Page 1 荧光检出器 PRIMAIDE 1440...
Page 2 日立仪器（大连）有限公司 Hitachi Instruments (Dalian) Co., Ltd. 中国大连市甘井子区辛寨子东街 15 号 No.15 Xinzhaizi East St. Ganjingzi District Dalian of China Copyright C Hitachi Instruments (Dalian) Co., Ltd. 2021. 5th Edition, 2021 All rights reserved. Printed in China. Part No. 8DD-9705...
Page 3 Hitachi Instruments (Dalian) Co., Ltd. 3. Hitachi Instruments (Dalian) Co., Ltd. assumes no liability for any direct, indirect, or consequential damages arising from use not described in this manual.
Page 4: Preface
Note that physiologically or biologically active samples are not applicable to the Primaide 1440 FL Detector because of possible infection with bacteria or viruses. This product is intended for use by persons having a basic knowledge of chemical analysis.
Page 5: About This Manual
ABOUT THIS MANUAL This instruction manual describes how to use and maintain the Primaide 1440 FL Detector. This instruction manual consists of the following sections. IMPORTANT (Warranty, Installation, Relocation, After-sale Technical Service, etc) SAFETY SUMMARY (collected and summarized) Section 1 OUTLINE (Basic Operation) Section 2 FUNCTIONS (Name and Function of Each Part on FL detector) Section 3 OPERATION (Basic Operation) Section 4 MAINTENANCE &...
Page 6: Important
IMPORTANT Warranty on Product Limited Warranty The Primaide 1440 FL Detector is warranted to be free from defects in material or workmanship under normal use within the product specifications indicated in this manual and under conditions given below. This warranty is void if the software is not used according to the instruction manual.
Page 7 Warranty Limitations and Exclusions Disclaimer of Warranty THE MANUFACTURER MAKES NO WARRANTIES, EITHER EXPRESS OR IMPLIED, EXCEPT AS PROVIDED HEREIN, INCLUDING WITHOUT LIMITATION THEREOF, WARRANTIES AS TO MARKETABILITY, MERCHANTABILITY, FOR A PARTICULAR PURPOSE OR USE, OR AGAINST INFRINGEMENT OF ANY PATENT. IN NO EVENT SHALL THE MANUFACTURER BE LIABLE FOR ANY DIRECT, INCIDENTAL OR CONSEQUENTIAL DAMAGES OF ANY NATURE, OR LOSSES OR EXPENSES RESULTING FROM ANY DEFECTIVE PRODUCT OR THE...
Page 8: Installation, Relocation And After-Sale Technical Service
(m) Failure due to a life-limited part that has exceeded the end of its useful lifetime. Limitations of Liability Hitachi Instruments (Dalian) Co., Ltd. shall not be liable in contract or in tort (including, without limitation, negligence, strict liability or otherwise) for claims by third parties (other then for bodily injury or property...
Page 9: Technical Seminars And Training Courses For Users
After-sales Service (a) For after-sale technical service of this instrument, please notify our local sales representative or service office. (b) A maintenance & service contract is available for servicing the instrument after the warranty period has ended (service available at charge).
Page 10: Caution On Disposal Of Instrument
Note, however, that the environmental protection laws and regulations may be revised or amended. Therefore, be sure to consult with your local Hitachi High-Tech Science sales or service representative when planning disposal of this instrument or its parts and accessories.
Page 11: Information For Users On Weee (Only For Eu Countries)
effect on its performance or functionality. Safety Requirement This instrument conforms to the LVD Directive 2014/35/EU, and has the CE conformity marking for it. The instrument is designed to satisfy the European Norm N61010-1 (2010). Note this instrument falls into Class-1 Pollution Level 2 of EN61010-1 (2010).
Page 12: Other Precautions
Other Precautions Handling of Chemicals and Samples (a) The user is responsible for following relevant laws and regulations in handling, storage and disposal of chemicals and samples used in analytical operation with this instrument. (b) Reagents, standard solutions and accuracy-control samples shall be handled, stored and discarded as instructed by the respective suppliers.
Page 13: Safety Summary
SAFETY SUMMARY Before using the Primaide 1440 FL Detector, be sure to read the following safety instructions carefully. The hazard warnings which appear on the warning labels on the product or in the manual have one of the following alert headings consisting of a safety alert symbol and signal word WARNING or CAUTION.
Page 14: General Safety Precautions
Disconnect the power cord plug from the power outlet. Then, after providing proper safety measures as required, contact the nearest service representative of Hitachi High-Tech Science. Using the instrument in such an abnormal condition could result in an electric shock or fire.
Page 15: Warning Precautions In The Manual
SAFETY SUMMARY WARNING Precautions in the Manual WARNING Ignition of Flammable Chemicals • This instrument is not explosion-proof. In unattended operation, do not use organic solvents having an ignition point below 70 C • Beware of ignition hazard when using flammable chemicals such as organic solvents.
Page 16 SAFETY SUMMARY WARNING precautions in the Manual (Continued) WARNING Electric Shock due to Contact with Inside of Instrument When removing the xenon lamp cover for part replacement, etc., there is a risk of electric shock. Be sure to turn OFF the power switch and disconnect the power cord from the receptacle in advance.
Page 17 SAFETY SUMMARY WARNING precautions in the Manual (Continued) WARNING Injury due to Xenon Lamp Explosion [In use] • When the cumulative turn-on time of the xenon lamp exceeds the guaranteed useful lifetime, the electrodes evaporate and the scattered matter sticks to the bulb wall, so its blackening progresses and heat dissipation is hindered.
Page 18 SAFETY SUMMARY WARNING precautions in the Manual (Continued) WARNING Injury due to Xenon Lamp Explosion [At mounting] (Continued) • Do not touch the quartz glass part of the xenon lamp with bare hands. If the quartz glass part of the xenon lamp is contaminated with dust or fingerprints, wipe it using a gauze sheet or absorbent cotton cloth slightly moistened with high-quality alcohol.
Page 19: Caution Precautions In The Manual
SAFETY SUMMARY CAUTION Precautions in the Manual CAUTION Touching Hot Part Could Result in Burns The light source lamp and its cover become hot during operation and remain hot for a while even after power-off. They can severely burn you if touched. Before replacement of the lamp, turn power off and wait for about one hour until it cools down sufficiently.
Page 20: Warning And Caution Labels On Instrument
SAFETY SUMMARY WARNING and CAUTION Labels on Instrument The warning labels shown below are attached on the Primaide 1440 FL Detector. Read the warning labels carefully , and check the instructions on them to attain a clear understanding with reference to actual parts. Periodically check the appearances of these warning labels to see if they are clean to allow easy reading over a safe distance.
Page 21 SAFETY SUMMARY WARNING and CAUTION Labels on Instrument (2) Explosion of Vapor from Flammable (3) Electric Shock due to Contact with Light Chemicals Source Power Supply (4) Before Turning on Xenon Lamp (6) Explosion of Xenon Front View Lamp 図 (5) Ignition of Flammable Chemicals (7) Burns due to Contact with Hot Part SAFETY - 9...
Page 22: Notice Precautions
SAFETY SUMMARY NOTICE Precautions Precautions on Use of Solvents • Fluororesin, PEEK, quartz and SUS316 materials are used for the wetted parts of the instrument. Never use solvents that would corrode these materials. • This instrument has internal parts made of materials that could be corroded by strongly acidic solutions, strongly alkaline solutions or organic solvents.
Page 23 SAFETY SUMMARY NOTICE precaution (Continued) Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally. If necessary, conduct measurement on a control sample. Possible Carryover When examining the results of measurements, take account of the possibility of occurrence of a carryover.
Page 24: Table Of Contents
CONTENTS PREFACE ....................... 1 ABOUT THIS MANUAL ..................2 IMPORTANT ..................IMPORTANT-1 Warranty on Product ..............IMPORTANT-1 Installation, Relocation and After-sale Technical Service ..IMPORTANT-3 Technical Seminars and Training Courses for Users .... IMPORTANT-4 Estimated Life time of the Instrument ........IMPORTANT-4 Caution on Disposal of Instrument .........
Page 25 3.1.4 Wavelength setting................3-6 3.1.5 Shutdown procedure ................ 3-7 3.1.6 Flushing the flow cell after use ............3-7 UTLTY Setting ....................3-8 3.2.1 Offset setting ..................3-8 3.2.2 Time constant setting ............... 3-9 3.2.3 Use time program setting ..............3-10 3.2.4 PMT voltage setting .................
