it in OF ic ae tional Groups Present in Organic Compounds ri re jrtle of the of alkaline sO rization of pink given organic compound in about 2 ml of water or acetone in a test tube. Add jution of KMnO, (1%) and shake the mixture. " ; colour of KMnO, indicates unsaturation. 0 a0 ‘OF REAGENTS | da 2 ml of liquid bromine in 100 ml of distilled water and shake, Decant off the clear | romaine wate fig promi jine KI anhydrous Na, ge in CCl, Shake 2 mil of liquid bromine in 100 ml of CCl, and stopper the bottle. MnO, (1%). Dissolve 1 g of KMnO, (solid) in 100 ml of distilled water. Now add 10 g of | CO, Shake to dissolve and stopper the bottle. | | ALCOHO! Ls unde in which the hydroxyl group (—OH) is linked to aliphatic carbon chain or in the side chain of an Pm pmpourd are called alcobols. The alcohols containing one, two or three hydroxyl groups per Je are called mono, di or trihydric alcohols respectively. Alcohols are further classified as primary (1°), secondary (2°) and tertiary (3°) according as _OH group is attached to primary, secondary or tertiary carbon atoms respectively. Ss ec cH. cH, ie CH,CH,OH exon cH,—C—OH Ethyl alcohol cH, | Primary) iso-Propyl alcohol CH, (Secondary) tert-Butyl alcohol (Tertiary) . | TESTS FOR THE ALCOHOLIC [R—OH] GROUP . | ao EHronsl | alcoholic group can be detected by any of the following tests: 1. Sodium metal test. 4 2. Ester test. WD 3. Ceric ammonium nitrate test’ 4 lodoform test for alcohols containing the CHF group OH SODIUM METAL TEST iste is based on the appearance of effervescence due to liberation of hydrogen gas when the alcohol Teacted with active metals like sodium. 2R—OH + 2Na—> 2R—O-Na* + H, t Alcohol Sodium alkoxide 2CH,OH + 2Na—> 2CH,—O'Na’ + HT Methanol Sodium methoxidePee opo1jo 144 moqe'y 2uporpue von A 10S apPxoxpAy urnypos yaw pauszem st punodwso> |. FOP at i a tat eau pe “apdgapreiane dq uani8 13801 1S31 WUOS soyé0> pats03quig Fo HNZ + ["FON)?0“HO'HO)] —*Fon)20"'HN) + HO—"H22 syduo> nen aoe peso yu uunwowure 7199 (HOY ‘ONHNG + ('CON)20°(HOW] —*CoN)*O"CHN) + HOWE dou syoyonye uo Jo vouasou aya soavoypuanoqe> pou zo undo 27uns02day 4S 0 jem ayeys pur auatees 97220 saw ua jo sdoup m2} © ppe ‘2qna-3sa Aap weap © ut Puno? uwani8 ayp 30 [MT a ‘sa 31VULIN WNINOWWY 21839 yooqo uv Jo aruaszud a4) 5922710 ous &amafy jus pe sag ew way 20286 P0730 _anoge oyu 3} nog “saynUTU QT INOgE 20 vung sazen e uo ama 249 EA ppe unydmns 2407 sip ¢-z pue pre a7are [eP>e[B JO TH T PPE ‘2d san Aap weap © ut prby wasid 2p JO [Ht T EL aunpa2did oy eee -dnoaB 2901 aners2e (NO o'n + HO—-0-—"H = ar HD + HOH \ a! sa8 poesnixogrey (OGY { OH + Y-O-I—A = Hope + HOT’ i H i i ) pe sums 2409 sons PPE we KG, passqere>) ox8 proe 2yjdxoques e pue dno’ / orooyuaase pare 51 a coqie? Wp 39eat STOYOTY Pe onzead eanpeayaqsioaax pe os © st aL "fe ue uaamaaq uorieas ayy, “#19189 BUTS yaams 140} 02 SPP" 7H isa yas 's200N uum aya 01 joyorz 210m PY W428 si uafioupty 91007 fe yaa 249 03 anp 22ua2saasa4J9 4s14q poyooyo uv saaw24puy 995 eer i ous: sate evous warupos jo aoard jews & ppe pur jem aaoutas 0} [jam axeys pure areydqas aind uaaid atp yo yw | anoge aye eunpercig ‘Sty “Suey posjzoid err?saony uo qu stad SEU ' un suvaddo ssouipnop jp al jouoore Axemnpsd ou pawoipu oa ‘527M oypur st ouoate A2¥P™ yoqoore Aawpaes 2 ssaunpnop Jo? pue aqna 3589 A5P wear: pe awnpu rer seadde otf UMOP AION am a a p © ut foUOTE AAP JO [HIT anoge yy) Svar sen] JO sdosp 01-8 PPE | ®1nparoig | (01 — HO'HO'HO | an ogorre ang? HOH — "Ho—"HO—H2—" HO DH De | HO quote ang 121 rego wana? ‘ p2—H —a HO—)—HO | DH DE ] "HD "HO corns ayp ur ssourpnop usar ayqnqosu! Bug tPrHM PPS tdoranjos zea # os ‘quoBeax sean ur 2pqnyos 278 PH ‘are sepuop [ype ‘uonDeax UO “PUFERQO St yn yuaBear Seow yal paveana st [Oyo ag 8H SRE Me 17 pue [DH Jo ammaxtu refounmba st Un [puz Jo aouasard amp Ul [DH Spry sjoyooye snouea jo sararyzeax anrejex wodn pased St sath isai svoM {STOHOOTV AUVILUAL UNV ‘AUVGNODAS ‘AUVWTYd NFIMLAT NOILNILSIC -auoray ape? uopoulsod 0yorqe hupau-r28 jounyya ‘jounyz2 saqu>%put uirofopo} Jo ayvz1d12a4d mop]a4 JO cqreq zayen & uo AB 0s aR os we ppe ont 7 “ ye oro un aq aun asiudoxp uormnjos aprxoxpay qe ppe pue aqn say Aap weap e ut punoduso> uaa amp J | aun paBrewpsip auoued « HOEND + ‘Ie + HOD HD « HO HOENZ + {1 8 ab spunodwuos » sf 1109 2100619 uy juasaig sdnosg DUO!I2u" analuornfos apLioyy> 12295 yAIM 39eaA | #spunoduro> 2140830 Jo sadéa xatp0 Auepy saxa[duio> posnojo> wi103 03 stot 21219) Yate I>eOI STOUDYA 4S31 JOINOTHD DIwya4 “@euogze> wntpos Jo uoRNIos snoanbe yal aouaDsani9y9 ue fons se Jou st jouayd se ang asox srip anid oste spIre syXxoqiey -a20Ny “quasaad aq Aowi drow yjouayd ‘pos ‘0 pmby waar ayz 30 doup & areyg ) eunpacoig 4s31 SAWLNt “3802 s,uupuuogar] -¢ “3893 apuoyy> ouusoq a 3892 snuuaty ~~ * ‘sisea Buwmorios axa Aq parsarap aq ue> dnow® syousdd oy, sfunyp noqo> aya Jy saded snuny anqq stows uo pryos 31 peaskao © x = 4N0ud [HO—*V] STIONaHa 4Od SISAL Tounrosay jowparea, Josa39-1 HO, “HD HO HO HO TOYOrTe Ur Aampqnjos ajqeioardde aavy ang 193em ApyBys Aype19uU98 yng aind uy sso} Pur 29qu1m ur pijos & st HO' HD jouayg “pin "21 pur Joypaye: ']0Saa2-d pur wu ‘o :aae sajdurexa raya 'joursyd asayci 7 He Buu snewore uv o3 paxpene sdno:s |4xoapAy 9101 10 U0 3 lousy doy 1 UL uo “teu praee Me 24 2Np pasnojo> TW Yoursros, “id pao_———sS—s yo ue ut ayn tage 40} 2401591 2H PDH Fog, yd jo3 10 PU PUMOdutOD 21498; oe oy 81 4s31 340 New My puss (uo P40 PLYP 2 ay, and 304 oud PPIMNSANS A PLO U4, : my eauon2ear agp nod pur (00) HPA rane aso} Aap ueap apne HE sdosp 7-1 PPEPU ssivadde mojo> ua918 10 anyq ayy 'ORN|OS aprxoxpAy wintpos 40 $882x9 Ue ppp, sung Moyo? dup ‘ATpnyaze> 427M PPY ‘sdojanap wo1aB4no]0? uaadd daap 40 an) 420p Y'S14U09 99 oy agen aya ayes pue pre sunydns “209 Jo [wT Noa ppe wa] 1909 03 1 MOTTE PUP Anu ep " ‘qua Axon 9} 1ouaydyo# T mogeppe pu agra sey AP UEP ‘ul yA UIMIPOS Jo sTeShay > om aunporey Noy (oma) wore jousdopet par Oem me OO (pan owudops I o(-{O)-#0 — wo) +Ho4(_ ) No youaydosonny- rousug w0-(C)-»0 ona ©) pp On ante apes Sosten + “ONHZ “——"os"H + “ONENZ 1 symydgns “2409 ut paappss Pe Suons yo wortppe ayy Aq ua9s8 20 anjq oy sa¥urey> sm0f0> BU], "PHE 3803 sp ani sjouad a8 scx pape ssi Uap pannpoid sf UMeNO}> W019 10 PR asa s.NNWWa382"* cmap TTR! sundoxp wre pa 202) a0 PPE MON sree en aeons sone at ¥ woe POND 28) TJ 2d PON 28H ATS PEE punoduio> pil wuonound 24 8 spunodwo> 2140610 u) yuasarg sdno49 12Comprehensive Practical Chem 86 emistry hte sodium hydroxide solution. Appearance of 5 d ws nolic —OH group in the com, Pin, Poung y beaker containing 15 carefully into a she pravence ore blue, green, red etc. colours indicates AND KETONES 9.04. ALDEHYDES 6 chydes and ketones a! my arbonyl gr —C—. This ompounds that contain Uy P. . : : j " £ compounds. In aldehydes, the cay UP ha Yl Bro aracteristi nerties which are shown by both classes 0 properties which are s ; 7 , “2 « rogen atom and to an aliphatic or aromatic radical. Formaldehyde is Bro, js attached to a hydrogen atom 4 Ee eee ere eroup ts atta ied to, uo nye 0 oO 1 i cH da C,H,—C—H ee Acetaldehyde Benzaldehyde In ketones, the carbonyl group is attached to two aliphatic or aromatic radicals. 