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Praktikum Kimia Analisis Instrumen

HALAMAN PENGESAHAN

Laporan lengkap praktikum Kimia Analisis Instrumen dengan judul


Spektroskopi Serapan dalam Daerah Tampak disusun oleh :
nama : Maryella Oktafrilly Lethe
nim : 1413442003
kelas : ICP A
kelompok : V
telah diperiksa dan dikoreksi oleh asisten dan koordinator asisten, maka dinyatakan
diterima.

Makassar, Desember 2016


Koordinator Asisten Asisten

Anwar Muh. Resky Yusuf

Mengetahui,
Dosen Penanggung Jawab

Maryono, S.Si., Apt., M.Si., MM


NIP. 19760307 200501 2 002

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A. TITLE OF EXPERIMENT
Absorption Spectroscopy Visible

B. OBECTIVES
At the end of the experiment, students are expected to:
1. Know the basics spectrophotometry and ways to operate spectrophotometer.
2. Determining the content of Cr (III) and Co (II) in the mixture using a spektronik 20.

C. PREVIEW OF LITERATURE
Spectroscopy is generally considered to have begun in 1666, with the
invention of Newton in the form of the solar spectrum / sun. Wollaston repeated the
experiments of Newton and in 1802 reported that the solar spectrum is intersected by
a number of dark lines. Fraunhofer lines investigate further and in 1823, Fraunhofer
was able to determine the wavelength. The initial discovery has been noticed that the
color delivered to the fire diffusion of alcohol by metal salts. However, more studies
about these colors is done on the development of water-gas flame coal mixed by
Bunsen. In 1859, Kirchhoff showed that these colors appear on the line spectra for
elements and not because the compound. He also showed that the wavelength they
relate to those of the Fraunhofer lines. Kirchhoff and Fraunhofer have observed each
atomic emission and atomic absorption (Ebdon, 1998: 1).
In the spectrophotometric analysis of the radiation source used that extends
into the ultraviolet region of the spectrum. From this, a definite wavelength of
radiation to the selected wavelength of less than 1 nm. This process requires the use
of more complex and consequently more expensive instruments. The instrument used
for this purpose is a spectrophotometer. Optical spectrometer is an instrument that
has an optical system that can produce a dispersion of the incident electromagnetic
radiation, and with measurements that can be made of the quantity of transmitted
radiation at wavelengths of the operator spectral range. A photometer is an
instrument for measuring the intensity of the transmitted radiation or function of this
quantity. When combined in a spectrophotometer, the spectrometers and photometer
employed together to produce a signal corresponding to the difference between the
transmitted radiation of reference materials and samples at selected wavelengths of
the tools (Jeffery, 1989: 645).
The tools used to measure the intensity of light absorbed by the atom or
molecule called a spectrophotometer. Type spectrophotometer available vary,
depending on the wavelength of light used, either a single light beam or sample and
comparison sexara file separately, and determine measurements made at a fixed
wavelength or scanning the spectrum at various wavelengths. Such as a major
analytical tool, accuracy, and cost is very varied presisis (Cairns, 2008: 155).
Spectrophotometer single-beam or double-beam, and instruments that
operate in different regions of the spectrum, all have critical components. According
to Underwood (2008: 397) As for the components of the spectrophotometer is as
follows:
1. The light source
The energy source of radiation is normal to the visible region (of) the spectrum and
near ultraviolet region to the near infrared is an incandescent bulb with a tungsten

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wire hair. Tungsten lamp output in regular operating conditions adequate from about
325 or 350 nm to about 3m.
2. The monochromator
Monochromator is an optical device for isolating a beam of radiation from a
sustainable source that has high spectral purity and a specific wavelength in the form
of a prism or diffraction grating.
3. Cells
Cells work to put fluid into the light beam spectrophotometer. Cells must be able to
pass the energy radiation in the spectral region of interest; so the glass cell airport
area looked, cell quartz or high silica glass special to the ultraviolet region.
4. Detectors
The detector should be at a high sensitivity in the spectral region of interest, linear
response to the radiation power, fast response time, it can be duplicated and high
stability. The detector converts the energy of incoming light into electrical energy to
be recorded or read.
The maximum wavelength ( max) is the wavelength where there is
electronic excitation which gives maximum absorbance. The reason was measured at
a wavelength of maximum absorbance change for each unit of concentration is
greatest at maximum wavelength, so that would be obtained the maximum sensitivity
of the analysis. If auxochrome attached to the chromophore group will result in a
shift in the absorbance band headed to larger wavelengths (bathochromic shift) is
accompanied by an increase in the intensity of wavelength (hyperchromic) thats all
make effect. (Tulandi, 2015: 171-172).
Measured at the maximum wavelength range of 230-350 nm. Results
showed that the maximum wavelength raw raw ketoprofen and ketoprofen in the
matrix is located at a wavelength of 255.4 nm and 255.0 nm. Based on the data
precision determination shows that ultraviolet-visible spectrophotometry method has
good accuracy, it can be seen from the price coefficient of variation (CV) of less than
2% in the amount of 0.38% (Noviyanto, 2014: 5-7).
Beer's law, groove absorbance against concentration, or log% T to
concentration groove known as Beer's law. To create a graph measured absobans
series of solution with a known concentration. Thick cell and the wavelength used is
taken anyway. If obtained a straight groove, means that the solution (and tools) to
follow the law of Lambert-Beer at the wavelength used, then this channel can be
used to determine the concentration of a solution. One of the requirements of law
Beer is light that used to be monochromatic. Therefore, at the same time some
wavelengths pass through the solution, it seems to Beer's law is not followed and
obtained groove is not straight (curved). To that end, the goal at the beginning of
most analyzes of optical wavelengths is seeking to produce legal channel Beer
straight or curved slightly once (Tim Lecturer, 2016: 7).
Chromium 0.5% can be determined by colorimetry in alkaline solution as
chromate; uranium and cerium can be annoying, but vanadium has only a small
influence. Transmittance of the solution is measured at 365-370 nm or with the aid of
filters that have a maximum transmission in the violet portion of the spectrum.
Standard solution used for the preparation of reference curve must have the same
alkalinity as the sample solution, and should have the same concentration of foreign

