instruction manual - horiba...the equipment is operated in a commercial environment. this equipment...

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INSTRUCTION MANUAL INSTRUCTION MANUAL LA-930 LA-930 Laser Scattering Particle Size Laser Scattering Particle Size Distribution Analyzer Distribution Analyzer First Edition First Edition June, 2003 June, 2003 HORIBA INSTRUMENTS, INC. HORIBA INSTRUMENTS, INC. Irvine, California Irvine, California U.S.A. U.S.A.

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Page 1: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

INSTRUCTION MANUALINSTRUCTION MANUAL

LA-930LA-930Laser Scattering Particle SizeLaser Scattering Particle Size

Distribution AnalyzerDistribution Analyzer

First EditionFirst Edition

June, 2003June, 2003

HORIBA INSTRUMENTS, INC.HORIBA INSTRUMENTS, INC.Irvine, CaliforniaIrvine, California

U.S.A.U.S.A.

Page 2: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used
Page 3: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

ELECTRIC SHOCKELECTRIC SHOCKMAINTAIN GROUND TO AVOIDMAINTAIN GROUND TO AVOID

ELECTRIC SHOCK. DO NOT GROUNDELECTRIC SHOCK. DO NOT GROUNDTHE UNIT TO A GAS PIPE OR TO ANTHE UNIT TO A GAS PIPE OR TO AN

INDIRECT GROUND, SUCH ASINDIRECT GROUND, SUCH ASANOTHER PIECE OF EQUIPMENT.ANOTHER PIECE OF EQUIPMENT.

Viton and Kalrez are trademarks of E. I. Dupont de Nemours and Co.Viton and Kalrez are trademarks of E. I. Dupont de Nemours and Co.

MS-DOS is a trademark of Microsoft CorporationMS-DOS is a trademark of Microsoft CorporationMS-Windows and Windows 2000 are trademarks of Microsoft CorporationMS-Windows and Windows 2000 are trademarks of Microsoft CorporationCompaq is a trademark of Compaq Computer CorporationCompaq is a trademark of Compaq Computer CorporationProduct names mentioned here may be trademarks and/or registered trademarks of other companies.Product names mentioned here may be trademarks and/or registered trademarks of other companies.

Copyright Copyright �� 2003 by H 2003 by HORIBA INSTRUMENTS, INC.ORIBA INSTRUMENTS, INC. First edition, Ver.1.0: June, 2003 First edition, Ver.1.0: June, 2003All rights reserved.All rights reserved.

No part of this No part of this Instruction Manual Instruction Manual may be reproduced or alteredmay be reproduced or alteredin any way without written permission fromin any way without written permission fromHORIBA INSTRUMENTS, INC.HORIBA INSTRUMENTS, INC.The information contained in this The information contained in this Instruction ManualInstruction Manual is subject to is subject tochange without notice, as improvements are made in specificationschange without notice, as improvements are made in specificationsand does not represent a commitment on the part of HORIBAand does not represent a commitment on the part of HORIBAINSTRUMENTS, INC.INSTRUMENTS, INC.

!! WARNINGWARNING

WARNING LABELSWARNING LABELS

The following warning labels are used on the LA-930 hardware.The following warning labels are used on the LA-930 hardware.The label titles conform to the given definitions:The label titles conform to the given definitions:

!! WARNING:WARNING: This indicates an imminently hazardous situation which,This indicates an imminently hazardous situation which,if not avoided, may result in death or serious injury.if not avoided, may result in death or serious injury.

!! CAUTION:CAUTION: This indicates a potentially hazardous situation which,This indicates a potentially hazardous situation which,if not avoided, may result in minor or moderate injury.if not avoided, may result in minor or moderate injury.

!! CAUTIONCAUTION

Use of procedures other than those specified hereinUse of procedures other than those specified hereinmay result in hazardous radiation exposure.may result in hazardous radiation exposure.

Page 4: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

This Instruction Manual explains the operation of the LA-930.This Instruction Manual explains the operation of the LA-930.

Be sure to read this Manual before using the LA-930. Please be sure to store the Instruc-Be sure to read this Manual before using the LA-930. Please be sure to store the Instruc-tion Manual so that it is readily available whenever necessary.tion Manual so that it is readily available whenever necessary.

The information in this Instruction Manual is subject to change without notice as improve-The information in this Instruction Manual is subject to change without notice as improve-ments are made in specifications, and does not represent a commitment on the part ofments are made in specifications, and does not represent a commitment on the part ofHORIBA INSTRUMENTS, INC.HORIBA INSTRUMENTS, INC.

Horiba's Warranty and ResponsibilityHoriba's Warranty and Responsibility

The LA-930 delivered to you is covered by Horiba's warranty for a period of one (1) year.The LA-930 delivered to you is covered by Horiba's warranty for a period of one (1) year.If any malfunction attributable to our responsibility should occur during this period, neces-If any malfunction attributable to our responsibility should occur during this period, neces-sary repairs or replacement of parts shall be made free of charge by Horiba. The warrantysary repairs or replacement of parts shall be made free of charge by Horiba. The warrantydoes not cover the following:does not cover the following:

→→ Any malfunction which is attributable to improper operation of the LA-930.Any malfunction which is attributable to improper operation of the LA-930.

→→ Any malfunction which is attributable to repair or modification by any other partyAny malfunction which is attributable to repair or modification by any other partythan a Horiba-authorized dealer.than a Horiba-authorized dealer.

→→ Any malfunction which is attributable to use of the LA-930 in an improper operatingAny malfunction which is attributable to use of the LA-930 in an improper operatingenvironment.environment.

→→ Any malfunction which is attributable to an accident or mishap not involving Horiba.Any malfunction which is attributable to an accident or mishap not involving Horiba.

→→ Any malfunction which is attributable to a natural disaster.Any malfunction which is attributable to a natural disaster.

→→ None of the following parts or expendable supplies are covered by the warranty:None of the following parts or expendable supplies are covered by the warranty:

•• light sourcelight source•• fusesfuses•• cellscells•• tubestubes

In preparing this Manual, every attempt has been made to include the latest equipment changesIn preparing this Manual, every attempt has been made to include the latest equipment changesand specifications. However, please keep in mind that our equipment evolves rapidly asand specifications. However, please keep in mind that our equipment evolves rapidly asimprovements are made, and this version of the Manual may not necessarily reflect all changesimprovements are made, and this version of the Manual may not necessarily reflect all changesin product design. Horiba reserves the right to modify its products at any time without neces-in product design. Horiba reserves the right to modify its products at any time without neces-sarily including these changes in the documentation.sarily including these changes in the documentation.

Horiba is not responsible for any damage that may occur/arise from any information otherHoriba is not responsible for any damage that may occur/arise from any information otherthan that included in this document.than that included in this document.

PREFACEPREFACE

PREFACE/WARRANTYPREFACE/WARRANTY

Page 5: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

HANDLE WITH CARE: Proper Use of Your LA-930HANDLE WITH CARE: Proper Use of Your LA-930

The LA-930 analyzer contains precision optical parts, a laser light source, a high-voltage light source,The LA-930 analyzer contains precision optical parts, a laser light source, a high-voltage light source,and a delicate motor. The instrument must be handled with care to avoid damage.and a delicate motor. The instrument must be handled with care to avoid damage.

1.1. Never subject the analyzer to jolts or excessive vibration.Never subject the analyzer to jolts or excessive vibration.

2.2. Never remove any of the panels, other than those specified in this Instruction Manual. If itNever remove any of the panels, other than those specified in this Instruction Manual. If itshould become necessary to remove any panel, contact our Customer Support Center orshould become necessary to remove any panel, contact our Customer Support Center orarrange for a service engineer to be present. When removing panels, be careful to:arrange for a service engineer to be present. When removing panels, be careful to:

A.A. Never look directly at the light source.Never look directly at the light source.B.B. Never touch any of the high-voltage componentsNever touch any of the high-voltage components

(all parts marked with a high-voltage warning.)(all parts marked with a high-voltage warning.)

3.3. Never dismantle or modify any components inside the LA-930 analyzer.Never dismantle or modify any components inside the LA-930 analyzer.

4.4. After turning the power supply ON, warm up the analyzer for 30 minutes to stabilize the laserAfter turning the power supply ON, warm up the analyzer for 30 minutes to stabilize the laserlight source.light source.

5.5. When using a volatile dispersant, be careful. The dispersant may be ignited by sparks from theWhen using a volatile dispersant, be careful. The dispersant may be ignited by sparks from themotor or other components. This analyzer is not explosion-proof.motor or other components. This analyzer is not explosion-proof.

6.6. Be careful about leakage or discharge of fluids when the dispersant or sample is a dangerousBe careful about leakage or discharge of fluids when the dispersant or sample is a dangeroussubstance.substance.

7.7. Operating the LA-930 analyzer in any manner other than described in this Instruction Manual isOperating the LA-930 analyzer in any manner other than described in this Instruction Manual isprohibited because it might shorten the life of the analyzer or damage various components.prohibited because it might shorten the life of the analyzer or damage various components.Take sufficient care in handling the cell. Never handle in a way that may scar or damage theTake sufficient care in handling the cell. Never handle in a way that may scar or damage thecell surface (e.g., never leave the cell immersed in the cleaning solution or solvent; nevercell surface (e.g., never leave the cell immersed in the cleaning solution or solvent; neverclean with an abrasive cleaner or tool; never use ultrasonic cleaning.)clean with an abrasive cleaner or tool; never use ultrasonic cleaning.)