9 i i CH. I CH. cH,—C —C—CH. —C— CHy CCH, He enone a “Benzophenone — ‘The carbonyl group in aldehydes and ketones is identified by the following tests: 1. 2, 4-dinitrophenyl hydrazine test. Sodium bisulphite test. The major difference between an aldehyde and a ketone is that an aldehyde is readily oxidized ty carboxylic acid whereas ketones cannot be oxidized easily. This difference forms the basis of the test for distinguishing aldehydes and ketones. They are generally distinguished by the following tests; Schiff’s test 2. Fehling’s test 5. Silver mirror test. ee TESTS FOR ALDEHYDIC AND KETONIC | [—CHO and —CO—] GROUPS _"; Oo oO hon na 2, A waat8 axp Jo (8 S'0 40) [Ur S'0 PP [ASIp Jo [ur T mnoge ut aprssnadonru umrpos Jo TersAs> & aAIOSSIT aunpa20id | ~ twonesnojo> Pax oy apsssesdonnin -¢l"HOOD°HO ‘ONS(ND)2a] ——-"HOOI"HD + -c[ON*(NO)?d] ) 0°H + 7HO00°HO <——-HO + *H900°HO ‘uot pamnojo> ui10} 03 wor apissnadosaru yaim s>eax TEE we Aq pausz03 auor2y ax Jo UOIUE aut S41 3ISSNYdOBLIN WNIGOS * sap pur 2g 3893 UTED © UF Z9TEM P: so sna oa 301 soop auouaydozuag :200N, sdnoad 230304 suuarfuo2 sepo4 kos yoy nop02 32]0}4 Jo s2un.vaddy “ayeys pue uornyos aprxoxpdy winmpos aanyfp Jo [Ur T Inoqe PPE MON, ‘suacuaqonrurp-u yprepnod fqaury 3038 [-9 mnoqe ppe pure aqna 3s91 weap Ut (Pros JO g'0 20) PMby| waa! a4 Jo [wt 0 27F -asoa sua saan sp pow 2tuuiog~ smoys Axoa 5} wox294 242 50382) sip ani You Ku 10 Kou apsyapIeauag t | smo \ cones <8HIN93 spyepry ) om O*HE + 0008 +t (07D ——|HOS + zPZ' + OHOU ‘dnou8 sphyappo ay3 Jo a2uasaad ays suisyuor e3031d}904d pas v Jo aounapaddy | . ceeeee ee eee eae meray 280 waar xp jo (8 z'0 40) Sdoxp G-p PPV 24123503 PUI g PUE Y WorINIOS sSuyag IOWPES TH TMEL y - aunpascid ° V7 Nai S.ONITHaS “E prov supyiny poe sued 3821 ayy sarvapayoquo> Kuna pio 3509 4014} 4aqys 2018 Py duoyd ocqap-p'z ani rouop hoya 1nq 382) 101s 10} apusod vad spunoduun jos2d24ne Sue ) s900N | aeans ofnz + SHINE + t8vz + OOD"HD — HOE + 01 o'nz + "HNP + ¢8vz + CODU— HOE * OF *Pdyoprw 243 Jo a>uasaad ays sucsyuo> ‘aqns 3823 943 Jo sym 243 wo ‘uosagi BMIMIYS Y toa, “oa as be 2 ay wiem pur (py}os j! 8 1 "W949 won 2014 sorrmayoednves) ~~; orth Cisse Groups Present in Organic Compounds es | REAGENTS SOS Tae .r10N OF Py nya itrophenyl hydrazine in 50 ml methanol necessary, ve 0.1 gp-rosanaline hydrochloride in 100 ml water and pass sulphur dioxide gas | charged. Filter and use the filtrate. solution A. Dissolve 35 g of crystallin copper sulphate in 500 ml water and add 2 ml conc. | jon B. Dissolve 173g of Rochelle salt (Sodium potassium tartrate) and 60 sodium | ‘ml water. |. CARBOXYLIC oe i ‘organic compounds containing the carboxylic group, —C—OH are called carboxylic acids. Oo Oo css Er eum wt tik RBS Benzoic acid Formic acid and acetic acid are liquids. Benzoic acid, oxalic acid, phthalic acid, salicylic acid and ricacds ae colourless crystalline solids. Aliphatic acids are soluble in water whereas aromatic acids sparingly soluble in water. ‘arn blue litmus red. The hydroxyl group in —COOH is far more acidic than in 4 t I \ R—C—OH+H,O === R—C—O + H,0" lure 4 drop of the given liquid (or a crystal of the solid) on a moist blue litmus paper and note the ein colour. Ifthe colour changes to red, carboxylic group or phenolic group is present. Note: Phenols also, give this test. =C Compre entee Practical cy, "em ity, mY 2. SODIUM HYDROGENCARBONATE TEST - with sodium hydrogencarbonate to give car! jon lioxide gas which; oftboxylic acids reac 4. This tests used to distinguish carboxylic acid from phy Mi, the effervescence produced. This testi " 0,7 + Ho HCO,—> RCOONa+ =— CO, , a “ve (Effervescence) Carboxylic acid Procedure . To 1 ml of orgenic liquid in a test tube, add a pinch of sodium hydrogencarbonate (NaHo, ) Abrisk effervescence indicates the presence of carboxylic group in the organic compen 3, ASTER TEST ‘A carboxylic acid reacts with an alcohol in presence of a little sulphuric acid to form an ester which, recognized by its fruity smell. H,S0, RCOOH + C,H,OH——> RCOOC,H, + H,0 Carboxylic Ester acid (Fruity smell) Procedure Take about 0.1 gof the organic compound, 1 ml of ethyl alcohol and 1-2 drops of conc. H,SO, nates tube. Heat the reaction mixture on a water bath for about five minutes. Pour the reaction mixture ins beaker containing water. A fruity smell indicates the presence of carboxylic group in the compound. 9.06. AMINES ‘Amines may be considered as substitution products of ammonia. When one hydrogen atom of ammoni 's replaced with an alkyl or aryl group,the resulting amine is called primary amine (R—NH,. Wiex ‘wo hydrogen atoms of ammonia molecule are replaced with two alkyl or aryl groups, the resulting compound is called secondary amine. The replacement of all the three hydrogen atoms of ammonia with allyl and aryl groups gives tertiary amine. Primary amines CH,NH, CH,CH,NH, O-ms Methyl amine Ethyl amine ‘Anitine, Secondary amines CH,NHCH, One Dimethyl amine N-Methyl aniline Tertiary amines (CH,).N Onn = cs N-Ethyl-N-methy! aniline ilea ‘dnox8 apéyapre 13a19p 01 pasn st ua8ea: aueBe04 5 38P5 309892 Hy “uor nos ae2U Z9ARS eotUowue (2urzesphytuaydossunp-5 2 gq “punoduto> e uy dnoad Auoqze> 32939p 03 pasn uaFe9x eau, “3801 5 Buyag pue asa suapoy gsetoroy woay sapAqapre YSMBUNSTP Y>YM $3893 0m) aureN 1, ’ 38236 oy “Can'’) auqqrue pur (HN''H"D) sutureydxoy waamseq