Page 26 4.2.3 Sensitivity check ................4-2 4.2.4 Wavelength accuracy check and calibration ........4-15 4.2.5 Leak sensor check ................4-18 4.2.6 Drain tray check ................4-20 Periodic Checks ................... 4-21 4.3.1 Xe lamp energy check ..............4-21 4.3.2 Wavelength accuracy check using Hg lamp ........4-21 4.3.3 Lamp logbook check ................
Page 27: Outline
1.1 Isocratic System The isocratic system has a simple configuration in which single- solvent analysis is performed. Primaide 1440 Fluorescence Detector Detector cell Mobile Phase...
Page 28: Low-Pressure Gradient System
In the low-pressure gradient system, two or more solvents are mixed in its low-pressure section from which a liquid feed is performed by a single pump. The composition of an eluent is made to vary with time in chromatographic separation. Primaide 1440 Fluorescence Detector Mobile phase Wash Solution...
Page 29: Functions
2. FUNCTIONS 2.1 Name and Function of Each Part on FL detector Power switch UI pad Drain tray Fig. 2-1 Front Panel Power switch : Turns power ON/OFF. UI pad (option) : A keypad required for unit operation. LEDs : Four LED indicators are provided for indicating the following states.
Page 30 LAMP OFF IN Analog signal output AUTO ZERO IN unit (option) e-Line Power source connector Ground terminal Fig. 2-2 Rear Panel Analog signal output unit (Option) :Provides PROCESSOR, RECORDER, MAKER IN terminal. Ground terminal :The terminals for grounding connection (three terminals). Power source connector :Connects the power supply cable.
Page 31: Name And Function Of Each Part On Ui Pad (Option)
Indication Function Remarks MARKER IN The marker function is activated by The marker function is started (option) means of contact signal input. when the short-circuit signal of more than one second is input. RECORDER Analog output for recorder The florescence intensity value (option) data is output.
Page 32 Table 2-3 Key Functions Indication Function Remarks Sets display and output to zero at each measuring wavelength. (Auto zero) Used to set each measuring wavelength. (Wavelength) (1) Sets offset value, time constant, etc (UTILTY). SET UP (2) Sets digital communication channel via the e-Line, UTLTY LCD contrast.
Page 33 Indication Function Remarks RECORD Used to specify the recorder full-scale range, recorder output speed, and output data. (Record) SPECT Obtains spectrum over a specified wavelength range and stores the spectrum in memory. (Spectrum) MARKER Places a marker on the recording. (Marker) (1) Used to return from data input mode to the monitor screen.
Page 34: Description Of Fluorometry
2.3 Description of Fluorometry 2.3.1 Principle of fluorometry Excitation Fluorescence or Phosphorescence Stable condition Unstable condition (Ground state) (Excited state) Radiationless Radiationless transition transition Excited state V = Excited triplet state Light Light Excitation light Ground state V = Absorption Fluorescence Phosphorescence Fig.
Page 35 When light strikes an organic molecule in the ground state, it absorbs radiation of specific wavelengths and several excited states are populated. A part of the excitation (absorbed) energy is lost in vibrational relaxation, i.e. radiationless transition to the lowest vibrational level in the excited state. The molecule can return to the ground state by;...
Page 36: Advantages Of Fluorometry
2.3.2 Advantages of fluorometry For verifying the advantage of fluorometry, the limitation of absorbance measurement in its application to low-concentration samples is explained first. In this discussion, we will consider the detection of a sample that has a transmittance of 99% (relative to the blank). If we assume that the inaccuracy of the % transmittance measurement is 0.1%, the reliability of the observed data is as follows: 100.0 ...
Page 37 A graphical description of why fluorescence can provide better sensitivity than absorbance is presented in Fig. 3-5. In this figure, the signal I is used to represent the difference between the intensity of the incident beam I and the intensity of the transmitted beam I in absorptiometry.
Page 38 In contrast, if the fluorescence spectra do not overlap (Fig. 3-6 (b)), quantitative analysis of each compound can be made by selecting the appropriate fluorescence emission wavelength (even if the absorption wavelengths of two components are the same). Absorption spectra Excitation spectra Fluorescence spectra Component A...
Page 39: Notes On Fluorescence Analysis
2.3.3 Notes on fluorescence analysis Raman Scattering When fluorescence is measured, two additional peaks may appear in the spectrum. The Rayleigh peak appears at the excitation wavelength and is due to scattered light, while the Raman peak appears at longer wavelength than the excitation.
Page 40 Raman scattering (nm) Excitation wavelength Fig. 2-7 Raman Spectrum of Water Notes on Handling Samples that Contain a High Concentration of the Compound of Interest When the concentration of the compound of interest is relatively high, various error factors will arise. The greatest factor is that the excitation beam is substantially absorbed near the entrance slit of a cell and it cannot reach the cell center adequately.
Page 41 If emission occurs only in the entrance area for excitation beam, such a sample needs to be diluted with an appropriate factor before measurement. The second factor is called “concentration quenching” where activity is disturbed by interaction of molecules. Another potential error that may occur when fluorescence detection is used is the re-absorption of fluorescence (self- absorption of fluorescence).
Page 42 Second-order and Third-order Radiation The Raman peak is described as a cautionary item when the excitation and emission wavelengths are comparatively close to each other. Conversely, when these wavelengths are comparatively distant from each other, the analyst should be aware of the second and third-order radiation phenomenon.
Page 43 In measurement of a fluorescence spectrum, many peaks appear besides that of sample fluorescence. It is necessary to find the correct sample peak according to the explanation given above. Temperature Dependency of Fluorescence Intensity In most cases, the fluorescence intensity decreases by 1 to 2% as the temperature of sample increases by 1 C.
Page 44: Principle Of Operation
2.3.4 Principle of operation Excitation Diffusion plate monochromator Plane mirror Sample Monitor detector Xenon lamp Measuring detector Emission monochromator Xenon lamp (Fluorescence starter monochromator) Xenon lamp Photomultiplier high ballast voltage circuit Monitor detector Sample amplifier fluorescence amplifier Operational circuit Recorder or integrator Electrical connection Optical path...
Page 45: Features Of Light Source
2.3.5 Features of light source The light source thermally dissociates ozone via the heat generated by the xenon lamp itself. This allows the use of a quartz-bulb xenon lamp that produces intense radiation even in the short wavelength region. As a safety measure against failure or stoppage of the cooling fan, a thermal sensor works to extinguish the xenon lamp in about 15 minutes if the fan stops during analysis at a room temperature of 27 C, or in about 20 minutes if the fan was...
Page 46 (10) Recorder output (Option): 10 mV Full scale. Full scale 1 to 1000 FLU (settable in steps of 1). (11) Processor output (Option): 1 V Full scale, digital by e-Line. -40 (-40 mV) to 1000(1000 mV) (12) Response: Changeable in 7 steps corresponding to time constants of 0.05 / 0.1 / 0.5 / 1.0 / 2.0 /4.0 / 8.0 seconds.
Page 47 (19) Time program Number of programs ....9 Settable time ......Up to 600 minutes in increments of 0.1 minute Number of steps storable ..100 steps for a total of 9 files Programmable parameters ..Measurement wavelength (Ex and Em) Baseline processing PMT gain (20) GLP support function:...
Page 48 (31) Dimensions: 340(W) mm  464(D) mm  297(H) mm (32) Weight: Approx. 26.7 kg NOTE: Please contact your local Hitachi High-Tech Science Corporation sales representative about a purchas of the Thermo cell. 2 - 20...
Page 49: Operation
3. OPERATION The method of FL detector operation using the optional UI pad is described here. CAUTION Fatigue due to Long-Hour Operation If you keep working with the display monitor and keyboard for long hours, your eyes and body will be fatigued to jeopardize your health.
Page 50 * The current channel setting LED and the Xe LAMP LED will light in blue. <Initial screen> FL Detector 8DD8440-00 © Hitachi High-Tech Science Corp.2017  <Initializing screen> WL DRIVE & LAMP INITIALIZING The sequence of wavelength drive (check of reference point for drive), lighting of the lamp and auto zeroing is performed.
Page 51 The 1st monitor screen (FL indication) TIME PROG LAMP Status Elapsed Program indicator time number Lamp Excitation indicator Fluorescence wavelength Emission intensity wavelength  key,  key or ESC key  key or  key The 2nd monitor screen (energy indication) MONITOR (Ex) (Em) LAMP...
