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FACULTY OF CHEMICAL ENGINEERING ABSTRACT

May 2, 2013

The experiment was conducted in order to determine whether selections of water samples are safe to drink. There are 2 water samples that being tested which are sample A and sample B. Sample A is simulated waste water which contained Zn element, while sample B is simulated waste water which contained Co element. This experiment was conducted by using Inductively Coupled Plasma (ICP) Mass Spectrometry. Before the experiment, we need to prepare stocks solution of ZnCl2 . 2H2O :100 ppm in 100mL conical flask. A stock solution is a concentrate, that is, a solution to be diluted to some lower concentration for actual use. We may use just the stock solution or use it as a component in a more complex solution (D. R. Caprette, 2005). Thus, a series of standard solution of 40 ppm, 25 ppm, 12.5 ppm and 6.25 ppm can be prepared. A standard solution is a solution of accurately known concentration prepared from a primary standard (a compound which is stable, of high purity, highly soluble in water and of a high molar mass to allow for accurate weighing) that is weighed accurately and made up to a fixed volume (RSC, n.d.). Using the Inductively Coupled Plasma (ICP) Mass Spectrometry, ICP 6000 series, the composition of the sample can be analysed. The results taken were interpreted into a graph of IR vs concentration.

FACULTY OF CHEMICAL ENGINEERING INTRODUCTION

May 2, 2013

Water is the common name applied to the liquid form (state) of the hydrogen and oxygen compound H2O. Pure water is an odourless, tasteless, clear liquid. Water is one of nature's most important gifts to mankind. (Quiles D et al, n.d.). Water is an essential part of human lives. Water contaminated with heavy metal 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 fresh water animals. Toxic metals can be present in industrial, municipal, and urban runoff, and by definition, are harmful to humans and aquatic biota. Increased urbanization and industrialization have increased the levels of trace metals, especially heavy metals, in waterways. There are over 50 elements that can be classified as heavy metals, but only 17 that are considered both very toxic and relatively accessible. Mercury, lead, arsenic, cadmium, selenium, copper, zinc, nickel, and chromium, however, should be given particular attention in terms of water pollution and discharge effects. Toxicity levels depend on the type of metal, its biological role, and the type of organisms that are exposed to it (Ohio State, n.d). Zinc is naturally present in water. The World Health Organization have stated a legal limit of 5 mg Zn2+/L. Zinc salts cause a milky turbidity in water in higher concentrations. Additionally, zinc may add an unwanted flavour to water. This occurs at concentrations of about 2 mg Zn2+/ L. The solubility of zinc depends on temperature and pH of the water in question. When the pH is fairly neutral, zinc in water insoluble. Solubility increases with increasing acidity. Above pH 11, solubility also increases. Industrial wastewaters containing zinc stem from galvanic industries, battery production, etc. Zinc leaks from zinc pipes and rain pipes, consequential to circulation of carbon rich water. Zinc compounds are present in fungicides and insecticides, and consequently end up in water. When inadequate safety measures are taken, zinc may be emitted from chemical waste dumps and landfills, or from dredge mortar (Lenntech B.V, n.d).

FACULTY OF CHEMICAL ENGINEERING

May 2, 2013

Cobalt is a hard ferromagnetic, silver-white, hard, lustrous, brittle element. It is a member of group VIII of the periodic table. Cobalt is stable in air and unaffected by water, but is slowly attacked by dilute acids. Most of the Earth's cobalt is in its core. Cobalt is of relatively low abundance in the Earth's crust and in natural waters, from which it is precipitated as the highly insoluble cobalt sulfine CoS. Cobalt is not found as a free metal and is generally found in the form of ores. Cobalt is usually not mined alone, and tends to be produced as a by-product of nickel and copper mining activities. Cobalt cannot be destroyed once it has entered the environment. It may react with other particles or adsorb on soil particles or water sediments. Cobalt will only mobilize under acidic conditions, but ultimately most cobalt will end up in soils and sediments (Lenntech B.V, n.d).

