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- Page 1 LKF and PKF ® Karl Fischer Moisture Analyzer User Manual TEL +1 713 784 0000 FAX +1 713 784 0001 KFMANUAL-0317 Email Sales@KAM.com KAM CONTROLS, INC. 3939 Ann Arbor Drive Houston, Texas 77063 USA An ISO 9001 certified company...
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Page 2: Table Of Contents
Introduction •Available models •Theory of operation Specifications Components • Front and rear panels • Display and keypad Operation • Glassware assembly/adding reagent • Base assembly • Setting date and time • Reset reagent life • Sample size and titration mode • Initial titration • Running samples (moisture content determination) • Sample dilution • Accessing sample data • USB data retrieval • BlueTooth data retrieval ® • BlueTooth Printer (optional) ® Maintenance • Reagent replacement procedure • Storage • Special Grease • Electrode cleaning procedures Ordering information KFMANUAL 0317 KAM CONTROLS, INC. -
Page 3: Introduction
® THEORY OF OPERATION Moisture Analyzers incorporate the coulometry principle applied to Karl Fischer titration to totally ® eliminate the troublesome procedures involved in conventional water determinations. Available in a lab model as well as a portable, KAM Moisture Analyzers are easy to use and fully automatic. The portable ® model has a rugged case for field usage and the capability to operate continuously for 10 hours on battery power before needing recharging. KF units can be used to rapidly and accurately determine the water content of liquid hydrocarbons ® for all custody transfer operations: pipeline, marine, or truck. The Moisture Analyzer can also be used to analyze crude oils, distillates, transformer oils, jet fuels, chemicals, and most other liquids. In the plant, it can monitor the moisture content of streams during start-ups, shutdowns, upsets, and normal operations. This can be especially important on units where expensive catalysts can be damaged by excessive mois- ture. The unit also can be used by machinists as part of a preventive maintenance program. By analyzing lube oil on compressors, turbines, etc., the Moisture Analyzer can detect cooling water leaks before they become severe enough to damage equipment. Karl Fischer titrimetry is an accurate moisture measurement method utilizing the quantitative reaction of water with iodine. In coulometric Karl Fischer titration, the sample is added to the Karl Fischer Reagent (io- dine ion and sulfur dioxide as principal components). Iodine, generated electrolytically at the anode, reacts with water in the sample as shown in Formula 1. Iodine is generated in direct proportion to the quantity of electricity according to Faraday’s Law. Formula 1: I + SO O 2HI + SO One mole of iodine reacts quantitatively to one mole of water; therefore, 1 mg of water is equivalent to 10.71 coulombs (Formula 2). Based on this principle, water content can be directly determined from the quantity of electricity required for electrolysis. This eliminates the need for addition of Reagent and tedious standardization procedures. Formula 2: 2I KFMANUAL 0317 KAM CONTROLS, INC. -
Page 4: Specifications
Generator electrode config.: With diaphragm Titration speed: 1000 μg H O/min. (max. at high H O concentrations) Power requirements: Operates on either AC or DC. AC - 110/120, 220/240 V, 50/60 Hz 12 V rechargeable lithium battery Ambient Temperature 5ºC – 40º C Communication: USB port, BlueTooth , Windows based software ® ® Printer: Optional Dimensions: Portable 15.5” x 8”x 10” (394 mm x 203 mm x 254 mm) Lab 10.5” x 8” x 9”(267 mm x 203 mm x 229 mm) Weight: Portable approx. 20 lbs. (9 kg) Lab approx. 10 lbs. (4.5 kg) KFMANUAL 0317 KAM CONTROLS, INC. -
Page 5: Components
Silica Gel Storage FRONT PANEL (portable model shown) Detector LCD Display Electrode Wire Keypad Cathode Solution Cell Wire Swivel Clamp Titration Cell Assembly Titration Cell Sleeve Power Button USB Storage Unit Base Rubber Septums Storage REAR PANEL (portable model shown) Power Jack (Portable models) USB Port Detector Electrode Jack (red) Cathode Solution Cell Jack (black) KFMANUAL 0317 KAM CONTROLS, INC. -