HANDLING THE LA-930HANDLING THE LA-930

Page 6: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

FDA WARNINGFDA WARNING

→→ This instrument is a Class 1 laser product complying with CFR 21, Chapter 1, Paragraph J.This instrument is a Class 1 laser product complying with CFR 21, Chapter 1, Paragraph J.

→→ The laser specifications are as follows:The laser specifications are as follows:

Laser tube:Laser tube: He-Ne laser, Model GLT2331He-Ne laser, Model GLT2331Output:Output: 1.0 mW1.0 mWWavelength:Wavelength: 632.8 nm632.8 nm

→→ Although this equipment is encased in a protective housing to prevent leakage of the laser beam,Although this equipment is encased in a protective housing to prevent leakage of the laser beam,there is a danger of exposure to laser radiation if the protective housing is removed. There is nothere is a danger of exposure to laser radiation if the protective housing is removed. There is noneed to open the protective housing during either ordinary operation or maintenance.need to open the protective housing during either ordinary operation or maintenance.

→→ This warning plate has been attached to the instrument:This warning plate has been attached to the instrument:

DANGERDANGER Laser radiation when open.Laser radiation when open.AVOID DIRECT EYE EXPOSUREAVOID DIRECT EYE EXPOSURE

→→ The instrument also has the following FDA label:The instrument also has the following FDA label:

Certification/Identification LabelCertification/Identification LabelThis product complies with 21 CFR Chapter 1 Paragraph J.This product complies with 21 CFR Chapter 1 Paragraph J.Manufacturer of record:Manufacturer of record: Horiba Instruments, Inc.Horiba Instruments, Inc.Address:Address: 17671 Armstrong Avenue, Irvine, California 9261417671 Armstrong Avenue, Irvine, California 92614Phone:Phone: 714-250-4811714-250-4811Date manufactured:Date manufactured:Model:Model:Serial Number:Serial Number:

(The address on the label may differ depending upon the location.)(The address on the label may differ depending upon the location.)

FCC WARNINGFCC WARNING

This equipment has been tested and found to comply with the limits for a ClassThis equipment has been tested and found to comply with the limits for a ClassA digital device, pursuant to Part 15 of the FCC rules. These limits areA digital device, pursuant to Part 15 of the FCC rules. These limits aredesigned to provide reasonable protection against harmful interference whendesigned to provide reasonable protection against harmful interference whenthe equipment is operated in a commercial environment. This equipmentthe equipment is operated in a commercial environment. This equipmentgenerates, uses, and radiates radio frequency energy and, if not installed andgenerates, uses, and radiates radio frequency energy and, if not installed andused in accordance with the instruction manual, may cause harmfulused in accordance with the instruction manual, may cause harmfulinterference to radio communications. Operation of this equipment in ainterference to radio communications. Operation of this equipment in aresidential area is likely to cause harmful interference in which case the userresidential area is likely to cause harmful interference in which case the userwill be required to correct the interference at his own expense.will be required to correct the interference at his own expense.

HANDLE WITH CARE: FDA & FCC Regulations Require Proper Labeling.HANDLE WITH CARE: FDA & FCC Regulations Require Proper Labeling.

FCC & FDA REGULATIONSFCC & FDA REGULATIONS

Page 7: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

*1*1*2*2*3*3

Certification/identification LabelCertification/identification LabelThis product complies with 21 CFR Chapter 1 Subchapter J.This product complies with 21 CFR Chapter 1 Subchapter J.Manufacturer of record:Manufacturer of record: Horiba Instruments, Inc.Horiba Instruments, Inc.Address:Address: 17671 Armstrong Avenue, Irvine, California 9261417671 Armstrong Avenue, Irvine, California 92614Phone:Phone: 714-250-4811714-250-4811Date Manufactured:Date Manufactured:Model:Model:Serial Number:Serial Number:

THIS EQUIPMENT COMPLIES WITH THETHIS EQUIPMENT COMPLIES WITH THEREQUIREMENTS IN PART 15 OF FCC RULES FORREQUIREMENTS IN PART 15 OF FCC RULES FORA CLASS A COMPUTING DEVICE. OPERATIONA CLASS A COMPUTING DEVICE. OPERATIONOF THIS EQUIPMENT IN A RESIDENTIAL AREAOF THIS EQUIPMENT IN A RESIDENTIAL AREAMAY CAUSE UNACCEPTABLE INTERFERENCEMAY CAUSE UNACCEPTABLE INTERFERENCETO RADIO AND TV RECEPTION REQUIRING THETO RADIO AND TV RECEPTION REQUIRING THEOPERATOR TO TAKE WHATEVER STEPS AREOPERATOR TO TAKE WHATEVER STEPS ARENECESSARY TO CORRECT THE INTERFERENCE.NECESSARY TO CORRECT THE INTERFERENCE.

FCC & FDA REGULATIONSFCC & FDA REGULATIONS

DANGERDANGER-Laser radiation when open.-Laser radiation when open.AVOID DIRECT EYE EXPOSURE.AVOID DIRECT EYE EXPOSURE.

FCC LabelFCC Label

*1:*1: MM. DD. YYYYMM. DD. YYYY*2:*2: LA-930LA-930*3:*3: 10-digit numerals10-digit numerals

FCC LabelFCC Label

Page 8: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

INSTALLATION ENVIRONMENTINSTALLATION ENVIRONMENT

This product is designed for the following environment:This product is designed for the following environment:

→→ Installation Categories II Installation Categories II→→ Pollution degree 2 Pollution degree 2

LIMITATION OF LIABILITY FOR DAMAGESLIMITATION OF LIABILITY FOR DAMAGES

HORIBA will not accept responsibility for damage or malfunction that may HORIBA will not accept responsibility for damage or malfunction that may occur as a result ofoccur as a result ofoperation or situation not recommended in this operation or situation not recommended in this manual. HORIBA shall not be liable for Customer’smanual. HORIBA shall not be liable for Customer’sincidental, incidental, consequential or special damages, or for lost profits or business consequential or special damages, or for lost profits or business interruption losses, ininterruption losses, inconnection with the operation of the Manufactured connection with the operation of the Manufactured Parts, CPU hardware, disk drives or Software.Parts, CPU hardware, disk drives or Software.

Page 9: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

CONTENTSCONTENTS

PREFACEPREFACE

HANDLE WITH CARE:HANDLE WITH CARE: Proper Use of Your LA-930Proper Use of Your LA-930

HANDLE WITH CARE:HANDLE WITH CARE: FDA & FCC Regulations Require Proper LabelingFDA & FCC Regulations Require Proper Labeling

Section ASection A SETTING UP THE ANALYZER UNITSETTING UP THE ANALYZER UNIT

Section BSection B SOFTWARESOFTWARE

Chapter OneChapter One OVERVIEWOVERVIEW

1.11.1 OverviewOverview .................................................................................................................................................................................................................................. 331.21.2 ConfigurationConfiguration........................................................................................................................................................................................................................ 44

Chapter TwoChapter Two NAMES AND FUNCTIONSNAMES AND FUNCTIONS

2.12.1 Front and Top Views of Main UnitFront and Top Views of Main Unit ........................................................................................................................................................ 772.22.2 Right Side View of Main UnitRight Side View of Main Unit ........................................................................................................................................................................ 882.32.3 Rear Panel of Main UnitRear Panel of Main Unit ........................................................................................................................................................................................ 992.42.4 Sample ChamberSample Chamber ........................................................................................................................................................................................................ 1010

Chapter ThreeChapter Three MAINTENANCEMAINTENANCE

3.13.1 Daily CareDaily Care ............................................................................................................................................................................................................................ 13133.23.2 Cleaning the CellCleaning the Cell.......................................................................................................................................................................................................... 14143.33.3 Replacing the FusesReplacing the Fuses ................................................................................................................................................................................................ 15153.43.4 StorageStorage .................................................................................................................................................................................................................................... 1616

APPENDIXAPPENDIX

A.A. SpecificationsSpecifications ......................................................................................................................................................................................................APP-3APP-3BB Principles of MeasurementPrinciples of Measurement ................................................................................................................................................................APP-4APP-4C.C. Principles of the LA-930 Optical SystemPrinciples of the LA-930 Optical System......................................................................................................................APP-9APP-9D.D. Spare Parts & OptionsSpare Parts & Options ......................................................................................................................................................................APP-12APP-12E.E. LA-930 RS-232C SpecificationsLA-930 RS-232C Specifications ........................................................................................................................................APP-13APP-13F.F. List of Refractive IndicesList of Refractive Indices..................................................................................................................................................................APP-14APP-14G.G. Sampling & DispersionSampling & Dispersion ......................................................................................................................................................................APP-18APP-18

Page 10: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used
Page 11: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

Chapter OneChapter One

OVERVIEWOVERVIEW

1.11.1 OverviewOverview ........................................................................................................................................ 33

1.21.2 ConfigurationConfiguration ............................................................................................................................ 44

Page 12: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used
Page 13: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

The measurement of particle size distribution is used for fundamental studies and quality control inThe measurement of particle size distribution is used for fundamental studies and quality control inproduction processes in many diverse fields such as fine ceramics, cement, pharmaceuticals, metalproduction processes in many diverse fields such as fine ceramics, cement, pharmaceuticals, metalpowders, industrial minerals and ores, explosives, solid fuels, food, drugs and beauty care emul-powders, industrial minerals and ores, explosives, solid fuels, food, drugs and beauty care emul-sions, micelles, polymers, coatings and adhesives, pigments and dyes, carbon black and othersions, micelles, polymers, coatings and adhesives, pigments and dyes, carbon black and othermineral additives, and fillers used in the rubber, plastics and paper industries.mineral additives, and fillers used in the rubber, plastics and paper industries.

