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ANKLESHWAR TEST METHOD FOR FINISHED GOODS DOCUMENT NO. TM.NO.22.01.312 Rev. : 1.

0 TITLE: TOTAL EXCHANGE CAPACITY IN CHLORIDE FORM.

PROCEDURE FOR DETERMINATION OF TOTAL EXCHANGE CAPACITY A. Requirement 1. Resin Testing Column. 2. 1% NaNO3, 5 % K2CrO4, 0.1 N AgNO3. B. Procedure 1. Take about 40 ml of resin sample in 50 mm dia resin testing column. Pass 1 liter of 7% HCl at a flow rate of about 15 ml/min. Rinse with D.M. water till effluent water shows chloride less than 30 ppm. (To 50 ml effluent add 2 ml of nickel nitrate buffer and 2 ml of diphenyl carbazone and titrate with 0.02 N mercuric nitrate, till the colour changes from green to blue (V ml). Carry out a blank titration with 50ml D.M. water (B ml). (V-B) should not be more than 1.5 ml.) Note: If pre-treated sample is available this step may be omitted. 2. Measure accurately 25 ml (Minimum Vibrated Volume) of pretreated resin and transfer it back to the column. 3. Pass 500 ml of 1% NaNO3 solution at a flow rate of 15 ml/min and collect the effluent in a 500 ml volumetric flask till it is filled upto the mark. Mix thoroughly. Note: Preserve same column if SBC to be done. 4. Pipette out 25 ml aliquot of the effluent in a 250 ml titration flask and titrate against 0.1 N standard AgNO3 solution using 5% K2CrO4 solution as the indicator. End point is change of colour of supernatant liquid from yellow to red orange that persists for 30 seconds under vigorous swirling. Note the reading (R ml). 5. Calculate Total Exchange Capacity as follows : Total Exchange Capacity (meq/ml) = R x N x 0.8 Total Exchange Capacity (meq/lts.) = R x N x 800 Total Exchange Capacity (Kg CaCO3/M3) = 40 x R x N Where, "R" = Reading in ml. (Step 4). "N" is the normality of AgNO3 solution. 6. Record the observations in Wb.22.01.00.08 and report in Fm.22.01.00.08. Enter the results in Rg.22.01.00.04

ISSUED BY DATE DEPARTMENT IN-CHARGE

APPROVED BY WORKS MANAGER

EFFECTIVE 20.08.2003 Page No. 1 of 1 ANKLESHWAR

TEST METHOD FOR FINISHED GOODS DOCUMENT NO. TM.NO.22.01.308 Rev. : 1.0

TITLE: % MOISTURE HOLDING CAPACITY IN CHLORIDE FORM.

PROCEDURE FOR DETERMINATION OF % WATER REGAIN (WR) / % MOISTURE HOLDING CAPACITY. A. Requirement 1. Sintered glass tubes. 2. Centrifuge. 3. 15 mm resin testing column. 4. 7% HCl, 0.02 N mercuric nitrate, nickel nitrate buffer, Diphenyl carbazone. B. Procedure 1. Take about 40 ml of resin sample in 15 mm dia resin testing column. Pass 1 liter of 7% HCl at a flow rate of about 15 ml/min. Rinse with D.M. water till effluent water shows chloride less than 30 ppm. (To 50ml effluent add 2ml of nickel nitrate buffer and 2ml of diphenyl carbazone & titrate with 0.02 N mercuric nitrate, till the colour changes from green to blue (V ml). Carry out a blank titration with 50ml D.M.water (B ml). (V-B) should not be more than 1.5 ml.) 2. Transfer about 1 gm of pretreated sample in a preweighted (T) sintered glass tube of porosity G-2. (Note: i.Carry out analysis in triplicate. ii.Preserve the remaining sample, if TEC to be done.) 3. Centrifuge at 2000 rpm for 20 minutes to remove unbound water from the resin sample. Weigh (TW). 4. Cover the top of the tube with a small piece of nylon mesh. (This is essential to avoid mechanical loss of resin during subsequent drying.) 5. Keep the centrifuge tubes in the vacuum oven for drying at 115 + 5C for 2 hours & 30 minutes. Cool in a desiccator and reweigh (TD). 6. Calculate Water Regain as follows : (TW - TD) WR (g/g) = -------------(TD - T) % Moisture Holding Capacity 1 + WR WR = -------------- x 100

7. Record the observations in Wb.22.01.00.08 calculate the mean of nearest two values. If the difference in two set of values is same calculate the mean of all the three values. Report mean value in Fm.22.01.00.08 and Enter the results in Rg.22.01.00.04.

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EFFECTIVE 20.08.2003 Page No. 1 of 1 ANKLESHWAR

TEST METHOD FOR FINISHED GOODS DOCUMENT NO. TM.NO.22.01.319 Rev. : 1.0

TITLE: STRONG BASE CAPACITY.

PROCEDURE FOR DETERMINATION OF STRONG BASE CAPACITY (SBC) A. Requirement: 1. 7% HCl, 7% NH4OH or 5% NaOH, 5% NaCl. A. Procedure 1. After determining total exchange capacity, convert the resin back to chloride form by passing 1 liter of 7% HCl at a flow rate of 15 ml/min. Rinse with D.M. water till effluent shows chloride less than 30 ppm. (To 50 ml effluent add 2 ml of nickel nitrate buffer and 2 ml of diphenyl carbazone and titrate with 0.02 N mercuric nitrate, till the colour changes from green to blue (V ml). Carry out a blank titration with 50 ml D.M. water (B ml). (V - B) should not be more than 1.5 ml.) 2. Pass 200 ml of 7% ammonia solution, or 5% caustic solution through the column at a flow rate of 15 ml/min. Rinse with D.M. water till the effluent is neutral to phenolphelein (pH < 10). 3. Pass about 200 ml of 5% NaCl solution at the rate of 15 ml/min. Rinse with D.M. water till effluent water shows chloride less than 30 ppm ( Tested as per in step 1.) 4. Pass 500 ml of 1% NaNO3 solution at the rate of 15 ml/min. Collect the effluent in a 500ml volumetric flask till it is filled up to the mark. Mix the contents thoroughly. 5. Pipette out 25 ml aliquot in a 250 ml titration flask and titrate against 0.1 N AgNO3 solution using K2CrO4 indicator. Note the reading (R ml). 6. Calculation Strong base capacity = R x N x 0.8 (meq/ml) Strong base capacity = R x N x 800 (meq/litre)

Where, R = Reading in ml. (Step - 5) N = Normality of AgNO3 solution. % SBC = SBC (meq/litre) ---------------------- x 100 TEC (meq/litre)

7. Record the observations in Wb.22.01.00.08 and report in Fm.22.01.00.08. enter the results in Rg.22.01.00.04.

ISSUED BY DATE DEPARTMENT IN-CHARGE

APPROVED BY WORKS MANAGER

EFFECTIVE 20.08.2003 Page No. 1 of 1

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