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GRADUATE STUDY FUCULTY OF NATURAL SCIENCE DEPARTEMENT OF MATI-MATICAL AND PHYSICAL SCIENCE SPECIALIZATION IN MATARIAL SCIENCE LABORATORY REPORT

ON MATERIALS SCIENCE EXPERIMENT

TITLE OF EXPERIMENT no 2
DETERMINATION OF UNKNOWN CONCENTRATION USING ATOMIC ABSORPTION SPECTROPHOTOMETER

By: - Dinsefa Mensur no..SGSMS/005/02

id

Submitted to: - PRF D.r S Mohan

January27/2011

TABLE OF CONTENT

Content page no 1 title of experiment the

2 objective ... 3 Theories .. 3.1 Job of the hollow cathode lamp.. 3.2 Job of the nebulizer. 3.3 Job of the flame.. 3.4 Job of the monochromater 3.5 Job of the photomultiplier tube (PMT) .. 3.6 The Hollow Cathode Lamp.. 4) Apparatus and chemical used 4.1 chemicals 4.2 apparatus 5 experimental procedures. 5.1 sample preparation 5.2 copper concentration preparations (standard) .. 5.3 Instrumentation

6 experimental .

data

7 data analysis . 7.1 preparation of desired standard concentration of cu 7.2 calculation of slop. 7.3 calculation of slop. 7.4) calculation of intercept using equation 2.. 7.5) determination of absorption of the unknown concentration . 7.6) calculation of required concentration .. 8) Error estimation.. 8.1standard deviation about the regression 8.2correlation coefficient . 9) Source of .. 10) Conclusions error

TITLE OF EXPERIMENT
DETERMINATION OF UNKNOWN CONCENTRATION USING ATOMIC ABSORPTION SPECTROPHOTOMETER

Experiment two
Date 12/05/03

1 TITLE OF THE EXPERIMENT


DETERMINATION ABSORPTION OF UNKNOWN CONCENTRATION SPECTROPHOTOMETER (AAS) USING ATOMIC

2) OBJECTIVE -To determine quantitatively the unknown concentration of cu -To understand the concept of AAS -To practice how to prepare desired concentration

3 Theories:Atomic absorption spectroscopy (AAS) determines the presence of metals in liquid samples. Metals include Fe, Cu, Al, Pb, Ca, Zn, Cd and many more. It also measures the concentrations of metals in the samples. Typical concentrations range in the low mg/L range. In their elemental form, metals will absorb ultraviolet light when they are excited by heat. Each metal has a characteristic wavelength that will be absorbed. The AAS instrument looks for a particular metal by focusing a beam of uv light at a specific wavelength through a flame and into a detector. The sample of interest is aspirated into the flame. If that metal is present in the sample, it will absorb some of the light, thus reducing its intensity. The instrument measures the change in intensity. A computer data system converts the change in intensity into an absorbance. As concentration goes up, absorbance goes up. The researcher can construct a calibration curve by running standards of various concentrations on the AAS and observing the absorbances. The computer data system will draw the curve for you! Then samples can be tested and measured against this curve.

Atomic absorption spectrophotometer

Fig 1 atomic absorption spectrophotometer 3.1 Job of the hollow cathode lamp Provide the analytical light line for the element of interest Provide a constant yet intense beam of that analytical line 3.2 Job of the nebulizer Suck up liquid sample at a controlled rate Create a fine aerosol for introduction into the flame Mix the aerosol and fuel and oxidant thoroughly for introduction into the flame 3.3 Job of the flame Destroy any analyte ions and breakdown complexes Create atoms (the elemental form) of the element of interest Fe0, Cu0, Zn0, etc. 3.4 Job of the monochromater Isolate analytical lines photons passing through the flame Remove scattered light of other wavelengths from the flame in doing this, only a narrow spectral line impinges on the PMT. 3.5 Job of the photomultiplier tube (PMT) As the detector the PMT determines the intensity of photons of the analytical line exiting the monochromator. 3.6 The Hollow Cathode Lamp The hollow cathode lamp (HCL) uses a cathode made of the element of interest with a low internal pressure of an inert gas. A low electrical current (~ 10 mA) is imposed in such a way that the metal is excited and emits a few spectral lines characteristic of that element (for instance, Cu 324.7 nm and a couple of other lines; Se 196 nm and other lines, etc.). The light is emitted directionally through the lamp's window, a window made of a glass transparent in the UV and visible wavelengths Using this instrument we can collect the absorption of the standard, sample and blank data then after we plot and determine the slope M=xyxx1 The intercept b is calculated by b=y-Mx2

y=Mx+b..3 Where y is the unknown concentration of absorbance, x is the unknown concentration, b is intercept and M is the slop of the graph.