ysmnsunstp wes nod yorym dq ase9e aureN 97 “De axoUL st pe ahe09se) sey Epppe aydxoqaes 20 jouoyd—sypre axour sf om3 ayp Jo y>TyM 5) “sooope Azerazay pu Arepuosas ‘Axewitad uaamiag ystButastp 09 pasn st, sey dauedeax seony jo asn ay stzeqM 9D aouaasaaraya 4stq Yate se8 waBospdy santB pure umnmpos YUM s12ea1 Ose 1aIEM asMENeG “sy £3803 jeyout umypos yno SurAzze> ox0yoq paxsp joyoote Ay sD oyppe azo st jousndy 57 {louayd e 20 joyooye we—arppe azour si ypyM 9D oN “8 épax zaded snurqyy anjq wamy sowdyre od $° ‘punoduros atpi Ut 3 == 5 10 J = J Jo aouasaid Suneotpur paBrey>stp 8198 1002 _ ‘punodusoo payeanaestm 03 pappe si (ayeuediuemzod umisseyod auipeye) yuaBeans 2a2eg ON, Euonzeanyesun 105 3503 5.104008 5 cuatp ar quased P09 = 9) puog age Hogi oq ya tog pereanaest HSU a a sua ase 520 quasord puog (9= 3) P40 afgnop uogee>-uoque> yal suogreoxpAy paves 7 “souAye puv souase ur yuasoad sdnox reuors>uny 249 HN (OHD—) dross per (toa —) dress oH un arobouty (Ho—) dross io jue own ssdnoad peuorssuny 100} & jiadoud ayy sourussayap 4yo3ae gdnoxd euon7e"y SYAMSNV H.LIM SNOILSANO VAIS x | a nun spunodwo 2140610 uy uasaid 54049 1 4 aa pajfe2 st punoduio> s1ueB 96‘2]dume U0) a | -aariisod ys} siya adr Jou saop [oUYIUT SeaLIYM 3593 sty} UT WAOJOPOT 3d 'Sar 03 | jo ‘ydd moyed saatd ouryag “3823 W1I0JOPOT Aq paysmBunstp aq ue? jouryie pue jouryiaW yo uta! gAqresturayp joueyge pure joueyzour waaMzeq ysm3unstp nod ue> MoH “spre yam Butreys 105 a[qereae soup Aqmy you st pue Bur auezuag Jaa pazifesojep st euyIue Ur ua8osqiu jo ated auo] asne2ag st 19 getuourure wey} aseq 2ayeem auTTTue st Aq un) 1 -uomezoqze> [Auayd 508 wey} a[qe3s axOUL ST 3[PS UINTUOZEIP JO uorjtsodurosap uo paulzoj uoWe20qr1e) [AYE asnerag st é4qM *s3es UMTUOZeIp a]qe3s u1203 30u op saurwre Areurrad sHeydye ‘sourure Areurtid sQeUIOTe 0} 3Se1}U0> UT ‘Jou st fouayd seazaym [DH aIN|Ip UI afqnyos st aurpuy ‘Jou s} auTTUe searayM UOIINTOs HORN Snoanbe ut aqnjos st [ouayg eAqrestmay> paysm3uysrp aq auyrue pue jouayd wes mow, “auture Areuntid 32a}ap 03 pasn st 3] guoreas ouruepAqies yo uoneoidde st 3eqy : paonpoid ‘be snoaqiu '5.g mopaq ainqezadura} & 3 [DH “TIP YIM payseaa st aque uinIpos way épeaedaad st poe snoxjru st moq (gq Burjyag) ayeaeyaey wintssejod wintpos BuIUIeIUO> aprxospAy wMIpes jo uonnyos e UTYa.J) uoIgnjos ayeydyns azaddoo yo saumnyoa [enba Suri Ag Peure}qo UoLN|os eB st 0 SB SLI] g4ounyos s Suryey staeuM eS $,9[]94Y2OY PaT]e> st ageareyziey winisseyod wintpo OS QUES 8, 27]qoY st3eqy ty ‘Sway 021,201 g aaremayousure 7) tO 17D “say 0z 0 -suy “6rd “suy “810 ‘suy 91d ‘suy stp0 “th ’ ‘ ° fi . got by cr mning the followin te pow ; Thue, the aad 194 be identify ‘ . RNP IN the ayy, Hye ye a) pa 0, tF < \* 9am, oo sakes place with dil HT ws Yn conc 4,80, tert ¢no action Fakes P - ‘ arm a pinch net ds" : ' and identify the gas evolved he aly ia indent croup (SO amdPa,) if the salt does not react with dil Hy « 5 i 14,50,. test for SO and PO,” by performing their individual y 2 tn re now discuss these tests in detail one by one cacID TEST 12.07 DILUTE SULPHUR! at tube and add 1-2 ml of dilute sulphuric acid. 14 lentigy antity of the salt ina tes le 12.7, Take @ small qui nd draw inferences from Tab! Jute Sulphuric Acid Test Table 12.7. Di —— | Inference ean \——“Gasevolved | Rada - = Gasevelwed | ___—Radical ZnSO, + HST wid ums lead acerate paper hi «uiphites-On treating solid sulphite with dil. H,SO,, SO, gas is evolved, which turns potassium sjvesmate solution green Na,SO, + H,S0,—+ Na,SO, + $0, t + H,0 K,Cr,0, + H,80,+350,—4 K$0,+ C(O, +H,0 Chromium sulphate (Greea) ic oxide (NO) gas is evolved which 1s On treating the solid nitrite with dil. H,SO, reagl gives dense brown fumes of NO, with oxygen of the air. KNO, + H,S0,—+ KHSO, + HNO, ] «3 3HNO, — HNO, + H,0 + 2NO eee 3KNO, + 3H,S0, —> 3KHSO, + HNO, + H,0 + 2NO 2NO +0,—+2NO, Colouess Brown fumes 208. POTASSIUM PERMANGANATE TEST chof salt in test tube add about 2 ml of dilute sulphuric acid. Boil off any gas evolvec, add little lute acid and then potassium permanganate solution dropwise. Note the changes as given in ‘8128. This test helps in detection of Cl-, Br I, C,0,2> and Fe” radicals, Table 12.8. Potassium Permanganate Test Observations [ infrme = permanganate decolourised without the | Presence of Fe sats | ‘olution of any gas, Potassium permanganate decolourised: With the evolution of chlorine. With the evolution of bromine With the evolution ofiodine. >) On warming a Ae ot, 1 With evolution of CO, __KYn0 not decolourised.163 ae gas ev 1 gesmay react with dilute sulphuric acid and give out vapours of acetic acid in dilute sulphuricacid wives with dilute sulphuric acid, then there is no need for performing conc. sulphuric acid test. ne aceti (0 poilthe salt with conc. sulphuric acid. On boiling, the acid may decompose to give SO, gas reactions Involved in conc. H,SO, Test "er on NaCl + H,S0,— NaHSO, + HCI nen" Sod. bisulphate . wit NaBr + H,SO,—>+ NaHSO, + HBr OY H,80, + 2HBr— SO, + Br, + 2H,0 ape KI + H,S0,—» KHSO, + HI i 1 H,$O, + 2HI—+ $0, + 1, + 2H,0 jetates CH COONa + H,S0,—+ NaHSO, + CH,COOH : - Acetic acid (Vinegar smell) COONa A 5, oxalates | +H,S0,—> Na,SO, + CO, t+ COT +H,0 COONa 110. TESTS FOR INDEPENDENT RADICALS (SO,7" AND PO,?>) ready discussed these radicals are not detected by dilute or concentrated H,SO,. They are tested vidually. sulphate (SO,?*) jjasmall amount of salt with dilute HCl in a test tube. Filter the contents, and to the filtrate add few of BaCL, solution. A white ppt. insoluble in conc. HCl indicates presence of sulphate. Phosphate (PO,3-) . HNO, to the salt in a test tube. Boil the contents and add excess of ammonium molybdate n. A yellow precipitate indicates presence of phosphate. 