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INORGANIC PRESENTATION

 TOPIC: THEORITICAL ASPECTS OF
            ANIONS

SUBMITTED BY: NIDHI CHAUDHARY
      B.Sc(H) CHEMISTRY
         VI SEMESTER
QUALITATIVE
     INORGANIC
     ANALYSIS
It is the analysis (i.e. detection and
identification) of the cations and
anions present in given compound
or salt mixture.
IDENTIFICATION OF ANIONS
    AND CATIONS
    Identification of anions/cations is done through
    a series of tests, broadly divided into :
   Preliminary tests : provide us with the idea of
    the cation/anion present in the compound.
   Confirmatory tests : confirm the presence of the
    cation/anion in a given compound.
ANIONS
   Anion is an ion with more electrons than
    protons, giving it a net negative
    charge (since electrons are negatively
    charged and protons are positively
    charged).
   Anions are contributed by acids, therefore,
    they are called as acid radicals.
    For example, the anion (or acid radical) Cl-
    in a water solution of salt sodium chloride
    (NaCl) comes from the hydrochloric acid
    (HCl) and the cation (or basic radical) Na+
    from the base sodium hydroxide (NaOH).
PREPARING TEST
SOLUTIONS
Most of the confirmatory tests of the cations/anions are not
  carried out with the solid mixture but with their solutions :
 Water Extract: If the given compound is soluble in water,
  then 1-2 g of mixture is dissolved in distilled water (10-20
  ml).
 Sodium Carbonate (soda) Extract: If the compound is
  insoluble in water, then 1 g of mixture is taken along with
  2 g Na2CO3 in distilled water (15-20 ml) and heated for
  15 minutes. Solution is filtered and the filterate is soda
  extract.
CLASSIFICATION OF ANIONS

Anions can not be classified into specific
  groups but their action with sulphuric
  acid divides them into three
  categories:
 Dilute Sulphuric Acid: CO 2-, NO -,
                             3         2
  CH3COO-, S2-, SO32-
 Conc. Sulphuric Acid: Cl-, Br-, I-, NO -,
                                         3
 Independent Radicals: SO 2-,PO 3-,BO 3-,
                              4      4     3
  C2O42-
SNo         EXPERIMENT              OBSERVATIONS           INFERENCE



1.    TEST FOR CARBONATE
              (CO32-)
      Pre. Test : To a pinch of   Colorless gas evolves   May be CO32- .
      mixture add few drops of    with brisk
      dilute sulphuric acid.      effervescence.
                                  2 H+ + CO32-   H2O +
                                  CO2

      Con. Test : Pass the gas    Lime water turns
      evolved in the above step   milky.
      through lime water.         M(OH)2 + CO2 MCO3       CO32-
                                  + H2O                   confirmed.
SNo.           EXPERIMENT                   OBSERVATIONS             INFERENCE
 2.         TEST FOR NITRITE
                  (NO2-)                Reddish brown vapors
       Pre. Test : To a pinch of        observed.                  May be NO2- .
       mixture in test tube, add dilute 2MNO2 + H2SO4    M2SO4
       sulfuric acid.                   + HNO2
                                        3MNO2      H20 + HNO3 +
                                        NO
                                        NO + O2     NO2 (brown
                                        fumes)
       Con. Test : (a) To the above     A deep blue coloration
       solution, add 0.5 ml of          observed.
       potassium iodide solution                                   NO2- confirmed.
                                        2KI + 2MNO2 + H2SO4
       followed by 0.5 ml of pure       K2SO4 + I2 + NO + H2O
       starch solution.
                                        I2 + STARCH BLUE
                                        COLORED COMPLEX

       (b) Take water extract or soda
       extract of the compound and      A dark brown or black
                                        coloration obtained.       NO2- confirmed.
       add dilute sulfuric acid
       followed by freshly prepared     MNO2 + H2SO4      MSO4 +
       ferrous sulphate solution.       HNO2
                                        HNO2     HNO3 + NO
                                        FeSO4 + NO     FeSO4.NO
SNo.           EXPERIMENT                    OBSERVATIONS             INFERENCE
 3.         TEST FOR ACETATE
                (CH3COO-)
       Pre. Test : A pinch of mixture   Vinegar like smell is     May be CH3COO- .
       is treated with dilute sulphuric obtained.
       acid .                           M(CH3COO) + H2SO4
                                        CH3COOH + MSO4
       OR,
       1-1.5 g of mixture is taken in   Vinegar like smell is
       watch glass to which a pinch     obtained.
       of oxalic acid and a few drops
       of water were added.

