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Table of Contents

1. Abstract .................................................................................................................................... 22. Introduction ............................................................................................................................. 2

3. Theory ...................................................................................................................................... 4

3.1. Inductive Coupled Plasma ................................................................................................ 4

3.2. The Workings of an ICP................................................................................................... 4

3.3. Advantages and Disadvantages ........................................................................................ 5

3.4. The ICP Torch .................................................................................................................. 6

4. Experimental Protocol ............................................................................................................. 8

4.1. Material and apparatus ..................................................................................................... 8

4.2. Procedure ........................................................................................................................ 10

5. Results ................................................................................................................................... 12

6. Discussion .............................................................................................................................. 13

Calculation ................................................................................................................................ 13

7. Conclusion ............................................................................................................................. 16

8. References ............................................................................................................................. 17

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1. ABSTRACT

This experiment is to determine the metal contained in the waste water samples and to

identify whether it is safer for drinking or not. Two water samples are selected from the

unknown sources to detect the amount of zinc element present in the samples. Standard solution

of zinc chloride was prepared by dilution process from stock solution with concentration 100

ppm to 12.5 ppm, 25 ppm and 50 ppm. Operate the iCAP 6000 series with guideline from

instructor using both of unknown sample with solution was prepared. Standard solution is

function to plot the calibration curve based on result. Concentration of zinc for the samples

wastewater can determine by that calibration curve. Concentration of zinc for sample A is

undefined because the intensity also cant define using iCAP 6000 series. Intensity of zinc for

sample B is determined to be 849715.2 Cts/s and the calculation for concentration of zinc is

determined to be using the calibration curve. Without using the calibration curve,

ICP-AES can detect direct to concentration zinc for sample A is 0.2997 ppm and sample B is

68.89 ppm. It is conclude that both of the sample A and B are not suitable use for drinking

because the present of heavy metal. The water samples must be treated before it has been using

by human in order to avoid the deseases.

2. INTRODUCTION

Water is an essential part of our lives. We need it to survive, for cleaning and

transportation, and it is the habitat for many aquatic animals, some of which humans consume.

Water contaminated with heavy metals has serious negative effects on health and the ecosystem.

Concentrations of heavy metals are believed to influence the distribution of certain crustaceans,

fish and other marine and freshwater animals. The World Health Organization (WHO) has

stipulated the level of heavy metals allowed in drinking water, but due to ever increasing levelsof knowledge regarding the effects of heavy metals the stipulated levels are constantly changing

to preserve our health.

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This experiment most prefer to detect heavy metal in wastewater sample to using ICP-

AES. An emission spectrum is produced by an electronic transition from a high energy level En

to a lower energy level Em. The acceptable transitions are given by the quantum mechanics

selection rules. A quantity of energy,Q is transferred to an atom by collision with another

particle, resulting in excitation of the atom. An electron from an outer layer of the atom is

excited to a higher energy level. Following this electron excitation, the electron returns, in one or

several stages, to its original energy level. The atomic emission technique measures the energy

lost by an atom passing from an excited state to a lower energy state. The energy is released in

the form of light rays with a wavelength, or more specifically, in the form of a photon with a

frequency,v carrying energy hv.

Figure 1: Energy transition

The atomic emission spectrum is composed of discrete spectral lines. The number of photons

emitted is proportional to the number of atoms of the element present. To be excited, the sample

must be atomized, meaning dissociated into free ions or atoms. The emission phenomena takes

place in a plasma. A plasma is an electrically neutral highly ionize ionized gas. The gas used is

typically argon.

The objective of this experiment is to determine whether selections of water samples are

safe to drink. Determination of zinc in wastewater by standard solution prepared from dilution

process of ZnCl. In experiment, must be provided a selection of water samples from an unknown

location and you will ascertain whether they are safe to drink. Using the ICP will analyze the

composition of the samples and with reference to WHO and USEPA health standards will decide

whether the water is potable. If any of the samples are unsafe for consumption and will need to

suggest a procedure or method by which it may be discharged in order to comply with regulatory

wastewater standards.