211. CONFIRMATION OF ACID RADICALS BY WET TESTS ‘dradical indicated by dil. H,SO, or conc. H,SO, tests is further confirmed by wet tests. ‘aration of Solution of the Salt for Wet Tests of Acid Radicals ‘nfirmatory tests for acid radicals are performed with the solution of the salt. ‘The solution used ‘hepurpose is any one of the following: bh * Aqueous solution or ‘water extract’. Shake alittle of the salt with water. If the salt dissolves, ‘his aqueous solution obtained is used for the wet tests of acid radic: : al and is called ‘water extract’ or' WE! 2 " Sodium carbonate extract. This is prepared only ifthe salt is insoluble in water. = -Fe On ; 165 jveanas® i san of Carbonate, co,? io oot fd test by occurrence of brisk effervescence and evolution of carbon dioxide), gin dlctesterd 05°) edi frmation of soluble carbonate Cont sives, soluble carbonate is indicated Confirmation of insoluble carbonate If the salt remains insoluble, the presence of jahesate dss insoluble carbonate is indicated | test | Les tion of the solution, add dil, HCI To the salt add dil. HCI goone porte sak effervescence and evolution of carbon oe de which turns lime water milky confirms erence of soluble carbonate. the pres Brisk effervescence and evolution of carbon diaxide which turns lime water milky confirms | the presence of insoluble carbonate. | | yagnesium sulphate test * ,another portion ofthe solution, add magnesium ccphate solution. sormation of White precipitate in the cold confirms the presence of soluble carbonate, ——_ Notes: Do not use sodium carbonate extract for performing the tests of carbonates because it contains carbonate. sodium 2. Perform magnesium sulphate test only in case of soluble carbonates. nfirmation of Sulphite, SO_2- indicated in dilute acid test by the evolution of sulphur dioxide). Experiment Observations 1. Barium chloride test Tike @ portion of aqueous solution (or sodium) A white Pt. is formed. carbonate extract and dil. acetic acid and boil off | 60,). Add barium chloride solution to it. Filter. Toa portion of the above ppt. add dil. HCL. ‘The ppt. dissolves with the evolution of sulphur dioxide 2 KMn0, test Toasecond part of the ppt. from (1) adda few drops of acidified potassium permanganate solution, K,cr,0, test ‘The pink colour is discharged To a portion of aqueous solution or sodium carbonate extract add potassium dichromate Solution acidified with dil. H,SO,, Agreen colouris obtained.166 Pracy. Ictic Confirmation of Sulphide, $? Calc, ‘cated in dilute acid test by the evolution of hydrogen sulphide), Experiment 1. Sodium nitroprusside test Take a portion of aqueous solution (or sodium carbonate extract) in a test tube and add a few drops of sodium nitroprusside solution | 2. Lead acetate test To a portion of aqueous solution (or sect | carbonate extract acidified with dil. acetic acid) | add lead acetate solution, Ablack PPt. is ob; rained, m | A yellow ppt. m 3. Cadmium carbonate test To a portion of aqueous solution (or sodiw carbonate extract) add a suspension of cadmius is formed, carbonate in water. Confirmation of Nitrite, No,- (Indicated in dilute acid test by the evolution of brown vapours of nitrogen dioxide) Experiment Observations 1. Ferrous sulphate test To a portion of aqueous solution, add some dil. acetic acid and ferrous sulphate solution. 2. Starch. A dark brown or black colouration is obtained, ‘iodide test | To a portion of aqueous solution add a few drops of dil. H,SO, and a few drops of potassium iodide solution followed by | freshly prepared starch solution, ls Diphenylamine test [osPettion of aqueous solution, addafew| A deep blue colouration is obtained, drops of diphenylamine, A blue solution is obtained. Chemical Reactions Involved in the Confirmation of Carbonate, Sulphite, Sulphide and Nitrite Carbonate (CO,?>) Reaction with dil. HCI luble Carbonates on reaction with dil. HCl give CO, gas which turns lime water milky. In case of solu! it i this test is carbonates this test is performed with water extract and in case of insoluble carbonates performed with the solid salt. CaCO, + 2HCc1I—, CaCl, + CO, + H,O Ca(OH), +CO,—+ Caco, +H,0 Lime water Milkinessa we analysts 167 fi t et is Per formed in case of soluble carbonates only tes 5 fis Na,CO, + MgSO,—> Mgco, | + Na,SO, (White ppt.) 7 50)? ) pie Na,SO, + BaCl, — 2NaCl + BaSO, J (White ppt.) BaSO, + 2HCl—- BaCl, + SO, t + H,0 te test nf 2KMnO, + 3H,S0,—+ K,S0, + 2MnSO, + 3H,0 + 5{0] Na,SO, + H,S0, —+ Na,SO, + SO, + H,0 SO, +H,0 + [0] > H,S0, . hromate test XL K,Cr,0, + 4H,S0, —> K,S0, + Cr,(SO,), + 4H,0 + 3[0] (orange) (green) Na,SO, + (0] —> Na,SO, iphide (S**) \ Xan ‘troprusside test Na,S + Na,[Fe(CN),NO]—> _Na,[Fe(CN),NOS] Sod. nitroprusside (Violet or Purple colour) tate test Na,S + (CH,COO),Pb—> PbS 4 + 2CH,COONa Black ppt. n carbonate test Na,S +CdCO,—> CdS) + Na,CO, ‘Yellow ppt. Nitrite (NO,) Ferrous sulphate test KNO, + CH,COOH—> CH,COOK + HNO, 3HNO,—> HNO, + 2NO +H,0 FeSO, + NO—> FeSO, .NO (Dark brown) tassium iodide test KNO, + CH,COOH—+ HNO, + CH,COOK 2HNO, + 2KI + CH,COOH —> 2CH,COOK + 2NO + 2H,0 + 1, I, + Starch — Blue complex |, turns starch paper blue. ae168 Confirmation of Chloride, Cl Confirmation of Bromide, Br- "ote: Chlorine water is prepared Experiment Sitwer nitrate test Acidify a portion of aqueous solution (or sodium | carbonate extract) with dil. HNO,. Boil for some time, cool and add silver nitrate solution, Manganese dioxide test Heat a pinch of the salt with a small quantity of manganese dioxide and conc. H,SO, Chromyl chloride test Mix a small quantity of the salt with a small amount of powdered potassium dichromate, Take the mixture ina test tube and add conc. H,S0,. Heat the tube and pass the red vapours evolved into the gas detector containing NaOH solution, To the yellow solution thus obtained, add dil. acetic acid and lead acetate solution. (No action with dilute HSO, ); but decomposed Experiment Silver nitrate test Adidify a portion of aqueous solu carbonate extract) with dil, HNO, add silver nitrate solution, Manganese dioxide test Heat a small quantit ™anganese dioxide Chlorine water t tion (or sodium =: Boil, cool and ty of the salt with solid and conc, H,SO, rest Acidity a Portion of carbonate extract) carbon disulphide with dilute H,SO, but decomposed by cone. H,S0, wy by conc. H, A white PPt. is ¢. ammonium hydro Evolution of Pungent irritating ¢,., Yellow —ao = ture, Ayellow ppt. is formed, | (SO, with the evolution Of bromine, Vapour) Observations Alight yellow ppt t. is obtained whichis soluble in NH,OH ns Evolution of yellowish brown vapour « bromine which turn starch paper yellow. Carbon disulphide layer acquires ont! colouration. by adding dro 'sjust discharged, the resul a Tne Solution is chlorine wa Se : inka! nc: HCI toa small volume of KMnO, solution till the P ter.