Control No. : ZTINEMAE-02 INSTRUCTION MANUAL For TOTAL NITROGEN ANALYZER MODEL TN-110 (TN-110 System Program Version 2.0-) MITSUBISHI CHEMICAL CORPORATION TOKYO, JAPANDECLARATION OF CONFORMITY Application of Council Directives : IC Electromagnetic Compatibility Directive : Electrical Equipment Designed for Use within Certain Voltage Limits : 73/23/BEC Standard to which Conformity is Declared : ENS5011 (1991) Class B, EN55082-1 (1992), EN61010-1/A2 (1995) Manufacturer’s Name +: Mitsubishi Chemical Corporation Manufacturer’s Address 2 31-19, Shiba 5-chome Minato-ku, Tokyo 108 Japan EU Office Address : Prinzenallee 13 40549 Duesseldorf Federal Republic of Germany Type of Equipment : Laboratory Equipment Model Name : Total Nitrogen Analyzer Model TN-110 Beginning of Serial Number _: C2R00018 (TN-110 Main Unit) Beginning of Serial Number —_: CON00018 (ND-100) Month and year of Manufacture : June 1999 I, the undersigned, hereby declare that the equipment specified above conforms to the above Directives and Standards. Katsuyuki Shimakawa General ManagerIMPORTANT SAFEGUARDS AND PRECAUTIONS ‘Many thanks for your purchase of our Total Nitrogen Analyzer Model “TN-110”. ‘You should read this instruction manual with care prior to its use. Keep the manual at hand when you are operating the analyzer. It should be noted that if you operate the analyzer in the way other than described in the manual, the security can not be assured. If you find questions, errors, and omissions, please contact our agency. WARNING [This manual contains information and warning which must be followed to ensure safe operation and retain the TN-110 in safe condition. Read and understand this manual thoroughly before operating the TN-110. For accurate and safe operation of the TN-110, correct operation and maintenance including periodic inspection are required. You should read the “IMPORTANT SAFEGUARDS AND PRECAUTIONS” and WARNINGS, CAUTIONS and NOTES for safety in the manual prior to practical use and maintenance. It is recommended that the TN-110 should be operated and maintained only by limited professional operators having a thorough knowledge of the TN-110, In this manual, the following marks are used to highlight information critical to the safe and accurate operation of the TN-110. [ACTIONS OR CONDITIONS THAT POSE A HAZARD(S) TO THE USER. CAUTION ACTIONS OR CONDITIONS THAT MAY DAMAGE THE TN-110 OR RESULT IN INCORRECT OPERATION. POINT (NOTE) INFORMATION IMPORTANT FOR THE ACCURATE USE OF THE ‘TN-110.WARNING [DO NOT ATTEMPT TO INJECT ORGANIC SUBSTANCES IN THE FLOW OF OXYGEN OR AIR IN THE PYROLYSIS TUBE AT HIGH TEMPERATURES. | NEVER INJECT ORGANIC SUBSTANCES IN THE STAGNANT GAS FLOW. ‘When you mix organic substances with Oxygen or air at high temperatures, EXPLOSION, BREAKAGE OF GLASS PARTS or other hazards may happen. To avoid these risks, since this unit carries out the combustion with Oxygen after samples are slowly vaporized under the Argon flow, possible causes for these risks such as gas leakage caused by loosening of the Argon gas tubing, deterioration of O-Rings and Septum and so on are to be checked on daily basis, Ifyou find the gas leakage or there is no combustion / no detection (No Peak) is found, take the following necessary steps: (1) Stop inserting the sample into the Electric Furnace. 2) Stop the Oxygen gas flow. 3) Switch OFF the heater, and leave it for 2 or 3 hours until the furnace cools down. (4) Check and identify the cause of the gas leakage and conduct 2 proper treatment. (©) Flow Argon gas sufficiently to ventilate the reaction system. © Restart measurements according to the manual. DO NOT TOUCH THE ELECTRIC FURNACE AND PARTS NEAR THE ELECTRIC FURNACE DURING OPERATION. ‘The electric furnace is heated up to 800 to 1,100 °C. Do not touch the electric furnace and parts such as both ends of the Pyrolysis Tube, side surface of the electric furnace, heat insulating boards near the electric furnace during operation.[DO NOT ATTEMPT TO SERVICE THIS PRODUCT YOURSELF. If this product does not operate as described when the detailed operating instructions are followed, do not attempt to open or remove covers or make any adjustments not described in the manual. Attempting to service this unit yourself may expose you to dangerous voltage or other hazards and will void warranty. Refer all servicing to qualified service personnel. Please contaet the local agency. WA’ ALWAYS CLOSE THE SAFETY COVER OF THE AUTOMATIC BOAT CONTROLLER (ABC) WHEN THE SYSTEM IS RUNNING. /DO NOT KILL THE FUNCTION OF THE LIMIT SWITCH OF THE SAFETY COVER. If the Safety Cover of the ABC is opened during the operation [Run-Method], the TN-110 System program automatically shut down. (Take emergency steps as turning off the heater, ozonizer off.) WARNING ALWAYS CHECK THE PRESSURE OF THE GAS CYLINDERS BEFORE OPERATING THE TN-110. IF THE GAS CYLINDER BECOMES EMPTY AND INJECT ORGANIC SAMPLES BY MISTAKE, EXPLOSION, BREAKAGE OF GALSS PARTS OR OTHER HAZARDS MAY HAPPEN. If the gas (Argon / Oxygen) drops down below 50 cc/min, the TN-L10 System program automatically shuts down. ( Take emergency steps as turning off the heater, ozonizer off.) This safety feature works at Run - Method only. USE ONLY MICROSOFT® WINDOWS®95/98 ENGLISH LANGUAGE | VERSION AS ITS OPERATING SYSTEM. IF OTHER LANGUAGE/VERSION OF WINDOWS® ARE USED, THE [PERFORMANCE OF THE SYSTEM CAN NOT BE GUARANTEED. ‘TN-110 System Program is designed for Windows@95/98 English language version only. Since the deference of each language version, the performance of the system ean not be assured, if the OS is out of specifications.'THE SPECIFICATIONS OF THE PC DESCRIBED IN THE MANUAL ARE MINIMUM REQUIREMENTS FOR RUNNING THE TN-110 SYSTEM PROGRAM. ‘TN-110 System Program is also designed for English / US type PC as hardware environments. If you use your own PC, the performance of the system can not be guaranteed. NOTE DO NOT USE OTHER APPLICATION SOFTWARE WHEN THE TN-110 SYSTEM PROGRAM IS RUNNING. THE PERFORMANCE/SECURITY / SAFETY OF THE SYSTEM CAN NOT BE ASSURED. ‘TN-110 System Program (PC) always monitors / controls the Heater, measurement status or status of the system by communicating with the TN-110 Main Unit in every 0.5 / 2.5 sec. For safety reasons, do not use other application software when the TN-110 System Program is running. ‘Due to a lack of memory / lack of the disk space, in the worst case, Windows may shut down unexpectedly. The analytical results may not be saved.[POINT Inappropriate sample for measurement Nitrogen in sample of sodium azide and sulfuric acid hydrazine mainly comes to N, when thermal cracking is done in the reaction tube Therefore, the recovery largely becomes low in the chemiluminescence and the correct: measurement can’t be done. POINT TN-110 is the equipment for the measurement of nonaqueous sample. POINT@ outline of obstruction ingredient in chemiluminescence obstruction ingredients in chemiluminescence are the one that indicates the positive interference that reacts with ozone and causes chemiluminescence and that deprives excitation energy from NO; in excitation and indicates the negative interference. @ Positive interference (a) Carbonyl compound of iron and nickel and (b) olefin such as ethylene and trimethylethylene (c) sulfide such as dimethlysulfide and hhydrogen sulfide are regarded as the possibility of indicating the positive interference. ‘The chemical luminosity of (a) is detected by the pile of measurement Angredient and ozone chemical luminosity and wavelength, but it might exist in these sample gas and it is right. The chemical luminosity by the ozone of (b) and (c) is not detected by the assembly of optics characteristic (optical filter), so it is right. @ Negative interference Negative interference is caused by the deprivation of excitation energy from excitation molecule by the interference ingredient, so it occurs only when measurement ingredient and interference ingredient coexist. ‘The indication of negative interference is water and carbon dioxide (co:). If the concentration of carbon dioxide is stable, it influences No concentration by the stable ratio. With decompression, the flow ratio of sample gas that is introduced into cell and oxygen contained ozone changes and the sample gas ratio diminishes. ‘The influence of carbon dioxide can be diminished, so it is right.Table of Contents Table of Contents Section I : Installation Overview 1-1, Analyzer Environment 1-2, Bench Space Requirement 13 1-3. Power Requirements 1-4. Analyzer Gas Lines 1-4 1-5. Gas Feed Tubing/Exhaust Tubing 15 Section 2 : Unpacking and Checking the Standard Accessories 2-1, Unpacking the TN-110 (Carton No.1) 21 2-2. Checking the TN-110 Main Unit Standard Accessories 21 2-3. Unpacking the ND-100 (Carton No.2) 22 2-4. Checking the ND-100 Standard Accessories 2.2 2-5. Unpacking the Model TX-3BC Automatic Boat Controller 2-3 (ABC) (Carton No.3) 2-6. Checking the ABC Standard Accessories 23 2-7. Unpacking the Vacuum Pump Model GLS-050 (Carton No.4) 2-4 2-8. Checking the Vacuum Pump Standard Accessories 24 Section 3 : Assembling the TN-110 3-1. Assembling the TN-110 Main Unit 3-1 3-1-1. Preparation of Gas Feeding Tubing 3-1 3-1-2. Setting the TN-110 Main Unit Power Voltage 3-2 3-1-3. Connecting the Power Cable 3-3 3-1-4, Assembling the Pyrolysis Tube 3-4 3-1-5. Setting the Pyrolysis Tube 3-6 3-2. Assembling the ABC 3-7 32-1, Attaching the Septum & Septum Holder 3-7 3-2-2. Fixing of the ABC Fixing Plate 3-8 3-2-3. Connecting the ABC to the Main Unit 3-9 3-2-4, Setting of the Ladle (Pushrod) to the Guide Tube 3-10 3-2-5. Setting the Guide Tube 3-11 3-3. Gas Tubing 3-12 3-4. Wiring & Tubing 3-13‘Table of Contents 3-5. Installing the PC System Program 3-16 3-5-1. System Requirements to Run the TN-110 System Program 3-16 3-5-2. Disk Space Requirements 3-17 3-5-3. Installing the TN-1 10 System Program on Windows ® 95/98 3-17 3-5-4, Installing the Microsoft Excel 3-18 Section 4 : Construction and Function of the TN-110 4-1. Configuration of the TN-110 41 4-1-1. Outer View of the TN-110 System 41 4-1-2. Standard and Optional Units of the TN-110 42 4-2. Component Names and Functions 43 4-2-1. Front View of the ND-100 4-3 4-2-2, Rear View of the ND-100 45 4-2-3, Front View of the TN-110 Main Unit 47 4-2-4, Rear View of the TN-110 Main Unit 49 4-2-5. Front View of the Automatic Boat Controller (ABC) 4-11 4-2-6, Rear View of the Automatic Boat Controller (ABC) 4-12 4-2-7, ABC Operation Panel 4-13 Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-1 Measurment Principles - 5. Sample inappropriate for measurement | 5 5-2. Preparation of Reagent 5-3. Analyzing Procedures -1. Operational Flow Chart 5-4 5. 3: -2, Interference at chemiluminescence method 5- 3. 5. : Eleotricity and Gas Supply 5-5 5-3-3. Getting Started with TN-110 and ND-100 5-6 5-3-4, System Setup [Definition of Accessory and Mode] 5-8 5-3-5, Setting the Analysis Parameters 5-1 5.3.6. Gas Flow Rate Setting and Gas Leakage Test 5-16 5-3-7. Heater ON 5-18 5-3-8. Ozone Generator ON 5-18 5-4, Pre-baking of the Sample Boat 5-19 5-5. Measurement of Standard Sample 5-24 5-5-1. Measurement of Standard Sample [Run Method] 5-24 5-5-2, Measurement of Standard Sample [Show/Edit Results] 5-32 5-5-3. Go Back to the Previous Run / Go to the Next Run 5-33 5-5-4, Measurement of Standard Sample [Add / Delete / Edit Functions] 5-34‘Table of Contents 5-6. Measurement of Sample 5.35 5-6-1. Measurement of Sample [Run Method] 5-35 5-6-2. Measurement of Sample [Show/Edit Results] 5-40 5-6-3. Go Back to the Previous Run / Go to the Next Run. 5-41 5-7. Database Report, Re-calculation & Browse Results 5-42 S-Tel. Report 5-42 3-7-2. Re-calculation 5-45 5-7-3. Browse Results 5-48 5-8. Heater Off & Stopping the ND-100 & TN-110 551 Section 6 : Maintenance 6-1. Daily Maintenance 61 6-2. Regular Maintenance 6-2 6-2-1. Replacement of the Ozone Scrubber 6-3 6. Replacement of the Vacuum Pump Oil 6-3 6-2-3. Replacement of the Activated Carbon and Ceramic Wool in the 6-4 ‘Vacuum Pump Scrubber 6-2-4, Maintenance of the catalyst 6-5 6-2-5, Replacement of the catalyst 6-5 Section 7 : Troubleshooting 7-1, Electrical & Mechanical Troubleshooting Tel 7-2. Analytical Troubleshooting 7-5 Appendix A : CONSUMABLE SPARE PARTS LIST Appendix B : ERROR MESSAGES Appendix C : STANDARD SPECIFICATIONSSection 1: Installation Overview Section 1 : Installation Overview This section tells you an installation overview and the basic installation requirements of the Total Nitrogen Analyzer Model TN-110, and the Model TX-3BC Automatic Boat Controller (ABC). 