Analiza spektrofotometrike e kompleksit acid salicilik-Fe (III).

Acidi salicilik nuk absorbon ne zonen e dukshme te spektrit , por ai formon nje ngjyre te dukshme ne raportin 1:1 I kompleksuar me Fe 3+ . Ne keto eksperimente do te percaktojme: Spektrin e absorbimit dhe max te kompleksit Fe-salicilate Pregatitjen e kurbes se kalibrimit per percaktimin e sasise se acidit ne nje moster te panjohur. Reagentet Tretesire Fe(III): Tresim 2.020 g Fe(NO)3 * 9 H2O ne afersisht 200 ml uje te distiluar ne nje balon 500 ml, shtojme 6 ml acid klorhidrik te perqendruar dhe e hollojme me uje te distiluar. E perziejme dhe e ruajme ne Tretesira e salicilatit te natriumit. Acidi salicilik nuk eshte shume I tretshem ne uje, keshtu qe ai shnderrohet ne kripe te natriumit, me vellim te vogel te hidroksidit te natriumit. Tresim 0.300 g acid salicilikne nje balon 500 ml dhe shto rreth 25 ml uje te distiluar. Shtojme 2 ml NaOH dhe e perziejme balonin nderkohe qe grimcat treten. E cojme ne vellimin e duhur me uje te distiluar dhe e ruajme ne shishe te errata. Eksperimenti 1 percaktimi I spektrit te absorbimit te kompleksit Fe-salicilate. Ndezim spektrofotometrin te ngrohet nderkohe qe pregatisim mostren. Vendos 5 ml Fe(III) dhe 2 ml tretesire salicilat natriumi ne balona 25 ml. shtojme uje te distiluar deri ne shenje e perziejme. Kjo eshte tretesira e kompleksit te salicilatit me Fe. Shtojme 5 ml tretesire Fe(III) ne nje tjeter balon vellimetrike. Dhe e hollojme me H2O distiluar deri ne shenje. Kjo eshte blank ose e quajtur ndryshe prova e bardhe. E perdorur si reference pa ngjyre per tretesiren komplekse. Marim ted y kyvetat e spektorofotometrit, njeren e mbushim me tretesire e Fe(III) dhe tjetren e mbushim me kompleksin e sapo pregatitur. Vishjme anet e kyvetes me Leter te bute. Zgjedhim gjatesine e vales nga 360 nm dhe rregullojme trasmitancen 0 % . Eksperimenti I 2. Pregatitja e kurbes se kalibrimit per te gjetur sasine e acidit salicilik ose joneve salicilat ne je moster te panjohur. Acidi salicilik nuk mund te percaktohet direkt me spektrofotometri ne zonen e dukshme sepse eshte pa ngjyre. Shtimi I nje sasie te madhe Fe (III) konverton te gjitha salicilatet ne moster ne kompleks me ngjyre. Prandaj absorbance e kompleksit eshte e lidhur me perqendrimin e joneve salicilate.

Procedura. Ndezim spektrofotometrin dhe e leme te ngrohet ne max per te pakten 15 minuta. Pergatiten tretesirat e meposhtme ne balona 50 ml. Mostra ml Fe(III) 1 10.00 2 10.00 3 10.00 4 10.00 5 10.00 6 10.00

ml saliilate

Perdor pipette vellimetrike Perdor pipette 10 ml

Pas pregatitjes se mostrave, fillon matje e tyre ne spektrofotometer. Fillimisht mbushet kyveta me shume pak tretesire behet larja e saj me moster derdhet dhe mbushet serish per te bere matje te absorbances ose trasmitances ne max . Me pas kyveta pas cdo matje shplahen me uje te distiluar dhe vazhdohen matjet edhe per mostrat e tjera. Analiza e te dhenave. 1. Ndertimi I kurbes se kalibrimit duke vendosur pikat e absorbances ne boshtin e ordinatave dhe perqendrimin ne boshtin e abshisave. Ne qoftese analiza eshte e orientuar ne ne gjetjen e perqendrimit te analiteve zakonisht ne boshtin e abshisave vendosim njesi te M, g/ml, ppm, etj.