In this experiment, we used Indcutively Coupled Plasma (ICP) Mass Spectrometry to analyse the samples. An inductively coupled plasma (ICP) is a very high temperture (7000-8000K) excitation source that efficiently desolvates, vaporizes, excites, and ionizes atoms. Molecular interferences are greatly reduced with this excitation source but are not eliminated completely. ICP sources are used to excite atoms for atomic-emission spectroscopy and to ionize atoms for mass spectrometry (Brian M, 2000).

AIM To to determine whether selections of water samples are safe to drink.

THEORY The analysis of wastewater for trace metal contamination is an important step in ensuring human and environmental health. Wastewater need to be measured for a variety of metals at different concentrations, in different wastewater matrices. A variety of inorganic techniques can be used to measure trace elements in waste water including atomic absorption spectroscopy (AAS), inductively coupled plasma optical emission spectroscopy (ICP-OES) and ICP mass spectrometry (ICP-MS).ICPOES is a good match with the productivity requirements of many laboratories and requires only a moderate investment. (Praveen Sarojam ,USA) Inductively coupled plasma-optical (or atomic) emission spectrometry (ICP-OES or ICP-AES) is an analytical technique used for determination of trace metals. This is a multi-element technique which uses a plasma source to excite the atoms in samples. These excited atoms emit light of a characteristic wavelength, and a detector measures the intensity of the emitted light, which is related with the concentration. (Geoff Tyler, French) 3

FACULTY OF CHEMICAL ENGINEERING EXCITED STATE

May 2, 2013

HV

GROUND STATE Figure 1: The excitation of atom (Thomas J. Manning and William Grow, Valdosta)

Samples are heated through 10000 C to atomize effectively which is an important advantage for ICP technique. Another advantage is multi element analysis. With ICP technique, 60 elements can be analysed in single sample run less than a minute simultaneously, or in a few minutes sequentially. Besides instrument is only optimized for one time for e set of metal analysis. High operating temperature lowers the interferences. Determinations can be accomplised in wide lineer range and refractory elements can be determined at low concentrations (B, P, W, Zr, U). On the other hand consumption of inert gas is very much higher than AAS techniques which cause high operating costs. ICP instruments can be axial and radial according to their plasma configuration. In radial configuration, the plasma source is viewed from the side. Emissions from axial plasma are viewed from horizontally along its length, which reduces background signals resulting in lower detection limits.The block diagram of ICP-OES is depicted in Figure 2. Generally, radio frequency (RF) powered torch as a source, polychromators as a wavelength selector, photomultiplier (PMT) or charge capacitive discharged arrays (CCD) as a detectors are used. (AsliBaysal, Nil Ozbek and SuleymanAkman)

Figure 2: Block Diagram of ICP-OES

FACULTY OF CHEMICAL ENGINEERING

May 2, 2013

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. Most analytical plasmas operate with pure argon or helium, which makes combustion.(Thomas J. Manning and William Grow, Valdosta)

1. Sample Preparation: Some samples require special preparation steps including treatment with acids, heating, and microwave digestion.

2. Nebulization: Liquid converted to aerosol.

3. Desolvation/Volatization: Water is driven off, and remaining solid and liquid portions are converted to gases.

FACULTY OF CHEMICAL ENGINEERING

May 2, 2013

4. Atomization: Gas phase bonds are broken,and only atoms are present. Plasmatemperature and inert chemical environmentare important at this stage.

5. Excitation/Emission: Atoms gain energy from collisions and emit light of a characteristic wavelength. 6. Separation/Detection: A grating dispersers light that is quantitatively measured.

Figure 3: Steps involve in the analysis of aqueous samples by ICP-OES (Thomas J. Manning and William Grow, Valdosta)

