Summary of Contents for erc RefractoMax524
- Page 1 RefractoMax524 RI Detector Operator’s Manual High Sensitive Refractive Index Detector for High Performance Liquid Chromatography Publication No. 77-5014-10...
- Page 3 Spare Parts Availability It is the policy of ERC to provide maintenance spare parts for a period of seven (7) years after the final production of the instrument. Spare parts may be available after the seven (7) year period but only on an “as available”...
- Page 4 Teflon® is Registered Trademark of E.I. du Pont de Nemours and Company. Before Starting: We thank you very much for your choosing RefractoMax524 Refractive Index Detector for your High Performance Liquid Chromatography System. RefractoMax524 Refractive Index Detector is designed to be an analytical device for pure research purpose and may not be suitable for in vitro diagnostic analysis.
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Page 5: Table Of Contents
INDEX SECTION 1. INTRODUCTION .............1 1-1. Principle of refractive index detection ............... 1 1-2. Specifications ....................3 SECTION 2. UNPACKING AND INSTALLATION ........4 2-1. Installation Site Requirements ................4 2-2. Power Requirements ..................4 2-3. Unpacking and Inspection ................. 4 2-4. - Page 6 3-4-8. Other Messages ..................19 SECTION 4. GETTING STARTED ............. 20 4-1. Just in Case ! ....................20 4-2. Start Up......................20 4-3. Parameter Setting ..................20 SECTION 5. MAINTENANCE AND VALIDATION ......21 5-1. Cell Cleaning ....................21 5-1-1. Preparations ..................... 21 5-1-2.
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Page 7: Section 1. Introduction
RefractoMax524 is a deflection or Snell type refractive index detector. Snell's law states that a parallel light beam, when passing through a dielectric interface separating two media of different refractive index at an angle of incidence greater than zero, will be refracted as a function of the magnitude of difference of the refractive indices of the two media. - Page 8 During operation, RefractoMax524’s reference and sample cells are filled with mobile phase. The reference cell is then isolated from the flow path and mobile phase flows through the sample cell only. As long as no difference exists between the refractive indices of the media of the two cells, there is no refraction of the light passing through them.
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Page 9: Specifications
1-2. Specifications Construction Deflection type Refractive Index Range 1.00 ~ 1.75 Range 1/4 ~ 512 µRIU Linearity 600 µRIU Noise 5 nRIU( Response : 3 seconds ) ≤ Response Time 0.1, 0.25, 0.5, 1.0, 1.5, 2, 3, 6 sec. Polarity Positive/Negative Auto Zero Optical &... -
Page 10: Section 2. Unpacking And Installation
Section 2. Unpacking and Installation 2-1. Installation Site Requirements To install RefractoMax524, please make sure that any of followings shall be kept away from it to prevent interference on your analysis. Refractive Index Detector, in general, is very sensitive to the change in ambient temperature and airflow that results a drift of baseline. -
Page 11: Standard Accessories
As you are installing RefractoMax524, please make sure to loosen these screws. 1. Move RefractoMax524 to the side of a bench to make the locking screws accessible while supporting it to prevent it from falling. 2. Loosen the locking screws, but do not remove them, using the 5mm hexagonal key. -
Page 12: Replacing Fuse
Electrically conducting spills can occur when conductive WARNING: HPLC solvents are spilled on or in the instrument. Ground the instrument properly to protect the operator SHOCK HAZARD from electrical shock. Proper grounding also protects the instrument from power line noise. Verify that the instrument is properly grounded through the power line ground terminal. -
Page 13: Tubing Connections
2-6-3. Tubing Connections Connection to the Inlet RefractoMax524 must be the last component in your LC system. No detector or backpressure regulator can follow it. CAUTION Do not use narrow-bore tubing for the outlet. Hook up the narrow-bore stainless steel tubing of the Standard Accessory (0.25 mm ID, 1m long) with the inlet (IN) port of front panel. -
Page 14: Solvent Recommendations
2-7. Solvent Recommendations Grade of Solvents HPLC grade solvents are recommended for better instrument performance and chromatographic data. Solvent Filtering All solvents, including deionized water, should be filtered by in-line solvent filter. Solvent Degassing Solvents should be properly degassed prior to use. Solvents that are not properly degassed may cause bubble formation in pump heads and in the detector cells potentially causing pressure flow problems and a noisy chromatographic baseline. - Page 15 Fluorocarbon solvents will alter Teflon® over long exposure. CAUTION Flush with pentane or another light hydrocarbon. If you want to replace one solvent with an immiscible one, flush note out the existing mobile phase with an intermediary solvent inter-miscible with your initial and final solvents. For example, you want to replace water in your HPLC with chloroform;...