Preparation of Acid-Base Indicators

The data on this Web page are in the public domain. Copying is encouraged. The quantities listed in the "Preparation" column did not come down with Moses from Mount Sinai. They ought to be considered to be only good approximations. The audience of users, the decision whether to determine a titration error for a particular color change and the experimental environment must be considered when deciding what quantity is best to use.
Indicator Methyl Violet Crystal Violet Ethyl Violet Malachite Green Methyl Green 2 - (p - dimethylaminophenylazo)pyridine o - Cresolsulfonephthalein (Cresol Red) Quinaldine Red p - (p - dimethylaminophenylazo) - benzoic acid, Na - salt (Paramethyl Red) m - (p - anilnophenylazo)benzene sulfonic acid, Na - salt (Metanil Yellow) 4 - Phenylazodiphenylamine Thymolsulfonephthalein (Thymol Blue) m - Cresolsulfonephthalein (Metacresol Purple) p - (p - anilinophenylazo)benzenesulfonic acid, Na - salt (Orange IV) 4 - o - Tolylazo - o - toluidine Erythrosine, disodium salt Benzopurpurine 48 N,N - dimethyl - p - (m - tolylazo)aniline 4,4' - Bix(2 - amino - l - naphthylazo)2,2' - stil benedisulfonic acid Tetrabromophenolphthaleinethyl ester, K - salt 3',3",5',5" - tetrabromophenol - sulfonephthalein (Bromophenol Blue) 2,4 - Dinitrophenol N,N - Dimethyl - p - phenylazoaniline (p Dimethylaminoazobenzene) Congo Red Methyl Orange - Xylene Cyanole solution Methyl Orange Ethyl Orange 4 - (4 - Dimethylamino - 1 - naphthylazo) - 3 methoxybenzenesulfonic acid pH Change 0.0 - 1.6 0.0 - 1.8 0.0 - 2.4 0.2 - 1.8 0.2 - 1.8 0.2 - 1.8, 4.4 5.6 0.4 - 1.8, 7.0 8.8 1.0 - 2.2 1.0 - 3.0 1.2 - 2.4 1.2 - 2.6 1.2 - 2.8, 8.0 9.6 1.2 - 2.8, 7.4 9.0 1.4 - 2.8 1.4 - 2.8 2.2 - 3.6 2.2 - 4.2 2.6 - 4.8 3.0 - 4.0 3.0 - 4.2 3.0 - 4.6 2.8 - 4.0 2.8 - 4.4 3.0 - 5.0 3.2 - 4.2 3.2 - 4.4 3. 4 - 4. 8' 3.5 - 4.8 Color Change yel to bl yel to bl yel to bl yel to bl grn yel to bl yel to bl, red to yel Preparation 0.01- 0.05 % in water 0.02% in water 0.1 g in 50 ml of MeOH + 50 ml of water water 0.1% in water 0.1 % in ETOH

yel to red, yel to 0.1 g in 26.2 ml 0.01M NaOH + 223.8 ml water red col to red red to yel red to yel red to yel 1 % in ETOH ETOH 0.01% in water 0.01 g in 1 ml 1M HCI + 50 ml ETOH + 49 ml water

red to yel, yel to 0.1 g in 21.5 ml 0.01 M NaOH + 229.5 mL water bl red to yel, yel to 0.1 g in 26.2 ml 0.01M NaOH + 223.8 ml water purp red to yel or to yel or,to red vt to red red to yel purp to red yel to bl yel to bl colorless to yel red to yel blue to red purp to grn red to yel red to yel vt to yel 0.01 % in water water 0.1% in water 0. 1 170 in water 0.1% in water 0.1 g in 5.9 ml 0.05 M NaOH + 94.1 ml water 0.1 % in ETOH 0.1 g in 14.9 ml 0.01M NaOH + 235.1 ml water saturated water solution 0.1 g in 90 ml in ETOH + 10 ml water 0.1% in water ready solution 0.01 % in water 0.05 - 0.2% in water or aqueous ETOH 0.1% in 60% ETOH

3',3",5',5" - Tetrabromo - m - cresol - sulfonephthalein (Bromocresol Green) Resazurin 4 - Phenylazo - l - naphthylamine Ethyl Red 2 - (p - Dimethylaminophenylazo) - pyridine 4 - (p - ethoxyphenylazo) - m - phenylene - diamine monohydrochloride Lacmoid Alizarin Red S Methyl Red Propyl Red 5',5" - Dibromo - o - cresolsulfone - phthalein (Bromocresol Purple) 3',3" - Dichlorophenolsulfonephthalein (Chlorophenol Red) p - Nitrophenol Alizarin 2 - (2,4 - Dinitrophenylazo) - l - naphthol - 3, 6 - disulfonic acid, di - Na salt 3',3" - Dibromothymolsulfonephthalein (Bromothymol Blue) 6,8 - Dinitro - 2,4 - (lH)quinazolinedione (m Dinitrobenzoylene urea) Brilliant Yellow Phenolsulfonephthalein (Phenol Red) Neutral Red m - Nitrophenol o - Cresolsulfonephthalein (Cresol Red) Curcumin m - Cresolsulfonephthalein (Metacresol Purple) 4,4' - Bis(4 - amino - i - Daphthylazo) 2,2'stilbene disulfonic acid Thymolsulfonephthalein (Thymol Blue) o - Cresolphthalein p - Naphtholbenzene Phenolphthalein Ethyl - bis (2.4 - dimethylphenyl)acetate Thymolphthalein 5 - (p - Nitrophenylazo)salicylic acid, Na - salt (Alizarin Yellow R) p - (2,4 - Dihydroxyphenylazo)benzene - sulfonic acid, Na salt 5,5' - Indigodisulfonic acid, di - Na - salt 2,4,6 - Trinitrotoluene 1,3,5 - Trinitrobenzene Clayton Yell

