Analisa Instrumen

Arumpuspa Azizah NIM : 1111102000060 Farmasi 5C

2.5
Consider the mass spectra below of two isomers (A and B) of molecular formula C10H14. Determine their structures and explain the major spectral features for each.

105

29

134

Ket: FM : 105 Base peak

FM : 29 C2H5 CHO Struktur :

91

134
14 29

Ket: FM : 91 Base peak

FM : 29 C2H5 CHO

FM : 14 CH2

Struktur :

2.6
The mass spectrum of o-nitrotoluene shows a substantial peak at m/z 120. similar analysis of ,,-tri-deutero-o-nitrotoluene does not give a peak at m/z 120 but rather at m/z 122. explain

2.7
Determine the structure for the mass spectrum shown below

43 89 47 61
14 15

76
13 29

118

Ket: FM : 43 Base peak

FM : 29 C2H5 CHO FM : 13 CH

FM : 15 CH3 FM : 14 CH2

Struktur :
H -O

2.8
Below find mass spectra for compounds C-F. Compound C has an M + 1 peak that is 2,5% of M (where M=100%). Compound F can easily be converted to compounds D and E. Compounds C-E each give precipitate from D is white, the other two are yellow. Deduce the structures of C-F

127

29

79

35

29

Ket: Compound C FM : 29 C2H5 CHO FM : 127 Compound D FM : 35 Cl FM : 91

Struktur : C2H5 - I I

Compound E FM : 79 C6H5 + 2H, Br FM : 91

Struktur:
- Br

- Cl

Compound F FM : 29 C2H5 CHO

Struktur: H

FM : 79 C6H5 + 2H, Br

2.9
The compound represented by an electronimpact spectrum and a chemical-ionization (methane) spectrum is an ester of a longchain, aliphatic alcohol. Interpret the spectra and identify the compound

3.2
Select a compound that best fits each of the following sets of IR bands (in cm-1). Each set corresponds to a list of just a few important bands for each compound. Benzamide Diphenyl sulfone Benzoic acid Formic acid Benzonitrile Isobutylamine Biphenyl 1-Nitroproppone Dioxane a. 3080 (w), nothing 3000-2800, 2230 (s), 1450 (s), 760 (s), 688 (s) b. 3380 (m), 3300 (m), nothing 3200-3000, 2980 (s), 2870 (m), 1610 (m), ~900 to ~700 (b) c. 3080 (w), nothing 3000-2800, 1315 (s), 1300 (s), 1155 (s) d. 2955 (s), 2850 (s), 1120 (s) e. 2946 (s), 2930 (m), 1550 (s), 1386 (s) f. 2900 (b,s), 1720 (b,s) g. 3030 (m), 730 (s), 690 (s) h. 3200-2400 (s), 1685 (b,s), 705 (s) i. 3350 (s), 3060 (m), 1635 (s) S=strong, m=medium, w=weak, b=broad

a. 3080 (w) : aromatik 2230 (s) : C N 1450 (s) : C = C 760 (s) : C H 688 (s) : C H, bend (alkena)

b. 3380 (m) : NH2 primer 3300 (m) : NH2 2980 (s) : C H stretch 2870 (m): C H stretch 1610 (m): 900 to 700 Jawaban : Isobutylamine

Jawaban : Benzonitrile

c. 3080 (w) : C=H (alkena) 1315 (s) : sulfone 1300 (s) : sulfone 1155 (s) : S=O Jawaban : Diphenyl sulfone

d. 2955 (s) = CH alkena 2850 (s) = CH alkena 1120 (s) = CO

Jawaban : Dioxane

e. 2946 (s) : C-H alkana 2930 (m) : C-H 1550 (s) : NO2 1386 (m) : NO2

f. 2900 (b,s) : C-H (alkana) 1720 (b,s) : ester

Jawaban : I-Nitropropane

Jawaban : Formic acid

g. 3030 (m) = C-H (alkuna) 730 (s) = aromatik 690 (s) = Jawaban : Biphenyl

h. 3200-2400 (s) : H 1685 (b,s) : C = O 705 (s) : aromatik Jawaban : Benzoic acid

i. 3350 (s) : NH2 3060 (m) : C-H (alkena) 1635 (s) : C = O

Jawaban : Benzamide

3.3
Spectra A-D 1,3-Cyclohexadiene Diphenylacetylene 1-octene 2-pentene

C-C alkene 3100-3000

CC 2250-2100 (w) C=C 1600 dan 1475 (m-w)