1-1. Analyzer Environment ‘Model TN-110 should be installed and operated in a general purpose laboratory environment only, Please note the following environment requirements when installing Model TN-110, CAUTIONS ‘Do not install the unit in a place where flammable items are not allowed. [Avoid installation in a place where extremely cold or hot temperatures may occur. Temperatures and humidity shall not exceed 15 to 35 °C and 45 to 80 % RH respectively. Avoid installation in direct sunlight or bright locations. Avoid installation in strong electric magnetic noise location.Section | ; Installation Overview Avoid installation in a place which may be exposed to considerable dust or dirt. Do not install the unit on an unstable or uneven surface. ‘The TN-110 must be placed in a level surface to permit proper operation, [Avoid installation in a place where the ventilation or air circulation is poor. [Avoid installation in a place where any flammable item such as curtain is located near the fans of the rear panel. @@@e@Section I : Installation Overview 1-2. Bench Space Requirement Tilustration 1-1. shows the ND-100 / Model TN-110, ABC and personal computer bench space requirement. Ifa printer or any other optional unit is used, you may need additional space. Size :ND-100 260(W) = 400(D) x 435(H) mm. Model TN-110 Main Unit 330(W) x 400(D) x 435(H) mm Model TX-3BC ABC 440(W) x 250(D) x 180(H) mm Weight: ND-100 ITkg Model TN-110 Main Unit 17 kg Model TX-3BC ABC I kg ‘TN-110 Main Uait PC By local disuibutor supply) ent ND-100 Printer (Option) “Approx. 2,000 mm [Note : Additional space for the Vacuum Pump is needed under the bench. Iustration 1-1, Bench Space RequirementSection I : Installation Overview 1-3. Power Requirements Table 1-1. shows the power requirements for the system, Make certain the electrical voltage is a constant source with no severe drops or spikes in the voltage. If the power source is not stable, install a power conditioner on the AC Tine. Make sure the correct fuse size to be used. Ttems Power Souree Capacity | Number of Plugs ‘ND-100 ‘AC 100/115/230/240 V, 500 VA. 1 50/60 Hz. ‘TN-110 Main Unit. | AC 100/115/230/240 V, | 1,000 VA 1 50/60 Elz ‘ABC ‘AC 100/115/230/240 V, 40VA 1 50/60 Hz Computer i Display Make sure the specifications. 1 Printer 1 Table 1-1, Power Requirements |-4. Analyzer Gas Lines ‘Two types of gases are required for ND-100 / TN-110 operation : * Argon © Oxygen ‘Table 1-2. shows the gas specifications. Gas Purity Recommended | Consumption Input Pressure ‘Argon 99.98% or more | 294-490 kPa 400 mi/min Oxygen 99.7% ormore | 294-490 kPa ‘500 mi/min ‘Table 1-2. Gas Specifications © Lkg/em’G = 98,066 kPaSection | : Installation Overview 1-5. Gas Feed Tubing / Exhaust Tubing Prepare the gas feed tubing (Argon, Oxygen) in the center of the installation place. Metallic tubing with a 3mm outer diameter is available. Use clean gas feed tubing free from contamination and foreign matter. Blow the gases through new tubing for a few minutes to remove foreign matter before connection. «Adjust the input pressures of Argon and Oxygen at the same pressure from 294 — 490 kPa ( - 5 kg/cm G). Prepare the analyzer exhaust tubing in the left side of the installation place. Illustration 1-2. shows the gas feed tubing arrangement. ‘Argon ‘Oxygen Ss 2.600 mm 750 mm Deey Mlustration 1-2. Gas Feed Tubing Arrangement. 1s‘Section 2 : Unpacking and Checking the Standard Accessories Section 2 : Unpacking and Checking the Standard Accessories 2-1. Unpacking the TN-110 (Carton No. 1) Carefully unpack and inspect the TN-110. If possible, please store the cartons and all packing material for possible future use. 2-2. Checking the TN-110 Main Unit Standard Accessories ‘Table 2-1. shows the Main Unit standard accessories. The following accessories are included in the Main Unit carton. Make sure that all parts and supplies are available. No. Description Quantity [Check 1_| Model TN-110 Main Unit 1 pe 2__| Thermal Insulator (Right) 1 set 3__| Thermal Insulator (Left) I set 4 | Fumace insulating Ring pe 5_| Clip, P18 Lpe 6 | Quartz Wool, 5g i bag 7_| Oxygen Gas Inlet Connector /30-GRU-SP Ipc 8 | Argon Gas Inlet Connector / 30-6RUE4-SP pe. ‘9 | O-Ring, P-16 5 pes/set 10_| Tweezers 1pe 11 [Argon / Oxygen Gas PIFE Tubing, 12m Lpe 12 | Oxygen Gas PTFE Tubing, 0.7m Lpe 13 | Main Unit Power Cable Tpe (AC 100/115V or AC 230/240V) 14 | 2P/3P Converting Plug Tpe [BY 15 | Fuse, (65 Dia x 321) 3.15A or 2A 2 pes/set 16 | Thermal Fuse 93 °C ipe 17 | RS-232C Cable, 9-pin, Cross Type Tpe 18 | Spanner (10X12) 2pes 19 | Screwdriver T pe 20 | TN-110 System Program 1 set 21 | Tnstruction Manual for TN-110 Ipe ‘Table 2-1. Main Unit Standard Accessories 2Section 2: Unpacking and Checking the Standard Accessories + * Mark : Quantity supplied as standard accessories are different from the actual sales unit for the spare parts. » See Appendix A “ Consumable Spare Parts List ”. 2-3. Unpacking the ND-100 (Carton No. 2) Carefully unpack and inspect the ND-100. If possible, please store the cartons and all packing material for possible future use. 2-4. Checking the ND-100 Standard Accessories ‘Table 2-2. shows the ND-100 standard accessories. The following accessories are included in the Main Unit carton. Make sure that all parts and supplies are available. No. Description ‘Quantity Check 1_[ND-100 Main Unit I set 2_| Female Ball Joint for Combustion Tube Tpe 3_| Fluororubber Joint Tube I pe 4 [Ozone Scrubber Tpe 3_[ Ozone Somber Holder Dpesiset 6 | Magnet Label S pesiset 7 | ND-100 Power Cable Tpe (AC 100/115 V or AC 230/240 V) & | 2/3P Converting Plug Tpe 1i5V Only 9 _| Fuse, (65 Dia x 321) 63A of 3.15A 2 peslset 10 | Signal Cable / RS-232C 25 pin Straight Type Tpe I1_[T type Union GTTT-B with copper tube) pe * 12 | Disposable Filter with PTFE Tube set 13 | Gastight Microsyringe, 1705-N, 50 ul T pe Table 2-2. ND-100 Standard Accessories 22Section 2: Unpacking and Checking the Standard Accessories 2-5. Unpacking the Model TX-3BC Automatic Boat Controller (ABC) (Carton No. 3) Carefully unpack and inspect the ABC. If possible, please store the cartons and all packing material for possible future use. 2-6. Checking the ABC Standard Accessories Table 2-3. shows the ABC standard accessories, The following accessories are included in the ABC carton, Make sure that all parts and supplies are available. 1 | ABC Main Uni 1 set 2_ | ABC Fixing Plate Lpe 3_| Outer Pyrolysis Tube with Catalyst ipe - 4 _| Inner Pyrolysis Tube pe 5__| Spring for Pyrolysis Tube 2 pos/set | * 6 | ABC Signal Cables’ I pe 7 | ABC Cooling Unit Power Cable lpe ‘(AC 100/115 V or AC 230/240. VY) 8 |2P/3P Converting. Plug pe 11s V Only 9 | Fuse {Cooling Unit), 2A’ 2 pe/ set 10 | Guide Tube Ipc 11_| Ladle (Pushrod) lpe 12_[ Magnet Lpe 13_| Sample Boat. 2 pel set | * 14 | Glass Petri Dish lpe 15 | Septum Holder lpe Already Installed 16 | Septum (Flat-type) 100pes/ 17_[ Packing for Sample Inlet Port 1 pe Table 2-3. ABC Standard Accessories Note * * Mark : Quantity supplied as standard accessories are different from the actual sales unit for the spare parts. «See Appendix A “Consumable Spare Parts List”. 23Section 2: Unpacking and Checking the Standard Accessories 2-7. Unpacking the Vacuum Pump Model GLS-050 (Carton No.4) Carefully unpack and inspect the Vacuum Pump. If possible, please store the cartons and all packing material for possible future use, 2-8. Checking the Vacuum Pump Standard Accessories Table 2-4. shows the Vacuum Pump standard accessories. The following accessories are included in the Vacuum Pump carton, Make sure that all parts and supplies are available. No. ie. z Quantit ‘Check Description : 1 | Vacuum Pump Model GLS-050 set (AC 100/115 V or AC 230/240 V) 2_| Vacuum Pump Oil (Demunum S-20) kg Lott 3_| Vacuum Pump Scrubber Tpe 4 | Vacuum Pump Suction Tube 2.5 m. 1pe 5__| Hose Clamp for Vacuum Pump Scrubber 1pe = 6_| Cup for Vacuum Pump Ipe_|* ‘Table 2-4. Vacuum Pump Standard Accessories Note « * Mark : Quantity supplied as standard accessories are different from the actual sales unit for the spare parts. «See Appendix A “Consumable Spare Parts List”. 24Section 3 : Assembling the TN-110 Section 3 : Assembling the 110 This section covers procedures for assembling (installing) the Model TN-110. 3-1, Assembling the TN-110 Main Unit 3-1-1. Preparation of Gas Feeding Tubing Use clean gas feed tubing free from contamination and foreign matter. Blow the gases through new tubing to remove foreign matter before connection. Tllustration 3-1. shows procedures for connecting gas feed tubings to the ND-100 and the TN-110 Main Unit (Rear). —cas-PuRcE— a SAMPLE ifr Ilustration 3-1. Connecting Gas Feed Tubing (Argon and Oxygen) to the TN-110 Main Unit and ND-100Section 3: Assembling the TN-110 3-1-2. Setting the TN-110 Main Unit Power Voltage WARNING a Always turn off the Main Power of the ND-100 and the TN-110 Main Unit and all optional units connected to it before setting the power voltage Set the voltage corresponding to the AC power line I Confirm the Voltage Setting Dial of the ND-100 corresponding to the AC power supply. If the setting is not correct, sot the Dial and Switch to the right voltage. 2 Confirm the Voltage Setting Dial of the TN-110 Main Unit corresponding to the AC power supply. Ifthe setting is not correct, set the Dial and Switch to the right voltage. Refer to Illustration 3-2. for setting the desired voltage TN-110 Main Unit. Set the Voltage Setting Dial corresponding to the AC power supply. ‘The Voltage Selector ND-100 must be set as same as TN-110 Main Unit. Upper Position : 100/115 V Lower Position : 230/240 V Must be Off position. Illustration 3-2. Setting the Power Voltage voltage setting of the Personal Computer and the Printer. 32Section 3 : Assembling the TN-110 3-1-3. Connecting the Power Cable Te ‘Turn off the Power Switch OFF before working. (TN-110 Main Unit, ND-100, ABC, PC, Printer...) ‘Tum the TN-110 Main Unit Power Switch on the rear panel OFF, and connect the power cable to the Power Connector. Also, connect the proper power cable to the ND-100. ARNING Incomplete grounding sometimes causes an electrical shock by touching metal parts of the body. Use a power line with electrical fluctuation less than + 10%.Section 3: Assembling the TN-110 3-1-4, Assembling the Pyrolysis Tube J Fittup about 25mm and 20mm Quartz Wool and 30mm Catalyst in the Outer Pyrolysis Tube. (See Illustration 3-3.) Optional Quartz Wool Poker : P/N TX2RTI is recommended. ‘The standar ND-100 includes the “Outer Pyrolysis Tube wit lyst : L po”. NOTE The length of the Quartz Wool (25mm and 20mm) and the Catalyst (30mm) is very important for analytical performance. 75mm Illustration 3-3. Plugging Quartz Wool and Catalyst 34Section 3 : Assembling the TN-110 2 insert the Inner Pyrolysis Tube into the Outer Pyrolysis Tube in which Quartz Wool and Catalyst have been plugged. Attach the Inner Pyrolysis Tube to Outer Pyrolysis Tube with two springs. (See Mustration 3-4.) Springs Outer Pyrolysis Tube Inner Pyrolysis Tube Illustration 3-4. Assembling the Pyrolysis Tube 35Section 3: Assembling the TN-110 3-1-5, Setting the Pyrolysis Tube Insert the Pyrolysis Tube (Assembled in 3-1-4) into the right side of the Main Unit. (Gee Iustration 3-5.) Fix the Thermal Insulators (Right & Left). Fumace Insulating Ring: PINTXSRPR Pyrolysis Tube With Catalyst Illustration 3-5. Setting the Pyrolysis Tube NOTE : Illustration 3-5 is not exactly the same. CAUTION Be careful not to break the Furnace Insulating Ring. [Fix the Thermal Insulator properly by the supplied Plus/Minus Screw Driver. | 36Section 3 : Assembling the TN-110 3-2. Assembling the ABC 3-2-1. Attaching the Septum & Septum Holder Attach the Septum and Septum Holder. (See Illustration 3-6,) Septum : P/N TNSSIS ‘Septum Holder : PIN TX3SED Illustration 3-6, Attaching the Septum and Septum Holder iT Septum Holder should be fixed with finger tight to avert danger of gas leakage! and avoiding to break the needle. Septum should be replaced every day.Section 3: Assembling the TN-110 3-2-2. Fixing of the ABC Fixing Plate Fix the ABC Fixing Plate to the left side of the ABC. (See Illustration 3-7.) ABC Fixing Plate : P/N TX3RKB. ‘IMustration 3-7. Fixing of the ABC Fixing PlateSection 3 : Assembling the TN-110 3-2-3. Connecting the ABC to the Main Unit I contiem thatthe O-Ring (P-16) in the Sample Inlet Port is nether damaged nor deformed. (See Dlustration 3-8.) 