Experiment 1 Assay of Alum Questions 1. What is gravimetric method?

Gravimetric analysis describes a set of methods in analytical chemistry for the quantitative determination of an analyte based on the mass of a solid. 2. Give the reason/s for the following a. use of ashless filter paper This is to prevent the addition of mass to the analyte. b. addition of ammonium chloride This is to minimize the coprecipitation of divalent cations. c. use of methyl orange It is used as the indicator in the analysis 3. Why is the mixture heated to boiling after the addition of methyl orange? To speed up the reaction and to increase solubility of precipitate. Experiment 2 Preparation and standardization of hydrochloric acid solution Questions 1. What is chemically pure HCl? Chemically pure reagents are for general applications. 2. What is a primary standard? Identify the primary standard used in the experiment?- It has known concentration and definitely high purity. 3. What type of standardization did you perform?- Primary standardization 4. Would it make a difference if phenolphthalein was used instead of methyl orange as and indicator. Explain. Yes, because Phenolphthalein is a base indicator and methyl orange is an acid indicator. Experiment 3 Preparation and standardization of sodium hydroxide solution Questions 1. Can sodium hydroxide be used as a primary standard? No, because it has low purity. 2. Can methyl orange be used as an indicator instead of phenolphthalein?why or why not? No, because methyl orange has a different range of acidity. 3. Why use a Mohr buret to contain the titrant sodium hydroxide? Mohr buret is for bases. Experiment 4 Assay of tartaric acid in white wine Questions 1. What type of titration did you perform?- This is alkalimetric titration. 2. What is acidiimetry?what is alkalimetry?-In acidimetry, the titrant is and acid while in alkalimetry, the titrant is basic. Experiment 5 Assay of aspirin Questions 1. What is residual titration? the reagent is added to a sample so that there is a subtle excess. Then, titrate the excess. 2. What is blank titration? This is a type of titration wherein the anlayte contains all other reagents except the sample. 3. In this assay, why do you have to perform a blank determination? To be able to compute or calculate the excess amount.

4. Write the structural formula of aspirin 5. Calculate the milliequivalent weight of aspirin. Meq wt = MM / 2000 = 0.09008g/meq

Experiment 6 Assay of Zinc Oxide Questions 1. Give reasons for using ammonium chloride. It increases the solubility of the zinc oxide 2. Explain the reaction/s that occurred in the experiment ZnO + NH4+ --- Zn(NH3)4+, ZnO +2HCL ---ZnCl2 + H20 3. What is indirect titration? This kind of titration involves preliminary reaction in which the analyte is replaced by an equivalent amount of another substance which is then determined by titration. Experiment 7 Assay of Unknown Acid Sample questions 1. Give the reason why sodium carbonate is not completely neutralized in phenolphthalein titration? -Sodium carbonate should be titrated twice using phenolphthalein and methyl orange as indicators. 2. Explain why sodium bicarbonate cannot be titrated with standard acid solution using phenolphthalein as the indicator? Methyl Orange is the appropriate indicator for this experiment. 3. Is it possible to have a mixture of sodium hydroxide and sodium bicarbonate? No. The mixture of sodium hydroxide and sodium bicarbonate will not produce any new product. Experiment 8 Preparation of Standard Silver Nitrate Solution Questions 1. Give the type of standardization performed. Primary Standardization 2. Why do you have to store the silver nitrate solution in an amber colored bottle? To prevent the decomposition of the reagent due to factors like light, temperature, and sound. Experiment 9 Preparation and Standardization of KSCN Solution Questions 1. What type of volumetric method was performed? this is a direct titration. 2. Why is the silver nitrate solution placed in a Geissler buret and not in a Mohr buret? this is due to the reaction that will take place when silver nitrate is on a Mohr buret. 3. Explain the flesh colored endpoint. The flesh colored endpoint is a combination of white precipitate of AgSCN and Fe(SCN)2+ which is blood red. Experiment 10 Fajans Titration in Chloride Questions 1. What is Fajans titration? Fajans titration is a direct titration where the basis of endpoint is the formation of colored adsorption product. It uses DCF as an indicator and the condition for it to be performed must not be lower than pH 6. 2. Why do you have to maintain the pH of the solution? How do you maintain it? The pH should be maintained to prevent the shift of the reaction to the reactant side. The pH can be maintained by adding a buffer which prevents sudden shifts in pH. 3. What is the role of dextrin? Dextrin keeps the AgCl in a dispersed state because greater surface area would result into maximal reaction. Experiment 11 Volhard Titration of Ammonium Chloride Questions