Page 6: Display And Keypad
Aug15 S a v e d S a m p l e s L a n g u a g e English Screen Navigation Arrows ENTER Key Karl Fischer Moisture Analyzer MENU Key: Returns to NEW SAMPLE Key: main menu from any Initializes titration screen and sample injection screen KFMANUAL 0317 KAM CONTROLS, INC. -
Page 7: Operation
Unscrew Injection Port (D and E) and place a new rubber Sep- tum (C) in the base of the Injection Port (D). Screw the top of the Injection Port (E) into the base and place the Injection Port into the indicated opening on the Generator Solution Cell lid (B). Apply a thin layer of Special Grease to the neck of Detector Electrode (F) and place in the remaining small opening of the Generator Solution Cell lid (B). Do not apply pressure to the Electrode. Rather, let it seat under its own weight. Rotate it half a turn backward and forward to ensure the grease is spread evenly and a seal has been created. Drop the ceramic Stir Bar (J) into the Generator Solution Cell. Apply a thin layer of Special Grease to the neck of Cathode Solution Cell (G) and its Stopper (H). Set aside. Pour entire contents of KAM Generator Solution A (100 ml) into the Generator Solution Cell through the remaining hole (should be the large hole near the center of the lid). The Generator Solution A (100 ml) is pre-measured to the appropriate volume. Place the Cathode Solution Cell (G) into in the Generator Solution Cell lid (B). Do not apply pressure. It will seat under its own weight. Rotate it half a turn backward and forward to ensure the grease is distributed evenly around the circumfer- ence of the seal. The sooner the hole is covered, the less mois- ture will be absorbed by the chemicals. KFMANUAL 0317 KAM CONTROLS, INC. -
Page 8: Base Assembly
Place a funnel in stopper hole at the top of the Cathode Solution Cell (G) and pour entire contents of KAM Generator Solution C (5 ml) ampoule into the Cathode Solution Cell (G). ® Remove funnel and place the glass Stopper (H) in place. NOTE: Generator Solution C ampule is glass. To open, hold the ampule in a paper or cloth towel, and apply pressure to the top of the ampule just above the small dot. Top should cleanly snap off the base of the ampule. BASE ASSEMBLY NOTE: Before assembling the base unit and glassware, ensure that the unit has been turned off. Turn the swivel clamp toward back of KF unit and place the entire Generator Solution Cell assembly into the Titration Cell Sleeve. Turn Swivel Clamp over the top of the cell and secure by hand tightening the screw on top of the clamp. Do not over tighten. Plug the free end of the Cathode Solution Cell Wire into the black colored jack on the side panel of the base unit, and the free end of the Detector Electrode Wire into the red colored jack. If using a portable unit, remove the power cord from packing or storage compartment and plug into the power jack on the back of the base. Plug unit into power source and press power but- ton. The power button should glow blue. If you are using a portable unit, the light will blink when the battery is charging. The LCD display should show the Main Menu. Detector Electrode Jack (red) Swivel Clamp Titration Cell Assembly Titration Cell Sleeve Cathode Solution Cell Jack (black) KFMANUAL 0317 KAM CONTROLS, INC. -
Page 9: Setting Date And Time
Reagent age: 7 days From the Main Menu, navigate to Reagent Life Days remaining: 0 days and hit ENTER. Volume injected: 25 ml 0 ml Volume remaining: The display will indicate the following: • Current reagent life in days (max 7) RESET REAGENT • Remaining days in current reagent life • Total volume of samples already run (max 25 ml) • Remaining volume of samples allowed Reset Ragent? “RESET REAGENT” will be highlighted at the bot- tom of the screen. Hit ENTER. A confirmation screen will appear and “Yes” will be highlighted. Hit ENTER again to reset the reagent life. The display will return to the Main Menu and Re- agent Life should be 100%. KFMANUAL 0317 KAM CONTROLS, INC. -
Page 10: Sample Size And Titration Mode