~w ye ae ty || ferric chloride test ; | poston neal sation with dilate acids but decomposed by conc. H,SO, with the evolution of CH,COOH vapours) __ beaker full of water. Stir. ggroaider | io ye gh tte Hy “ sqetest cee ¢ aqueous solution (or sodium th dil. HNO,, Boil, cool and port pep wil ract) 1h ext at olution. sate som ge dioxide test ee antity of the salt with a little wt nal ot 5 oxide and conc. H,SO, res ater test ofthe aqueous solution (or sodium ape act) with ai. HCL, add 1-2 ml of a aseuiphide ‘and then chlorine water. Shake om met yand allow to stand. pepe a eel 169 (0, but decomposed by conc. H,SO, with the evolution of vapours of iodine) A yellow ppt. is formed which is insoluble in NH,OH, | Evolution of violet vapours of iodine which turn starch paper blue. Carbon disulphide layer acquires a violet | colouration. Experiment Observations Gulicacid test teasmall quantity of the salt on a watch glass. init with solid oxalic acid. Prepare paste of it sithafew drops of water. Rub the paste and smell. ) Ester test Jakeasmall quantity of the salt in a test-tube. Add conc. H,$0, (2ml) and heat. Now add ethyl alcohol (1ml), Shake and pour the contents of the tube in Take water extract of the salt. Add neutral ferric chloride solution, Filter and divide the filtrate into ‘wo portions. Toone part, add dil. HCI. To second part, add water and boil Smell like that of vinegar. Pleasant fruity smell of ester. Reddish coloured filtrate. Reddish colour disappears. Reddish brown ppt. ' Iorderto prepare neutral ferric chloride solution, take about 5 ml of ferric chloride solution and add ammonium Pydroxide solution dropwise until a small but permanent precipitate of ferric hydroxide is obtained. Boil the solution ndremove the precipitate (if any) by centrifugation or filtration, The clear solution thus obtained is neutral ferric ‘hloride solution,tag + O*HZ + 'OSUIN + YOSHZ —"os’He + “uyy + tae ‘specoxpfe umnruourure wr afqnfos A[auureds are aprioag ons yo add mona ape (288 mores ara) t3a8v + "ON —‘ondy + agy (4a) epraoag, (244 nope) stewonyp peo PNOOD"HDZ+ f¥0ID9d = —4a"(009°HD) + "ODEN srewoxtp pos Dene +O'HZ+ TOON —HoENP+D'OD sPuo|N yowtea OEY “DioHDe + ¥osHZ + "osHENr —tos*H9 +4044 + ENP V7D + OfHz + osu + fostenz —Tosthe “oun + Dene xapdtso> p@rpos OfHz + 1D /CHN)8¥] —HO'HNZ + 8V add ary, FONEN+ tIo8y ©=<——“onfy +1DN (19) @PHOLYD @40]0xO PUD 24D}20y “ny By = “ePUOIYD Jo UoDUUYUOD O44 Ul PArjoAu) SUCHIAY /O2WI4 a ] won 880940 uorngona ayp yuu | €-% PPE PLE es ou Jo mnoj0> yu at) ‘Saajosstp add ou Pauses shad ory y (i ae Puneg 24° wontons aya y im OSH ag, t “0 o>, Novy, ob > 1d PoP opo inne) . £5 ‘oaepexo jo wopemLryuO)rae + ‘ ros HOO -rostue + "om o's + on0T +"osuz+’osu— |S +" OSTHE + "OWE HOOD add ouyy D'HNe + yf0%"9 — Soe +*0'0" HN) (2'0°9) aveperg 2d usoug aappey HOOD*HDZ + 4 #4 “(HO)(000"HD) — O'NZ + 2°(00D"HD) ToeNE + 93°(00D"HO) ——108d + FNOOD"HDE wf ws pus 4m) / area7e 1 O°H + “H°0000°H) — HOH) + HOOD"HD HOOD"HOZ + "0s7=N —"os"H + €NOOD"HIZ (ete 124i) poe onr>y Noo HOOD HooHZ = + | ——enoon'Hoz+ | ®No0D HOOD (.009°H)1*" sake] *199 yp 04 mopo> aajora e syzedun "yD ur ajqnyos BuIeq UE" "+Dae —"D +z “1+ o'Wt + ‘osu + osenz —"os‘He + “oun + Diz (odd nog) iy +*ON —‘ondy + aade] "199 84) 01 anoJ09 aBueso ue syed "[DD UL |qMIOS 44 IZ — 4p + 1gNe uaCovrgen ; Chews o Confirmation of Sulphate, SO, : (NA indicated in dilute and concentrated H,SO, acid tests) Ww Experiment | Barium chloride test To a part of the aqueous solution of the salt add A white barium chloride solution Ppt. dil Hel, p Match stick test Mix 2 small amount of the salt with sodium Violet streaks carbonate and a little powdered charcoal so as to Te Produceg get a paste. Take some of this paste on one end of | a wooden splinter and heat in the reducing flame till the mass fuses. Dip the fused mass into sodium nitroprusside solution taken ina china dish. Lead acetate test To a part of aqueous solution of the salt add lead ___acetate solution ointment bie ne, Confirmation of Phosphate, PO,3- oo (Not indicated in dilute and concentrated H,SO,, acid test), Experiment Observations Ammonium molybdate test To the aqueous solution or sodium carbonate A deep yellow ppt. or colouration ischins extract (or the original salt) add concentrated nitric acid and boil. Add ammonium molybdate solution in excess and again boil. Magnesia mixture test ‘Take @ portion of aqueous solution (or a part of Awhite ppt. is obtained, sodium carbonate extract, add hydrochloric acid to acidify it and boil off CO,). Add magnesia mixture ‘to prepare it, add solid NH,Cl to magnesium chloride solution. Boil, cool and add NH,OH till 2 strong smell of ammonia is obtained) and allow tostand. Chemica)Reactions Involved in the Confirmation of $O,? and Po,> Sulphate (s0,?-) Na,SO, + BaCl, —s BaSO, 4 + 2NaCl white Na,SO, + BaCl, —+ BaSO, 4 + 2NaCl BaSO, + Na,CO,—5 Na,SO, + BaCO, Na,SO, + 4C—4 Na,$ + 4CO Na,S + Na,[Fe(CN),NO]—> Na,[Fe(CN),NOS] Purple“ne, 175 ; Table 12.11. Group Reagents | ] | Form in which cations |] | Group reagent Cations | are precipitated | Ne Pee ss Sean ite He [py | Chlorides Group! [Hsin tn {-° } —— = { © Presence of dilute Hc] | pb, cu? Sulphides Group Il NH.OH in the pe, | w ip 7 ae Presence of NHC] | Fe, AB Hydroxides : ta the presence of NH,OH [NP Mae Zn” Coe | Sulphides LH), co, t u { uiphides No the Presence of NHOH [ca Ba, sy | Carbonates — : sen 12.13. THEORY OF PRECIP, sheclassifcation of cations into diffe ITATION OF DIFFERENT GROUPS . rent groups in th, . iowledge of solubility produeqs cr Ps in the inorganic qualitative analysis is based upon the asic radicals. For example, chlorides of Hg,”*, Pb? ‘ucts. On the basi ed as their chlori ion, another ¢ alts of these b; ind Ag’ have very low solubility prod sogether in group-I and are precipitat adjusting the conditions for Precipitati sl, Before we consider the preci common ion effect. is of this knowledge these radicals are grouped ffect plays very ‘important let us discuss in brief the concept (OMMON ION EFFE Vx (kids and weak bases ae ionised ong pitentin their aqueous solutions. In their solutions, sinised molecules are in dynamic equilibrium with ions, The degree of ionisation ofa weak electrolyte weakacid