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Prof. Dr. Mona Bedair
Analysis for anions (acid radical) and for cations (basic radical), the two parts of inorganic qualitative analysis, are carried out separately. Either part may be attacked first. Cations are positively charged fragments or ions of salt or compound. radicals. In studying an unknown, a visual examination should come first. If the unknown is a solution, what color is it ? Color is important because some inorganic ions reveal their identities through color alone. If the unknown is a solid, the color is also important, but it does not necessarily indicate the colors of the individual ions. Thus, Pb 2+ and I- are both colorless, but they combine to give the bright yellow PbI2. Identification of cations can not be performed by tests on the original substances (or salts), therefore we have to do some schemes for the systematic separation of cations. Flowcharts are used to represent the steps in qualitative analysis, particularly for the analysis of cations, which is more systematic than the analysis of anions. A flowchart is a schematic outline that begins with the ions in question, indicated the reagents and the conditions for each step, and gives the formulas for the chemical products that result. In considering qualitative analysis and in carrying out the procedures in the laboratory, keeping track of the analytical steps is essential. We recommend that you refer to the flowcharts frequently. Flowcharts can be written in various ways, in which precipitates or undissolved solids are carried to the left and ions in solution are carried to the right. They are frequently referred to as the metals or basic
ANALYTICAL SEPARATION OF CATIONS
Fe+++. Sb+++ Al+++. Mn++. MnS. NH3 in presence of NH4Cl IIIB (Zinc group) H2S in presence of aq. Mn3+ Ni++. Fe(OH)3 Mn(OH)3 NiS. for purposes of qualitative analysis. Bi2S3. a precipitate is obtained consisting of the chlorides of silver. Pb++. into a number of groups. forms H2S in presence of dilute HCl Aq. NH4+ Formula of Precipitate AgCl. Thus by the addition of a slight excess of dilute hydrochloric acid to a solution containing all the common carions. Cd++. Group I (Silver group) II (Copper and arsenic groups) IIIA (Iron group) Group Reagent Dilute HCl ions Ag+. Bi+++. As2S3. sulphides. Hg2Cl2 HgS. CdS. the members of any group are precipitated by a particular group reagent. the remaining cations are separated into different groups. K+. hydroxides and carbonates. Co++. similarly by the use of the appropriate group reagents. Sn++ As+++ . NH3 and NH4Cl IV (NH4)2CO3 in (Calcium group) presence of aq. ZnS BaCO3. The various groups are summarised in the following Table. PbCl2. NH3 and NH4Cl V (Alkali group) No particular reagent 4 . Na+. SnS. Pb++. CoS. PbS. Sb2S3 Al(OH)3. Hg2++ Hg++. Zn++ Ba++. Cu++. CuS. CaCO3 different ppted. Sr++. lead and mercurous. analytical separation of cations depends on the varying solubilities of their chlorides.Common cations (basic radical) may be divided. Cr+++. Generally. Cr(OH)3. Ca++ Mg++. SrCO3.
Mn2+. CuS. Ni . NH4+ Cold. Cd . Zn2+. Mg2+. dil HCl Residue Hg2Cl2. Co . Sb2S3 Al3+. Ca2+. NH4+ GroupV Mg2. Ni2+. Cd2+. Cr3+. Mg2+.Ag+. K+. Cr3+. Al3+.3 M HCl Bi2S3. HgS. As3+. Pb2+. PbCl2. Fe2+. NH4+ H2S/NH4Cl/NH4OH Centrifugate Co2-. MnS (NH4)2CO3/NH4Cl/NH4OH Group IIIB Residue Centrifugate CaCO3. Sr2+. As3+. Ba2+. NH4+ As2S3. Cr3+. Ba2+. K+. NH4+ Group I Residue Centrifugate H2S/0. Group IIIA Residue Centrifugate CoS. Fe3+. Ca2+. Mg2+. BaCO3. Sn . Bi3+. Sr2+. Mn2+. Ba . Mg2+. Na+. Flowchart for separation of cations into groups 5 . ZnS. Ni2+. Cu2+. Cu . CdS. Zn . Sr2+. Fe(OH)3. Bi . SrCO3 Group IV + K + Na+. Sb3+. Ca . Sn2+. Hg2+. Ni2+. Hg22+. Na+. Ba2+. Co2+. Zn2+. Sr2+. NiS. Mn2+. K+. Sb . Al3+. Fe3+. Mn(OH)3 Ca2+. Cr(OH)3. Zn2+. AgCl 22+ 2+ 2+ 2+ 2+ 3+ 2+ 3+ 2+ 2+ Centrifugate Hg . PbS. Na+. K+. SnS NH4Cl/NH4OH Group II Residue Al(OH)3. Co2+. Na+.