Mono substitusi

Senyawa: diphenylacetylene

Siklo 3100-2990

Senyawa: 1,3-cyclohexadiene

C-C

C-H alkuna

2 pentene

C-H

C-C C-H

1 - oktene

3.4
Spectra E-I Butyl acetate Butyramide Isobutylamine Lauric acid Sodium propionate

CH Alkana (s)

C=O

CO

Senyawa Butylacetat

O-H (broad) -CH- bend C=O (s)

Senyawa: Lauric Acid

C-alkana

CH (1450 dan 1375)

C=O (s)

Senyawa: Sodium propionate

NH oop CN (1350-1000) (broad)

NH primer

C=O (1680-1630

Senyawa : Butyramide

1. Pada panjang gelombang 3500 3100 diperkirakan merupakan N-H 2. Diperkirakan pada panjang gelombang 2850 3000 merupakan C-H 3. Diperkirakan panjang gelombang 1465 merupakan CH2 Kesimpulan diperkirakan spektrum I merupakan isobutilamide

3.5
Spectra J-M Allyl pheny ether Benzaldehyde O-cresol M-toluic acid

OH C-H C=O 1700 AN C=C aromatik

M-toluic acid

ORTO

CH C=C C-O ORTO

O-cresol

MONO CH Mono sidoop

C=C AROMATIK

C-o

Allyl phenyl ether

C-H

C-H aldehida

C=C aromatik C=O

Mono substitusi

Benzaldehid

3.6
Spectra N-R Aniline Azobenzene Benzophenone oxime Benzylamine Dimethylamine hydrochloride

C-N Amin C-H primer C-C aromatik

Benzilamin

Mono substitusi

C=C aromatik

Mono substitusi

Azobenzen

OH C=C aromatik

Mono substitusi

Benzophenone oxime

Mono substitusi

N primer C=C

C-N Mono substitusi

Aniline

3.7
Deduce the structure of a compound (S) whose formula is C2H3NS from the spectrum below

Rumus Struktur CH3-N=CS

Alkana CH3 CNS di 2125

3.8
Point out evidence for enol formation of 2,4pentane-dione (Compound T). Include explanations of the two bands in the 17001750 cm-1 range, the 1650 band, and the very broad band with multiple maxima running from 3400 to 2600 cm-1 (only the peaks at 3000-2900 result from C-H stretching)

1
For the analysis of cement samples, a series of standards was prepared and the emission intensity for sodium and pottasium was measured at 590 and 768 nm, respectively. Each standard solution contained 6300 g/mL of calcium as CaO to compensate for the influence of calcium on the alkali readings. The result are shown in the table. For each cement sample 1000 g was dissolved in acid and diluted to exactly 100 mL. calculate the persent of Na2O and K2O Dalam tabel, setiap sampel semen 1.000 g dilarutkan dalam asam dan diencerkan hingga 100 ml. Hitung persentase dari Na2O dan K2O !!

Emission reading Concentration (g/ml) 100

75 50 25 10 0 Cement A Cement B Cement C

NaO 100
87 69 46 22 3 28 58 42

KO 100
80 58 33 15 0 69 51 63

Jawaban
g/ml 100 NaO 100 KO 100 (NO) - (NO) 54, 5 45, 5 (KO) 47,667 - (KO) 52,333 x 43,333 x-x 56,667

