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IS converted to C02 under the Instrument conditions 3.4 The system blank IS the value obtained 10 8 2 fpr an Irradiated, recirculated reagent distilled water sample 4. Sample Handling and 'Preservation 4.1 Sampling and storage of samples must be clone In glass bottles Caution Do not leave any headspace 10 the sample bottle as thiS may contribute to loss of purgeable organics 4 2 Because of the POSSibility of OXidation or bactenal decomposition of some components of aqueous samples, the lapse of tIme between collection of samples and start of analysIs should be kept to a minImum Also, samples should be kept cool (4°C) and protected from sunlight and atmosphenc oxygen 4 3 When analYSis cannot be performed within two hours from time of sampling. the sample should be acidlfled to pH 2 with H2S04 Note HCr should not be used because It IS converted to chlorine dunng the analysIs This causes damage to the Instrument 6. Interferences 6.1 If a sample IS homogenized to reduce the size of the particulate matter, the homogenizing may cause loss of purgeable organic carbon, thus yielding erroneously low results 6. Apparatus 6.1 Apparatus for blending or homogeniZing samples A household blender or similar deVice that Will reduce particles in the sample to less than 02 mm 6.2 Apparatus for Total Organic Carbon' The essential components for the apparatus used In thiS method are A sparge assembly, flow SWitching valves. a pyrolYSIS furnace, quartz ultraviolet reactor cOil, redUCing column, flame Ionization detector, electrometer and Integrator ThiS method IS based on the Dohrmann Envlrotech DC-54 Carbon Analyzer Other Instruments having Similar performance characterrstlcs may be used when analyzmg samples with eaSily purgeable organics so as to minimiZe losses carbonate-bicarbonate stock solution 10 a 100 mL volumetrrc flask and dilute to the mark With reagent distilled water (7 1) 8 Procedure 8 1 Allow at least 30 mmutes warm-up time Leave mstrument console on continuously when In dally use, except for the ultraviolet light source, which should be turned off when not 10 use for more than a few hours 8 2 Adjust all gas flows, temperatures and cycle times to manufacturer s speCifications Perform the System Cleanup and Calibration procedure In the manufacturer s speCifications each day ReCirculate a sample of Irradiated distilled water until two consecutive readings wlthm 10% of each other are obtained Record the last value for the system blank ThiS value IS a function of the total Instrument operation and should not vary Significantly from preViOUS runs Reasons for Significant changes In the value should be Identified 8 3 Check the effectiveness of the CO2 scrubber by analyZing the carbonate-bicarbonate standard solutlon(7 8) Add 1 mL of aCidified persulfate reagent (7 6) to 50 mL of the solution Transfer 10 mL of the solutlon-wlth-reagent to the first sparger and start the analYSIS cycle No response, or a very minor reading, should be obtained from thiS solution Add 1 mL of aCidified persulfate reagent (7 6) to 50 mL of reagent distilled water (7 1) blank, standards 7 3, 74, and 7 5 and the samples 8 5 Calibrate the analyzer as follows Sampling DeVices Any 6 3 apparatus that Will reliably transfer 10 mL of sample to the sparger A 50 mL glass syrmge IS recommended Reagents 7 7 1 Distilled water used In preparation of standards and for dilution of samples should be ultra-pure to reduce the magnrtude of the blank Carbon diOXide-free, double distilled water IS recommended The water should be distilled from permanganate or be obtamed from a system mvolvmg distillation and carbon treatment The reagent distilled water value must be compared to a system blank determmed on a recirculated distilled Reagent Distilled Water water sample The total organic carbon value of the reagent distilled water should be less than 60 tlg/L Purgeable organrc carbon values of the reagent distilled water should be less than 4 tlglL 72 Potassium hydrogen phthalate, stock solution 500 mg carbon/liter Dissolve 1 063 g of potassIum hydrogen phthalate (Primary Standard Grade) 10 reagent distIlled water (7 1) and dilute to 1 liter 7 3 Potassium hydrogen phthalate (2 mg/L) Pipet 4 mL of potassIUm hydrogen phthalate stock solutIOn (7 2) mto a one liter volumetnc flask and dilute to the mark With reagent distilled water (7 1} 74 Potassium hydrogen phthalate (5 mg/L) Pipet 1 mL of potassium hydrogen phthalate stock solution (72) mto a 100 mL volumetnc flask and dilute to the mark With reagent distilled water (7 1) 7 5 Potassium hydrogen phthalate (10 mg/L) Pipet 2 mL of potassium hydrogen phthalate stock solution (7 2) mto a 100 mL volumetnc flask and dilute to the mark With reagent distIlled water (7 1) 8 4 7 6 Place 100 mL of reagent distilled water (7 1) In a container Add 5 g of potassium persulfate Add 5 g (3 mL) of concentrated (85%) phosphoriC aCid ACidified Persulfate Reagent 7 7 solution, 1000 mg carbon/liter Place a 3500 g of sodium bicarbonate and 04418 g of sodium carbonate 10 a 100 mL volumetrrc flask Dissolve With reagent distilled water (7 1) and dilute to the mark 7 8 Carbonate-bicarbonate, standard solution 50 mg/L Place 5 ml of the Carbonate-bicarbonate, stock Dec 1982 4152-2 85 1 (7 1) and 5 a mg/L standard (74) Transfer 10 mL of the solutlon-wlth- reagent to the first sparger and start analyzer cycle Ignore the meter reading for the first cycle Transfer a second 10 mL of the solution-with-reagent to the first sparger and start the analYSIS cycle Record the meter reading (see 9 1) of the final carbon value for each of the reagent distilled water (7 1) and the standard (7 4) If the meter read109 IS more than 25% above or below the calculated value of standard 7 4, reanalyze the standard Run the reagent distilled waterPDF Image | Methods for Chemical Analysis of Water and Wastes
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