e: (decrease the solubility of the chloride precipitates of group I) Example : AgCl AgCl soluble HCl moderate excess Ag+ + Cl - H+ + Cl c. (2) 6M cold hyrochloric acid Use of a moderate excess of hydrochloric acid to precipitate the group serves two purposes : (1) The excess chloride ion encourages the precipitation of group I (Le Chatelier’s principle) by the common ion effect of the Cl i. The group reagent is cold.Cation Group I Silver Group Mercurous Hg22+ Lead Pb2+ Silver Ag+ Cations Group I brings together three metal ions that form chlorides which are insoluble in acidic solution.e. 7 . dilute hydrochloric acid.i. Condition of precipitation (1) Cold hydrochloride acid is used to prevent the solubility of PbCl2 in hot solution. or the silver group. The chlorides of all the other cations in our cation analysis scheme are soluble in acidic solution. the chloride group. and this group is sometimes known as the hydrochloric acid group.
Sb3+) by the common ion effect of the H+. if the unknown contains Cd 2+ and Sn4+ (from the subsequent groups).i. Cd2+ + Clor Sn4+ + Cl- [CdCl4]2[SnCl6]2 8 .e.+ H2O Sb3+ + Cl. Bi3+ + Cl. Too large excess of the acid is avoided : (1) Dissolves the silver and lead chlorides by complex formation. Mercury (I) chloride does not dissolve because the chloro complexes of mercury (I) are very unstable.e. Example : AgCl + ClLarge excess [AgCl2]Silver dichloride soluble complex [PbCl3]or [PbCl4]2Lead trichloride Lead tetrachloride soluble complexes PbCl2 + ClLarge excess (2) Also. if the unknown contains Bi 3+ or Sb3+(from the subsequent group) the hydrogen ion prevents precipitation of them as oxychlorides. i.(2) Also.+ H2O HCl moderate excess BiOCl + 2H+ SbOCl + 2H+ Cl+ H+ c. the high chloride concentration forms stable soluble complexes with them and inhibits the precipitation of CdS and SnS2 by H2S/H+. Solubility of BiOCl or SbOCl if these cations are present with group I cations (Bi3+.
KI HNO3 until acidic (Procedure 5) AgCl white Pb2+ present Hg22+ present Ag+ present Flowchart for Analysis of Cation Group I 9 . Otherwise save for Cation Group II) Centrifugate PbCl2 Divide into 3 portions (Procedure 3) (Procedure 1) Residue Hg + HgNH2Cl black white Centrifugate [Ag(NH3)2]++Cl- H2SO4 Cool K2CrO4 PbSO4 PbCl2 PbCrO4 white white yellow Dissolve in aqua regia Evaporate. AgCl all white ppt H2O. Ag+ Cold 6M HCl Residue Hg2Cl2.Separation of Cation group I Hg22+. discard. test with 1. NH4OH (procedure 4) Centrifugate (If only Cation Group I present. Pb2+. AgCl Conc.SnCl2 2. PbCl2. boil (Procedure 2) Residue Hg2Cl2.
Procedure 1: The solubility product of the precipitates of group I cations are PbCl2 AgCl Hg2Cl2 Ksp Ksp Ksp 1.AgCl + xss HCl [AgCl2].+ K+ silver dicyanide 3. Silver (I) ion (Ag+) Reactions Important in the Separation and Identification of Ag+ Group Precipitation Ag+ + ClAgCl white Dissolution by Complex Ion Formation 1.+ H+ silver dichloride 10 .AgCl + 2KCN [Ag(CN)2].AgCl + 2NH3 (aq) [Ag(NH3)2]+ + Clsilver diammine 2.6 x 10-5 1.1 x 10-10 3.0 x 10-18 Solubility product constants indicate that lead (II) chloride is much more soluble than the chlorides of mercury (I) or silver (I).