                                        Deep red colored
       Con. Test: (a) 1 ml of           precipitate is observed
       water/soda extract is            due to formation of a
       neutralized with dilute acetic   complex.
       acid followed by addition of
       ferric chloride solution.        CH3COO- + Fe3+ + H2O      CH3COO- confirmed.
                                        [Fe3(OH)2(CH3COO)6]+ +
                                        2H+
                                        [Fe3(OH)2(CH3COO)6]+ +
                                        H2O     CH3COOH +
                                        [Fe(OH)2(CH3COO)] + H+
SNo.          EXPERIMENT                   OBSERVATIONS          INFERENCE


(b)    To 1 ml of water/soda                                  CH3COO- confirmed.
                                   Blue color is obtained.
       extract lithium nitrate
       solution and potassium
       iodide solution were added.
       After this, few drops of
       dilute ammonia solution was
       added and the resultant
       solution was heated.


(c)    Equal volume of soda/water
                                                              CH3COO- confirmed.
       extract and pure calcium       Yellow precipitate is
       hydroxide is taken in a test   obtained.
       tube. Heat the solution and    Ca(OH)2 + M(CH3COO)
       pass the evolved vapors into   CH3COCH3
       a solution of 2,4 DNP
       hydrazine.                     CH3COCH3 +
                                      H2NHC6H5(NO2)
                                      (CH3)2CNNHC6H5(NH2)2
SNo.          EXPERIMENT                     OBSERVATIONS                INFERENCE

 4.       TEST FOR SULPHIDE
                    (S2-)
       Pre. Test: Take a pinch of      A colorless gas evolves       May be S2- .
       mixture in a test tube and      which smells like rotten
       add dilute sulphuric acid.      egg.
                                       S2- + H2SO4    H2S + SO42-

       Con Test: a) Pass the above     Yellow precipitate is
       gas in cadmium acetate.         obtained.
                                       Cd(CH3COO)2 + H2S       CdS
                                                                     S2- confirmed.
                                       + CH3COOH

       Acidify 1-2 ml of soda/water    Black precipitate obtained.
(b)    extract with dilute acetic      H2S + Pb(CH3COO)2 PbS
       acid and boil the solution to   + CH3COOH
       expel carbon dioxide. To this                                 S2- confirmed.
       add 1-2 ml of lead acetate
       solution.
       Add 1-2 ml of freshly
(c)    prepared sodium                 Violet coloration obtained.
       nitroprusside solution to the   S2- + Na2[Fe(CN)5NO]
       soda/water extract.                                           S2- confirmed.
                                       Na4[Fe(CN)5NOS]
SNO          EXPERIMENT                   OBSERVATIONS                 INFERENCE


5.       TEST FOR SULPHITE
               (SO32-)
      Pre. Test: Take a pinch of     A colorless and pungent       May be SO32-
      mixture and add 2-3 ml of      smelling gas evolves.
      dilute sulphuric acid.

      Con.Test: (a) Take 1-2 ml of   A green color is obtained.
      soda/water extract; add 2-3    3Na2SO3 + K2Cr2O7 + 4H2SO4
      ml of dilute sulphuric acid        Cr2(SO4)3 (Green color)
      and few drops of potassium                                   SO32- confirmed.
      dichromate solution.           + 3Na2SO4 + 4H2O + K2SO4



(b)   Take a pinch of mixture and    Sulphur dioxide is evolved.
      add 2-3 ml of dilute
      hydrochloric acid.                                           SO32- confirmed.
                                     White precipitate is
      Pass the gas evolved           obtained.
      through lime water.
SNo           EXPERIMENT                   OBSERVATIONS                 INFERENCE