2 Fix the ABC to the right side of the Main Unit. Tighten the O-Ring Holder lightly, and insert the Pyrolysis Tube to the end. (See Mlustration 3-8.) ‘Screw for Sample Inlet Port : PIN TX3BOF Fasten with the Screw Driver (© Ring ( P-16) : P/N'TX020 Ilustration 3-8. Connecting the ABC to the Main unit Connect the ABC to the Main Unit carefully not to break the Pyrolysis Tube 39Section 3: Assembling the TN-110 3-2-4, Setting of the Ladle (Pushrod) to the Guide Tube I Take outthe Ladle from its case, and insert it into the Guide Tube. (See Mustration 3-9.) 2 Put the Magnet on the surface of the Guide Tube. (See HMustration 3-9.) 3 set the Magnet so that the end of the Guide Tube projects 20 to 30 mm. (See Mlustration 3-9.) Guide Tube : P/N TX3RTG Ladle : PIN TX3RDL fe —$———— SSS Mognet: PNTIRIM Illustration 3-9. Setting of the Ladle and the Guide Tube 3410Seetion 3 Assembling the TN-110 3-2-5, Setting the Guide Tube A Conficm thatthe O-Ring (P-16) in the ‘Sample Inlet Port is neither damaged nor deformed. (See Illustration 3-10.) 2 Tighten the O-Ring Holder lightly, and insert the Guide Tube completely. (See Illustration 3-10.) ‘Ax Gas Intet Comnector /30-6RUE4-SP : PINTXOBIL Lightly tighten with your hand Screw for Sample Inlet Port : PIN TX3BOP (O-Ring (P-16) : PIN TX020 ‘Mlustration 3-10. Setting the Guide Tube BulSeation 3 : Assembling the TN-110 3-3. Gas Tubing I Place the Oxygen Gas Inlet Connector over the branch of the Outer Pyrolysis Tube. Fasten the joint completely, and tighten the box nuts with a spanner slightly. (See Illustration 3-11.) 2 Pace the Argon Gas Inlet Connector over the Guide Tube inlet. Fasten the joint completely, and tighten the box nuts with a spanner slightly. (See IMustration 3-11.) 3 Connect one end of the Oxygen Gas PTFE tubing to the Oxygen Gas Outlet on the rear side of the Main Unit and the other end to the Gas Inlet Connector which has been connected to the Outer Pyrolysis Tube as mentioned 1. Insert completely, and tighten the box nut with a spanner. (See Illustration 3-11.) 4 Connect one end of the Argon / Oxygen Gas PTFE tubing to the Argon Gas Outlet on the rear side of the Main Unit and the other end to the Gas Inlet Connector which has been connected to the Guide Tube as mentioned 2. Insert completely, and tighten the box nut with a spanner. (See Mustration 3-11.) ‘Oxygen Gas Inlet Connector /30-GRU4-SP = PIN TNDITG ‘Argon Gas Inlet Connector / 30-6RUE4- SP : PIN TXIBIL Iustration 3-11. Gas Tubing 342Section 3 : Assembling the TN-110 3-4. Wiring & Tubing (CAUTION Always tum off the power to the ND-100 and TN-110 Main Unit and the ABC| before connecting the necessary cables. I Connect the end of the Pyrolysis Tube to the Female Bell Joint for Comeustion Tube: P/N TNSLIT and Fluororubbet Joint Tube : P/N TNSJTF. And then, connect it to PTFE Tube (3x2 mm). (See Illustration 3-12.) Female Ball Joint for Combustion ‘Tube : PIN TNSLIT Bad of the Pyrolysis Tube lip, P-18: PIN TX020 Fluororubber Joint Tube : PIN TNSITF Mlustration 3-12. Connecting the Female Ball Joint 2 Connect the end of the ABC Signal Cable to the ABC Port on the back ofthe Main Unit, Connect the other end of the ABC Signal Cable to the ABC Signal Cable Connector (Main Unit) on the back of the ABC. | 3 Connect the end of the RS-232C Cable (9-pin, Cross Type) to the ‘Computer Port on the | back of the Main Unit. Connect the other end of the RS-232C Cable to the COM 1 Port on. ' the back of the PC. Connect the ND-100 Power ‘Cable(), TN-110 Main Unit Power Cable (@) and the ABC Cooling Unit Power Cable. (Connect also the power cable of the PC and printer.) (See Mustration 3-13.) J Connect the end of the RS-232C Cable (25-pin, Straight Type) to the OPTION 2 Port (@) on the back of the TN-110 Main Unit. Connect the other end of the RS-232C Cable to the RS-232C (®) on the back of the ND-100, (See Illustration 3-13.) 343Section 3 : Assembling the TN-110 6 Connect the Disposable Filter with PTFE Tube (©) between the sample out (From ‘TN-110) and the SAMPLE back of the ND-100. (See Illustration 3-13.) 7 Connect the Ozone Serubber with Tube (®) to the Vacuum Pump. (See Ilustration 3-13.) TN-110 aL Y @ \? ad o Fa + ND-i00 Sy _| FE [ ° el Gn Mlustration 3-13. Wiring and Tubing ND-100 314Section 3: Assembling the TN-110 8 Assemble the Vacuum Pump Model GLS-050, 1. Fill the Vacuum Pump Oil up to the middle of oil level gauge. (Demnum S-20, lkg : P/N TNSVGF) 2. Fix the Vacuum Pump Scrubber : P/N TNSVPR. 3. Connect and fix the Vacuum Pump Suction Tube. Oil level gauge Illustration 3-14, Assembling the Vacuum Pump 35Section 3 : Assembling the TN-110 3-5. Installing the PC System Program 3-5-1. System Requirements to Run the TN-110 System Program Following are the recommended system requirements for running TN-110 System Program. . . PROCESSOR : Pentium 133MHz or higher RAM : 32 megabytes or higher DISPLAY : 800 x 600 Monitor Resolution / 256 Color or higher os : Microsoft® Windows® 95/98 English Language Version Only DRIVE + CD-ROM C. Tt should be noted that if your computer does not meet the above specifications, the performance can not be assured. CAUTION Use only Microsoft® Windows® 95/98 English Edition. If other language of Windows® 95/98 is used, the performance can not be $ J assured. c Do not use other application software when the TN-110 System Program is running, The performance of the system can not be guaranteed.Section 3 : Assembling the TN-110 3-5-2. Disk Space Requirements Hard Disk space needed for installing the TN-110 System Program is approx. 10 megabytes. ‘More than 40 megabytes free space would be needed to save all the analysis results and graphs for 1 year operation. Also, more than 10 megabytes free space would be required for Windows®95/98, 3-5-3. Installing the TN-110 System Program on Windows®95/98 ‘You can use the TN-110 System program / Setup Program to install on your hard disk from CD-ROM. [CAUTION Ifyou are using a virus-detection utility, disable it before you run the Setup Program. Also close any open Windows® applications. [Installation by CD-ROM] I Insert the Setup CD-ROM in CD-ROM drive. 2 Click the Start button, click “Settings”, and then click “Control Panel”, 3 Double-click the “Add / Remove Program” icon, 4 On the Install / Uninstall tab, click the “Install” button, J Follow the Setup instructions on the screen, 3417Section 3: Assembling the TN-110 3-5-4. Installing the Microsoft Excel I insert the Excel CD-ROM in CD-ROM drive. 2 Click the Start button, click “Settings”, and then click “Control Panel”. 3 Double-click the “Add / Remove Program” icon. 4 On the Install / Uninstall tab, click the “Install” button. 5 Follow the Setup instructions on the screen. 6 When installing Excel, select “custom setup”. Set up “Visual Basic Data Access Object” of “Data Access Function” option. CAUTION Please note : It is strongly recommended to install Microsoft Excel by “custom setup”, Otherwise, TN-1 10 system program [can not be operated.Section 4 : Construction and Function of the TN-110 Section 4 : Construction and Function of the This section describes about construction and function of the TN-110. 4-1. Configuration of the TN-110 4-1-1, Outer View of the TN-110 System Mlustration 4-1. shows the ND-100, Model TN-110, ABC and personal computer, printer outer view. (ND-100, TN-110 MAIN UNIT, AUTOMATIC BOAT CONTROLLER, PERSONAL COMPUTER, PRINTER/OPTIONAL) PC (By local distributor supply) ‘TN-110 Main Unit Mlustration 4-1. Outer View of the TN-110 System aSection 4 : Construction and Function of the TN-110 4-1-2, Standard and Optional Units of the TN-110 Ilustration 4-2. shows standard and optional units of the Model TN-110. Model TN-110 Standard Set Personal, Computer (By local distributor supply) ND-100 TN-110 Main Unit ‘Automatic Boat Controller Model TX-3BC Vacuum pump Illustration 4-2. Standard and Optional Units of the TN-110 42Section 4 : Construction and Function of the TN-110 4-2, Component Names and Functions 4-2-1. Front View of the ND-100 Illustration 4-3. shows the front view of the Main Unit and Table 4-1. shows the names and functions. 4, Ozone Generator Power LED 2. ND-100 Power LED 4. ND-100 Power Switch 3, Ozone Generator Power Switch Illustration 4-3. Front View of the ND-100 43Section 4 : Construction and Function of the TN-110 No. Name Symbol Funetion ND-100 Power Switch ‘Power supply to ND-100, POWER ND-100 Power LED ‘This LED (green) is lit when Power ——- _| Switch is turned on. Ozone Generator Power Switeh Power switch for the Ozone Generator. (CAUTION), This switch should not be turned ON without connecting the Vacuum Pump. When the sample measurement is not performed, it is recommended that this switch is TURNED OFF! OZONIZER NEVER turn this switch ON unless the Oxygen gas is flowing. Ozone Generator Power LED This LED (green) is lit when the Ozone ——— _| Generator Power Switch is turned on. The Ozonizer is controlled by the TN-110 System Program. [System-Ozonizer] ‘Table 4-1, Names and functions of the ND-100 Front PanelSection 4 : Construction and Funetion of the TN-110 4-2-2. Rear View of the ND-100 Illustration 4-4, shows the rear view of the Main Unit and Table 4-2. shows the names and functions. | |) spe | } EBS Le B 3 a Illustration 4-4. Rear View of the ND-100 45Section 4 : Construction and Function of the TN-L10 4-2-3. Front View of the TN-110 Main Unit Mlustration 4-4. shows the front view of the Main Unit and Table 4-3. shows the names and functions. 5 1 [Power Connector | acPOWER | For powe: supply to the ND-100 Detector Unit. 2 | Fuse Holder FUSE | 6.3 Amps (for AC 100- 120V) and 3.15 Amps (for AC 220 - 240V). Verify the correct fuse size for the line voltage to be used. 3 | Ground Terminal GND | Ground terminal for the ND-100. 4 | Ozone Scrubber ‘OZONE _ | Activated carbon is packed in. SCRUBBER | Excess ozone gas is absorbed here. The life time is about half a year. The Vacuum Pump Suction Tube : ‘INSVPT is connected to the outlet. 3 | Recorder Terminal | RECORDER | Analog output for the recorder. (DC 0-1 V Full Seale} © | RS-232C Port RS-232C__| Use this port to connect the RS-232C Signal Cable to the TN-110 Main Unit (Option 2 Port). Use RS-232C 25 pin, straight type cable. 7 | Flow Adjuster PCV (Os) _| Adjusts Oxygen gas flow used for generating ‘Ozone gas. 8 | OxygenGas Inlet | GAS IN (O;) | Gas inlet for Oxygen. Use stainless steel tube, 3mm OD. ‘9 | Sample Gas Inlet_| SAMPLE | Sample Gas from the TN-110 is fed in here. 10 | Oxygen Gas Bypass O2 ‘Oxygen is released into the air here. Line 11 | Sample Gas Bypass [sample _] Sample gas from the TN-110 is released into Line the air here. 12 | Voltage Selector | VOLTAGE power vonage 100V/1SVA30v240V used. SELECTOR |} Remove the protection cover and set the required voltage with this switeh. Refer to “3-1-2. Setting the TN-110 Main Unit Power Voltage” for the detail. 13 | Power Connector PUMP | For power supply to the Vacuum Pump. for the Vacuum ‘When turning the ozonizer switch on at Pump TN-110 program ide, pump starts up. ‘When turning the ozonizer switch off at ‘TN-110 program side, pump stops after three minutes. ‘Table 4-2. Names and functions of the ND-100 Rear Panel 46Section 4: Construction and Function of the TN-110 Illustration 4-5. Front View of the TN-110 Main Unit arSection 4 : Construction and Function of the TN-110 No. Name Symbol Function Power Switch POWER ‘Power supply to Main Unit and ABC. For heating, switch on both POWER. and HEATER. Power LED This LED (green) is lit when Power Switch is turned on, Heater Switch HEATER This switch is a pilot switch for heating. Heater on/off is controlled by PC. Heater LED This LED (green) is lit when the Electric Furnace is under control. Adjustment Knob for Argon 7 Oxygen Ar/O For adjusting flow rate of Argon/ Oxygen. Actual flow rate is displayed on the sereen (PC). When the knob is turned to counterclockwise, thee flow rate is increased. ‘Oxygen LED ‘This LED (red) is lit when Oxygen flows in the Inner Pyrolysis Tube. Adjustment Knob for Oxygen For adjusting flow rate of Oxygen. Actual flow rate is displayed on the sereen (PC). When the knob is turned to counterclockwise, the flow rate is increased. ‘Table 4-3. Names and functions of the Main Unit Front Panel 48Section 4 : Construction and Function of tae TN-110 4-2-4. Rear View of the TN-110 Main Unit Mlustration 4-6. shows the rear view of the Main Unit and Table 4-4, shows the names and functions. Ilustration 4-6, Rear View of the TN-110 Main Unit — 49Section 4 : Construction and Function of the TN-110 No. Name Symbol Function 1 | Computer Port COMPUTER | Use this port to connect the PC. (RS-232C/ 9-pin / cross type cable is used.) 2 | ABC Port ABC Use this port to connect the ABC, (Unphenol 25-pin cable is used.) 3 | Option 1 Port OPTION 1 | Use this port to connect optional units such as CRI, ASC. (RS-232C/ 25-pin /straight type cable is used.) 4 | Option 2 Port OPTION 2 _ | Use this port to connect the ND-100. 