Ag+ + NaOH Ag2O black Ag2O + excess NaOH insoluble (non amphoteric) Lead(II) ion (Pb2+) Its oxide is amphoteric (dissolves in both acid and alkali) Reactions Important in the Separation and Identification of Lead (Pb2+) group Precipitation cold Pb 2+ + 2Cl - PbCl2 PbS in group I in group IIA Pb2+ + S2-/H+ Dissolution By oxidation of sulphide PbS + HNO3 Pb2+ + So + NO + H2O Reaction with sodium hydroxide Pb+2 + NaOH Pb(OH)2 [HPbO2].or [Pb(OH)3]- Pb(OH)2 + excess NaOH Reaction with ammonium hydroxide Produces white basic salts (ppt) which is insoluble in excess NH4OH 11 .Reaction with NaOH Produces black precipitate insoluble in excess NaOH.
PbCrO4 + HNO3 PbCr2O7 + H2O lead dichromate (soluble) Also if we use strong alkaline medium. As if we use strong acidic medium (mineral acids) as dil HNO 3.Pb2+ + CrO42- PbCrO4 yellow The reaction of Pb2+ with chromate gives yellow precipitate in weakly acidic medium (dil acetic acid).Pb2+ + KI PbI2 yellow lead iodide PbI2 + excess KI (PbI4)2soluble complex lead tetraiodide 12 . the yellow precipitate of PbCrO4 will dissolve (amphoteric character) 3.Pb2+ + SO42PbSO4 white CH3COOH 2. it will dissolve the yellow precipitate of PbCrO4 and transform it to soluble dichromate salt.PbCl2 + NH4OH Pb(OH) Cl Lead hydroxychloride white basic salt Confirmatory Tests 1.
The Hg22+ ion is found in a number of solid compounds. The loss of one electron by a mercury atom gives a mercurous ion (Hg22+) which is unique among ions in that it has a single (6s) electron in its outermost orbit. Each mercury atom has two (6s). Two of these ions combine to form the ion (+Hg:Hg+) or simply Hg22+. Therefore precipitation reactions involving mercurous ion are complicated by disproportionation reactions yielding elemental mercury and mercuric compounds. its existence is limited to the pH region below about 3 to 4. Example : Hg2Cl2 + 2NH3 HgNH2Cl + Hgo + Clwhite black mercuric mercury amino chloride metal 13 . The loss of two electrons by a mercury atom produces the mercuric ion (Hg2+). Hg22+ Mercuric (II) ion. in which the two mercury atoms are bonded together by a pair of shared electrons (a covalent metal-metal bond).Mercurous (I) ion. In aqueous solutions. a disproportionation reaction with water or hydroxide ion takes place: H2O Hg22+ Hgo + Hg2+ mercury mercuric ion metal This also may called self oxidation-reduction reaction. Hg2+ The mercurous ion is precipitated as chloride in the silver group. the mercuric ion is precipitated as sulphide in the copper-arsenic group. At higher pH values.
Reactions Important in the Separation and Identification of Mercurous (Hg22+) Group Precipitation Hg22+ + 2ClHg2Cl2 white mercurous chloride Complex formation Hg22+ + 4CNHgo + [Hg(CN)4]2mercuric tetracyanide Hgo + [HgI4]2mercuric tetraiodide Hg22+ + 4I- Reaction With NaOH (non amphoteric) Hg22+ + 2OHHgo + HgO + H2O mercury yellow metal mercuric oxide Confirmatory Test Hg2Cl2 + 2NH4OH Hgo + Hg(NH2)Cl + NH4+ Clblack white mercury mercuric metal amino chloride Reactions Important in the Separation and Identification of Mercuric (Hg2+) 14 .