Page 52: Parameter Setting
3.1.2 Parameter setting For entering a value, press numeric key, then ENT (enter) key. (a) Single numeric input Parameter name Input range NO.(1 – 9) SET PROGRAM Input part (b) Plural numeric input Input item Parameter name LAMP CHANGE (MM, DD, YYYY) <1 - 12>...
Page 53 (iii) Numeric inputs are accepted by the ENT key, and moves to the next item. When an input error has occurred, the cursor is set to the front line in the input part while displaying inputs, and then waits for retype. Press the ESC key to return to the initial screen (monitor screen).
Page 54: Auto Zero Adjustment
3.1.3 Auto Zero adjustment The output value should be zeroed when zero point adjustment is required or when the data baseline deviates from the recorder zero point. Press the key. The FL indication on the 1 monitor screen is reset to zero and output signal becomes zero.
Page 55: Shutdown Procedure
Then, the cursor moves to Em. Set an emission wavelength (Em). <Em wavelength setting screen> (250 – 900,0) nm Press numeric keys ((2 5 0 to 9 0 0)) and then the ENT key. * This wavelength is settable within a range from 250 to 900 nm in increments of 1 nm.
Page 56: Utlty Setting
3.2 UTLTY Setting The UTILITY key sets the following conditions. • OFFSET • TIME CONSTANT • USE PROG (whether to use time program or not) • PMT VOLT (photomultiplier voltage) • OTHERS 3.2.1 Offset setting The OFFSET is a set input signal amount that is added to the actually measured value for output.
Page 57: Time Constant Setting
 Typically, the negative input limit for an integrator or data processor is approximately -10 mV. If the baseline decreases below this level, it becomes impossible to integrate the peaks in the chromatogram (see Fig. 3-2 (a)). In such a case, the offset function is used to adjust the shifted baseline to the allowable input signal range of the data processor (see Fig.
Page 58: Use Time Program Setting
Select TIME CONSTANT. Press numeric key 2 and then the ENT key. The following display will be presented. <Time constant setting screen> TIME CONSTANT (0.05s=1, 0.1s=2, 0.5s=3, 1.0s=4, 2.0s=5, 4.0s=6,8.0s=7) Set a time constant value. Press numeric key (1 to 7, usually input 4) and then the ENT key.
Page 59: Pmt Voltage Setting
Select use (YES=1) or non-use (NO=0) of a time program. Press a numeric key (1 or 0) and then the ENT key. * 1: Time program starts by start input. 0: Time program does not start despite start input. * Default value: 1 Selection or avoidance of a time program is now completed and the 1 monitor screen returns.
Page 60: Other Settings
Set a photomultiplier voltage. Press numeric key (1 to 5, usually input 3) and then the ENT key. * Default value: 3 Photomultiplier voltage setting is now completed and the 1 monitor screen returns. 3.2.5 Other settings Set the following items. •...
Page 61 (d) The following display will be presented. <Em bandwidth selecting screen> Em BANDWIDTH (STANDARD=1, WIDE=2) Set an Em bandwidth value. Press numeric key (1 or 2, usually input 1) and then the ENT key. * Default value: 1 (e) Em bandwidth setting is now completed and the 1 monitor screen returns.
Page 62 (c) The following display will be presented. <Others setting screen> OTHERS (Em BANDWIDTH=1, ERROR OUT=2, LEAK SENSOR=3, LAMP=4) Select ERROR OUT. Press numeric key 2 and then the ENT key. (d) The following display will be presented. <Error out signal selecting screen> ERROR OUT SIGNAL (DISABLE=0, ENABLE=1) Invalid (0) or valid (1) status of error out signal output is settable.
Page 63 (c) The following display will be presented. <Others setting screen> OTHERS (Em BANDWIDTH=1, ERROR OUT=2, LEAK SENSOR=3, LAMP=4) Select LEAK SENSOR. Press numeric key 3 and then the ENT key. (d) The following display will be presented. <Leak sensor selecting screen> LEAK SENSOR (OFF=0, ON=1) Select use (ON=1) or non-use (OFF=0) of the leak sensor.
Page 64 Select OTHERS. Press numeric key 5 and then the ENT key. (c) The following display will be presented. <Others setting screen> OTHERS (Em BANDWIDTH=1, ERROR OUT=2, LEAK SENSOR=3, LAMP=4) Select LAMP. Press numeric key 4 and then the ENT key. (d) The following display will be presented.
Page 65: Glp Functions
3.3 GLP Functions For this function, the following items are settable. • Xe lamp LOGBOOK data display and resetting • Hg lamp LOGBOOK data display and resetting • KEY LOCK setting • WL CHECK (wavelength accuracy check) by using Hg lamp •...
Page 66: Xe Lamp Logbook Data Resetting
The following display will be presented. <Logbook selecting screen> LOGBOOK (REPORT=1, RESET=2) Select Report. Press numeric key 1 and then the ENT key. On the logbook report screen, the total on period of the Xe lamp and its standard lifetime (in parentheses under Xe LAMP), the number of switching-on times and the date of the last lamp change will be indicated.
Page 67 The following display will be presented. <Lamp selecting screen> LAMP SELECT (Xe=1, Hg=2) Select Xe. Press numeric key 1 and then the ENT key. The following display will be presented. <Logbook selecting screen> LOGBOOK (REPORT=1, RESET=2) Select RESET. Press numeric key 2 and then the ENT key. Next, advance to the Xe lamp change date setting screen for setting the date of xenon lamp change.
Page 68: Hg Lamp Logbook Data Display
(c) Input a year for YYYY. <Xe lamp change date setting screen (year)> Xe LAMP CHANGE YYYY) <1-31> 2010 Press numeric keys (2 0 0 0 to 2 1 0 0) and then the ENT key. * Even when the same year as desired is indicated, its numeral must be input again without fail.
Page 69: Hg Lamp Logbook Data Resetting
The following display will be presented. <Logbook selecting screen> LOGBOOK（REPORT=1, RESET=2） Select Report. Press numeric key 1 and then ENT key. On the logbook report screen, the total ON period of the Hg lamp, the number of switching-on times and the date of the last lamp change will be indicated.
Page 70 Select Hg. Press numeric key 2 and then ENT key. The following display will be presented. <Logbook selecting screen> LOGBOOK（REPORT=1, RESET=2） Select RESET. Press numeric key 2 and then ENT key. Next, advance to the Hg lamp change date setting screen for setting the date of mercury lamp change.
Page 71: Key Lock Setting
* Even when the same year as desired is indicated, its numeral must be input again without fail. Logbook setting is now completed and the 1st monitor screen returns. * When a mercury lamp change date is set, the total ON period of the Hg lamp and the number of switching-on times will be automatically reset accordingly.
Page 72: Wavelength Accuracy Check By Using Hg Lamp
3.3.6 Wavelength accuracy check by using Hg lamp Whether wavelength is normal or not can be checked by using the 254 nm bright line of mercury lamp. Press the key. The following display will be presented. <GLP initial screen> (LOGBOOK=1, KEY LOCK=2, WL CHECK=3, Xe CHECK=4) Select WL CHECK.
Page 73: Xe Lamp Energy Check
* If ESC key is pressed prior to ENT key, or if this status continues for 5 minutes or longer, the system will return automatically to the 1 monitor screen. The result of emission wavelength (Em) check will now be displayed.
Page 74 <Xe lamp energy check screen> (energy check is in progress) CHECKING LAMP ENERGY (Xe) The result of Xe lamp energy check will be displayed automatically. <Xe lamp energy check result> Xe ENERGY 1200 Press the ENT or ESC key. * If 5 minutes or more elapses without pressing ENT or ESC key, the system will return automatically to the 1st monitor screen.
Page 75: Operating Instructions
3.4 Operating Instructions 3.4.1 Time program setting A time program is used for automatic change of the chromatograph measurement conditions with time. The time program takes priority over other settings. The following items can be set. • Measurement time (TIME) •...
Page 76 PROG Press the key. The time program No. setting screen appears. <Time program No. setting screen> SET PROGRAM NO. (1-9) Press a numeric key 1 to 9 and then the ENT key to create or change the program No., or select the existing program * Initial (default) value: 1 * If the setting will not be changed, press the ESC key to return to the 1st monitor screen.
Page 77 Setting of first step (start conditions) of time program: (a) Set the TIME. <Step setting screen (TIME indicated)> TIME BASE _ 0.0 Press numeric keys 0.0 and then the ENT key. * Be sure to enter “0.0” for TIME. * Initial (default) value: 0.0 * The program No.