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salt. Standard solution can be made of potassium chromate for testing to be


performed (Jeffery, 1989: 686-687).

D. TOOLS AND CHEMICALS


1. Tools
a. Spectronic-20D 1 buah
b. Cuvet 3 buah
c. Measure Pumpkin 25 ml 9 buah
d. Volumetric Pipette 5 mL 1 buah
e. Volumetric Pipette 10 mL 1 buah
f. Volumetric Pipette 20 mL 1 buah
g. Beaker Glass 100 mL 2 buah
h. Beaker Glass 50 mL 5 buah
i. Ball pipette 1 buah
j. Drop pipette 3 buah
k. Spray Bottle 1 buah
l. Stirrer Bar 1 buah
2. Chemicals
a. Chromium (III) Nitrate Solution (Cr(NO3)3) 0,0500 M
b. Cobalt (II) Nitrate Solution (Co(NO3)2) 0,1880 M
c. Aquadest (H2O)
d. Tissue
e. Aluminium foil

D. WORK PROCEDURE
1. How To Operated Tools
Spektronik-20 is connected to a power source.
b. Spektronik-20 ignited by turning the knob left front until the number on the
monitor shows 0% T and instruments is heated for 20 minutes.
c. Shifting the filter on the appliance in accordance with the wavelength to be used.
d. The desired wavelengths set by turning a knob top.
e. Knop left part is rotated counter-clockwise until it shows 0% T.
f. 1 cuvette containing distilled water as a reference solution is cleaned with a tissue
and then inserted into the sample holder and then closed.
g. Knop left rotated clockwise as much as possible until the monitor shows 100% T.
h. 1 removed from the cuvette sample holder is then inserted cuvette containing
standard solution 2 which had been cleaned with a tissue, then closed.
i. % T solution is read and recorded.
j. Cuvette 2 removed then 100% T zeroed.
k. 1 a clean cuvette is put back into the sample holder, the knob is rotated up to 100%
T and ejected.
l. 3 cuvette containing standard solution more cleaned and then inserted into the
sample holder.
m. % T solution is read and recorded.

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2. Preparation of Standar Solution


a. Standard solution of Cr (III) was prepared at a concentration of 0.0100
respectively; 0.0200; 0.0300; and 0.0400 M by taking the mother liquor Cr (NO3)
3 0:05 M respectively 5, 15, 20 mL in 25 mL flask were then diluted to mark
boundaries. Then covered with aluminum foil.
b. Solution of Co (II) was prepared at a concentration of 0.0376 respectively; 0.0752;
0.1128; and 0.1540 M by taking the mother liquor Co (NO3) 2 0.1880 M
respectively 5, 10, 15, and 20 mL of the mother liquor into a 25 mL flask and
diluted to mark the boundary. Then covered with aluminum foil.
3. Optimization of Maximum Wavelength
a. Solution of Cr (III) with the highest concentration of 0.0400 M that have been
made previously to be puted into a clean cuvette.
b. Solution of Co (II) with the highest concentration of 0.1540 M that have been
made previously to be puted into a clean cuvette.
c. Cuvette 1 is filled with distilled water as a blank.
d. Insert the sample into the sample holder interchangeably with blanks.
e. The maximum wavelength for a solution of Cr (III) and Co (II) set at the
measurement wavelength range from 340-610 nm with an increase of 10 nm.
f. Record the% T that have been readed.
4. Calibration Curve
a. Standard solution of Cr (III) was prepared at a concentration of 0.0100
respectively; 0.0200; 0.0300; and 0.0400 M.
b. Standard solution of Co (II) was prepared at a concentration of 0.0376
respectively; 0.0752; 0.1128; and 0.1540 M.
c. Each sample is introduced into the cuvette interchangeably.
d. Wavelengths in the devices are set up to show 510 nm.
e. Samples and blanks are alternately inserted into the sample holder.
f. % T is legible note and calibration curves were made for the solution of Cr (III)
and Co (II)
5. Analysis Compound of Cr (III) and Co(II)
a. A mixture of Cr (III) -CO (II) was prepared by taking 10 mL solution of Cr (III)
and 10 mL of 0.0500 M Co (II) 0.1880 M from the mother liquor into each flask
25 mL. Then diluted to mark the boundary.
b. Samples were inserted into the cuvette clean.
c. Samples and blanks inserted into the sample holder alternately
d. Wavelength is set between 375 nm and 625 nm, with 25 nm spacing between each
observation and% T generated note.