Particle sizes ranging from 0.02 to 2000 microns are divided into 85 sectors, and the full range isParticle sizes ranging from 0.02 to 2000 microns are divided into 85 sectors, and the full range ismeasured at one time with no adjustments. Measurement time is adjustable, but usually 20 secondsmeasured at one time with no adjustments. Measurement time is adjustable, but usually 20 secondsis sufficient.is sufficient.

Many options such as a Fraction Cell and holder, an AutoSampler, and a Reservoir are availableMany options such as a Fraction Cell and holder, an AutoSampler, and a Reservoir are availablefor wet analyses. A PowderJet Dry Feeder is available for dry analysis.for wet analyses. A PowderJet Dry Feeder is available for dry analysis.

Note:Note:

Any sample cell other than those specificallyAny sample cell other than those specificallydesigned for the LA-930 cannot be used.designed for the LA-930 cannot be used.

1.11.1 OVERVIEWOVERVIEW

1. OVERVIEW1. OVERVIEW

33

Page 14: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

1.21.2 CONFIGURATIONCONFIGURATION

The LA-930 is configured as shown below. The sample carrying liquid is circulated by the centrifu-The LA-930 is configured as shown below. The sample carrying liquid is circulated by the centrifu-gal circulation pump. The computer screen is used for displaying and setting the conditions forgal circulation pump. The computer screen is used for displaying and setting the conditions formeasuring, retrieving, and displaying data.measuring, retrieving, and displaying data.

There are two light sources: a long-life 632.8 nm He-Ne laser expanded by a beam expander and aThere are two light sources: a long-life 632.8 nm He-Ne laser expanded by a beam expander and ablue (405 nm) wavelength from a monochromatic tungsten lamp. The light emitted from the laserblue (405 nm) wavelength from a monochromatic tungsten lamp. The light emitted from the laserand the tungsten lamp is focused on the particles suspended in the liquid.and the tungsten lamp is focused on the particles suspended in the liquid.

After the laser beam has been dispersed and scattered by the particles in the flow cell, it passesAfter the laser beam has been dispersed and scattered by the particles in the flow cell, it passesthrough the condenser lens and is focused on the forward ring silicon diode array , comprised of 75through the condenser lens and is focused on the forward ring silicon diode array , comprised of 75separate detection elements, and on six (6) wide-angle silicon diode detectors. The scattered lightseparate detection elements, and on six (6) wide-angle silicon diode detectors. The scattered lightfrom the tungsten lamp is sensed by another six (6) wide-angle silicon diode detectors, ranging infrom the tungsten lamp is sensed by another six (6) wide-angle silicon diode detectors, ranging inangles up to 138angles up to 138°° from the forward direction. The intensity of this scattered light from both the laser from the forward direction. The intensity of this scattered light from both the laserand tungsten lamp is converted into electrical signals, which are then used to calculate the sizeand tungsten lamp is converted into electrical signals, which are then used to calculate the sizedistribution of the particles.distribution of the particles.

Fig. 1-1:Fig. 1-1: Configuration of LA-930 System Configuration of LA-930 System

1. CONFIGURATION1. CONFIGURATION

44

Page 15: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

Chapter TwoChapter Two

NAMES AND FUNCTIONSNAMES AND FUNCTIONS

2.12.1 Front and Top Views of Main UnitFront and Top Views of Main Unit .............................................................. 77

2.22.2 Right Side View of Main UnitRight Side View of Main Unit ............................................................................ 88

2.32.3 Rear Panel of Main UnitRear Panel of Main Unit ............................................................................................ 99

2.42.4 Sample ChamberSample Chamber .............................................................................................................. 1010

Page 16: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used
Page 17: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

77

2.12.1 FRONT AND TOP VIEWS OF MAIN UNITFRONT AND TOP VIEWS OF MAIN UNIT

Fig. 2-1:Fig. 2-1: Front View Front View

Pre-treatment Section Lid:Pre-treatment Section Lid: Sample dispersion chamber lid of the centrifugalSample dispersion chamber lid of the centrifugalpump recirculation system.pump recirculation system.

Sample Cell Chamber Lid:Sample Cell Chamber Lid: Lid to chamber containing sample cell.Lid to chamber containing sample cell.

Sample Chamber LidSample Chamber Lid

Pre-treatmentPre-treatmentSection LidSection Lid

Pre-treatment Section LidPre-treatment Section Lid

2. FRONT & TOP VIEW2. FRONT & TOP VIEW

Power IndicatorPower Indicator

Fig. 2-2:Fig. 2-2: Top View Top View

Page 18: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

88

2.22.2 RIGHT SIDE VIEW OF MAIN UNITRIGHT SIDE VIEW OF MAIN UNIT

Fig 2-3:Fig 2-3: Right Side View Right Side View

Out To Auto-Sampler:Out To Auto-Sampler: Used to connect to AutoSampler input jets locatedUsed to connect to AutoSampler input jets locatedon rear of AutoSampler.on rear of AutoSampler.

Dispersant Fluid Input:Dispersant Fluid Input: Used to connect to customer dispersion fluid supplyUsed to connect to customer dispersion fluid supplyline or reservoir.line or reservoir.

Drain Outlets:Drain Outlets: Used to connect to the drain hoses.Used to connect to the drain hoses.

DispersantDispersantFluid InputFluid Input

2. RIGHT SIDE VIEW2. RIGHT SIDE VIEW

Main DrainMain DrainOutletOutlet

Cell ChamberCell ChamberDrain OutletDrain Outlet

Out ToOut ToAuto-SamplerAuto-Sampler

Page 19: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

99

2.32.3 REAR PANEL OF MAIN UNITREAR PANEL OF MAIN UNIT

ResetReset Switch Switch

RS-232CRS-232CConnectorConnector

ConnectorsConnectorsfor Optionsfor Options

Fig. 2-4: Fig. 2-4: Rear Panel Rear Panel

2. REAR PANEL2. REAR PANEL

Power Switch:Power Switch: Used to turn on the LA-930.Used to turn on the LA-930.

AC Connector:AC Connector: Used to connect the power cable to.Used to connect the power cable to.

Fuses:Fuses: Fuses for the LA-930. Their ratings are 3.15A time lag.Fuses for the LA-930. Their ratings are 3.15A time lag.

Vents for Fan:Vents for Fan: Vents for the fan which is used to cool the powerVents for the fan which is used to cool the powersource. Never block them.source. Never block them.

RS-232C Connector:RS-232C Connector: Used to connect the RS-232C cable from the PC to.Used to connect the RS-232C cable from the PC to.

Reset Switch:Reset Switch: Pressing this switch resets the unit.Pressing this switch resets the unit.

Connectors for Options:Connectors for Options: These connectors are used for the optionalThese connectors are used for the optionalAutoSampler, Reservoir, and PowderJetAutoSampler, Reservoir, and PowderJetDry Feeder.Dry Feeder.

Vents for FanVents for Fan

AC ConnectorAC Connector

PowerPowerSwitchSwitch

FusesFuses

Page 20: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

2.42.4 SAMPLE CHAMBERSAMPLE CHAMBER

Fig. 2-5: Fig. 2-5: Sample Chamber, Top view Sample Chamber, Top view

Sample Cell Holder:Sample Cell Holder: A unit to hold the sample cell.A unit to hold the sample cell.

Tube for SampleTube for SampleCirculation:Circulation: A tube used to circulate the sample through the cell.A tube used to circulate the sample through the cell.

Retaining Screws:Retaining Screws: Screws used to retain the cell holder to theScrews used to retain the cell holder to themounting plate on the main unit.mounting plate on the main unit.

2. SAMPLE CHAMBER2. SAMPLE CHAMBER

SampleSampleCell HolderCell Holder

Tube forTube forCirculationCirculation

RetainingRetainingScrewsScrews

1010

Page 21: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

Chapter ThreeChapter Three

MAINTENANCEMAINTENANCE

3.13.1 Daily CareDaily Care.................................................................................................................................. 1313

3.23.2 Cleaning the CellCleaning the Cell .............................................................................................................. 1414

3.33.3 Replacing the FusesReplacing the Fuses ...................................................................................................... 1515

3.43.4 StorageStorage .......................................................................................................................................... 1616

Page 22: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used
Page 23: INSTRUCTION MANUAL - Horiba...the equipment is operated in a commercial environment. This equipment generates, uses, and radiates radio frequency energy and, if not installed and used

3.13.1 DAILY CAREDAILY CARE

3. DAILY CARE3. DAILY CARE

At start-upAt start-up

1.1. While warming up the unit, circulate dispersant fluid for a minimum of 30 minutes.While warming up the unit, circulate dispersant fluid for a minimum of 30 minutes.

