Erc RefractoMax524 Manual de usuario

RefractoMax524 RI Detector

Operator’s Manual

High Sensitive Refractive Index Detector

for High Performance Liquid Chromatography

Publication No. 77-5014-10

Important Notice

The information contained in this manual is subject to change without notice.

ERC Inc. (ERC) assumes no responsibility for any errors that may appear in this manual. This

manual is believed to be complete and accurate at the time of publication.

In no event shall ERC be liable for incidental or consequential damages in connection with or

arising from the use of this manual.

If the detector is used in a manner not specified by this Operator's Manual, the protection

provided by the detector may be impaired.

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” basis.

The following is a Federal Communication Commission advisory:

WARNING:

This equipment generates, uses, and can radiate radio frequency energy and if not installed and

used in accordance with the instruction manual may cause interference to radio communications.

It has been tested and found to comply with the limits for Class A computing device pursuant to

Subpart J of Part 15 of FCC rules, which are designed to provide reasonable protection against

such interference when operated in a commercial environment. Operation of this equipment in

a residential area is likely to cause interference in which case the user at his own expense will

be required to take whatever measures may be required to correct the interference.

Operating Instructions

This manual is provided to help you establish operating conditions that will make safe and

efficient use of your equipment available.

Special considerations and precautions are also described in this manual that shall appear in the

form of WARNING, CAUTION and NOTE as described below.

It is important that you operate your equipment in accordance with this manual and any

additional information that may be provided by ERC from time to time.

Alert you to potentially hazardous situations that could result in

serious injury, and how to avoid these situations.

Alert you to situations that may cause moderate injury and/or

equipment damage, and how to avoid these situations.

CAUTION

WARNING

Information to help you to achieve optimal performance from

your equipment.

The following Trademarks and Registered Trademarks are

found in this manual.

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.

To operate RefractoMax524 Refractive Index Detector properly, you are strongly recommended

to go through this Operator’s Manual. Improper use of this detector shall be dangerous and

may cause a hazardous result.

Limited Warranty Policy

ERC warrants its products against defects in materials and workmanship for the period of twelve

(12) months from the date of shipment out of its factory.

ERC will, at its option, repair or replace products that are proved to be defective.

The aforementioned warranty policy shall not be applied to defects being caused by:

(1) Improper or Inadequate maintenance, adjustment, calibration or operation by the user(s);

(2) User-supplied software, hardware, interfacing or consumable;

(3) Unauthorized modification or misuse;

(4) Operation outside of the environmental and electrical specifications for the product;

(5) Improper site preparation and maintenance; or

(6) User induced contamination or leaks.

note

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. Standard Accessories ....................................................................................... 5

2-5. Loosing the locking screws............................................................................... 5

2-6. Making a connection......................................................................................... 5

2-6-1. Power Line ................................................................................................. 5

2-6-2. Replacing Fuse .......................................................................................... 6

2-6-3. Tubing Connections.................................................................................... 7

2-6-4. Cable Connections..................................................................................... 7

2-7. Solvent Recommendations............................................................................... 8

2-8. Characteristics of commonly used mobile phase ............................................ 10

SECTION 3. FUNCTION KEYS AND DISPLAYS...............................11

3-1. Front Panel......................................................................................................11

3-2. Rear Panel ..................................................................................................... 12

3-3. Side View ....................................................................................................... 12

3-4. LCD Display (User Screens)........................................................................... 13

3-4-1. Default Screens (Start Up Screens).......................................................... 13

3-4-2. Screen Sequence..................................................................................... 13

3-4-3. Parameter Setting Screen ........................................................................ 13

3-4-3. Parameter Setting Screen ........................................................................ 14

3-4-4. Auto Set Up Information Screen............................................................... 16

3-4-5. Validation Information Screen .................................................................. 16

3-4-6. Validation Execute Screen ....................................................................... 17

3-4-7. Error Messages........................................................................................ 18

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. Cleaning................................................................................................... 21

5-2. Validation........................................................................................................ 22

5-2-1. Validation Information............................................................................... 22

5-2-2. Span Validation ........................................................................................ 23

5-2-3. Auto Set Up Execute ................................................................................ 24

SECTION 6. SHUTDOWN PROCEDURE ..........................................25

6-1. Corrosive Solvents.......................................................................................... 25

6-2. No Flow Shutdown Versus Reduced Flow Shutdown...................................... 25

6-3. Long-Term Storage......................................................................................... 25

SECTION 7. TROUBLESHOOTING ..................................................26

7-1. Introduction..................................................................................................... 26

7-2. Make sure how the detector itself is working................................................... 26

7-3. To isolate the cause of problem ...................................................................... 26

7-4. Troubleshooting (Diagnosis Chart).................................................................. 27

Appendix. Miscibility Chart of Solvents................................................................ 29

Section 1. Introduction

1-1. Principle of refractive index detection

RefractoMax524 Refractive Index Detector (called as “RefractoMax524” hereafter) is a

high-performance universal detector designed for analyses requiring the continuous monitoring

of the refractive index of a flowing liquid with respect to a reference.