E. OBSERATION RESULT
1. Making a solution
a. Preparation of Cr(NO3)3 solution
Known:
V2 Cr(NO3)3 = 25 ml
M1 Cr(NO3)3 = 0,0500 M
M2 = 0,01 M; 0,02 M; 0,03 M; 0,04 M
Asked:

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V1 = .....?
Answer:
1) M2 = 0,01 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,01 M
V1 = = = 5 mL
M1 0,05 M
2) M2 = 0,02 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,02 M
V1 = = = 10 mL
M1 0,05 M
3) M2 = 0,03 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,03 M
V1 = = = 15 mL
M1 0,05 M
4) M2 = 0,04 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,04 M
V1 = = = 20 mL
M1 0,05 M
b. Preparation of Co(NO3)2 solution
Known:
V2 Co(NO3)2 = 25 ml
M1 Co(NO3)2 = 0,1880 M
M2 = 0,0376 M; 0,0752 M; 0,1128 M; 0,1504 M
Asked:
V1 = .....?
Answer:
1) M2 = 0,0376 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,0376 M
V1 = = = 5 mL
M1 0,1880 M
2) M2 = 0,0752 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,0752 M
V1 = = = 10 mL
M1 0,1880 M
3) M2 = 0,1128 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,1128 M
V1 = = = 15 mL
M1 0,1880 M
4) M2 = 0,1504 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,1504 M
V1 = = = 20 mL
M1 0,1880 M

2. Optimization of Maximum Wavelength


Cr(III) Co(II)
No. (nm) %T A %T A
1. 340 26,6 0,5751 27,6 0,5590
2. 350 27,4 0,5622 28,0 0,5528
3. 360 27,8 0,5559 29,2 0,5346
4. 370 29,0 0,5376 31,4 0,5030

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5. 380 30,6 0,5142 36,2 0,4412


6. 390 32,8 0,4841 44,4 0,3526
7. 400 35,6 0,4485 57,6 0,2395
8. 410 39,2 0,4067 74,0 0,1307
9. 420 41,4 0,3829 81,8 0,0872
10. 430 42,6 0,3705 78,6 0,1045
11. 440 45,8 0,3391 71,8 0,1438
12. 450 50,6 0,2958 65,4 0,1844
13. 460 53,0 0,2757 57,4 0,2410
14. 470 60,8 0,2160 50,6 0,2958
15. 480 65,2 0,1857 46,8 0,3297
16. 490 66,8 0,1752 42,6 0,3705
17. 500 65,8 0,1817 26,4 0,5783
18. 510 26,4 0,5783 63,2 0,1992
19. 520 61,2 0,2132 38,6 0,4179
20. 530 59,0 0,2291 40,6 0,3914
21. 540 55,0 0,2696 44,6 0,3506
22. 550 51,6 0,2873 49,6 0,3045
23. 560 48,2 0,3169 59,8 0,2232
24. 570 47,6 0,3223 47,6 0,3223
25. 580 44,8 0,3487 74,6 0,1272
26. 590 45,4 0,3429 81,0 0,0915
27. 600 30,8 0,5114 85,6 0,0705
28. 610 51,8 0,2856 86,6 0,0624

3. Standar Curve
= 510 nm
a. Standar Curve of Cr(III) solution
No. Concentration (M) %T A
1. 0.04 53,6 0,2708
2. 0.03 56,8 0,2456
3. 0.02 60,8 0,2160
4. 0.01 66,0 0,1804

b. Standar Curve of Co(II) solution


No. Concentration (M) %T A
1. 0.1504 66,2 0,1791
2. 0.1128 68,2 0,1662
3. 0.0752 69,0 0,1611
4. 0.0376 73,2 0,1354

4. Observation Result of Cr(III) dan Co(II) compound


No. (nm) %T A
1. 375 29,8 0,5257
2. 400 39,2 0,4067

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3. 425 52,4 0,2806


4. 450 56,4 0,2487
5. 475 59,0 0,2291
6. 500 45,0 0,3467
7. 525 43,8 0,3585
8. 550 51,2 0,2907
9. 575 38,4 0,4156
10. 600 61,6 0,2104
11. 625 66,0 0,1804

G. DATA ANALYSIS
1. Making a Standard Solution
a. Making a solution of Cr(NO3)3
Known:
V2 Cr(NO3)3 = 25 ml
M1 Cr(NO3)3 = 0,0500 M
M2 = 0,01 M; 0,02 M; 0,03 M; 0,04 M
Asked:
V1 = .....?
Answer:
1) M2 = 0,01 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,01 M
V1 = = = 5 mL
M1 0,05 M
2) M2 = 0,02 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,02 M
V1 = = = 10 mL
M1 0,05 M
3) M2 = 0,03 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,03 M
V1 = = = 15 mL
M1 0,05 M
4) M2 = 0,04 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,04 M
V1 = = = 20 mL
M1 0,05 M
b. Making a solution of (NO3)2
Known:
V2 Co(NO3)2 = 25 ml
M1 Co(NO3)2 = 0,1880 M
M2 = 0,0376 M; 0,0752 M; 0,1128 M; 0,1504 M
Asked:
V1 = .....?
Answer:
1) M2 = 0,0376 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,0376 M
V1 = M1
= 0,1880 M
= 5 mL