1. What is Volhard Titration? Determination of the halogen content of a solution by titration with a standard thiocyanate solution. 2. Why do you have to remove the precipitate before titrating the excess silver nitrate? To prevent the production of AgSCN that can cause a negative error. 3. Explain why ammonium chloride is assayed through residual titration. Ammonium chloride will initially react with the excess silver nitrate. Unreacted silver ions will react with thiocyanate ion producing silver thiocyanate. Experiment 12 Assay of Sodium Chloride in Dried Fish by Mohr Method Questions 1. What is Mohr titration? How does it differ from Fajans and Volhard method? This method utilizes chromate as an indicator. Chromate forms a precipilate with Ag+ but this precipitate has a greater solubility than that of AgCl, for example. Therefore, AgCl is formed first and after all Cl- is consumed, the first drop of Ag+ in excess will react with the chromate indicator giving a reddish precipitate. Volhard is an indirect method for chloride determination where an excess amount of standard Ag+ is added to the chloride solution containing Fe3+ as an indicator. The excess Ag+ is then titrated with standard SCN- solution untill a red color is obtained which results from the reaction. Fluorescein and its derivatives are adsorbed to the surface of colloidal AgCl. After all chloride is used, the first drop of Ag+ will react with fluorescein (FI-) forming a reddish color. 2. Explain the orange or reddish-brown endpoint. The red brown endpoint indicates the formation of silver chromate. An excess of Ag+ is added to produce enough precipitate to be seen Experiment 13 Preparation and Standardization of EDTA solution Questions 1. What is compleximetry? It is a kind of titration that is based upon the formation of a complex. 2. What is a complex? A ligand? A complex is a structure consisting of a central atom or molecule weakly connected to surrounding atoms or molecules. A ligand a ligand is an atom, ion, or molecule (see also: functional group) that generally donates one or more of its electrons through a coordinate covalent bond to, or shares its electrons through a covalent bond, or through a pi-bond, with one or more central atoms or ions (these ligands act as a Lewis base). Fewer examples exist where a molecule can be described as a ligand that does not accept electrons from a Lewis base 3. What type of ligand is EDTA?-EDTA is a hexadentate ligand. 4. Explain the color changes. Compex EBT is color red. Uncomplex EBT is blue. 5. Give the reason for using a buffer solution. A buffer will maintain the pH requirement of the reaction. Experiment 14 Determination of the Total Hardness of Water Questions 1. What does hardness of water mean?- Hardness of water refers to the waters mineral content of Ca2+ and/or Mg2+. 2. What is the significance of the experiment? - Once the hardness of water is determined one would no if it is usable for practical means like bathing and cleaning. If not it would still undergo purification. Experiment 15 Preparation and Standardization of Potassium Permanganate solution Questions 1. Justify the following a. Boiling of the potassium permanganate solution- hasten decomposition of organic materials b. Allowing the solution to stand for at least 2 days to allow complete reaction c. Filtration of the solution using asbestos to isolate the MnO2 that speeds up decomposition of KMnO4 d. Addition of concentrated H2SO4- to acidify solution

2. 3. 4. 5.

e. Maintenance of the 70 degrees temperature during titration- to speed up reaction What type of volumetric titration is performed? - REDOX What indicator is used in the experiment? - KMnO4 itself Why does the color at the endpoint persist only for several seconds? - Because of the color of Mn +2. What buret must be used for KMNO4?why? - Use Geisler buret because the rubber in the Mohr will react with KMnO4.