Aqua regia (1:3) Conc.With ammonium hydroxide NH4OH HgCl2 + 2NH4OH HgNH2Cl + NH4+ + Clwhite 2. but dissolves in hot aqua regia with the formation of a chloro complex. HNO3 : Conc. black stannic hexachloride 15 .and complex ion formation with mercuric boil 3HgS + 8H + 12Cl + 2NO3 3[HgCl4]2. Group Precipitation H+ Hg2+ + H2S HgS + 2H+ black mercuric sulphide Dissolution by : 1.Mercury(II) sulfide (group II) is the least soluble sulfide.Hypochlorite reagent HgS + NaOCl [HgCl4]2. It is not soluble in either dilute nitric acid or hydrochloric acid.With stannous chloride reagent SnCl2 HgCl2 + SnCl2 Hg2Cl2 + [SnCl6]2white mercurous stannic hexachloride chloride Hg2Cl2 + SnCl2 Hgo + [SnCl6]2xss.+ 4H2O + 3So + 2NO ___________________ aqua regia slightly ionized + - 2. HCl Oxidation of S2.+ SO2 Confirmatory Tests 1.
How can you separate and identify mixture of Hg22+ / Hg2+ ?? 16 .mercury metal It is an oxidation-reduction reaction.With potassium iodide HgCl2 + KI HgI2 scarlet red [HgI4]2mercuric tetraiodide soluble complex HgI2 + KI xss Differentiate between mercuric and mercurous. 3.
. Sb5+ Sn4+ 17 .CATION GROUP II COPPER-ARSENIC GROUP Group IIA : Mercury Bismuth Copper Cadmium Lead Hg2+ Bi3+ Cu2+ Cd2+ Pb2+ Group IIB : Arsenic Antimony Tin As3+ Sb3+ Sn2+ . As5+ .
for a saturated solution of H2S. therefore. decreases the dissociation of H 2S in H2O and hence decreases the sulphide ion concentration. antimony and tin. copper and lead.This analytical group of cations is composed of eight cations which are subdivided into the copper group consisting of mercuric.1 or [H+]2+ [S2-] = constant H2S HCl 2H+ + S2H+ + Clc. cadmium.1 M. shift the equilibrium to the left. [H+]2 [S2-] Ka = _____________________ = 1. 18 . and the arsenic group consisting of arsenic. The group reagent (precipitating agent) of cation group II is hydrogen sulphide in acid medium (0. [H+]2 [S2-] Ka = _____________________ 0. H2S 2H+ + S2H2S + CH3COONH4 The real significance of the [H+] as a control of [S2-] can be seen by examining the ionization of H2S. it is hydrolysed in acid solution to give hydrogen sulphide CH3CSNH2 + 2H2O thioacetamide.i.e. bismuth. increasing the concentration of H+ ions in solution of H2S in water.3 x 10-20 [H2S] A saturated solution of H2S is approximately 0. Thioacetamide may also be used. According to the theory of common ion effect. the expression may be simplified to.3 M HCl).
b) Dissolution of sulphides of group IIB as thioanions (see group IIB). PbS. A decrease in [S2-] by increasing the acidity (> 0.Adjustment of the acidity An increase in [S2-] by decreasing the acidity (< 0. [SbCl4]-. 19 . SnS 2 (have higher solubility products). b) Formation of stable soluble complexes as [CdCl4]2-. [SnCl62-].3 M HCl) results in : a) Precipitation of sulphides of group IIIB.3 M HCl) results in : a) Prevention of the precipitation of CdS. so they can not precipitate by addition of H2S.
N. therefore. The subdivision is based on the differences in the electronegativity values. Thus. 20 . the members of the arsenic group are sufficiently electronegative to dissolve in alkali sulphides giving thioanions. : The electronegativity and the acidity increases by increasing the oxidation number. insoluble in alkali sulphides or alkali hydroxides.Subdivision Of Cation Group II into IIA and IIB Cation group II contains eight elements. the members of the copper group have low electronegativity values and are. On the other hand.B. this large number is too difficult to analyse satisfactorily unless it is subdivided into two subgroups: group IIA (copper group) and IIB (aresnic group). and in alkali hydroxides giving both thioanions and oxyanions (amphoteric sulphides).