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2) M2 = 0,0752 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,0752 M
V1 = = = 10 mL
M1 0,1880 M
3) M2 = 0,1128 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,1128 M
V1 = = = 15 mL
M1 0,1880 M
4) M2 = 0,1504 M
V1 x M1 = V2 x M2
V2 M 2 25 ml 0,1504 M
V1 = = = 20 mL
M1 0,1880 M
2. Optimiation of maximum wavelength (max)
a. Cr(III)
1. = 340 nm
%T = 26.6
T = 0.266
1 1
A1 = log T = log 0.266 = 0,5751
2. = 350 nm
%T = 27,4
T = 0.274
1 1
A2 = log T = log 0,274 = 0,5622
3. = 360 nm
%T = 27.8
T = 0.278
1 1
A3 = log T = log 0.278 = 0,5559
4. = 370 nm
%T = 29,0
T = 0,29
1 1
A4 = log T = log 0.29 = 0,5376
5. = 380 nm
%T = 30,6
T = 0,306
1 1
A5 = log T = log 0,306 = 0,5142
6. = 390 nm
%T = 32,8
T = 0,328
1 1
A6 = log T = log 0.328 = 0,4841
7. = 400 nm
%T = 35,6
T = 0,356
1 1
A7 = log T = log 0.356 = 0,4485
8. = 410 nm
%T = 39,2

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T = 0,392
1 1
A8 = log T = log 0,392 = 0,4067
9. = 420 nm
%T = 41,4
T = 0,414
1 1
A9 = log T = log 0,414 = 0,3829
10. = 430 nm
%T = 42,6
T = 0,426
1 1
A10 = log T = log 0,426 = 0,3705
11. = 440 nm
%T = 45,8
T = 0,458
1 1
A11 = log T = log 0,458 = 0,3391
12. = 450 nm
%T = 50,6
T = 0,506
1 1
A12 = log T = log 0,506 = 0,2958
13. = 460 nm
%T = 53,0
T = 0,53
1 1
A13 = log T = log 0,53 = 0,2757
14. = 470 nm
%T = 60,8
T = 0,608
1 1
A14 = log T = log 0,608 = 0,2160
15. = 480 nm
%T = 65,2
T = 0,652
1 1
A15 = log T = log 0,652 = 0,1857
16. = 490 nm
%T = 66,8
T = 0,668
1 1
A16 = log T = log 0,668 = 0,1752
17. = 500 nm
%T = 65,8
T = 0,658
1 1
A19 = log T = log 0,658 = 0,1817
18. = 510 nm
%T = 26,4
T = 0,264

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1 1
A18 = log T = log 0,264= 0,5783
19. = 520 nm
%T = 61,2
T = 0,612
1 1
A19 = log T = log 0,612 = 0,2132
20. = 530 nm
%T = 59,0
T = 0,59
1 1
A10 = log T = log 0,59 = 0,2291
21. = 540 nm
%T = 55,0
T = 0,55
1 1
A11 = log T = log 0,55 = 0,2696
22. = 550 nm
%T = 51,6
T = 0,516
1 1
A12 = log T = log 0,516 = 0,2873
23. = 560 nm
%T = 48,2
T = 0,482
1 1
A13 = log T = log 0,482 = 0,3169
24. = 570 nm
%T = 47,6
T = 0,476
1 1
A14 = log T = log 0,476 = 0,3223
25. = 580 nm
%T = 44,8
T = 0,448
1 1
A15 = log T = log 0,448 = 0,3487
26. = 590 nm
%T = 45,4
T = 0,454
1 1
A16 = log T = log 0,454 = 0,3429
27. = 600 nm
%T = 30,8
T = 0,308
1 1
A19 = log T = log 0,308 = 0,5114
28. = 610 nm
%T = 51,0
T = 0,51
1 1
A18 = log T = log 0,51= 0,2856

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b. Co-(II)
1. = 340 nm
%T = 27,6
T = 0,276
1 1
A1 = log T = log 0.276 = 0,5590
2. = 350 nm
%T = 28,0
T = 0,28
1 1
A2 = log T = log 0,28 = 0,5528
3. = 360 nm
%T = 29,2
T = 0,292
1 1
A3 = log T = log 0.292 = 0,5346
4. = 370 nm
%T = 31,4
T = 0,314
1 1
A4 = log T = log 0.314 = 0,5030
5. = 380 nm
%T = 36,2
T = 0,362
1 1
A5 = log T = log 0,362 = 0,4412
6. = 390 nm
%T = 44,4
T = 0,444
1 1
A6 = log T = log 0,444 = 0,3526
7. = 400 nm
%T = 57,6
T = 0,576
1 1
A7 = log T = log 0.576 = 0,2395
8. = 410 nm
%T = 74,0
T = 0,74
1 1
A8 = log T = log 0,74 = 0,1307
9. = 420 nm
%T = 81,8
T = 0,818
1 1
A9 = log T = log 0,818 = 0,0872
10. = 430 nm
%T = 78,6
T = 0,786
1 1
A10 = log T = log 0,786 = 0,1045
11. = 440 nm