6.        TEST FOR CHLORIDE
                   (Cl-)
      Pre Test: To a pinch of        Greenish yellow gas having   May be Cl- .
      mixture, add 1-2 ml of conc.   pungent smell evolves.
      sulphuric acid.                Dense white fumes observed.
      Bring a glass rod dipped in    NaCl + H2SO4    NaHSO4 +
      ammonium hydroxide near        HCl
      the mouth of the above test
                                     HCl + NH4OH      NH4Cl + H2O
      tube.
                                     White precipitate formed
      Con. Test: (a) To the          which is soluble in excess of
      water/soda extract, add dilute ammonium hydroxide.
      nitric acid and few drops of   AgNO3 + NaCl       AgCl +
      silver nitrate.                NaNO3
                                                                     Cl- confirmed.
                                     AgCl + 2NH4OH
                                     [Ag(NH3)2Cl] (soluble
                                     complex) + 2H2O
SNO          EXPERIMENT                    OBSERVATIONS                 INFERENCE


(b)   Chromyl Chloride Test -        Yellow precipitate is formed.   Cl- confirmed.
      Take about 0.2 g of mixture    K2Cr2O7 + 4NaCl + 6H2SO4
      in a test tube and add about    2CrO2Cl2
      0.3 g of solid potassium       (chromyl chloride) + 2KHSO4
      dichromate and 2 ml of         + 4NaHSO4 + 3H2O
      conc. sulphuric acid. Heat
      the mixture and pass the gas
      evolved into a tube            CrO2Cl2 + 4NaOH
      containing sodium              Na2CrO4 + 2NaCl + 2H2O
      hydroxide solution. Add 1 ml
      of lead acetate solution.
                                     Na2CrO4 + Pb(CH3COO)2
                                     PbCrO4 (yellow) +
                                     2CH3COONa
SNO          EXPERIMENT                   OBSERVATIONS               INFERENCE
7.       TEST FOR BROMIDE
                  (Br-)
      Pre. Test: To a pinch of       Reddish brown vapors
      mixture, add conc.             with a pungent smell        May be Br-.
      sulphuric acid.                evolved.
                                     KBr + H2SO4     KHSO4 +
                                     HBr
                                     2HBr + H2SO4    Br2 + SO2
                                     + 2H2O

      Con Test: (a) Take 0.5 ml of
      soda/water extract and         Yellow precipitate obtained
      then add 0.5 ml of dilute      which is sparingly soluble
      nitric acid and few drops of   in ammonium hydroxide.
      silver nitrate solution.       NaBr + AgNO3       AgBr     Br- confirmed.
                                     + NaNO3
                                     AgBr + 2NH4OH
                                     [Ag(NH3)2]Br + 2H2O
SNO         EXPERIMENT                   OBSERVATIONS                 INFERENCE



(b)   Take 0.5 ml of soda/water     Organic solvent layer         Br- confirmed.
      extract of the mixture and    attains orange color due to
      add 0.5 ml of carbon          dissolution of evolved
      tetrachloride or chloroform   bromine in it.
      followed by 1 ml of conc.     NaBr + HNO3       NaNO3 +
      nitric acid or chlorine       HBr
      water. Warm the mixture
      and shake the test tube.      2HBr + 2HNO3        Br2 +
                                    2NO2 + 2H2O
SNO          EXPERIMENT                  OBSERVATIONS                INFERENCE



8.          TEST FOR IODIDE
                    (I-)
      Pre. Test: To a pinch of       Violet vapors of iodine     May be I-.
      mixture, add conc sulphuric    evolved due to partial
      acid.                          decomposition of the
                                     formed HI.
                                     KI + H2SO4     KHSO4 +
                                     HI
                                     2HI + H2SO4    I2 + SO2 +
                                     2H2O


      Con Test: (a) Take 0.5 ml of
      soda/water extract and then    Yellow precipitate
      add 0.5 ml of dilute nitric    obtained which is
      acid followed by 0.5 ml of     insoluble in ammonium       I- confirmed.
      silver nitrate solution.       hydroxide.
                                     NaI + AgNO3     AgI +
                                     NaNO3
SNO           EXPERIMENT                   OBSERVATIONS                 INFERENCE


(b)   Take 0.5 ml of soda/water        Organic solvent layer        I- confirmed.
      extract of the mixture and            attains violet color
      add 0.5 ml of carbon                  due to dissolution of
      tetrachloride or chloroform           iodine in it.
      followed by 1 ml of conc.        NaI + HNO3       NaNO3 +
      Nitric acid or chlorine water.        HI
      Warm the mixture and shake
      the test tube vigorously.        4HI + O2      2I2 + 2H2O
SNO          EXPERIMENT                   OBSERVATIONS               INFERENCE