Plea se Wai t 0.1043% The stir bar should begin to spin and the display will show “Removing Excess Water. ” This may take several minutes after reagents have been Detection changed or if the instrument has been out of the Titration titration mode for a long period of time. When all excess water has been removed, the unit will beep and the display will alternate 09:21 Aug 15, 2016 between “Analysis Complete” and “Press New Sample # 78 / Size: 0.5 Sample. ” Press New Sample NOTE: Prepare physical sample in accordance 0.1098% with instructions on page 11 of this manual prior to pressing the NEW SAMPLE button. Detection Titration KFMANUAL 0317 KAM CONTROLS, INC. -
Page 11: Running Samples
Sample # 79 / Size: 0.5 Processing Insert syringe needle through the Sample Injection 0.0574% Port, piercing the Septum and continuing into the cell until the needle tip is fully submerged in the Detection Reagent. Titration Inject the sample into the Reagent. This should be done in a single, swift movement, but do not allow the sample to splash up against the wall of the Generator Solution Cell or the needle to touch the 09:21 Aug 15, 2016 sides of the cell. Sample # 79 / Size: 0.5 Titration Complete Electrolysis begins automatically by the injection of 0.1098% the sample. When the analysis is completed, the unit beeps and the results will be displayed on the Detection Titration Complete screen. Titration KFMANUAL 0317 KAM CONTROLS, INC. -
Page 12: Sample Dilution
08/14/2016 Sample73 08/14/2016 Data for any individual sample can be retrieved Sample72 08/14/2016 by using the UP/DOWN arrows to navigate to the desired sample number and pressing ENTER. The display will show the date, time, water percentage, Sample79 and sample size of the sample in question. The Date: 08/15/2016 next or previous sample can be viewed using the Time: 09:45 UP/DOWN arrows. Water Cont.: 0.1098% Mode: % Hit ENTER to return to Sample Log/Saved Sample Size: 0.5 Samples. Reagent age: 0 Days Volume injected: 0.65 ml KFMANUAL 0317 KAM CONTROLS, INC. -
Page 13: Usb Data Retrieval
D a t e & Ti m e Aug15 BlueTooth and Download from Files. ® S a v e d S a m p l e s L a n g u a g e English Click on Download via BlueTooth, and follow steps 10-12 above. KFMANUAL 0317 KAM CONTROLS, INC. -
Page 14: Bluetooth ® Printer (Optional)
C a l i b r a t i o n Use the RIGHT/LEFT arrows to navigate to Printer and press ENTER. BT Mode Modem Printer The display will show “Scanning for Printer. ” This may take up to 30 seconds. Scanning for Printer If a BlueTooth connection cannot be made, the display ® will show “No Printers Available. Press Menu to Exit. ” Press the MENU button and return to step 3 above. Ensure that the printer is turned on. No Printers Available Press Menu to Exit KFMANUAL 0317 KAM CONTROLS, INC. - Page 15 S a v e d S a m p l e s L a n g u a g e English Use the navigation arrows to choose the sample record Samples Saved to be printed and press ENTER. Sample79 08/15/2016 Sample78 08/15/2016 Sample77 08/15/2016 Sample76 08/15/2016 Sample75 08/15/2016 Sample74 08/14/2016 Sample73 08/14/2016 Sample72 08/14/2016 KFMANUAL 0317 KAM CONTROLS, INC.
- Page 16 BT Mode Ve r s i o n I n f o Use the RIGHT/LEFT arrows to select Modem under BT C a l i b r a t i o n Mode. Hit ENTER The LCD display should show the Main Menu and the BlueTooth icon will no longer be at the top of the ® BT Mode screen. Modem Printer KFMANUAL 0317 KAM CONTROLS, INC.
- Page 17 4. OPERATION continued PRINTER TROUBLESHOOTING If the printer fails to print a sample record, the BlueTooth connection with the KAM KF unit ® ® might be lost. Turn off the KAM KF unit. ® Press the power button on the side of the printer two times in quick succession. The printer will shut down. Wait until the blue light on the printer stops blinking and turns off. Then, press the power button once more. The printer should turn on. It will take approximately 10 seconds to warm up. Turn on the KF unit and repeat the Pairing Process instructions starting from step 3 on page 14 of this manual. KFMANUAL 0317 KAM CONTROLS, INC.