Page 78 Press numeric keys 2 5 0 to 9 0 0 and then the ENT key. * Setting range: 250 to 900 nm It is recommended to set the same wavelength as was set for Em of the measuring wavelengths. * Initial (default) value: blank The cursor next moves to BASE.
Page 79 Setting of second and subsequent steps of time program: (a) Set the TIME to be changed. <Step setting screen (TIME indicated)> TIME BASE _ 10.0 Press numeric keys 0 to 6 0 0 and then the ENT key. * Setting range: 0 to 600 minutes, in increments of 0.1 minute The cursor now moves to Ex.
Page 80 (d) Set the BASE (baseline processing) to be changed. <Step setting screen (BASE indicated)> TIME BASE 10.0 Press a numeric key (1 or 2; usually 2) and then ENT key. * Enter 2 so as to match the baseline in the present step with the one in the previous step.
Page 81: Time Program Starting
(b) When the time program settings are completed, the 1 monitor screen reappears. Addition of steps Press the INSERT key to add a step to the program during step input. The step setting screen will appear, so make the addition in the same procedure as described above. However, the addition must be made within the time entered at the final step.
Page 82 HOLD Auto zero START STOP TIME (minutes) 10.0 20.0 Ex (nm) Em (nm) HOLD Described here is an example of newly setting a time program at program No. 1. Ten minutes after the start (1), photomultiplier voltage is changed from MID to LOW, excitation wavelength from 250 to 270 nm, emission wavelength from 350 to 370 nm, and hold function is applied, then measurement is completed after 20 minutes...
Page 83 PROG Press key.  SET PROGE NO. (1 - 9) Press 1 key and then the ENT key.  EDIT MODE (MODIFY=0, NEW=1) Press 1 key and then the ENT key.  TIME BASE Press 0 key and then the ENT key. Press 2 5 0 keys and then the ENT key.
Page 84 Check of time program Take the following procedure for checking the program that was set in the above. PROG Press the key.  SET PROGE NO. (1 - 9) Press 1 key and then the ENT key.  EDIT MODE (MODIFY=0, NEW=1) Press 0 key and then the ENT key.
Page 85: Spectrum Measurement
3.4.5 Spectrum measurement Set the wavelength scan range (maximum and minimum values) for excitation (Ex) and emission (Em), then measure and record the spectral data for each. * Carry out recording of spectral data with sample contained in the cell (sample not flowing, but stationary in cell). NOTE: The spectral bandwidth is 15 nm on both excitation and emission sides (bottom width of peak is about 30 nm).
Page 86 <Scan range setting screen (indicate WL1)> SCANNING WL RANG (WL1 WL2) nm FL (Ex) <200-800> 200 - 600 Press numeric keys 2 0 0 to 8 0 0 and then the ENT key. * Setting range : 200 to 800 nm * Initial (default) value : 200 * If setting will not be changed, press ...
Page 87 The scan monitor screen appears, and spectral acquisition within the set range is carried out. <Scan monitor screen (spectral acquisition under way)> SCANNING SPECTRUM NO.: 1 MODE: FL (Ex) Ex: ***nm Em: 350 nm * Pressing the ESC key during spectral acquisition will cancel the process.
Page 88 Press numeric keys 2 5 0 to 8 5 0 and then the ENT key. * Setting range : 250 to 850 nm * Initial (default) value : 250 * If setting will not be changed, press  key to proceed to WL2 setting.
Page 89: Recorder And Spectrum Output Factors Setting
* Pressing the ESC key during spectral acquisition will cancel the process. Spectral data will not be memorized. * The memorize spectrum No. set in the preceding step will be indicated at SCANNING SPECTRUM * Em is effective within the scan range set above. (g) When the spectral data memorization is completed, the system returns to the 1 monitor screen automatically.
Page 90 Full Scale Range of Recorder (a) Press the RECORD key. (b) The recorder setting screen appears. <Recorder setting screen> RECORD (RCD RANGE=1, RCD SPEED=2, SPECT RCD=3) Press numeric key 1 and then the ENT key to select RCD RANGE (recorder range). (c) The recorder full scale range setting screen appears.
Page 91 (c) The recorder speed setting screen appears. <Recorder speed setting screen> RCD SPEED (40 nm/min=1, 60 nm/min=2) Press numeric key 1 or 2 and then the ENT key to set a recorder speed. * Initial (default) value: 2 (d) When the setting of recorder output speed is finished, the system returns to the 1 monitor screen.
Page 92 <Background spectrum No. setting screen> BACKGROUND SPECTRUM NO. (0 ~ 4) Press a numeric key 0 to 4 and then the ENT key to select whether or not to correct the output spectrum. : Spectrum selected at RECORD SPECTRUM NO. will be output as it is. 1 - 4 : Spectral data obtained by subtracting the specified background data from the spectrum selected at RECORD...
Page 93: Marker Operation
* The output spectrum No. set before will be indicated at RCD NO. (g) When the spectrum output is finished, the 1 monitor screen will return automatically. 3.4.7 Marker operation A marker line is indicated only on the recorder. It is usable as an event marker to indicate, for example, the start of measurement or the point where set conditions were changed during measurement.
Page 94: Set Up Setting
3.5 Set Up Setting Before analytical operation, communication channel (CH) and liquid crystal display contrast (LCD CONTRAST) need to be set. • This setting is not required every time. When unnecessary, skip this setting. • The default value or currently set value is indicated before your input.
Page 95 Channel setting is now completed and the setup initial screen appears. Under DETECTOR, the selected channel setting is indicated. <Setup initial screen> SETUP: DETECT CONTRAST S. NO. 02AB-111 * When you press the ENT key here, the setup items selecting screen is presented to allow reentry. Or you can advance to LCD contrast setting.
Page 96: Liquid Crystal Display Contrast Setting
3.5.2 Liquid crystal display contrast setting Set a contrast (brightness) level of the LCD screen. SET UP UTLTY Turn on the power switch with the key held down. The following display will be presented. <Setup initial screen> SETUP: DETECT CONTRAST S.
Page 97: Standard Xenon Lamp Lifetime Setting
* When you press the ENT key here, the setup items selecting screen is presented to allow reentry. * The selected setting will be fetched upon turning on power supply at the next time. Turn OFF the power switch. 3.5.3 Standard xenon lamp lifetime setting WARNING Injury due to Xenon Lamp Explosion When the cumulative turn-on time of the xenon lamp exceeds...
Page 98 Select EXCHANGE STANDARD. Press numeric key 3 and then ENT key. The following display will be presented. <Standard Xe lamp lifetime setting screen> XE LAMP EXCHANGE STANDARD (1 - 2500) H _500 The standard lifetime of the Xe lamp is settable here. Press numeric key (to input 1 to 2 5 0 0) and then the ENT key.
Page 99: Before Performing Analysis
3.6 Before Performing Analysis This chapter describes the basic items to be careful about before starting analysis. WARNING Ignition of Flammable Chemicals • This instrument is not explosion-proof. In unattended operation, do not use organic solvents having an ignition point below 70 C. •...
Page 100: Selection Of Mobile Phase And Cautions On Handling
WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Safety Data Sheets (SDS).
Page 101 (b) When performing analysis with a UV detector in the short wavelength range or highly sensitive analysis with an RI detector, degassing the mobile phase before use is not enough, and the baselines may be fluctuated by the bubbles. In such a case, use degassing unit which can degas mobile phase on-line.
Page 102 Table 3-1 Reagents for Mobile Phase that may be Restricted Use is Use is Possible if Use is Possible if 10% or Reagents Unsuitable for Possible 50% or Lower Lower SUS316 Phosphoric Acetic acid Disodium phosphate Ammonium chloride acid Ammonium citrate Ammonium formate Potassium chloride Sodium...
Page 103: Characteristics Of Organic Solvents
3.6.2 Characteristics of organic solvents Characteristics of organic solvents as mobile phase for liquid chromatograph are shown in Table 3-2. Use it for reference. WARNING Ignition of Flammable Chemicals This instrument is not explosion-proof. In unattended operation, do not use organic solvents having an ignition point below 70 C.
Page 104 WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Safety Data Sheets (SDS).