2.2. When the analyzer has been warmed up, drain off the dispersant fluid, inject a freshWhen the analyzer has been warmed up, drain off the dispersant fluid, inject a freshsupply of dispersant fluid, and circulate it briefly (for about 30 seconds) and drain itsupply of dispersant fluid, and circulate it briefly (for about 30 seconds) and drain itoff again. Do this once again with another fresh supply of dispersant fluid.off again. Do this once again with another fresh supply of dispersant fluid.

At shutdownAt shutdown

1.1. Drain off the fluid in the cell, rinse, inject fresh dispersant fluid again, circulate for 3Drain off the fluid in the cell, rinse, inject fresh dispersant fluid again, circulate for 3minutes and drain off. If a water soluble-solution is used as the dispersant fluid, theminutes and drain off. If a water soluble-solution is used as the dispersant fluid, thecirculation system can be cleaned more easily by injecting in 1-2 drops of a natural orcirculation system can be cleaned more easily by injecting in 1-2 drops of a natural orweak alkaline liquid detergent. (Do not inject excessive detergent as this will hinderweak alkaline liquid detergent. (Do not inject excessive detergent as this will hinderthe rinsing operation.)the rinsing operation.)

2.2. If the outer surfaces of the analyzer are dirty, clean them with a dry cloth or wipe offIf the outer surfaces of the analyzer are dirty, clean them with a dry cloth or wipe offwith a gauze dampened with a neutral detergent.with a gauze dampened with a neutral detergent.

3.3. Clean the sample cell.Clean the sample cell.

1313

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1414

3.23.2 CLEANING THE CELLCLEANING THE CELL

3. CLEANING THE CELL3. CLEANING THE CELL

1.1. After making sure that there is no dispersant in the cell, loosen the four retainingAfter making sure that there is no dispersant in the cell, loosen the four retainingscrews holding the top sample cell transition piece on the cell holder, and remove thescrews holding the top sample cell transition piece on the cell holder, and remove thetop transition piece.top transition piece.

2.2. Clean the cell and the O-ring with the dispersant.Clean the cell and the O-ring with the dispersant.Use a cotton applicator or soft cloth for this purpose.Use a cotton applicator or soft cloth for this purpose.

Fig. 4-1: Fig. 4-1: Cleaning the Cell Cleaning the Cell

!! Caution: Caution:Since the outside cell surface is coated so as to decreaseSince the outside cell surface is coated so as to decrease

reflection of light, take care that it is not exposedreflection of light, take care that it is not exposedto detergent or chemical agent when cleaning the cellto detergent or chemical agent when cleaning the cell..

3.3. Use a cotton applicator to clean the O-ring grooves in the holder, top and bottom.Use a cotton applicator to clean the O-ring grooves in the holder, top and bottom.

4.4. Fit the O-ring and the cell to the cell holder. Place the top transition piece on the cellFit the O-ring and the cell to the cell holder. Place the top transition piece on the cellholder and then turn the retaining screws clockwise to retain the cell.holder and then turn the retaining screws clockwise to retain the cell.

!! Caution: Caution:→→ If samples that adhere to the cell were measured, If samples that adhere to the cell were measured,clean the cell, and also make sure that the sampleclean the cell, and also make sure that the sample

does not adhere to the wet part of the cell.does not adhere to the wet part of the cell.

→→ If too much sample adheres, remove it from If too much sample adheres, remove it fromeach part using sponge or a plastic scraper.each part using sponge or a plastic scraper.

→→ The outside surface of the cell should be cleaned with a The outside surface of the cell should be cleaned with acotton applicator or soft professional, lens cleaning cloth.cotton applicator or soft professional, lens cleaning cloth.

Never scrub it, nor touch it with anything hard.Never scrub it, nor touch it with anything hard.

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1515

3.33.3 REPLACING THE FUSESREPLACING THE FUSES

3. REPLACING THE FUSES3. REPLACING THE FUSES

If the fuses are blown, replace them with those delivered with the LA-930.If the fuses are blown, replace them with those delivered with the LA-930.

11.. Turn off the power switch.Turn off the power switch.

2.2. Disconnect the power cable.Disconnect the power cable.

3.3. Replace the fuses. There are two fuses. The locations of the fuses are shown in Fig. 3-4. NeverReplace the fuses. There are two fuses. The locations of the fuses are shown in Fig. 3-4. Neveruse any fuse that is not specified.use any fuse that is not specified.

4.4. Connect the power cable.Connect the power cable.

5.5. Turn on the power switch.Turn on the power switch.

6.6. Check to see that the LA-930 operates normally.Check to see that the LA-930 operates normally.

!! Caution: Caution:If the fuses are still blown after the replacement,If the fuses are still blown after the replacement,

immediately turn off the power switch, disconnect theimmediately turn off the power switch, disconnect thepower cable, and then contact a service center.power cable, and then contact a service center.Never use any fuse other than those specified.Never use any fuse other than those specified.

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1616

3.43.4 STORAGESTORAGE

3. STORAGE3. STORAGE

1.1. After carrying out the shut-down procedure described above, drain off all the dispers-After carrying out the shut-down procedure described above, drain off all the dispers-ant fluid, dry thoroughly, place the dust cover over the unit and store carefully.ant fluid, dry thoroughly, place the dust cover over the unit and store carefully.

2.2. The analyzer must be stored where it will not be exposed to temperatures exceeding aThe analyzer must be stored where it will not be exposed to temperatures exceeding arange of 5range of 5°°C(40C(40°°F) - 40F) - 40°°C(104C(104°°F).F).

3.3. If the unit has been stored for a long time, be sure to carry out all the appropriateIf the unit has been stored for a long time, be sure to carry out all the appropriatesteps described above before attempting to conduct measurements.steps described above before attempting to conduct measurements.

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APPENDIXAPPENDIX

A.A. SpecificationsSpecifications ............................................................................................................ APP-3APP-3

B.B. Principles of MeasurementPrinciples of Measurement ...................................................................... APP-4APP-4

C.C. Principles of the LA-930 Optical SystemPrinciples of the LA-930 Optical System ............................ APP-9APP-9

D.D. Spare Parts & OptionsSpare Parts & Options .............................................................................. APP-12APP-12

E.E. LA-930 RS-232C SpecificationsLA-930 RS-232C Specifications ................................................ APP-13APP-13

F.F. List of Refractive Index ValuesList of Refractive Index Values ...................................................... APP-14APP-14

G.G. Sampling & DispersionSampling & Dispersion ............................................................................ APP-18APP-18

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A.A. SPECIFICATIONSSPECIFICATIONS

APP-3APP-3

APPENDIX: SPECIFICATIONSAPPENDIX: SPECIFICATIONS

Principles of Measurement:Principles of Measurement: Based on Mie scattering theoryBased on Mie scattering theory

Range of Particle Size Displayed:Range of Particle Size Displayed: 0.02 to 20000.02 to 2000µµm.m.

Measurement Time:Measurement Time: Approx. 20 seconds, normally from start ofApprox. 20 seconds, normally from start ofmeasurement to display of data (max. 3 min.).measurement to display of data (max. 3 min.).

Amount of Sample LiquidAmount of Sample LiquidRequired for Measurement:Required for Measurement: 10 mg to 1 g per measurement, about 140 ml10 mg to 1 g per measurement, about 140 ml

of dispersant fluid when using the flow cell.of dispersant fluid when using the flow cell.(This figure depends on the sample.)(This figure depends on the sample.)

Optical System:Optical System: Light source:Light source: →→ 632.8 nm He-Ne laser, 1 mW632.8 nm He-Ne laser, 1 mW→→ Tungsten halogen lamp, 50 W.Tungsten halogen lamp, 50 W.

Photo-cell detector:Photo-cell detector: →→ 75-division, ring shaped75-division, ring shapedsilicon photo-diode arraysilicon photo-diode array

→→ Silicon photo-diode x 12.Silicon photo-diode x 12.

Sample Recirculation System:Sample Recirculation System: →→ Ultrasonic chamber 30 W, 22.5 kHz.Ultrasonic chamber 30 W, 22.5 kHz.→→ Circulation pumpCirculation pump

Centrifugal pump, discharge volumeCentrifugal pump, discharge volume8 L/min (in case of distilled water),8 L/min (in case of distilled water),15-step selection, teflon-tubing15-step selection, teflon-tubing

→→ Sample flow cell, Tempax glass.Sample flow cell, Tempax glass.

Power:Power: 100/110 to 200/220 to 240 VAC,100/110 to 200/220 to 240 VAC,selectable, 50/60 Hz approx. 300 VA.selectable, 50/60 Hz approx. 300 VA.

Communications:Communications: RS-232C.RS-232C.

Proper OperationProper OperationTemperature and Humidity:Temperature and Humidity: 1010°°C (50C (50°°F) to 35F) to 35°°C (95C (95°°F)F)

less than 85% RH (no condensation)less than 85% RH (no condensation)

Dimensions:Dimensions: 690 (W) x 525 (D) x 355 (H) mm690 (W) x 525 (D) x 355 (H) mm27.2(W) x 20.6 (D) x 14(H) inch27.2(W) x 20.6 (D) x 14(H) inch

Weight:Weight: Approx. 55 kg, 121 lb.Approx. 55 kg, 121 lb.