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Page 18: Maintenance
P L E A S E R E P L A C E R E A G E N T reagents, follow the steps below. Refer to pages 7-8 for part images. Unplug Detector Electrode and Cathode Cell wires from their respective jacks. Loosen screw on the top of the swivel clamp and turn clamp toward back of unit. Carefully remove entire glassware unit and place on a clean surface. Remove Glass Stopper from the Cathode Solution Cell and wipe free of grease. Also remove grease from opening at the top of the cell. Remove the Cathode Solution Cell from the Generator Solution Cell by gently twisting and lifting. DO NOT pull using the wire. Remove grease from the exterior of the Cathode Solu- tion Cell and opening in the Generator Solution Cell opening. Remove Detector Electrode (do not pull by wire), Sample Injection Port, and Drying Tube from the Generator Solution Cell. Remove the Glass Stopper from the Cathode Solution Cell. Empty contents of Cathode Solution Cell by pouring into a suitable container or aspirating from the cell. Dispose of fluids according to SDS sheet(s). Empty contents of Generator Solution Cell by pouring into a suitable container or aspiration. Dispose of fluids according to the SDS sheet. Thoroughly wash the Generator Solution Cell with water and dish soap, then rinse with water and dry by inserting a paper towel in large hole in lid and wiping down inside walls of the cell. Follow steps for Glassware Assembly and Base Assembly on pages 7-8 of this manual. Follow steps to Reset Reagent Life on page 9 of this manual. Follow steps for Initial Titration on page 10 of this manual. KFMANUAL 0317 KAM CONTROLS, INC. -
Page 19: Storage
SPECIAL GREASE To keep the Generator Solution Cell performing accurately and effectively be sure that a thin layer of Special Grease is applied to all glass tapered joints each time the Reagents are replaced. Frequent greasing will prevent the glassware from seizing and causing damage to the cell. The Special Grease does not absorb moisture, so it will not hinder the results of the analysis. NOTE: No other grease should be used with a KAM KF Karl Fischer Moisture Analyzer due ® to the potential for the other types of grease to absorb moisture and interfere with titration if it is silicon based. KAM CONTROLS is not responsible for problems resulting from the use of improper grease. CATHODE CELL ELECTRODE CLEANING PROCEDURES Dirty electrodes (platinum grids) usually result in the following problems: • A decrease in titration efficiency resulting in a longer measuring time • An increase in the blank (residual) value of titration current due to absorption of moisture in the dirty area • Unstable titration current and lack of reproducible results • Staining on the ceramic frit at the bottom of the Cathode Solution Cell NOTE: KAM recommends the use of chromic sulfuric acid (3 ml of potassium dichro- ® mate+400 ml of reagent grade sulfuric acid). Because nitric acid produces corrosive fumes, be sure and conduct all parts of this procedure in an appropriately ventilated environment. Acid should NOT be reused. Follow appropriate disposal procedures. performs this service as a part of annual unit recertification and highly recommends end ® users send unit to factory for electrode cleaning if a suitable environment and/or chemicals are not available. Follow steps for glassware disassembly on page 18 of this manual. KFMANUAL 0317 KAM CONTROLS, INC. - Page 20 MAINTENANCE continued Remove any exterior contamination from Cathode Solution Cell with tissue paper and acetone being careful not to damage the platinum wires and screen on the outside of the cell. Fill the Cathode Cell with acetone and stopper the inlet joint. Shake the unit until any dirt is removed. This should be repeated several times. Pour out and discard acetone. Wash the outer surface with acetone. Pour approximately 5 ml of acid into the Cathode Solution Cell. Place the cell in a 50 ml beaker and fill the beaker with acid to the same level as is in the cell. Secure the Cathode Solution Cell so that it will not fall over. Allow the cell to remain in the solution overnight. After the cell has stood overnight, discard the nitric acid in the cell, and rinse the inside and outside of the cell with running tap water until the yellow color disappears. Place distilled water in the cell and place it in a 400 ml beaker filed with distilled water. Place the beaker on a hot plate and bring the water to a slow boil for at least one hour. Repeat this operation until there is no coloration of the water. Remove the Cathode Solution Cell from the water and fill it with acetone to overflowing, flooding the outside of the cell as well. Shake the cell, dump out the acetone, then refill and repeat. Dry the cell with a forced air dryer. NOTE: Do not use compressed air as the increased pressure could damage the compo- nents. Place the entire assembly in a laboratory oven and continue to dry it for several hours at 120º F . NOTE: The Detector Electrodes can be cleaned in a similar manner if required. KFMANUAL 0317 KAM CONTROLS, INC.