Page 105 Table 3-2 Characteristics of Organic Solvents Ignition Point Vapor Specific Polarity Viscosity Refractive UV Cut Flash Boiling Density Gravity (cP20 C) Lower Upper Index off (nm) Point (C) Point (C) C (Air: 1) (Water: 1) Limit Limit Fluoroalkanes -0.25 1.25 n-Pentane 0.00 0.23...
Page 106 Notes for Using Organic Solvents as Mobile Phase When using organic solvents, be careful about UV cut off wavelength. • UV cut off wavelength Light cannot be transmitted in the range shorter than this wavelength. For example: Cut off wavelength of chloroform is 245 nm. Chloroform cannot be used in the range shorter than 245 nm (e.g.
Page 107: Cautions On Static Electricity
3.6.3 Cautions on static electricity WARNING Ignition of Flammable Chemicals by Static Electricity When using flammable chemicals, be careful about possible ignition due to static electricity. To prevent the build-up of static electricity, use a conductive container for waste solution and provide proper grounding connection to Since flammable organic solvents are used for the high speed liquid chromatograph, be careful about heat and fire.
Page 108: Preparation
3.7 Preparation NOTE: When using an ultrasonic cleaner etc., follow the instruction manual for it. 3.7.1 Degassing and removing dust from mobile phase Degas mobile phase before use without fail. Oxygen gas and nitrogen gas contained in mobile phase cause the following when used under high pressure. (a) Change in quality of mobile phase sample (b) Loss of column efficiency caused by bubbles (c) Noise of detector caused by bubbles...
Page 109 Remove cap. Mobile phase container Ultrasonic cleaner (a) Set mobile phase container well stirred into ultrasonic cleaner. * When using a mixed mobile phase, stir it completely by using a stirrer, or else low repeatability or baseline drift may be caused. NOTE: Degas mobile phase of organic solvent by using ultrasonic cleaner with water.
Page 110 Devices to be prepared • Ultrasonic cleaner (Put water in the bath without fail.) • Aspirator with rubber stopper which fits the mouth of mobile phase container Rubber stopper should fit the mouth of container. Ultrasonic cleaner Mobile phase container Aspirator (a) Set mobile phase container in ultrasonic cleaner after sufficient stirring.
Page 111: Removing Dust From Mobile Phase
(g) Shut off the city water. (h) Turn off the power of ultrasonic cleaner. Take mobile phase container out of ultrasonic cleaner, wipe the water from the container, and set it to liquid chromatograph. NOTE: Bubble generation depends on constitution of mobile phase.
Page 112: Sample Pretreatment
3.7.4 Sample pretreatment Filter samples without fail if they may contain fine dust. Dust can clog column and deteriorate it. Remove foreign matter from samples without fail. Foreign matter can lower the reliability of data, e.g. generating abnormal peaks etc. (a) Example of filtering samples Dust in sample can be removed easily as follows.
Page 113 (b) Example of Removing foreign matters in sample For example, when analysis is performed with Reversed Phase Column (e.g. ODS Column), foreign matters can be removed as follows. Take sample in Syringe, attach Normal Phase cartridge, and perform filtering. See the figure left. NOTE: There are various ways for removing foreign matters in sample.
Page 114: Maintenance And Troubleshooting
4. MAINTENANCE AND TROUBLESHOOTING 4.1 Operational Check Check the operation when the instrument has been installed. Prepare the instrument for operation as instructed in this manual. Turn on the power switch of the detector. Check that measurement conditions (time constant, output range, etc.) can be properly set.
Page 115: Wavelength Accuracy Check By Using Hg Lamp
4.2.2 Wavelength accuracy check by using Hg lamp Check the wavelength accuracy by using the bright line at 254 nm of the Hg lamp (see section 3.3.6). “GOOD” will appear on the display when the wavelength error is within 3 nm, or “FAIL” will appear when the error exceeds 3 nm.
Page 116 Primaide 1440 FL Flow cell D-2500 Chromato-data processor Detector Distilled water Waste Primaide 1110 solution Pump Fig. 4-1 Tubing Diagram Measurement of Raman Spectrum of Water Set the flow cell unit in place, measure the Raman spectrum of water under the conditions given below, and record the results (see sections 3.4.2, 3.4.3, 3.4.5,3.4.6 and...
Page 117 <Wavelength setting screen (Ex indicated)> (200 - 850.0) Press numeric keys 3 5 0 and then the ENT key. (ii) An emission (Em) wavelength will not be set here. Leave the present setting as it is. <Wavelength setting screen (Em indicated)> （250 - 900.0）...
Page 118 <Utility setting screen> UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, PMT VOLT=4, OTHERS=5) Press numeric key 4 and then the ENT key. The pmt voltage setting screen appears. <Pmt voltage setting screen> PMT VOLTAGE (SUPER HIGH=1, HIGH=2, MID=3, LOW=4, SUPER LOW=5) Press numeric key 3 and then the ENT key.
Page 119 The 1 monitor screen returns. (d) Setting of spectrum measurement: Press the SPECT key. The scan mode setting screen appears. <Scan mode setting screen> SPECTRUM MODE (FL (Ex)=1, FL (Em)=2) Press numeric key 2 and then the ENT key. (ii) Set a scanning range.
Page 120 acquisition begins. <Scan monitor screen (spectrum acquisition under way)> SCANNING SPECTRUM NO.: 1 MODE: FL (Em) Ex: 350 nm Em: *** nm When the recording of spectral data finishes, the monitor screen returns automatically. (e) Setting of recorder full scale range, speed and memory No.: Press the RECORD key and the recorder setting screen appears.
Page 121 Press numeric key 2 and then the ENT key. (vi) The 1 monitor screen returns. (vii) Press the RECORD key. The recorder setting screen reappears. <Recorder setting screen> RECORD (RCD RANGE=1, RCD SPEED=2, SPECT RCD=3) Press numeric key 3 and then the ENT key. (viii) The output data spectrum No.
Page 122 (xi) The spectrum output screen appears, and spectrum output begins. <Spectrum output screen> RCD NO. SPEED MODE 1000.0 (xii) When the spectrum output is completed, the 1 monitor screen returns automatically. NOTE: Set the following conditions for the D-2500 chromato-data processor. CHART SPEED : 60 mm/min NOTE: If the detector and data processor are...
Page 123 NOTE: When the instrument is combined with Primaide System Manager/ChromAssist Data Station, the Raman signal intensity can be obtained automatically by means of the furnished maintenance software. For details refer to the instruction manual on the maintenance software. Measurement of Noise With the excitation wavelength left at 350 nm, set the emission wavelength at 397 nm (other conditions may be the same as in preceding subsection (2)), and check the FL indication.
Page 124 S/N Ratio Calculation for Raman Spectrum of Water Perform calculation according to the S and N obtained in the preceding subsections (3) and (5). (a) Excitation spectrum bandwidth: 15 nm S/N ratio = S/N (baseline method, S/N ratio ≥ 700) S/N ratio = S/N (tangent method, S/N ratio ≥...
Page 125 substance may mix in with the distilled water. (ii) Check the position and useful life of the xenon lamp. (b) When peak separation is not good Check the distilled water. * Distilled water should be used soon after its purification. If left for a long time in a container made of resin or the like, fluorescent substance may mix in with the distilled water.
Page 126 Create a time program as indicated below for measuring the Raman spectrum of water. TIME BASE (A/Z=1, HOLD=2) NOTE: The above time program shows an example where the minimum FL value was obtained at 380 nm and the maximum at 400 nm. For the top Em of the program, set a wavelength that includes the wavelengths where the maximum and minimum FL values were...
Page 127 Read out the value corresponding to “S” from the spectrum obtained with the time program. (tangent method) (baseline method) Baseline Tangent Fig. 4-4 Calculate the Raman Peak of Water When using the D-2500 chromato-data processor, calculation can be made using the length (L in mm) of S on the chart.
Page 128: Wavelength Accuracy Check And Calibration
Raman spectrum of Baseline (emission water wavelength 397 nm) S (tangent method) 15 minutes (baseline method) Drift: Baseline D/A x 100  3%/15min Max. 450 nm wavelength Emission wavelengths Conditions: Excitation(Ex) wavelength ..... 350 nm Response ....... 2 seconds Flow cell ......12 L Distilled water in cell Room temperature kept constant Fig.
Page 129 (b) Check of wavelength accuracy Check the wavelength accuracy by using the bright line at 254 nm of the Hg lamp (see section 4.4.4 (6)). “GOOD” will be indicated if the wavelength error is within 3 nm, or “FAIL” will be indicated if the error exceeds 3 nm.