5 | Balance Port BALANCE ‘Use this port to connect a balance. 6 | Heater 15A HEATER | No Fuse Breaker. 7 | Power Connector | ACPOWER | For power supply to the Main Unit. 8 | Fuse Holder FUSE 3 Amps (for AC 100 - 120V) and 2 Amps (for AC 220 - 240V). Verify the correct fuse size for the line voltage to be used. 9 | Ground Terminal GND Ground terminal for the Main Unit. 10 | Main Power MAIN POWER | Switch for main power (Leakage Breaker). Switch Usually, itis left “ON”. 11_| Leakage Indication LEAK | When leakage eauses the power to go Button “OFF”, this button comes out of the front. 12 | Leakage Test TEST For leakage test. Button 13 | Oxygen Gas Tnlet_| GASIN(;) | Gas inlet for Oxygen. Use stainless steel tube, 3 mm OD. 14 | Argon GasTnlet_| GASIN(Ar) _| Gas inlet for Argon. Use stainless stecl tube, ‘3mm OD. IS | Oxygen Gas Outlet | GAS OUT (02) | Gas outlet for Oxygen. 4 mm OD PTFE tube is connected. 16 | Argon Gas Outlet | GAS OUT (An) | Gas outict for Argon. 4 mm OD PIFE tube is connected. I7 | Voltage Selector Power voltage 100V/115V/230V/240V is used. Remove the protection cover and set the required voltage with this switch. Refer to “3-1-2, Setting the TN-110 Main Unit Power Voltage” for the detail. 18 | Cooling Fan Fan motor for cooling the inside of the Main Unit Table 4-4. Names and functions of the Main Unit Rear Panel 410Section 4 : Construction and Function of the TN-110 4-2-5. Front View of the Automatic Boat Controller (ABC) Ilustration 4-7, shows the front view of the ABC and Table 4-5, shows the names and functions. Mlustration 4-7. Front View of the ABC ae Name Function 1 | Operation Panel | ABC operation panel. See “4-2-7. ABC Operation Panel” for the detail 2 | Magnet Arm An arm for transferring the Ring Magnet, 3_| Sample Inlet Port_[ A box for insertion and taking out of die Sample Boat, 4 | Cooling Unit For cooling sample boat. 5_| Guide Tube Stand [A fixing metal for the Guide Tube. 6 | Safety Cover A protection cover against explosion. IFit opens during automatic operation, ABC automatically stops. The Safety Cover must be closed all the time. Table 4-5. Names and function of the ABC Front Panel 4‘Section 4 ; Construction and Function of the TN-110 aiaSection 4: Construction and Function of the TN-110 4-2-6. Rear View of the Automatic Boat Controller (ABC) Ilustration 4-8, shows the rear view of the ABC and Table 4-6, shows the names and functions. Illustration 4-8, Rear View of ABC No. Name Symbol Function 1 | Cooling Unit Power | COOLING | Power supply to the Cooling Unit. Switch UNIT POWER 2 ‘Power Connector AC POWER] For power supply to the Cooling Unit. 3 Fuse Holder FUSE 2AT |~ 3 Amps (for AC 100 - 120V) and 2 Amps (for AC 220 - 240V), Verify the correct fuse size for the line voltage to be used. 4 | ABC Signal Cable MAIN UNIT | Signal cable connector of the ABC to Connector the Main Unit, 5-_| Ground Terminal === | Ground terminal for the ABC. 6 | ABC Fixing Plate For fixing the ABC to the Main Unit, Table 4-6. Names and functions of the ABC Rear Panel 413Section 4 : Construction and Function of the TN-110 4-2-7, ABC Operation Panel Illustration 4-9. shows the ABC operation panel and Table 4-7. shows the names and functions. Zh f Ilustration 4-9, ABC Operation Panel bd Name Symbol Function 7 | Automatic LED ‘AUTO | This LED (green) is lit during the automatic operation. 2 | Oxygen LED 02 ‘This LED (red) is lit when Oxygen flows in the Inner Pyrolysis Tube. 3 | Power LED POWER | This LED (green) is lit when Power Switch is turned on. 4 | Forward Switeh FWD __ | Switch to move Sample Boat forward in manual mode. It works only in the ABC ‘Manual Operation. 5 | Reverse Switeh REV | Switch to move Sample Boat backward in manual mode. It works only in the ABC Manual Operation. ‘Table 4-7, Names and functions of the ABC Operation Panel 414Section 5 : Measurement of Nitrogen in Solid end Liquid Samples Section 5 : Measurement of Nitrogen in Solid and Liquid Samples This section covers procedures for measuring Nitrogen in solid and liquid samples. 5-1. Measurement Principles The sample is introduced into the combustion tube packing oxidative catalyst under Argon ‘cartier gas. High temperature oxidation (800 - 900 °C) occurs here and all chemically bound nitrogen is converted to nitric oxide (NO). NO then moves to the chemiluminescense detector where it is mixed with ozone to form excited nitrogen dioxide (NO2"). NO + 03 > NO}* + 0, > NO, +0, +hy Rapid decay of the NOz* produces light in the 590 - 2,900 nanometer range. Itis detected and amplified by a photomultiplier tube. The result is calculated from the signal produced and showed in ppm or % etc. 5-1-1. Sample inappropriate for measurement For nitrogen in sample such as sodium azide and hydrazine sulfate, No is generated as main when heated in pyrolysis tube. Therefore, recovery is extremely low at chemiluminescence method and measurement can be done accurately. Aqueous sample shows minus interference at chemiluminescence method and ‘measurement can be done accurately. 5-1-2. Interference at chemiluminescence method . Interference constituent concept At chemiluminescence method interference constituents are two types. The first is constituent which shows plus interference reacting with ozone and generating chemiluminescence. ‘The second is constituent removing excitation energy from NO2 and showing minus interference. . Plus interference sa5 : Measurement of Nitrogen in Solid and Liquid Samples ‘The following matter can show plus interference. (a) Carbonyl compound of iron and nickel (b) Olefin such as ethylene and trimethyl ethylene (© Sulfide such as dimethyl sulfide and hydrogen sulfide ‘At (a) chemiluminescence, the wavelength of measurement constituent overlaps with chemiluminescence one and photometry is done. But these substances is unlikely to exist in sample gas. At chemiluminescence of (b) and (c) substances by ozone, the wavelength of measurement is not detected by optical filter. Therefore, this has no influence on measurement. Minus interference ‘When interference constituent removes excitation energy from excitation molecule, minus interference occurs. Therefore the interference occurs when measurement constituent coexists with interference one. Water and carbon dioxide show minus interference. Therefore, aqueous sample is inappropriate for measurement. When carbon dioxide concentration is stable, NO one is influenced at fixed rate. But the pressure in reduced pressure chemiluminescence cell is reduced by vacuum. pump and interference between molecule is decreased. ‘The influence of carbon dioxide can be decreased and this has no influence on measurement, 32 oSection $ : Measurement of Nitrogen in Solid and Liquid Samples 5-2. Preparation of Reagent Please refer to the following list which mentioned necessary reagents for measuring Nitrogen. Refer to Table 5-1, No. Reagents Needed for Nitrogen Prepared by Measurement Customer? 1 | Nitrogen Standard Solution YES (Pyridine in Toluene Solution ) 2 | Nitrogen Standard Solution for Heavy Oil YES ( Standard Heavy Oil ) Table 5-1. List of Reagents ( Nitrogen Measurement ) Preparation of the Pyridine in Toluene Solution. Accurately weigh about 5.64 g of pyridine CsHsN (Special Reagent Grade) and put it in a volumetric flask of 1000 ml. Add toluene (Special Reagent Grade) up to the meniscus and dissolve all of it in the toluene. The nitrogen concentration in the solution is given by the following equation: N (ppm) = (Weight (g) CsHsN/ 1,000 ml) x (14.007 / 79.10) x 10° Take 1.00 ml of the stock solution prepared in the previous section and dilute itn the toluene from a newly opened bottle to exactly 100 ml. The concentration of the standard solution is one hundred of N (ppm) given in the above ‘equation. $3Section 5 : Measurement of Nitrogen in Solid and Liquid Samples e 3. Analyzing Procedures }-1, Operational Flow Chart E32 Electricity and Gas Supply { 53-3 Getting Started with TN-110 & ND-100 1 53-4 } System Setup [Definition of Accessory and Mode] L 53-5 Setting the Analysis Parameters L Gas Flow Rate Setting & L S32 Heater ON L 538 Ozone Generator ON 1 Sd Pre-baking of the Sample Boat } J 55 Measurement of Standard Sample ) 1 56 ) Measurement of Sample t Database Report, Re-calculation & Browse Results 4 8 eater Off & Stopping the a4Section 5 : Measurement of Nitrogen in Solid and Liquid Semples 5-3-2. Electricity and Gas Supply I Connect the ND-100 Power Cable, TN-110 Main Unit Power ‘Cable, ABC Cooling Unit Power Cable, Power Cable for PC and Printer ( If connected ). (See Illustration 3-13. for more detailed information) Table 5-2. shows the power requirements for the system. Make certain the electrical voltage isa constant source with no severe drops or spikes in the voltage. If the power source is not stable, install a power conditioner on the AC line. Make sure the correct fuse size is used. Tems Power source Capacity [Number of Plugs ‘AC 100/115/230240V, ND-100 ean 500 VA 1 TN-110 Main Unit | AC 100/115230240V, tachi 1,000 VA 1 “ABC ‘AC 100/115/230240 V, 50/60 Hz oe Z Computer I Display Make sure the specifications. 1 Printer 1 Table 5-2. Power Requirements 2 open the main valvos ofthe Oxygen and Argon gas cylinders. (See Table 53) Table 5-3. shows the required gas lines for the system and the gas specifications ‘Two types of gases are required for the ND-100 operation : *¢ Argon ¢_ Oxygen d Recommended ; Gas Purity Input Pressure _| Consumption Argon 99.98 % or more 294-490 kPa 400 mi/min Oxygen 99.7 % or more 294-490 kPa 500 ml/min ‘Table 5-3. Gas Specifications © Lkg/om?G = 98.066 kPa Adjust the input pressures (secondary pressures of the gas cylinder) of Argon and Ox, at the same pressu rs S 8 55Section §: Measurement of Nitrogen in Solid and Liquid Samples 5-3-3. Getting Started with TN-110 and ND-100 I tum the Power Switch of ND-100 Power Switch (Front Panel) Ozone Generator power Switch : ‘TN-110 Main Power Switch (Rear Panel) : 110 Power Switch (Front Panel) : ‘TN-110 Heater Switch (Front Panel) : ABC Cooling Unit Power Switch (Rear Panel): ‘Vacuum Pump GLS-050 Power Switch Personal Computer (PC) Printer (If Connected.) eeeeeekee 2 Click the Start Button, click Programs, and then click TN-110 System-TN-110 System. The TN-110 System Program is getting started. The first window “Analyst ID Window “ comes up as follows. See Iustration 5-1. ‘Mlustration 5-1. “Analyst ID” Window 3 Type “ TN-110 ” for a first entry. Click OK. “ TN-110 ” is a common ID when the operator wants to enter the system. There are registrable unique IDs to avoid risks. Click System-Preference to add Analyst ID. CAUTION Only the authorized user can enter into the ‘TN-110 System Program. 56‘Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 4 1-110 System Program status screen is shown, (See Ilistration 5-2.) Ilustration 5-2. TN-110 System Program Status ScreenSection 5 ; Measurement of Nitrogen in Solid and Liquid Samples 5-3-4, System Setup [Definition of Accessory and Mode] I Press F5 key ot click the menu System and System Setup. + “System Setup” is a definition of the connected accessories and modes. + “System Setup” must be done at the beginning of today’s run, 2 Select the Accessory which is actuary connected with the TN-110 & ND-100. In this case, Choose ABC. If the balance is connected, choose a balance. Confirm the configuration and press “Transmit”. ‘After “Transmit” button is pressed, the TN-110 System Program (PC) sends| typical parameters (i.e. Analysis Parameters) to the TN-110} ‘Main Unit, Do not choose a wrong Accessory and Mode. This may cause an error. ‘The System Setup must be done at the beginning of the measurement. 