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1 LMCHE010
TABLE OF CONTENTS S. No. 1 2 3 4 5 6 7 8 9 10 11 12 Title of the Experiment To detect the presence of acid radicals (oxyanions - carbonate, sulphate and nitrate) in a given salt. To detect the presence of acid radicals (halides - chloride, bromide and iodide) in a given salt. To detect the presence of basic radicals (Gp I, II Pb+2, Cu+2). To detect the presence of basic radicals (Gp III Al+3, Fe+2,Cr+3). To detect the presence of basic radicals (Gp IV, V Zn+2,Ni+2,Ca+2,Ba+2). To detect the presence of basic radicals (Gp VI Mg+2, K+, NH4+). To detect the presence of one cation and one anion from a given mixture. To determine Electrochemical Chemical Equivalent of Copper using Copper sulphate solution and Copper electrodes. To determine the percentage of iron in the given ferrous alloy by potassium permanganate method. To prepare phenol formaldehyde resin (bakelite). To determine carbon monoxide content in emission from petrol vehicle. To determine dissolved oxygen in a water sample. Page No. 4-8 9-13 14-18 19-23 24-30 31-35 36-41 42-46 47-50 51-53 54-56 57-61
2 LMCHE010
Some rules to be followed in the Lab: GENERAL RULES: 1. Entry without lab coat in chemistry lab is strictly prohibited. 2. Mobile phones should be switched off and kept in the bag during lab hours. 3. No group discussions are allowed in the lab. 4. Clean the apparatus as well as the slab after your experiment is finished. 5. Do not do any undisciplined activity in lab as you are under strict cc-TV surveillance. 6. Do not use laptop while performing the experiments. 7. Switch off electrical apparatus after their use. 8. Do not throw filter papers in sink, dispose all waste in dustbin. PRECAUTIONARY RULES: 1. Never pipette out strong acids and base with your mouth, it can be dangerous, therefore use measuring cylinders for such chemicals. 2. Never try to smell the chemicals as it can be dangerous for you. 3. Cap the bottles after taking chemical as uncovered bottles can be a source of harmful fumes. 4. In case of any accidental spill over of any chemical on you, report your teacher or lab technician immediately. 5. Report your lab technician if any breakage of glass apparatus takes place.
3 LMCHE010
EXPERIMENT NO. 1 Aim: To detect the presence of acid radicals (oxyanions: carbonate, nitrate and sulphate) in a given salt. Equipments to be used: Test tube, test tube holder, Bunsen burner, tripod stand, test tube and watch glass. Chemicals required: Inorganic salt, conc. H2SO4, Dil. H2SO4, Learning objective: (i) Student will be able to understand that anions detected by dil. and conc. H2SO4 tests can be detected by the evolution of different gases. (ii) Some of the anions like SO42- which are not evolved as gases on treatment with by dil. and conc. H2SO4 tests, can be detected by their independent tests. Outline of the procedure: Preparation of Salt solution: 1. Preparation of Water extract (for water soluble salts): Dissolve a small amount of salt in 2-3 mL of distilled water, filter it and collect the filtrate for various tests. 2. Preparation of Sodium Carbonate extract (for water insoluble salts): Boil a small amount of salt with 300-400 mg solid sodium carbonate and add 5-6 mL of distilled water, filter and collect the filtrate for various identification tests. Test for detection of carbonate S.No. 1 Experiment Dilute H2SO4 test: To the small amount of salt add 1-2 mL of dil. H2SO4 Observation Colourless, odourless gas evolved with brisk effervesnce Inferance CO32-present
Confirmatory test for Carbonate: S.No. 1 Experiment Lime water test: Pass the gas through lime water Pass more of the gas through lime water Observation Lime water turns milky Milkiness disappears Inferance CO32- confirmed CO32- confirmed
4 LMCHE010
Test for detection of nitrate (NO3-) S.No. Experiment 1 Dilute H2SO4 test: To the small amount of salt add 1-2 mL of dil. H2SO4 Conc. H2SO4 test: Heat a small amount of salt with conc. H2SO4
Confirmatory test for Nitrate: S.No. 1 Experiment Add copper turnings to the above test tube Ring test: To water extract, add freshly prepared ferrous sulphate and mix thoroughly. Cool the mixture under the tap. Add 2 mL conc. H2SO4along the sides of the test tube without shaking. S.No. 1 Test for detection of sulphate (SO42-) Experiment Dilute H2SO4 test: To the small amount of salt add 1-2 mL of dil. H2SO4 Concentrated H2SO4 test : Heat a small amount of salt with conc. H2SO4 BaCl2 test: Take 1 mL water extract of the salt in water or sodium carbonate and after acidifying with dilute hydrochloric acid add BaCl2 solution. Lead acetate test: To the water extract or sodium carbonate extract add glacial acetic acid and lead acetate solution. Observation No gas evolved Inferance CO32- absent NO3- absent SO42- present Observation Brown fumes intensify Inferance NO3- confirmed NO3- confirmed
No gas evolved
White precipitate insoluble in conc. HCl or conc. HNO3 is obtained. Appearance of white precipitate
SO42- confirmed
5 LMCHE010
Required Results: The given salt contains ________________________anion. Parameters: NA Relationship: NA Graphs: NA Error Analysis: NA Cautions: i. Since the experiment deals with acidic and basic conditions. The acids and the bases should be handled with care and dropper or a measuring cylinder should be used for addition of it. ii. Bases like NH4OH and conc. HNO3, HCl, H2SO4 should be used carefully, since they fume in air the bottle should be corked immediately after its use. iii. iv. Many solution bumps out while heating; test tube should be kept in a slant position with its mouth away from the person carrying the experiment to avoid bumping on face. Concentrated acids should be added along the sides of the testube.
Requirements for Lab Technician: 1. Inorganic salt samples (Salts containing nitrate, sulphate and carbonate) 2. Dil. H2SO4 3. Conc. H2SO4 4. BaCl2 solution 5. Lime water 6. Glacial acetic acid 7. Lead acetate solution 8. Copper turnings
6 LMCHE010
Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To detect the presence of acid radicals (oxyanions: carbonate, nitrate and sulphate) in a given salt. Observation table: Sample A Experiment Observation Inferance
7 LMCHE010
Learning Outcomes (what I have learnt): to be written by the students in 50-70 words.