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3. THEORY

3.1. Inductive Coupled Plasma

Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) is one of several

techniques available in analytical atomic spectroscopy. ICP-AES utilizes plasma as the

atomization and excitation source. Plasma is an electrically neutral, highly ionized gas that

consists of ions, electrons, and atoms. The sun, lightning, and the aurora borealis are examples of

plasmas found in nature. The energy that maintains analytical plasma is derived from an electric

or magnetic field; they do not burn. Most analytical plasmas operate with pure argon or

helium, which makes combustion impossible. Plasmas are characterized by their temperature, as

well as their electron and ion densities. Analytical plasmas typically range in temperature from

600 to 8,000 K. As a comparison, the temperature of the suns interior is millions of degrees,

while its surface temperature is approximately 10,000 K. Figure 2 summarize the steps involved

in determining the elemental content of an aqueous phase sample by ICPAES.

3.2. The Workings of an ICP

CP hardware is designed to generate plasma, which is a gas in which atoms are present in an

ionized state. The basic set up of an ICP consists of three concentric tubes, most often made of

silica. These tubes, termed outer loop, intermediate loop, and inner loop, collectively make up

the torch of the ICP. The torch is situated within a water-cooled coil of a radio frequency (r.f.)

generator. As flowing gases are introduced into the torch, the r.f field is activated and the gas in

the coil region is made electrically conductive. This sequence of events forms the plasma.

The formation of the plasma is dependent upon an adequate magnetic field strength and the

pattern of the gas streams follows a particular rotationally symmetrically pattern. The plasma is

maintained by inductive heating of the flowing gases. The induction of a magnetic field

generates a high frequency annular electric current within the conductor. The conductor, in turn,

is heated as the result of its ohmic resistance.

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In order to prevent possible short-circuiting as well as meltdown, the plasma must be insulated

from the rest of the instrument. Insulation is achieved by the concurrent flow of gasses through

the system. Three gases flow through the system--the outer gas, intermediate gas, and inner or

carrier gas. The outer gas is typically Argon or Nitrogen. The outer gas has been demonstrated to

serve several purposes including maintaining the plasma, stabilizing the position of the plasma,

and thermally isolating the plasma from the outer tube. Argon is commonly used for both the

intermediate gas and inner or carrier gas. The purpose of the carrier gas is to convey the sample

to the plasma.

An ICP typically includes the following components:

sample introduction system (nebulizer) ICP torch High frequency generator Transfer optics and spectrometer Computer interface

3.3. Advantages and Disadvantages

Advantages of using an ICP include its ability to identify and quantify all elements with

the exception of Argon; since many wavelengths of varied sensitivity are available for

determination of any one element, the ICP is suitable for all concentrations from ultratrace levels

to major components; detection limits are generally low for most elements with a typical range

of 1 - 100 g / L. Probably the largest advantage of employing an ICP when performing

quantitative analysis is the fact that multielemental analysis can be accomplished, and quite

rapidly. A complete multielement analysis can be undertaken in a period as short as 30 seconds,

consuming only 0.5 ml of sample solution. Although in theory, all elements except Argon can be

determined using and ICP, certain unstable elements require special facilities for handling the

radioactive fume of the plasma. Also, an ICP has difficulty handling halogens--special optics for

the transmission of the very short wavelengths become necessary.

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3.4. The ICP Torch

The ICP is a radiofrequency-(RF, 27.12 MHz, 40 MHz) induced plasma that uses an

induction coil to produce a magnetic field (H). The ICP operates between 1 and 5 kilowatts. The

induction coil is wrapped two or three times around the ICP torch and has water flowing through

it for cooling purposes. All ICPs have a capacitor bank that is continuously tuned to match the

plasmas inductance. In order for the RF to travel along the surface of the hollow coil with

minimum resistance, the coil is either gold or silver plated. Neither gold nor silver forms metal

oxides upon contact with air. Although the RF power supply maintains the plasma, a tesla coil is

used to ignite the plasma through the generation electrons and ions that couple with the magnetic

field.

The most common ICP torch in use today has evolved over decades of development (see

Figure 3). The circular quartz tube (1230 mm OD) has three separate gas inlets. The only gas

routinely used is argon. The gas enters the plasma through the outer channel with a tangential

flow pattern at a rate of 820 Lmin-1. The auxiliary gas, which travels up the center channel, also

has a tangential flow (0.53 L min-1) pattern. The nebulizer gas has a laminar flow pattern (0.1 to

1.0 Lmin-1

) and injects the sample into the plasma. The analytical zone is approximately 1 cm

above the coils and offers the best optical viewing area for maximum sensitivity. The plasma

temperature in the analytical zone ranges from 50008000 K (the temperature varies with power,

flow rate, etc.). The high temperature assures that most samples are completely atomized,

although some molecular species (e.g., N2, N2+, OH, C2, etc.) do exist and can be readily

measured in the plasma.