Experiment 16 Preparation and Standardization of Oxalic Acid Solution Questions 1. Between KMnO4 and H2C2O4, which will act as the oxidizing agent? The reducing agent? KmnO4 is the oxidizing agent and H2C2O4 is the reducing agent. 2. Without the concentrated H2SO4, will the reaction take place? Why or why not? -No, this should be prepared through addition of H2S2O4. Experiment 17 Assay of Hydrogen Peroxide Questions 1. Why use 6N H2SO4 instead of concentrated H2SO4? Low pH will decompose the hydrogen peroxide 2. Based on the equation given, how many electron/s is/are lost/gained? there are 5 electrons gained and 2 electrons lost. Experiment 18 Assay of Sodium Nitrite Questions 1. Why do you have to immerse the tip of the pipet beneath the surface of the KMnO4 solution? this is done to prevent air oxidation or volatilization of nitric acid. 2. Why do you have to warm the mixture to 40C before adding the H2C2O4 solution? this is done because 40 degrees is the optimum temperature of sodium nitrite. 3. Why 80C and not 70C like in the previous experiments? Is there a difference? -80 degrees Celsius is the optimum temperature of oxalic acid. 4. Can sodium nitrate be assayed using direct method? Why or why not? No, because it can no longer be oxidized to a higher state. Experiment 19 Preparation and Standardization of Iodine Solution Questions 1. Rationalize the use of starch as an indicator. The amylose component of starch is a helical structure that traps the iodine with in. This leads to the formation of the iodo-starch complex which then gives out a dark blue color. Thus, starch is used as an indicator in this experiment. 2. Give the roles of the ff. a. potassium iodide- helps maintain the solubility of iodine b. hydrochloric acid- to neutralize the base present and to prevent the formation of hypoiodite and iodide c. methyl orange- to indicate if the solution is acidic d. sodium bicarbonate- to prevent reverse reaction 3. Why do you have to place the iodine solution in an amber colored bottle?- to avoid exposure to light which might affect the solution Experiment 20 Preparation and Standardization of Sodium Thiosulfate Questions 1. What buret is used for sodium thiosulfate solution?why? Mohr buret 2. What is the reason for using sodium carbonate in the preparation of sodium thiosulfate solution?

Sodium carbonate prevents the thiol bacteria and also control the pH of the solution. Experiment 21 Assay of Tartar Emetic Questions: 1. What is the chemical formula for tartar emetic? - KOSbC4H406 H2O 2. Describe the reaction/s that took place in the experiment. H2O + OSbC4H406- + I2 OSbC4H4062 + H + + 2IThe reducing power of several reducing agents is increased in neutral solution thus; equilibrium is affected by H+ concentration. Experiment 22 Detemination of Ascorbic Acid in Vitamin Tablets Questions: 1. What is iodimetric method?- The titrant is Iodine and the analyte is a reducing agent. 2. Why do you have to cover the flask with a cardboard during titration? This is done to prevent the volatilization of the I2. 3. Why should the volumetric flask be completely dry before placing the tablets? The water will interfere with the volume of solutions. Experiment 23 Assay of Cupric Sulfate Questions 1. What is iodometric method? This method makes use of the fact that practically all oxidizing agents oxidize iodide in dilute acid solutions to free iodine. 2. Give the reason/s for using the following: a. Acetic acid helps in liberating the Iodine b. Starch TS this will serve as the indicator Experiment 24 Assay of Vanillin in Vanilla Extract Questions 1. Account for the use of the ff. reagents: a. lead acetate- upon addition it would turn the solution into a colorless one b. phophotungstic-phosphomolybdic reagent- a coloring reagent c. 20% Na2CO3- to make it basic d. sodium phosphate- acts as buffer 2. Why should the absorbance of vanillin sample be read at 430 nm? That is the wavelength where vanillin gives maximum wavelength and where Beers law is obeyed. 3. Give the relationship between absorbance and transmittance? Absorbance is directly proportional to transmittance.