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J12ANM ANALYTICAL MEASUREMENT

Lab Activity 1: Determination of Copper Concentration in a Wastewater Sample Group no. Group members (name and i.d.) (1) (2) (3) (4)

Date Time 1. Background


The purpose of this experiment is to determine the degree of contamination by copper in a simulated wastewater sample. Atomic absorption spectrometry (AAS) is widely used for the analysis of metals at the trace element level as it is a relatively simple technique and can be a low cost form of analysis. Depending upon the dissolution method used, detection limits in the order of a few part per million in a wastewater or soil sample should be achievable. Although there are many circumstances where these detection limits are not sufficiently low, for a pollution monitoring exercise as outlined below, these detection limits should be adequate. By the time you have completed this experiment, you should understand the basic principles of atomic absorption spectrometry; you should also appreciate some of the problems related to the restricted linear range of the calibration curves used. In addition, you should have an understanding on the role of instrument conditions, such as wavelength selection, slit ratio and burner angling in analysis and how these conditions can be adjusted to enable more efficient analyses. Overcoming some of the restrictions that these phenomena impose on cation analysis in general by AAS should also be apparent. There are three parts of the practical outlined in the experimental procedure. The first part involves the calibration experiment. In the second part, you will analyse a number of wastewater samples and determine their respective concentrations. The third part focuses on instrument condition variation, including wavelength selection, slit ratio and burner angle experiment. You should liaise together to discuss your results. All sets of results are necessary for a complete understanding of the technique, and for calculating the concentration of copper in the wastewater.

2. Objectives
(1) To perform a calibration experiment using standard solutions. (2) To determine the concentrations of copper found in wastewater samples. (3) To investigate the effect of instrument condition variations on the readings produced.

3. Materials
standard solution of copper in deionised water simulated wastewater samples of copper chloride dihydrate in deionised water graph papers

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4. Experimental Procedure:
4.1 Standard solution preparation
(1) A stock copper ion solution is provided, prepared by dissolving pure copper ion solution in deionized water. (2) 5 sets of standard solutions are prepared from the stock solution, labelled as AF accordingly. (3) Perform calibration experiment using these samples, list the corresponding concentrations in section 5 (Results and Discussion).

4.2

Standard Operating Procedure (SOP) for the operation of AAS


Important note: you will be given a briefing and demonstration by the lab technician/ research assistant prior to operating the instrument. DO NOT attempt to start operating the equipment without having been briefed first.

(1) Identify the main components involved: a. Fuel gas b. Oxidant c. Instrument d. Blower e. Lamp f. Flame location (2) Close the air release valve of the compressor. (3) Turn on the acetylene gas by turning the knob anti-clockwise. (4) Switch on the power supply for air compressor. (5) Switch on the AAS instrument. (6) Turn on the blower (to remain on during the course of experiment). (7) Open the software WinLab32 a. Window will show system status wait till green light comes on. (8) Create work station. a. Flame b. Manual analysis control c. Lamp set up choose lamp (9) Create a new method. a. File New Method b. Starting condition c. Element choose element, then click OK d. Method Editor define element i. Spectrometer do not change ii. Sampler do not change iii. Calibration iv. File save as name (10) To start, go to: open method lamp station (11) Flame control: on (12) Manual analysis control: analyse blank (13) Insert sampling tube into Standard 1 click analyse standard a. When result appears, remove tube, re-insert into water to rinse sample residue. (14) Repeat step (13) until all samples are analysed. (15) To stop the experiment: a. Turn off flame b. Turn off lamp c. Switch off instrument d. Turn off acetylene and compressor e. Release air from compressor.

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5.

Results and Discussion


Table 1: Default instrument settings.
Fuel gas Oxidant Lamp type Wave length (unit?) Slit ratio Burner position Calibration method Background correction

Table 2: Calibration data (with default setting) set I.


Standard solution Blank A B C D E F Concentration

Table 3: Calibration data (with default setting) set II.


Standard solution Blank W X Y Concentration

Table 4: Concentrations of copper in wastewater samples (with default setting).


Wastewater sample Concentration (displayed by instrument) Actual Concentration

H J K L M *Note: the samples used in the AAS analyses have been diluted. You need to determine the actual concentrations based on the dilution factor used.

Table 5: Wavelength selection.


Wave length Slit ratio

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Table 6: Calibration data (with new WL setting).


Standard solution Blank W X Y Concentration

Table 7: Concentrations of copper in wastewater samples (with new WL setting).


Wastewater sample H J K L M Concentration (displayed by instrument) Actual Concentration

Comment on linearity:

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Comment on the effects of instrument condition variation to the results produced. (1) Wavelength

How can the sensitivity be adjusted? What are your recommendations to achieve the most efficient analysis?

Calculations:

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