Environmental Express MicroBloc - Manual (Page 19)

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HotBlock: Operation and Instruction Manual MicroBlock TM Distillations
TOTAL Recoverable phenolics With the MicroBlock™ Continued
6.3 Standard Phenol, Solution B
Dilute 10.0mL of Standard Phenol Solution A to 100mL with reagent water.
1.0mL = 0.001mg phenol.
6.4 Standard Phenol, Solution C
Dilute 10.0mL of Standard Phenol Solution B to 100mL with reagent water.
1.0mL = 0.0001mg phenol.
6.5 Sodium Hydroxide, 0.1 N [1+9]
Dissolve 4.0g of NaOH in 1L of reagent water.
6.6 Sulfuric Acid, 10% [1+9]
Slowly add 10mL of concentrated sulfuric acid to 70mL of reagent water. Cool and dilute to 100mL.
6.7 Ferrous Ammonium Sulfate
Dissolve 0.55g of ferrous ammonium sulfate in 250mL reagent water containing 0.5mL sulfuric acid and dilute to
500mL.
7.0 PROCEDURE
7.1 Pipette 50mL of sample into a beaker. Adjust pH to 4 with NaOH [1+9] or with Sulfuric Acid [1+9]. Transfer to the
skirted Reaction Tube. For soil samples, weigh 1g or less into beaker and 50mL reagent water. Adjust pH to 4 with
NaOH [1+9] or sulfuric acid [1+9] while stirring and transfer to the skirted Reaction Tube. Add a pinch of boiling
chips.
7.2 Repeat 7.1 for all samples to be distilled up to a maximum of 10.
7.3 Assemble the distillation glassware setup as shown in Figure 4h and position in the heater block.
7.4 Turn on the tap water to cool the Cold Finger after ensuring all tubing connections are tight. Check for leaks.
7.5 Turn power ON and set heater block temperature to 190°C and timer to 60 minutes.
7.6 When approximately 45mL of sample is distilled add 5mL of reagent water using a syringe by piercing the rubber
septum located on the top of the Distillation Head.
7.7 When 50mL of sample is collected in the Receiver Tube remove by unscrewing the cap containing the Short Stem.
7.8 When all samples have distilled turn the power OFF.
7.9 Add 5mL increments of reagent water to the Reaction Tube by piercing the septum using a syringe. Since the heater
block is still hot the distillation process will continue. Place a collection tray or beakers to catch any further distillate.
7.10 After each use clean exterior with a damp sponge.
7.11 When the heater temperature falls below 100°C, the next run can be started.
Note: If boil over occurs, add 2-3 drops of Antifoam B agent to the sample prior to distillation.