Download - طرق التحليل الطيفي والتحليل الطيفي الجزيئي (عملي)

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אאאאFFEE

אא

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אאאא

٢٦٢٢٦٢

א٢٦٢אאאאFE

،،אא،אW

אאאאאאאאאאא א א א א א א ،א

אאאאאאאאאאאאW

אאאK

אאאאאאא א ،א אא

א ، אא א אא אא،אאאאאאאאאאאאאאאאא

א א ،א אא،אאK

א א ? א א FE ? ?א

?אאאאאאאK

אאאאאאא،א،אאאא

אאאאאK

א אא א WאK

אאאא

א٢٦٢אאאFE

אאאאאאאאאKאאאא

אאאKאאאא

אאאאאאאאאאאK

אKאאאאא،אאא،אא،א

אאK،אאאאאא،אאאאאאK

אא،אאאאאאאKאאאא

אא،אאאאK

אאאאאא

אאאאFFEE

אאאã¹]<gè…‚jÖ]æ<ËÖ]<Üé×Ãj×Ö<íÚ^ÃÖ]<퉉ö¹]

אאאא

א

א

א

١

א٢٦٢ אאאאאF( אאא

- ١ -

אאWאאאאאא

אאאאאאאאKאאW

אאW١- אאWFiEאאאK

• אאאאK • λmaxK • אאK•אאאK

FiiEאאK• λexλemK•אאאK

FiiiEאאאK• אאאK • אאאאאאK ٢- אאאK

אאאWאאא١٠٠K٪

אאW٤٠KאאW

،،،،א،א،א،،،א،K

אאWאאאK

א٢٦٢ אאאאאF( אאא

- ٢ -

אאאאאא

אWאאאאאא

אKאאאאאאאאאא،אKאא

אFאאEvisible molecular spectrometry (colorimetry) אאאא(380-780 nm)אאא،ultraviolet

molecular spectrometryאאאאא(200-380 nm)Kאאא(Radiation source)