Cation group II 1) Biol with H2O2 and expel the excess 2) Adjustment of the acidity 3) Add H2S or thioacetamide Residue Suphides ppt of group II NaOH Na2S or Residue ppt of sulphides of subgroup IIA Centrifugate soluble complexes of subgroup IIB (continue as scheme for subgroup IIB separation) Flowchart for separation of cation group II to subgroup IIA and II B 21 .
B. The stannic (Sn 4+) has higher oxidation number and higher electronegativity). to separate stannous with the subgroup IIB cation sulphides. Therefore. we have to oxidize stannous to stannic (Sn4+) by boiling with hydrogen peroxide. docompose 2H2O2 2H2O + O2 xss strong boiling H2O2 + H2S So + 2H2O colloidal sulphur 22 . otherwise it will oxidize the H2S reagent to colloidal sulphur which is difficult to separate. : Stannous sulphide is not amphoteric so. HCl Sn2+ + H2O2 Sn4+ + H2O The excess H2O2 must be decomposed by boiling.N. it is incompletely soluble in either NaOH or Na2S.
Cd2+ . Cd2+ . Cu2+ white dissolve in ammonium Conc.xss H2O 2.KI Residue Centrifugate [Cd(NH3)4]2+ colourless [Cu(NH3)4]2+ blue Test fo Cd2+ in presence of Cu2+ KCN + H2S Bi(OH)3 white gelatinous dissolve in HCl Test for Bi3+ 1. CdS brown ppt yellow ppt heat with 1:1 HNO3 Residue HgS .Copper Subgroup (Cation Group IIA) Hg2+ . HgO dissolve in aqua regia or hypochlorite Test for Hg2+ 1) SnCl2 2) NH4OH 3) KI Centrifugate Bi3+ . PbS. Cu2+. CuS . Cu2+ . NH4OH acetate Test for Pb2+ 1. Cd2+ .Sodium stannite Test for Cu2+ in presence of Cd2+ 1) Acetic acid + ferrocyanide 2) KI Flowchart for analysis of cation group IIA 23 .3 M [H+] 2) add H2S HgS . black ppt Bi2S3 . Pb2+ 1) adjustment of the acidity at 0. Pb2+ ethanol.acetic acid + K2CrO4 2. Bi3+ . H2SO4 Residue Centrifugate PbSO4 Bi3+ .
Bi3+ + Conc.Oxysalt formation Addition of large excess water will give white turbidity soluble in excess acid by common ion effect of the H+. NH4OH Bismuth is separated from Cu2+ and Cd2+ by precipitation with Conc.Reaction with conc.Mercuric (II) ion (Hg2+) Previously discussed with cation group I Bismuth (III) ion (Bi3+) Reactions Important in the Separation and Identification of Bismuth (Bi3+) Group reagent 0. NH4OH Bi(OH)3 + NH4 white gelatinous We dissolve this precipitate in HCl Bi (OH)3 + HCl BiCl3 + H2O Test for bismuth by two tests : 2. NH4OH.3 M Bi3+ + H2S [H+] Bi2S3 + H+ dark brown Dissolution By oxidation of sulphide BiS3 + HNO3 Bi3+ + So + NO + H2O Confirmatory Test 1. 24 . The precipitate is insoluble in excess of the reagent (no ammine complex).
SnCl2 + 2NaOH Sn(OH)2 Stannous hydroxide [HSnO2]. the sodium stannite reagent under goes self oxidation-reduction and black precipitate of tin is formed by time Sno + [Sn(OH)6]2autoxidation black Reaction with NaOH. N. : Sodium stannite reagent must be freshly prepared.B.or [Sn(OH)4]2stannite Sn(OH)2 + xss NaOH On standing (by time). the bismuth hydroxide is formed which is 2[Sn(OH)4] 2- insoluble in excess NaOH (not amphoteric) Bi3+ + NaOH Bi(OH)3 xss NaOH insoluble 25 .BiCl3 + H2O soluble large excess BiOCl + HCl or HNO3 3.Sodium Stannite Test Bi3+ + [HSnO2]stannite reagent BiOCl + 2H+ white turbidity bismuth oxychloride BiCl3 + 2H+ soluble Bio + black bismuth metal [Sn(OH)6]2stannic hexahydroxide soluble complex This is an oxidation-reduction reaction where the bismuth ion is reduced to metallic bismuth (black precipitate) and the stannous ion is oxidized to stannic.