9.        TEST FOR NITRATE
                (NO3-)
      Pre. Test: To a pinch of    Light brown fumes               May be NO3-
      mixture, add conc sulphuric observed which intensify
      acid.                       on heating the mixture
                                  with copper turnings.
                                  NaNO3 + H2SO4
                                  NaHSO4 + HNO3
                                      4HNO3     4NO2   + O2 +
                                      2H2O


      Con Test: Take around 1 ml      A brown black ring at the
      of soda/water extract and       junction of two layers is
      acidify with dilute sulphuric   formed.
      acid. Add 2-3 ml of freshly     NaNO3 + H2SO4               NO3- confirmed.
      prepared ferrous sulphate       NaHSO4 + HNO3
      solution and then pour
                                      2HNO3 + 6FeSO4 + 3H2SO4
      conc. sulphuric acid slowly
      in thin stream along the            3Fe2(SO4)3 + 2NO +
      sides of the test tube.         4H2O
                                      FeSO4 + NO
                                      FeSO4.NO(brown ring)
SNO          EXPERIMENT                    OBSERVATIONS                 INFERENCE

10.       TEST FOR OXALATE
                (C2O42-)
      Pre. Test: Add conc             Evolved gas burns with a      May be C2O42-.
      sulphuric acid(1-2 ml) to a     blue flame.
      pinch of given mixture(0.1 g)   (COONa)2 + H2SO4
      and heat the solution. .        Na2SO4 + (COOH)2
      Bring the mouth of the test     (COOH)2      CO + CO2 +
                                      H2O
      tube near the flame.
      Also pass the gas in the lime
      water.                          Lime water turns milky.



      Con Test: (a) Acidify 1 ml of
      soda/water extract of the       White precipitate obtained.
      mixture with dilute acetic      (COONa)2 + H2SO4
      acid and boil the solution.     Na2SO4 + (COOH)2
      Then add 1 ml of calcium
      chloride solution and shake     (COOH)2 + CaCl2
      the test tube.                  (COO)2Ca + 2HCl
SNO           EXPERIMENT                    OBSERVATIONS             INFERENCE


      Dissolve the precipitate in      Pink color of potassium   C2O42- confirmed.
                                       permanganate gets
      minimum quantity of dilute
                                       discharged.
      sulphuric acid and then add
      potassium permanganate           (COO)2Ca + H2SO4
      solution drop wise.              (COOH)2 + CaSO4

                                       2KMnO4 + 3H2SO4 +
                                       5(COOH)2     2MnSO4 +
                                       K2SO4 + 10CO2 + 8H2O


(b)   Acidify soda/water extract
      with dilute acetic acid and      Yellow precipitate
      boil the solution. Add ferrous   obtained.
      sulphate solution.                                         C2O42- confirmed.
                                       C2O42- + Fe2+
                                       [Fe(C2O4)]2-
SNO          EXPERIMENT                     OBSERVATIONS               INFERENCE


11.     TEST FOR FLUORIDE
               (F-)
      Pre. Test: Take 0.1 g of the   Oily droplets are formed      May be F-
      mixture and add 1 ml of        along the sides of the test
                                     tube.
      conc. sulphuric acid.
                                     2NaF + H2SO4      Na2SO4 +
                                     2HF




      Con Test: Add a pinch of       White gelatinous deposit
      sand to the above reaction     on the glass rod observed.
      mixture. Heat it. Bring a                                    F- confirmed.
                                     4NaF + H2SO4 + SiO2
      glass rod moistened with
      water near the mouth of        SiF4   + 2Na2SO4 + 2H2O
      the test tube.                 3SiF4 + 4H2O     H4SiO4 +
                                     2H2SiF6 (hydrofluorosilicic
                                     acid; waxy appearance)
SNO           EXPERIMENT                     OBSERVATIONS                INFERENCE

12.      TEST FOR SULPHATE
               (SO42-)
      To the soda/water extract (1      White precipitate obtained   SO42- confirmed.
      ml) add dilute hydrochloric       which is insoluble in conc
      acid (1 ml) so as to remove       hydrochloric acid.
      the carbonate (if present).       Na2SO4 + BaCl2       BaSO4
      Add 1 ml of barium chloride        + 2NaCl
      solution.