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%T = 71,8
T = 0,718
1 1
A11 = log T = log 0,718 = 0,1438
12. = 450 nm
%T = 65,4
T = 0,654
1 1
A12 = log T = log 0,654 = 0,1844
13. = 460 nm
%T = 57,4
T = 0,574
1 1
A13 = log T = log 0,574 = 0,2410
14. = 470 nm
%T = 50,6
T = 0,506
1 1
A14 = log T = log 0,506 = 0,2958
15. = 480 nm
%T = 46,8
T = 0,468
1 1
A15 = log T = log 0,468 = 0,3297
16. = 490 nm
%T = 42,6
T = 0,426
1 1
A16 = log T = log 0,426 = 0,3705
17. = 500 nm
%T = 26,4
T = 0,264
1 1
A19 = log T = log 0,264 = 0,5783
18. = 510 nm
%T = 63,2
T = 0,632
1 1
A18 = log T = log 0,632= 0,1992
19. = 520 nm
%T = 38,6
T = 0,386
1 1
A19 = log T = log 0,386 = 0,4179
20. = 530 nm
%T = 40,6
T = 0,406
1 1
A10 = log = log = 0,3914
T 0,406
21. = 540 nm
%T = 44,6

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T = 0,446
1 1
A11 = log T = log 0,446 = 0,3506
22. = 550 nm
%T = 49,6
T = 0,496
1 1
A12 = log T = log 0,496 = 0,3045
23. = 560 nm
%T = 59,8
T = 0,598
1 1
A13 = log T = log 0,598 = 0,2232
24. = 570 nm
%T = 47,6
T = 0,476
1 1
A14 = log T = log 0,476 = 0,3223
25. = 580 nm
%T = 74,6
T = 0,746
1 1
A15 = log T = log 0,746 = 0,1272
26. = 590 nm
%T = 81,0
T = 0,81
1 1
A16 = log T = log 0,81 = 0,0915
27. = 600 nm
%T = 85,0
T = 0,85
1 1
A19 = log T = log 0,85 = 0,0705
28. = 610 nm
%T = 86,6
T = 0,866
1 1
A18 = log T = log 0,866= 0,0624

3. Standar Curve
= 510 nm
a. Standard Curve Cr(III)
1. Concentration of Cr(III) = 0.01
%T = 66,0
T = 0,66
1 1
A = log T = log 0,66 = 0,1804
2. Concentration of Cr(III) = 0.02

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%T = 60,8
T = 0,608
1 1
A = log T = log 0,608 = 0,2160
3. Concentration of Cr(III) = 0.03
%T = 56,8
T = 0,568
1 1
A = log T = log 0,568 = 0,2456
4. Concentration of Cr(III) = 0.04
%T = 53,6
T = 0,536
1 1
A = log T = log 0,536 = 0,2708
Tabel 1. Relation between Concentration and Adsorbance Cr(III)
No. Concentration (M) Absorbance
1 0,01 0,1804
2 0,02 0,2160
3 0,03 0,2456
4 0,04 0,2708

Standard Curve Solution Cr (III)


0.3

0.25

0.2
Absorbance

y = 3.008x + 0.153
0.15 R = 0.994
0.1

0.05

0
0 0.01 0.02 0.03 0.04 0.05
Concentration (M)

Grafik.1. Standard Curve Solution Cr(III)

b. Standard Curve of Co(II)


1. Concentration Co(II) = 0,0376
%T = 73,2
T = 0,732
1 1
A = log T = log 0,732 = 0,1354
2. Concentration Co(II) = 0,0752
%T = 69,0
T = 0,69
1 1
A = log T = log 0,69 = 0,1611
3. Concentration Co(II) = 0,1128

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%T = 68,2
T = 0,682
1 1
A = log T = log 0,682 = 0,1662
4. Concentration Co(II) = 0,1504
%T = 66,2
T = 0,662
1 1
A = log T = log 0,662 = 0,1791

Tabel 2. Relation between Concentration and Adsorbance Co(II)


No. Concentration (M) Absorbance
1 0,0376 0,1354
2 0,0752 0,1611
3 0,1128 0,1662
4 0,1504 0,1791

Standard Curve of Co(II)


0.2
0.18
0.16
0.14
Absorbance

0.12 y = 0.3622x + 0.1264


0.1 R = 0.9194
0.08
0.06
0.04
0.02
0
0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.16
Concentration (M)

Grafik.2. Standard Curve Solution Co(II)

4. Cr(III) dan Co(II) Compound


a. = 375 nm
%T = 29,8
T = 0,298
1 1
A = log T = log 0,298 = 0,5257
b. = 400 nm
%T = 39,2
T = 0,392
1 1
A = log T = log 0,392 = 0,4067
c. = 425 nm
%T = 52,4
T = 0,524

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1 1
A = log T = log 0,524 = 0,2806
d. = 450 nm
%T = 56,4
T = 0,564
1 1
A = log T = log 0,564 = 0,2487
e. = 475 nm
%T = 59,0
T = 0,59
1 1
A = log = log = 0,2291
T 0,59
f. = 500 nm
%T = 45,0
T = 0,45
1 1
A = log T = log 0,45 = 0,3467
g. = 525 nm
%T = 43,8
T = 0,438
1 1
A = log T = log 0,438 = 0,3585
h. = 550 nm
%T = 51,2
T = 0,512
1 1
A = log T = log 0,512 = 0,2907
i. = 575 nm
%T = 38,4
T = 0,384
1 1
A = log T = log 0.384 = 0,4156
j. = 600 nm
%T = 61,6
T = 0,616
1 1
A = log T = log 0,616 = 0,2104
k. = 625 nm
%T = 66,0
T = 0,66
1 1
A = log T = log 0,66 = 0,1804
Table 3. Wavelength variation in sample compound
No. (nm) %T A
1. 375 29,8 0,5257
2. 400 39,2 0,4067
3. 425 52,4 0,2806
4. 450 56,4 0,2487
5. 475 59,0 0,2291
6. 500 45,0 0,3467