Cu2+ + KI [Cu(NH3)4]2+ deep . KCN is called masking reagent Confirmatory Tests 1.Cu2+ + 4NH4OH 2.blue colour Cu2 I2 + I2 white cuprous iodide brown solution 26 .Copper (II) ion (Cu2+) Reaction Important in the Separation and Identification of Copper (Cu2+) Group Precipitation 0.3 M Cu 2+ + H2S [H+] CuS + 2H+ black Dissolution : By oxidation of sulpide reaction CuS + dil HNO3 Cu2+ + 2NO + H2O + So Complex formation reaction * with NH4OH Cu2+ + 4NH4OH [Cu(NH3)4]2+ + 4H2O blue copper tetramine (soluble complex) * with KCN Cu2+ + KCN [Cu(CN)4]3cuprocyanide complex (tetracyanocuprous complex) stable complex.
Cu 2+ + [Fe(CN)6] 4- Cu2 [Fe(CN)6] choclate N.B. Cd2+ Reaction Important in the Separation and Identification of Cadium (Cd2+) Group precipitation and Confirmatory Test 0.3 M Cd2+ + H2S [H ] + CdS cadmium sulphide yellow Dissolution : By Oxidation of sulphide CdS + dil HNO3 27 Cd2+ + NO + H2O + So . ion. : To carry out the test with ferrocyanide on the soluble copper ammine complex we have to acidify first with dil acetic acid (until the blue colour disappear) to decompose the copper complex. and liberate the free Copper ion in the medium [Cu(NH)42+] + dil 4CH3COOH Reaction with NaOH xss NaOH Cu2+ + CH3COONH4 insoluble (not amphoteric) Cu2+ + NaOH Cu(OH)2 blue CuO black Cadmium II.HAC 3.
HCl Cd2+ + Conc. CuS ? 28 . : How can you separate and identify a mixture of CdS. Complex Formation * with NH4OH Cd2+ + 4NH4OH [Cd(NH3)4]2+ cadium tetramine complex * with Conc.B. HCl * with KCN (masking agent) Cd2+ + 4KCN [Cd(CN)4]2cadium tetracyanide unstable complex [CdCl4]2- N.
Sb3+ . Arsenic . Sn2+ Arsenious. These precipitates are soluble in NaOH (separation of subgroups IIA & IIB) (or Na2S) producing a mixture of thio. Antimonous . AS2S3 yellow ppt AS2S5 Sb2S3 orange ppt Sb2S5 SnS2 brown ppt Because of their high electronegativities.and oxysalts (centrifugate in the separation of subgroup cation precipitate of IIA & IIB). Sb5+ . Antimonic . and tin As3+ . As5+ . antimony. the acidity is adjusted at 0. 29 . their sulphides (except SnS) are amphoteric. Stannous When group II is boiled with H2O2.Arsenic Subgroup Cation Group IIB The elements of this group are arsenic.3 M HCl and H2S or thioacetamide is added. the following amphoteric sulphide precipitates of subgroup IIB are formed.
.add H2S or thioacetamide Residue As2S3 ..Magnesia mixture reagent. (4) add HgCl2 Test for Sb3+ in presence Sn4+ 1..acidification with acetic acid . Sb2S5 orange ppt SnS2 brown ppt Contrifugal discard heat with 1:1 HCl (12 M) Just before boiling ... Sn+4 1....boil with Conc. As2S5 yellow ppt Sb2S3 .acetic acid and solid sodium thiosulphate 3... 2.. SnCl4 Alkalinize with NH4OH Flowchart for analysis of cation group IIB 30 ... HCl and iron wire .. Sb+3. HNO3 . 3.Battendroff reagent Test for Sn4+ in presence of Sb3+ . (5) 2...Ammonum molybdate reagent. (2) Residue As2S3 As2S5 heat to dissolve in Conc.Group IIB Cations As+3.oxalic acid and H2S . (1) 2.excess H2O Contrifugate SbCl3. (3) Test for arsenic 1.
