ANALISIS INSTRUMEN
ACARA II
ANALISIS ION KOMPLEKS [Fe(SCN)n]3-n
DISUSUN OLEH:
Hasil
• Diambil 1 mL dari tiap labu ukur
• Diencerkan kembali hingga tanda batas
Hasil
• Dimasukkan dalam kuvet
• Diukur absorbansinya pada λ = 480 nm
Hasil
Hasil
Hasil
• Diukur absorbansinya pada λ = 480 nm
Hasil
Hasil
• Dimasukkan dalam kuvet
Hasil
Hasil
Tabel 4: Seri larutan ion kompleks [Fe(SCN)n]3-n
0 mL, 1 mL, 2 mL, 3 mL, 4 mL larutan Fe3+ 0,0025 M
• Dimasukkan kedalam labu takar 10 mL
• + 1 mL larutan HNO3 4 M
Larutan 1: + 3 mL KSCN 0,01 M
Larutan 2: + 4 mL KSCN 0,01 M
Larutan 3: + 5 mL KSCN 0,01 M
Larutan 4: + 6 mL KSCN 0,01 M
Larutan 5: + 7 mL KSCN 0,01 M
• Dikocok hingga homogen
• Diberi label 1, 2, 3, 4, 5
Hasil
• Dimasukkan dalam kuvet
• Diukur absorbansinya pada λ = 480 nm
Hasil
DAFTAR PUSTAKA 4/5
Dachriyanus. 2004. Analisis Struktur Senyawa Organik Secara Spektroskopi.
Palang: Lembaga Pengembangan Teknologi Informasi dan Komunikasi
Universitas Andalas.
Hidayah, H., Suhendar, D., Sudiarti, T., & Maesaroh, E. (2019). Studi keadaan
oksidasi besi pada air hujan. al-Kimiya: Jurnal Ilmu Kimia dan Terapan,
6(1), 15-21.
Pratiwi, R. A., & Nandiyanto, A. B. D. (2021). How to Read and Interpret UV-VIS
Spectrophotometric Results in Determining the Structure of Chemical
Compounds. Indonesian Journal of Educational Research and
Technology, 2(1), 1-20.
Saad, H., Rahman, M. K. A., Yassin, I., & Muad, A. M. (2017). Characterization
Of Ethanol Concentrations At Ultraviolet Wavelength Region. Journal of
Fundamental and Applied Sciences, 9(4S), 384-400.
Wardani, G., A. Abiya, S., L. Setiawan, F. (2020). Analysis Of The Lead On Lip
Tint Cosmetics On The Market Using Uv-Vis Spectrophotometry Method.
Jurnal Kimia dan Pendidikan, 5(1), 87-100.
5/5
1
Departemen Kimia, Universitas Pendidikan Indonesia, Indonesia
Correspondence: E-mail: nandiyanto@upi.edu
Article History:
UV-VIS spectrophotometry is one of the methods used to Received 28 Apr 2021
Revised 8 May 2021
perform qualitative and quantitative analysis of organic and Accepted 10 Jun 2021
inorganic compounds. However, until now there has been no Available online 13 Jun 2021
further research that studies and describes the detailed
analysis of UV-VIS spectral data in terms of determining the Keyword:
Chromophores,
structure of chemical compounds. Therefore, this paper UV-VIS Spectrophotometry,
contains guidelines that are used as information on how to UV-VIS Spectrum
read and interpret data from the UV-VIS spectrum in terms
of determining the structure of chemical compounds. Steps
on how to analyze the UV-VIS spectrum are presented. This
paper is expected to provide useful information for
researchers and novice students who are studying UV-VIS
spectrophotometry.
1. INTRODUCTION
Spectroscopy is the study of methods for producing spectra. The interpretation of the
resulting spectrum can be used to analyze elements and chemical compounds, examine
molecular structures, and determine the composition of a material (Danusantoso, 1995). UV-
VIS spectrophotometry is one of the analytical methods that is widely used in chemical
research for qualitative and quantitative analysis of organic and inorganic compounds. This
method is widely applied and is generally used for the determination of compounds in very
small quantities (Skoog & West, 1971). One example of the application of the UV-VIS
spectrophotometric method is the analysis of chlorophyll content at several positions of palm
leaf (Arenga pinnata) shoots with a UV-Vis spectrophotometer (Kamagi et al., 2017).