Options:Options: →→ Reservoir Unit (for filling, automaticReservoir Unit (for filling, automaticconcentration adjustment and rinsing)concentration adjustment and rinsing)

→→ Auto-sampler (automatic injection andAuto-sampler (automatic injection andmeasurement of up to 24 samples)measurement of up to 24 samples)

→→ Fraction cell holder with magnetic stirrerFraction cell holder with magnetic stirrer→→ Fraction cellFraction cell→→ PowderJet Dry FeederPowderJet Dry Feeder

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This analyzer measures the particle size distribution by angular light scattering techniques.This analyzer measures the particle size distribution by angular light scattering techniques.The scattered light intensity of particles at the photo-cell detector is shown below in Figure B-2.The scattered light intensity of particles at the photo-cell detector is shown below in Figure B-2.

When light goes into a spherical particle of radius r, the following three types of light will beWhen light goes into a spherical particle of radius r, the following three types of light will beemitted, as shown in Fig.B-1.emitted, as shown in Fig.B-1.

Fig. B-1: Fig. B-1: Illustrations from M.Kerker, Illustrations from M.Kerker,The Scattering of Light and Other Electromagnetic Radiation,The Scattering of Light and Other Electromagnetic Radiation,

Academic Press (1969)Academic Press (1969)

1.1. Light which reflects at the outer surface of the particleLight which reflects at the outer surface of the particle

2.2. Light which passes through the inside of the particle and then reflects at the innerLight which passes through the inside of the particle and then reflects at the innersurface of the particlesurface of the particle

3.3. Light which passes through the inside of the particle, and refracts and continues toLight which passes through the inside of the particle, and refracts and continues topass through the particle.pass through the particle.

APP-4APP-4

B.B. PRINCIPLES OF MEASUREMENTPRINCIPLES OF MEASUREMENT

APPENDIX: PRINCIPLES OF MEASUREMENTAPPENDIX: PRINCIPLES OF MEASUREMENT

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(( ))

General geometrical handling of scattering phenomenaGeneral geometrical handling of scattering phenomena

All of these phenomena can be handled as light scattering. Generally, light scattering can beAll of these phenomena can be handled as light scattering. Generally, light scattering can beexplained by the Mie scattering theory which was obtained by a strict application ofexplained by the Mie scattering theory which was obtained by a strict application ofMaxwell’s electromagnetic equation. The Mie scattering theory is precise, but difficult toMaxwell’s electromagnetic equation. The Mie scattering theory is precise, but difficult touse. Therefore, a simple approximation is generally used, i.e., relationships between theuse. Therefore, a simple approximation is generally used, i.e., relationships between theincident wavelength incident wavelength λλ and the particle radius and the particle radius rr can be stated as: can be stated as:

When the particle size is considerably less than When the particle size is considerably less than λλ, it is considered to be Rayleigh scattering., it is considered to be Rayleigh scattering.When the particle size is considerably greater than When the particle size is considerably greater than λλ, it is considered as Fraunhofer diffraction., it is considered as Fraunhofer diffraction.

According to Fraunhofer diffraction theory, the scattered light intensity distribution of aAccording to Fraunhofer diffraction theory, the scattered light intensity distribution of aparticle, as shown in Fig. B-2, can be expressed by the following equation:particle, as shown in Fig. B-2, can be expressed by the following equation:

Fig. B-2: Fig. B-2: Fraunhofer Diffraction Fraunhofer Diffraction

II == I I 22JJ11(x)(x)

........... 5.1.1........... 5.1.1xx

II00 :: Intensity at the center of the diffraction patternIntensity at the center of the diffraction patternJJ11 :: First order spherical primary Bessel functionFirst order spherical primary Bessel function

xx ==22ππrr22

........... 5.1.2........... 5.1.2λλff

r :r : Radius of particleRadius of particles :s : The radial distance as measured from the optical axisThe radial distance as measured from the optical axisλλ:: Wavelength of incident lightWavelength of incident lightff :: Focal length of the lensFocal length of the lens

APPENDIX: PRINCIPLES OF MEASUREMENTAPPENDIX: PRINCIPLES OF MEASUREMENT

APP-5APP-5

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APP-6APP-6

APPENDIX: PRINCIPLES OF MEASUREMENTAPPENDIX: PRINCIPLES OF MEASUREMENT

According to the Mie scattering theory, when monochromatic light enters a single sphericalAccording to the Mie scattering theory, when monochromatic light enters a single sphericalparticle, the intensity, Iparticle, the intensity, Iθθ, of scattered light in a certain direction from that particle is, as, of scattered light in a certain direction from that particle is, asshown in Fig. B-3, determined by (A) the particle-size parameter, shown in Fig. B-3, determined by (A) the particle-size parameter, αα (= 2 (= 2ππ r/r/λλ) which is) which isdefined by the ratio of the circumferential length of the sphere to the wavelength of thedefined by the ratio of the circumferential length of the sphere to the wavelength of theincident light, incident light, λλ , and (B) the relative refractive index, m, ( = , and (B) the relative refractive index, m, ( = µµ22//µµ11) which is the ratio of the) which is the ratio of therefractive index of the particle to that of the medium. See the diagram below.refractive index of the particle to that of the medium. See the diagram below.

Fig. B-3: Fig. B-3: Coordinates for the observation of scattered light from a particle Coordinates for the observation of scattered light from a particle

IIθθ ==λλ22

((ii11 + + ii22)) ........... 5.1.3........... 5.1.388ππ22RR22

wherewhere

λλ:: Wavelength of incident lightWavelength of incident lightRR:: Distance from the particle to the observation positionDistance from the particle to the observation position

ii11 and and ii22 denote the polarized components in which the progressive vibration directions of the denote the polarized components in which the progressive vibration directions of theincident light are vertical and horizontal to the observed surface.incident light are vertical and horizontal to the observed surface.

∞∞

ii11 == ΣΣ 22nn + 1 + 1{{aannππnn ++bbnnττnn}}

2 2

nn((nn + 1) + 1)nn = 1 = 1

........... 5.1.4........... 5.1.4

∞∞

ii22 == ΣΣ 22nn + 1 + 1{{bbnnππnn ++aannττnn}}

2 2

nn((nn + 1) + 1)

where...where...

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aann

==SSnn

'' ( (ββ))SSnn((αα) - ) - mSmSnn'' ( (αα))SSnn((ββ))

SSnn'' ( (ββ))φφnn((αα) - ) - mmφφnn

'' ( (αα))SSnn((ββ))

bbnn

==mSmSnn

'' ( (ββ))SSnn((αα) - ) - SSnn'' ( (αα))SSnn((ββ))

mSmSnn'' ( (ββ))φφnn((αα) - ) - φφnn

'' ( (αα))SSnn((ββ))

SSnn((αα)) ==√√παπα

JJ22 nn+1/2+1/2

((αα))

CCnn((αα)) == (-1)(-1)nn √√ παπα

JJ ((αα))22 -(n-(n+1/2)+1/2)

φφnn((αα)) == SSnn((αα) + ) + iiCCnn((αα))

ππnn ==11

PPnn(1)(1)((coscosθθ))sinsinθθ

ττnn ==δδ

PPnn(1)(1)((coscosθθ))δδθθ

J is the Bessel function and PJ is the Bessel function and Pnn(1)(1) the “associated function” of Legendre, i.e., the “associated function” of Legendre, i.e.,

ii == √√-1-1

mm ==µµ22

µµ11

µµ11 :: Refractive index of light in mediumRefractive index of light in mediumµµ22 :: Refractive index of light in particleRefractive index of light in particle

ββ == mama

αα ==2π2πrrλλ

The scattering intensity, IThe scattering intensity, Iθθ, varies depending on the direction in which light scatters from the, varies depending on the direction in which light scatters from theparticle, i.e., according to the scattering angle. As shown in Fig. B-4, the scattered light isparticle, i.e., according to the scattering angle. As shown in Fig. B-4, the scattered light isclassified according to the scattering angle as follows:classified according to the scattering angle as follows:

0 0 ≤≤ θθ < 90 < 90°° :: forward scatteringforward scatteringθθ = 90 = 90°° :: side scatteringside scattering9090° < ° < θθ < 180 < 180°°:: back scatteringback scattering

APP-7APP-7

APPENDIX: PRINCIPLES OF MEASUREMENTAPPENDIX: PRINCIPLES OF MEASUREMENT

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APPENDIX: PRINCIPLES OF MEASUREMENTAPPENDIX: PRINCIPLES OF MEASUREMENT

APP-8APP-8

The intensity, The intensity, IIθ θ , of the scattered light is in an infinite series, as shown in Equation 5.1.4., of the scattered light is in an infinite series, as shown in Equation 5.1.4.Therefore, calculations will take a very long time, especially when the particle size is large.Therefore, calculations will take a very long time, especially when the particle size is large.