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Page 16: Characteristics Of Commonly Used Mobile Phase
2-8. Characteristics of commonly used mobile phase Those in bold should not be employed Flash Boiling Fire Point Polarity Viscosity Refractive Vapor Point Point Cut-off Gravity Index Density Upper Lower (nm) Fluoroalkanes -0.25 1.25 n-Pentane 0.00 0.23 1.358 <-40 308.9 36.1 Hexane 0.00... -
Page 17: Section 3. Function Keys And Displays
Section 3. Function Keys and Displays 3-1. Front Panel [13] [12] [11] [10] Power Switch Press this key once to turn on or off the unit. Event Marker Key: Press to generate a marker signal. (5% of Full Scale) Purge Key: Press to turn purge valve on or off to change flow path. -
Page 18: Rear Panel
3-2. Rear Panel [14] [15] [16] [17] [18] [19] [13] [12] [11] [20] [21] [22] [11] MAKER IN: External Signal In (Event Marker) [12] ZERO IN: External Signal In (Auto Zero) [13] PURGE IN: External Signal In (Purge On) [14] ERROR OUT: Signal Out (Error) [15] LEAK OUT: Signal Out (Solvent Leak) -
Page 19: Lcd Display (User Screens)
3-4. LCD Display (User Screens) RefractoMax524 has a LCD display on the front panel as shown in 3-1. Front View here above. The display consists of following four screens and by solvent delivery pump, connect a tubing line directly from the pump to RefractoMax524 inlet port bypassing the column. Some cleaning solutions should be injected, however, directly into the flow cells by syringe due to their high corrosiveness or safety concern. -
Page 20: Parameter Setting Screen
3-4-3. Parameter Setting Screen PARAMETER Parameter Setting Screen Home SETTING Recorder Range Setting By pressing Enter key, a cursor appears to indicate the range PARAMETER is selectable. REC. RANGE 512uRIU Select 512, 256, 128, 64, 32, 16, 8, 4, 2, 1, 0.5 or 0.25 by pressing Up or Down Arrow keys . - Page 21 Default Setting PARAMETER If you want to reset parameter setting and bring it back to SELECT DEFAULT default setting, press Enter key. A cursor and “NO” show up. Select “YES” by Arrow keys . Press Enter key to confirm the selection. Default Setting (2) ERASE After pressing Enter key above, this message shows up to...