Page 130 Wavelength calibration is conducted by entering a new offset value (value to which the deviation is added). Press numeric keys (from 1 to 2 0) and then the ENT key. Input range for offset value: 1 to 20 Calculation of new offset value: New offset value = present offset value –...
Page 131: Leak Sensor Check
(iii) The 1 monitor screen appears. 4.2.5 Leak sensor check Operational Check of Leak Sensor (a) Drip water onto the leak sensor. Drip water Leak sensor Fig. 4-6 Leak Sensor Check (b) Confirm that a leak error is detected. Specification: A leak error must be detected. NOTE: Observe the following precautions before using the leak sensor which detects a liquid leak.
Page 132 Cleaning of Liquid Leak Sensor <Item to be prepared> • Hexagonal wrench (P/N: N315003, size: B2.5) (a) Separate the liquid leak sensor from the drain tray by removing the liquid leak sensor fastening screw with the furnished hexagonal wrench. (b) Wipe off the water adhering to the liquid leak sensor and drain tray, and then fasten the sensor to the drain tray again.
Page 133: Drain Tray Check
4.2.6 Drain tray check WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Safety Data Sheets (SDS).
Page 134: Periodic Checks
4.3 Periodic Checks Frequency of Check Item Check Procedure Remarks Check Drain tray Daily Check the drain tray, and wash it when needed. Check that “Xe” is indicated on LEDs. Lighting of lamp Daily Liquid leakage Daily Visually check that liquid is not leaking from the mobile phase bottle, tubing and waste bottle.
Page 135: Lamp Logbook Check
NOTE: If “FAIL” is indicated, wavelength calibration is required. Refer to section 4.2.4 (2) for the calibration. 4.3.3 Lamp logbook check The cumulative turn-on time, number of lightings, and last replacement date for the Xe and Hg lamps can be checked via the GLP function (see 3.3).
Page 136: Flow Cell Unit Checks
4.4 Flow Cell Unit Checks WARNING Ignition of Flammable Chemicals • This instrument is not explosion-proof. In unattended operation, do not use organic solvents having an ignition point below 70 C. • Beware of ignition hazard when using flammable chemicals such as organic solvents. Do not bring a heat or flame source near the instrument.
Page 137: Check And Washing Of Flow Cell
4.4.1 Check and washing of flow cell If the inside of the flow cell is contaminated, it must be cleaned. Prepare the following items for the cleaning. • Glass syringe with capacity of about 10 mL • Wash fluid Flow cell unit (P/N 893-5350) Retaining screw Fig.
Page 138 (Fig. 5-7). NOTE: This flow cell unit (P/N 890-2967) uses a part similar to the one used in the Primaide 1440 FL Detector. Be careful not to mount the part of the flow cell unit to the detector and vice versa.
Page 139: Disassembly And Cleaning Of Flow Cell
From the pump Fig. 4-10 Removing Air Bubbles NOTE: Applying too much pressure may damage the flow cell. Set the pressure limiter of the pump at 1.0 MPa max. before removing air bubbles. 4.4.2 Disassembly and cleaning of flow cell Disassembly of Flow Cell If contamination is not removed by just flushing the interior of the flow cell, then disassemble and clean the cell in the...
Page 140 (c) Remove the cell clamp. (d) Loosen setscrews. (e) Take out the flow cell. Cell window Flow cell clamp Flow cell Retaining screw 1 Retaining screw 2 Fig. 4-12 Disassembly of Flow Cell Unit Washing of Flow Cell (a) Wash the flow cell in running water. If the contamination cannot be removed with running water, then use an ultrasonic cleaner.
Page 141 Assembly of Flow Cell (a) Assemble the flow cell into the cell holder in the orientation shown in Fig. 4-13 and fix it with the cell clamp. (b) Tighten the upper and lower retaining screws 1 and 2. View from top Enlarged view of flow cell Polished surface (Instrument front)
Page 142: Leakage From The Flow Cell
4.4.3 Leakage from the flow cell It is important to check for any liquid leakage from the flow cell unit prior to analysis. If a leak is found, stop the pump immediately and remove the flow cell unit. Take the following procedure to remedy the leak.
Page 143: Cautions On Storage Of The Flow Cell
4.4.4 Cautions on storage of the flow cell If the flow cell will be left unused for more than a few days, clean the flow cell interior thoroughly by pumping distilled water or alcohol through it and then store it in a safe place. If the period of nonuse is less than a few days, the inside of the cell may be filled completely with a solvent such as ethanol or acetonitrile and then stored.
Page 144: Troubleshooting
4.5 Troubleshooting Symptom Cause Judgment/Check Remedy Self-diagnosis The power cord plug is Visual check Plug in the power cord (initialization) is not not securely plugged in. securely. performed when the The fuse is blown. Check the fuse for Replace the fuse with a POWER switch is continuity.
Page 145 Symptom Cause Judgment/Check Remedy ⎯ Excessive drift The warm-up period is Wait until the instrument not sufficient. becomes stable (at least 10 minutes). Mobile phase is leaking Check each fitting. Retighten the offending from a fitting. fitting. An impurity is eluting Stop feeding liquid Wait until elution is from the column.
Page 146: Error Messages
1) Press CL key, and 1st monitor PRESS “CL” KEY TO screen returns. CLEAR MESSAGE. 2) Contact your nearest service office of Hitachi High-Tech Science sales representative. RAM ERROR RAM is faulty. 1) Press CL key, and 1st monitor PRESS “CL” KEY TO screen returns.
Page 147 Message Description Remedy LAMP OFF BY Lamp has been turned off due 1) Release the key lock if it has EXTERNAL ERROR to an external error. Busy been activated. PRESS “CL” KEY TO status is assumed. 2) Press CL key and light up the TURN ON.
Page 148 1) Cannot be released by key ERROR ADC initialization. operation. 2) Turn on power again. 3) Contact your nearest service office of Hitachi High-Tech Science sales representative. ADC ERROR Data transfer from ADC has 1) Cannot be released by key been interrupted.
Page 149: Spare Parts
5. SPARE PARTS 5.1 Replacement Parts and Consumables Table 5-1 lists the replacement parts and consumables for this instrument. It is suggested that a suitable quantity of each item be stocked in the laboratory to minimize down time. For many of these items (e.g.
Page 150 Part Number Part Name Estimated Service Life Remarks Example use: 8DD-9109 Ferrule (SUS) 9600 hours/5 years Connecting pipe Example use 893-0825 Fitting 9600 hours/5 years Column outlet connection For outer diameter : 1.57 mm 5 - 2...
Page 151: Lamp Replacement
5.2 Lamp Replacement 5.2.1 Xe lamp replacement WARNING Injury due to Xenon Lamp Explosion Before removing the xenon lamp for replacement, turn off the xenon lamp (turn off power to the instrument) and then wait for at least one hour until the xenon lamp becomes sufficiently cool to reduce its internal pressure the normal safety level.
Page 152 <Utility setting screen> UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, PMT VOLT=4, OTHERS=5) Press numeric key 5 and then the ENT key. (b) The others setting screen appears. <Others setting screen> OTHERS (Em BANDWIDTH=1, ERROR OUT=2, LEAK SENSOR=3, LAMP=4) Press numeric key 4 and then the ENT key. (c) The Xe lamp setting screen appears.
Page 153 Replacement of the Xe Lamp WARNING Electric Shock due to Contact with Inside of Instrument The xenon lamp is supplied with high voltage of 30 kV, which could cause an electric shock to result in serious or fatal injury. Before removing the light source cover for replacement of the light source lamp, be sure to turn off the power switch.
Page 154 (c) Put on safety goggles for the subsequent steps. (d) Detach the connector between lamp house and main body, and loosen the lamp house retaining screw. Connecter Lamp house Retaining screw Grip Fig. 5-2 Removal of Connector and Retaining Screw (e) Lift the grip of the lamp house lightly and pull it toward you, then detach the lamp house from the main body.
Page 155 Anode cable Lamp igniter Cathode cable Xenon lamp Grip Fig. 5-4 Lamp House after Removal Removal of old xenon lamp WARNING Injury due to Xenon Lamp Explosion (at disposal) The xenon lamp is filled with high-pressure gas (approx. 1 MPa at room temperature, approx. 4 MPa under operating condition), and this high-pressure gas still remains in the xenon lamp after it is demounted for replacement.