To be filled in by faculty S.No Parameter (Scale from 1-10, 1 for very poor and 10 excellent) Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty Marks Obtained Maximum Marks 20 20 10 Total marks Obtained
1 2 3
8 LMCHE010
EXPERIMENT NO. 2 Aim: To detect the presence of acid radicals (halides: chloride, bromide and iodide) in a given salt. Equipments to be used: Test tube, test tube holder, Bunsen burner, tripod stand, test tube stand and watch glass. Chemicals required: Sample salt, Dil. H2SO4, Conc. H2SO4. Learning objective: (i) To detect various halogens present in the given salt (ii) To identify and differentiate them on the basis of Silver nitrate test Outline of the procedure: Preparation of Salt solution: 1. Preparation of Water extract (for water soluble salts): Dissolve a small amount of salt in 2-3 mL of distilled water, filter it and collect the filtrate for various tests. 2. Preparation of Sodium Carbonate extract (for water insoluble salts) : Boil a small amount of salt with 300-400 mg solid sodium carbonate and add 5-6 mL of distilled water, filter and collect the filtrate for various identification tests. S.No. 1 Test for detection of halides Experiment Dilute H2SO4 test: To the small amount of salt add 1-2 mL of dil. H2SO4 Concentrated H2SO4 test: Heat a small amount of salt with conc. H2SO4 Observation No gas evolved Inferance CO32- absent Cl- present
A colourless gas with pungent smell,which gives dense white fumes when a rod dipped in ammonium hydroxide is brought near the mouth of the test tube. Reddish brown colour gas with pungent odour is evolved Violet vapours
Br- present
I- present
9 LMCHE010
Confirmatory test for chloride 1 MnO2 test: Add a pinch of MnO2 to above colourless gas AgNO3(Silver nitrate) test: To Soda extract/ water extract, add HNO3 till effervescence stops, heat and then add AgNO3 solution greenish yellow gas evolves curdy white ppt is obtained which is soluble in NH4OH and which disappear on addition of dil. HNO3. Cl- confirmed Cl- confirmed
Confirmatory test for bromide 3 AgNO3(Silver nitrate) test: To Soda extract/ water extract, add dil. HNO3 till effervescence stops, heat and then add AgNO3 solution yellow ppt is obtained which is soluble in NH4OH and which disappear on addition of dil. HNO3. Organic layer turns orange Br- confirmed
To Soda extract/ water extract, add dil HNO3, then 3-4 mL carbon tetrachloride/ carbon disulphide and 1 mL of conc. HNO3. Shake vigorously.
Br- confirmed
Confirmatory test for iodide: 5 Take 1 mL of salt solution neutralised with HCl and add 1 mL chloroform/ carbon tetrachloride/carbon disulphide. Now add an excess of chlorine water drop wise and shake the test tube. AgNO3 (Silver nitrate) test: Take 1 mL of sodium carbonate extract acidify it with dil. HNO3 (or take water extract). Add, silver nitrate solution. A violet colour appears in the organic layer I- confirmed
I- confirmed
10 LMCHE010
Required Results: The given salt contains ______________anion Parameters: NA Relationship: NA Graphs: NA Error Analysis: NA Cautions: 1. Since the experiment deals with acidic and basic conditions. The acids and the bases should be handled with care and dropper or a measuring cylinder should be used for addition of it. 2. Bases like NH4OH and conc. HNO3, HCl, H2SO4 should be used carefully, since they fume in air the bottle should be corked immediately after its use. 3. Many solution bumps out while heating; test tube should be kept in a slant position with its mouth away from the person carrying the experiment to avoid bumping on face. Requirements for Lab Technician: 1. Inorganic salt samples (Salts containing chloride, bromide and iodide) 2. Dil. H2SO4 3. Conc. H2SO4 4. AgNO3 solution 5. Manganese dioxide 6. Dil. HNO3 7. Conc. HNO3 8. Carbon disulphide
11 LMCHE010
Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To detect the presence of acid radicals (halides: chloride, bromide and iodide) in a given salt. Observation table: Sample A Experiment Observation Inference
12 LMCHE010
Learning Outcomes (what I have learnt): to be written by the students in 50-70 words.
To be filled in by faculty S.No Parameter (Scale from 1-10, 1 for very poor and 10 excellent) Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty Marks Obtained Maximum Marks 20 20 10 Total marks Obtained
1 2 3
13 LMCHE010
EXPERIMENT NO.3 Aim : To detect the presence of basic radicals (Gp I,II Pb+2,Cu+2) Equipments to be used: Test tube, test tube holder, Bunsen burner, tripod stand, test tube and watch glass. Chemicals used: Inorganic sample, Dil. HCl, Conc. HCl, H2S. Learning Objectives: (i) The purpose of the experiment is to make the students understand how the basic radicals are classified into six groups. (ii) Student shall come to know that the cations of group I are precipitated as chlorides by adding dil. HCl. (iii) Student will also understand that the cations of group II are precipitated only in group II as their sulphides in the acidic medium on passing H2S. Outline of the procedure: Preparation of Original Solution (O.S.): Dissolve 0.1 g of salt in water, dil. HCl or conc. HCl as per solubility Analysis of Group I S.No. 1 Experiment To aqueous solution of salt, add 5-10 drops of dil. HCl Observation White ppt Inferance Gp I (Pb2+ present)
Wash the residue with water and heat. Centrifuge and collect the filterate and residue. 2. 3. To the filtrate, add 3-5 mL of dil. H2SO4 To the filtrate, add 3-5 mL of KI and ammonium acetate White ppt Yellow ppt Pb2+ is confirmed. Pb2+ is confirmed.