אאא(sample cell)אא،אאאאא،א

אmonochromatorKאאאאא،אא،א

אאאאdetectorאאאאאאאאK

0.000א

א

א

א

F١WEאאא

א٢٦٢ אאאאאF( אאא

- ٣ -

אאאW١JאאSingle-Beam SystemW

אאאאF١Eאא،אאאאאא

אאא،אאאאFאאE،אאא

Blank SolutionKאאאא٢JאאDouble-Beam SystemW

אאאאKאאאא،אאאא

F٢KEאאא،אא

א

FW٢Eאאא

א

א

א

א

א

א

א

א٢٦٢ אאאאאF( אאא

- ٤ -

١J١J١אאאאColorimeter

אWא،אא

אא،אF٣KEאאFxE،אאאFyKE

C

A

y

x

F٣Eאאא

א٢٦٢ אאאאאF( אאא

- ٥ -

אאאאW• אK • K

אאאW• אK • 100 mlK • א50 mlK • K • K

אאWWאאW

١- 10 g/lאאא100 mlK

٢J אאאאאW0.5, 1, 1.5, 2, 2.5 g/lא50 mlאאF10 g/lKE

WאאאλmaxW١. אאאאאאK٢. אאאאאאאא

אאאF430__710 nmEאK ٣. אאאλmaxאאK

WאW١. λmaxאא،0.0אאאK٢. אאאאאKKKKKK

אK ٣. אאאK

א٢٦٢ אאאאאF( אאא

- ٦ -

אאWאאW١- אא10 g/lא

100 mlK٢- אאאאאאאאW

F0.5, 1, 1.5, 2, 2.5 g/lKE٣- אאאאאאאK٤- אאאλmaxK٥- אאאאאאא

אK٦- אאאאK٧- אאK٨- אא1221 CACA •=•K

א٢٦٢ אאאאאF( אאא

- ٧ -

٢J١J١אאאאSpectronic 20D

אW،אאא

אא،אF٤KEאאFxEאאא،FyKE

אאאאאאאFxKE

אאאאW

• אאK • K

C

A

y

x

F٤EWאאא

א٢٦٢ אאאאאF( אאא

- ٨ -

אאאW• אK • 100 mlK • 250 mlK • א50 mlK • K • K

אאWWאאW

١- 20 g/lאאאא250 mlK

٢- אאאאאW3, 6, 9, 12, 15 g/lא50 mlאאF20 g/lKE

WאאאλmaxW١- אאאאאאK٢- אאאאאאאא

אאאF370__410 nmEאK ٣- אאאλmaxאאK

WאW١- λmaxאא،0.0אאאK٢- אאאאאKKKKKK

אK ٣- אאאK

א٢٦٢ אאאאאF( אאא

- ٩ -

אאWאאW١- אאא20 g/lא250 mlK٢- אאאאאאאאW

F3, 6, 9, 12, 15 g/lKE٣- אאאאאאאK٤- אאאλmaxK٥- אאאאאאאאK٦- אא،אא

אא؟אא٧- אאK٨- אא1221 CACA •=•K

א٢٦٢ אאאאאF( אאא

- ١٠ -

λ

A

x Y

λ1 λ2

F٥WEאא

Fx+yE

٣J١J١אJMnO4אא-2OCr 72אאאא

אWאאאא

λ1λ2אF٥KE

• xאλ1،yאλ2K

• אאאאW

1.…………… yc · yε1 + xc· xε1 = 1λA1

2Aλ2 = 2εx · cx + 2εy · cy ………….2

א٢٦٢ אאאאאF( אאא

- ١١ -

• ε1

x،2εx1εy، 2εyx ،yאא

cA=εאFb = 1KE

• 1A2Aאאλ1λ2K

• א12אאcxcyW

……………….3

yεxεyεxε

yεAyεA

xC 1221

1221

•−•

•−•=

………............4

xεyεxεyε

xεAxεAyC 2112

2112

•−•

•−•=

א٢٦٢ אאאאאF( אאא

- ١٢ -

אאאאW• אאK • אאKIO4K • אF0.002 MEW

1.0 g אא110° CK300.08 g400 ml150 mlאא

א250א mlאאאK• אא-OCr 2

72K2F0.017 ME250 mlW

2.0 gאאאא120° CK30-401.25 g400 ml150 mlא

אא250א mlאאאK

אאאW• א250 mlK • 10 mlK • אK • א250 mlK • 400 mlK • K

אאWJ אאFεEW

١- אאאW10 , 15 , 25 mlאאא250 ml50 mlK

٢- 10 mlאאא0.5 gאאKIO4K

٣- אאאK

א٢٦٢ אאאאאF( אאא

- ١٣ -

٤- אא250 mlאאK

٥- אאא440 nm545 nmא0.5M אK

٦- אאאεWFCAε = Eאא440 nm545

nmK

J אאFεEאW ١- אאאW10 , 15 , 25 mlאאאא

250 ml100 mlK٢- 10 mlאאא

אאאאK ٣- אאא440 nm545 nmא0.5M

אK ٤- אאאεאא440 nm545 nmK

J אW • −