38Section 5 : Measurement of Nitrogen in Solid and Liquid Samples | ACCESSORY ] ABC : Automatic Boat Controller Model TX-3BC |ABC _: Automatic Boat Controller Model TX-3BC. [ABC is the Standard Accessory for TN-110] : Automatic Solid Sampler Model ASC-120S : Automatic Liquid Sampler Model ASC-150L : Gas Injector Model GI-100 : Constant Rate Injector Model CRI-L00H(CRI Mode) : Manual [MODE : For measuring Nitrogen in solid, liquid and gaseous samples, 59Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 3 The following window is appeared. If ABC is not in the home position, ABC moves to the home position for initializing. Mlustration 5-5. “ABC Home” in 5-10Section $ : Measurement of Nitrogen in Solid and Liquid Samples 5-3-5. Setting the Analysis Parameters J cick ti icon {ff or click the menu System and Analysis Parameters, RE Illustration 5-6. Menu “Analysis Parameters” SlSection 5 : Measurement of Nitrogen in Solid end Liquid Samples 2 The following window is appeared. Confirm the parameters. If you changed the values, press “Transmit” button to send/update new parameters to the TN-110 Main Unit. ‘Ilustration 5-7. “Analysis Parameters” Window NOTE ‘The Analysis Parameters can’t be changed during the measurement (Run-Method). S12Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 3 set the “Range”(“Sens”) to a proper value. Normally, set to “Middle”. Range [ppm] High Middle Expected Nitrogen Concentration. Less than 100 ppm Less than 500 ppm Recommended Middle Low More than 500 ppm 10ul Low ‘More than 1000 ppm 10,1 Table 5-4. “Sens” Setting 4 Recommended “Analysis Parameters” are writen below. Analysis Typical Values Parameter [Recommended] Sens Middle Integ. Delay [0 200 Slope End 20 - 50 End Thrsh (%) [10 % Det Time 5 Scan Rate a D/dat Gain 10 Normal End ON. Timer End 300 sec Base Correct |ON Min. Area 40000 Base Line 25 & Interval End 999 Temp. 1 800 TC Temp. 2 900 C Blank 0 Ax Time 30 2 Time 600 ‘Table 5-5. Typical Analysis Parameters SettingSection 5 : Measurement of Nitrogen in Solid and Liquid Samples Descriptions on Analysis Parameters Analysis Descriptions Parameter Sens "This means the sensitivity of the Detector. Tnteg. Dela; ‘The delay time for the integration, "The slope thresh old of the signal data used for detecting the starting point. The dita processing starts when the slope is larger than this thresh hold as designated in “Det Time”. ‘When the “Sens = Range” is set at “Ultra”, input “1,000” in “Slope Start”, Slope End The slope thresh hold of the signal data used for detecting the end point. The data processing ends when the slope is as many times smaller than this thresh hold as designated in “Det Time”. End Thrsh(%) “The level thresh hold of the signal data used for initiating the detection of the data processing end point. ‘The detection of the end point begins when the signal data comes down to the following thresh hold : ‘The percentage of the set “Sens” + signal level of the starting point. Det Time ‘The data checking times used for detecting the start and end points of | the data processing. Scan Rate The basic signal data is sampled every 200msec. ‘These data are collected as many as the numbers assigned in “Sean Rate”. The average value of the collected data are stored into ‘memory and used for the data processing. D/dt Gain This value is the proportional constant forthe first derivative, Normal End ‘ON: The data processing end point is determined by the signal data. [Slope End and Det Time] ‘When the analysis time exceeds the time of 1.1 Timer End, however, the data processing stops and the message is displayed. OFF : The data processing end point is determined by conditions ‘other than the signal data, fe.g. Timer End] Timer End (sec) “The assignment of the time between the start point and the end point of the data processing. In case that “Normal End” is ON, the end point is determined by the condition whichever comes earlier, Timer End or Normal End. Base Correct The base line of the signal data is corrected to a transitional one, the cend point level of the previous analysis, when the end point of the data processing is determined by Timer End. Min. Area Tn order to distinguish a signal from a noise, the minimum thresh hold area is set. If an integrated area is smaller than this thresh hold area, itis not regarded as effective signal. S14Section 5 : Measurement of Nitrogen in Solid and Liquid Samples Base Line (%) ‘When the base line becomes extreme during the data processing, the Start of the following measurement is blocked. ‘The thresh hold of extremity, the percentage of the NO range + signal level of the starting point, it set by this parameter. Interval End (sec) ‘This interval time is a timer to detect the starting signal. JEthe Interval End passes and still the signal is not detected, the analysis is automatically interrupted. Temp. 1 (C) Furnace inlet temperature. Temp. 2 (C) Furnace outlet temperature. The following parameters can not be inputted here. (See ABC program.) Blank Solvent blank. Normally “07~ Ar Time After the ABC reaches to the end position, the Ar Time starts. 0, Time Time to flow the Oxygen after the Ar Time is over. Table 5-6. Analysis Parameters DescriptionsSection 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-3-6. Gas Flow Rate Setting and Gas Leakage Test TIO} Do not skip the gas leakage test. Do not use the instruments, if gas leakage is found. Do not turn the Heater on before finishing the gas leakage test. Replace the Septum every day before operating the TN-110. ‘Turn the Argon/Oxygen Gas Adjustment Knob and Oxygen Gas Adjustment Knob slowly. I Click the menu System, click Temp./Flow.... The following window is appeared. ‘This window is shown after the System Setup is successfully finished. Actual temperature of Heater 1 (Inlet) and Heater 2 (Outlet) are displayed. Process Temp. 1 800 °C Process Temp. 2 900 °C oa Tay. See 4-2-2 Rear view of the ND-100 and Actual gas flow rates of Argon/Oxygen and main Oxygen are displayed. sear: : 4-2.3 Front view of the main unit. i avoz Car 400 m/min | 02 302 min 205 Sa _ bic Pev(Gs) coe CD 6B 66 Increase gas flow. 2 open the Argon and Oxygen stop valves, Set the flow rates at “ Ar/O, : 400 + 10 ml/min” and “ O, : 300 + 10 ml/min”. “O; : 200 + 10 ml/min.” 3 Close the Argon gas stop valve. After 10 - 30 sec, the process flow rate of Ar gas shows ~ Ar: 0 - 10 ml/min” and “ O, : 300 + 10 ml/min”. pen the Argon gas stop valve, Close the Oxygen gas stop valve. After 10 -30 see, the process flow rate of Ar gas shows “ Ar: 400 + 10 ml/min ” and “ QO, : 0-10 ml/min”. 5 Open the both Argon and Oxygen gas stop valves. After 10 - 30 sec, the process flow rates are “ Ar: 400 + 10 ml/min ” and “ O, : 300 + 10 ml/min”. 516Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 6 In this conditions, connect the optional flow meter or commercially available one to the end of the Pyrolysis Tube and confirm the scale “660 + 50 ml/min” by Argon scale. 7 If there is a gas leakage, check the following points by using a soap water. Do not proceed to the next step after the gas leakage test is successfully finished. Please contact the local agent if gas leakage symptom still remains, Septum and Septum Holder ‘O-Ring (P-16) and Screw for Sample Inlet Port Septum and Septum Holder Packing / Glass Plate for Sample Inlet Port Argon Gas Inlet Connector Oxygen Gas Inlet Connector oO Pyrolysis Tube see eee Packing / Glass Plate for Sample Inlet Port O-Ring (P-16) and Sefew for Sample Inlet Port Oxygen Gas Inlet Connector Argon Gas Inlet Connector Pyrolysis Tube SeT‘Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-3-7. Heater ON Click this icon 34 or click the menu System, click Heater.... The following window is, appeared. Make sure the setting values ( Normally T1: 800 °C/T2 : 900 °C). Setting Temp (T1, T2) are displayed. Ti: Heater 1 (Inlet) 2: Heater 2 ( Outlet ) Confirm the setting values. 5-3-8. Ozone Generator ON ‘Tum the Power Switch of Ozonizer ON. Click this icon él or click the menu System, click Ozonizer.... The following window is appeared. Check “On” and press “OK” button. Pump starts up at the same time. ike eben ation 5-10. Ozone Generator (Ozonizer) ON It would take the Ozonizer to be stabilized about 30 minutes. SBSeation 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-4. Pre-baking of the Sample Boat CAUTION Even if a new sample boat is used, the sample boat might be contaminated. Always pre-bake the sample boat before analyzing blanks, standard samples and samples. Disconnect the Female Ball Joint before performing the boat pre-baking. Once a sample boat has been pre-baked, do not touch it with dirty tweezers or bare hands. | Always use 2 or 3 sample boats for pre-baking and keep the clean sample boats at the glass petri dish, J Giick tis icon 3 or click the menu Run, click Boat Prebake. Input the “Repeat times”, 2 Recommended numbers for boat prebaking are “2”. Type “2” and press “Next” to proceed. Illustration 5-11. Menu “Boat Prebake” 3 The following window is appeared. ustration 5-12, Menu “Boat Prebake” s19Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 4 Press “OK" to start the boat prebaking. Iustration 5-14 is displayed. When referring to ABC program, click the ABC Program button. The following display is indicated. (Illustration 5-13) Ilustration 5-13. ABC Program “Boat Pre-baking” Press this button to edit the ABC program. (No usual edit ) ‘When clicking Cancel, illustration 5-13 retum to illustration 5-12. 5.20Section 5 : Measurement of Nittogen in Solid and Liquid Samples J After Pressing the OK button, the TN-110 System Program status screen is changed. The Start button starts flickering, Without clicking Accessory button, Accessory-ABC isn’t displayed. Make sure the ABC Program No. and] | [parameters. E 4 Process Temp. 1 800 °C le F] PwocessTemp.2 900 °c Le After the both temperatures reach to the setting values, go on to the next step. 521Section $ : Measurement of Nitrogen in Solid and Liquid Samples 6 open the cover of the Sample Inlet Port, and fix the Sample Boat to the Ladie with clean tweezers. Close the cover and lock the key. Press start to proceed. a [Fill up a small amount of the |Quartz Woo! into the Sample [Boat ‘Dlustration 5-16, Setting the Sample Boat to the Ladle 5.22Section 5 : Measurement of Nitrogen in Solid and Liquid Semples 7 Bout Pre-baking i in process. ABC runs the program. After the sample boat reached to the End position, Ar Time (30 seconds) starts. The Ar gas will automatically switch to Oxygen gas after the Ar Time is finished. ABC stays at the End Position for 330 seconds to burn the sample boat in the flow of Oxygen atmosphere. ABC will move to the Cool Position and stay 60 seconds for cooling the sample boat. The whole routine of the ABC program is completed when the Cool Time (60 seconds) is finished. Steam cot Te 20 o eo Oo 60 le . — SED - a ee Zo = BSS Mlustration 5-17. “Boat Pre-baking” is in Process The second run will be automatically started, 9 The Start button stats flickering again. Take out the clean sample boat and set the next boat. Press start to continue, 10 When you finished the Boat Pre-baking, press b= button to exit 5.23Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-5. Measurement of Standard Sample 5-5-1. Measurement of Standard Sample | Do not operate the unit if gas leakage is found. If gas leakage is found, repair the leaking part, and check again for gas Teakage before operating the TN-110. Never start analysis until the base line [NO value] is becoming stable. Bla ule I cick the shorteat icon Fi or click the menu System, click Temp./Flow.... The following window is appeared. Confirm that Argon/O2 gas and main Oxygen gas are properly set. “ Ar/O, : 400 + 10 ml/min and “ O, : 300 + 10 ml/min” * 03: 200 + 10 ml/min”. Connect the Female Ball Joint to the end of the Pyrolysis Tube. (See Section 3-4 Process Temp. 1 Process Ternp. 