Leong et al., 2018; Dachriyanus, 2003 has explained about how to read and interpret data
from UV-VIS spectrophotometry. However, most of the research does not explain the stages
and the knowledge base for conducting structural analysis of chemical compounds. In fact, a
basic and step-by-step understanding of UV-VIS spectrum analysis for researchers and novice
students is necessary.
This paper discusses how to read and interpret UV-VIS spectrophotometric data in terms
of determining the structure of a chemical compound. Reference analysis from various
sources is used to make it easier for readers to understand and interpret the data. The steps
in interpreting the data are also shown in this paper descriptively.
Generally, UV-VIS spectra can be used with confirmation by comparing the spectra of the
suspected compound (Christian et al., 2014). For determining the overall structure, data from
other instruments, such as FTIR, NMR and other supporting data are usually used (Pavia et
al., 2008). This paper can be used as a guide for researchers and novice students in
understanding and interpreting UV-VIS spectrum data.
2. CURRENT KNOWLEDGE FOR UNDERSTANDING UV-VIS SPECTRA
1
Faculty of Electrical Engineering, Universiti Teknologi MARA, 40450 Shah Alam, Selangor,
Malaysia
2
Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor,
Malaysia
3
Faculty of Electrical Engineering, Universiti Kebangsaan Malaysia, Bangi, Selangor,
Malaysia
ABSTRACT
This paper presents the measurement of optical absorption spectrum for different
concentrations of ethanol at ultraviolet wavelength. Ethanol absorption spectrum was
measured using portable spectroscopy setup from Avantes. It consists of Balanced Deuterium
Halogen light source and spectrometer. The light source can deliver a continuous broad
spectrum ranging from 0.2 to 2.5 µm and the spectrometer has the detection range of 0.2-1.1
µm. Several mixtures of ethanol in de-ionized water were prepared with various
concentrations of 0%, 0.1%, 0.5%, 1.0%, 2.5%, 5%, 10%, 15%, 25%, 50% and 100 vol%.
The baseline of the absorption spectrum was being analyzed and corrected using MATLAB
software. From the results, the spectroscopy setup was successfully detecting ethanol
concentration from 2.5-100vol%. However, only concentration range from 2.5-50vol% has
shown 99% of fulfilment towards the Beer ’s Lambert Law.
Journal of Fundamental and Applied Sciences is licensed under a Creative Commons Attribution-NonCommercial 4.0
International License. Libraries Resource Directory. We are listed under Research Associations category.
M. K. A. Rahman et al. J Fundam Appl Sci. 2017, 9(4S), 384-400 387
The typical spectroscopy setup consists of three main parts; light source, transparent sample
holder with internal width of 1cm cell known as cuvette and a light detector or a spectrometer.
These can be shown as in Fig. 2. The light source can deliver a continuous broad
spectrum ranging from 0.2 to 2.5 µm and a spectrometer has the detection range of 0.2-1.1
µm. The cuvette was placed in between the light source and the spectrometer. Before making
a measurement, spectrometers must be calibrated by means of the absorbency of a reference
substance is set as a baseline value, so the absorbencies of all other substances are recorded
relative to the initial reference substance. Here, DI water was used as a reference substance.
The ratio of the sample spectrum to the reference spectrum is directly related to the sample's
absorption spectrum.
The absorption spectrum for ethanol at UV wavelength was recorded by simply setting up
three important spectrometer parameters such as integration time to 1.14ms, scanning
averages to 100 times and 10 units of smoothing. This chosen setting parameters was advised
by the technical specialist from Aseptec Sdn. Bhd.
The measurement process was started with injecting ethanol-water mixture into the cuvette by
using a syringe until two-third full. Spectrometer will qualitatively and quantitatively compare
the fraction of the light that passes through a reference solution and the test solution. Their
absorbance spectrum was taken once the reading became stabled. After that, the cuvette was
rinsed in the way of injecting de-ionized water into cuvette several times. For each
measurement, the cuvette was rinse thoroughly with de-ionized water as to ensure no residual
particle from the previous test sample. Then, the measurement process was repeated for the
whole concentration of ethanol-water mixture samples.
