Kimia Analisis

TKK 110/3 sks

Jurusan Teknik Kimia UGM

Tahun 2004
Kontrak Perkuliahan (1)
 MATA KULIAH : KIMIA ANALISIS
 Kode : (TKK103)
 JUMLAH SKS : 3 SKS
 PENGAJAR-1 : DR. DWI SISWANTA
 PENGAJAR-2 : DRS. MUDJIRAN
 BUKU ACUAN:
 Skoog, West and Holler, Analytical Chemistry: an
Introduction
 David Harvey, Modern Analytical Chemistry
 Christian, Analytical Chemistry
Kontrak (2)
1) Penilaian:
1) Tugas-tugas (3x) : 15%
2) Ujian Sisipan : 30%
3) Ujian Akhir : 45%
2) Sistem Penilaian: Kombinasi Nilai Mutlak dan
Relatif:
1) A > 90%
2) B > 70%
3) C > 50%
4) D > 35%
5) E < 35%
Kontrak (3)
1) Presensi: mengikuti aturan Jurusan
Teknik Kimia
2) Sistem ujian: Buku terbuka (Open Book)
dalam Bahasa Inggris.
Materi & Jadwal Perkuliahan
(1):DS
1 29-Agust Pendahuluan - Kesetimbangan dalam larutan
2 05-Sep Kesetimbangan Kompleks - Ladder Diagram
3 12-Sep Titrimetri Asam-basa
4 19-Sep Kesetimbangan Kompleks/EDTA
5 26-Sep Libur lebaran (?)
6 03-Okt Libur lebaran (?)
7 10-Okt Libur lebaran (?)
8 17-Okt Titrimetri Kompleks/EDTA
9 24-Okt Ujian Sisipan
10 31-Okt Ujian Sisipan
Materi & Jadwal Perkuliahan
(2): Mudjiran
11 07-Nop Titrimetri Pengendapan

12 14-Nop Titrimetri Pengendapan

13 21-Nop Titrimetri Redoks

14 28-Nop Titrimetri Redoks

15 05-Des Gravimetri

16 12-Des Gravimetri

17 19-Des Cadangan
Bab 1: Pendahuluan
 Pengertian Kimia Analitik:
 Kimia analitik meliputi pemisahan, identifikasi, dan
penentuan jumlah relatif komponen yang
menyusun suatu sample bahan.
 Analisis kualitatif mengungkapkan identitas kimia
dari analit
 Analisis kuantitatif menunjukkan seberapa banyak
analit dalam bentuk angka.
 Analit = komponen dari sampel yang akan
ditentukan/dianalisis.
Peran Kimia analitik dalam ilmu
pengetahuan:

 Kimia analitik semula sebagai the art of

recognizing substances and determining
their constituents (Ostwald, 1894)
 Sekarang menjadi sains yang
diterapkan mulai dari industri, obat-
obatan, dan semua ilmu lain.
Contoh penerapan kimia analitik:
 Pengukuran Ca2+ dalam serum darah
membantu diagnosis penyakit parathyroid
untuk pasien manusia.
 Analisis baja selama proses produksi
memungkinkan pengaturan kadar C, Ni dan
Cr untuk mendapatkan produk dengan
kekuatan, kekerasan, ketahanan korosi dan
duktilitas.
 Kontrol pengotor dalam Ge dan Si kristalin
dalam studi semikonduktor.
Klasifikasi metoda analisis:
 Gravimetri
 Volumetri
 Elektroanalitik
 Spektroskopi
 Spektrometri massa
Tahapan dalam analisis kuantitatif
(satu contoh)
1) Pilih metoda
2) Ambil sampel
3) Buat sampel lab.
4) Tentukan replikat
5) Larutkan sampel
6) Hilangkan interferensi
7) Ukur sifat analit
8) Hitung hasilnya
9) Perkirakan reliabilitas hasil
Tahapan problem-solving
 Identify and define the problem:
 Identify type of infromation needed: qualitative,
quantitative, characterizzation or fundamental
 Identify contect of the problem
 Design the experimental procedure:
 Establish design criteria: accuracy, precision, scale
of operation, sensitivity, selectivity, cost, speed.
 Identify interferents
 Select method
 Establish validation criteria
 Establish sampling strategy
Tahapan (2)
 Conduct an experiment
 Calibrate instrument and equiment
 Standardize reagents
 Gather data
 Analyze the experimental data
 Reduce or transform data
 Analyze statistics
 Verivy results
 Interpret result
 Propose a Solution
 Conduct external evaluation
Konsentrasi larutan:
 Molar
Molar analitik: kosentrasi total
Molar keseimbangan: konsentrasi dalam
keseimbangan.
 Konsentrasi persen: w/w; v/v; w/v
 Ppm, ppb, ppt
Densitas dan berat jenis:
 Densitas = berat per satuan volume
(Kg/L; g/mL)
 Berat jenis = rasio massa zat dengan
massa air dengan volume yan sama
pada temperatur 4 oC. (tanpa satuan)
Perhitungan stoikiometri:
 Hubungan massa antar spesies kimia
yang bereaksi.
 Massa -> mol -> mol -> massa
 (1) (2) (3)
 (1) dibagi dengan massa molar
 (2) dikalikan dengan rasio stoikiometri
 (3) dikalikan dengan massa molar
Basic Equipment: balance
Measuring volume (1)
Measuring volume (2)
Skema Analisis Ni (konvensional)
Desiccator
Furnace
Analisis Ni (modern)
The Language of Analytical
Chemistry