13.      TEST FOR PHOSPHATE
                (PO43-)
      Take a pinch of the given                                      PO43- confirmed.
      mixture in a test tube and add
                                        Yellow precipitate is
      about 1 ml of conc nitric acid.
                                        obtained.
      Boil the contents and add
      excess of ammonium                PO43- + 12MoO42- + 24H+
      molybdate solution.               PMo12O403-   + 12H2O
SNO          EXPERIMENT                   OBSERVATIONS               INFERENCE

14.       TEST FOR BORATE
                (BO33-)

      In a porcelain dish, take a     Green flame is observed.   BO33- confirmed.
      small amount of the mixture,    Na3BO3 + 3H2SO4
      say 0.2-0.3 g, and add nearly   Na2SO4 + 2H3BO3
      1 ml of conc sulphuric acid
      followed by 1 ml of ethyl
      alcohol. Heat the dish and      H3BO3 + C2H5OH
      bring a burning paper over      B(OC2H5)3 + H2O
      it.

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Qualitative analysis of anions

  • 1. INORGANIC PRESENTATION TOPIC: THEORITICAL ASPECTS OF ANIONS SUBMITTED BY: NIDHI CHAUDHARY B.Sc(H) CHEMISTRY VI SEMESTER
  • 2. QUALITATIVE INORGANIC ANALYSIS It is the analysis (i.e. detection and identification) of the cations and anions present in given compound or salt mixture.
  • 3. IDENTIFICATION OF ANIONS AND CATIONS Identification of anions/cations is done through a series of tests, broadly divided into :  Preliminary tests : provide us with the idea of the cation/anion present in the compound.  Confirmatory tests : confirm the presence of the cation/anion in a given compound.
  • 4. ANIONS  Anion is an ion with more electrons than protons, giving it a net negative charge (since electrons are negatively charged and protons are positively charged).  Anions are contributed by acids, therefore, they are called as acid radicals. For example, the anion (or acid radical) Cl- in a water solution of salt sodium chloride (NaCl) comes from the hydrochloric acid (HCl) and the cation (or basic radical) Na+ from the base sodium hydroxide (NaOH).
  • 5. PREPARING TEST SOLUTIONS Most of the confirmatory tests of the cations/anions are not carried out with the solid mixture but with their solutions :  Water Extract: If the given compound is soluble in water, then 1-2 g of mixture is dissolved in distilled water (10-20 ml).  Sodium Carbonate (soda) Extract: If the compound is insoluble in water, then 1 g of mixture is taken along with 2 g Na2CO3 in distilled water (15-20 ml) and heated for 15 minutes. Solution is filtered and the filterate is soda extract.
  • 6. CLASSIFICATION OF ANIONS Anions can not be classified into specific groups but their action with sulphuric acid divides them into three categories:  Dilute Sulphuric Acid: CO 2-, NO -, 3 2 CH3COO-, S2-, SO32-  Conc. Sulphuric Acid: Cl-, Br-, I-, NO -, 3  Independent Radicals: SO 2-,PO 3-,BO 3-, 4 4 3 C2O42-
  • 7. SNo EXPERIMENT OBSERVATIONS INFERENCE 1. TEST FOR CARBONATE (CO32-) Pre. Test : To a pinch of Colorless gas evolves May be CO32- . mixture add few drops of with brisk dilute sulphuric acid. effervescence. 2 H+ + CO32- H2O + CO2 Con. Test : Pass the gas Lime water turns evolved in the above step milky. through lime water. M(OH)2 + CO2 MCO3 CO32- + H2O confirmed.