Page 156 Loosen the anode nut of the lamp and detach the anode terminal of the lamp (marked +) from the metal fixture on the ceramic plate (Fig. 5-5). Be careful not to touch the lamp bulb. Note that a thin metal wire is attached near the center of the bulb, which facilitates ignition of the lamp.
Page 157 (h) Mounting of new xenon lamp WARNING Injury due to Xenon Lamp Explosion (at mounting) Do not touch the quartz glass part of the xenon lamp with bare hands. If the quartz glass part of the xenon lamp is contaminated with dust or fingerprints, wipe it using a gauze sheet or absorbent cotton cloth slightly moistened with high-quality alcohol.
Page 158 Attach a new xenon lamp in place. Attach the cathode lead plate to the threaded part of the cathode, and secure the lead plate with the cathode nut (Fig. 5-6). Mount the lamp so that the protrusion on the bulb faces the instrument front panel (Fig.
Page 159 Lamp protrusion (faces instrument front panel) Metal wire Fig. 5-7 Orientation of Lamp Bulb Protrusion As shown in Fig. 5-6, put the anode terminal (marked “+”) of the lamp into the metal fixture on the ceramic plate. Then, using the anode nut, mount the lamp so that the protrusion on the bulb is positioned as shown in Fig.
Page 160 (k) When installation of the lamp house is finished, close the light source cover and turn ON the power (check that the lamp comes on). Now proceed to positional adjustment of the Xe lamp. Positional Adjustment of Xe Lamp CAUTION Direct Gazing at Illuminating Xenon Lamp Could Cause Eye Damage The xenon lamp radiates intense ultraviolet light when it is...
Page 161 Lamp position adjustment screw cover Cover fastening screw Fig. 5-8 Lamp Position Adjustment Screw Cover HORIZONTAL FOCUS VERTICAL Fig. 5-9 Lamp Positional Adjustment (a) Coarse adjustment Set the excitation (Ex) wavelength at 550 nm, and make the adjustment while observing the image of the light beam.
Page 162 Turn ON the power switch, and the 1 monitor screen appears. <1 monitor screen> TIME PROG LAMP (ii) In the present status, pull out the flow cell unit (see Fig. 5-2). “****” will be indicated at FL on the 1 monitor screen.
Page 163 (iii) Press the WL key and the wavelength setting screen appears. Set an excitation (Ex) wavelength. <Wavelength setting screen (Ex indicated)> (200 - 850.0) Press numeric keys 5 5 0 and then the ENT key. (iv) Emission (Em) wavelength will not be set here. Leave the present setting as it is.
Page 164 Observe excitation beam on paper strip Fig. 5-10 Observation of Ex Beam (b) Fine adjustment Following the coarse adjustment, set the excitation (Ex) wavelength at 350 nm make a fine adjustment while observing the data. Take the procedure given below (refer to sections 3.1.1, 3.1.4). Re-mount the flow cell unit.
Page 165: Hg Lamp Replacement
<Wavelength setting screen (Em indicated)> (250 - 900.0) Press the ENT key. (iv) The 1 monitor screen appears. Press  or  key and the 2 monitor screen appears. <2 monitor screen> MONITOR (Ex) (Em) LAMP ******* ******* (vi) In the present status, turn the FOCUS, HORIZONTAL and VERTICAL adjusting screws gradually in a repetitive manner while watching the MONITOR (Ex) value on the screen until this...
Page 166 Retaining screws Fig. 5-11 Removal of Light Source Cover (c) Loosen the screw retaining the mercury lamp cover (Fig. 5-12). Retaining screw Hg lamp cover Fig. 5-12 Removal of Hg Lamp Cover (d) Pull the Hg lamp cover straight out, and the Hg lamp will be seen attached at the right side interior of the main body (Fig.
Page 167 (e) Detach the connector between the Hg lamp and main body, loosen two retaining screws and detach the Hg lamp. Hg lamp Close-up view Connector Retaining screws Fig. 5-13 Removal of Hg Lamp Attach a new Hg lamp in place. Fasten the lamp with the two retaining screws, then connect the connector with the main body.
Page 168: Fuse Replacement
5.3 Fuse Replacement WARNING Electric Shock due to Contact with Inside of Instrument When replacing the fuse with a new one, be careful not to receive an electric shock. To prevent this, be sure turn off the power switch and unplug the power cord before proceeding to fuse replacement.
Page 169: Index
6. INDEX Assembling ......................... 2-9 AUTO ZERO IN ........................2-2 A/Z (Auto zero) ..................... 2-4, 3-6, 4-1 Baseline..........................4-11 CL (Clear) ........................... 2-5 Checking the Contents ..................APPENDIX1-6 Consumables........................5-1 DEL (Delete) ........................ 2-5, 3-5 Drift Measurement ......................4-15 E-Line ........................2-2, 3-46 ENT (Enter) ........................
Page 170 Fluorometry/An Example of a Fluorescence Spectrum ............. 2-14 Fluorometry/Features of Light Source ................2-17 Fluorometry/Notes on Fluorescence Analysis ..............2-11 Fluorometry/Principle of Fluorometry .................. 2-6 Fluorometry/Principle of Operation ................... 2-16 Fluorometry/Second-order and Third-order Radiation ............2-14 Fluorometry/Temperature Dependency of Fluorescence Intensity ........2-15 Frequency ......................
Page 171 NOISE/Measurement ......................4-10 NOISE/Noise Calculation ....................4-10 OFFSET ..........................3-8 Operation ..........................3-1 Organic Solvents ......................3-56 Performance/Check ......................4-1 Power/Turning On the Power ....................2-1 Power/Shutdown Procedure ....................3-7 Power Supply/voltage ..................APPENDIX1-2 PROCESSOR (option) ......................2-3 PROG ..........................2-4 Power consumption ......................
Page 172 TIME CONSTANT ......................3-8 TIME PROGRAM/Setting of Time Program ..............3-10 Troubleshooting ........................ 4-31 Tubing ......................APPENDIX1-12 UI Pad (option) ........................2-1 UTILTY (Utility) ........................2-4 VERTICAL ........................5-12 WL (Wavelength) ........................ 2-4 Wavelength/Accuracy Checking by using Hg Lamp ........... 4-2, 4-21 Wavelength/Calibration of Wavelength Accuracy ..............
Page 173: Appendix
If relocation of the instrument becomes necessary after delivery, please be sure to consult your dealer or nearest Hitachi High- Tech Science authorized maintenance service agent in order to avoid possible trouble involved in relocation.
Page 174: Installation Conditions
2. Installation Conditions Confirm that the following requirements are satisfied before installing the instrument. Power Supply Power supply voltage : 100 to 240 V AC Fluctuation should be within 10% of the rated voltage. Frequency : 50 or 60 Hz Fluctuation should be within 0.5 Hz of the rated frequency.
Page 175 WARNING Electric shock due to improper grounding! This instrument is designed in conformity with the specifications of Class I in Annex H of the IEC 61010-1 (International Electrotechnical Commission Standards) - Issue 1. To prevent an electric shock hazard, provide a proper grounding connection.
Page 176 (b) Grounding Connection when grounded 3P power outlet not available 2P power outlet (15A) Grounded 3P table tap Power cord (standard Primaide1440 accessory) Ground fluorescence detector terminal 750 mm or Grounding more resistance: underground Connector 100  or less Ground wire (green) Rear panel Screw diameter : M4 or larger...
Page 177: Installation Place
In an example of a total system arrangement, Primaide organizer, Primaide 1110 pump, Primaide 1210 autosampler, Primaide 1310 column oven, and Primaide 1440 fluorescence detector, stacked in two blocks, are included. Check and prepare an installation place satisfying the space requirements for your actual system and OA equipment to be used in combination.
Page 178: Checking The Contents
Other Conditions (a) Avoid placing the instrument near a window where it would be exposed to direct sunlight. Exposure to sunlight may cause a degraded performance and/or discoloration of the painted surfaces. (b) Protect the instrument from drafts. (c) Do not allow the instrument to be exposed to any strong vibration or shock.
Page 179: Assembling
6. Assembling 6.1 Removal of Transport Screws There are three screws for transport installed on the bottom of the instrument. Remove the transport screws with a phillips screwdriver. Transport screw 3. (For lamp house fixing) Transport screw 1. Transport screw 2. (For the instrument (For the instrument fixing)
Page 180 Anode nut Xenon lamp Lamp house Cathode nut Appended Fig. 1-4 Mounting Xenon Lamp Install the xenon lamp in the lamp house. And mount it to the instrument (see ⑧ to ⑪ in section 5.2.1 (2).) Adjust the position of the xenon lamp. (see section 5.2.1 (3).) NOTE: After removing the transport screws, please store them.