4MnO−272OCrאאא

440א nm545 nmK

אאWאאWאאאאאא -١

K٢- אאאאK ٣- אאεאאאא440 nm

545 nmאאK ٤- אεאאאאא440 nm545

nmK

א٢٦٢ אאאאאF( אאא

- ١٤ -

٥- אאאאאא440 nm545 nmK

٦- nm440εnm545εnm440εnm545εאאאFAEλmax =440 nmλmax =545 nm

אאאאאאאאW

⎟⎠⎞

⎜⎝⎛

⎟⎠⎞

⎜⎝⎛

⎟⎠⎞

⎜⎝⎛

⎟⎠⎞

⎜⎝⎛

×−×

×−×=−

545440545440

440545545440

4 CrMnMnCr

ACr

ACr

MnOC

εεεε

εε

⎟⎠⎞

⎜⎝⎛

⎟⎠⎞

⎜⎝⎛

⎟⎠⎞

⎜⎝⎛

⎟⎠⎞

⎜⎝⎛

×−×

×−×=−

545440545440

545440440545272 CrMnMnCr

AMn

AMn

OCrC

εεεε

εε

א٢٦٢ אאאאאF( אאא

- ١٥ -

٤J١J١אאאא

אWאאא١،١٠אFe 2+،

K

N

N

3+Fe2+

N

3

Fe

N

אאאאאא،λmaxאאאאאλmaxא

אאאאאאKאאpHא3.5،א

אאא+2FeWOHHONFeOHNHFe 242

242234 +++++→++אאאאW

• אא10 p.p.m0.0702 gאאOHSONHFe 26.2)4(2)4(אאא

،2.5 mlאאאאK • אאWא0.1 g١،١٠100 mlאא

K • אWא10 g

אHClא100 mlK

א٢٦٢ אאאאאF( אאא

- ١٦ -

• אWא10 gא100 mlאאK

אאאW• 1LK • אK • K • א100 mlK • K

אאW١. 25 ,10 ,5 ,2 ,1א mlאאא

100 mlK٢. 50א mlאא100 mlK٣. אאא100 mlאK٤. אאאאא1 mlא

5 mlאא8 mlאאאאאאK

٥. א15אאאאאא،K

٦. אאאאאאאאp.p.mאא١K

٧. אאאאאאאאאאאאאא400 nm700 nmא

אאאλmaxK٨. אאאאאאא

אאλmax،אאאλmax،אאאK

א٢٦٢ אאאאאF( אאא

- ١٧ -

אאWאאW

١- אאאאא٦K٢- λmaxאאK٣- אאאאאK٤- אאאאp.p.mK٥- אεFאאEאאאא

אp.p.mK

א٢٦٢ אאאאאF( אאא

- ١٨ -

٥J١J١אאאא

אWאא،א

אא،אאאאאאאא،אאאאא

אאKאאאאW

• אאK • K

אאאW• אK • 100 mlK • א25 mlK • 100 mlK • K • אK

אאWWאאW

١- 10 g/lאא100 mlK

٢- אאאאאW1, 2, 3, 4, 5 g/lא25 mlאאF10 g/lKE

א٢٦٢ אאאאאF( אאא

- ١٩ -

WאאאλmaxW١- אאאאאאK٢- אאאאאאאא

אאאאF240__340 nmEאK ٣- אאאλmaxאאK

WאW١- λmaxאא،0.0אאאK٢- אאאאאKKKKKK

אK ٣- אאאK

אאWאאW١- אאא10 g/l100 mlK٢- אאאאאאאאW

F1, 2, 3, 4, 5 g/lKE٣- אאאאאאאK٤- אאאאλmaxK٥- אאאאאאאK٦- אאאאλmaxK٧- אאאאאאאאK٨- אאאאK٩- אאK١٠- אא1221 CACA •=•K

א٢٦٢ אאאאאF( אאא

- ٢٠ -

٦J١J١אאאאאUV-1601PC

אWאאאאאאא

אאא،א،אאאאK

Wאאאא• אאK • אK • אאK • אאK • אK • K • K

אאאW• 100 mlK • 500 mlK • 1000 mlK • א100 mlK • K • K • K • אK • K

א٢٦٢ אאאאאF( אאא

- ٢١ -

אאWWאW

١. א1.0 gא10 mlאאFHNO3E100 mlK

٢. אאאFNO2E،אאאאאK

٣. אK٤. 5 mlאאK٥. אאאאאאFNO2Eא،

אK٦. אא

אאK٧. אK٨. א500 mlK٩. אאאK

WאאW١. 1000 p.p.mאאא

1000 mlK ٢. אאאאאp.p.mW200, 400, 600,

800, 1000א100 mlאאF1000 p.p.mKEWאאאλmaxW

١- אאאאאאK٢- אאאאאאאא

אאאF390__800 nmEאK ٣- אאאλmaxאאK

א٢٦٢ אאאאאF( אאא

- ٢٢ -

אWאW١- λmaxאא،0.0אאאK٢- אאאאאKKKKKK

אK ٣- אאאK

אאWאאWא1000 p.p.mאאא -١

1000 mlK٢- אאאאאאאאW ٣- F200, 400, 600, 800, 1000 p.p.m Eא100 mlK٤- אאאאאאאK٥- אאאλmaxK٦- אאאאאאאאK٧- אאאאאK٨- אאp.p.mK٩- אאאK