If the incident wavelength is constant, when the particle size is larger than the incident wave-If the incident wavelength is constant, when the particle size is larger than the incident wave-length, the scattered light focuses almost entirely in only the forward direction, length, the scattered light focuses almost entirely in only the forward direction, <<9090⋅⋅, and varies, and variesdepending on the particle size. More specifically, the relation between the particle-size distri-depending on the particle size. More specifically, the relation between the particle-size distri-bution and the light-intensity distribution is the ratio of 1:1. Therefore, if the light-intensitybution and the light-intensity distribution is the ratio of 1:1. Therefore, if the light-intensitydistribution of the particle to be measured is known, its particle size can be determined.distribution of the particle to be measured is known, its particle size can be determined.

On the other hand, when the particle size is smaller than the incident wavelength, the scatteredOn the other hand, when the particle size is smaller than the incident wavelength, the scatteredlight gradually shifts toward the side and rear, and finally spreads in all directions. When thelight gradually shifts toward the side and rear, and finally spreads in all directions. When theparticle size is smaller than 0.1 particle size is smaller than 0.1 µµm, the absolute value of the scattered-light intensity variesm, the absolute value of the scattered-light intensity variesmuch more than before.much more than before.

In this situation, the intensity distribution of the front scattering does not depend on the particleIn this situation, the intensity distribution of the front scattering does not depend on the particlesize, becoming almost constant.size, becoming almost constant.

Therefore, even if the particle size is different in this region, there will be no difference in theTherefore, even if the particle size is different in this region, there will be no difference in theintensity distribution of the forward scattered light. Accordingly, the size of a very smallintensity distribution of the forward scattered light. Accordingly, the size of a very smallparticle can be no longer determined by only the information from the forward scattered light.particle can be no longer determined by only the information from the forward scattered light.

Fig. B-4: Fig. B-4: Changes in scattering angle and intensity Changes in scattering angle and intensityG. Mie: Ann. d. physik 94) 25, 429 (1908)G. Mie: Ann. d. physik 94) 25, 429 (1908)

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APP-9APP-9

APPENDIX: PRINCIPLES OF THE LA-930 OPTICAL SYSTEMAPPENDIX: PRINCIPLES OF THE LA-930 OPTICAL SYSTEM

C.C. PRINCIPLES OF THE LA-930 OPTICAL SYSTEMPRINCIPLES OF THE LA-930 OPTICAL SYSTEM

The optical system in an ordinary laser-diffraction type analyzer condenses the forward scatteringThe optical system in an ordinary laser-diffraction type analyzer condenses the forward scatteringfrom a laser beam with a condenser Fourier lens and forms an image on the ring-shaped detectorfrom a laser beam with a condenser Fourier lens and forms an image on the ring-shaped detectorlocated at the focal distance.located at the focal distance.

Using only this method, however, it is difficult to measure the range of small particle sizes, in particu-Using only this method, however, it is difficult to measure the range of small particle sizes, in particu-lar, particles under 0.1 lar, particles under 0.1 µµm. Very small particles cannot be measured merely by means of them. Very small particles cannot be measured merely by means of theforward scattering using the wavelength of a He-Ne laser beam, i.e., 632.8 nm. To measure suchforward scattering using the wavelength of a He-Ne laser beam, i.e., 632.8 nm. To measure suchparticles, it is necessary to have either information from the side and back scattering or that from theparticles, it is necessary to have either information from the side and back scattering or that from thepolarization scattering intensity. polarization scattering intensity. Therefore, as shown in Figure C-1, Therefore, as shown in Figure C-1, the new optical system in thethe new optical system in theModel LA-930 uses thirteen separate sets of detectors, twelve for the wide angle and back scatter-Model LA-930 uses thirteen separate sets of detectors, twelve for the wide angle and back scatter-ing, and a third detector array composed of 75 elements for the forward scattering. The lighting, and a third detector array composed of 75 elements for the forward scattering. The lightsources used for detecting scattered light at wide angles and back scattering in the Model LA-930sources used for detecting scattered light at wide angles and back scattering in the Model LA-930are a tungsten lamp, filtered at 405 nm, plus theare a tungsten lamp, filtered at 405 nm, plus theHe-Ne laser. This means: (1) the small angle forward scattered light is conventionally given by theHe-Ne laser. This means: (1) the small angle forward scattered light is conventionally given by theHe-Ne laser and detected by the ring detector array, and (2) the wide angle and back scatteredHe-Ne laser and detected by the ring detector array, and (2) the wide angle and back scatteredlight is given by the tungsten lamp/laser combination and detected by individual photo-diodeslight is given by the tungsten lamp/laser combination and detected by individual photo-diodeslocated at larger angles from the forward detector array.located at larger angles from the forward detector array.

Fig. C-1:Fig. C-1: Schematic representation of the LA-930 optical system Schematic representation of the LA-930 optical system

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APP-10APP-10

APPENDIX: PRINCIPLES OF THE LA-930 OPTICAL SYSTEMAPPENDIX: PRINCIPLES OF THE LA-930 OPTICAL SYSTEM

Particle size distribution analysisParticle size distribution analysis

Particles of various sizes exist in an actual sample dispersion, and their scattered light differsParticles of various sizes exist in an actual sample dispersion, and their scattered light differsaccording to their size. Equation 5.2.1 shows the relationship between the intensity distribu-according to their size. Equation 5.2.1 shows the relationship between the intensity distribu-tion of the scattered light and the particle size distribution.tion of the scattered light and the particle size distribution.

∞∞

g(g(θθ)) == ∫∫KK((θθ,D,D))ff((DD))dDdD ........... 5.2.1........... 5.2.1oo

wherewhere

g(g(θθ) :) : the intensity distribution of the scattered lightthe intensity distribution of the scattered lightK(K(θθ,D):,D): response coefficient of scattered lightresponse coefficient of scattered lightf(D):f(D): particle size distribution coefficientparticle size distribution coefficientD:D: particle diameterparticle diameterθθ:: scattering anglescattering angle

In reality, measurement is performed by N number of detectors. As the Mie scattering theoryIn reality, measurement is performed by N number of detectors. As the Mie scattering theoryis used in combination for the response function, the equation corresponding to equationis used in combination for the response function, the equation corresponding to equation5.2.1 becomes equation 5.2.2.5.2.1 becomes equation 5.2.2.

nn

g(g(NN)) == ΣΣKK((N,DiN,Di))ff((DiDi))∆∆DD ........... 5.2.2........... 5.2.2ii=1=1

wherewhere

g(N) :g(N) : output of N-th detectoroutput of N-th detectorK(N,D):K(N,D): response coefficient of N-th detectorresponse coefficient of N-th detectorf(Df(Dii):): Particle size distributionParticle size distributionDDii :: i-th representative radiusi-th representative radius∆∆D:D: particle size segment numberparticle size segment number

The particle size distribution f(DThe particle size distribution f(Dii) is calculated from the relationship between the output of) is calculated from the relationship between the output ofthe detector (expressed by equation 5.2.2) and the response function of the detector. f(Dthe detector (expressed by equation 5.2.2) and the response function of the detector. f(Dii) is) iscalculated on the basis of volume.calculated on the basis of volume.

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APP-11APP-11

APPENDIX:APPENDIX: PRINCIPLES OF THE LA-930 OPTICAL SYSTEM PRINCIPLES OF THE LA-930 OPTICAL SYSTEM

The particle size distribution by area, length and number basis are calculated byThe particle size distribution by area, length and number basis are calculated byequations 5.2.3 to 5.2.5.equations 5.2.3 to 5.2.5.

Distribution by area basis:Distribution by area basis: ==mm

ff((DiDi)/)/DiDi........... 5.2.3........... 5.2.3

ΣΣ {{ff((DiDi)/)/DiDi}}ii=1=1

Distribution by length basis:Distribution by length basis: ==mm

ff((DiDi)/)/DiDi22

........... 5.2.4........... 5.2.4

ΣΣ {{ff((DiDi)/)/DiDi22}}ii=1=1

Distribution by number basis:Distribution by number basis: ==mm

ff((DiDi)/)/DiDi33

........... 5.2.5........... 5.2.5

ΣΣ {{ff((DiDi)/)/DiDi33}}ii=1=1

The specific surface area is calculated by equation 5.2.6, on the assumption that the particles beingThe specific surface area is calculated by equation 5.2.6, on the assumption that the particles beingmeasured are perfectly spherical.measured are perfectly spherical.

mm

Specific surface areaSpecific surface area = = 6 6 xx 10 1044ΣΣ{{ff((DiDi)/)/DiDi}(}(cmcm22//cmcm33)) ........... 5.2.6........... 5.2.6ii=1=1

wherewhere

DDii::representative particle diameterrepresentative particle diameter

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Spare PartsSpare Parts Part numberPart number

Fraction cellFraction cell U802030100U802030100

Flow cellFlow cell U802030000U802030000

KalRez O-ring for cellKalRez O-ring for cell 602376602376

Viton O-ring for cellViton O-ring for cell 602375602375

Ultrasonic probe tipUltrasonic probe tip 526330526330

Tungsten lampTungsten lamp 512404512404

Table D-1:Table D-1: Spare Parts Spare Parts

OptionsOptions Part numberPart number

LY-201 ReservoirLY-201 Reservoir 361658361658

LY-202 AutosamplerLY-202 Autosampler 361659361659

LY-203 Fraction cell holderLY-203 Fraction cell holder 361661361661(Use with Fraction cell.)(Use with Fraction cell.)