The plasma emits a continuum of background radiation that extends from the visible into

the ultraviolet region (see Figure 1). The radiation originates from electrons, Ar and Ar+, as well

as various atomic and molecular species in the matrix. Although sample blanks can help offsetthe unwanted flux of background photons, there is a certain level of instability in the continuum

background and this instability plays a role in limiting the sensitivity of ICP-AES.

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Figure 2: Schematic of an ICP torch

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4. EXPERIMENTAL PROTOCOL

4.1. Material and apparatus

Figure 3: Analytical balances Figure 4: Volumetric flask

Figure 5: ZnCl2 Figure 6: Distilled water

Figure 7: Pipette

Spatula

Plastic

trace

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Figure 8: iCAP 6000 series

Figure 9: ASX-520 Auto Sampler

Spray chamber

Pum

Capillarytubing

Radial torch

Nebulizer

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4.2. Procedure

a) Preparation the standard solution

1. Prepared all suitable material and apparatus for this experiment.2. Weight out the desired amount of ZnCl is 0.01g using analytical balances. (Refer

figure 3).

3. Place ZnCl into volumetric flask and adds the required amount of distilled water untilthe volume achieve 100ml. Concentration for this stock solution know that is

100ppm.

4. After got the stock solution, prepared dilution method for make the standard solutionin concentrations are 50, 25 and 12.5 ppm. (refer figure 10)

5. Many stock solution the same components but often in varying concentrations. Toavoid having to make every stock solution from scratch, it is useful to prepare several

concentrated stock solutions and dilute as needed (standard solution). To make 50 ml

of 50 ppm ZnCl standard solution, combine 25ml of a 100ppm stock solution and

added distilled water until volume for standard solution 50ml. The following is useful

for calculating amounts of standard solution needed: M1V1=M2V2, where M1=initial

concentration or conc of stock solution; V1=initial vol, or amount of stock solution

needed, M2=final concentration or conc of desired solution; V2=final vol, or volume

of desired solution.

6. Repeat step 5 to get the other standard solution in volume of 50ml at differentconcentration of 25 ppm and 12.5 ppm.

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Figure 10: Preparing solution

b) ICP determination of metal in waste water

1. Pour all solution 100, 50, 25 and 12.5 ppm in different test tube and also pour

wastewater samples in test tube.

2. Place all that test tube on ASX-520 Auto Sampler as in figure 9.

3. Running the iCAP 6000 Series with guideline from lab instructor.

4. Get the automatic recorded result and print out as a reference.

12.5ppm

25ppm 50ppm

Stock

solution,

100ppm

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5. RESULTS

Intensity, (Cts/s) Intensityintensity of

blank, (Cts/s)

Standard

derivative,

%RSD

Blank 584.8 0.0 18.8 3.219

Sample A Undefined - 0.0 0.0

Sample B 850300 849715.2 929 0.1093

Standard solution

12.5 ppm

92780 92195.2 856 0.9222

Standard solution

25 ppm

169900 169315.2 672 0.3953

Standard solution

50 ppm

321300 320715.2 1876 0.5837

Standard solution

100 ppm

573000 572415.2 1263 0.2204

Table 1: Experiment data

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6. DISCUSSION

Figure 11: calibration curve

Calculation (Equation of linear line)

For sample A:

intensity = undefined

concentration = undefined

For sample B:

Absorbance = 849715.2 Cts/s (average)

y = 5462.6x + 32603

0

100000

200000

300000

400000

500000

600000

700000

800000

900000

0 50 100 150

intensity,

Cts/s

concentration, ppm

intensity versus concerntration

standard solution

sample A

sample B

Linear (standard solution)

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The purpose of this experiment is to determine the amount metal which is in the sample

of water A and B. From the experiment done, it will shows whether the samples are safer to be

drink or not. Based on the graph above, it shows the calibration of intensity of zinc versus

concentration. Concentration on element zinc is proportional to the intensity whereas when

concentration increase, the intensity of the sample also increases. For sample A, metal zinc could

not be detected by calibration curve which is mean element zinc is not present in the sample A

but the concentration of zinc is still obtained in sample A was 0.2997 ppm from a sample report.

The difference in result is because the sample element are detected by using two ways

which is using calibration curve based on standard solution and other one by ICP machine

detector. The concentration of zinc present in sample A are less compared to standard water

quality regulation which 1mg/L. Hence, it is suitable use for drink. Besides that, others element

also present in the sample A such as Aluminum, Arsenic, Barium, Calcium, Cobalt, Chromium,

Cuprum, Ion, Lithium, Magnesium, Manganese, Nickel, Scandium, Silicon, Stanum, Titanium,

Thallium, Vanadium in small amount.