2 lustration 5-18. Confirmation of the Gas Flow 2 cick this icon EY. or cick the Menu File, click New Method, ‘Iilustration 5-19. Menu “File” “New Method” 5.24Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 3 The following window is appeared, Confirm the Accessory : ABC and Mode : TN Input the Method Name and click OK. New Mothod Select the Accessory which is |! actually connected to, | Do not choose a wrong Accessory, Select TN. ‘Type the Method Name here. Ilustration 5-20, “New Method” Window 5.25Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 4 The new Method “STD” is opened. Select the “Calibration” as Target and type “Concentration” and “Injection Std. Volume”. Select the “ABC Program”. Press “Add” button to specify the numbers of run. Select the “ABC Program”. Select “Calibration” as| Target. = Type “Concentration” and “Std, Volume” Sa ‘Tustration 5-21. “New Method Entry” Window Recommended ABC Program for Standard Sample (Heater 1: 800 °C / Heater 2 : 900°C ) 1" Position 280-85 mm 1* Position Time : 10 - 60 sec 2™ Position 105-125 mm CAUTION 2" Position Time : 30 - 60 sec 3" Position 125 - 160 mm 3™ Position Time : 30 - 60 sec Depending on the furnace temperature, the ABC Program and Parameters must be changed, The typical recommended values are listed. End Time 2 100 - 180 sec Cool Time £30 - 60 secs Boat Speed : 20 mm/sec Ar Time 230 sec O, Time 7300 - 600 sec Home Cool Time : 120 sec (Set in Preference Acc. of system.) 5-26Section $ : Measurement of Nitrogen in Solid and Liquid Samples 5 Afr all necessary items are inputted, confirm the numbers and press “ Run Method ” button, Items Descriptions | 78PYt 7 ait Range Concentration tag7T Zbendard Semple 0 - 9999.99 | [ug/ml Concentration toed Std. Volume Std. Sample 0 - 999.9 Cw Li [mg) injection volume Mass Witrogen Tal Concentration {Theoretical value Sample Size Sample size 0.01 - (21) fmg] 9999.99 {mij [gl Density Density 0.0001 - 9.999 Sample Date Sampling Date Sample Weighed | Sample weight 0-001 = imi} tail 999.9999 [g]_tmgl Total solvent 0.1 - 9999.9 | [mi] Total Solvent volume when the sample is diluted. Dilation Rate Dilution ratio ‘Table 5-7. Method Entry Values a7Section $ : Measurement of Nitrogen in Solid and Liquid Samples 6 The following window is shown. Type the Data ID. The Data ID is a unique key ID for saving all data to the Database. The TN-110 System program will show you a example Data ID (Year/ Month /Date.001). Type the data ID you want touse. The Data ID is very important when you query the results from the database. CAUTION Never press the “Run” button, if Ar/O, and > gas are not supplied. The Error “O; GAS FLOW ERROR”(086) or “ArlO, GAS FLOW ERROR"(087) may be shown and the system may shut down. In one Data ID, the following contents are kept. © Measurement condition (Heater, Temps, Gas, Flows, Accessories, ete.) @ Blank, Calibration & Sample Results. ‘When using the same method and separating the Data ID, the separate average and RSD% are calculated. About the same sample ID in the same Data ID, average and RSD% of all the data are calculated. In addition, plural methods are the same Data ID, and printing can complete once. 5.28Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 7 The Start button starts fickering, The Sample Boat must be pre-baked. (See Section 5-5. Pre-baking of the Sample Boat ) Inject 10 0 ul of the Standard ‘Sample slowly into the Sample Boat. When the Micro-syringe is pilled out, touch the needle tip to the inner wall of the Sample Boat so that no standard sample remains on the tip. When injection is finished, click the Start button, CAUTE [Never operate the unit, if the gas leakage is found. Do not inject more than 50 w | organic sample. 5.29Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 8& Analysis starts. The analysis proceeds and the measurement ends automatically. ‘The buzzer ( Beep 1 Times ) sounds, and the Rep 1/3 is completed. The Start button starts flickering again when the base line goes down to a certain level. The Sample Boat must be sufficiently cooled before proceedin; Continue the routine according to the instructions. Wait until the potential becomes stable, Sampling 50.0 Tlustration 5-23. Status Screen “Run Method, Status : Sampling” 330Section $ : Measurement of Nitrogen in Solid and Liquid Samples QNow, Reps 1/3, 2/3, 3/3 are finished. By clicking th results of 3 runs. Process Temp. 1 Process Temp. 2 894 °C 398 mldmin 297 enldmin 200 mifmin a 5287424 5035761 4898391 Sapa cases Sod Illustration 5-24. Status Screen “Run Method, Status : Busy” abbr 132-| Calibratior! Illustration 5-25, “Results” Window 531Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-5-2, Measurement of Standard Sample [Show / Edit Results] I ciick the menu Results, click Calibration. oi ‘Ilustration 5-26. Menu “Results” “Calibration” 2 The following window is shown. If you sec a bad result, select the result to edit. ‘Add : Add data by key input. Delete : Delete results. No Used __: The selected result is not used for calculation. But, the data is stored in the Database. If the calibration curve is good enough, click OK to save the results into the Database. Calibration data are kept per Sens Accessory. When changing “Sens” of Analysis Parameter, calibrate again or input in Key In. ‘The values inputted by operator are marked with “k”. 532Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 3 When you finished the Measurement of Standard ‘Sample, Press exit By pressing the Exit button, 5-5-3 operation can’t be done, so be careful. 5-5-3. Go Back to the Previous Run / Go to the Next Run The TN-110 System program is allowed to retty the run or skip the run by using the Back Next button. <3 Go to the next run. Go back to the previous run. 533‘Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-5-4. Measurement of Standard Sample [Add / Delete / Edit Functions] The TN-110 System Program is allowed to add / delete runs in the middle of the measurement. This section covers the procedures for adding / deleting runs into the Method. J click the = button. The Results Table window is shown. 2 Click the Open Method button. Mlustration 5-28. “Results” “Open Method” 3 the Method Window is shown. (See Illustration 5-21.) In this window, you can ; ‘Add Runs, Delete Runs, Copy Runs and Delete All Runs. ‘Also, changing the ABC Program is possible. By clicking the “Run Method” to update the measurement orders. 534Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-6. Measurement of Sample 5-6-1. Measurement of Sample [Run Method] Do not operate the unit if gas is leaking, If gas leakage is found, repair the leaking part, and check again for gas leakage before operating the TN-110. 1 ciictc this icon CY or ctck the Menu Fite and New Method. 2 The following window is appeared. Confirm the Accessory : ABC and Mode : TN, Input the Method Name and click OK. Ilustration 5-30. “New Method” Window 535Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 3 ‘he new Method “SAMPLE ABC” is opened. Select the Target “Sample” and input all items, Select the “ABC Program”, If necessary, create your own ABC Program for each sample. Press “Add” button to specify the numbers of run. Select the “ABC Program”. | “Type “Sample 1D” or select. [Sample [Sample [SAMPLE a-O1 eee SAMPLE FO odour oO [2 |Samcie—|SanPLE A ‘o.00ur [1.0000 =]5_ [sample —_[saneLqA) 0,00 ut [7.0000] “Type “Sample Size” and “Density”. |: ___| Ifthe sample is diluted, input the 2 | numbers here. Ilustration 5-31. “New Method Entry” Window ‘When registering the date of sampling, input. The data of measurement is automatically registered. ‘© The ABC Programs listed are typical examples. Depending on the conditions of the furnace temperatures, the ABC Parameters and must be 536Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 4 Click Run Method. 5 The foliowing window is show, Type the Data ID. The Data ID is a ‘unique key ID for saving all data to the Database. The TN-110 System program will show you a example Data ID (Year / Month / Date. 001). Type the Data ID. ‘The Data ID is very important when you query the results from the database. 99/05/06 15:56 Sie ‘Ilustration 5-33, “Data ID Entry’ CAUTION Never press the “Run” button, if Ar/O, and > gas are not supplied. The Error “O, GAS FLOW ERROR(086) or “Ar/O, GAS FLOW ERROR(087) may be shown and the system may shut down, OTE Data ID In one Data ID, the following contents are kept. © Measurement condition (Heater, Temps, Gas, Flows, Accessories, etc.) @ Sample results ‘When using the same method and separating the Data ID, the separate average and RSD% are calculated. About the same sample ID in the same Data ID, average and RSD% of all the data are calculated. Inaddition, plural methods are the same Data ID, and printing can complete once. 537‘Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 6 ‘the Start button starts flickering. ‘The Sample Boat must be pre-baked. (See Section 5-4, Pre-baking of the Sample Boat ) Liquid Samples} 1. Inject the sample slowly into the Sample Boat. When the Micro-syringe is pilled out, touch the needle tip to the inner wall of the Sample Boat so that no standard sample remains on the tip. 2. If the injection is finished, click the Start button. [Solid Samples) 1. Put sample on the sample boat and weight by electric balance. Equal to or less than 30 mg.) 2. Open method file. (See 5-5-4.) 3. Input sample size. 4, Click Run Method button. 5. Click Close button. 6. Open the cover of the Sample Inlet Port and fix the Sample Boat with the Ladle with clean tweezers. 7. Close the cover and lock the key. 8. Click the Start button. Tes) Illustration 5-34. Status Screen “Run Method, Status : Ready” 538Section 5 : Measurement of Nitrogen in Solid and Liquid Samples Always turn the power on the ABC Cooling Unit for measuring organic samples. Be careful for an incomplete combustion. [Never open the Safety Cover of the ABC. |CAUTION [Never operate the unit, if the gas leakage is found Do not inject more than 50. Lor 30mg organic sample. 7 Analysis starts. Analysis proceeds, the potential comes up the starting potential, and the measurement ends automatically. ‘The buzzer (Beep 1 Times ) sounds, and the Reps 1/3 is completed. ‘The Start button starts flickering again when the potential goes down to a certain level. The Sample Boat must be sufficiently cooled before proceeding to the next run, Continue the routine according to the instructions. &.Now, Reps 1/3, 2/3, 3/3 are finished. By clicking the results of 3 runs, Tilustration 5-35. “Results” Window 539Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-6-2, Measurement of Sample [Show / Edit Results] I ctick the menu Results, click Sample. Mlustration 5-36. Menu “Results” “Sample” 2 The following window is shown. If you see a bad result, select the result to edit. Not Used _: The selected result is not used for calculation. But, the data is stored in the Database. Click OK to save the results into the Database. 1150500 1160369 1169873 5-40Section 5: Measurement of Nitrogen in Solid and Liquid Semples 3 When you finished the Measurement ofthe Sample, Press ‘button to exit. By pressing the Exit button, 5-6-3 operation can’t be done, so be careful. 5-6-3. Go Back to the Previous Run / Go to the Next Run ‘The TN-110 System program is allowed to retry the run or skip the run by using the Back / Next button. It is valid until clicking the Exit button. Go to the next run. Go back to the previous run. SALSection 5 : Measurement of Nitrogen in Solid and Liguid Samples 5-7. Database Report, Re-calculation & Browse Results 5-1-1. Report Choice of the Report Format I Click the menu Database, click Report, Ilustration 5-38. Menu “Database” “Report” 2 The following window is shown. ‘Two types of report formats are available in the menu “Database” “Report”. «¢ Summary Report [ Sample Average Report ] Customized Report [ Selected items can be printed out ] Select the Data ID. Click items to be marked. Press “Print” to start printing report. By clicking “Print”, the printer dialogue box is displayed and press “OK” to start printing. ‘ilustration 5-39. “Report” Window 5.42Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 3 By clicking the “Preview” button to show the following window. Tlustration 5-40. “Preview’ By clicking “Print”, the printer dialogue box is displayed and press “OK” to start printing By clicking “Cancel”, “Report” window returns. | <} With plural pages, for displaying the first page With plural pages, for displaying the front page With plural pages, for displaying the next page With plural pages, for displaying the last page For enlarging the display For shortening the display 543Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 4 When inputting Header in Summary Report, click “Edit Header” of Hlustration 5-39 “Report” window. a LU : : : a a : arSUBISH CHEMICAL CORPORATION oo REPORT i : i ~ e Mlustration 5-41. “Edit Header-Report” Window When printing comment in Summary Report, click the “Edit? button to show the following window, Even Llustration 5-42, “Edit - Comments-Report” ‘Window S84Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-7-2. Recalculation. I Click the menu Database, click Recale, ‘Ilustration 5-43. Menu “Database” “Recale” 2 The following window is shown. Click “Sample” to show you the results ofthe sample Tlustration 5-44. “Recale” Window 545Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 3 The following window is shown. Edit results here. If you wish to delete the results after, the measurement is completed, select the data and click “Delete” button. Illustration 5-45, “Sample-Recale” Window Descriptions The Area value is shown at the text box. When clicking this button, “Copy” changes to “Overwrite”. 