PowderJet Dry FeederPowderJet Dry Feeder 526347526347

Table D-2:Table D-2: Options Options

APPENDIX: SPARE PARTS & OPTIONSAPPENDIX: SPARE PARTS & OPTIONS

APP-12APP-12

D.D. Spare Parts & OptionsSpare Parts & Options

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APP-13APP-13

APPENDIX: LA-930 RS-232C SPECIFICATIONAPPENDIX: LA-930 RS-232C SPECIFICATION

E.E. LA-930 RS-232C SPECIFICATIONLA-930 RS-232C SPECIFICATION

Transmission formatTransmission format

The transmission format is as follows:The transmission format is as follows:(If the settings need to be changed, please contact HORIBA for advice and assistance. HORIBA(If the settings need to be changed, please contact HORIBA for advice and assistance. HORIBAwill reset the setting as necessary.)will reset the setting as necessary.)

Baud rate:Baud rate: 9600 bps 9600 bps

Data length:Data length: 8 bits8 bits

Parity check:Parity check: NONENONE

Parity:Parity: NONENONE

Stop bit:Stop bit: 11

RS-232C cableRS-232C cable

The LA-930 should be connected to the Compaq PC by the supplied cable.The LA-930 should be connected to the Compaq PC by the supplied cable.

Fig. E-1:Fig. E-1: Connection diagram for the RS-232C cable Connection diagram for the RS-232C cable

RS-232C Connector terminal numbersRS-232C Connector terminal numbers

Fig. E-2:Fig. E-2: Cable end as seen from terminal side Cable end as seen from terminal side

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APPENDIX: LIST OF THE REFRACTIVE INDEX VALUESAPPENDIX: LIST OF THE REFRACTIVE INDEX VALUES

APP-14APP-14

G.G. LIST OF THE REFRACTIVE INDEX VALUESLIST OF THE REFRACTIVE INDEX VALUES

Inorganic Subst ancesInorganic Subst ances

SubstanceSubstance CompositionComposition SpecificSpecific RefractiveRefractive RelativeRelativeGravityGravity index, nindex, n1 ,1 , refractiverefractive

index (RRI)index (RRI)m(nm(n00=water)=water)

Lead whiteLead white PbPb33(CO(CO33))22(OH)(OH)22 6.86.8 2.022.02 1.511.51

Zink flowerZink flower ZnOZnO 5.65.6 2.002.00 1.501.50

Titanium oxide(rutile)Titanium oxide(rutile) TiOTiO22 4.24.2 2.752.75 2.062.06

Titanium oxide(anatase)Titanium oxide(anatase) TiOTiO22 3.93.9 2.502.50 1.881.88

Zinc sulfideZinc sulfide ZnSZnS 4.04.0 2.372.37 1.781.78

Lead titanateLead titanate PbTiOPbTiO 22 7.37.3 2.702.70 2.032.03

Ziconium oxideZiconium oxide ZrOZrO 5.75.7 2.402.40 1.801.80

Barium sulfateBarium sulfate BaSOBaSO44 4.44.4 1.621.62 1.221.22

Barium carbonateBarium carbonate BaCOBaCO33 4.34.3 1.601.60 1.201.20

Calcium carbonateCalcium carbonate CaCOCaCO33 2.82.8 1.581.58 1.181.18

GypsumGypsum CaSOCaSO44..2H2H22OO 2.42.4 1.551.55 1.161.16

AluminaAlumina AlAl22OO 33 -- 1.661.66 1.251.25

Iron oxideIron oxide FeFe22OO33 4.84.8 2.902.90 2.172.17

Red leadRed lead PbPb33OO44 8.98.9 2.422.42 1.821.82

Mercuric sulfideMercuric sulfide HgSHgS 8.08.0 2.952.95 2.212.21

Lead chromateLead chromate PbCrOPbCrO44 6.06.0 2.402.40 1.801.80

Cadmium sulfideCadmium sulfide CdSCdS 4.44.4 2.422.42 1.811.81

Zinc yellowZinc yellow ZnCrOZnCrO44 3.53.5 1.871.87 1.401.40

Strontium yellowStrontium yellow SrCrOSrCrO44 -- 1.961.96 1.471.47

Barium yellowBarium yellow BaCrOBaCrO44 4.44.4 1.631.63 1.221.22

Chrome greenChrome green -- 4.14.1 2.402.40 1.801.80

Emerald greenEmerald green -- 3.23.2 1.971.97 1.481.48

Chromium oxideChromium oxide CrCr22OO33 5.15.1 2.502.50 1.881.88

Cobalt greenCobalt green CoOCoO..xxZnOZnO -- 1.971.97 1.481.48

Ultra marineUltra marine NaNa77AlAl66SiSi66OO2424SS33 2.42.4 1.571.57 1.181.18

Prussian bluePrussian blue FeFe44[Fe(CH)[Fe(CH)66]]33 1.81.8 1.561.56 1.171.17

Cobalt blueCobalt blue CoOCoO..xAlxAl22OO 33 3.83.8 1.741.74 1.311.31

CelurieneCeluriene CoOCoO..xxSnOSnO22 -- 1.841.84 1.381.38

Cobalt violetCobalt violet CoCo33(PO(PO44))22 -- 1.721.72 1.291.29

Manganese violetManganese violet (NH(NH44)2Mn)2Mn22(P(P22OO77))22 -- 1.701.70 1.281.28

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APP-15APP-15

APPENDIX: LIST OF THE REFRACTIVE INDEX VALUESAPPENDIX: LIST OF THE REFRACTIVE INDEX VALUES

Inorganic SubstancesInorganic Substances

SubstanceSubstance CompositionComposition SpecificSpecific RefractiveRefractive RelativeRelativeGravityGravity index, nindex, n1 ,1 , refractiverefractive

index (RRI)index (RRI)m(nm(n00=water)=water)

Silver chlorideSilver chloride AgClAgCl -- 2.082.08 1.561.56

FluoriteFluorite CaFCaF -- 1.431.43 1.071.07

GermaniumGermanium GeGe -- 4.104.10 3.073.07

Potassium bromidePotassium bromide KBrKBr -- 1.581.58 1.16*1.16*

Potassium chloridePotassium chloride KClKCl -- 1.801.80 1.32*1.32*

Lithium fluorideLithium fluoride LiFLiF -- 1.391.39 1.041.04

Magnesium oxideMagnesium oxide MgOMgO -- 1.761.76 1.321.32

SiliconSilicon SiSi -- 3.503.50 2.632.63

QuartzQuartz SiOSiO22 -- 1.451.45 1.091.09

Rock crystalRock crystal SiOSiO22 -- 1.541.54 1.161.16

DiamondDiamond CC -- 2.412.41 1.811.81

SapphireSapphire AlAl22OO 33 -- 1.761.76 1.321.32

Magnesium fluorideMagnesium fluoride MgFMgF22 -- 1.371.37 1.031.03

MicaMica KAlKAl22(AlSi(AlSi33OO1010)(OH))(OH)22 -- 1.591.59 1.191.19

BaCaBaCa22(C(C33HH55OO22))66 -- 1.451.45 1.091.09

Barium fluochlorideBarium fluochloride BaCBaC1212..BaFBaF22 -- 1.641.64 1.231.23

Barium fluorideBarium fluoride BaFBaF22 -- 1.471.47 1.101.10

Barium phosphateBarium phosphate BaHPOBaHPO44 -- 1.621.62 1.221.22

Barium sulfideBarium sulfide BaSBaS -- 2.162.16 1.591.59

Calcium alminateCalcium alminate CaCa33AlAl22OO33 -- 1.711.71 1.281.28

Calcium borateCalcium borate CaOCaO..BB22OO33 -- 1.601.60 1.201.20

CarbonCarbon CC -- 1.92-0.5221.92-0.522 1.881.88

Chromium oxideChromium oxide CrCr22OO33 -- 2.502.50 2.032.03

Copper oxideCopper oxide CuCu22OO -- 2.712.71 1.271.27

Copper sulfateCopper sulfate CuSOCuSO44 -- 1.731.73 1.241.24

Magnesium orthoborateMagnesium orthoborate 3MgO3MgO..BB22OO 33 -- 1.651.65 1.101.10

Potassium carbonatePotassium carbonate KK22COCO33 -- 1.501.50 1.091.09

Potassium hydrogencarbonatePotassium hydrogencarbonate KHCOKHCO33 -- 1.481.48 1.041.04

Potassium cyanidePotassium cyanide KCNKCN -- 1.411.41 1.221.22

Potassium chloratePotassium chlorate KClOKClO 33 -- 1.621.62 1.201.20

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APPENDIX: LIST OF THE REFRACTIVE INDEX VALUESAPPENDIX: LIST OF THE REFRACTIVE INDEX VALUES

APP-16APP-16

Inorganic SubstancesInorganic Substances

SubstanceSubstance CompositionComposition SpecificSpecific RefractiveRefractive RelativeRelativeGravityGravity index, nindex, n1 ,1 , refractiverefractive

index (RRI)index (RRI)m(nm(n00=water)=water)

Sodium bromideSodium bromide NaBrNaBr -- 1.641.64 1.061.06

Sodium cyanideSodium cyanide NaCNNaCN -- 1.451.45 1.121.12

Sodium metasilicateSodium metasilicate NaNa22SiOSiO33 -- 1.521.52 1.141.14

Sodium sulfateSodium sulfate NaNa22SOSO44 -- 1.551.55 1.281.28

Strontium dichromateStrontium dichromate SrCrSrCr22OO77..3H3H22OO -- 1.711.71 1.081.08