3.8 - 5.4 3.8 - 6.4 4.0 - 5.6 4.0 - 5.8 0.2 - 1.8, 4.4 5.6 4.4 - 5.8 4.4 - 6.2 4.6 - 6.0 4.8 - 6.0 4.8 - 6.6 5.2 - 6.8 5.2 - 6.8 5.4 - 6.6

yel to blue or to vt red to yel col to red

0.1 g in 14.3 ml 0.01 M NaOH + 235.7 ml water water 0.1 % in ETOH 0.1 g in 50 ml MEOH + 50 ml water

yel to red, red to 0.1 % in ETOH yel or to yel red to bl yel to red red to yel red to yel yel to purp yel to red col to yel 0.1% in water 0.2% in ETOH 0.2 g in 100 mL of 1.5% HCl 0.02 g in 60 ml ETOH + 40 ml water ETOH 0.1 g in 18.5 ml 0.01M NaOH + 231.5 ml water 0.1 g in 23.6 ml 0.01 M NaOH + 226.4 ml water 0.1% in water

5.6 - 7.2, 11.0 - yel to red, red to 0.1 % in MEOH 12.4 purp 6.0 - 7.0 6.0 - 7.6 6.4 - 8.0 6.6 - 7.8 6.6 - 8.0 6.8 - 8.0 6.8 - 8.6 0.0 - 1.0, 7.0 8.8 yel to bl yel to bl col to yel yel to or yel to red red to amb col to yel 0.1% in water 0.1 gin 16 ml 0.01 M NaOH + 234 ml water 25 g in 115 ml M NaOH + 50 ml boiling water 0.292g of NaCl in 100 ml water 1 % in water 0.1 gin 28.2 ml 0.01M NaOH + 221.8 ml water 0.01 g in 50 ml ETOH + 50 ml water 0.3170 in water

red to yel, yel to 0.1 g in 26.2 ml 0.01 M NaOH + 223.8 ml water red ETOH

7.4 - 8.6, 10.2 - yel to red 11.8 1.2 - 2.8, 7.4 9.0 8.0 - 9.0 1.2 - 2.8, 8.0 9.6 8.2 - 9.8 8.2 - 10.0 8.2 - 10.0 8.4 - 9.6 9.4 - 10.6 10.1 - 12.0 11.4 - 12.6 11.4 - 13.0 11.5 - 13.0 12.0 - 14.0

red to yel, yel to 0.1 gin 26.2 ml 0.01M NaOH + 223.8 ml water purp bl to red red to yel col to red or to bl col to pink col to bl col to bl yel to red yel to or bl to yel co] to or col to or 0.1 gin 5.9 ml 0.05 M NaOH + 94.1 ml water 0.1 g in 21.5 ml 0.01 M NaOH + 228.5 ml water 0.04% in ETOH I % in dil. alkali 0.05 gin 50 mL ETOH + 50 mL water saturated solution in 50% acetone alcohol 0.04 g in 50 ml ETOH + 50 ml water 0.01 % in water 0.1 % in water water 0.1 - 0.5% in ETOH 0.1 - 0.5% in ETOH

Tema 1: identifikimi I nje komponimi kimik inorganik duke u bazuar ne spektrin UV-VIS. Tretesira 0.001 M (0.001 mole subs ne 1 L) Sasia qe do te peshohet do te llogaritet ne baze te mases molare * me nr e moleve. Kjo sasi kalohet ne nje balon te taruar 1 L. Me pas do te behet matja. Nga 380 nm- 780 nm duke levizur me nga 5 nm. Perfundimi: Ndertohet lakorja dhe llogaritet koeficenti molar I absorbimit. Team 2: Do pregatiten tretesirat 0.001 M te seciles prej vitaminave. Vitamina A (C20H30O) Masa molare: 288.4516 g/mol Vitamina C.

Formula

C6H8O6

Mol. mass

176.12 g/mole