א٢٦٢ אאאאאF( אאא

- ٢٣ -

אאאFאEא

אWאfluorescenceאאאא10-6-10-9sec.אאK

אאאא٠א

אF٦EאאW

مصدر

حاجز

أشعة نافذة

طول موجة اإلثارةλex

وعاء العينة

مقدر آلة عرض

تألق تألق

تألق تألق

حاجز

موحد طول الموجة األولى

موحد طول الموجة الثاني

طول موجة االنبعاثλem

F٦WEאא

א٢٦٢ אאאאאF( אאא

- ٢٤ -

אאאאאאאאKאFאא٠אאא

אאאאJW

F = KØI0 (2.303 ε b c)

אאאאאF cאאאW

F = Kc

אFcא AcJKאאFcאאK

א٢٦٢ אאאאאF( אאא

- ٢٥ -

١J٢J١

אאאאאאW

אאאאאאW

COOHO C

O

CH3+ 2OH

- COO-

OH + CH3COO +H2O

Salicylate ionAcetylsalicylic acid

אא400 nmFEא310 nmFKE

אאאאW• K• אK • א4 MFKE

אאאW• 100 mlK • אK • 2LK • K • 1LK • K • א100 mlK

א٢٦٢ אאאאאF( אאא

- ٢٦ -

אאW١- א0.1א g100 mlK٢- אאא2 LאK ٣- א1 LK ٤- אאאאאK ٥- אאאאאF500 ml E٠ ٦- אאאאאאK ٧- 100 p.p.mא100 ml K ٨- 6א100 mlFWU،5،4،3،2،1KE ٩- 2 mlאאאאאK ١٠- אאאאF1-5 Eאאא