  • 8. SNo. EXPERIMENT OBSERVATIONS INFERENCE 2. TEST FOR NITRITE (NO2-) Reddish brown vapors Pre. Test : To a pinch of observed. May be NO2- . mixture in test tube, add dilute 2MNO2 + H2SO4 M2SO4 sulfuric acid. + HNO2 3MNO2 H20 + HNO3 + NO NO + O2 NO2 (brown fumes) Con. Test : (a) To the above A deep blue coloration solution, add 0.5 ml of observed. potassium iodide solution NO2- confirmed. 2KI + 2MNO2 + H2SO4 followed by 0.5 ml of pure K2SO4 + I2 + NO + H2O starch solution. I2 + STARCH BLUE COLORED COMPLEX (b) Take water extract or soda extract of the compound and A dark brown or black coloration obtained. NO2- confirmed. add dilute sulfuric acid followed by freshly prepared MNO2 + H2SO4 MSO4 + ferrous sulphate solution. HNO2 HNO2 HNO3 + NO FeSO4 + NO FeSO4.NO
  • 9. SNo. EXPERIMENT OBSERVATIONS INFERENCE 3. TEST FOR ACETATE (CH3COO-) Pre. Test : A pinch of mixture Vinegar like smell is May be CH3COO- . is treated with dilute sulphuric obtained. acid . M(CH3COO) + H2SO4 CH3COOH + MSO4 OR, 1-1.5 g of mixture is taken in Vinegar like smell is watch glass to which a pinch obtained. of oxalic acid and a few drops of water were added. Deep red colored Con. Test: (a) 1 ml of precipitate is observed water/soda extract is due to formation of a neutralized with dilute acetic complex. acid followed by addition of ferric chloride solution. CH3COO- + Fe3+ + H2O CH3COO- confirmed. [Fe3(OH)2(CH3COO)6]+ + 2H+ [Fe3(OH)2(CH3COO)6]+ + H2O CH3COOH + [Fe(OH)2(CH3COO)] + H+
  • 10. SNo. EXPERIMENT OBSERVATIONS INFERENCE (b) To 1 ml of water/soda CH3COO- confirmed. Blue color is obtained. extract lithium nitrate solution and potassium iodide solution were added. After this, few drops of dilute ammonia solution was added and the resultant solution was heated. (c) Equal volume of soda/water CH3COO- confirmed. extract and pure calcium Yellow precipitate is hydroxide is taken in a test obtained. tube. Heat the solution and Ca(OH)2 + M(CH3COO) pass the evolved vapors into CH3COCH3 a solution of 2,4 DNP hydrazine. CH3COCH3 + H2NHC6H5(NO2) (CH3)2CNNHC6H5(NH2)2
  • 11. SNo. EXPERIMENT OBSERVATIONS INFERENCE 4. TEST FOR SULPHIDE (S2-) Pre. Test: Take a pinch of A colorless gas evolves May be S2- . mixture in a test tube and which smells like rotten add dilute sulphuric acid. egg. S2- + H2SO4 H2S + SO42- Con Test: a) Pass the above Yellow precipitate is gas in cadmium acetate. obtained. Cd(CH3COO)2 + H2S CdS S2- confirmed. + CH3COOH Acidify 1-2 ml of soda/water Black precipitate obtained. (b) extract with dilute acetic H2S + Pb(CH3COO)2 PbS acid and boil the solution to + CH3COOH expel carbon dioxide. To this S2- confirmed. add 1-2 ml of lead acetate solution. Add 1-2 ml of freshly (c) prepared sodium Violet coloration obtained. nitroprusside solution to the S2- + Na2[Fe(CN)5NO] soda/water extract. S2- confirmed. Na4[Fe(CN)5NOS]
  • 12. SNO EXPERIMENT OBSERVATIONS INFERENCE 5. TEST FOR SULPHITE (SO32-) Pre. Test: Take a pinch of A colorless and pungent May be SO32- mixture and add 2-3 ml of smelling gas evolves. dilute sulphuric acid. Con.Test: (a) Take 1-2 ml of A green color is obtained. soda/water extract; add 2-3 3Na2SO3 + K2Cr2O7 + 4H2SO4 ml of dilute sulphuric acid Cr2(SO4)3 (Green color) and few drops of potassium SO32- confirmed. dichromate solution. + 3Na2SO4 + 4H2O + K2SO4 (b) Take a pinch of mixture and Sulphur dioxide is evolved. add 2-3 ml of dilute hydrochloric acid. SO32- confirmed. White precipitate is Pass the gas evolved obtained. through lime water.