4) APPARATUS AND CHEMICAL USED 4.1 CHEMICALS 10ml 0f Hydrochloric acid , 4ml of Nitric acid, 03ppm 0.1ppm 0.3ppm 0.6ppm concentration of Copper 4.2 APPARATUS Atomic absorption spectrophotometer, Copper Hallow cathode lamp, three 100ml and four 50ml volt metric flasks, Sparker, pepatet filter, two beaker, washing bottle 5 EXPERIMENTAL PROCEDURES 5.1 SAMPLE PREPARATION Take water 100ml bicker and add oxidizing agent to brake (dissociate) the bond the oxidizing agents are here I used 5ml of hydrochloric acid and 2ml of nitric acid .also I prepare in other biker 5ml HCl and HNO3(nitric acid) w/c is blank that I used as reference. Then after put both on the stove until the sample evaporate and remain only 20ml in order to get concentrated Cu in the sample that I was prepared, but the blank only for a few minute. After the sample is prepared I can poured the 20ml of sample in100ml volumetric flask and diluted with water the same thing did for the blank.

5.2 COPPER CONCENTRATION PREPARATIONS (STANDARD) I have cu solution from the supplier its concentration is 1000ppm from this where prepare 10ppm in 100ml of volumetric flask by using dilution low .again from this cu concentration 0.03ppm, 0.1ppm, 0.3ppm, 0.6ppm each in 50ml of volumetric flask. Dilution low V1C1=V2C2.1 WhereV1 is volume of required concentration, C1 is concentration of cu from the supplier, V2 is the volume of volumetric flask in w/c prepared the standard and C2 is concentration to be prepared 5.3 INSTRUMENTATION The AAS that used to determine concentration of copper the following value is adjust as fixed value on the instrument
wave length =324.7

Sample energy

E=3.899 A=00

Current Slit size 6 EXPERIMENTAL DATA Ser Concentration . no

I=1.5mA s=0.7nm

Absorbance of cu

Absorbance of sample

Absorbance of blank

1 2 3 4

0.03 0.1 0.3 0.6

0.003812 0.011574 0.030904 0.069077

0.03

0.021

Table 1 absorbance of cu of prepared concentration. Sample and blank 7 DATA ANALYSIS 7.1 preparation of desired standard concentration of cu We want to prepare 0.03ppm, 0.1ppm, 0.3ppm, 0.6ppm concentration of cu from 10ppm cu on 50ml so we aplay dilution low i.e. equn 1 V1C1=V2C2 V1= V2*C2C1 By Using such relation we take V1=0.15ml, V2=0.5ml, V3=1.5ml, V4=3.0ml from 10ppm copper concentration to get 0.03, 0.1, 0.3, 0.6 ppm concentration in 50ml flask respectively. Graph of absorption verses concentration Plot the graph of absorption verses concentration graph and determined the slop of the graph by using the ratio of standard deviation at x at y and at x at x that is M= xyxx = i=1nxi-x(yi-y)i=1nxi-x24 Or = i=1nxiyi-i=1nxiyini=1nxi2-i=1nxi2n5
Fig 1 absorption verses concentration graph

7.3 CALCULATION OF SLOP Slop can be determined by using equation 1or also from the graph m=xyxx= i=1nxi-xyi-yi=1nxi-x2

Where xi is absorption reading of AAS and yi is concentration of standard cu solution x is themean of AAS reading and y is the mean of standard concentration of cu x =x1+x2+x3+x4n =0.2575, y=y1+y2+y3+y4n =0.028842 where n is sample size in this case n=4 m=i=1nxi-xyi-yi=1nxi-x2=0.0222820.195675=0.11387 7.4) CALCULATION OF INTERCEPT USING EQUATION 2 b= y-mx =0.028842-(0.11387)*(0.2575) =-4.7952510-4

7.5) DETERMINATION OF ABSORPTION OF THE UNKNOWN CONCENTRATION


From table 1 we have the experimental data of absorption of sample and blank hence the difference b/n the absorption of sample and blank gives the absorption of required concentration one Y=As-Ab Where y is the required concentration absorption As sample absorption Ab blank absorption y=0.03-0.21 =910-3

7.6) CALCULATION OF REQUIRED CONCENTRATION y=m x+ b x=(y-b)/m =910-3-(-4.7952510-4)0.113873 =0.08325ppm 8) ERROR ESTIMATION 8.1STANDARD DEVIATION ABOUT THE REGRESSION =yy-m2xxN-2 Whereyy=i=1nyi-y2, xx=i=1nxi-x2, m is slop of the graph =0.002548-0.01296706(0.195675)(4-2) =0.00231 Error (100*0.00231)/0.08325 2.775% X x = [0.08094 _0.08556] Hence the calculated result is b/n the following range

8.2) CORRELATION COEFFICIENT


=i=1nxi-xyi-yi=1nxi-x2i=1nyi-y212 From the slop calculation i=1nxi-xyi-y=0.022282

From standard deviation about regression calculation I have i=1nxi-x2=0.195675, i=1nyi-y2=0.002548 =0.0222824.98579910-4 =0.022282/0.022328902 =0.998 9) SOURCE OF ERROR -the error may arise during preparation of standard copper concentration. -instrumental error -reading error 10) CONCLUSIONS
1) It is possible to determine the presence of metals from a solution 2) Also can determine quantitatively the concentration of the metal from the solution

3) The lab water (our sample) has b/n the range [0.08094 _0.08556] concentration of cu 4 the calculated value is deviated from the regression 0.00231 i.e. 2.775% error