Catalog Number 2265308 Distillation Apparatus USER MANUAL 02/2013 Edition 5 Visit us at www.hach.com Table of Contents Section 1 General Description.........................................................................................................5 1.1 Introduction..................................................................................................................................5 1.1.1 Heater.................................................................................................................................5 1.1.2 Operator Controls and Indicators........................................................................................5 1.2 Heater and Support Apparatus....................................................................................................6 1.2.1 General Purpose Apparatus...............................................................................................6 1.2.2 Arsenic Distillation Apparatus.............................................................................................7 1.2.3 Cyanide Distillation Apparatus............................................................................................8 1.3 Using the Distillation Apparatus...................................................................................................9 1.3.1 Burn In................................................................................................................................9 1.3.2 Operational Notes.............................................................................................................10 Arsenic Distillation.........................................................................................................................................11 Cyanide Distillation........................................................................................................................................15 Fluoride Distillation........................................................................................................................................19 Nitrogen–Ammonia Distillation.................................................................................................................21 Nitrogen–Ammonia Distillation for ISE..................................................................................................27 Phenols Ammonia Distillation...................................................................................................................31 Selenium Distillation......................................................................................................................................35 Volatile Acid Distillation...............................................................................................................................39 Replacement Parts ........................................................................................................................................43 3 Table of Contents 4 Section 1 General Description 1.1 Introduction The Hach Distillation Apparatus adapts easily for a variety of distillation needs. It is suitable for wastewater, water and seawater testing requiring distillation pretreatment. Applications for the General Purpose Apparatus include: albuminoid nitrogen, ammonia nitrogen, fluoride, phenols, selenium, and volatile acids. In addition to the General Purpose Apparatus, arsenic requires the Arsenic Distillation Apparatus Set and cyanide requires the Cyanide Distillation Apparatus Set. All connecting glassware is manufactured with threaded connectors for easy use and safety. The General Purpose Heater and Support Apparatus provide efficient heating and anchoring of the glassware. 1.1.1 Heater The heater is a single-element, 200-watt mantle with adjustable heat and a variable speed, bi-directional magnetic stirring motor. The heater block is sized for a 500-mL distillation flask. Operating controls include a heat control, a stir speed control, and a power switch. Indicator lights show when the power and heater circuits are energized. The power requirements are 115 or 230 Vac, 50-60 Hz, 200 W. 1.1.2 Operator Controls and Indicators Figure1 on page 6 illustrates the heater assembly and control indicators. A functional description of the controls is given in Table 1. Table 1 Name Function Power Indicator Indicates when the heater is plugged in. Heat Indicator Indicates when the heater circuit is operating Controls the rotation speed of the stir bar. Counter-clockwise (1-10) rotation of the Stir Speed Control knob increases the rotation speed. The power indicator must be on to operate the stir motor. Stir Mode Switch Selects for 3 functions: 1 (highest position) Bi-direction with a reversing period of about 20 seconds 2 (middle position) One direction up to about 150 rpm 3 (lowest position) Manual capture. If stirring action is lost due to excessive rotation, reduce the stir speed and depress the stir mode switch to this position to recapture the stir bar in the magnetic field. Stir Indicator Indicates when the magnetic stirring motor is on. Stir On/Off Switch Turns stirring motor on or off. The stir light will light when the switch is on. Controls electrical current to the heating element. The off position is marked 0 and the temperature increases as the knob is turned clockwise to 10. The heater Heater Control indicator will light when the heating element is on and go off when the selected temperature level is reached. 5 General Description Figure1Electromantle Heater 1.2 Heater and Support Apparatus The heater comes with a support rod, three universal clamps and three clamp holders. The support rod is inserted into the holder on the back of the heater base and is secured with a hand-operated screw. Clamp holders and clamps are positioned on the support rod to secure the distillation glassware. 1.2.1 General Purpose Apparatus The General Purpose glassware is used for all distillations except arsenic and cyanide (additional glassware is necessary for those tests). 1. The heater comes with a support rod, 3 universal clamps and 3 clamp holders. Insert the support rod into the holder on the back of the heater base and secure it with a hand-operated screw set. 2. Position the clamp holders on the support rod to secure the glassware. 3. Assemble the general purpose glassware as shown in Figure2. 6 General Description 4. Assemble the condenser so cold water enters through the lower port and leaves from the upper port. Secure tubing to both ports with cable ties. Figure2General Purpose Distillation Apparatus Assembly 1.2.2 Arsenic Distillation Apparatus Figure 3 shows the distillation apparatus setup for arsenic. Assemble as shown, using these instructions: 1. Complete Steps 1 and 2 from the General Purpose assembly procedure. 2. Use the distillation flask and J-tube from the General Purpose Apparatus, along with the gas scrubber, gas bubbler, and cylinder from the Arsenic Distillation Apparatus to assemble the glassware as illustrated in Figure3. 7 General Description Figure3Arsenic Distillation Apparatus Assembly 1.2.3 Cyanide Distillation Apparatus The distillation setup for cyanide is shown in Figure4. Assemble as shown, using the following instructions: 1. Complete Steps 1 and 2 from the General Purpose glassware assembly procedure. 2. Use the distillation flask, condenser and J-tube from the General Purpose Apparatus along with the gas bubbler, cylinder, flow meter, filter flask, and aspirator from the Cyanide Distillation Apparatus to assemble the Cyanide Glassware as illustrated. 8 General Description 3. Assemble the condenser so the cold water enters through the lower port and leaves from the upper port. Secure tubing to both ports with cable ties. 4. The aspirator requires a 3/8-inch NPT inside thread. Adapters for other thread connectors may be purchased commercially. 5. Secure all tubing connections with cable ties except at the gas bubbler port. Figure4Cyanide Distillation Apparatus Assembly 1.3 Using the Distillation Apparatus 1.3.1 Burn In When first used, the surface of the heating element will smoke slightly as the fabric dressing burns away (burn-off). The element will become discolored and then gradually revert back to white. It is 9 General Description advisable to burn off the mantle before inserting any glassware to avoid staining the flask. 1.3.2 Operational Notes Wipe the distillation flask thoroughly to ensure it is clean and dry before placing it on the mantle. Be sure the bottom of the flask makes good contact with the heating element. Use a slight rotary action when installing or removing the flask from the mantle. If a spill occurs, turn off the heater immediately and allow it to cool. The mantle must be cleaned and dried before using it again. 10