  • 13. SNo EXPERIMENT OBSERVATIONS INFERENCE 6. TEST FOR CHLORIDE (Cl-) Pre Test: To a pinch of Greenish yellow gas having May be Cl- . mixture, add 1-2 ml of conc. pungent smell evolves. sulphuric acid. Dense white fumes observed. Bring a glass rod dipped in NaCl + H2SO4 NaHSO4 + ammonium hydroxide near HCl the mouth of the above test HCl + NH4OH NH4Cl + H2O tube. White precipitate formed Con. Test: (a) To the which is soluble in excess of water/soda extract, add dilute ammonium hydroxide. nitric acid and few drops of AgNO3 + NaCl AgCl + silver nitrate. NaNO3 Cl- confirmed. AgCl + 2NH4OH [Ag(NH3)2Cl] (soluble complex) + 2H2O
  • 14. SNO EXPERIMENT OBSERVATIONS INFERENCE (b) Chromyl Chloride Test - Yellow precipitate is formed. Cl- confirmed. Take about 0.2 g of mixture K2Cr2O7 + 4NaCl + 6H2SO4 in a test tube and add about 2CrO2Cl2 0.3 g of solid potassium (chromyl chloride) + 2KHSO4 dichromate and 2 ml of + 4NaHSO4 + 3H2O conc. sulphuric acid. Heat the mixture and pass the gas evolved into a tube CrO2Cl2 + 4NaOH containing sodium Na2CrO4 + 2NaCl + 2H2O hydroxide solution. Add 1 ml of lead acetate solution. Na2CrO4 + Pb(CH3COO)2 PbCrO4 (yellow) + 2CH3COONa
  • 15. SNO EXPERIMENT OBSERVATIONS INFERENCE 7. TEST FOR BROMIDE (Br-) Pre. Test: To a pinch of Reddish brown vapors mixture, add conc. with a pungent smell May be Br-. sulphuric acid. evolved. KBr + H2SO4 KHSO4 + HBr 2HBr + H2SO4 Br2 + SO2 + 2H2O Con Test: (a) Take 0.5 ml of soda/water extract and Yellow precipitate obtained then add 0.5 ml of dilute which is sparingly soluble nitric acid and few drops of in ammonium hydroxide. silver nitrate solution. NaBr + AgNO3 AgBr Br- confirmed. + NaNO3 AgBr + 2NH4OH [Ag(NH3)2]Br + 2H2O
  • 16. SNO EXPERIMENT OBSERVATIONS INFERENCE (b) Take 0.5 ml of soda/water Organic solvent layer Br- confirmed. extract of the mixture and attains orange color due to add 0.5 ml of carbon dissolution of evolved tetrachloride or chloroform bromine in it. followed by 1 ml of conc. NaBr + HNO3 NaNO3 + nitric acid or chlorine HBr water. Warm the mixture and shake the test tube. 2HBr + 2HNO3 Br2 + 2NO2 + 2H2O
  • 17. SNO EXPERIMENT OBSERVATIONS INFERENCE 8. TEST FOR IODIDE (I-) Pre. Test: To a pinch of Violet vapors of iodine May be I-. mixture, add conc sulphuric evolved due to partial acid. decomposition of the formed HI. KI + H2SO4 KHSO4 + HI 2HI + H2SO4 I2 + SO2 + 2H2O Con Test: (a) Take 0.5 ml of soda/water extract and then Yellow precipitate add 0.5 ml of dilute nitric obtained which is acid followed by 0.5 ml of insoluble in ammonium I- confirmed. silver nitrate solution. hydroxide. NaI + AgNO3 AgI + NaNO3
  • 18. SNO EXPERIMENT OBSERVATIONS INFERENCE (b) Take 0.5 ml of soda/water Organic solvent layer I- confirmed. extract of the mixture and attains violet color add 0.5 ml of carbon due to dissolution of tetrachloride or chloroform iodine in it. followed by 1 ml of conc. NaI + HNO3 NaNO3 + Nitric acid or chlorine water. HI Warm the mixture and shake the test tube vigorously. 4HI + O2 2I2 + 2H2O