אWF5 ml،4،3،2،1EאKFאאאאאאKE

١١- אאFUE5mlאאאFאאאאאKE

١٢- אאאFאאEp.p.mאK

Wא0.1 gאאKאא

3.65 p.p.mאאאאKאW• אp.p.mZ3.65• אmgZ3.65• אgZ3.65 ×10-3

אg3.65 × 10-3• אZאאZ138.12Z2.64 × 10-5

א٢٦٢ אאאאאF( אאא

- ٢٧ -

QאZאFאE • אאZ2.64 × 10-5• אgZא×אאK

Z2.64 × 10-5×180.12Z4.76 × 10-3 g 100 • אאZ4.76 × 10-3 C5Z0.096 g

אg

∴אאאZא

C100

0.096 Z0.1C100Z96%

אאW אאאאאאW

Kאאא •• אK • אK • אp.p.mK • אmggK • אFאאאKE • אK • אgK • אאאK

א٢٦٢ אאאאאF( אאא

- ٢٨ -

٢J٢J١B2אאא

אWB2FRibo FlavinE5%،א

אK

אאאאW• B2K • א5% V/VK

אאאW• אK • 100 mlK • 1000 mlK • א100 mlK

אאWWאאW

١. 100 p.p.mB2א0.01 g5% V/VאאאK

٢. אאאאאW0.0, 0.2, 0.4, 0.6, 0.8, 1

p.p.mאא5%א100 mlKWאW

١. אאאאאK ٢. אא0.0א p.p.m،

אK

א٢٦٢ אאאאאF( אאא

- ٢٩ -

٣. אאאא0.6 p.p.mאFאEא،אא

אאK٤. אאאK ٥. אK ٦. אאK

אאW

אאW• B20.01 g K • אאאאF0.0, 0.2, 0.4, 0.6, 0.8, 1 p.p.mEא

א100א p.p.mK • 5% V/VאK • אאאאK • אK

א٢٦٢ אאאאאF( אאא

- ٣٠ -

אאאאאאא

Infra-red Spectroscopy אWאאאאFאE

אאאאאאאאKאאאאאW

J אאאK J אאאאK

אאאאאאWK אאK K אאאאאאאK

אאאא،אאאאאאאFאאE،א

אאאאאא،אאאאmass

spectroscopyאא،אא،N.M.RKאאאאλא

אµmאאKאאאאאאcm-1אאאאK

א٢٦٢ אאאאאF( אאא

- ٣١ -

אאאWאאאF٧EW

אWאא،אKאאאW،אאאאאא

אאאאאאאKאF١EאאאאאאאW

FµmEאאא

א0.16 ___ 4

א0.13 ___ 9

א0.13 ___ 12

א0.2 ___ 25

א0.25 ___ 40

F١WEאאאאאא

א

א א

F٧WEאאא

אאאא

א٢٦٢ אאאאאF( אאא

- ٣٢ -

אאאאאאאאאאאאK

אאאא،אאאאאK

אFאWEאאאאאW

J אאאKJ אאאK J אאאK J K

א٢٦٢ אאאאאF( אאא

- ٣٣ -

F٢WEאאאK

אא אאcm-1

C – H

FEאאFE

א

٢٨٥٠ – ٣٠٠٠ ٣٠٠٠ – ٣١٠٠ ٣٠٥٠ – ٣١٥٠

٣٣٠٠ ٢٨٠٠ – ٢٩٠٠ ٢٧٠٠ - ٢٨٠٠

C = C

١٦٠٠ – ١٦٨٠ ١٤٧٥ و ١٦٠٠

C ≡ C ٢١٠٠ – ٢٢٥٠

C = O

א

١٧٢٠ – ١٧٤٠ ١٧٠٥ – ١٧٢٥ ١٧٠٠ – ١٧٢٥ ١٧٣٠ – ١٧٥٠ ١٦٤٠ – ١٦٧٠ ١٦٧٠ و ١٨١٠

١٨٠٠C - O،א

،אא

١٠٠٠ - ١٣٠٠

H _Oא

٣٦٠٠ – ٣٦٥٠ ٣٢٠٠ – ٣٥٠٠ ٢٤٠٠ – ٣٤٠٠

N - Hאאאאא٣٠٠ - ٣٥٠٠ C – N١٠٠٠ – ٣٥٠ C = Nא١٦٤٠ – ١٦٩٠

N ≡C٢٢٤٠ – ٢٢٦٠

N = OC-XXZ

ZZ

١٣٥٠ – ١٥٥٠ ١٠٠٠ – ١٤٠٠

٦٠٠ – ٨٠٠

٦٦٧قل من أ

א٢٦٢ אאאאאF( אאא

- ٣٤ -

١J٣J١

אאאאאאאאאFIREאW

אאאאאאאאאאאא،א

אאאאK

אאאאW• אאK • אK • K • K

אאאW• אאKBrK

אאWWאאW

١. אאK٢. אאאאא

א،אאK

WאאאW

١- אאאאאK٢- אאאאאK

א٢٦٢ אאאאאF( אאא

- ٣٥ -

٣- אאאאאאK

٤- אאאאK

אאW

אאW• אאאK • אK

א٢٦٢ אאאאאF( אאא

- ٣٦ -

٢J٣J١אאאאאאאאאFIRE

אWאאאאאא

א،אאאאאאאאאאK

אאאאW• אFKE • אK • K

אאאW• אאK • אK • K

אאWWאאW

١J 0.001 gאK ٢J 0.1 gאK ٣J אאא،אאאK ٤J אאאאא،

אK ٥J אאאאK ٦J אאא1000א kgK ٧J אאK ٨J אא،אאK ٩J אאאK

א٢٦٢ אאאאאF( אאא

- ٣٧ -

WאאאW١J אאאאאK ٢J אאאאK ٣J ،אאאאא

אKאW

אאW• אאאאאאK • אK

א٢٦٢ אאאאאF( אאא

- ٣٨ -

אאF١EאאW

F١EJאאאאאKF٢EJאאאאאאKF٣EJKF٤EJאאאεKF٥EJλmaxKF٦EJאאאKF٧EJאאאאאאאKF٨EJאאאאFCoSO4.7H2OEא