The main analytical advantages of the ICP over other excitation sources originate from its capability for efcient andreproducible vaporization, atomization, excitation, and ionization for a wide range of elements in various sample matrices. This is mainly due to the high temperature, 60007000 K, in the observation zones of the ICP. This temperature is much higher than the maximum temperature of ames or furnaces (3300 K). The high temperature of the ICP also makes it capable of exciting refractory elements, and renders it less prone to matrix interferences. Other electrical-dischargebased sources, such as alternating current and direct current arcs and sparks, and the MIP, also have high temperatures for excitation and ionization, but the ICP is typically less noisy and better able to handle liquid samples. In addition, the ICP is an electrode less source, so there is no contamination from the impurities present in an electrode material. Furthermore, it is relatively easy to build an ICP assembly and it is inexpensive, compared to some other sources, such as a LIP. The following is a list of some of the most benecial characteristics of the ICP source such as low background emission, relatively low chemical interference, high stability leading to excellent accuracy and precision, applicable to the refractory elements and cost-effective analyses. (Geoff Tyler, France)

FACULTY OF CHEMICAL ENGINEERING MATERIAL AND APPARATUS:

May 2, 2013

Material: ZnCl2.2H2O Sample A ( simulated waste water containing Zn element) Sample B ( simulated waste water containing Co element) Distilled water

Apparatus: iCAP 6000 Series Conical flask (50 ml and 100 ml) Analytical balance Burete

PROCEDURE: 1. Zinc chloride is weighted accuratelyabout 0.0021mg for sample processing. 2. Mixed the zinc with the distilled water in the 100ml flask until it reach the level of the meniscus. The solution is called as stock solution. 3. Then, shake the solution properly. 4. Measure the volume of stock solution that we had calculated before this for 40 ppm, 25 ppm, 12.5 ppm and 6.25 ppm by using buret. The volume of the solutions that we measured is called as standard solutions. 5. Every standard solution is put in the 50ml flask and distilled water is used until the solutions reach the level of meniscus. 6. Blank water is put in the test tube of the ICP 6000 series and three quarter for every solution also is put there. 7. Then put the sample of waste water in the test tube A and B as references. 8. ICP 6000 series will analysis for each of the sample. 9. The reading of the sample showed in the computer.

FACULTY OF CHEMICAL ENGINEERING RESULTS:

May 2, 2013

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FACULTY OF CHEMICAL ENGINEERING CALCULATION: Stock solution used is:- ZnCl2.2H2O = 100 ppm = 0.0021 g

May 2, 2013

Preparation of standard solution: a) 40 ppm M1V1 (100)(V1) V1 = M2V2 = (40)(50) = 20 mL

20 mL of 100ppm is transferred into 50mL volumetric flask and diluted with distilled water. b) 25 ppm M1V1 (100)(V1) V1 = M2V2 = (25)(50) = 12.5 mL

12.5 mL of 100 ppm is transferred into 50 mL volumetric flask and diluted with distilled water. c) 12.5 ppm M1V1 (100)(V1) V1 = M2V2 = (12.5)(50) = 6.25 mL

6.25 mL of 100 ppm is transferred into 50 mL of volumetric flask and diluted with distilled water. d) 6.25 ppm M1V1 (100)(V1) V1 = M2V2 = (6.25)(50) = 3.125 mL

3.125 mL of 100 ppm is transferred into 50 mL of volumetric flask and diluted with distilled water.

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FACULTY OF CHEMICAL ENGINEERING DISCUSSION:

May 2, 2013

Water is an essential part of our lives. Thus, we are conducted an experiment to determine the concentration of the heavy metal that contain in the waste water and directly to conclude either the water that we collect from the unknown location are safe to drink or not. To achieve the objectives, we had prepared the standard solution from the stock solution which concentration is 100ppm. Stock solution can be known as the primary solution which has high purity of the solution. While for the standard solution, it can be defined as the solution that prepared with the certain amount of concentration from the stock solution. From the result, the correlation that had been calculated is 0.9746 and it show that there are deviation between the concentration of standard solution that we prepared which are 100 ppm, 40 ppm, 25 ppm. 12.5 ppm and 6.25 ppm. Based on the theory, the best correlation is 0.9999 which show the almost accurate concentration of standard solution. By the calibration curve that plotted based on the concentration of standard solution, the concentration of the samples also can be known if the concentration is under a range of 6.25 ppm until 100 ppm. From the data collected, the solutions are sucked into the analytical instrument for 3 times and the average of data is calculated. Based on the data, the sample 1 recorded that the average concentration is 39.817 ppm where the reading of concentration 1, 2 and 3 are 41.137 ppm, 39.3345 ppm and 38.9795 ppm respectively. While for the data of sample 2 recorded that the average concentration of zinc in the waste water is 0.751211 ppm. The concentration 1, 2 and 3 that are recorded are 0.792233 ppm, 0.73197 ppm and 0.72943 ppm respectively. Thus, compare the concentration of zinc between two samples that are collected from an unknown location, it showed that the sample 2 had lowest concentration of zinc in the water samples which are 0.792233 ppm in contrast with sample 1 that had higher amount of zinc which is 39.817 ppm. Furthermore, we can conclude that the sample 2 is classified as a safe drink because the amount of heavy metal in the waste water is not more than 3.00 ppm which are stated at the WHO (World Health Organization). While the sample 1 cannot be drink and not allowed to used because it had higher concentration of heavy metal that affect our health. This is due to the higher concentration of heavy metal such as zinc it can contribute negative effects on our health and ecosystem.