For sample B, the intensity of zinc is determined to be 850300 Cts/S with concentration

of 149.583 ppm by using a linear equation of calibration curve. Other way, the concentration of

zinc obtained in sample B is 68.89 ppm that was detected by ICP machine. It is mean that higher

amount of element zinc present in sample B. The concentration of zinc present in sample B is

exceeding the standard water quality regulation of zinc amount in water. Hence, sample B are

harmful to human health and not suitable use for drink. Others element also present in the sample

B in small amount same as in sample A. The calibration curves of intensity versus concentration

are plotted which is as a references to determined the amount of zinc element in both sample of

water.

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Maximum Effluent Parameter Limits Standards A and B.

Parameters (Units) StandardA (1) B (2)

1 Temperatureo

C 40 402 pH - 6.0 - 9.0 5.5 - 9.0

3 BOD5 @ 20oC mg/l 20 50

4 COD mg/l 50 100

5 Suspended Solids mg/l 50 100

6 Mercury mg/l 0.005 0.05

7 Cadmium mg/l 0.01 0.02

8 Chromium, Hexalent mg/l 0.05 0.05

9 Arsenic mg/l 0.05 0.10

10 Cyanide mg/l 0.05 0.10

11 Lead mg/l 0.10 0.5

12 Chromium, Trivalent mg/l 0.20 1.0

13 Copper mg/l 0.20 1.0

14 Manganese mg/l 0.20 1.0

15 Nickel mg/l 0.20 1.0

16 Tin mg/l 0.20 1.0

17 Zinc mg/l 1.0 1.018 Boron mg/l 1.0 4.0

19 Iron (Fe) mg/l 1.0 5.0

20 Phenol mg/l 0.001 1.0

21 Free Chlorine mg/l 1.0 2.0

22 Sulphide mg/l 0.50 0.50

23 Oil and Grease mg/l No detectable 10.0

Table 2: Environmental Quality (Sewage and Industrial Effluents) Regulations, 1979.

1. Standard A for discharge upstream of drinkingwater take-off

2. Standard B for inland waters

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7. CONCLUSION

The experiment was performed in order to determine the metal amount in sample of

waste water. In sample A, the concentration of zinc present was 0.2997 ppm that is in smallamount. Although the amount of zinc is less in sample A, it also contained the higher amount of

cobalt element which is can harmful to human health. The concentration of zinc presented in

sample B was 149.583 ppm by calibration curve and 68.89 ppm from sample report. The amount

of zinc present in sample B was exceeding the standard water quality of amount of zinc in

drinking water take-off. However, toxicity can occur when an excessive amount of zinc is

ingested in the human body.

Higher amount of zinc present in drinking water can adverse health effects such as

stomach cramps, nausea and vomiting. Besides that, zinc deficiency may induce a number of

critical functional abnormalities, including impaired reproductive performance, depressed

immune function and secondary increases in the incidence and severity of infections, growth

failure and secondary nutritional stunting, and abnormalities of neurobehavioral development.

Hence, as a conclusion both of the sample A and B are not suitable use for drinking

because the present of heavy metal. The water samples must be treated before it has been usingby human in order to avoid the deseases. Some of the method are suggest to ensure the amount

of metal in drinking water are comply with the water quality standard which is the water tested

for zinc and other metals. The public water systems also should test for zinc on a regular basis.

Otherwise, adding more tests especially to determine the concentration of toxic metals such as

mercury, and reactive metals such as potassium to the samples of water.

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8. REFERENCES

Douglas, H. S. (2007). Principles of Instrumental Analysis. USA: THOMSON BROOKS/COLE.

Sherman, C.-P. (n.d.). Separation Sciences Research and Product Development.InfraredSpectroscopy , chepter 15.

Silverstein, W. D. (2005). Spectrometric Identification of Organic Compounds. New York:

Wiley.

Williams, F. (2008). Spectroscopic Method in Organic Chemistry. New York: McGraw-Hill.

Internet

http://www.thermo.com/com/cda/article/general/0,,1147,00.html

http://www.labmate-online.com/news/chromatography-and-spectroscopy/1/thermo-fisher-

scientific/affordable-icp-for-everyone/5990/

http://www.jobinyvon.com/usadivisions/Emission/applications/TN12.pdf