14 LMCHE010
Analysis of Group II S.No. 1 Experiment To Original solution (O.S) add 5-10 drops of dil. HCl Pass H2S to small portion of acidic solution (dil. HCl). Filter and collect the residue. Observation No ppt. Inferance Gp I absent
2.
Black ppt.
Gp II present
(I) Boil the precipitate of Group II A with dilute nitric acid and add a few drops of alcohol and dil. H2SO4. Filter the residue a) Dissolve the precipitate in ammonium acetate solution. Acidify with glacial acetic acid and divide the solution into two parts. (i) To the first part add potassium chromate (K2CrO4) solution. Yellow ppt. of lead chromate (PbCrO4) Pb2+ confirmed White ppt. Pb2+ may be present
Pb2+ confirmed
(ii) Acidify it with glacial acetic acid and add potassium ferrocyanide solution.
Cu2+ is confirmed
Required Results: The given salt contains _______________ Parameters: NA Relationship: NA Graphs: NA 15
cation.
LMCHE010
Error Analysis: NA Cautions: 1. Since the experiment deals with acidic and basic conditions. The acids and the bases should be handled with care and dropper or a measuring cylinder should be used for addition of it. 2. Bases like NH4OH and conc. HNO3, HCl, H2SO4 should be used carefully, since they fume in air the bottle should be corked immediately after its use. 3. Many solution bumps out while heating; test tube should be kept in a slant position with its mouth away from the person carrying the experiment to avoid bumping on face. Requirements for Lab Technician: 1. Inorganic salt samples (Salts containing Cu2+ and Pb2+) 2. Dil. HCl 3. Dil. H2SO4 4. H2S gas 5. Potassium iodide 6. Ammonium acetate 7. Potassium chromate 8. Glacial acetic acid 9. Ammonium hydroxide 10. Potassium ferrocyanide
16 LMCHE010
Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To detect the presence of basic radicals (Gp I, II Pb+2, Cu+2) Observation table: Sample Experiment Observation Inference
17 LMCHE010
Learning Outcomes (what I have learnt): to be written by the students in 50-70 words.
To be filled in by faculty S.No Parameter (Scale from 1-10, 1 for very poor and 10 excellent) Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty Marks Obtained Maximum Marks 20 20 10 Total marks Obtained
1 2 3
18 LMCHE010
EXPERIMENT NO. 4 Aim: To detect the presence of basic radicals (Gp III Al+3,Fe+2,Cr+3) Equipments to be used: Test tube, test tube holder, Bunsen burner, tripod stand, test tube and watch glass. Chemicals used: Inorganic salt, dil. HCl, Conc. HCl, H2S, NH4Cl, NH4OH. Learning Objectives: (i) Student will be able to understand how Al+3, Fe+2, Fe3+and Cr+3 are precipitated as hydroxides in alkaline medium. (ii) Student will be able to distinguish between Fe2+ and Fe3+. Outline of the procedure: Preparation of O.S.: Dissolve 0.1 g of salt in water, dil. HCl or conc. HCl as per solubility Analysis of Cations: S.No. 1 Experiment To Original solution (O.S) add 5-10 drops of dil. HCl Pass H2S to small portion of acidic solution (dil. HCl). Filter and collect the residue. Add 2-3 drops of conc. HNO3 to O.S., which oxidise Fe2+ ions to Fe3+ ions. Heat the solution for a few minutes. After cooling add a small amount of solid ammonium chloride (NH4Cl) and an excess of ammonium hydroxide (NH4OH) solution till it smells of ammonia. Shake the test tube. Observation No ppt. Inferance Gp I absent
2.
No ppt
Gp II absent
3.
Gp III present
Collect the residue and add 3-4 mL of water and then add 100 mg sodium peroxide. Separate the residue and filtrate. (a) To the above residue add dil. HCl and divide the solution in 3 parts. Brown ppt Iron Fe2+ / Fe3+ present
19 LMCHE010
(i) To part 1, add potassium ferricyanide K3[Fe(CN)6] solution (ii) To part 2 add potassium ferrocyanide K4[Fe(CN)6] solution (iii) To part 3 add ammonium thiocyanate (NH4CNS)
Blue ppt
Fe2+ confirmed
Fe3+ confirmed
Fe3+ confirmed
(b) Divide the filtrate in 2 parts. If filtrate is yellow Cr3+ is present (i) To part 1, add 3-4 mL of glacial acetic acid and then 3 mL of lead acetate solution (ii) To part 2 of filtrate, add NH4Cl and heat Yellow ppt
Cr3+ confirmed
White ppt
Al3+ present
Dissolve the white precipitate in dilute HCl and divide into two parts. (i) To the first part add sodium White ppt soluble in hydroxide solution and warm. sodium hydroxide (ii) To the second part first add blue litmus solution and then ammonium hydroxide solution drop by drop along the sides of the test tube. Blue floating mass in colourless liquid is obtained
Al3+ confirmed
Al3+ confirmed
Required Results: The given salt contains ___________cation. Parameters: NA Relationship: NA Graphs: NA Error Analysis: NA Cautions: i. Since the experiment deals with acidic and basic conditions. The acids and the bases should be handled with care and dropper or a measuring cylinder should be 20 LMCHE010
used for addition of it. ii. Bases like NH4OH and conc. HNO3, HCl, H2SO4 should be used carefully, since they fume in air the bottle should be corked immediately after its use. iii. Many solution bumps out while heating; test tube should be kept in a slant position with its mouth away from the person carrying the experiment to avoid bumping on face. Requirements for Lab Technician: 1. Inorganic salt samples (Salts containing Al3+, Fe2+, Fe3+ and Cr3+) 2. Dil. HCl 3. Dil. H2SO4 4. H2S gas 5. Ammonium chloride 6. Ammonium hydroxide 7. Sodium peroxide 8. Potassium ferricyanide 9. Ammonium thiocyanate 10. Potassium ferrocyanide 11. Glacial acetic acid 12. Lead acetate 13. Sodium hydroxide 14. Blue litmus
21 LMCHE010
Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To detect the presence of basic radicals (Gp III Fe+2, Fe+3, Cr+3, Al3+) Observation table: Sample Experiment Observation Inference
22 LMCHE010
Learning Outcomes (what I have learnt): to be written by the students in 50-70 words.
