- Take 10 ml of your Prepared solution in step 1, and put it into 250ml conical flask with 2 drops of ph.ph. indicator. Titrate solution with calibrated standard NaOH. Continue the titration until change of color appears from colorless to pink color, 3- Determine the concentration of CH 3COOH in vinegar. | 4- Calculate the weight of CH ;COOH. | 5- Calculate the percentage of CH ;COOH wt/wt% and wt/vol.%, 24 Scanned with CamScanner1-Calculate Nacetic acid.? Nit Viz N * Va N= Cone. of NaOH aay dE V,= volume of ‘NaO!] i i f dist. N,=Cone. of Acetic acid after diluted in 100ml Water V2 = volume of vinegar (410ml) Nac.=? Equivalent weight of acetic acid = 60.05 2- calculate wt of CH; COOH (® . wt _ 1000 O ow Vw 3- The theoretical weight vinegar= density of vinegar*volume of vinegar 0.9gm/em**10ml 4- The percentage of acetic acid in vinegar Acetic acid extracted weight practically %= 7 Weight vinegar extracted theory Discussion: 1- why use the indicator ph.ph in the process of Titration in this experiment? 2- What kind of reaction Titration in the experiment? 25 Scanned with CamScannerAnalytical Chemistry Experiment(7) Oxidation - Reduction Reaction Called interactions that accompany the transfer of electrons from the reduced material To the Oxidizing material (Oxidation - Reduction Reaction ) Article oxidizing : Article are those that receive electrons from the reducing substances in Oxidation- Reduction reactions and examples that potassium permanganate , iodine and potassium second chromate Article reducing: Article are those that give electrons To the oxidizing substances inOxidation- Reduction reactions Examples of sodium Aczalat , oxalic acid, and ferrous sulfate Alamouniakih, Hypo sodium sulfate A- Standardization of Potassium Permanganate (KMno4) Solution: Oxalic acid reacts with potassium permanganate according to the following reaction: SHsC,0r4SE80, 12KMn0, —> TMnSO,+0C0, 1,80, + 8H,0" anate (KMnO,) is considered as one of the agent when it is presented in acid media. In ganese ion has initial oxidation-number of shown in the Potassium Permang: strongest oxidizing this media the man; f (+7) and the final oxidation number is (+2) as following equation: Mat"0-, + 8H" Se Ma? 180 Mit _ 1585 KMn0Os eq.wt.= @-gain Scanned with CamScanneri here the carbon it ucing agent W carb ee (+3) and the final oxidation z . in the following equation Oxalic acid is cons has initial oxidation number is (+4), as shown ry 4 7 < CO2+2e (°c,0.]” a ivalent weight of Oxalic acid: Mwt _ 80 HoC20s4 eq. wt. = Floss a) The equi Procedure: 1- Take out (10ml) of (0.1N) Oxalic Acid (H 2C 20,4) using a pipette to aconical flask. 2- Add (10ml) of (2N) Sulfuric Acid(H 2S0,) to the same flask. 3+ Heat the solution in water bath of (60°C) with gentle stirring. 4- Titrate against KMnO, until the color changes from colorless to light violet with keeping on both heating and stirring. 5- The reaction is ended when having stable violet color inside the flask. Then record the consumed volume of KMnO, from the burette. Calculation: (KMn0,) (H2€ 204) Ny *Vy = N* V2 Noamnoy* Vfrom burette =0.1 *10 N=KMno, 2 Scanned with CamScanner7 Analytical Chemistry eterminati ‘mination of Feso, Solution Normality; Ferrous ion it actin a with Permanganate in acid media and is ill be converted to Ferric ions, while the a ganese of (+7) initial oxidation state will have final oxidation state oe (+2), a chown below B- KIMn0, 5780, p80,» 1/,K,S0, +0 590), 8,0 Procedure 1- Transfer (10ml) of Ferrous sulfate solution into a conical flask. 2- Add (10ml) of (2N) Sulfuric Acid to the same flask. 3- Titrate against standard KMno, solution from a burette until the solution color changes from colorless to light violet. 4- Take the reading of volume consumed from the burette. Calculation (KMn0» (FeSo,) N * Vi = Mm * V2 N=FeSO, | CFeSO,.N * eqWt | 28 ne LLL Scanned with CamScannereen Discussion: 1- Why Oxalic Acid was heated to (6 ; titration? Why this specific temperature I 2- Why H,SOx is used in this type © 0°) before and during is applied? 7 f titration? 3- Why there was 10 need to use any indicator in both titrations? So, solution wasn't heated? 5- In calculating the equivalent weight of KMno, why the molecular weight was divided by (5)? 6- Why KMnO, solution can be considered as secondary standard solution? 