Apparatus Beakers (100/200 mL), graduated cylinder ( 10 mL ), volumeric flasks ( 100 mL and 250 mL ), pipet (50/10/5/2 mL), heating

mantel, water bath, analytical balance, UV/Vis Spectrometer, distilled water.

Chemicals KMnO4 (0.01 M, pre-prepared in the lab), Sodium Bisulfite (NaHSO3), Sulfuric acid (H2SO4, concentrated), Nitric acid (HNO3, concentrated), Ammonium peroxodisulfate / ammonium persulfate ((NH4)2S2O8), Fosforic acid (H3PO4, 85%), Potassium periodate (KIO4), Potassium Nitrite (KNO2), sample: Steel wool

Procedure A) Preparation of sample Three sets of steel wool sample was weighed about 0.1 g (to nearest 0.1 mg) in 250 mL beakers. The exact weight was recorded respectively. The sample was dissolved in 40mL of water and 10 mL of concentrated HNO3 and was boiled in the fume hood for 2 minutes. The mixture was cooled and added 0.5 g of (NH4)2S2O8 cautiously. The mixture was gently heated for 10 minutes. A pinch of sodium bisulfite was added to the pink solution and is heated for few more minutes. Then, 100 mL of distilled water was added into the mixture respectively.

B) Preparation of Stock and Standard Solutions Preparation of KMNO4 solution (~110 ppm): the 50 mL of KMnO4 was pipetted into a beaker. A little of NaHSO3 in 2 mL concentrated H2SO4 was added into the beaker until the purple color of KMNO4 decolorize. Then, the mixture was heated to boil in the fume cupboard to release SO2. Next, the mixture was transferred into 250 mL volumetric flask and was dilute to the mark. The volume of Mn stock was calculated to prepare the 5 series of the standards. The table 1.0 shows in the results. The volume as calculated for each standard was pipetted into 200 mL beakers. 100 mL if distilled water was approximately added to each standards.

C) Treatment of Samples and Standards 10 mL H3PO4 (85%) and 0.5 g KIO4 was added into the sample and standards as prepared in A and B. The mixture was boiled for 2 minutes and continued for 5 minutes. The sample and

standards were cooled at room temperature. Then, each mixture was transferred into 250 mL volumetric flask and diluted until mark by distilled water. The sample was dilute again into 100 mL volumetric flask with ratio 1:5. The sample was diluted with distilled water until mark. 10 mL of the most colored sample was measured into a small beaker. The interferences was corrected from Cr (IV) by adding a few drops of KNO2 until the color of permanganate disappears. The solution was used as a reference when measuring the absorbance of the sample.

D) Measurement The absorbance of the standards solutions was measured using distilled water as a BLANK. While, the absorbance of the sample was measured using the solution prepared in part C2 as a BLANK. The samples were dilute because the readings of absorbance do not fall in the range of the standards. A calibration graph of absorbance versus concentration was constructed and the concentration of Mn in the each sample was determined. The average, standard deviation and the percentage of Mn in the steel wool sample was calculated and the result showed in the calculation part.

Result and calculation

A. Preparation of sample Table 1: Weight of Triplicate Sample Steel Wool Replicate samples Weight of steel sample 1 0.1023 2 0.1021 3 0.1002

B. Preparation of stock and standard solution Dilution of 110 ppm stock solution into 4 ppm M1V1 = M2V2 110 ppm (V1) = 4 ppm (250 mL) = 4 (250) V1 = 9.09 mL M1V1 = M2V2 M1 (250) mL = 110 ppm (1 mL) = 110 (250) M1= 0.44ppm

Table 2: Volume of Mn needed for preparation of Standards Solutions

Concentration (ppm) 0.44 1.32 2.20 3.08 3.96

Volume Mn needed (mL) 1 3 5 7 9

C. Measurement Table 3: Absorbance reading for Sample and Standards Solutions

Concentration (ppm) Blank 0.44 1.32 2.20 3.08 3.96 Blank Sample Sample 1 Sample 2 Sample 3

Absorbance 0.00000 0.00613 0.05954 0.08064 0.12474 0.13374 0.06325 0.05531 0.05728 0.04970

Graph 1: The graph shown absorbance against concentration.

Graph of absorbance versus concentration

0.16 0.14 0.12 Absorbance 0.1 0.08 0.06 0.04 0.02 0 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 Concentration y = 0.0365x + 0.0005 R = 0.9695

From the graph the equation: y= 0.0365x + 0.0005

Sample 1, the absorbance, y = 0.05531 0.05531= 0.0365x + 0.0005 x= 1.5017 ppm Therefore, the concentration of Mn for sample 1= 1.5017 ppm The concentration of Mn for sample 2 = 1.5556 ppm The concentration of Mn for sample 3= 1.3479 ppm x DF Dilution Factor = Final volume / Initial volume = 250mL / 50mL =5 Therefore, the concentration of Mn for sample 3 = 1.3479 x 5 = 6.7397 ppm

Mass of Mn in each sample:

Replicate 1: 1.5017 mg/L x 0.25L x (1/1000) g/mg = 3.7543 x 10-4 g Replicate 2: 3.8890 x 10-4 g Replicate 3: 1.6849 x 10-3 g

Average: [(3.7543 x 10-4 g + 3.8890 x 10-4 g + 1.6849 x 10-3 g) / 3] = 8.1621 x 10-4 g

Percentage Mn of Steel Sample:

-4 Replicate 1: 3.7543 x 10 g x100% 0.37%

0.1023g

4 Replicate 2: 3.8890x10 g x100% 0.38%

0.1021g

-3 Replicate 3: 1.6849 x 10 g x100% 1.68%

0.1002g