2 Select the data and press this button to delete. ‘When you use this button, the selected data is omitted 3 just from the calculation. The data is stored in the database. * ee Click this button one more time to cancel the symbol “*”, [an] "You can add the data manually by this button. The “Add” button will be effective when and after the “copy” | K ® function is used. ‘Table. 5-8 Recale Functions 5-46Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 4 “Detsis-Recale” i displayed by clicking “Details” button of Mustration 5-45. “Sample-Recalc” Window. Gray items are unchangeable. Input items to be corrected. Click OK to show Illustration 5-45, “Sample-Recale” Window. = Illustration 5-46. “Details-Recale” J Click OK in Ihustration 5-45 “Sample-Recalc” Window. R is automatically added into the front of Data ID when the re-calculation is done. j i — 5-47Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 5-7-3. Browse Results I Ciick the menu Database, click Browse Results. on ‘Slustration 5-48. Menu “Database” “ Browse Results” 2 ‘he following window is shown. raasar pan) Illustration 5-49. “Browse Results” 5-48Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 3 Select Title “Main” or “Sub” or “Date” and input the arbitrary browse conditions. Illustration 5-50. “Inputting browse conditions”Section 5 : Measurement of Nitrogen in Solid and Liquid Samples 4 Ctick DB Query Run. The Results are shown. Click the Parameter, Blank, Calibration, ‘Sample, L-ASC Spike. Not inputting the retrieval conditions, all results are displayed. Illustration 5-51. “ Result Display” 5-50Section 5 : Measurement of Nitrogen in Solid and Liquid Semples 5-8. Heater Off & Stopping the ND-100 & TN-110 I Click this icon @ilor click the Menu System, click Heater.... Check “Off? and press “OK”. Turn the heater off. Illustration 5-52. “Heater On/Off” Window 2 Click this icon Zor click the Menu System, click Ozonizer.... Check “Off” and press “OK”. Ozonizer turns to Off. After three minutes, the pump stops. 3 Tum the Heater Switch (ND-100 Main Unit Front Panel) OFF. 4 Turn the Ozonizer Switeh (TN-110 Unit Front Panel) OFF. J Click the menu File, click Exit. “Are you sure you want to exit TN-110 System?” Click OK. Illustration 5-53. Menu “File” “Exit” S51Section 5S : Measurement of Nitrogen in Solid and Liquid Samples 6 Tum the Power Switch of : ND-100 : OFF ABC Cooling Unit : OFF Personal Computer : OFF Printer (If connected.) : OFF 7 After forty minutes of heater-off (when the Furnace temp is lower than 300°C), switch OFF the TN-110 Main Unit. 8 Close the main valves of the gas cylinders. 9 Confirm the Vacuum Pump[GLS-050] power is turned to OFF.Section 6 : Maintenance ction 6 : Maintenance This section tells you procedures for the maintenance of the TN-110. 6-1. Daily Maintenance Table 6-1. shows the procedures for daily maintenance. Items How Often ? © Replacement of the septum. * Everyday [Septum : P/N: TNSSIS] ‘Table 6-1. Everyday Maintenance eI6-2. Regular Maintenance Table 6-2. shows the procedures for regular maintenance. Seotion 6 : Maintenance [Outer Pyrolysis Tube : P/N: TX3QPG] [Inner Pyrolysis Tube : P/N : TX3QPN] Items How Often ? ‘* Transparency check of the Pyrolysis Tube. |* Every 2 Weeks Quartz, Wool : PIN : TNOWL] Replacement of the Quartz, Wool. ° Every 2-3 Weeks re-generation of the Catalyst. [Catalyst, 7g : P/N : TNSCAT] © Replacement of the Catalyst or ° When the conversion performance becomes inferior. Joint. [Female Ball Joint : P/N : TNSLJT] © Replacement or cleaning of the Female Ball | + Every 3-4 Weeks. [Fluororubber Joint Tube : P/N : TNSJTF] __ ¢ Replacement of the Flurorubber Joint Tube. | + Every 2-3 Weeks [Disposable Filter : P/N : TS6ND1] © Replacement of the Disposable Filter. . Every 3-4 Weeks. Every 6 Months, Every 600 Hours. [Vacuum Pump Scrubber : P/N : TNSVPR] ‘© Replacement of the Vacuum Pump Oil. | [Vacuum Pump Oil : P/N : TNSVPF] © Replacement of the Ozone Scrubber. . [Ozone Scrubber : P/N : TN6RPZ] ‘Replacement of the Vacuum Pump . Scrubber. Every 600 Hours. ‘Table 6-2. Regular Maintenance 62Section 6 : Maintenance 6-2-1, Replacement of the Ozone Scrubber The contents of the Ozone Scrubber should be replaced every 600 hours in the following way: 1) Remove the scrubber column from the ND-100 Unit when it is not under operation. 2) Attach the new scrubber in the same manner that the old one was attached. 3) Fill the new date in the label for the Ozone Scrubber replacement date. 6-2-2. Replacement of the Vacuum Pump Oil [CAUTION] DO NOT use the oil which is not recommended by MCC. When the TN-110 is used about 8 hours/day. replace the oil every 6 months. ‘When the TN-110 is used 24 hours/day, replace the oil every 3. months. 1) Remove the Ozone Scrubber from the ND-100 Optional Unit when itis not under operation, 2) Prepare the empty vessel to receive the used oil. 3) Drain the oil from the Vacuum Pump by removing the drain plug. 4) Screw in the drain plug manually as it was. After this, fasten the screw by another half rotation with a wrench, 5) Feed the new oil through the scrubber hole using a funnel. Check the oil is in the middle of oil level gauge. (in the middle of maximum line and minimum line) ©) Perform a trial operation of the pump and check the oil level again. At this moment, if the level has changed lower, add the oil. 7) Connect the scrubber as it used to be. 63Section 6 : Maintenance 6-2-3. Replacement of the Activated Carbon and the Ceramic Wool in the Vacuum Pump Scrubber The scrubber is used to absorb an oil mist in the vent gas and| an odor. Replace the activated carbon and the ceramic wool in the following way. 1) Detach the scrubber from the vacuum pump using a wrench. 2) Remove the used activated carbon and the ceramic wool in the vent cap. 3) Remove the used ceramic wool both ftom the main tube and from the bottom tube. 4) Wash the vent cap, the main tube and the bottom tube, with detergent and dry it naturally. 5) Cat off the ceramic wool. 6) Put the larger piece of the ceramic wool into the larger cylinder of the main tube by rolling it cylindrically. 7) Connect the main tube with the bottom tube. 8) Put a small piece of ceramic wool at the bottom of the shorter cylinder of the main tube. 9) Pack 100ml (60g) of the activated carbon on the ceramic wool. 10) Put two small pieces of ceramic wool on the above activated carbon. 11) Cover the shorter cylinder with the vent cap. 12) Install the whole scrubber to the vacuum pump, at first manually then using a wrench. 64Section 6 : Maintenance 6-2-4. Maintenance of the catalyst When the NO value on the display is not stable, replace the quartz wool: ‘When the NO value is still unstable, recondition the catalyst in the following procedure: 1) Remove the catalyst from the combustion tube. 2) Wash the catalyst in distilled water stirring with a glass rod, 3) Dry it naturally. 4) Pack the catalyst in the combustion tube. DO NOT connect the female ball joint to the combustion tube, 5) Install the combustion tube in the TN-110 Main Unit. 6) Raise the furnace temperature flowing gases as the same condition as a sample measurement for a few hours. 6-2-5. Replacement of the catalyst When the NO value can not be stabilized even after the reconditioning of the catalyst, replace the catalyst in the following procedures: 1) Pack the new catalyst in the combustion tube, DO NOT connect the female ball joint to the combustion tube. 2) Set the furnace temperatures T1: 800 °C T2: 900°C. 3) Flow Oxygen gas [Ar/O2 =O; : 500 ml/min and O; : 300 ml/min]. 4) Under the above conditions, keep conditioning for five hours. 65Section 6 : Maintenance 66Section 7 : Troubleshooting n 7 : Troubleshootin, This section is a guide for correcting problems which may be arisen while operating the TN-110. 7-1. Electrical & Mechanical Troubleshooting 1. If the power of the Main Unit is not switched on. REFER TO THE FOLLOWING INSTRUCTIONS. Q) A POWER CABLE IS NOT CONNECTED. A) CONNECT THE POWER CABLE. Q) THE MAIN POWER IS OFF POSITION. A) SEE Illustration 7-1. AND TURN THE MAIN POWER TO ON. Q) TN-110 VOLTAGE SETTING DIAL IS NOT CORRECTLY SET. A) SEE TN-110 INSTRUCTION MANUAL SECTION 3-1-2. AND SET THE DIAL CORRESPONDING TO THE POWER SUPPLY. Q) THE FUSE OF THE MAIN UNIT IS BURNT OUT. A) TAKE OUT THE FUSE AND CHECK IT WITH A TESTER. IF BROKEN, REPLACE IT. PLEASE CONTACT THE LOCAL AGENT, IF THE SYMPTOM STILL REMAINS AETER CHECKING THE ABOVE ITEMS. Mlustration 7-1. Back View of the TN-110 Main Unit rHSection 7 : Troubleshooting 2. If the electric furnace does not heat up. (TN-110 Main Unit) REFER TO THE FOLLOWING INSTRUCTIONS. Q) THE HEATER SW OF THE FRONT PANEL IS OFF POSITION. A) TURN THE SW ON. Q) THE THERMAL FUSE 91°C IS BROKEN. A) PLEASE CONTACT THE LOCAL AGENT. Q) FURNACE COIL IS BURNT OUT. A) PLEASE CONTACT THE LOCAL AGENT. Q) SYSTEM SETUP IS NOT PROPERLY DONE. A) START FROM THE “SYSTEM SETUP”. Q) THE THERMOCOUPLE IS BROKEN / ERROR(62). A) IF YOU SEE THE ERROR MESSAGE 62 : THEMOCOUPLE OFF ERROR, PLEASE CONTACT THE LOCAL AGENT. PLEASE CONTACT THE LOCAL AGENT, IF THE SYMPTOM STILL REMAINS, AFTER CHECKING THE ABOVE ITEMS. 3. If the solenoid valve roars. The solenoid valve roars when the Argon/ Oxygen gas is turned over. REFER TO THE FOLLOWING INSTRUCTIONS. A) THE SECONDARY PRESSURES OF ARGON AND OXYGEN ARE DIFFERENT. ADJUST THEM TO THE SAME PRESSURE FROM 290 TO 490 kPa, (3 ~ 5 kg/cm’ ) A) FOREIGN SUBSTANCES ARE INCLUDED IN THE VALVE. INCREASE A GAS FLOW RATE, AND TURN OVER THE GAS TO OXYGEN AND TO ARGON SEVERAL TIMES. Q) THE SOLENOID VALVE IS BROKEN. A) PLEASE CONTACT THE LOCAL AGENT. PLEASE CONTACT THE LOCAL AGENT, IF THE SYMPTOM STILL REMAINS AETER CHECKING THE ABOVE ITEMS. 1aSection 7 : Troubleshooting 4. If the process value of the gas flow rate is different from the actual value or the process value shows 0 ml/min. REFER TO THE FOLLOWING INSTRUCTIONS. Q) GAS LEAKAGE MAY BE HAPPENED, A) REFER TO THE SECTION 5-3-6. GAS LEAKAGE TEST. Q) SYSTEM SETUP IS NOT PROPERLY DONE. A) START FROM THE “SYSTEM SETUP”. (5-3-4) Q) THE MASS FLOW SENSOR IS BROKEN, A) PLEASE CONTACT THE LOCAL AGENT. ZASE CONTAI LOCAL AI IF THE SYM] STILL REMAINS AFTER CHECKING THE ABOVE ITEMS. 