QUANTITATIVE AND QUALITATIVE ANALYSIS Identification of ions

 

WEEK 2

TOPIC: QUANTITATIVE AND QUALITATIVE ANALYSIS

CONTENT:

  1. Identification of ions
  2. Test for gases
  3. Identification of fats and oils

Sub-topic 1: IDENTIFICATION OF IONS

IDENTIFICATION OF CATIONS AND ANIONS

CATIONS: Zn2+, Al3+, pb2+ , Ca2+ ,Fe2+ Fe3+, Cu2+, NH4+

  1. THE USE OF NaOH(aq): If a few drops of NaoH(aq) is added to aqueous solutions of the salts of the above cations the following observations will be made. If it is:

a. Zn2+: There will be formation of a white gelatinous precipitate which will be soluble in excess NaoH(aq).

b. Al3+There will be formation of a white gelatinous precipitate which will be soluble in excess NaoH (aq).

c. Pb2+:There will be formation of a white precipitate which will be soluble in excess NaoH(aq).

d. Ca2+: There will be formation of a white precipitate which will be soluble in excess NaoH(aq).

e. Fe2+: There will be formation of a green gelatinous precipitate which will be insoluble in excess NaOH(aq).

f. Fe3+ There will be formation of reddish- brown gelatinous precipitate which will be insoluble in excess NaoH(aq).

g. Cu2+: There will be a formation of a blue precipitate which is insoluble in excess NaoH(aq).

h. NH4+: If NaoH(aq) is added to the test solution and warmed, a colourless gas with irritating smell which will turn moist red litmus paper to blue will be evolved. Thus, showing that the test solution is containing NH4+ i. e. the test solution is an NH4+ salt solution.

ANIONS: Cl, NO3, SO42-, SO32-, CO32-:

The following tests help to identify these anions:

  1. Cl : To the test solution add dilute HNO3 acid (there will not be visible reaction), followed by AgNO3(aq), (there will be formation of a white precipitate). To the precipitate add NH3(aq) in excess and shake . If the precipitate dissolves then the test solution is containing Cl ions.
  2. NO3: To the test solution add FRESHLY prepared FeSO4 solution followed by concentrated H2SO4 acid. Formation of a brown ring indicates the presence of NO3 ions.
  3. SO42- : To the test solution add dilute HCI acid,(there will not be any visible reaction, this is just to get rid of any other ions that may tamper with the experiment), followed by BaCl2(aq). There will be formation of a white precipitate which will be insoluble in excess dil.HCI. This shows that SO42- is present in the test solution.
  4. SO32-: To the test solution add BaCl2(aq). There will be formation of a white precipitate which will be soluble in dil. HCl acid
  5. CO32-: The test for CO32-, is also carried out exactly in the same way as in (d) above. The same result is obtained. To differentiate between SO32- and CO32- , add MgSO4(aq) solution to solutions containing SO32-and CO32- ions in different test tubes. The one that gives a white precipitate is CO32- . The example below shows how to report salt analysis.

Worked Example

  1. Credit will be given for strict adherence to instructions, for observations precisely recorded and for accurate inferences. All tests, observations and inferences must be clearly entered in your work book, in ink, at the time they are made. C is a mixture of two salts. Carry out the following exercises on C. Record your observations and identify any gas (es) evolved. State the conclusion you draw from the result of each test. (a) Put all of C in a test tube and add about 10cm3 of distilled water. Shake thoroughly and filter. Keep both the filtrate and the residue. Divide the filtrate into three portions. (i) To first portion, add NaOH(aq) in drops and then in excess. (ii) To the second portion, add NH3 solution in drops and then in excess. (iii) To the third portion, BaCl2(aq) followed by dilute HCl. (b) Divide the residue into two portions. (i) Heat the first portion strongly in a test tube. (ii) Add dilute HCl to the second portion.

Solution

TESTOBSERVATIONINFERENCE
(a)(i) C + H2O,

then filter

Green residue and blue filtrate were observedC is a mixture of soluble and

insoluble salts.

(ii) Filtrate + NaOH(aq) in drops,

then in excess

A blue gelatinous precipitate which is insoluble in excess was formed.Cu2+ present
(iii) Filtrate + NH3(aq) in drops, then in excessA pale blue gelatinous precipitate was formed. The precipitate dissolves or is soluble in excess NH3(aq) to give deep blue solution.Cu2+ is confirmed
(iv) Filtrate + BaCl2 + dil. HClA white precipitate, insoluble in dil. HCl was observed.SO42- is present
(b)(i) First portion of residue + heatThe colour changed from green to black powder
(ii) Second portion of residue + dil. HClThere was effervescence and a colourless, odourless gas which turn lime water milky was given offGas is CO2 from CO32-

EVALUATION

  1. Credit will be given for strict adherence to instructions, for observations precisely recorded and for accurate inferences. All tests, observations and inferences must be clearly entered in your work book, in ink, at the time they are made. C is a mixture of two salts. Carry out the following exercises on C. Record your observations and identify any gas(es) evolved. State the conclusion you draw from the result of each test. (a) Put C into a beaker and add about 10cm3 of distilled water, stir the mixture and filter. Test the filtrate with litmus papers. Keep the residue and filtrate. (b)(i) To about 2cm3 of the filtrate, add few drops of aqueous HNO3 followed by AgNO3(aq) .

(ii) Add excess NH3 solution to the resulting mixture. (c) To about half of the residue from 1(a) above, add about 5cm3 of dilute HNO3 in drops. Divide the resulting solution into two equal portions. (d) (i) To the first portion, add ammonia solution in drops and then in excess. (ii) To the second portion, add dilute HCl.

Sub-topic 2: Test for gases

SO2, H2S, NH3, CO2, NO2, HCI, O2, CI2 and H2

GASODOURCOLOURCOMFIRMATORY TESTSUSPECTED SALT
SO2Irritating smellColourlessChanges acidified k2cr207 solution from orange to green. Change acidified KMNO4 solution from purple to colourless. It turns moist blue litmus paper to red.SO32- of Na or K
H2SRotten egg smellColourlessIt changes acidified K2Cr2O7 solution from orange to green with yellow sulphur deposit. It changes acidified KMnO4 Solution from purple to colourless with yellow sulphur deposits

Turns (CH3 COO2)Pb solution or paper black. Turns Pb(NO3)2 paper or solution to black. Turns moist blue litmus paper red.

S2- of metal e.g.

FeS

NH3Choking smellColourlessTurn moist red litmus paper to blue. Gives white fumes with HCINH4+ salts
CO2OdourlessColourlessTurns moist blue litmus paper red. Turns lime water milkyHCO3and CO32- Salts
NO2Irritating smellReddish-brownIt turns moist blue litmus paper to red. Turns moist starch-iodide paper to blue-blackNO3 of heavy metals e.g.Pb(NO3)2
HCISharp irritating smellColourlessTurns moist blue litmus paper red. Form white fumes with ammonia gas.CI salts
O2OdourlessColourlessRekindle a glowing splintKClO3
CI2Pungent smellGreenish- yellowTurns moist blue litmus paper to pink then bleaches it. Turns moist starch – iodide paper to dark blue.Cl of Na, Mg
H2OdourlessColourlessGives a pop sound when ignited in the air.H2 is obtained when certain metals e.g. Zn, Sn and Al react with acids, water, steam or hot concentrated NaOH or KOH Solution.