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.

Snell's Law

incident beam

rrefracted beam

interfac

Optical System of RefractoMax524

[1] Tungsten lamp [2] condense lens [3] First Slit [4] Collimator Lens

[5] Second Slit [6] Flow Cell [7] Mirror [8] Null Glass [9] Photodiode

Light from a low-power, long-lifetime tungsten lamp is collimated by a lens and slit and passed

through reference and sample cells, reflected off a mirror, passed back through the optical cells,

and focused by lenses onto a pair of photo sensing diodes (photo sensor).

= =

sin

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.

[1] Light Beam [2] Sample Cell [3] Reference Cell [4] Light Axis (Ns>Nr)

[5] Light Axis (Ns=Nr) [6] Distance between …[4]&[5] at the photo sensor

[7] Photo sensor

Ns: Refractive Index of mobile phase in Sample Cell

Nr: Refractive Index of mobile phase in Reference Cell

The light shines on a pair of photodiodes, each of which gives an electrical signal; these signals

are amplified and the difference between the two signals is measured. Zero refraction should

generate a zero-volt difference in these signals. An electrically controlled mechanical linkage

allows the user to optimize the photodiodes’ outputs for zero deflection via a refractive lens in the

optical path. Additional circuitry enables the user to easily correct the signal output to electronic

zero.

Ns = Nr Ns > Nr

[1] photo sensor A [2] photo sensor B [3] light beam

When a change occurs in the refractive index of the mobile phase, the light passing through the

interface between the sample and reference cells is refracted, causing the light intensity on one

photodiode to increase and on the other to decrease. This difference gives a signal having both

amplitude and polarity; the signal is amplified to drive a chart recorder or integrator.

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 & Electrical Auto-Zero

Auto Zero Range All Refractive Index Range

Auto Zero Resolution

≤

1 (@8mV/µRIU) / 4 (@2mV/µRIU) nRIU

Offset Range 0 to 500mV (same with Integrator output sensitivity)

Offset Resolution 10mV (same with Integrator output sensitivity)

Integrator Output 0 to 1V/FS (Sensitivity: 2mV/µRIU, 8mV/µRIU)

Recorder Output 0 to 10mV/FS

Event Marker Marker out:

≥

5% of FS

Temperature Control OFF, 30 to 55

C (1

C increment): 80

C Thermal Protector

Operator Support Span Check/Validation Display

External Communication RS232C

Cell Volume 2.5µl

Maximum Flow Rate 1 ml/min (mobile phase: pure water)

Pressure Rating 50 kPa (0.5 kgf/cm

)

Internal Volume Inlet Port / Flow Cell: approx. 10µl

Flow Cell / Outlet Port: approx. 120µl

Total: approx. 130µl

Wetted Material SST316, Teflon, Quarts Glass

Power Requirement AC100 ~ 240V +/- 10%: 50-60Hz

Power Consumption 120VA maximum

Dimensions H150 x W260 x D450 (mm)

Weight 12 kgs (26 lbs)

EMC Standards EN61326-1,EN61326-2-1

Safety Standards EN61010-1

Conditions to secure safety (EN61010-1)

Indoor use

Altitude up to 2000m

Temperature 5

℃

to 40

℃

Maximum relative humidity 80% for temperatures up to 31

℃

decreasing linearly to 50% relative humidity at 40

℃

Transient over voltages according to installation category Ⅱ

Pollution Degree 2 in accordance with EC 60664

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.

Air fan (air-conditioner-cooler, heating equipment and ventilation)

Open doors or windows

Direct sunlight

Dart or dusts

Vibration source

Electro-Magnetic Wave or High Frequency

2-2. Power Requirements

RefractoMax524 requires 50-60 Hz single-phase power source capable of providing AC

100/240 +/- 10%.

Running RefractoMax524 on a voltage other than the correct

single-phase supply will void the warranty.

RefractoMax524 is designed to operate with single-phase

(phase-neutral) power ONLY.

If your facility provides only phase-phase (i.e., three-phase)

power consult ERC.

2-3. Unpacking and Inspection

This section describes in details how to install RefractoMax524. This detector is designed to

be operator installed.

Each steps of the installation site preparation must meet local

safety, electrical, and building codes. These codes take

precedence over any recommendations in these instructions,

and compliance to them is the responsibility of the customer.

RefractoMax524 weighs 12 kgs (26 lbs). Use proper lifting

techniques to avoid potential injuries.

To remove the detector from the box, hold the bottom of the

cabinet. Never attempt to lift by front panel or terminals.

RefractoMax524 is packed with a number of accessories.

Do not discard the packing material until all parts are

accounted for.

Check the detector carefully for evidence of shipping damage.

If there is any evidence of damage, any item(s) missing in the

carton or discrepancies, please notify that to the carrier

immediately and to ERC.

CAUTION

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