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MALAYSIAN STANDARDS PARAMETERS

NATIONAL

DRINKING

WATER

QUALITY

MANDATORY STANDARD SHOULD NOT MPN/100ml EXCEED 10

HEALTH INVESTIGATION

TEST METHODS

COLIFORM ORGANISM

SHOULD NOT BE DETECTABLE IN 2 CONSECUTIVE SAMPLES THROUGHOUT A YEAR, 95% OF COLI FORM IN 100ml USING MEMBRANE FILTER METHOD ARITHEMATIC MEAN OF ALL MONTHLY SAMPLES IS 1 COLONY/100ml NOT MORE THAN 4 COLONIES/100ml IN 2 CONSECUTIVES SAMPLES E. COLI ABSENT IN 100ml SAMPLE FAECAL STREP TOCCOCI ABSENT CL. PERFRINGES " VIRUSES " 1 (a) 1(b) RECOMMENDED STANDARD 5 5 7.0 - 8.5 MANDARATORY STANDARD 5 15 6.5 - 8.5 0.1

20 MPN/100ml

AS RECOMMENDED IN STANDARD METHODS OF EXAMINATION ALPHA AND AWWA LATEST EDITION

2/100ml

HEALTH INVESTIGATION LEVEL

TURBIDITY (NTU) COLOUR (TCU) pH TEMPERATURE Sp. CONDUCTANCE DISSOLVED OXYGEN RESIDUAL CHLORINE TOTAL DISSOLVED SOLIDS CCE CHLORIDE (CI) ANIONIC DETERGENT (MBAS) AMMONIA (N) NITRATE (N) IRON AS Fe FORRIDE AS F

6.5 - 9.2 -

200 0.2 0.1 -

0.5 250 1 0.5 10 0.3 1.5

600

10 5 14

FACULTY OF CHEMICAL ENGINEERING HARDNESS AS Ca CO3 ALUMINIUM (AI) MERCURY (Hg) CADMIUM (Cd) SELENIUM (Se) ARSENIC (As) CYANIDE (CN) LEAD (Pd) CHROMIUM (Cr) SILVER (Ag) COPPER (Cu) MANGANESE (Mn) MAGNESIUM (Mg) ZINC (Zn) SODIUM (Na) SULPHATE (SO4) PHOSPHATE (PO4) HYDROGEN SULPHIDE (H2 S) MINERAL OIL PHENOL CHLOROFORM BIOCIDES (TOTAL) PESTICIDES ALDRIN/ DIELDRIN CHLORODANE 24D DDT HEPTACLOR & HEPTACHLOR EXPOXIDE HEXACHLOROBENZENE LINDANE METHOXYCHLOR RADIOACTIVITY GROSS GROSS 100 0.2 0.01 0.001 0.1 Bg/1 1 Bg/1 500 0.2 0.001 0.005 0.01 0.05 0.1 0.05 0.05 0.05 1 0.1 150 5 200 400 -

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0.001 0.005 0.01 0.05 0.1 0.05 0.05 0.05 10

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ND 0.3 0.002 0.03 0.1 0.00003 0.1 0.1 0.001 0.0001 0.000001 0.003 0.03 0.1 Bg/1