Fig. 4 shows the results for the absorption spectrum of ethanol-water mixture at the UV
wavelength region with difference concentration from 0.5% to 100%. From the figure, notice
that, the recorded spectrum data measured at UV wavelength have unstable baseline because
the spectra were seemed slanted and not aligned properly at the reference axis.
0.6
218.4
0.5
0.4
Absorbance (AU)
214.2
0.3
0.2
268.4
0.1
0
180.0 220.0 260.0 300.0 340.0 380.0 420.0 460.0 500.0 540.0 580.0
-0.1
Wavelength (nm)
100% 50% 25% 15% 10%
5% 2.50% 1.00% 0.50%
pack the molecules together in the liquid phase which produces the macroscopically observed
increase in density and total volume reduction of sample [18-19].The interaction between the
ethanol and the water itself most probably caused the maximum absorption wavelength varied
from 100% to 50% concentration.
3.2. Validation to Beer’s Lambert Law
According to the Beer’s Lambert law, the absorbance is directly proportional to the path
length and the concentration of the absorbing analytes. Therefore, the relationship between
absorbance and the concentration of ethanol should be plotted as to see how many percent the
samples obeys the law. In order to find the relationship, maximum absorption wavelength at
214.2nm was chosen for all the concentrations since most of the absorption wavelength
occurred at this wavelength. Table 3 summarizes the absorption intensity at 214.2 nm.
Table 3. Absorbance and intensity for different concentration of ethanol at 214.2nm
wavelength
Percentage of Absorbance Absorbance
Ethanol (Vol%) Wavelength (nm) Intensity (AU)
100 214.2 0.49
50 214.2 0.33
25 214.2 0.16
15 214.2 0.08
10 214.2 0.04
5 214.2 -0.01
2.5 214.2 -0.03
1.0 214.2 Not significant
0.5 214.2 Not significant
From Table 3, as the concentration of ethanol reduced, the absorbance intensity also reduces.
However, at 2.5% and 5% concentration, the absorbance intensity has negative values.
According to the Beer’s Lambert law, absorbance should be positive if the molar absorption
coefficient (ε) and the concentration (c) is both positive. Therefore, this negative absorption
reading might be happened if more light is being emitted and detected than the supplied light
source.
Fig. 6 shows the relationship between the absorbance intensities and 0.5-100vol%
2
concentration of ethanol at 214.2nm. From the linearity profile, denoted by R , it is only 95.72%
of the data followed Beer’s Lambert Law.
EduChemia Vol.5, No.1, 2020
(Jurnal Kimia dan Pendidikan) e-ISSN 2502-4787
Program Studi S1 Farmasi STIKes Bakti Tunas Husada Tasikmalaya, Jl. Cilolohan No. 36 Kota Tasikmalaya
E-mail: *gatutariwardani@stikes-bth.ac.id
Abstract: Analysis of the lead on lip tint cosmetics on the market has been successfully
carried out. Before conducting the lead analysis, the method is first validated using the
standard addition and measured by UV-Vis spectrophotometry. The validation of the lead
content analysis method in lip tint using the UV-Vis spectrophotometry method was stated to
meet the validity requirements. The validity parameters include linearity test (correlation
coefficient = 0.9916), limit of detection (0.17 ppm), limit of quantitation (0.57 ppm),
accuracy test (% recovery for a concentration of 4 ppm = 97.5%, 8 ppm = 93.8%, and 14
ppm = 98.6%), and precision (< 2% for all concentrations). Imported lip tint samples
circulating in the market area of the Tasikmalaya city contain lead with a concentration of
2.149 ppm, so it is still declared safe for use by the public.
Keywords: Lip tint; lead; UV-Vis spectrophotometry; validation
Abstrak: Analisis timbal pada kosmetik lip tint yang beredar di pasaran telah berhasil
dilakukan. Sebelum melakukan analisis timbal, terlebih dahulu dilakukan validasi metode
menggunakan metode penambahan standard dan diukur dengan spektrofotometri UV-Vis.
