Chng1.

PH HNG NGOI Infrared (IR) spectroscopy

Thng thng th n v ca bc sng c s dng trong ph hng ngoi l m ( 1 m = 10- 4 cm) v thay cho tn s (Hz), ngi ta s dng n v l s sng:

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Vng bc x hng ngoi (IR) l mt vng ph bc x in t rng nm gia vng trng thy v vng vi ba; vng ny c th chia thnh 3 vng nh: - Near-IR 400-10 cm-1 (1000- 25 m)

- Mid-IR 4000 - 400 cm-1 (25- 2,5m)

- Far-IR 14000- 4000 cm-1 (2,5 0,8m) Phng php phn tch ph hng ngoi ni y l vng ph nm trong vng c s sng 4000 - 400 cm-1. Vng ny cung cp cho ta nhng thng tin quan trng v cc

dao ng ca cc phn t do l cc thng tin v cu trc

ca cc phn t
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 c th hp th bc x hng ngoi, phn t phi p ng cc yu cu sau: - di sng chnh xc ca bc x: mt phn t hp th bc x hng ngoi ch khi no tn s dao ng t nhin ca mt phn phn t (tc l cc nguyn t hay cc nhm nguyn t to thnh phn t ) cng l tn s ca bc x ti.

-Mt phn t ch hp th bc x hng ngoi khi no s hp th gy nn s bin thin momen lng cc ca chng.
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Tng quan gia ph dao ng v cu trc phn t

Cc nhm chc, nhm nguyn t v lin kt trong phn t c cc m ph hp th hng ngoi c trng khc nhau .

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Mc d phng php ph dao ng l mt trong nhng phng php hu hiu nht xc nh cc cht v nh tnh cng nh nh lng, c ng dng rng ri trong nghin cu khoa hc cng nh trong kim tra cng nghip, phng php ny cng c nhng hn ch nht nh: Bng phng php ph hng ngoi khng cho bit phn t lng (tr trng hp c bit). Ni chung ph hng ngoi khng cung cp thng tin v cc v tr tng i ca cc nhm chc khc nhau trn mt phn t. - Ch ring ph hng ngoi th i khi cha th bit l cht nguyn cht hay cht hn hp v c trng hp 2 cht c ph hng ngoi ging nhau.
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ng dng :
1. Nhn bit cc cht - Trc khi ghi ph hng ngoi, ni chung ta c th c nhiu thng tin v hp cht hoc

hn hp cn nghin cu, nh: trng thi vt l, dng

bn ngoi, tan, im nng chy, im chy. Nu c th th cn bit chc mu l cht nguyn cht hay hn hp. Sau khi ghi ph hng ngi, nu cht nghin cu l hp cht hu c th trc tin nghin

cu vng dao ng co gin ca H xc nh xem

mu thuc loi hp cht vng thm hay mch thng hoc c hai.
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Sau nghin cu cc vng tn s nhm xc nh c hay khng c cc nhm chc. Trong nhiu trng hp vic c ph (gii ph) v tm cc tn s c trng khng nhn bit mt cch ton din v cht nghin cu, nhng c l l c th suy on c kiu hoc loi hp cht. 2. Xc nh tinh khit. 3. Phn tch nh lng.

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Hng dn Gii Ph IR - NMR

Ph hng ngoi (FT-IR) v ph cng hng t ht nhn (1H-NMR, 13C-NMR) c coi l 2 cng c c bn nht thc hin php xc nh cu trc cc hp cht hu c. Cc bc thc hin vic gii 1 bi tp v ph vi cng thc tng qut cho trc:

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BC 1. Tnh KHNG BO HA (degree of unsaturation - DU) t trong cng thc tng qut xem trong phn t c bao nhiu vng, bao nhiu lin kt i.
Gi s ta c 1 cng thc l CnHmXi - Nu X l Halogens th coi n l H => CnHm+i - Nu X l O, S th b => CnHm - Nu X l N th tr i H tng ng => CnHm-i DU= n - m/2 + 1 VD: C5H10O => DU = 5-10/2+1=1 C8H11N => DU =8-10/2+1 = 4 NU: DU = 1 c th c 1 LK i hoc vng DU = 2 c th c 2 LK i, 2 vng, 1 LK ba hoc 1 LK i + 1 vng DU = 3 c th c 3 LK i, 3 vng, 1 LK i + 2 vng, 2 LK i + 1vng, 1 LK ba + 1 LK i hoc 1 LK ba + 1 vng DU = 4 ngh ngay ti vng benzen DU = 5 c th l vng benzen + 1 LK i hoc vng benzen + 1 vng DU = 6 c th l vng benzen + 2 LK i hoc 2 vng hoc 1 LK ba hoc 1 LK i + 1 vng. 67

BC 2. Nhn vo ph IR ti vng s sng ln hn 1500cm-1

Kt hp cc d kin c t cng thc tng qut, DU v ph IR: nu Nu c 1 lin kt i v nguyn t O c th ngh ti nhm carbonyl Nu khng c lin kt i m li c O th c th ngh ti ether hoc ru

BC 3. S dng ph NMR xc nh cc lin kt trong phn t

T cc nhm chc xc nh t B2, vit cu trc phn t v da vo ph NMR nh gi xem cng thc hp l cha.
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BC 4. Kim tra s O, C, H, Hal, ... xem ph hp vi cng thc tng qut cha.
Kim tra ha tr cc nguyn t xem ph hp cha Nu cha ng, vit cu trc phn t khc v kim tra li

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Tn s dao ng c trng ca ph IR

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Chng 2: Ph NMR
Ph 1H-NMR l mt k thut s dng xc nh cu trc ha hc ca hp cht hu c. Ph proton cho ta bit c s loi proton c trong phn t . Mi loi proton s c tnh cht khc nhau v th s c dch chuyn khc nhau trn ph proton. Ngi ta s dng TMS ( tetra methyl silan ) lm cht chun trong ph proton v dch chuyn ha hc ca proton trong TMS c chn l 0 pmm
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S tng tc ca cc proton (H) xung quanh s gy ra s tch vch theo quy tc (n+1): 4.quartet 1.singlet 5.pentet 2.doublet 6.sextet 3.triplet 7.septet 8.octet...

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 dch chuyn ha hc (chemical shift) ca Hydrogen ph NMR 0,9ppm: RCH3 1 aliphatic 1,3ppm: R2CH2 2 aliphatic 1,5ppm: R3CH 3 aliphatic

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2 - 2,7 ppm: nhm ti v tr ny lin kt vi nhm carbonyl

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3,7 - 4,1 ppm: nhm ti v tr ny lin kt vi nhm oxygen

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9 - 10 ppm: nhm aldehyde

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6,5 - 8,5 ppm: Aromatic 2,2 - 3 ppm: H ca nhm gn vo Aromatic

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10 - 13,2 ppm: acid

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0,5 - 3 ppm: amin aliphatic 3 - 5 ppm: amin Aromatic

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4 - 4,4ppm: H ca nhn gn vi NO2

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4 - 12ppm: H ca ru

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Alkyl Halides

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Ph 13C - NMR
Nu nh ph 1H-NMR cho cc tn hiu ca cc loi H th 13C-NMR cho cc tn hiu ca cc loi C v th vi cc cht hu c kt hp 2 ph ny c th xc nh c cu trc ca hu ht cc cht.

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Bng tm tt dch chuyn ha hc trong ph 13C-NMR

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Tng quan so snh gia 1H-NMR vi 13C-NMR

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