אF1.0 g/lE100 mlKF٩EJF2.0 g/lE100 ml

F10 g/lKEF١٠EJאאאא

F100 p.p.mE100 mlK

א٢٦٢ אאאאאF( אאא

- ٣٩ -

אאF٢EW

F١EJאאPH=3.5אאKF٢EJאאאKF٣EJאאאאאאKF٤EJאאאאאKF٥EJאאאאKBrאאאKF٦EJאאאאאאKF٧EJאאאאאKF٨EJ١،١٠אאK

א٢٦٢ אאאאאF( אאא

- ٤٠ -

אאF٣EאאאW

F١EJWKMKAKT%KE

F٢EJאWKµgKKnmKmg

F٣EJאאλWKµgKngKnmKmg

F٤EJאאאWKאpHאKאKאאKא

F٥EJאאאאאאWKאKאKאאKא

F٦EJאאאWKאKKKK

F٧EJ1 p.p.mWK1 g/lK1 µg/lK1 ng/mlK1 µg/ml

F٨EJא150 p.p.m15 p.p.m50 mlאאW

K500 mlK0.2 mlK5 mlK45 mlF٩EJ0.01א،0.61،אεW

K0.0061K0.061K6.1K61F١٠EJ1 mole/lFEאאא23W

K23 p.p.mK230 p.p.mK2300 p.p.mK23000 p.p.m

א٢٦٢ אאאאאF( אאא

- ٤١ -

אאאF١EF١EJKאKאKאKאKF٢EJאאאאF380-780 nmE

אאאאF200-380 nmEF٣EJאאאKF٤EJ

CA=εK

F٥EJאאאKF٦EJאאא،KF٧EJא،אאאאא

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א٢٦٢ אאאאאF( אאא

- ٤٢ -

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- ٥٢ -

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- ٥٥ -

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- ٥٧ -

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- ٥٩ -

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F١EJאאאאאאאKF٢EJאאאאאKF٣EJאאאאאKF٤EJאאאאאKF٥EJאWאאאאKF٦EJאאאאאאאKF٧EJאאאאKF٨EJ1.0 mlאאWNa, K, Alאאא

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א٢٦٢אאאאאFEאאא

- ٦١ -

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00.20.40.60.8

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p.p.m

א٢٦٢אאאאאFEאאא

- ٦٢ -

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- ٦٣ -

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F١٠EJאאא0.6אא1200 p.p.mא

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K360 p.p.mK1440 p.p.m

K4000 p.p.m

א٢٦٢אאאאאFEאאא

- ٦٤ -

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1000

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- ٦٥ -

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- ٦٦ -

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- ٦٧ -

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- ٦٨ -

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٢٠. אאאאאK

WאאאW١. אאאאK ٢. אאאאאK ٣. א،אא،אאאK ٤. אא،אאאאא،אא

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אאK

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- ٦٩ -

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1) Gary D. Chritian, Analytical Chemistry, fifth edition, John Willy & sons, Inc, 1986.

2) G.W. Ewing, Instrumental methods of Chemical Analysis, Fourth edition, McGraw-Hill, New York, 1975.

3) A.I. Vogel, Textbook of Quantitative chemical Analysis, fifth edition, Longman,

London 1975.

4) J.S. Fritz & G.H. Schenk, Quantitative Chemistry, Fourth edition, Allyn Bacon, Boston, 1979.

5) D.A. Skoog & D.M. West, Principles of Instrumental Methods of Analysis, sixth

edition, Holf Rinehart & Wiston, New York, 1991.

6) PAVIA & LAMPMAN, Introduction to spectroscopy, Saunders College Publishing.

٧E אKKאאKאאK،אאKאאאא،א،אא

א،١٩٨٦K

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