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7. 525 43,8 0,3585


8. 550 51,2 0,2907
9. 575 38,4 0,4156
10. 600 61,6 0,2104
11. 625 66,0 0,1804

5. Concentration Compound of Cr(III) and Co(II) using regretion equation


a. Concentration of Cr(III) in compound
1) Known: y = 3,008x + 0,153
= 375 nm
A(y) = 0,5257
Asked : x = ....?
Answer:
y = 3,008x + 0,153
0,5257 = 3,008x + 0,153
3,008x = 0,153 0,5257
3,008x = 0,3727
x = 0,1239 M
2) Known: y = 3,008x + 0,153
= 400 nm
A(y) = 0,4067
Asked : x = ....?
Answer:
y = 3,008x + 0,153
0,4067 = 3,008x + 0,153
3,008x = 0,153 0,4067
3,008x = 0,2537
x = 0,0843 M
3) Compound: y = 3,008x + 0,153
= 425 nm
A(y) = 0,2806
Asked : x = ....?
Answer:
y = 3,008x + 0,153
0,2806 = 3,008x + 0,153
3,008x = 0,153 0,2806
3,008x = 0,1276
x = 0,0424 M
4) Known: y = 3,008x + 0,153
= 450 nm
A(y) = 0,2487
Asked : x = ....?
Answer:
y = 3,008x + 0,153
0,2487 = 3,008x + 0,153
3,008x = 0,153 0,2487

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3,008x = 0,0957
x = 0,0318 M

b. Concentration o Co(II) in compound


1) Known: y = 0, 362x + 0,126
= 375 nm
A(y) = 0,5257
Asked: x = ....?
Answer:
y = 0, 362x + 0,126
0,5257 = 0, 362x + 0,126
0,362x = 0,126 0,5257
0,362x = 0,3997
x = 1,1041 M
2) Known: y = 0, 362x + 0,126
= 400 nm
A(y) = 0,4067
Asked : x = ....?
Answer:
y = 0,362x + 0,126
0,4067 = 0,362x + 0,126
0,362x = 0,126 0,4067
0,362x = 0,2807
x = 0,7754 M
3) Known: y = 0,362x + 0,126
= 425 nm
A(y) = 0,2806
Asked: x = ....?
Answer:
y = 0,362x + 0,126
0,2806 = 0,362x + 0,126
0,362x = 0,126 0,2806
0,362x = 0,1546
x = 0,4271 M
4) Known: y = 0,362x + 0,126
= 450 nm
A(y) = 0,2487
Asked : x = ....?
Answer:
y = 0,362x + 0,126
0,2487 = 0,362x + 0,126
0,362x = 0,126 0,2487
0,362x = 0,1227
x = 0,3389 M

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H. DISSCUSSION
Spektroskopi adalah ilmu yang mempelajari interaksi cahaya dengan materi.
Spektrofotometri adalah suatu metode dalam kimia analisis yang digunakan untuk
mengukur konsentrasi sampel secara kuantitatif, berdasarkan interaksi materi dengan
cahaya. Spektrofotometer adalah suatu instrumen untuk mengukur transmitans atau
absorbansi suatu sampel pada suatu panjang gelombang tunggal (Underwood, 2001:
396). Percobaan ini bertujuan untuk mengenal dasar-dasar spektrofotometri serta
cara-cara mengoperasikan alat dan untuk menentukan kadar Cr3+ dan Co2+ dalam
sampel campuran menggunakan metode spektrofotometri Spektronik-20.
1. Cara pengoperasian Spektronik-20
Spektronik-20 adalah suatu alat yang mempunyai rentang panjang gelombang
dari 340 nm sampai 600 nm. Alat ini hanya dapat mengukur absorbansi larutan yang
berwarna (Jeffery, 1989: 646). Sumber cahaya alat ini berupa lampu tungsten yang
akan memancarkan sinar polikromatik. Setelah melewati pengatur panjang
gelombang, hanya sinar yang monokromatik dilewatkan ke larutan dan sinar yang
melewati larutan dideteksi oleh fotodetektor. Dalam spektronik-20 memiliki
komponen terpenting yaitu sumber cahaya yaitu lampu tungsten yang
berkesinambungan yang meliputi daerah sinar tampak (38075 nm), monokromator
yakni suatu komponen untuk menyeleksi pita panjang gelombang dari spektrum
lebar yang dipancarkan oleh sumber cahaya, kuvet dari kaca, detektor yang
mengubah energi cahaya menjadi energi listrik, sistem baca (skala absorbansi atau
%T dengan jarum penunjuk) yang menyatakan besarnya energi listrik (Underwood,
2001: 405). Prinsip dasar dari spektroskopi serapan dalam daerah tampak adalah jika
seberkas sinar dipancarkan dengan panjang gelombang tertentu dan mengenai larutan
sampel berwarna di dalam sebuah medium maka sinar tersebut akan diserap,
diteruskan, dan dipantulkan sesuai dengan konsentrasi larutan sampel. Prinsip kerja
dari spektronik-20 adalah interaksi antara valensi materi (elektron valensi) dengan
cahaya, dimana elektron memancarkan sinar yang polikromatis yang diubah menjadi
sinar monokromatis yang dilewatkan pada larutan. Kemudian, sinar yang telah
melewati suatu larutan akan dideteksi oleh detektor dan dilakukan pembacaan skala
(Khopkar, 1990: 194). Percobaan ini alat dinyalakan terlebih dahulu sekitar 20 menit
sebelum digunakan. Hal ini bertujuan untuk memanaskan alat agar alat dapat bekerja
maksimal pada proses pembacaan skala karena alat yang digunakan pada percobaan
ini tidak stabil. Kemudian mengatur 0%T yang berfungsi untuk mengembalikan
fungsi alat ke keadaan awal dan 100%T yang berfungsi untuk membaca nilai
transmitan yang akan diperoleh pada saat sampel dimasukkan kedalam sampel
holder. Aquades digunakan sebagai blangko yang digunakan untuk kalibrasi dan
bertujuan untuk menetralkan alat agar dapat diketahui bahwa alat bisa berfungsi
dengan baik. Selain itu, untuk menjamin tingkat ketelitian dalam pengukuran pada
alat.
2. Pembuatan Larutan Standar
Larutan standar yang digunakan pada percobaan ini adalah Cr(NO3)3,
Co(NO3)2. Sampel terlebih dahulu diencerkan dari larutan Cr(NO3)2 0,05M menjadi
0,01M; 0,02M; 0,03M; 0,04M, sedangkan Co(NO3)2 0,1880M menjadi 0,0376M;
0,0752M; 0,112M; 0,1128M; dan 0,1504M. Percobaan dilakukan pada konsentrasi
berbeda dimaksudkan untuk mengetahui pengaruh konsentrasi terhadap absorbansi