To be filled in by faculty S.No Parameter (Scale from 1-10, 1 for very poor and 10 excellent) Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty Marks Obtained Maximum Marks 20 20 10 Total marks Obtained
1 2 3
23 LMCHE010
EXPERIMENT NO. 5 Aim: To detect the presence of basic radicals (Gp IV, V Zn+2, Ni+2, Ca+2, Ba+2) Equipments to be used: Test tube, test tube holder, Bunsen burner, tripod stand, test tube and watch glass. Chemicals used: Inorganic salt, dil. HCl, Conc. HCl, H2S, NH4Cl, NH4OH and (NH4)2CO3. Learning Objectives: (i) Student will be able to know that group IV cations i.e. Zn+2and Ni+2 are precipitated as sulphides in alkaline medium on passing H2S. (ii) Student will be able to distinguish between Zn2+ and Ni2+ by various tests. (iii) Student will be able to know that the cations of group V are precipitated as their carbonates in alkaline medium by the action of ammonium carbonate. Outline of the procedure: Preparation of O.S.: Dissolve 0.1 g of salt in water, dil. HCl or conc. HCl as per solubility Analysis for Gp IV cations: S.No. 1 Experiment To Original solution (O.S) add 5-10 drops of dil. HCl Pass H2S to small portion of acidic solution (dil. HCl). Filter and collect the residue. Add 2-3 drops of conc. HNO3 to O.S., Heat the solution for a few minutes. After cooling add a small amount of solid ammonium chloride (NH4Cl) and an excess of ammonium hydroxide (NH4OH) solution till it smells of ammonia. Shake the test tube. Pass H2S to above alkaline solution, shake and filter 24 LMCHE010 Observation No ppt. Inference Gp I absent
2.
No ppt
Gp II absent
3.
No ppt
Gp III absent
Gp IV present
If White ppt, then Zn2+ may be present. Dissolve the precipitate in dilute HCl by boiling. Divide the solution into two parts. (i) To one part, add sodium hydroxide White precipitate soluble in excess of solution. (a) Zn2+ confirmed sodium hydroxide solution (ii) Neutralise the second part with ammonium hydroxide solution and add potassium ferrocyanide K4[Fe(CN)6] solution (b) If black ppt, then Ni2+ may be present (i) DMG test: Dissolve the precipitate in aqua regia (3 drops of conc. HNO3 and 6 drops of conc. HCl). Heat thesolution to dryness and cool. Dissolve the residue in water. Add ammonium hydroxide solution till it becomes alkaline. Add a few drops of dimethyl glyoxime and shake the test tube. Analysis for Gp V cations: S.No. 1 Experiment To Original solution (O.S) add 5-10 drops of dil. HCl Pass H2S to small portion of acidic solution (dil. HCl). Filter and collect the residue. Add 2-3 drops of conc. HNO3 to O.S., Heat the solution for a few minutes. After cooling add a small amount of solid ammonium chloride (NH4Cl) and an excess of ammonium hydroxide (NH4OH) solution till it smells of ammonia. Shake the test tube. Pass H2S to above alkaline solution, shake and filter 25 LMCHE010 Observation No ppt. Inference Gp I absent
Bluish ppt
Zn2+ confirmed
Ni2+ confirmed
2.
No ppt
Gp II absent
3.
No ppt
Gp III absent
No ppt
Gp IV absent
Take original solution and add a small amount of solid NH4Cl and an excess 5 White ppt Gp V present of NH4OH solution followed by solid ammonium carbonate (NH4)2CO3. Preserve a part of ppt for flame test and dissolve rest of the white precipitate by boiling with dilute glacial acetic acid and divide the solution into two parts (i) To the first part add potassium chromate solution. Ba2+ confirmed Yellow ppt (ii) Flame test: Take a platinum wire and dip it in conc. HCl. Heat it strongly until the wire does not impart any colour to the non-luminous flame.Now dip the wire in the paste of the (Group V) precipitate in conc. HCl. Heat it in the flame. (b) If Ba2+ is absent, then Ca2+ may be present (i) To another part of the solution, add ammonium oxalate solution and shake well. (ii) Flame test: Take a platinum wire and dip it in conc. HCl. Heat it strongly until the wire does not impart any colour to the non-luminous flame.Now dip the wire in the paste of the (Group V) precipitate in conc. HCl. Heat it in the flame. White ppt
Ba2+ confirmed
Ca2+ confirmed
Ca2+ confirmed
Required Results: The given salt contains ___________ cation Parameters: NA Relationship: NA Graphs: NA Error Analysis: NA Cautions: i. Since the experiment deals with acidic and basic conditions. The acids and the bases should be handled with care and dropper or a measuring cylinder should be used for addition of it. ii. Bases like NH4OH and conc. HNO3, HCl, H2SO4 should be used carefully, since they 26 LMCHE010
fume in air the bottle should be corked immediately after its use. iii. Many solution bumps out while heating; test tube should be kept in a slant position with its mouth away from the person carrying the experiment to avoid bumping on face. Requirements for Lab Technician: 1. Inorganic salt samples (Salts containing Zn2+, Ni2+, Ca2+ and Ba2+) 2. Dil. HCl 3. Dil. H2SO4 4. Dil. HNO3 5. H2S gas 6. Conc. HCl 7. Ammonium chloride 8. Ammonium hydroxide 9. Ammonium carbonate 10. Potassium ferrocyanide 11. Dimethyl glyoxime 12. Potassium chromate 13. Ammonium oxalate 14. Ethanol
27 LMCHE010
Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To detect the presence of basic radicals (Gp IV, V Zn+2, Ni+2, Ca+2, Ba+2) Observation table: Sample Experiment Observation Inference
28 LMCHE010
29 LMCHE010
Learning Outcomes (what I have learnt): to be written by the students in 50-70 words
To be filled in by faculty S.No Parameter (Scale from 1-10, 1 for very poor and 10 excellent) Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty Marks Obtained Maximum Marks 20 20 10 Total marks Obtained
1 2 3
30 LMCHE010
EXPERIMENT NO. 6 Aim: To detect the presence of basic radicals (Gp VI Mg+2, K+, NH4+) Equipments to be used: Test tube, test tube holder, Bunsen burner, tripod stand,test tube and watch glass. Chemicals used: Inorganic salt, dil. HCl, Conc. HCl, H2S, NH4Cl, NH4OH and (NH4)2CO3. Learning Objectives: (i) Students will be able to understand that the cations of group VI i.e. Mg+2, K+, NH4+ are neither precipitated as chlorides, sulphides and carbonates. (ii) Student will be able to detect the presence of independent cations namely Mg+2, K+, NH4+. Outlines of the procedure: Preparation of O.S.: Dissolve 0.1 g of salt in water, dil. HCl or conc. HCl as per solubility Analysis for Gp VI cations: S.No. 1 Experiment To Original solution (O.S) add 5-10 drops of dil. HCl Pass H2S to small portion of acidic solution (dil. HCl). Filter and collect the residue. Add 2-3 drops of conc. HNO3 to O.S., Heat the solution for a few minutes. After cooling add a small amount of solid ammonium chloride (NH4Cl) and an excess of ammonium hydroxide (NH4OH) solution till it smells of ammonia. Shake the test tube. Pass H2S through above alkaline solution. Take original solution and add a small amount of solid NH4Cl and an excess of NH4OH solution followed by solid ammonium carbonate (NH4)2CO3. Observation No ppt. Inference Gp I absent
2.