or weak base) is further suppressed if Some strong electrolyte which can furnish some ion onmoa with the ions furnished by weak electrolyte, is added to its solution. This effect is called common on of NH,OH (a weak base) is suppressed by the additions of (astrong electrolyte). The ionisation of NH,OH and NH, Clin solution is represented as follows: NH,OH (aq) —— | NH, (aq) | + OH (aq) ... weakly ionised (12.1) NH,CI—, | NH," (aq) | + Cr (aq) strongly ionised (12.2) Common ion Due to the addition of NH,Cl, which is ‘increases in the solution, Therefore, acc: imeffect. For example, degree of ionisati is strongly ionised in the solution, concentration of NH, ‘ording to Le-Chatelier’s Principle equilibrium in equation 21) shifts in the backward direction in favour of unionised NH,OH. In this way, addition of NH,Cl ‘Fesses the degree of ionisation of NI HOH. Thus, the concentration of OH “Sely reduced and the weak base NH,OH becomes stil weaker hase The suppression of the deg me strong electrolyte havi a a tions of group II (Pb?*, Cu) are precipitated as their sulphides. Solubility products of “hides *f eoup TI radicals are very low. Therefore, even with low concentration of ins “S(Q,) exceed the value of their solubility products (K,,) and the radicals of group II ge ions in the solution is ree of ionisation of a weak electrolyte (weak acid or weak base) by the addition ng a common ion, is called the common ion effect. “cation of concept of common ion effect in the qualitative analysis is illustrated as follows: brodyPo parendiaid sou panies vB Appaneyas Butaey [A dnoa8 jo steatpex rao ue , 3yy Seoxaym pareitdnad FT gonpaud AaEATOS P992%2 S12NPOId 21UOr 2H stor “D> yo uoKenua>u09 passazddns we, uy peo] au A STEDIPEY f\Gn038 Jo soxeuogies yo simpoid Aumiqnjos ng u0> ath s9seax29p aouay pu wayo wor ouTUD> hq “93 ‘q)puonestuot jo 20x89p aya sassaaddns 1)" HN "HO" HN Pur [D"HIN Jo souasaid ap ut “oo'CHN) rape aa Aq soveuoque sTatp Se povertdiard are (,,89 ‘,,4g ‘ eg) A dnox8 jo sjerrpry “TI Gnoa8 jo sjearpex yam Buoye parendiraad aq osye rua 2, ‘A's sino jo sjexpes aya ‘passoaddns you s} suo! 110 Jo uomesyua>U0D axa 5] “pareudioaid 198 Set pur Sonposd Aamiqnjos paa2xe sionpord >1uor x1243 suo! _HO Jo woResU22u0D passaiddns “Seven Ho}r2q, mo] aamb axe speoypes 11] dros8 3o saprxosphy jo siompord Aamqnyos au, wor wou “D+ —D'HN -HO+ ==no'HN aa ‘UOT _}1O Jo uoHREI;UB2uED axp asea:D9p 03 19pI0 Ut Som30 kg Hokey Hos ta ap He INJO Worsestu01 jo aaxBap aya ssaaddns 02 51 |" HN Jo a8odand auy “1D” HIN JO HN 44 s2ppcoxpdy aroun se payeatdipaad axe (gf 2d) IH dnoad jo speaipey S10 onenee e a P24 328 J dno: Jo sjeorper pur sionpoid Aartqnjos paaaxe simpoid NPPMOD Paseaxour stip yim ‘saseaITUT StOT 76 Jo UOMENUADUO? '2U9}] OH == -HO+-H -HO + "HN == HO'HN “8+ HZ = S'H 1u110} pasiuo! jo anoaey H 10x} suo! ,}1 Yim BUIqUIO? HO"HN wioas SuOr jormnjos ayy ysnop seB gH Buissed 4g paaany>e {81q aq prnoys suot _,s jo woRENUa>UO> 280 29pi0 yy -ysiy aunb are sap! IN 30 sous Sone dU ses au jo su Wu22U0> ys NH “ase snp uy 1d oro) yey ee UE 8 ou "9! 4HJ0 [eaouay yr 0} ang “¢%} ys. 2. ob(24d) 1 dnory jo sisheuy ‘ZU AGEL “CL TL Age] ut se sururexa pur zazeM paystp yam “3dd ax ysem pure rayqy z “yuasaad st (_.qq) Anoad aszy ‘pausio; st ayeatdroaad age e 3] ‘pre 20TYD0IpAY EP Ppe UORN|os [eULS1I0 ayo] + 38N039044 “pre sr0pppoapAy “Tp st dnoaZ sry 2103 yuaSea dnorg *,-qq Aquo Apnys Teys am ‘yxaqu02 quasard aup urang *,,°3}] pue ,8y ‘..qq sapnput dno sty (dNOUD YAATIS) | NOU JO SISATVNV ‘SL'Z1 dd umorg quaseay sra[ssany CH + DL + 18H O8H'N'H — Hone + °HN + PIBEINZ qsal quadvay s, soumy ayy Aa DEN —DH+*HN URN + 0°H +1DeN HORN + DTHN sishjouy 0497-dnoig UL Paajoauy suoysDay [02!WEH) “SHIN Jo ase ut ydd umozq aar8 prom 31 quagear S2]Ssan YBnoryy passed si seB ay3 UayM £ saqna 3893 9p Jo Yynou ayy reaU IYBNoIg St [DH “Np ur paddip por SSPpB e UaYM sauMy azry sanis se3 UL “Tews peseruourure stay eHY) 183823 Butmoyjoy ayy Aq, Peurayuod st se3 eruouUTe Jo UONNIOAg, -yuasaid a ‘saajoaa sed eruoumure ‘ase? uy “aprxorpAy UUINIPOS Jo UOIyNIos payexjuarUOd YIM payeay SEES pues 3yna300 sit ‘ATES pyos Buisn BuruurBaq ayy ut payarap st wor ,” HN 40} oa Aueur ut pappe axe HO" HN Pur ID" HN SUOHP> Jo siskreue aug Suma -wone> ,"HN sepnpe yl (."HN) OWAZ—dNOUD JO SISATVNY ; Ti LL siskpouy an! > .Compre 178 “ent p, Chemical Reactions Involved in Group | Analysis ill precipitate Pb?’ as chloride “etic io ‘y, ddition of HCI to the solution w he addition of HCI te Pb(NO,), + 2HCI—> PbCL, L + 2 No, White ppt | | When the white ppt i boiled with water, the precipitates disso, eCaUse the Dy in hot water CI Confirmatory tests , On cooling, precipitates settle down as PbCl, is less soluble in cold w, . . ater, : pbcl, + 2KI—> Pbl,d 42K) | (Hot solution) Yellow ppt. PbCl, + K,CrO, —> PbCrO,1 + 2K), (Hot solution) Yellow ppt. 12.16. ANALYSIS OF GROUP II (COPPER GROUP) ‘This group includes Pb?* and Cu?*. These are precipitated as their sulphides, 1¢ grou tests for radicals of group Il are -arried out. Group reagent for this groupisk,s ee + " Prete, of dil. HCI. PROCEDURE Take about 2 ml of the original solution in a test tube. Make it acidic with dil. HCl and wam: contents. Through this solution pass H,S gas from the Kipp’s apparatus by turning the stop ca shown in Fig. 12.10. Formation ofthe black precipitates indicates the presence ofgroupltiai Hy is observed, pass more of H,S gas to ensure complete precipitation of the radical sulphide Cans and separate the precipitates. Stop cock Rubber cork H,S Gas tron sulphide i Sulphuric acid Fig. 12.10. Kipp’s apparatus for H,$ gas179 Table 12.13. Analysis of Group II — Black ppt. (Pb* or Cu2*) cat the black ppt. with minimum quantity (1-2 ml) of 50% HNO, ppt. dissolves, see Toone part of the above solution, add dl H,SO, and alcohol. | _— - No white ppt | hen FE To rest of the solution add NH,OH in excess | pb") ( | | confirmation ive the ppt. in hot ammonium acetate | Blue coloured solution istion. Divide the solution into two parts cs | Confirmation | potassium iodide test 1. Potassium ferrocyanide test | ‘To one part add pot. iodide solution. Yellow ppt. To one part of the blue solution add acetic acid and | is formed. The ppt. dissolves in boiling water and Pot. ferrocyanide solution. A chocolate brown | on cooling recrystallises. ppt. is formed. | . Potassium chromate test 2. Potassium iodide test | To another part add pot. chromate solution. To another part add acetic acid and pot. iodide | Yellow ppt. is formed which dissolves in NaOH solution. Awhite ppt. is formed in solution, brown oloured |___ solution, | emical Reactions Involved in the Analysis of Group I ssing of H,S gas through the acidified original solution will precipitate the radicals Pb*and Cu2* as ir sulphides. PbCl, +H,S—>2HCl+ pbs) (Black ppt.) CuCl, +H,S—> 2HCl+ cust (Black ppt.) ad (Pb2+) ack ppt. of PbS dissolves in 50% nitric acid. On adding sulphuric acid, lead sulphate precipitates. 