Spektroskopi Serapan dalam Daerah Tampak


Praktikum Kimia Analisis Instrumen

suatu zat. Selain itu panjang gelombang juga dibuat bervariasi agar dapat diketahui
pada panjang gelombang beberapa sampel dapat menyerap sinar sacara maksimal.
3. Optimasi Panjang Gelombang Maksimum
Percobaan ini bertujuan untuk mengetahui absorpsi suatu larutan telah
mencapai maksimum sehingga meningkatkan proses absorpsi larutan terhadap sinar
(Rohman 2007). Panjang gelombang maksimum digunakan dalam penentuan kurva
kalibrasi. Jika pemilihan panjang gelombang memiliki spektrum perubahan besar
pada nilai absorbansi saat panjang gelombang sempit, maka terjadi penyimpangan
kecil pada cahaya yang masuk dan akan mengakibatkan kesalahan besar dalam
pengukuran. Semakin besar panjang gelombangnya maka akan semakin kecil nilai
absorbansinya. Hal ini dapat diakibatkan sinar putih pada setiap panjang gelombang
dapat terseleksi lebih detail oleh prisma (Underwood 1990). Percobaan ini
menggunakan larutan standar yang paling tinggi konsentrasinya yaitu larutan Cr(NO-
3)3 0,04 M dan larutan Co(NO3)2 0,1504 M. Percobaan ini dilakukan pada panjang
gelombang 340 nm-610nm dengan jarak 10 nm. Sehingga diperoleh panjang
gelombang maksimum (max) dari masing-masing larutan. Panjang golombang
maksimum artinya panjang gelombang pada saat absorbansi paling tinggi. Sampel
Cr(III) dan Co(II) dimasukkan ke dalam kuvet dan diukur secara bergantian dengan
blangko. Dari percobaan ini diperoleh panjang golombang maksimum untuk Cr(III)
dan Co(II) adalah 510 nm (A=0,5783) dan 500 nm (A=0,5783). Hasil yang
didapatkan tidak sesuai dengan teori bahwa panjang gelombang maksimum untuk
Cr(III) adalah 357,9 nm dan Co(II) adalah 510 nm (Underwood, 2002: 392).
Perbedaan ini terjadi karena pada saat percobaan alat spektronik-20 yang digunakan
berada dalam keadaan tidak stabil saat pembacaan skala. Sehingga sangat sulit
dilakukan pembacaan skala yang tepat untuk setiap pengukuran nilai absorbansi
masing-masing panjang gelombang.
4. Kurva Kalibrasi
Percobaan ini bertujuan untuk membuat kurva standar dan mendapatkan nilai
regresi dari grafik yang telah dibuat untuk menentukan konsentrasi Cr3+ dan Co2+
dalam campuran. Kurva standar, yaitu hubungan antara konsentrasi terhadap
absorbansi larutan standar pada panjang gelombang tertentu. Interaksi yang terjadi
pada percobaan ini adalah interaksi antara materi dan energi. Energi dalam hal ini
adalah energi dari sinar visible yang kemudian dilewatkan pada suatu larutan sampel
yang mengandung Cr(III) atau Co(II) dengan konsentrasi tertentu. Untuk membuat
kurva, dilakukan pengukuran absorbansi terlebih dahulu dengan konsentrasi yang
telah diketahui. Jika diperoleh aluran grafik yang lurus, artinya larutan dan alatnya
mengikuti hukum Beer, maka aluran ini dapat dipakai untuk menetukan konsentrasi
Cr3+ dan Co2+ dalam sampel campuran (Tim Dosen, 2016: 7).
Berdasarkan hasil percobaan, pada panjang golombang 510 nm, larutan
standar Cr(NO3)3 0,01 M; 0,02 M; 0,03 M; dan 0,04 M diperoleh absorbansi secara
berturut-turut adalah 0,1804; 0,2160; 0,2456 dan 0,2708. Hal ini sesuai dengan teori,
pada kurva standar didapatkan nilai R2 sebesar 0,994, sedangkan pada larutan standar
Co(NO3)2 0,0376 M; 0,0752 M; 0,1128 M; dan 0,1504 M diperoleh absorbansi
secara berturut-turut adalah 0,1354; 0,1611; 0,1662 dan 0,1791. Hasil absorbansi
yang diperoleh pada larutan ini tidak sesuai dengan teori, karena alat yang

