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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
29
134
91
134
14 29
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
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 CE each give precipitate from D is white, the other two are yellow. Deduce the structures of C-F Ar F Cl Br I : 19 : 35 : 79 : 127
127
29
79
35
29
Struktur : C2H5 - I I
Struktur:
- Br
- Cl
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
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 Benzoic acid Benzonitrile Biphenyl 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) Diphenyl sulfone Formic acid Isobutylamine 1-Nitroproppone
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)
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
Jawaban : Dioxane
e. 2946 (s) : C-H alkana 2930 (m) : C-H 1550 (s) : NO2 1386 (m) : NO2
Jawaban : I-Nitropropane
g. 3030 (m) = C-H (alkuna) 730 (s) = aromatik 690 (s) = aromatik Jawaban : Biphenyl
h. 3200-2400 (s) : H 1685 (b,s) : C = O 705 (s) : aromatik Jawaban : Benzoic acid
Jawaban : Benzamide
3.3
Spectra A-D 1,3-Cyclohexadiene Diphenylacetylene 1-octene 2-pentene
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)
C=O
CO
Senyawa Butylacetat
C-alkana
C=O (s)
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
M-toluic acid
ORTO
O-cresol
C=C AROMATIK
C-o
C=O
Benzaldehid
3.6
Spectra N-R Aniline Azobenzene Benzophenone oxime Benzylamine Dimethylamine hydrochloride
Benzilamin
Azobenzen
OH C=C aromatik
Mono substitusi
Benzophenone oxime
Mono substitusi
N primer C=C
Aniline
3.7
Deduce the structure of a compound (S) whose formula is C2H3NS from the spectrum below
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)
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) 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 75 50 25 10 0 NaO 100 87 69 46 22 3 KO 100 80 58 33 15 0 (NO) - (NO) 54, 5 45, 5 32, 5 14, 5 -8, 5 -32, 5 -51, 5 (KO) 47,667 - (KO) 52,333 32,333 10,333 -14,667 -32,667 -47,667 x 43,333 x-x 56,667 31,667 6,667 -18,333 -33,333 -43,333
(x- ) (-) NaO 2578,3485 1029,1775 96,6715 155,8305 1083,3225 2231,6495 = 7175 *NaO+ b= =
(x- ) (-) KO 2965, 5541 1023,8891 68,8901 268,8901 1088,8891 2065, 5541 = 7481,6664
%= *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=
%=
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:
Emission Reading Boron present g/ml 0 50 100 150 200 A B C 518-nm peak 36 44 52 60, 5 68, 5 45 85 66 505-nm minimum 33 36 39 42, 5 45, 5 36, 5 65 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
y 45 45 35,9 9,1 x = 35,9 + 0,163x = 35,9 + 0,163x = 0,163x = 0,163x = 55,83 ppm
A pada 505 nm
y = 32,9 + 0,063x 36,5 = 32,9 + 0,063x 36,5 32,9= 0,063x 3,6 = 0,063x x = 57,14 ppm
B pada 518 nm
y 85 85 35,9 49,1 x = 35,9 + 0,163x = 35,9 + 0,163x = 0,163x = 0,163x = 301,23 ppm
B pada 505 nm
y 65 65 32,9 32,1 x = 32,9 + 0,063x = 32,9 + 0,063x = 0,063x = 0,063x = 509,52 ppm
C pada 518 nm
y 66 66 35,9 30,1 x = 35,9 + 0,163x = 35,9 + 0,163x = 0,163x = 0,163x = 184,66 ppm
C pada 505 nm
y 50 50 32,9 17,1 x = 32,9 + 0,063x = 32,9 + 0,063x = 0,063x = 0,063x = 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) 0 0,25 0, 5 1,0 2, 5 5,0 7, 5 10,0 No Calcium 0 2 6 16 44 94 150 200 Calcium Added 13 18, 5 24 36 70 125 181 238