  • 19. SNO EXPERIMENT OBSERVATIONS INFERENCE 9. TEST FOR NITRATE (NO3-) Pre. Test: To a pinch of Light brown fumes May be NO3- mixture, add conc sulphuric observed which intensify acid. on heating the mixture with copper turnings. NaNO3 + H2SO4 NaHSO4 + HNO3 4HNO3 4NO2 + O2 + 2H2O Con Test: Take around 1 ml A brown black ring at the of soda/water extract and junction of two layers is acidify with dilute sulphuric formed. acid. Add 2-3 ml of freshly NaNO3 + H2SO4 NO3- confirmed. prepared ferrous sulphate NaHSO4 + HNO3 solution and then pour 2HNO3 + 6FeSO4 + 3H2SO4 conc. sulphuric acid slowly in thin stream along the 3Fe2(SO4)3 + 2NO + sides of the test tube. 4H2O FeSO4 + NO FeSO4.NO(brown ring)
  • 20. SNO EXPERIMENT OBSERVATIONS INFERENCE 10. TEST FOR OXALATE (C2O42-) Pre. Test: Add conc Evolved gas burns with a May be C2O42-. sulphuric acid(1-2 ml) to a blue flame. pinch of given mixture(0.1 g) (COONa)2 + H2SO4 and heat the solution. . Na2SO4 + (COOH)2 Bring the mouth of the test (COOH)2 CO + CO2 + H2O tube near the flame. Also pass the gas in the lime water. Lime water turns milky. Con Test: (a) Acidify 1 ml of soda/water extract of the White precipitate obtained. mixture with dilute acetic (COONa)2 + H2SO4 acid and boil the solution. Na2SO4 + (COOH)2 Then add 1 ml of calcium chloride solution and shake (COOH)2 + CaCl2 the test tube. (COO)2Ca + 2HCl
  • 21. SNO EXPERIMENT OBSERVATIONS INFERENCE Dissolve the precipitate in Pink color of potassium C2O42- confirmed. permanganate gets minimum quantity of dilute discharged. sulphuric acid and then add potassium permanganate (COO)2Ca + H2SO4 solution drop wise. (COOH)2 + CaSO4 2KMnO4 + 3H2SO4 + 5(COOH)2 2MnSO4 + K2SO4 + 10CO2 + 8H2O (b) Acidify soda/water extract with dilute acetic acid and Yellow precipitate boil the solution. Add ferrous obtained. sulphate solution. C2O42- confirmed. C2O42- + Fe2+ [Fe(C2O4)]2-
  • 22. SNO EXPERIMENT OBSERVATIONS INFERENCE 11. TEST FOR FLUORIDE (F-) Pre. Test: Take 0.1 g of the Oily droplets are formed May be F- mixture and add 1 ml of along the sides of the test tube. conc. sulphuric acid. 2NaF + H2SO4 Na2SO4 + 2HF Con Test: Add a pinch of White gelatinous deposit sand to the above reaction on the glass rod observed. mixture. Heat it. Bring a F- confirmed. 4NaF + H2SO4 + SiO2 glass rod moistened with water near the mouth of SiF4 + 2Na2SO4 + 2H2O the test tube. 3SiF4 + 4H2O H4SiO4 + 2H2SiF6 (hydrofluorosilicic acid; waxy appearance)
  • 23. SNO EXPERIMENT OBSERVATIONS INFERENCE 12. TEST FOR SULPHATE (SO42-) To the soda/water extract (1 White precipitate obtained SO42- confirmed. ml) add dilute hydrochloric which is insoluble in conc acid (1 ml) so as to remove hydrochloric acid. the carbonate (if present). Na2SO4 + BaCl2 BaSO4 Add 1 ml of barium chloride + 2NaCl solution. 13. TEST FOR PHOSPHATE (PO43-) Take a pinch of the given PO43- confirmed. mixture in a test tube and add Yellow precipitate is about 1 ml of conc nitric acid. obtained. Boil the contents and add excess of ammonium PO43- + 12MoO42- + 24H+ molybdate solution. PMo12O403- + 12H2O
  • 24. SNO EXPERIMENT OBSERVATIONS INFERENCE 14. TEST FOR BORATE (BO33-) In a porcelain dish, take a Green flame is observed. BO33- confirmed. small amount of the mixture, Na3BO3 + 3H2SO4 say 0.2-0.3 g, and add nearly Na2SO4 + 2H3BO3 1 ml of conc sulphuric acid followed by 1 ml of ethyl alcohol. Heat the dish and H3BO3 + C2H5OH bring a burning paper over B(OC2H5)3 + H2O it.