3PbS + BHNO, —> 3Pb(NO,), + 4H,0 + 2NO +35 Pb(NO,), +H,SO,—> 2HNO,+ PbSO, 4 (White ppt.) P Potassium iodide test: \ Pb(NO,), + 2KI— 2KNO,+ PbI, + (Yellow ppt.) ’otassium chromage test: ioe. +K,CrO,— 2KNO, + PbCrO, 4 (Yellow ppt.) 2. Pp180 \ Copper (Cu?) Black ppt. of CuS dissolves in 50% nitric acid and a blue solution is obt. ‘ained on addit ion of NH,OH a 58 of 3Cus + SHNO, —> 3Cu(NO,), + 4H,0 + 2NO +35 Cu(NO,), + 4NH,OH —> [Cu(NH,),] [NO], + 44,0, (Blue solution) [Cu(NH,),] SO, + 4CH,COOH — CuSO, + 4CH,COONH, 2CuSO, + K,[Fe(CN),] — Cu,[Fe(CN),] 4 + 2K,S0, (Chocolate brown colour) 2CuSO,+4KI—> Cul, b+ I, +2K,S0, White ppt.) Brown, colouration 12.17. ANALYSIS OF GROUP III (IRON GROUP) ‘The cations present in this group are Fe”*, Fe®*, Cr>* and Al3*, Only Fe?*/Fe** and Al are included in the syllabus of this class. These cations are precipitated as hydroxides by adding ammonium hydroxide in presence of ammonium chloride. Thus, group reagent for this group is NH,OH in the presence of NH,Cl. PROCEDURE In case, first and second groups are absent proceed for group III with the original solution. Take about 5 ml of the original solution and add 4-5 drops of conc. nitric acid, Boil the solution for sometime. Add to it about 2 g of solid NH,CI and boil again. Cool the solution under tap water. Add excess of ammonium hydroxide to it and shake. A ppt. shows the presence of some cation of group III. Filter the ppt. and wash with water. Note the colour of the ppt. If the ppt. is reddish brown in colour, it indicates the presence of Fe* and if the colour is white, it indicates the presence of Al’*. Analyse the ppt. and draw inferences as in Table 12.14. Table 12.14. Analysis of Group III (Fe** and Al>*) Fe? (Reddish brown ppt.) AP* (White ppt.) _ Dissolve the reddish brown ppt. in dilute HCl, and | divide the solution into two parts | Confirmation | Confirmation | Potas ium ferrocyanide test. To one part of | 1 | the above solution add potassium ferrocyanide solution, Prussian blue colouration, Lake test. Dissolve the white ppt. in eae hydrochloric acid. Add to it two drops of Bt litmus solution. To this, add NH,OH re | blue colour develops. Blue ppt. floating i= °* colourless solution. ium sulphocyanide test. To the second part, add a little potassium sulphocyanide solution od red colouration. cavity! Cobalt nitrate test. Perform charcoal os Cobalt nitrate test with the salt. Blue mas ie addition of cone. nit + The oe cid only ifthe cat eof potassium fern few ire SFE antity of ammonium c is afer ea dicals of third group. eee tthe solution gives th dun NHO! a volved in the ecipitated as hy tions \ sare PY ms FeCl, + 3NH,O! “ qicl, +3NH,01 \ et Fe(OH), is diss Fe(OH), + 3F ferrocytinide test S “ qFeCl, + 3K,[Fe(CN way Si yanide test FeCl, + 3K gpnbrown ‘isin (AI?*) test AI(OH), + 2 AlCl, + 3NH ANALY "alias Prese: ‘ing SIS OF GROU nt in this group are | 88s through the ammo "oUp reagent for this gro181 dition of come. nitric a The ada THIN acid only if the cation ig t0 oxidise Fe?" ions to Fe? cid in the analysis of group III serves to oxidi Fe otherwise the addition of nitric acid may be avoided. To test assum ferricyanide solution to the original salt solution. A deep blue colouration Tatty of ammonium chloride otherwise the hydroxides of higher group may be precipitated "Aha of third grin The group III Cations are pe Nalysis of Group Ill “ipitated as hydro; ( “ides on the addition of excess of ammonium hydroxide \ FeCl, + 3NHon—, 3NH,Cl + Fe(OH), J (Reddish brown ppt.) Al(OH), 4 (White ppt.) Ne \ AlCl, + 3NH,OH— 30H, c1 + jron (Fe**) { whe reddish brown ne Fe(OH), is dissolved in Hc] Fe(OH), + 3Hc]_, FeCl, + 3H,0 ssium ferrocytinide test 7 C+ 3K fFe(cny P neo test: FeCl, + 3KCNS—, 3KC1+ Fe(CNs), ] —+ 12K + Fe, [Fe(CN),), Ferric ferrocyanide (Prussian blue) Ferric sulphocyanide (Blood red colouration) luminium (AI>*) AI(OH), + 3HCl—> AlCl, + 3H,0 dissolution ( AICI, + 3NH,OH — 3NH,Cl+ Al(OH), 4 Blue colour adsorbs on. this ppt. 218. ANALYSIS OF GROUP IV (ZINC GROUP) : " 2+ ‘radials present in this group are Co?*, Ni2*, Mn2* and Zn’ . These are precipitated as sulphides “80g 1. gas through the ammonical solution of the salt. Te group reagent for this group is H,S gas in the presence of NH,Cl and NH,OH. Petative Analys”® jt 183 lysis of Group Iv actions Involved in the Anal ‘cal R oe gas through the group III solution wil} Precipitate the radicals Co?*, Ni?+, Mn?" and 2n2* of H.® EM Formation of black ppt, (CoS or Nig) indicates cob; means) indicates Manganese ang dirty w alt or nickel a Co(OH), + Hs—, 2H,0 + Cogs | (Black ppt.) Ni(OH), + Hs, 2H,0 + Nis | (Black ppt.) 2n(OH), + Hys—_, 2H,0 + 2ns | (White ppt.) Mn(OH), + H,S—, 2H,0 + Mns L (Buff-coloured ppt.) sulp iv TF Sotoured iP ( cobalt (Co”) Wis CCl, + 2KNO,—, 9k), Cowno,) (Os) Cobaltous ce ENO; + CHSCOOH— cH cooy., HNo, Co(NO,), + 2HNO, —, CONO,), + ,.04NO Cobaltic ‘Nitrite | Co(NO,), + 3KNO,—, Klcowo,), Pot. cobalti nitrite Gellow ppt) 2. Ammonjuefi thiocyanate ether test Amios Owaddition of ether and a er blue colour due to the formation of. ystal of ammonium thio ammonium cobalti cyanate (shaki, ing and allowing to stand), thiocyanate, is obtained in the ethereal layer, CoCl, + 4NH,CNS—, (NF), [Co(CNS),) + 2NH,Cl Sickel (Ni?*) ‘oxime test (with O.S, ). j OH ° ‘) CH,—C = NOH CH.