Validasi metode analisis kadar timbal dalam lip tint menggunakan metode spektrofotometri
UV-Vis dinyatakan memenuhi syarat validitas. Parameter-parameter validitas terbebut antara
lain adalah uji linieritas (koefisien korelasi = 0,9916), batas deteksi (0,17 ppm), batas
kuantitasi (0,57 ppm), uji akurasi (% recovery untuk konsentrasi 4 ppm = 97,5%, 8 ppm =
93,8%, dan 14 ppm = 98,6%), dan presisi (< 2% untuk semua konsentrasi). Sampel lip tint
impor yang beredar di pasaran wilayah kota Tasikmalaya mengandung timbal dengan
konsentrasi 2,149 ppm, sehingga masih dinyatakan aman untuk digunakan oleh masyarakat.
Kata kunci: Lip tint; timbal; spektrofotometri UV-Vis; validasi
87
Analysis Of The Lead On Lip Tint Cosmetics... 93
e-ISSN 2502-4787
94 EduChemia,Vol.5, No.1, 2020 Wardami, Abiya, Setiawan
Kurva Kalibrasi
e-ISSN 2502-4787
96 EduChemia,Vol.5, No.1, 2020 Wardami, Abiya, Setiawan
dinyatakan sebagai persen perolehan diperoleh yaitu tidak ada yang lebih dari
e-ISSN 2502-4787
al-Kimiya, Vol. 6, No. 1 (15-21) Juni 2019/Syawwal 1440 H
Keywords: Rainwater is a source of surface water and ground water. Rainwater is formed through
rainwater; iron ; several processes namely condensation, precipitation, evaporation and transpiration.
complex; UV-Vis Rainwater has an iron content in the form of particulates and dissolves such as ferro (Fe2+)
Spectrophotometer; and ferric (Fe3+). The purpose of this study is to determine the content of total Fe, Fe(II) and
AAS. Fe(III) in rainwater and its comparison with rainwater from three different places and to
study the content of rainwater that can reduce Fe(III). Total Fe was analyzed using Atomic
Absorption Spectrophotometer (AAS) instrument. Fe(II) and Fe(III) ions were analyzed with
an UV-Vis spectrophotometer using Fenantrolin and KSCN ligands to form complex
compounds [Fe(C12H8N2)3]2+ and [Fe(SCN)6]3-. The degree of acidity of rainwater was
analyzed using a pH meter while the oxidation state of iron in rainwater was analyzed using a
UV-Vis spectrophotometer by dissolving aqua dm and falling rainwater in industrial estates,
mountains and settlements. The results of the analysis show the content of total Fe, Fe(II) and
Fe(III) in rainwater that falls around the industry, mountains and settlements respectively,
namely Fe total 0.5655; 1.6854; and 2.4232 mg/L, Fe(II) 0.0867; 0.2232 and 0.0731 mg/L,
and Fe(III) 0.5198; 0.4994 and 0.5672 mg/L. From the comparison of the maximum
wavelength shear of the visible light the technical and pro FeSO4.7H2O solution with
phenanthroline complexing was obtained that the rain water had a reduction in the Fe3+ ion.
15
al-Kimiya, Vol. 6, No. 1 (15-21) Juni 2019/Syawwal 1440 H
HASIL DAN PEMBAHASAN dihasilkan dalam air hujan sebagian besar adalah
sebagai Fe(III) karena Fe(III) keberadaannya lebih
Pengukuran Fe Total dalam Air Hujan stabil dibandingkan Fe(II). Perbedaan tingginya
kandungan Fe total di setiap kawasan dipengaruhi
Analisis logam Fe total dalam air hujan oleh partikulat yang terdapat di masing-masing
menggunakan metode Spektrofotometer Serapan kawasan tidak bertahan lama di atmosfer sehingga
Atom (SSA). Penentuan kandungan logam Fe turun kembali ke permukaan melalui air hujan.
dalam sampel air hujan dilakukan pada panjang Kandungan Fe total terendah berada di kawasan
gelombang 248,3 nm. Panjang gelombang ini industri karena partikulat yang dihasilkan di
merupakan panjang gelombang optimum untuk kawasan ini akan berefek ke kawasan yang
logam Fe dengan metode Spektrofotometer jaraknya jauh dari kawasan industri.