75
50 25 10 0

87
69 46 22 3

80
58 33 15 0

32, 5
14, 5 -8, 5 -32, 5 -51, 5

32,333
10,333 -14,667 -32,667 -47,667

31,667
6,667 -18,333 -33,333 -43,333

(x- ) (-) NaO 2578,3485 1029,1775 96,6715

(x- ) (-) KO 2965, 5541 1023,8891 68,8901

(x- ) Konsentrasi 3211,1489 1002,7989 44,4489

155,8305 1083,3225
2231,6495 = 7175 [NaO] b= =

268,8901 1088,8891
2065, 5541 = 7481,6664

336,0989 1111,0889
1877,7489 = 7583,3334

y = a+ bx 54, 5 = a + 0,9462 (43,333) 54, 5 = a + 41,0017 a = 54, 5 41,0017 = 13,4983

y= a+bx y= 13,4983 + 0,9462 x

A: 28= 13,4983 + 0,9462x 14,5017 = 0,9462x x=

C: 42= 13,4983 + 0,9462x 28,5017 = 0,9462x

x=

%= [KO] b= y= a+bx
47,667= a+ 0,9866 (43,333) 47,667= a+ 42,7523 a= 47,667 42,752 a= 4,915

%=
B: 58= 13,4983 + 0,9462x 44, 5017= 0,9462x x=

%=

y= a+bx y= 4,915 + 0,9866x A: 69= 4,915 + 0,9866x 64,085 = 0,9866x

C: 63= 4,915 + 0,9866x 58,085= 0,9866x

x= %=

x= %=
B: 51= 4,915 + 0,9866x 46,085 = 0,9866x

x= %=

2
In problem 1, what contributed to the emission reading of the blank at the analytical wavelength for sodium, but did not for potassium. A small quartz spectrometer was used to obtain the results. Would the blank reading be larger, smaller, or the same if a filter photometer equipped with glass absorption filters had been used.

3
Boron gives a series of fluctuation bands due to the radical BO2 that lie in the green portion of the spectrum. Although the overlapping band system present a problem in the measurement of the flame background, the minimum between adjacent band heads can be used. These results were obtained: Berapa konsentrasi boron (BO2) dalam sampel unknown???

Emission Reading Boron present g/ml 0 518-nm peak 36 505-nm minimum 33

50
100 150 200 A B C

44
52 60, 5 68, 5 45 85 66

36
39 42, 5 45, 5 36, 5 65 50

What are the concentrations of boron in these unknows?

Kurva kalibrasi 518 nm

80 70 60 Absorbansi 50 40 30 20 10 0 0 50 100 150 200 250 konsentrasi y = 0.163x + 35.9 R = 0.9999 absorbansi 50 45 40 35 30 25 20 15 10 5 0 0

Kurva kalibrasi 505 nm

y = 0.063x + 32.9 R = 0.9992

50

100

150

200

250

konsentrasi

Boron dalam 518 nm

y = 0,163x + 35,9 x = (y 35,9): 0,163 x = (45-35,9): 0,163 x = 9,1 : 0,163 = 55,828 ppm Sampel B (y = 85) y = 0,163x + 35,9 x = (y 35,9): 0,163 x = (85-35,9): 0,163 x = 49,1 : 0,163 = 301,227 ppm Sampel C (y = 66) y = 0,163x + 35,9 Sampel A (y = 45) x = (y 35,9): 0,163 x = (66-35,9): 0,163 x = 30,1 : 0,163 = 184,663 ppm Sampel A (y = 36,5) y = 0,063x + 32,9 x = (y 32,9): 0,063 x = (36,5-32,9): 0,063 x = 3,6 : 0,063 = 57,143 ppm Sampel B (y = 65) y = 0,063x + 32,9 x = (y 32,9): 0,063 x = (65-32,9): 0,063 x = 32,1 : 0,063 = 509,524 ppm Sampel C (y = 50) y = 0,063x + 32,9 x = (y 32,9): 0,063 x = (50-32,9): 0,063 x = 17,1 : 0,063 = 271,429 ppm

4
A calibration curve for strontium, taken at 460,7 nm. Was obtained in the absence of added calcium. These results are shown in the table. (a) graph the calibration curve on rectilinear graph paper and alsoo on log-log paper. (b) what might be the cause of the upward curvature in the region of low concentrations on the rectilinear graph when calcium is absent? (c) why does the addition of calcium straighten the calibration curve and increase the net emission reading for strontium?

Emission Reading Strontium present (g/ml) No Calcium Calcium Added

0
0,25 0, 5 1,0 2, 5 5,0 7, 5 10,0

0
2 6 16 44 94 150 200

13
18, 5 24 36 70 125 181 238