No ppt
Gp II absent
3.
No ppt
Gp III absent
No ppt
No ppt
31 LMCHE010
S.No 1 2.
Confirmatory tests for K+, Mg2+, NH4+ Experiment Observation Inference Mg2+ confirmed K+ confirmed
3.
4. 5.
To O.S., add dil. HCl solution. Add White ppt on scratching NH4OH and Na2HPO4 solution. To O.S., add glacial acetic acid and Yellow ppt sodium cobalt nitrate Take a platinum wire and dip it in conc. HCl. Heat it strongly until the wire does not impart any colour to the nonPurple flame luminous flame. Now dip the wire in the paste of the (Group V) precipitate in conc. HCl. Heat it in the flame. Brown ppt To O.S., add Nesslers reagent To O.S., add NaOH and heat Pungent smelling gas is evolved
K+ confirmed
Required Results: The given salt contains _____________ cation. Parameters: NA Relationship: NA Graphs: NA Error Analysis: NA Cautions: i. Since the experiment deals with acidic and basic conditions. The acids and the bases should be handled with care and dropper or a measuring cylinder should be used for addition of it. ii. Bases like NH4OH and conc. HNO3, HCl, H2SO4 should be used carefully, since they fume in air the bottle should be corked immediately after its use. iii. Many solution bumps out while heating; test tube should be kept in a slant position with its mouth away from the person carrying the experiment to avoid bumping on face.
32 LMCHE010
Requirements for Lab Technician: 1. Inorganic salt samples (Salts containing Zn2+, Ni2+, Ca2+ and Ba2+) 2. Dil. HCl 3. Dil. H2SO4 4. Dil. HNO3 5. H2S gas 6. Conc. HCl 7. Ammonium chloride 8. Ammonium hydroxide 9. Ammonium carbonate 10. Sodium hypophosphate 11. Glacial acetic acid 12. Sodium cobalt nitrate 13. Nesselers reagent 14. Sodium hydroxide
33 LMCHE010
Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To detect the presence of basic radicals (Gp VI Mg+2, K+, NH4+) Observation table: Sample Experiment Observation Inference
34 LMCHE010
Learning Outcomes (what I have learnt): to be written by the students in 50-70 words
To be filled in by faculty S.No Parameter (Scale from 1-10, 1 for very poor and 10 excellent) Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty Marks Obtained Maximum Marks 20 20 10 Total marks Obtained
1 2 3
35 LMCHE010
EXPERIMENT NO. 7 Aim: To detect the presence of one cation and one anion from a given salt Equipments to be used: Test tube, test tube holder, Bunsen burner, tripod stand, test tube and watch glass. Chemicals used: Inorganic salt, Dil. H2SO4, Conc. H2SO4, dil. HCl, Conc. HCl, H2S, NH4Cl, NH4OHand (NH4)2CO3. Learning Objectives: (i) Student will be able to detect cation and anion from any given salt. (ii) Student will be able to understand that the cations of group IV are not precipitated in group II. Outline of the procedure: As per the detection and confirmatory tests mentioned in Experiment 1 to Experiment 6, the cation and anion can be detected from a given salt. For example the salt under analysis is MgSO4, the procedure will be as follows: Analysis for Anion Preparation of Water extract (for water soluble salts): Dissolve a small amount of salt in 2-3 mL of distilled water, filter it and collect the filtrate for various tests. Experiment Dilute H2SO4 test: To the small amount of salt add 1-2 mL of dil. H2SO4 acid Conc. H2SO4 test: Heat a small amount of salt with conc. H2SO4 BaCl2 test: Take 1 mL water extract of the salt in water or sodium carbonate and after acidifying with dilute hydrochloric acid add BaCl2 solution. Observation No gas evolved Inferance CO32-absent Cl-, Br-, I- and NO3absent SO42- present
S.No. 1
No gas evolved
36 LMCHE010
Analysis of basic radical Preparation of Original Solution (O.S.): Dissolve 0.1 g of salt in water or dil. HCl or conc. HCl as per solubility. Experiment To the original solution add 5-10 drops of dil. HCl Pass H2S gas throughabove solution. Add 2-3 drops of conc. HNO3 to O.S., Heat the solution for a few minutes. After cooling add a small amount of solid ammonium chloride (NH4Cl) and an excess of ammonium hydroxide (NH4OH) solution till it smells of ammonia. Shake the test tube. Pass H2S through above alkaline solution. Take 1-2 mL original solution and add a small amount of solid NH4Cl and an excess of NH4OH solution followed by solid ammonium carbonate (NH4)2CO3. To O.S., add dil. HCl solution. Add NH4OH and Na2HPO4 solution. Observation No ppt No ppt Inference Gp I absent
S.No. 1 2.