0.03 0.1

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FACULTY OF CHEMICAL ENGINEERING CONCLUSIONS:

May 2, 2013

Based on the calibration curve, the curve that obtained are not linear. The calibration is supposed to be linear and the correlation expected is 0.9999. But, from the experiment, the correlation that we got is 0.9746. To make sure that the graph can be linear and the correlation is near to 0.9999, the concentration range must be conducted between 6.25 ppm to 33.00 ppm. The concentration of zinc in water sample 1 is higher than the concentration of zinc in water sample 2. The concentration of zinc in water sample 1 is 39.817 ppm while the concentration of zinc in water sample 2 is 0.792233 ppm. This is shows that the water sample 1 has higher heavy metal content in the unknown waste water which is it not safe to use and drinks. In the other hand, the water sample 2 has lower heavy metal content is safe to drink due to the concentration of zinc in the water sample that is not more that 3.00 ppm.

REFERNCES:

Ministry of health malaysia (2000, December). National standard for drinking water quality. Retrieved from

https://www.google.com.my/url?sa=t&rct=j&q=&esrc=s&source=web&cd=5&cad=rja&v ed=0CGAQFjAE&url=http%3A%2F%2Fwww.forumair.org.my%2Fv1%2Findex.php%3Fopti on%3Dcom_phocadownload%26view%3Dcategory%26download%3D45%3Adrinkingwater-quality.pdf%26id%3D2%3Awater-campaignbrochures%26Itemid%3D62&ei=fleBUfyHFo3wrQezroDAAQ&usg=AFQjCNGNdFQSoQPu VN_CDzG18EcwQacHlg&sig2=2j1nM1kKQlsscGToYfVRug

Asli Baysal, N. O. (n.d.). Determination of Trace Metals in Waste Water and. Retrieved April Wednesday, 2013, from http://cdn.intechopen.com/pdfs/41608/InTechDetermination_of_trace_metals_in_waste_water_and_their_removal_processes.pdf Geoff Tyler. (n.d.). ICP-OES, ICP-MS and AAS Techniques Compared. Retrieved April Wednesday, 2013, from http://www.jobinyvon.com/usadivisions/Emission/applications/TN05.pdf MANNING, T. J. (n.d.). InductivelyCoupled Plasma -Atomic EmissionSpectrometry. Retrieved April Wednesday, 2013, from http://www.scribd.com/doc/5363861/icp

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Sarojam, P. (n.d.). Analysis of Waste Water by using ICP-OES. Retrieved April Wednesday, 2013, from http://www.perkinelmer.com/CMSResources/Images/4474211APP_MetalsinWastewater.pdf Tyler, G. (n.d.). Jobin Yvon S.A.S, Horiba Group. Retrieved April Wednesday, 2013, from http://www.jobinyvon.com/usadivisions/Emission/applications/TN05.pdf Lenntech BV. Cobalt Co. Retrieved http://www.lenntech.com/periodic/elements/co.htm April 30, 2013, from

M. B. (2000). Inductively-Coupled Plasma (ICP) Excitation Source. The Chemistry Hypermedia Project. Retrieved April 30, 2013, from http://www.files.chem.vt.edu/chem-ed/spec/atomic/emission/icp.html OHIO State. Measures of Toxic Metals in Water. Retrieved April 30, 2013, from http://tycho.knowlton.ohio-state.edu/heavyinfo.html Sandi, D. Q. The Importance of Water. Alpha Omega Marketing. Retrieved April 30, 2013, from http://www.aomega.com/mpure/water.htm Lenntech BV. Zinc (Zn) and water. Retrieved April 30, http://www.lenntech.com/periodic/water/zinc/zinc-and-water.htm 2013, from

Caprette, D. R. (2005, May 20). Working with Stock Solutions. Retrieved May 1, 2013, from http://www.ruf.rice.edu/~bioslabs/methods/solutions/stocks.htm Royal Society of Chemistry. Standard Solutions . Retrieved May 1, 2013, from http://chem-ilp.net/labTechniques/StandardSolutions.htm

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FACULTY OF CHEMICAL ENGINEERING APPENDIX:

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