—¢ = MN UONe io | NiCl, + 2NH,OH +2 | - | Ni ° CH,—C = NOH CH—C=N—W Ny ces, | 0 OH i thyl Bright red complex | Dimethyl glyoxime (op) +2NH,Cl+2H,0 | i “lum hydroxide-bromine water test | NiCl, + 2NaOH —> 2NaCl + Ni(OH), 4 | ; (green ppt.) Br, + HO—> 2HBr + [0] 2Ni(OH), + H,O + [0] — 2Ni(OH), + Nickelic hydroxide (Black ppt.)a appr . “OUTIL a1qey, ut se paasoid pue syred aay out sane “TEP 304 UE Add 943 Sajossiq -saxeM yum “add ay ysem pue saxty “UOTE? sat a Td aya sovenspur dd eure Jo 2>uezeoddy ‘uoninjos 'o5%(hyn) pe uty, "eruourue oe anles aup II HO"HN PPP PUP [00 ‘Tog ‘ID"HN pros jo wi3 ¢-z ppe ‘s'o aya OL gat OF ‘A doa Jo sje>tper 10) paaroid uayp ‘uasqe st dnoxB yainos ayp JI aunai20ud ‘go'HN PUD 1D" HN Jo a>uasaed 943 11 °03°( HN) 6) dno43 5143.10) su2Bo04 dns uo sory se pavertdivasd aze Suone? 259U], “4, PUP dno15 (dNOUD WNID1V5) A dNOUD 4O SISATWNV “61°ZL ada oarqoe -ysrnya 20 249 . Ton + ¢ Pono)ea}*uz — Ponoyeal’a + 1Uzz, . 4801 op stapes add arena O*HZ + “OUz*eN <— HORNZ + “(HO)UZ add anya TORNZ + ¢ “(HO)UZ — HOENZ + “108z 1591 HOON | S°H + Touz — Hz + SUZ “go paptog st ¢}y pur ‘IH “TP UF seajossip Suz Jo "add aay auL, -antym st AI dnoag ur poureago guz yo arendisoad au, (ez) mz : wopmnjos ud - O'H2 +*Fonqas + "ouWHz <—‘ONH9 + “Odds + “CON)BNZ S*H + *Gon)U — SONHZ * SUN add unoig 4 HO)OUN — [0] * (HO) (ol + 44H — OH + 4 eduew u to an “OVO POHL P 221m “2g Buippe uo umosq suany aprxoxpay asouedTuent jo “icc cia. OL add oyna TDeNz + 7 “(HOU — HOENZ + D8 Ls"H + oun ¢ H Pte ‘spriony asouedueu u ssip spt ssouvduey, GeaW "m Id Premoyorgh vel PDde§ on 2third portion of the n, add 1-2 ml of amm, scratch the sides. White ppt. 2. Plame test Flame tert Perform the flame test with the tong rae original salt. Brick red flame. if is confirmed, do not tes for Ca?* (Original solution can be preferably used for testing Sr* and Ca? cpemical Reactions Involved in the Analysis of Group V Radicals inen (NH,);CO, is added to a salt solution containing NH,Cl and NH OH, the carbonates of Ba*, Sr2* pitated. BaCl, + (NH,),CO, —+ BaCO, + 2NH,CL SrCl, + (NH,),CO,—> $rCO, 4+ 2NH,CL CaCl, + (NH,),CO;—> CaCO, | + 2NH,CI Teinscluble carbonates dissolve in acetic acid due to formation of corresponding\goluble acetates iam (Ba) te ppt. of BaCO, dissolves in hot dilute acetic acid. BaCO, + 2CH,COOH— (CH. 1,CO0),Ba + CO, 1 +H,0 chromate test (CH,COO),Ba + K,CrO, —s 2CH,COOK + BaCrO, 4 (elow ppt) ‘uum imparts grassy green colour to the flame. "atium (S12+) “SRFSICO, dissolves in hot dilute acetic acid. 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Why § a cobalt nitrate is avoided because i forms black cob + Faaloa masks the other colours which ris ol alt oxide in the oxidising flame ight be produce d during the test sodium imparts flame test, so Inthe Yellow colour to the flame while magnesium does impart any colour, Why? not i incaseot magnesium, the energy of fame ig nab cas © 0 promote the electron tohigher energy level, hence, no colour is ™Parted to the flame. level What is the chemistry of the flame test, 2s Q s. In flame test, the valence electron of the atom gets &xcited and jumps to the higher level a eee Jumps back to the ground State, the radiation ig emitted whose frequency falls in the visible region 26. What is the function of blue 8lass in flam Q og s. The blue glass can absorb a part of whole of the coloured light in eosin different colour wh certain cases. Therefore, : Sn Viewed through blue glass. This helps in identification of some basic radicals, fe test? 8 Paste of the salt for the flame test? ans, In order to convert metal salts into met: q.28. Why can ‘ing flame test? ilicate which imparts its own golden yellow colour to the flame. 28. Why is platinum metal Preferred to other metals for flame test? Ans. Because platinum does not react with acids and does Not itself impart any characteristic colour tothe flame. 430. Ans. 31 & & z § Why should only a particle or two of the given salt should be touched with the bead 4 inborax bead test? te s. B, Ee 'saltis used in excess an opaque bead is formed Why borax bead test is not applicable in case of white salts? White salts do not form coloured meta-borates, What is Nessler’s Reagent? & ‘tsa solution of mercuric iodide in potassium iodide. ts formula is K,(Hgl,] Name the acid radic: als detected with dil. H,SO ye "00,2 92. 50,2-, No,- isa re ne i i lil. HCI? of the Vis dil, H,SO, preferred while testing acid radicals over d hero along ith he v s “> the salt is treated with HCI, during reaction HCI gas is also gi evolved h ‘ ith H,SO,, no sucl by the salt. So the actual gas cannot be identified whereas with H,; e salt. 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Q.50. Ans. ‘ gst, Why doers darkbrown ring form atthe junction of two Ans. “ans. Heat a small amount of the mixture Qs4. ass. 056. sy, Use, Why isthe hot reaction mixture in case of conc. H,50, st not thrown into the sink? ing, du dlothes and may resi 0, being heavier forms the lower la 7080, atits surface, therefore, a bro amount of nitrate and wn Fing appears atthe junction ofthe two layers what sche formla of sodium nitropracness Na,[F(CN), NO] whats chromyl chloride test? with conc. H,SO, and solid K,Cr, rromyl chloride are formed, Pase t Add to this solution NaOH, acetic 1e mixture, Deep brownish red vapours of chy low sol. of HCO, is formed « ppt. confirms chloride in th 20, ina dry test tube these vapours in water. acid and lead acetate, a 2KBr + Cl, —s 2KC1 + ty 2KI + Cl— 2k +1, Why do bromides and iodides not respond to chromyl chloride test? Because chromyl bromide (CrO,Br,) and chromyl iodide (C1Oq1,) compounds are not formed, instead of these bromine and iodine are evolved, KsCr,0, + 6K1+7H,S0,—s 31, +Cr(S0,),¢ 4K,S0, +7H,0 KiCr,0, + 6KBr + 7H,S0, —+ 3Br, + Cr (S0,), + 4K,S0, + 7H,0. Describe the chemistry of match stick test. Inmatch stick test, the sulphate is reduced to sulphide by carbon of match stick which then ives violet colour with sodium nitroprusside solution, 2nSO, + Na,CO, —s 2nCO, + Na,S0, NaSO, + 4C —4 NaS+4c0 (tach ih) Na,S + Na,{Fe(CN),NO] — Na,{Fe(CN), NOS) Porple colour Why does iodine give a blue colour with starch solution? The blue colour is due to the formation of a complex between iodine and starch. Why is original not prepared in conc. HNO,? ENO, isan oxidising agent which on decomposition gives oxygen. A yellow ppt. of sulphur “Sobtained in presence of HNO, when HH, is passed. 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