Spektroskopi Serapan dalam Daerah Tampak


Praktikum Kimia Analisis Instrumen

digunakan pembacaannya tidak stabil sehingga mempengaruhi pembacaan %T dan


berdasarkan grafik didaptkan nilai R2 sebesar 0,919.
5. Analisis campuran Cr(III) dan Co(II)
Percobaan ini pada prinsipnya sama dengan prosedur kerja pada langkah
pertama. Dalam percobaan ini larutan Cr(III) 0,05 M dengan larutan Co(II) 0,1880 M
dicampur dan diukur panjang golombang yang digunakan antara 375 625 nm
dengan jarak 25 nm. Tujuan dari percobaan ini adalah untuk mengetahui kadar Cr 3+
dan Co 2+ dalam campuran. Berdasarkan hasil perhitungan dan analisis data, pada
panjang gelombang 375 nm, 400 nm, 425 nm, 450 nm diperoleh konsentrasi Cr3+
menggunakan persamaan regresi y = 3,008x + 0,153 yang diperoleh dari grafik 1
yaitu 0,1239 M; 0,0843 M; 0,0424 M; 0,0318 M, sedangkan konsentrasi Co2+
menggunakan persamaan regresi y = 0,362x + 0,126 yang diperoleh dari grafik 2
adalah 1,1041 M; 0,7754 M; 0,4271 M; 0,3389 M. Kadar dari setiap logam yang
diperoleh tidak termasuk dalam lingkup kurva kalibrasi hal ini dikarenakan
pengukuran tidak dilakukan pada rentang panjang gelombang maksimum.

F. CONCLUSION AND SUGESSTION


1. Conclusion
From the experimental results, we can conclude that:
a. Spektronik-20 is an instrument used to measure the intensity of light at specific
wavelengths solution. The working principle spektronik-20 is a white light
emitted by a tungsten lamp is passed through the entrance slit and dispersed by a
diffraction grating or prism tape. Narrow wavelength bands (ideally
monochromatic) rays that difraksikan through the second slit is passed into the
sample being measured. Rays that are not absorbed by the sample solution but
passes through a solution, until the phototube of instruments then measure the
intensity of light that is transmitted electronically by the detector.
b. At a wavelength of 375 nm, 400nm, 425 nm, 450 nm is obtained Cr(III)
concentration using the regression equation y = 3,008x + 0,153 obtained from
chart 1 that is 0.1239 M; 0.0843 M; 0.0424 M; 0.0318 M, whereas the
concentration of Co(II) using a regression equation y = 0,362x + 0.126 obtained
from chart 2 is 1.1041 M; 0.7754 M; 0.4271 M; 0.3389 M. levels of each metal
obtained does not fall within the scope of calibration curve this is because the
measurement is not carried out in the wavelength range maximum
2. Sugesstion
It is expected that the next practitioner to use the tools in accordance with
how it works and is expected to use the tool carefully to avoid damage to the
appliance.

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Praktikum Kimia Analisis Instrumen

BIBLIGRAPHY

Cairns, Donald. 2008. Intisari Kimia Farmasi Edisi 2. Jakarta: Penerbit Buku
Kedokteran EGC.

Ebdon, L., E. H. Evans., A. Fisher dan S. J. Hill . 1998. An Introduction to Analytical


Atomic Spectrometry. England: Joh Wiley & Sons, Ltd.

Jeffery, G.H., J. Bassett., J. Mendham dan R.C. Denney. 1989. Vogels Textbook of
Quantitative Chemical Analysis Fifth Edition. New York: Longman Scientific
& Technical.

Khopkar, S.M. 2007. Konsep Dasar Kimia Analitik. Jakarta: UI-Press.

Noviyanti, Fajrin., Tjiptasurasa., dan Pri Iswati Utami. 2014. Ketoprofen, Penetapan
Kadarnya dalam Sediaan Gel dengan Metode Spektrofotometri Ultraviolet-
Visibel. Jurnal Pharmacy Vol. (11) No. (01) ISSN: 1693-3591.

Tim Dosen. 2016. Penuntun Praktikum Kimia Analisis Instrumen. Makassar:


Universitas Negeri Makassar.

Tulandi, Grace Pricilia., Sri Sadewi., dan Widya Astuty Lolo. 2015. Validasi Metode
Analisis untuk Penetapan Kadar Parasetamol dalam Sediaan Tablet secara
Spektrofotometri Ultraviolet. Jurnal Imu Farmasi Vol. (4) No. (4) ISSN:
2302-2493.

Underwood, A.L., R.A. Day. 2008. Analisis Kimia Kuntitatif Edisi Keenam. Jakarta:
Erlangga.

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