Tugas Analisa Instrumen

Disusun oleh

Nama : Erlin Febriyanti

NIM : 1111102000069
Farmasi 5-C
SILVERSTEN

HAL 41-44
 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

134
29
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
118
76
61
14 15 13 29
Ket:
FM : 43
Base peak

FM : 29 FM : 15 Struktur :
C2H5 CHO CH3 H
-O
FM : 13 FM : 14
CH CH2
 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

Ar F : 19
Cl : 35
Br : 79
I : 127
127 29
79

35 29
Ket:
Compound C Compound E
FM : 29 Struktur : C2H5 - I FM : 79 Struktur:
C2H5 CHO C6H5 + 2H, Br - Br

FM : 127 I FM : 91

Compound D
FM : 35 Cl

FM : 91

Compound F
- Cl
FM : 29 Struktur:
C2H5 CHO H

FM : 79
C6H5 + 2H, Br
 2.9

The compound represented by an electron-

impact spectrum and a chemical-ionization
(methane) spectrum is an ester of a long-
chain, aliphatic alcohol. Interpret the spectra
and identify the compound
BM = 125
125 111 = 14 CH2
111 97 = 14 CH2
97 83 = 14 CH2
83 69 = 14 CH2
69 55 = 14 CH2
55 43 = 12 C
Problem 2.9 (CI Metana) BM = 229
229 199 = 30 CH2NH2,
NO
199 185 = 14 CH2
185 169 = 16 O
169 127 = 42 C3H6,
C2H2O
127 113 = 14 CH2
113 99 = 14 CH2
99 85 = 14 CH2
85 71 = 14 CH2

Rumus molekul
 m/z = 229
85 C5H9O
229-199 = 30 CH2O
199-185 = 14 CH2
185-169 = 16 CH4
169 127 = 42 C2H2O
127 113 = 14 CH2
113 99 = 14 CH2
99 85 = 14 CH2
85 71 = 14 CH2
Molecular formula = C13H25O3
SILVERSTEN

HAL 111
 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 b. 3380 (m) : NH2 primer
2230 (s) : C N 3300 (m) : NH2
1450 (s) : C = C 2980 (s) : C H stretch
760 (s) : C H 2870 (m): C H stretch
688 (s) : C H, bend 1610 (m):
(alkena) 900 to 700

Jawaban : Benzonitrile Jawaban : Isobutylamine

c. 3080 (w) : C=H (alkena) d. 2955 (s) = CH alkena
1315 (s) : sulfone 2850 (s) = CH alkena
1300 (s) : sulfone 1120 (s) = CO
1155 (s) : S=O

Jawaban : Diphenyl Jawaban : Dioxane

sulfone
e. 2946 (s) : C-H alkana f. 2900 (b,s) : C-H (alkana)
2930 (m) : C-H 1720 (b,s) : ester
1550 (s) : NO2
1386 (m) : NO2

Jawaban : I-Nitropropane Jawaban : Formic acid

g. 3030 (m) = C-H (alkuna) h. 3200-2400 (s) : H
730 (s) = aromatik 1685 (b,s) : C = O
690 (s) = aromatik 705 (s) : aromatik

Jawaban : Biphenyl 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
 CC
2250-2100
C-C alkene
(w)
3100-3000
C=C 1600 dan Mono
1475 (m-w) substitusi

Senyawa: diphenylacetylene
 Siklo 3100-2990

Senyawa: 1,3-cyclohexadiene
 C-C

C-H

alkena

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) CO
C=O

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
 Amine primer C-H alkana
C-N (amine)

Isobutylamine
 3.5
Spectra J-M
Allyl pheny ether
Benzaldehyde
O-cresol
M-toluic acid
 OH
C=O 1700 AN
C-H C=C
aromatik

M-toluic acid
 ORTO

CH

ORTO
C=C C-O

O-cresol
 MONO

CH Mono
C=C AROMATIK C-o sidoop

Allyl phenyl ether

 C-H
C-H
aldehida
C=C
aromatik Mono substitusi

C=O

Benzaldehid
 3.6
Spectra N-R
Aniline
Azobenzene
Benzophenone oxime
Benzylamine
Dimethylamine hydrochloride
 C-N
Amin
primer C-H 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-N

