Specimen copy of salt analysis
EXPERIMENT
1.PHYSICAL EXAMINATION Noted the colour of the salt
OBSERVATION
white
INFERENCE
Cu2+,Mn2+,Ni2+,Fe3+,Co2+ May be absent. NH4+,S2- ,CH3COO- MAY be absent
Noted the smell of the salt. 2.Dry heating test Heated a pinch of salt in a dry test tube and noted the following: y Gas is evolved.
No specific odour.
Reddish brown fumes. Colourless gas with smell of vinegar or pungent smell
NO2-/ NO3-/Br- may be present.
CH3 COOCl- may be present
Decrepitation crackling sound Sublimation Pb2+, NO3- , Ba2+ may be present. No/Sublimate formed. NH4+ abs / present.
Colour of the residue
Yellow when hot,white when cold Zn2+ may be present
3.Flame Test Prepared a paste of the salt with conc.HCl and performed flame test with a platinum wire. Analysis of Anion 4.Dil. H2SO4 test Treated a pinch of salt with dil. H2SO4.
Green Crimson Brick red
Ba2+ Sr2+ Ca2+
No effervescence No Rotten egg smell No Brown fumes No burning sulphure smell
CO32- abs S2- abs NO2- abs SO3 2- abs
5.Conc.H2SO4 test: Heated a pinch of salt with conc. H2SO4 . A glass rod dipped in NH4OH was shown to mouth of the test tube.
A colourless gas with suffocating smell was evolved. White fumes intensified.
May be Cl-.
OR A colourless gas with smell of vinegar was evolved. OR Colourless gas when passed through lime water, it turns milky. OR Brown fumes evolved,which intensified on addition of MnO2 Brown fumes intensified with copper turnings. Depending on the observation,confirmatory test to be performed there. 6.Test for phosphate Salt solution+ammonium molybdate and heated. 7.Test for sulphate Salt soln+Dil.HCl+BaCl 2 soln Analysis cation 8.test for NH4+ Heated a pinch of the salt with 2-3 ml NaOH solution.
May be acetate.
May be oxalate
May be BrMay be nitrate
canary yellow colour.
confirmed
white precipitate insoluble in Conc.HCl and conc.HNO3 confirmed
Smell of NH3 gas evolved. A rod dipped in Conc.HCl shown to evolved gas,dense white fumes were seen. White precipitate
NH4+ present
9.test for Group-1 To the salt solution,add dil.Hcl solution. Filter the precipitate and dissolve in hot water.Divide the solution into 2 parts. (i) + KI soln (ii) + k2CrO4
Pb2+
yellow ppt Yellow ppt (if Pb2+ is absent,use same soln for gr2) confirmed
10.Test for Group-2 To the above solution, pass H2S. Dissolve the ppt in 50% HNO3 and divide into 2 parts. 1 2 + NH4OH +Pottasium ferrocyanide Black ppt was formed. Cu2+ present
deep blue colour chocolate brown ppt
11.Test for Group-3 To the saltsolution,add 3-4 drops of Conc.HNO3.Boil the content for sometime.Add NH4Cl,NH4OH in excess.
Gelatinous white or Reddish brown ppt Al3+ Or Fe3+ (Confirmatory test)
12.Test For Group-4 To the salt solution,add NH4Cl,NH4OH and H2S
black ppt Buff coloured ppt White ppt
Ni2+,Co2+ Mn2+ Zn2+
(confirmatoty
test for ions)
13.Test for Group-5 To the salt solution,add NH4Cl,NH4OH and (NH4)2CO3 Filter the ppt,dissolve in acetic acid. divide into 3 parts. 1+potassium chromate soln 2+ammonium sulphate soln 3+ ammonium oxalate soln
White ppt
Ba2+,Ca2+,Sr2+
Yellow ppt White ppt White ppt
Ba2+, Sr2+ Ca2+, This sequence has to be followed whether Sr or Ca or Ba is present)
Conclusion: Acid radical-----Basic radical is -----------------Chemical equations for positive detections: 1 2. 3. 4.
Neatly written Answer sheet impresses every one. Volumetric Analysis
Aim: Apparatus:burette,pipette,volumetric flask,weighing bottle,clamp stand,conical flask,funnel,tile,weight box,balance ,beaker etc Chemicals: Theory: Titration between KMnO4 and Oxalic acid/Mohrs salt solution is a redox titration where KMnO4 oxidises oxalic acd or ferrous ion in Mohrs salt solution to CO2 and ferric ions respectively,itsef is reduced to Mn2+ ions in acidic medium. IONIC EQUATION:
Molecular equation:
Solution in burette:KMnO4 solution in pipette:10 ml oxalic acid / mohrs salt solution
Solution in the conical flask:10ml oxalic acid / mohrs salt solution and half test tube H2SO4 Indicator:KMnO4 is self indicator End point:Colourless-pink Temperature of the reaction:50 60 degree in case of oxalic acid Room temperature in case of mohrs salt solution Medium of the reaction: Acidic Catalyst used: Mn2+ions in case of oxalic acid Calculation for preparation of oxalic acid / Mohrs salt solution: Molarity = no.of moles / vol. of the solution
Wt. of the sample = x g Wt of weighing bottle = W1 g
Wt of weighing bottle + sample = W2 g Wt of the sample = W2 W1 g
OBSERVATION TABLE S.N 1 2 3 Calculation: M1 =molarity of kMnO4 solution M2 =molarity of oxalic acid or Mohrs salt solution V2 = volume of oxalic acid or Mohrs salt solution (10ml) n2 = Stoichiometric coefficient oxalic acid or Mohrs salt solution initial burette reading in ml p q r Final burette reading in ml q r s Difference in volume ( ml) q-p same same
V1 = volume of KMnO4 used
n1 = Stoichiometric coefficient of KMnO4
M1V1 = M2V2 n1 M1 = ? Strength of KMnO4 solution = M1 x 158 = g/l Precautions: Rinse the burette and pipette with respective solutions. Do not heat the mixture in conical flask more than 60 degrr. Add H2SO4 to Mohrs salt while preparing solution. Always take upper meniscus of KmnO4 Take enough care while weighing the sample in analytical balance Do not add KMnO4 soln. from the burette at a stretch. Clean conical flask properly after taking an observation. Add anything u would like to . n2