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Page 22: Auto Set Up Information Screen
Parameter Default Setting Parameter Setting value Unit Default 0.25, 0.5, 1, 2, 4, 8, 16, 32, 64, REC. RANGE RIU/10mV µ 128, 256, 512 (12 steps) INTEG. RANGE 125 or 500 RIU/1V µ TEMPERATURE Celsius OFF, 30 to 55 (increment: 1 TIME CONSTANT 0.1, 0.25, 0.5, 1, 1.5, 2, 3, 6 (8 steps) Second... -
Page 23: Validation Execute Screen
SPAN Result (Span) of the latest Validation of this unit 512.5µRIU LAMP VOLTAGE Current Lamp Voltage of this unit 3.75V 3-4-6. Validation Execute Screen Validation Execute Screen Home VALIDATION EXECUTE Press Enter key to get into following screen sequence. Enter Validation Date Entry Screen INPUT DATE Refer to 5-2-2. -
Page 24: Error Messages
If you are commanding Auto-Zero via external control devise, refer to the procedure for “Optical Balance Error. If you have this error as you are turning on RefractoMax524, please contact our local representatives in your area. Overheating Error 100.0 µRIU 70 This indicates overheating of optical block. -
Page 25: Other Messages
3-4-8. Other Messages There are four other messages as described below. Some of them are more like a warning message. Low Light Intensity 0.0 µRIU INTENSITY This indicates inadequate light intensity. There are several possible causes for this error as follow. 1. -
Page 26: Section 4. Getting Started
Section 4. Getting Started 4-1. Just in Case ! Prior to operation, check the following one more time. Locking screws are loosened. Mobile phase solvent is freshly made and degassed well. All wetted parts are chemically compatible to the mobile phase solvent. Mobile phase flushed through the entire flow path;... -
Page 27: Section 5. Maintenance And Validation
To introduce cleaning solution into RefractoMax524 by solvent delivery pump, connect a tubing line directly from the pump to RefractoMax524 inlet port bypassing the column. Some cleaning solutions should be injected, however, directly into the flow cells by syringe due to their high corrosiveness or safety concern. -
Page 28: Validation
The sample and reference cells should be filled with water or air (blown dry) before proceeding. Filled the syringe with cleaning solution and connect to the inlet port of the RefractoMax524. Carefully inject the cleaning solution. For safety, make sure that outlet tubing is led to drain bottle. -
Page 29: Span Validation
Dissolve in the 100 ml de-ionized, filtered, degassed water and dilute to flask’s mark. note Use freshly made sucrose solution always. (2) Equilibrate RefractoMax524 by pumping de-ionized water through both reference and sample cells. Use the same de-ionized water as that used to prepare the sucrose standard solution. -
Page 30: Auto Set Up Execute
The remaining time of execution (min) 100.0 µRIU AUTO PURGE 100min Comment display column SSEQ mode ZERO: AUTO ZERO PURGE: PURGE ON F: FINE UNTEMP: TEMP.UNSTABLE S: STANDRD INTENS: INTENSITY C: COARSE Indicates that RefractoMax524 is under Auto Set Up... -
Page 31: Section 6. Shutdown Procedure
Keep a small amount of flow to keep down the amount of corrosive chloride impurities in the cell. 6-3. Long-Term Storage If RefractoMax524 will not be used for a week or more, the sample and reference cells should be blown dried. If the detector is to be exposed to sub-freezing temperatures, an antifreeze flush, such as methanol must be used. -
Page 32: Section 7. Troubleshooting
You will begin by adding the pump to RefractoMax524 first and you will add the column last. If another type of detector is available, it is a good idea to use it before RefractoMax524 to aid in troubleshooting as reference. -
Page 33: Troubleshooting (Diagnosis Chart)
7-4. Troubleshooting (Diagnosis Chart) Problem Possible Cause Solution Noise Bubble in the pump. Purge pump heads. Use only premixed/degassed mobile phase. Bubble in the detector. Elevate drain reservoir above the level of the flow cells to create slight backpressure. Premix and degas mobile phase well. - Page 34 Problem Possible Cause Solution Drift Contaminated or non-HPLC grade Prepare fresh mobile phase solvents. (premixed/degassed) (continued) Vapor pressure of mobile phase is Reduce or turn temperature too high for operating temperature control off. causing bubble formation in Modify method to exclude or reference cell.
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Page 35: Appendix. Miscibility Chart Of Solvents
Appendix. Miscibility Chart of Solvents Acetic Acid Acetonitrile Chloroform Cyclohexane Methylene Chloride X = Immiscible Dimethyl Formamide Dioxane Ethyl Ether Hexane Methanol Methyl t-Butyl Ether Trimethylpentane Pentane Propanol-2 Tetrahydrofuran Water... - Page 36 ERC Inc. Customer Support Desk 5-8-6 Nishi-Aoki, Kawaguchi, Saitama 332-0035, Japan Phone: Japan (81) 48-240-5750 Facsimile: Japan (81) 48-259-0715 URL: http://www.erc.jp e-mail: erc-sales@erc.jp...
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