Page 181 Power Supply The Primaide1000 Series system is provided with a organizer which is capable of connecting one pump, one autosampler, and one detector. The column oven has its own power cord. In an instance where provision of a single organizer is insufficient for the use of two detectors, use an AC adapter suitable for each instrument.
Page 182 （2）Isocratic System/Low-pressure Gradient System (stacked in two blocks) AC adapter (option) Primaide 1410/1430 ① UV/DAD detector Primaide 1440 Fluorescence Detector To AC power supply Primaide 1310 Column Oven Primaide 1000 Organizer Primaide 1210 Autosampler Primaide1110 Pump Appended Fig. 1-5 Power Cable Connection Diagram...
Page 183 6.3 Wiring Arrangement In the Primaide1000 series, it is required to connect the e-Line cable between the instruments. On the left rear of each instrument, insert the e-Line cable into the e-Line connector. e-Line connector Rear side of the instrument Appended Fig.1-6 e-Line Connector on the Rear of Instrument...
Page 184 Isocratic System/Low-Pressure Gradient System (stacked in one block) Primaide Organizer Primaide1410/1430 UV/DAD Detector e-Line cable Primaide1310 Column Oven e-Line cable Primaide1210 Autosampler Interface Control Board e-Line cable Primaide1110 Pump APPENDIX 1 - 12...
Page 185 Isocratic System/Low-pressure Gradient System (stacked in two blocks) Primaide1410/1430 e-Line cable ① UV/DAD Detector e-Line cable ② Primaide1440 Fluorescence Detector e-Line cable ③ Primaide1310 Column Oven Primaide Organizer Primaide1210 Autosampler Primaide 1110 Pump Interface Control Board Table 1-2 Cables to be Used e-Line cable （50 cm）...
Page 186 System Tubing In the Primaide1000 series, the inlet tube up to the pump and drain tube are fastened to the right/left side face of each unit with tube clamps. And the tubes are connected from the pump to the autosampler, column and detector through the central hole of each module unit.
Page 187 (2) Isocratic System(stacked in two blocks) Primaide 1440 Fluorescence detector Detector cell Mobile phase Wash fluid Primaide 1310 Column oven Column Primaide 1000 Organizer Primaide 1210 Autosampler Primaide 1110 Pump Degassing device Drain Drain Appended Fig. 1-8 Isocratic System Connect the inlet tube of the mobile-phase container to the IN port of the degassing device.
Page 188 Low-Pressure Gradient System (stacked in one block) Connect the inlet tube of mobile phase to the IN port of the degassing device. Connect the OUT port of the degassing device to the IN port of the proportioning valve. Connect the OUT port of the proportioning valve to the four-way joint.
Page 189 (4) Low-pressure Gradient System Primaide 1440 Fluorescence detector Detector cell Mobile phase Wash fluid Primaide 1310 Column oven Mixer Column Primaide 1000 Organizer Primaide 1210 Primaide 1110 Autosampler Pump Four-way joint Degassing Drain Proportioning valve device Appended Fig. 1-9 Piping Arrangement for Low-pressure...
Page 190 Drain Tubing When setting up eluent / waste tubings as below, follow the steps ① Place CLAMP SHEET (8DD-1095) as shown. ② Decide position of clamp (8DD-1920) and clamp (8DD- 1921). Use the cutout of CLAMP SHEET. ③ Degrease the surface by ethanol etc… ④...
Page 191 (b) stacked in two blocks Primaide 1440 Fluorescence detector Primaide 1310 Column oven Primaide Organizer Primaide 1210 Primaide 1110 Autosampler Pump Drain Appended Fig. 1-10 Tubing Diagram for Drain (when stacking module units in two blocks) APPENDIX 1 - 19...
Page 192 6.6 Fastening between Component Units CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over. When installing the instrument, provide a proper means for fastening between module units. On the rear of each module unit, a cabling cover is attached. The adjacent models are fastened with each other by attaching the fastening plate between the cabling covers.
Page 193: Appendix 2. Description On Contact Signal Communication
APPENDIX 2. Description on Contact Signal Communication 1. Outline The following two types of contact signals are used in the Primaide1000 series. Contact signals (START, ERROR, BUSY) entering the e-Line connector. These are contact signals having input/output functions that are used in common for each unit. These signals are respectively formed from the START (IN/OUT), ERROR (IN/OUT), and BUSY (IN/OUT) lines.
Page 194 Connection with L-2000 Series Use the e-DIO cable (8DD-0584)for connection. ERROR START STOP e-Line connector To L-2000 To Primaide1000 series series instrument instrument e-Line connector BUSY 3-pin connector e-DIO cable e-DIO cable (8DD-0584) (8DD-0584) APPENDIX 2 - 2...
Page 195 Connection with Model D-2500 Use the e-DIO cable (8DD-0585) for connection. D-2500 START START EXTERNAL To Primaide1000 series instrument BUSY e-Line BUSY connector Connect the START L and G terminals of the e-DIO cable (8DD-0585) to the EXTERNAL-COM terminal of the Model D-2500.
Page 196: Individual Contacts Of Each Unit
3. Individual Contacts of Each Unit Contact Signal Input Terminals These are contact signal input terminals for control using contact signals from an external switch, relay etc. Any of the signals is activated by shorting the terminal for 0.1 second or longer. The input circuit is shown in Fig. 3. Contact signal Output Terminals These are contact signal input terminals for control using contact signals of an external unit.
Page 197 +5 V 320  Max. 10 mA Primaide1000 series unit External unit Activated upon shorting contacts of external unit. Fig. 3 Contact Signal Input Circuit 0.1 A max. 30 V max. Primaide1000 series unit External unit Fig. 4 Contact Signal Output Circuit APPENDIX 2 - 5...
Page 198: Appendix 3. Glossary
APPENDIX 3. GLOSSARY Initial screen ........After power on, the initial screen appears upon completion of initialization. Auto zero [A/Z] .......Absorbance is electrically adjusted to zero to cancel insignificant parts of data. In common analytical practice, perform auto zero adjustment immediately before or after the start of operation.
Page 199 Scan ..........Means a sequential shifting operation of monochromator wavelength for spectral measurement. Stokes law ........The law states that the wavelength of a fluorescent emission is always longer than the excitation wavelength. Time Program ........Used to adjust such measurement parameters as detection wavelength according to measurement time.
Page 200 Lamp turn-on count .......Indicates the number of times the light source lamp has been turned on. Lamp turn-on cumulative time ..Indicates a cumulative total time of lamp turn-on periods. Ex (Excitation wavelength) ....Used for exciting a sample. Recorder (RECORDER) ....Used for analog output to a recorder. Logbook.........Means the information containing records of instrument operating conditions.
Page 201: Flowpath Figures
FLOWPATH FIGURES General flowpath figures are shown below. Please select a plumbing according to your system configuration and the purpose. :Stainless-steel pipe :Teflon tube Numbers :Inside diameter. Isocratic System (stacked in one block) 1.5 TT Inlet tube Mobile Phase Washing Solution Primaide Organizer Detector cell...
Page 202 (2) Isocratic System (stacked in two blocks) Primaide 1440 FL Detector Detector cell 0.25TT Mobile Phase 0.25ST Wash Solution Primaide 1310 Column Oven 1.5 TT Column 0.33TT Primaide Organizer Primaide 1210 0.8ST Autosampler Primaide 1110 Pump 1.5 TT Degassing device...
Page 203: Low Pressure Gradient System
Low-Pressure Gradient System (stacked in one block) 1.5 TT Mobile Phase Washing Solution Inlet tube Organizer (option) Detector cell Primaide1410/1430 UV/DAD Detector 0.25 TT 0.25 ST Primaide1310 Column Oven Column 0.33 TT Primaide1210 Autosampler Injection valve Syringe valve 0.8 ST Drain valve Primaide1110 Pump...
Page 204 (4) Low-Pressure Gradient System (stacked in two blocks) Primaide 1440 FL Detector Detector cell Wash Solution Mobile Phase 0.25TT 0.25ST Primaide 1310 1.5 TT Column Oven Mixer Column Primaide 0.33TT Organizer 0.8ST Primaide 1210 Primaide 1110 Autosampler Pump Degassing 1.5 TT...

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