Serapan Atom (SSA). Metode ini merupakan
metode yang menggunakan mekanisme atomisasi Pengukuran Fe(II) dalam Air Hujan
dengan proses pengubahan sampel dalam bentuk
larutan menjadi spesies atom dalam nyala. Larutan Pengukuran Fe(II) dalam sampel air hujan
sampel diubah menjadi uap atom sehingga nyala bertujuan untuk mengetahui kandungan Fe(II)
mengandung atom unsur-unsur yang dianalisis. dalam air hujan di beberapa lokasi penampungan
Beberapa atom akan tereksitasi secara termal oleh air hujan diantaranya sekitar industri, pegunungan
nyala, tetapi kebanyakan atom akan tetap tinggal dan pemukiman. Lokasi penampungan sampel air
sebagai atom netral dalam keadaan dasar. hujan diambil dari berbeda lokasi, hal ini
Pada analisis kandungan Fe total dalam dilakukan untuk mengetahui perbedaan
sampel air hujan, digunakan larutan HNO3 pekat kandungan Fe(II) antar lokasi tersebut. Penentuan
yang bertindak sebagai asam pengoksidasi kuat kadar Fe(II) menggunakan Spektrofotometer UV-
sehingga sampel air hujan akan teroksidasi Vis dapat dilakukan dengan mereaksikan sampel
sempurna dengan meninggalkan elemen-elemen dengan agen pengkompleks sehingga akan
pada larutan asam dalam bentuk senyawa menghasilkan warna yang spesifik sesuai dengan
anorganik yang sesuai untuk dianalisis. Tabel.1 pengkompleks yang digunakan.
merupakan hasil pengukuran kandungan Fe total Pengkompleks yang digunakan adalah ligan
dalam air hujan di berbagai lokasi yaitu sebagai fenantrolin. Fenantrolin menyumbangkan dua
berkut: atom donor dalam pembentukan ikatan kovalen
koordinat. Ketika Fe(II) direaksikan dengan ligan
Tabel 1. Hasil Pengukuran Fe total dalam air hujan fenantrolin dapat membentuk senyawa kompleks
Lokasi Kandungan Fe total yang menghasilkan warna merah jingga dengan
Sampling (mg/L) menyerap daerah sinar tampak pada panjang
Industri 0,5655 gelombang 509 nm. Reaksi yang terjadi yaitu:
Pegunungan 1,6854
Pemukiman 2,4232 Fe2+ (aq) + 3C12H8N2 (aq) [Fe(C12H8N2)3]2+(aq) (1)
18
al-Kimiya, Vol. 6, No. 1 (15-21) Juni 2019/Syawwal 1440 H
Pengukuran kandungan Fe(III) dalam air pH air hujan yang dihasilkan dari berbagai
hujan menggunakan metode analisa kawasan penampungan air hujan dapat dilihat
spektrofotometer UV-Vis dimana metode ini pada Tabel 4.
dilakukan dengan mengkomplekskan zat yang
akan dianalisa dengan pengkompleks besi yang Tabel 4. Hasil Pengukuran pH dalam air hujan
akan membentuk suatu warna yang spesifik.
Lokasi Sampling pH
Fe(III) direaksikan dengan ligan SCN- akan Industri 5,67
membentuk senyawa kompleks [Fe(SCN)6]3-. Pegunungan 5,93
Senyawa kompleks ini dapat menyerap daerah Pemukiman 5,92
sinar tampak pada panjang gelombang 483 nm.
Reaksi yang terjadi yaitu: Tabel 4 dapat dilihat pada bahwa rata-rata
hasil pengukuran yaitu diantara 5,67-5,93. Hasil
Fe3+(aq) + 6SCN-(aq) [Fe(SCN)6]3-(aq) (2) tersebut menunjukkan bahwa pH air hujan dari
tiga lokasi ini termasuk ke dalam air hujan alami.
(Kuning (Tak (Merah Tua)
Karena pH air hujan alami yaitu sekitar 5,56.
kecoklatan) berwarna)
Namun terdapat perbedaan pH hasil pengukuran
antar lokasi. Pada lokasi industri menunjukkan pH
19