5. If the process value of the gas flow rate shows positive values when Argon / Oxygen gas are not supplied. REFER TO THE FOLLOWING INSTRUCTIONS. A) THE ZERO SETTING DIAL OF THE MASS FLOW SENSOR IS NOT. ADJUSTED CORRECTLY. THERE ARE TWO DIALS IN THE BACK OF THE MAIN UNIT AND THESE DIALS ARE SET TO “0” AT THE FACTORY SETTING. WARNING ‘DO NOT ATTEMPT TO ADJUST DIALS YOURSELF. CONTACT THE [LOCAL AGENT FOR FURTHER SERVICING. If this product does not operate as described when the detailed operating instructions are followed, do not attempt to open or remove covers or make any adjustments not described in the manual. Attempting to service this unit yourself may expose you to dangerous voltage or other hazards and will void warranty. Refer all servicing to qualified service personnel, 13Section 7 : Troubleshooting ‘ZERO SETTING DIALS FOR ARGON / OXYGEN MASS FLOW SENSORS. Mlustration 7-2, Ar/Oz Gas Mass Flow Sensor Zero Dials, 1ASection 7 : Troubleshooting 7-2. Analytical Troubleshooting 1, Analysis time is too long. REFER TO THE FOLLOWING INSTRUCTIONS. INO Value is stable?] Q) NO Value on the display is stable? A) Cheek the combustion tube. Catalyst and the quartz wool are recommended to be changed. INo Gas leakage?] Q) Have you checked the gas leakage test? ‘A) Refer to the Section 5-3-6 and confirm the gas leakage. [Female Ball Joint is connected?] Q) Have you connected the Female Ball Joint? A) Refer to the Section 3-4 and confirm the connection. PLEASE CONTACT THE LOCAL AGENT, IF THE SYMPTOM STILL REMAINS AFTER CHECKING THE ABOVE ITEMS. [No Contamination? SAMPLE INLET PORT PYROLYSIS TUBE SAMPLE BOAT DISPOSABLE FILTER (Internal filter) CLEAN THEM IN THE FOLLOWING MANNER. «SAMPLE INLET PORT (SEE ILLUSTRATION 7-3.) After cooling down the fumace and also after stopping the gas supply, clean the inside of the Sample Inlet Port carefully with gauze containing acetone.Section 7 : Troubleshooting. * PYROLYSIS TUBE (SEE ILLUSTRATION 7-4.) Take out the Pyrolysis Tube after sufficiently cooled. + Contamination with organic samples Wipe the inside with gauze containing acetone. * Contamination with inorganic samples. Remove it by burning with a bumer etc, Clean carefully inside tube with a brush and a natural detergent, wash away the detergent with distilled water. Then pack the quartz wool. Alustration 7-4. Cleaning of the Pyrolysis Tube SAMPLE BOAT (SEE ILLUSTRATION 7-5.) Take out the Sample Boat after sufficiently cooled. Contamination Clean it carefully with a brush and a natural detergent with distilled water and dry the boat. Illustration 7-5. Cleaning of the Sample Boat 2. If the result is unstable. REFER TO THE FOLLOWING INSTRUCTIONS. GAS LEAKAGE INCORRECT GAS FLOW SETTING INCORRECT GAS PRESUURE SETTING CONTAMINATION INCORRECT TEMPERATURE SETTING SAMPLE INJECTION VOLUME IS NOT PROPER 16‘Appendix A : CONSUMABLE SPARE PARTS LIST. APPENDIX A : CONSUMABLE SPARE TS LI Appendix A covers consumable spare parts and maintenance spare parts for the TN-110 system, A-1. ND-100 Spare Parts ‘Table A-1. shows the TN-110 Main Unit spare Description Part Sales | Numbers for 2 Number _| Quantity | Years Operation 1. Outer Pyrolysis Tube TX3QPG |__I pe Apes 2. Inner Pyrolysis Tube TX3QPN | pe 4 pes 3. Spring for Pyrolysis Tube SX1QSP | 4 pes/set 4 sets 4. Female Ball Joint for Combustion Tube__| TNSLIT | I po 4 pes: 5. Fluororubber Joint Tube TNSITF |__Ipc 4 pes 6.Clip, P18 TXOI7 | Zpchet 2 sets 7. Fluororesin Tube (3%2 mma) Im ‘TNSFTS | Ipc 4 pes 8. Ozone Scrubber TNORPZ | 1 pe 2 pes 9. Microsyringe, 1705-N, 301 MSi705 [Ipc 2 pes 10. Disposable Filter (PTFE) TSONDI_| 5 pes/set 4 sets 11, Disposable Filter Fitting TS6ND?2 | 10 pes/set 2 sets 12. T type Union TX3PPU |_| pe 2 pes 13. Catalyst TNSCAT |__1po I pe Table A-L. ND-100 Spare Parts A-2, Vacuum Pump Spare Parts ‘Table A-2. shows the Vacuum Pump spare parts. Deseription Part Sales | Numbers for 2 Years Number | Quantity Operation 1, Vacuum Pump Oil (Demunum $-20) INSVGF | 1 bil 2btls 2. Vacuum Pump Scrubber INSVPR [Ipc ‘4 pes 3. Vacuum Pump Suction Tube 10m ‘TNSVPT. pe 2 pes 4. Activated Carbon for Vacuum Pump ‘INSVPC | _ 1 bag 4 bags Scrubber ‘5. Hose Clamp for Vacuum Pump Scrubber_| TNSHB9 | 11 pesisct Tset ‘Table A-2. Vacuum Pump Spare Parts“Appendix A : CONSUMABLE SPARE PARTS LIST A-3. TN-110 Main Unit Spare Parts ‘Table A-3. shows the TN-110 spare parts. Part Sales] Numbers for Description Number | Quantity | 2 Years Operation 1. O-ring, P16 ‘Tx020__[ SPCSISET | 3SETS 2. PTRE Tubing, 4/2 mm, 10M TX3RPP [_1PC 3PCS 3. Ar Gas Inlet Connector / 30-6RUE4-SP Tx2BiL [| _1PC 3PCS 4, Oy Gas Inlet Connector /30-6RU4-SP. INDITG |_2PC 3 PCS 5. Thermal Insulator (Right) TX3RHP [1 PC 1PC 6. Thermal Insulator (Left) IN3REP [1 PC 1PC 7, Furnace Insulating Ring TX3RPR [_1PC 2PCS 8, Optional Accessory Fixing Plate TX3RKK |__1PC — 9. Thermocouple ‘Tx3rHc [1 PC 2 PCS 10. Thermal Fuse, 93 °C FU93TR [__1PC 2PCS 1. Flow Meter For TOX-100"1 TX3RPF |__1PC PC] 12. RS232C Cable 9-Pin Cross Type ‘CBRS23 |__1PC — 13. Fuse, 3.15A or2 A FU3iMS | 2PCS/SET | 2SETS /FU02MS 14, Quartz Wool, 10g TNQWL |_{BAG | 5 BAGS 15. Quartz Wool Poker #1 TX2RTL | __1PC [PC] Table A-3. TN-110 Main Unit Spare Parts List *1: RECOMMENDED ITEM FOR MAINTENANCE PURPOSE. Numbers for 2-vear operation are recommended numbers from manufacturer.‘Appendix A : CONSUMABLE SPARE PARTS LIST A-4. ABC Spare Parts ‘Table A-4, shows the ABC spare parts. | Description Part Sales Numbers Number | Quantity | for 2 Years Operation 1. ABC Fixing Plate TSRKB] 1 pC — 2, ABC Signal Cable TxCBB | 1PC = 3. Guide Tube TXIRTG |___1PC 3PCS 4, Pushrod (Ladle) TXIRDL |___1PC 4PCS 3. Magnet TX2RTM| __1PC 2 PCs 6. Sample Boat Tx2SBr_| SPCSISET | 10 SETS [7. Septum Holder ‘TX3SED | 10PCS/SET | 10 SETS | 8, Septum (Flat-type) INSSIS | 100PCS/SET | _10 SETS 9. Packing For Sample Inlet Port TXPKG 1PC SPCS 10. Glass Plate For Sample Inlet Port "TX3BSI 1PC 2PCS 11. Packing For Sample Injection Port TN10SP_ | 4PCSISET |__4 PCS 12. Screw For Sample Inlet Port ‘TX3BOF |__1PC 2PCs 13, Fuse, 2A FUO2MS | 2PCS/SET | _3PCS Table A-4. ABC Spare Parts List‘Appendix A : CONSUMABLE SPARE PARTS LIST‘Appendix B: TN-110 ERROR MESSAGES APPENDIX B: TN-110 ERROR MESSAGES ‘DESCRIPTIONS AND REMEDY }ERROR (056) 50 [OPTION SETUP ERROR (050) Incomplete option setup Click “System™ then click “System Setup” and set a proper option. 51 [MODE SETUP ERROR (051) Incomplete mode setting. Click “System” then click “System Setup” and set a proper mode, 35 |; CHANGE ERROR (055) ‘Impossible to change gas flow to Oxygen, if the connected option is not in home position. 36 Impossible to change Analysis Parameters during analysis. 37 ;ALANCE PARAMETERS ERROR fron PARAMETERS CHANGE| 1(057) [THERMOSTAT ON ERROR (061) False balance parameters, Click “System” then click “System Setup” and set a proper balance. Immediately turn off the TN-110 System. Furnace bay temp. rose suddenly. Please contact the local agent. 62 63 64 5 |THERMOCOUPLE OFF ERROR (062) JOVER TEMP. 1 ERROR (063) jovER ‘TEMP. 2 ERROR (064) [UNDER TEMP. 1 ERROR (065) | ‘Immediately tum off the TN-110 System, ‘Thermocouple was down, Please contact the local agent. Immediately tum off the TN-110 System, Heater temp. 1 exceeded more than 50 degrees from the setting value, ‘TN-L10 automatically stopped controlling. Please contact the local agent, Immediately tum off the TN-110 System. Heater temp. 2 exceeded more than 50 degrees from the setting value. ‘TN-110 automatically stopped controlling. Please contact the local agent. Immediately turn off the TN-110 System. Heater temp. | fell down more than 50 degrees from the setting value, Heater temp. 2 fell down more than 50 degrees from“Appendix B: TN-110 ERROR MESSAGES the setting value. 10 automatically stopped controlling. Please contact the local agent.Appendix B: TN-110 ERROR MESSAGES DESCRIPTIONS AND REMEDY 67 [BALANCE SETUP ERROR (067) 69 [OVER TEMP. ERROR (069) 70 |0; CHANGE ERROR (070) Incomplete balance setting. Click “System” then click “System Setup” and set a proper balance, Titration current tumed off. Confirm the connection. (Anode, Cathode) ‘Immediately turn off the TN-110 System. Heater temp. got out of control. ‘TN-110 automatically switched off the AC power supply. Please contact the local agent, Impossibie to change gas flow from Argon to Oxygen during analysis, Retry after analysis is finished. 71 [HEATER SW OFF ERROR O71) Heater switch of TN-110 is off position. Retry after switching on, 74_|STOP ERROR (074) Impossible to press Stop button except for analysis. 75 |SETUP ERROR (075) Impossible to setup during analysis. 76 |ANALYSIS PARAMETERS SETUP | Incomplete Analysis Parameters setting, ERROR (076) Communication error occurred. Retry from the System Setup. [COMMUNICATION ERROR (077) Immediately turn off the TN-110 System. 77 80 [RAM CHECK ERROR (080) Immediately tum off the TN-110 System. RAM check error occurred. TN-110 automatically exited the program, Please contact the local agent.Appendix B: TN-110 ERROR MESSAGES ‘DESCRIPTIONS AND REMEDY lO, GAS FLOW ERROR (081) Possible for explosion. Stay out of the TN-110 system. TN-110 automatically initialized the connected option and exited the program. Please contact the local agent. 82 |AR/O; GAS FLOW ERROR (082) | Possible for explosion. Stay out of the TN-110 system. ‘TN-110 automatically initialized the connected option and exited the program. Please contact the local agent. $3 [HEATER SW OFF ERROR (083) ‘Heater switch of TN-110 tumed off. 84 [0, CHANGE SW ERROR (084) ‘Impossible to change gas flow from Argon to ‘Oxygen during the connected option is running. 85 [HEATER OFF ERROR (085) ‘Immediately tum off the TN-110 System. Furnace bay temp. rose suddenly. Please contact the local agent. 86 | 0: GAS FLOW ERROR (086) Confirm the input pressure. 87 |AR/O; GAS FLOW ERROR (087) Failure in H/W test. 90 |H/W TEST ERROR (090) Retry from the menu “System” “System Setup”, ‘91 [B/W TEST P-FILE ERROR (091) _ | Impossible to send analysis parameters during H/W test. ‘92 |A/W TEST GATE OPENERROR | Gate is closed during H/W test. \co92) 93 [BOAT PREBAKE ERROR (093) Impossible to nin Boat prebake during the Test Titration. 94 [MODE SETTING ERROR (094) (Confirm the mode setting. 95 [OXYGEN GASSWITCHERROR | O; ON error. (095) 96 [ARGON GAS SWITCH ERROR (096) mn ON exror. 97 [COMMAND ERROR (097) Confirm the cable setting. 8 [BOAT HOME ERROR (098) Impossible to send analysis parameters durin,Appendix B: TN-110 ERROR MESSAGES [HAW test. Boat home error.Appendix B: TN-110 ERROR MESSAGES INO. ‘DESCRIPTIONS AND REMEDY 101 |CABLE CONNECTION ERROR (101) Signal cable between TN-110 and ABC is not, 105 |COVER OPEN ERRROR (105) connected. Confirm the cable connection and restart the system. ‘ABC safety cover is being opened. Close the safety cover and retry. 150 SENSOR ERROR (150) ‘Sensors or motor may be out of order. Tum off the power and retry. Please contact the local agent if the system is still wrong. 151 ERROR (151) Invalid parameters setting, Confirm the ABC parameters are properly inputted, 1 |CABLE CONNECTION ERROR (601) TTN-110 automatically stopped controlling. Please contact the local agent. 602 |OZONE GENARATOR GAS ‘Oxygen gas supply to the Ozonizer is below IFLOW ERROR (602) 100mV/min, TIN-110 System Program automatically shuts down the power to the ozonizer. 605 [PMT VF OVERFLOW Confirm the analysis parameter “SENS” and [ERROR (605) injection volume, concentration. 608 [OZONE GENARATOR POWER Ozonizer switch is OFF position. |SWITCH OFF ERROR (608) 632 |OZONE GENARATOR HIGH ‘Thermal fuse on the Ozonizer may be broken. [TEMP ERROR (632) 634 INO SENSOR HIGH TEMP Thermal fuse on the NO Sensor may be broken. JERROR (634) 652 [OZONE GENARATOR GAS FLOW | Oxygen gas supply to the Ozonizer is below JERROR (652) 100mI/min. 660 |AREA FAILURE ERROR (660) ‘TN-110 System Program automatically shuts down the power to the ozonizer. Area value is failure.Appendix C : STANDARD SPECIFICATIONS APPENDIX C : STANDARD SPECIFICATIONS © Total Nitrogen Analyzer Model TN-110 Method Catalytic oxidative pyrolysis/chemiluminescence Samples Liquids, solids and gaseous samples *1 Furnace Temperature | Max. 1,100 °C (By TN-110, Main Unit) Catalyst Platinum Catalyst ‘Measuring Range 0.5 5,000 ppm Sample Size Liquid *2 : 50,1 [or less, Solid : 30 mg or less Measuring Time 3- 10min Data Processing Function | Using a personal computer. Display Function Displayed on a PC-CRT. Printing Function Printout using an external printer "3 ‘Keyboard PC fall keyboard ‘Interface Balance Input (RS232C) : 1 channel (TN-110, Main Unit) ‘Analog Output DC 0-1 V fill sale Gas Requirements ‘Argon (purity : 99.98 % or more, 294 - 490 kPa) Oxygen (purity : 99.7 % of more, 294 - 490 kPa) *4 Power Supply "TN-110 Main Unit : AC 100/115/230/240 V, 50/60 Hz, 1,000 VA ABC + AC 100/115/230/240 V, 50/60 Hz, 40 VA ND-100 : AC 100/115/230/240 V, 50/60 Hz, 500 VA Dimensions and Weight | TN-110 Main Unit : Approx. 330(W) x 400(D) x 435(H) mm, Approx. 17 kg ABC + Approx. 440(W) x 250(D) * 180(E) min, Approx. LI kg ND-100 Approx. 260(W) x 400(D) x 435(H) mm, Approx. 17 kg ‘Vacuum Pump ——_: Approx. 400(W) x 200(D) x 500(41) mm Approx. 14 kg Personal Computer (System Requirements to Run TN-110 System Program ) *5 Processor Pentium® 133 MHz or higher RAM 32 MB ot higher HD. Requires at least 100 MB of available disk space Drive ‘CD-ROM Display Display resolution of at least 640 > 480 Printer Windows®-compatible printer *1 : The optional Gas Injector is needed for measuring gaseous samples. *2: When used with the optional Constant Rate Injector, more quantity of liquid sample (Max. 200 1) could be injected. *3 : A printer is needed for printing reports. "4: 1 kg/em’G= 98.066 kPa *5 : Available only with the English-language version of Windows® 95/98. ‘The specifications for the personal computer are minimum requirements to run the System Program.‘Appendix C : STANDARD SPECIFICATIONS © Reproducibility by Standard Sample Pyridine / Toluene Solution Concentration Sample Size RSD (%) <3 500 u g/ml 201 100 g/mi 2041 =3 10 g/ml 20u1 <5 Lu g/ml 401 <8