Gp II absent
3.
No ppt
Gp III absent
No ppt
No ppt
The cation present in the salt is Mg2+ Required Results: The anion ____________ and cation __________________ is present in the salt. Parameters: NA Relationship: NA Graphs: NA Error Analysis: NA Cautions: 1. Since the experiment deals with acidic and basic conditions. The acids and the bases should be handled with care and dropper or a measuring cylinder should be used for addition of it. 2. Bases like NH4OH and conc. HNO3, HCl, H2SO4 should be used carefully, since they fume 37 LMCHE010
in air the bottle should be corked immediately after its use. 3. Many solution bumps out while heating; test tube should be kept in a slant position with its mouth away from the person carrying the experiment to avoid bumping on face. Requirements for Lab Technician: 1. Inorganic salt samples (Salts containing any cation or anion) 2. Dil. HCl 3. Dil. H2SO4 4. Dil. HNO3 5. H2S gas 6. Conc. HCl 7. Ammonium chloride 8. Ammonium hydroxide 9. Ammonium carbonate 10. Sodium hypophosphate 11. Glacial acetic acid 12. Sodium cobalt nitrate 13. Nesselers reagent 14. Sodium hydroxide
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Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To detect the presence of one cation and one anion from a given mixture Observation table: For Anion: Sample Experiment Observation Inference
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40 LMCHE010
Learning Outcomes (what I have learnt): to be written by the students in 50-70 words
To be filled in by faculty S.No Parameter (Scale from 1-10, 1 for very poor and 10 excellent) Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty Marks Obtained Maximum Marks 20 20 10 Total marks Obtained
1 2 3
41 LMCHE010
EXPERIMENT NO. 8 Aim: To determine Electrochemical Chemical Equivalent of Copper using Copper sulphate solution and Copper electrodes Equipments to be used: Copper voltameter, four copper plates, battery of 4 to 5 cells, a rheostat, one way key, connecting wires, sand paper, weighing balance, ammeter and stop watch Chemicals used: Copper sulphate, Conc.H2SO4, distilled water, dil HNO3 Learning Objectives:To know about Faradays first law of electrolysis: According to Faradays first law of electrolysis, the electrochemical equivalent, Z, is given by the relation: = where w is the mass of metal deposited, I is the current in amperes and t is the time in seconds. If the value of Z comes out to be fairly constant by passing the same current for different times, first law of electrolysis is verified. Procedure: Clean all the copper plates with nitric acid and wash them thoroughly in running tap water. Dry one of the plates and clean it with a piece of fine sand paper. Wash it and let it dry. Weigh accurately. Dissolve 30 g of powdered copper sulphate in 200 mL water by warming in beaker. Cool the solution and add Conc. H2SO4 to it. Fill the copper voltameter with this solution. Arrange the circuit as shown in figure
. Take out the central plate. Measure its length and breadth dipped in electrolyte. Calculate the area of plate and double it for total area of both sides dipped in the electrolyte. Put the plate in electrolyte. A good deposit is obtained when a current of one ampere is passed for every 100 sq cm of the cathode dipping in electrolyte.
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To test the connections, put the plug in key K and adjust the value of the current approximately equal to the calculated value. See that the current remains constant for about 5 mins. If on removing the central plate red deposits are seen on it, the connections are correct. Replace the central plate by the weighed copper plate, put in the key K and start the stop watch. Note the reading of the ammeter at intervals and see that the current remains constant. Adjust the current with a rheostat. Stop the stop watch after 30 minutes and at the same time take out the plug from the key K. Remove the cathode plate carefully, rinse it immediately in dil. H2SO4 and then wash it thoroughly in running water. Rinse it with alcohol. Dry it and find its weight accurately. Repeat the experiment by passing the current for 45 minutes. Note the current in ammeter after every 15 minutes. Calculate the electrochemical equivalent for the two observations.
Calculations: Length of the plate dipped = l cm Breadth of the plate dipped = b cm Total area dipped, a = 2l x b cm2 Current to be adjusted = a/100 amperes Initial weight of cathode w1(g) Final weight of cathode w2(g) Weight of copper deposited w = w2w1 Electrochemical equivalent =
S.No.
Current I (A)
Time t (s)
1. 2.
Result: The Electrochemical equivalent of copper is __________ g/C Scope of the result: As the value of the electrochemical equivalent of copper, Z, comes out be fairly constant, it verifies first law of electrolysis. Parameters: NA Relationships to be determined: NA Graphs/Plots: NA Error Analysis: NA. to
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Cautions: i. ii. The cathode plate must be cleaned thoroughly, dried and weighed accurately. The current should be constant throughout the experiment and should be adjusted at the rate of one ampere for every 100 sq.cm of the area of the copper plate dipping in copper sulphate solution. The plates should not touch each other. The electrolyte should be fresh and free from impurities. The weighed plate must be connected to the negative pole of battery. The plate must be rinsed in dilute sulphuric acid as it is removed from the electrolyte, otherwise the deposit will turn black due to oxidation.
Requirement for Lab Technician: 1. Copper plates 2. Copper sulphate 3. Conc. H2SO4 4. Ethanol 5. Dil. HNO3
44 LMCHE010
Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To determine Electrochemical Chemical Equivalent of Copper using Copper sulphate solution and Copper electrodes. Observations and Calculations: Length of the plate dipped = l cm Breadth of the plate dipped = b cm Total area dipped, a = 2l x b cm2 Current to be adjusted = a/100 amperes Weight of Electrochemical Initial Final copper equivalent weight of weight of Current Time t S.No. deposited cathode cathode I (A) (s) = w = w2 w1(g) w2(g) w1 1. 2. Results and Discussion:
Error Analysis: Learning Outcomes (what I have learnt): to be written by the students in 50-70 words.
