ANALYSIS BY ATOMIC ABSORPTION SPECTROPHOTOMETRY (Putu Pratiwi Surya Rahayu_1013031003) Introduction Atomic absorption spectrophotometry is the method of analysis

instrumentation based on the absorption of electromagnetic radiation by free atoms of the element being analyzed. The principle of this method of analysis is the decomposition of footage into free atoms of the molecule with the help of a flame produced from fuel combustion, known as the atomization process. In this process, the sample to be analyzed is absorbed through the capillary tube and sprayed in flame, so that the sample atomization events will occur. Free atoms are then given by the electromagnetic radiation of certain wavelengths generated from the source to promote a valence electron to a higher energy level, known as excitation. The basic concept of the AAS method is the absorption of light by neutral atoms in a gaseous state, where the rays are usually absorbed the visible light range is very narrow absorption lines is about 0.0002. This is because the band is not affected by the atomic structure such as vibrational and rotational molecular absorption bands. AAS method can be determined by the total concentration of metals in the samples by measuring the absorption of radiation by atoms in a gas with a specific wavelength of the atom (Ismono, 1990). Wavelength for each element must be selected so as to produce a sharp spectral lines (resonance lines) and with maximum intensity. AAS method can be used to analyze metal elements on the concentration of the quantity of trans (microscopic) quantity until macro. This method is able to analyze the levels of metals in various solvents. The intensity of electromagnetic radiation that is absorbed by the atoms that exist in the sample in the excitation process can be determined quantitatively by the following Lambert-Beer law
A log T abC

where, T = transmitasi A = Absorbance a = absorptivity (L / g cm) b = width of the flame (cm) C = concentration of sample (g / L) From these equations it appears that the absorbance is directly proportional to the concentration of the sample. This method can be used for quantitative analysis of elements in very small quantities. The Way to determine the concentration of the sample solution is to create a calibration curve of the concentration of the relationship between the absorbance of standard solutions in the form of a straight line). The next sample solution absorbance measured absorbance and the data obtained are plotted in a calibration curve, in order to obtain the sample concentration. In this practicum will make calibration curve toward the concentration of metal, determining the linear curve equation, to determine the concentration of metal and determine the content of metal in sample.

Methods In analysis by atomic absorption spectrophotometry experiment was used some equipments and materials for conduct the experiment. There some step when do this practicum, such as making standard iron solution, making standard magnesium solution, making sample solution. First, making standard iron solution was used Fe(NO3)3. 0.216 gram of Fe(NO3)3 is dissolved in 500 mL of aquades. From this solution, making standard solution (Fe3+) 0, 2, 4, 6, 8, 10 ppm. The color of solution is yellowish. Second, making standard magnesium solution was used Mg(NO3)2. 0.196 gram of Fe(NO3)3 is dissolved in 500 mL of aquades. From this solution, making standard solution (Mg2+) 0; 0.2; 0.4; 0.6; 0.8; 1.0 ppm. The color of solution is colorless. Third, making sample solution. It was used sample 3 and that has already dried then crushed and balancing the mass of sample on 0.100 gram. Then, put in beaker teflon + 5 mL HNO3. It is heated until brown vapor of NOx disappear. Add 1 mL HF 40% , heat again. Filter and it is diluted. After that, measure the standard solution with sample using atomic absorption spectrophotometry Shimadzu AA-6300. Result and Discussion Tabel 1. The absorbance of Fe3+ standard solution Ppm 2 4 6 8 10 Sample 3 Concentration 3,0632 -7,6250 36,6671 5,20074 8,4944 -2,0462 Absorbance -0,0042 -0,0153 0,0369 -0,0010 0,0026 -0,0096 BG 0,0230 0,0142 0,0632 0,0225 0,0311 0,0163

Based on the table above, the curve calibration absorbance of Fe in standard solution is:

absorbance curve of Fe
0.04 0.03 absorbance 0.02 0.01 0 -0.01 -0.02 0 1 2 3 4 5 6 7 8 9 10 absorbance Linear (absorbance)

y = 0.0011x - 0.0027 R = 0.058

concentration (ppm)

Based on the calibration curve above, it was gotten the linear curve by equation y= 0.0011x - 0.0027. Manually, the slope/gradient and intercept can be obtained by using the following formula: Abs = mC + b Whereas,m = curve gradient b = intercept (interception point concentration to absorbance) C = concentration (ppm) m score (gradient) get from : A 0.0369 (0.0153) m = Fe 10.0 2 = 6.525 x 10-3 b score find by using equation on the absorbance score: example A = -0.0042 C = 2 ppm so : A = 6.525 x 10-3 C + b -0.0042 = 0.006525 . 2 + b b = - 0.01725 So the equation based on manual calculation is: A = 0.006525 C - 0.01725 (so far to the score by using excel). It happened because the solution was kept in long time. So, the solution was broken and contaminated with the other substances. Determination of concentration of iron in sample (ppm). Based on data above, the absorbance of sample was gotten about -0.0096. Based on the equation (A = 0.0011C - 0.0027) of the line, can be carried out calculations on the iron content of the sample 3 A = 0.0011C 0.0027