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Page 21: Ordering Information
ORDERING INFORMATION KF KARL FISCHER MOISTURE ANALYZERS ® P# 09100 KAM PKF PORTABLE KARL FISCHER MOISTURE ANALYZER: Battery powered Ana- lyzer includes Recharger (120 VAC), Titration Cell, Electrodes, Stir Bar, Drying Tube, and Carrying Case. P# 09150 KAM LKF LAB KARL FISCHER MOISTURE ANALYZER: includes Titration Cell, Electrodes, Stir Bar, Drying Tube, and 120 VAC Power Adapter. P# 09041 STARTER KIT: Contains all required items for analysis, including: Generator Solution A (1), Generator Solution C (1), Calibration Verification Check Solution (1), 1 ml and 10 µl Gastight Syringes, 14 and 19 gauge Needles, package of rubber Septums (100), Funnels (2), Special Grease (1) and Silica Gel (1). REAGENTS and CONSUMABLES P# 09004 GENERATOR SOLUTION A (Anode): pack of 6, 100 ml bottles P# 09006 GENERATOR SOLUTION C (Cathode): pack of 6, 5 ml ampoules P# 09032 CALIBRATION VERIFICATION CHECK SOLUTION: box of 10, 4 ml ampoules (1% water content), certificate included P# 09013 SILICA GEL: 100 ml bottle GLASSWARE P# 09052 COMPLETE TITRATION CELL ASSEMBLY: includes Generator Solution Cell, Cathode Solution Cell, Detector Electrode, Drying Tube, Sample Injection Port, Stir Bar P# 09064 DETECTOR ELECTRODE P# 09063 CATHODE SOLUTION CELL P# 09062 GENERATOR SOLUTION CELL KFMANUAL 0317 KAM CONTROLS, INC. - Page 22 ORDERING INFORMATION CONTINUED SYRINGES AND NEEDLES P# 09010 GASTIGHT SYRINGE, 10 µl P# 09023 GASTIGHT SYRINGE, 50 µl P# 09021 GASTIGHT SYRINGE, 250 µl P# 09022 GASTIGHT SYRINGE, 500 µl P# 09008 GASTIGHT SYRINGE, 1 ml P# 09001 GASTIGHT SYRINGE, 2.5 ml P# 09002 NEEDLE, 19-gauge, 4” P# 09003 NEEDLE, 14-gauge, 4” SPARE PARTS P# 09049 SAMPLE INJECTION PORT P# 09044 STIR BAR P# 09050 DRYING TUBE P# 09029 RUBBER SEPTUM, pack of 100 P# 09015 SPECIAL GREASE, 25 g tube P# 370420 REPLACEMENT RECHARGEABLE BATTERY (for model 09031) P# 370400 POWER ADAPTER, 110/120 or 220/240 VAC ACCESSORIES P# 09014 HOMOGENIZER DRIVE UNIT, 110/120 or 220/240 VAC with speed control P# 09019 DISPERSING TOOL FOR HOMOGENIZER, 18 mm (for 50-2000 ml volume) P# 09009 DISPERSING TOOL FOR HOMOGENIZER, 25 mm (for 500-4000 ml volume) P# 09018 HOMOGENIZER STAND KFMANUAL 0317 KAM CONTROLS, INC.
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