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To be filled in by faculty Parameter (Scale from 1-10, 1 for S.No very poor and 10 excellent) 1 2 3 Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty
Marks Obtained
Maximum Marks 20 20 10
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EXPERIMENT NO. 9 Aim:To determine the percentage of iron in the given ferrous alloy by potassium permanganate method. Equipments to be used: Titration flask, pipette, burette, beakers, glass rod, funnel and burette stand Chemicals used:M/100 KMnO4, sample ferrous alloy solution (20g/L) and Dil. H2SO4. Learning Objective: (i) To determine the percentage of iron in given alloy :The molarity of the given solution of alloy can be determined by titrating it with standard KMnO4 solution in which the following redox reaction takes place which is based on the oxidation and the reduction reaction. The oxidising agent i.e Potassium permanganate oxidises the reducing agent ferrous sulphate and ferrous ammonium sulphate in acidic medium to ferric sulphate.The strength of alloy can be calculated and hence percentage of iron can be determined. (ii) To understand the redox reaction in the experiment. MnO4- + 8H+ + 5e- Mn2+ + 4H2O (Reduction) 5Fe2+ 5Fe3+ + 5e(Oxidation)
MnO4- + 8H+ + 5Fe2+ Mn2+ + 5Fe3+ + 4H2O (Overall Reaction) Indicator: KMnO4 acts as self-indicator. End point: Colorless to faint pink. Outline of Procedure Wash the whole apparatus thoroughly with distilled water. Rinse and fill the burette with the given solution of M/100 KMnO4 solution. Rinse the pipette with the given ore solution and pipette out 20 mL of the given ore solution in a titration flask. Add 20 mL of dil. H2SO4. Note the initial reading on the burette and start adding KMnO4 solution from the burette into the titration flask till light pink colour appears. Note the final reading on the burette and find the volume of KMnO4 solution used. Repeat the titration to get three concordant readings
Observation Table S.No. 1 2 3 47 LMCHE010 Burette reading Initial Final Volume of KMnO4 used
Calculations: Step 1 To calculate the molarity of ore solution Let the volume of KMnO4 solution used be = x mL Applying the molarity equation; i.e.
M1V1
n1 (Mohr salt)
M2V2 n2 (KMnO4)
n1 = 5
M 1 20 5
1 100
x 1
Molarity of iron in ore solution (M1) = x/400 M Step 2 To calculate the strength of iron in ore solution Since, Strength = Molarity Molecular mass Therefore strength of iron in ore solution = x/400 56 = y g/L Step 3 To determine percentage of iron Percentage of iron = y/20 x 100 Result: The percentage of iron is z% Parameters: NA Relationships to be determined: NA Graphs/Plots: NA Error Analysis: NA. Cautions: i. ii. iii. Dont hold the pipette from the bulb. Dont rinse the titration flask. Dont blow off the last drop from the pipette.
Requirement for Lab Technician: 1. M/100 KMnO4 2. Mohr salt solution (20g/L) 3. Dil. H2SO4
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Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To determine the percentage of iron in the given ferrous alloy by potassium permanganate method. Observation Table: S.No. 1 2 3 Calculations: Burette reading Initial Final Volume of KMnO4 used
Results and Discussion: Error Analysis: Learning Outcomes (what I have learnt): to be written by the students in 50-70 words.
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To be filled in by faculty Parameter (Scale from 1-10, 1 for S.No very poor and 10 excellent) 1 2 3 Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty
Marks Obtained
Maximum Marks 20 20 10
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EXPERIMENT NO. 10 Aim: To prepare phenol formaldehyde resin (bakelite). Equipments to be used: Beaker, glass rod, funnel and filter paper Chemicals used: Formaldehyde (40%), conc. H2SO4, distilled water, Glacial glacial acetic acid and phenol. Learning Objectives: i. To understand the concept of condensation polymerization: It is the one which is formed by combination of monomers accompanied by release of small molecules like H2O and NH3. To study the preparation of Bakelite: Bakelite formation involves the following reactions
ii.
Procedure: Place 5 mL of glacial glacial acetic acid and 5 mL of 40% formaldehyde solution in a 500 mL beaker. Add to it 2 grams of phenol with continuous stirring. Add a few drops of conc. H2SO4 with constant stirring. A pink solid plastic mass appears in the beaker. Wash the solid mass with water and dry it in the folds of filter paper. 51 LMCHE010
Calculate the yield of the product. Required Results: The yield of bakelite resin is __________ g Parameters: NA Relationships to be determined: NA Graphs/Plots: NA Error Analysis: As the polymerization is taking place theoretical yield cannot be calculated. The expected yield is 2g. Cautions: i. ii. While adding conc. H2SO4, it is better to stay little away from the beaker, since the reaction sometimes becomes vigorous. The reaction mixture should be stirred continuously. Requirement for Lab Technician: 1. 40% Formaldehyde 2. Phenol 3. Conc. H2SO4 4. Glacial acetic acid
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Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To prepare phenol formaldehyde resin (bakelite) Observations:
Results and Discussion: Error Analysis: Learning Outcomes (what I have learnt): to be written by the students in 50-70 words.
To be filled in by faculty Parameter (Scale from 1-10, 1 for S.No very poor and 10 excellent) 1 2 3 Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty
Marks Obtained
Maximum Marks 20 20 10
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EXPERIMENT NO. 11 Aim: To determine carbon monoxide content in emission from petrol vehicle. Equipments to be used: Old newspaper, plastic bag, rubber band or twist tie, tape, scissors, carbon monoxide detector and test automobile Learning Objectives: (i) The purpose of the experiment is to determine the carbon monoxide content. (ii) Student will be able to get an idea about how carbon monoxide is detected at various pollution control centers and how much is the toxicity level. (iii) Student will be able to compare the level of carbon monoxide emission from various petrol vehicles. Outline of the procedure: (I) Collection of the exhaust sample: Cut a 2-3mm hole toward the bottom of the plastic bag. Using a permanent marker, make a circle around the hole in the bag. Place a small piece of tape over the hole and make sure it is secure. Fold the end of the tape onto itself to create a small tab. Wrap the outside of the tailpipe with newspaper without blocking the exhaust. Compress the bag to remove all of the air from it and make sure the tape over the sampling hole is secure before collecting the sample. Hold the plastic bag against the newspaper that is wrapped around the tailpipe.