 Analysis= a process that provides

chemical or physical infromation about
the constituents in the sample or the
sample itself.
 Analyte= the components of interest in
the sample
 Matrix= all other constituents in a
sample except for the analytes
Analysis, determination and measurement

 Determination: an analysis of a sample

to find the identity, concentration, or
properties of the analyte.
 Measurement: an experimental of an
anlyte’s chemical or physical properties.
Techniques, Methods, Procedures and
Protocols

 Technique: a chemical or physical principle

that can be used to analyze a sample
 Method: a means for analyzing a sample for a
specific analyte in a specific matrix
 Procedure: written directions outlining how to
analyze a sample.
 Protocol: a set of written guidelines for
analyzing a sample specified by an agency.
 Illustration

Technique
Graphite furnace atomic absorption spectroscopy

Methods
Pb in water Pb in Soil Pb in blood
Procedures
APHA ASTM

Protocols EPA
Classical vs instrumental
 Signal; an experimental measurement that is
proportional to the amount of analyte (S)
 SA= knA
 Total Analysis Technique (classical
techniques) = the signal is proportional to the
absolute amount of the analyte.
 Concentration technique (instrumental
technique) = the signal is proportional to the
concentration
Accuracy, Precision, Sensitivity and
Selectivity
 Accuracy= a measure of how closely the result of an
experiment agrees with the expected result.
 Precision= an indication of the reproducibility of a
measurement or result.
 Sensitivity= a measure of a method’s ability to
distinguish between two samples; reported as the
change in signal per unit change in the amount of
analyte.
 Selectivity= A measure of a method’s freedom from
interferences as defined by the methods’s selectivity
coefficients.
 Sellectivity coefficient (KA, I)= a measure of a
method’s sensitivity for an interferent relative to that
for the analyte.
Robustness and Ruggedness
 Robust= a method that can be applied
to analytes in a wide variety of matrices
 Rugged = a method that is insensitive
to changes in experimental conditions.
Scale of Operation
Equipment, time and cost
 Equipment: instrumental vs titrimetry
 Time: for lab with high volume of
samples
 Cost: equipment, reagent, hiring
analyst, the number of samples per
hour.
Calibration and
Standardization
 Calibration is the process of ensuring that the
signal measured by a piece of equipment or
an instrument is correct.
 Standardization is the process of establishing
the relationship between the amount of
analyte and a method’s signal.
 Calibration curve= the result of a
standardization showing graphically how a
method’s signal changes with respect to the
amount of analyte.
 Validation= the process of verifying that a
procedure yields acceptable results.
Evaluating analytical data
 Tendency:
 Mean
 Median
 Spread:
 Range
 Standard Deviation
 Variance
 Experimental Error
 Accuracy
 Precision
Propagation of Uncertainty