4- Why in the second titration Fe’ 7- Why KMn0, solution is preserved in dark bottles? 8- From the reaction of FeSO, with KMnO,, write down the reducing agent equation (ionic form) with showing the oxidation state Scanned with CamScannerAnalytical Chemistry Experiment(8) Identification of First Positive Group (Silver Group) Reaction and separation of Group I Metals: The common metallic ions may be divided into a number of groups which may be identified and separated according to their selective precipitation by a particular anionic functional group. There are, for the purpose of qualitative analysis, five metal groups: Group I (Silver Group): Ag” 5 Pb** ,Hg,** G art pat? pit. oa"? Ca" rou CaperGrompy i, PHBE", CoC , . > tt Group I A (ron Group): Al'**,cr***, Fe Group II B (Zine Group ): Ni‘* Co, Mn**, Zn** Group IV (Calcium Group): Ba, Sr, Ca* Group IV (Alkali Group ): Mg + Na’, K’, NH,* | Each of the five groups above (except Group V) shows a articular reagent , which forms distinguished affinity toward a pi Upon chemical reaction a ppt that can be easily separated. In this experiment only group I of metals, shall be studied. | 30 Scanned with CamScanner* +e A) Identification of Lead ion phe: ff q into a test tube. 1) Introduce 2ml Jead nitrate solution pb (Nos)2 x ic aci il all 2) Add few drops of hydrochloric acid HCL until pb++Pprecipitates as @ white pbCL2 p-pt 3) Dissolve some of the p-pt. in hot water. 4) Add few drops of potassium Chromate Solution. A yellow p.pt. of lead Chromate indicates the positive presence Of lead ions pb** Pb(No;)) +2HCL—+ PbCh +2HNO; PbCL, +K2CrO4—+ PbCrO, +2 KCL B) identification of silver ion Ag* :- 1) introduce 2ml of silver Nitrate Solution AgNO; into a test tube. 2) Add few drops of hydrochloric acid HCL until all Silver Ag+ precipitates as a white p.pt. of AgCL : 3) Take some of the p.pt. and add to it few drops of Ammonium Hydroxide Solution NH ,OH (in a test tube). 4) Add few drops of Nitric Acid HNO; .A white p.pt. of AgCL will form again : AgNO; + HCL—> AgCL +HNOs AgCL + 2NH;—> Ag(NH3) CL Ag(NH;)CL +2HNO; AgCL + 2NH,NOs 31 Scanned with CamScannerAnalytical Chemistry Coa identi; ication o Mercurous Jon HF; 1) introduce 2, ml of Me i into a test tube, ‘Tcurous silver Ntrate Solution Hg,(NO3). 2) Add Mercuro: few drops of hydrochloric acid solution HCL, until all us ions precipitates as a white Ppt. of Hg,CL. 3) Add few drops of concentrated Ammonium Hydroxide NH 40H solution HCL to the ppt .A blackish Solution of free mercury will form: Hg (NOs), + 2HCL— Hg, CL +2HNO; Hg2ClL, + 2NH;+ Hg(NH,)CL +Hg +HN,CL D) Identification and Separation of Group I mixture: Add 2ml of dilute hydrochloric acid into a mixture of Group I ions Pb” Ag+ ,Hg”** in test tube. Filter the p.pt. and discard the ppt. Wash with few milliliters of dilute HCL. Transfer the p.pt. into a test tube and heat with Sml distilled water. Filter hot. 32 enn RO Scanned with CamScanneri i R and “trate: May contain PbCLy, Residue: May contain HeRIRCLR2 sitet: ay : pee wash with distilled water. ‘Add 4mlof) aga potassium chromate warm dilute NHB solution over solution to the hot filtrate A pot yellow p-pt- of lead chromate PbCrO, medicates lead Filtrate: May contain Residue : Black presence. Hg+Hg(NH2)Cl. Mercury present (Ag(NH3)2)CL. Acidify with dilute HNO3. White ppt. of AgCL Silver present L Discussion: 1- Why HCL is used to separate the Ions of first group? 2- Why add hot water to precipitate first group? 3- What is the difference between quantitative analysis and qualitative analysis? Scanned with CamScannerReferences: ———e Analytical Chemistry a Roberts, & MC. Caseros, "Basic Principles of 7 era Chemistry", W.A, Benjamin, Ir c., New York, Solomons, G.W., "Organic Chemistry", 4PthP Ed., John Wiely and Sons, Inc., USA. 663, 1 (2001). Hart, R.D., Scuet3, " Organic Chemistry A Short Course " SPthP Ed., Oughon Mifflin Comp., Boston. USA. 19, 26 (2001). RK. Bansal, "Organic Reaction Mechanism" 3PrdP Ed., (2000). R.T. Morrlson, & R.N. Boyd, "Organic Chemistry", Inc., New York, (2001). Scanned with CamScanneras ~ Analytical Chemistry eat tubes crucible ‘and cover > Volumett flask Waien lass Erlenmeyer Assorted ubber stoppers. Droppor Forceps Scanned with CamScanneri Gu Ag [Pm pala Na asm Eu |i Ng, Scanned with CamScanner