HNO3 As2S5 + Conc.Arsenious (III) ion and Arsenic (V) ion. A filter paper moistend with AgNO3 is exposed to the arsine gas produced from the previous reaction.Gutziet Test The arsenic sulphide is dissolved by Conc. H3AsO4 + Zno / H+ AsH3 + Zn2+ arsine gas Ago + H3AsO3 black 31 AsH3 + AgNO3 . HNO3 As2S3 + Conc. As5+ Group precipitation H+ 2As3+ + 3H2S 2As5+ + 5H2S H+ As2S5 + 6H+ As2S5 + 10H+ yellow } Dissolution oxidation by Conc. HNO3 H3AsO4 arsenic acid Separation and Confirmatory Tests 1. As5+ Reactions Important in the Separation and Identification of As3+. As3+. Blackening to the filter paper occurs. HNO 3 and treated with zinc dust in acid medium (strong reducing agent).
Battendroff Test The stannous chloride in conc. HCl It is an oxidation-reduciton reaction. NH4Cl. HCl. Aso + SnCl62. Sb5+ Group precipitation H+ 2Sb3+ + 3H2S H+ 2Sb5+ + 3H2S Sb2S5 + 10H+ orange Sb2S3 + 6H+ Separation and Confirmatory Test 1. MgCl2) H3AsO4 + NH4+ + Mg2+ MgNH4AsO4 white crystalline ppt magnesium ammonium arsenate 3. reduces arsenic salts to metallic arsenic H3AsO4 + SnCl2 + C. Sb5+) Reaction Important in the Separation and Identification of Sb3+.Magnesia mixture Test Mixture of (NH4OH.Oxysalt formation SbCl3 + H2O large excess SbOCl + H+ white turbidity antimony oxychloride basic salt This reaction is reversed by adding HCl 32 .2.+ H2O Antimonous (III) ion and Antimonic (V) ion (Sb3+.
But the Sn 4+ interferes and give the brown ppt of SnS 2. so on passing H2S.Iron wire Test H+ Sbo + 3Fe2+ black deposit Oxidation-reduction reaction Sb3+ + 3Feo 3. orange ppt of Sb2S5 is formed. 33 . we add oxalic acid which forms two complexes with Sb 3+ and Sn4+. while that with Sb3+ is unstable. COOSn4+ + COO[Sn(C2O4)3]2stable COOSb3+ + COOoxalate [Sb(C2O4)3]3unstable + H2S Sb2S3 orange Oxalic acid is called masking agent. To get rid of this interference.SbOCl + HCl or HNO3 (common ion effect of H+) SbCl3 + H2O soluble 2.Test for Sb3+ in presence of Sn4+ Here we test for Sb3+ by H2S to give orange ppt. The complex with Sn4+ is stable.
Stannic (IV) Ion (Sn2+.Sn4+) Reaction Important in the Separation and Identification of Sn2+. The test may give white ppt (Hg 2Cl2) or grey ppt (Hg2Cl2 + Hgo) or finally black ppt (Hgo) (oxidation-reduction reaction). Then HgCl2 oxidizes Sn2+ to Sn4+ and being reduced according to the amount of HgCl2 used. Sn4+ Group precipitation Sn2+ + H2O2 + 2H+ + H+ Sn4+ + H2S SnS2 brown Sn4+ + 2H2O Separation and Confirmatory Test 1. Sn4+ + Feo + H+ (iron wire/H+) Sn2+ + HgCl2 Sn2+ + Fe2+ white Hg2Cl2 + [SnCl6]2white Hgo + [SnCl6]2black Hg2Cl2 + xss SnCl2 4.Test for stannic in presence of Sb3+ We have to boil with iron wire (Feo) in acid medium for two reasons: H+ Sb3+ + 3Feo + H+ Sn4+ + 2Feo Sn2+ 2Fe2+ 34 Sbo 3Fe2+ removed by filtration .Stannous II ion.Mercuric chloride test We have to reduce the Sn4+ to Sn2+ using iron wire in acid medium.
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