Mono
C=C substitusi

Aniline
 3.7

Deduce the structure of a compound (S)

whose formula is C2H3NS from the
spectrum below
 Rumus Struktur CH3-N=CS

S M

Alkana

CH3
CNS di 2125
 3.8

Point out evidence for enol formation of 2,4-

pentane-dione (Compound T). Include
explanations of the two bands in the 1700-
1750 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)
 C-C-C
C-H stretch C=O C=O CH3
O
WILLARD

HAL 225
 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
 Emission reading

Concentration (g/ml) NaO KO

100 100 100

75 87 80

50 69 58

25 46 33

10 22 15

0 3 0

Cement A 28 69

Cement B 58 51

Cement C 42 63
 Jawaban

g/ml NaO KO (NO) - (NO) (KO) - (KO) x x-x

100 100 100 54, 5 45, 5 47,667 52,333 43,333 56,667
75 87 80 32, 5 32,333 31,667
50 69 58 14, 5 10,333 6,667
25 46 33 -8, 5 -14,667 -18,333
10 22 15 -32, 5 -32,667 -33,333
0 3 0 -51, 5 -47,667 -43,333
 (x- ) (-) NaO (x- ) (-) KO (x- ) Konsentrasi
2578,3485 2965, 5541 3211,1489
1029,1775 1023,8891 1002,7989
96,6715 68,8901 44,4489
155,8305 268,8901 336,0989
1083,3225 1088,8891 1111,0889
2231,6495 2065, 5541 1877,7489
= 7175 = 7481,6664 = 7583,3334

*NaO+

b= =

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

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

14,5017 = 0,9462x

x= %=

%= *KO+
b= =
B: 58= 13,4983 + 0,9462x
44, 5017= 0,9462x y= a+bx
47,667= a+ 0,9866 (43,333)
x= 47,667= a+ 42,7523
a= 47,667 42,752
a= 4,915
%=
y= a+bx C: 63= 4,915 + 0,9866x
y= 4,915 + 0,9866x 58,085= 0,9866x

A: 69= 4,915 + 0,9866x

x=
64,085 = 0,9866x %=
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:
 Emission Reading
Boron present g/ml 518-nm peak 505-nm minimum
0 36 33
50 44 36
100 52 39
150 60, 5 42, 5
200 68, 5 45, 5
What are the concentrations of boron in these unknows?
A 45 36, 5
B 85 65
C 66 50
 Persamaan regresi 518 nm
a = 35,9 b = 0,163 r = 0,829
y = 35,9 + 0,163x
Persamaan regresi 505 nm
a = 32,9 b = 0,063 r = 0,6556
y = 32,9 + 0,063x
 A pada 518 nm A pada 505 nm
y = 35,9 + 0,163x y = 32,9 + 0,063x
45 = 35,9 + 0,163x 36,5 = 32,9 + 0,063x
45 35,9 = 0,163x 36,5 32,9= 0,063x
9,1 = 0,163x 3,6 = 0,063x
x = 55,83 ppm x = 57,14 ppm
 B pada 518 nm B pada 505 nm
y = 35,9 + 0,163x y = 32,9 + 0,063x
85 = 35,9 + 0,163x 65 = 32,9 + 0,063x
85 35,9 = 0,163x 65 32,9 = 0,063x
49,1 = 0,163x 32,1 = 0,063x
x = 301,23 ppm x = 509,52 ppm
 C pada 518 nm C pada 505 nm
y = 35,9 + 0,163x y = 32,9 + 0,063x
66 = 35,9 + 0,163x 50 = 32,9 + 0,063x
66 35,9 = 0,163x 50 32,9 = 0,063x
30,1 = 0,163x 17,1 = 0,063x
x = 184,66 ppm x = 271,43 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 13
0,25 2 18, 5
0, 5 6 24
1,0 16 36
2, 5 44 70
5,0 94 125
7, 5 150 181
10,0 200 238