-0.0096 = 0.0011C 0.0027 C = -6.27 ppm

So based on the calculation above the concentration of iron in ppm is -6.27 ppm. The sample being measured is made of 0.1 gram sample 3 of soil into 100 mL solution. C -6.27 ppm = -6.27 ppm = -6.27 mg/L = -6.27 x 10-3 g/103 mL = -6.27 x 10-6 g/mL x 100 mL = -6.27 x 10-4 gram

The molarity of Fe can be found by the following calculation: M=

MassFe 1000 x Ar Fe V

- 6.27 x 10 4 1000 x = 56 100

= -1.119 x 10-4M The percentage of Fe in 0.1 gram of sample is: %Fe =
mass Fe in sampel x 100 % mass sampel

- 6.27 x 10 -4 gram x 100 % 0.1gram

= -0.627 % Tabel 2. The absorbance of Mg2+ standard solution Concentration Absorbance BG (ppm) 0,2 8,0504 0,3712 0,0032 0,4 3,7536 0,2723 0,0028 0,6 8,3227 0,4325 0,0033 0,8 3,8277 0,3409 0,0028 1 2,3226 0,2999 0,0031 Sample 3 2,9624 0,3026 0,0029 Based on the table above, the curve calibration absorbance of Fe in standard solution is: Ppm

absorbance curve of Mg
0.5 0.45 0.4 0.35 0.3 0.25 0.2 0.15 0.1 0.05 0 -0.05 0 y = 0.2243x + 0.174 R = 0.3087

absorbance

absorbance Linear (absorbance)

0.2

0.4 0.6 0.8 concentration (ppm)

Based on the calibration curve above, it was gotten the linear curve by equation y= 0.2243x + 0.174.

Manually, the slope/gradient and intercept can be obtained by using the following formula: Abs = mC + b. Whereas, m = curve gradient, b = intercept (interception point concentration to absorbance), C = concentration (ppm). m score (gradient) get from : A 0.4325 (0.2723) m= Fe 1 0.2 = 0.20025 b score find by using equation on the absorbance score: example A = 0.3712, C = 0.2 ppm. So, A = 0.20025 C + b 0.3712 = 0.20025 x 0.2 + b b = 0.3315 So the equation based on manual calculation is: A = 0.20025 C + 0.3315 (so far to the score by using excel). It happened because the solution was kept in long time. So, the solution was broken and contaminated with the other substances. Determination of concentration of magnesium in sample (ppm) Based on data above, the absorbance of sample was gotten about 0.3026. Based on the equation (A = 0.2243C + 0.174) of the line, can be carried out calculations on the iron content of the sample 3 A = 0.2243C + 0.174 0.3026 = 0.2243C + 0.174 C = 0.57 ppm So based on the calculation above the concentration of iron in ppm is 0.57 ppm. The sample being measured is made of 0.1 gram sample 3 of soil into 100 mL solution. C = 0.57 ppm 0.57 ppm = 0.57 mg/L = 0.57 x 10-3 g/103 mL = 0.57 x 10-6 g/mL x 100 mL = 0.57 x 10-4 gram = 5.7 x 10-5 gram The molarity of Mg can be found by the following calculation: M=
MassMg 1000 x Ar Mg V

5.7 x 10 5 1000 x 24 .3 100

= 2.345 x 10-5M The percentage of Mg in 0.1 gram of sample is: %Mg =

mass Mg in sampel x 100 % mass sampel

5.7x 10 -5 gram x 100 % = 0.1gram

= 0.057 %

Conclusion Based on the explanation above, it can be concluded that: a. Absorbance calibration curve for the metal can be determined through the curve equation, A = mC + b, the equation of Fe and Mg sequence based on this curve was A = 0.0011C - 0.0027 and A = 0.2243C + 0.174 b. The concentration of Fe and Mg sequence in the sample was -6.27 ppm or -1.119 x 10-4M and 0.57 ppm or 2.345 x 10-5M The percentage of Fe and Mg metals in the sample was -0.627 % and 0.057 % References Day & Underwood. 1998. Quantitative Analysis Sixth Edition. Translated by: Sofyan, Iis. Jakarta: Erlangga. Ismono. 1978. Cara-cara Optik Dalam Analisis Kimia. Diktat. Bandung: Jurusan Kimia ITB Khopkar, S.M. 1990. Basic Concepts of Analytical Chemistry. Terj. Saptoraharjo, A. Konsep Dasar Kimia Analitk. Jakarta: UI-Press. Muderawan, I Wayan. 2008. Spectroscopy Instrumental Analysis. Singaraja: Ganesha University of Education.