Start up the exhaust source while another person is ready to collect the sample of exhaust and twist the bag closed once it fills with the car exhaust by tying a rubber band. (II) Testing the sample Carefully pull back the tape covering the sampling hole and insert the carbon monoxide detector into the bag. Keep the detector inserted in the bag till it beeps. Note the reading on the detector. (III) Repeat the procedure for other sources. 54 LMCHE010
Required Results: The level of carbon monoxide is highest in _______________ and lowest in __________________. Parameters: NA Relationship: Between levels of carbon monoxide in exhaust from various petrol vehicles. Graphs: NA Error Analysis: NA Cautions: i. ii. iii. Exhaust should be collected carefully. Remember to cover the hole with the tape before collecting the exhaust. Keep you face away from the exhaust source.
Requirement for Lab Technician: 1. Carbon monoxide detector 2. Automobile exhaust 3. Rubber band 4. Tape 5. Polythene bag
55 LMCHE010
Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To determine carbon monoxide content in emission from petrol vehicle. Observation table: Automobile source Carbon monoxide level (ppm)
Learning Outcomes (what I have learnt): to be written by the students in 50-70 words
To be filled in by faculty S.No Parameter (Scale from 1-10, 1 for very poor and 10 excellent) Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty Marks Obtained Maximum Marks 20 20 10 Total marks Obtained
1 2 3
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EXPERIMENT NO. 12 Aim:To determine the amount of Dissolved Oxygen (DO) in the given water sample. Equipments to be used: 300 mL BOD bottles, titration flask, pipette, burette, beakers, glass rod, funnel and burette stand Chemicals used: Manganous sulphate, Alkali-iodide-azide, Concentrated H2SO4, Starch solution, 0.025M Sodium thiosulphate and Potassium iodide Learning Objectives:(i) To learn the importance of Dissolved oxygen as the measure of water contamination.:The concentration of Dissolved Oxygen (DO) in natural water and wastewater is a function of the temperature of the air and water, the degree of hardness of the water, and the demand for oxygen in the body of water. The solubility of oxygen increases with decreasing water temperature (oxygen solubility in water is inversely proportional to temperature). DO is an important parameter in wastewater treatment processes, most notably when dealing with an activated sludge system. (ii) To make the students learn about the reactions taking place in this method: Divalent manganese salt in solution is precipitated by alkali to manganese hydroxide MnSO4 + 2KOH Mn(OH)2 + K2SO4 In alkaline solution, dissolved oxygen is oxidized to form trivalent or higher valency hydroxide 2Mn(OH)2 + O2 2MnO(OH)2 Iodide ions reduce hydroxides to stable divalent ion by liberating equivalent amount of iodine. MnO(OH)2 + 2KI + H2O Mn(OH)2 + I2 + 2KOH Thiosulphate solution is used with starch indicator, to titrate iodine. I2 + 2S2O32- S4O62-+ 2IThe Iodine is equivalent to dissolved oxygen present in the sample. Indicator: Freshly prepared starch End point: Blue to colourless Outline of the procedure: Fill a 300mL BOD bottle with the sample to be analyzed. Pipette out 2 mL of manganous sulphate. Pipette out 2 mL of alkali-iodide-azide. Fix the stopper and invert the bottle several times to mix. Allow the precipitates to settle in the solution to about half the volume of the bottle. Invert the bottle several times to mix the precipitates back into the solution. Allow the precipitates in the solution to settle to about half the volume of the bottle.
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After settling, add 1 mL concentrated sulphuric acid along the sides of the bottle, fix the stopper and gently invert several times. Continue until the precipitate has dissolved back into solution. If a brown colour develops, dissolved oxygen is present in the sample. If no colour develops or it is very faint, it may be appropriate to obtain another sample at this time to ensure that there has not been an error in the sample preparation. Titration Take 200 mL of the above sample in a 500mL titration flask. Fill the burette with standard sodium thiosulphate solution (0.025M) Titrate the sample by adding sodium thiosulphate solution dropwise till solution of the flask turns pale yellow. Add 2-3 drops of starch solution and continue titrating dropwise until the disappearance of the blue / purple colouration. Note the volume used for thiosulphate used. Burette reading Initial Final
S.No. 1 2 3
Volume used
Calculations: When a 200mL sample is used, 1mL of sodium thiosulphate solution (0.025M) is equivalent to 1mg/L Dissolved Oxygen in the sample. (If 8.7mL of sodium thiosulphate was used, then DO of the sample is 8.7mg/L).
Result: The value of dissolved oxygen in the given sample of water was found to be mg/L. Parameters: NA Relationships to be determined: NA Graphs/Plots: NA Error Analysis: NA. Cautions: i. Always add concentrated H2SO4 in small amounts, along the sides of the bottle. ii. End point should be noted carefully. iii. Dont blow off the last drop of the pipette.
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Requirement for Lab Technician: 1. Waste water sample 2. Manganous sulphate 3. Alkali-iodide-azide 4. Conc. H2SO4 5. Starch solution 6. Potassium iodide solution 7. 0.025M Sodium thiosulphate
59 LMCHE010
Date of Performance: ________ Worksheet of the student Registration No.______________ Aim: To determine the amount of Dissolved Oxygen (DO) in the given water sample. Observation Table: Burette reading S.No. Volume used Initial Final 1 2 3 Mean volume :________________ml
Calculations
Error Analysis:
Learning Outcomes (what I have learnt): to be written by the students in 50-70 words.
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To be filled in by faculty S.No Parameter (Scale from 1-10, 1 for very poor and 10 excellent) Understanding of the student about the procedure/apparatus. Observations and analysis including learning outcomes Completion* of experiment, Discipline and Cleanliness Signature of Faculty Marks Obtained Maximum Marks 20 20 10 Total marks Obtained
1 2 3
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