Strontium fluorideStrontium fluoride SrFSrF22 -- 1.441.44 1.581.58

Strontium sulfideStrontium sulfide SrSSrS -- 2.112.11 1.221.22

Zinc metasilicateZinc metasilicate ZnSiOZnSiO33 -- 1.621.62 --

IronIron FeFe -- 2.4-1.4i2.4-1.4i --

ZincZinc ZnZn -- 2.4-5.5i2.4-5.5i --

GoldGold AuAu -- 0.34-3.2i0.34-3.2i --

SilverSilver AgAg -- 0.19-3.4i0.19-3.4i --

CopperCopper CuCu -- 0.6-3.6i0.6-3.6i --

AluminumAluminum AlAl -- 1.6-5.4i1.6-5.4i --

AntimonyAntimony SbSb -- 3.2-5.0i3.2-5.0i --

MagnesiumMagnesium MgMg -- 0.4-4.6i0.4-4.6i --

ManganeseManganese MnMn -- 2.5-4.0i2.5-4.0i --

NickelNickel NiNi -- 1.8-3.6i1.8-3.6i --

PlatinumPlatinum PtPt -- 2.9-4.5i2.9-4.5i --

Table G-1:Table G-1: Taken from 1) “Handbook of Chemistry and Physics”., C.R.C. Press, Taken from 1) “Handbook of Chemistry and Physics”., C.R.C. Press,2)”American Institute of Handbook”., MaGraw-Hill and2)”American Institute of Handbook”., MaGraw-Hill and

3) “The Merck Index”., MERCK & Co., Inc.3) “The Merck Index”., MERCK & Co., Inc.

*n*n00 of this value is methanol. of this value is methanol.

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APP-17APP-17

APPENDIX: LIST OF THE REFRACTIVE INDEX VALUESAPPENDIX: LIST OF THE REFRACTIVE INDEX VALUES

Organic SubstancesOrganic Substances

SubstanceSubstance CompositionComposition SpecificSpecific RefractiveRefractive RelativeRelativeGravityGravity index, nindex, n1 ,1 , refractiverefractive

index (RRI)index (RRI)m(nm(n00=water)=water)

AsphaltAsphalt -- -- 1.631.63 1.221.22

EboniteEbonite -- -- 1.661.66 1.251.25

OpalOpal -- -- 1.441.44 1.081.08

Canadian balsamCanadian balsam -- -- 1.521.52 1.141.14

AmberAmber -- -- 1.541.54 1.161.16

IvoryIvory -- -- 1.541.54 1.161.16

Vinyl chloride resinVinyl chloride resin -- -- 1.541.54 1.161.16

Vinylidene chloride resinVinylidene chloride resin -- -- 1.611.61 1.211.21

Vinyl acetate resinVinyl acetate resin -- -- 1.461.46 1.101.10

Silicon oilSilicon oil -- -- 1.401.40 1.051.05

Tetrafluoroethylene resinTetrafluoroethylene resin -- -- 1.351.35 1.011.01

NylonNylon -- -- 1.531.53 1.151.15

PolyethylenePolyethylene -- -- 1.531.53 1.151.15

PolystyrenePolystyrene -- -- 1.601.60 1.201.20

Methylmethacrylic acid resinMethylmethacrylic acid resin -- -- 1.491.49 1.121.12

Melamine resinMelamine resin -- -- 1.601.60 1.201.20

Table G-2:Table G-2: Taken from 1) “Handbook of Chemistry and Physics”., C.R.C. Press, Taken from 1) “Handbook of Chemistry and Physics”., C.R.C. Press,2)”American Institute of Handbook”., MaGraw-Hill and2)”American Institute of Handbook”., MaGraw-Hill and

3) “The Merck Index”., MERCK & Co., Inc.3) “The Merck Index”., MERCK & Co., Inc.

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H.H. Sampling & DispersionSampling & Dispersion

APPENDIX: SAMPLING & DISPERSIONAPPENDIX: SAMPLING & DISPERSION

APP-18APP-18

1.1. Sampling MethodsSampling Methods

A representative sample is required in order to measure the particle size distribution ofA representative sample is required in order to measure the particle size distribution ofpowders or particles suspended in a liquid. This measurement sample must, therefore, havepowders or particles suspended in a liquid. This measurement sample must, therefore, havethe same particle size distribution as the overall sample.the same particle size distribution as the overall sample.

Obviously, when extracting measurement samples from a large reaction vessel, sampleObviously, when extracting measurement samples from a large reaction vessel, sampledrawn from the top will have a different particle size distribution from samples drawn fromdrawn from the top will have a different particle size distribution from samples drawn fromthe bottom.the bottom.

Small and heavy particles collect at the bottom of the vessel. This is called “segregation.”Small and heavy particles collect at the bottom of the vessel. This is called “segregation.”Taking samples from the upper and lower levels of the vessel is appropriate if the degree ofTaking samples from the upper and lower levels of the vessel is appropriate if the degree ofparticle settling is to be measured, but for particle size distribution measurements, meaning-particle settling is to be measured, but for particle size distribution measurements, meaning-less, unreproducible data will be obtained unless suitable sampling techniques are employed.less, unreproducible data will be obtained unless suitable sampling techniques are employed.

Sampling methods for powdersSampling methods for powders

1.1. Take samples of equal weight from throughout the material.Take samples of equal weight from throughout the material.

2.2. Use a twin divider or rotary splitter (see Figure H-1).Use a twin divider or rotary splitter (see Figure H-1).

3.3. Use the flow division method. (see Figure H-2).Use the flow division method. (see Figure H-2).

4.4. Disperse a large amount of the sample in a 215-315 ml dispersion medium.Disperse a large amount of the sample in a 215-315 ml dispersion medium.

5.5. Disperse evenly with ultrasonic energy or a stirrer.Disperse evenly with ultrasonic energy or a stirrer.

6.6. Draw off a measurement sample while agitating and pour it into the cell.Draw off a measurement sample while agitating and pour it into the cell.

Particles suspended in a liquidParticles suspended in a liquid

11.. Do not dilute at once in a large amount of dispersion medium, but carry out theDo not dilute at once in a large amount of dispersion medium, but carry out thedilution over several smaller stages.dilution over several smaller stages.

2.2. Agitate well while diluting.Agitate well while diluting.

3.3. Dilute in the same dispersion medium as the medium used in the original sample.Dilute in the same dispersion medium as the medium used in the original sample.

4.4. Disperse evenly with ultrasonic energy or a stirrer.Disperse evenly with ultrasonic energy or a stirrer.

5.5. Draw off a measurement sample while agitating and pour it into the cell.Draw off a measurement sample while agitating and pour it into the cell.

Although the concept is rather difficult to explain, the sampling method must be chosen toAlthough the concept is rather difficult to explain, the sampling method must be chosen tosuit the properties of the sample, as some particles (particularly fine particles) adhere due tosuit the properties of the sample, as some particles (particularly fine particles) adhere due tostrong surface forces, or cluster together if they are made damp by humidity.strong surface forces, or cluster together if they are made damp by humidity.

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APP-19APP-19

APPENDIX: SAMPLING & DISPERSIONAPPENDIX: SAMPLING & DISPERSION

Particles in solids, e.g. pigments in plasticsParticles in solids, e.g. pigments in plastics

1.1. Dilute the solid containing the particles in an appropriate dispersantDilute the solid containing the particles in an appropriate dispersant

(a)(a) Use the diluted samples as the measurement sample.Use the diluted samples as the measurement sample.(b)(b) Remove only the particle and measure.Remove only the particle and measure.

Clean until the dissolved solid has completely been removed and extract the particles.Clean until the dissolved solid has completely been removed and extract the particles.All further operations are the same as in (a).All further operations are the same as in (a).

Fig. H-1:Fig. H-1: Rotary Splitter Method Rotary Splitter Method

Fig. H-2:Fig. H-2: Flow Division Method Flow Division Method

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2. Dispersing Methods for Samples2. Dispersing Methods for Samples

As the LA-930 carries out measurements with the particles in a diluted state, the dispersed state ofAs the LA-930 carries out measurements with the particles in a diluted state, the dispersed state ofthe particles is an important factor in measurement accuracy.the particles is an important factor in measurement accuracy.

Even if the sampling of powders is carried out correctly, large particles that should not exist areEven if the sampling of powders is carried out correctly, large particles that should not exist aremeasured and the distribution is unnatural if particles agglomerate.measured and the distribution is unnatural if particles agglomerate.

Alternatively, when a dispersant of the sort that dissolves the powder is used, particles are mea-Alternatively, when a dispersant of the sort that dissolves the powder is used, particles are mea-sured to be smaller than they are, and this error causes inaccurate results.sured to be smaller than they are, and this error causes inaccurate results.

In order to carry out accurate measurement without any of the above problems, the dispersant usedIn order to carry out accurate measurement without any of the above problems, the dispersant usedand the dispersion method must be chosen carefully.and the dispersion method must be chosen carefully.

Dispersion MethodsDispersion MethodsSamples with Stable ParticlesSamples with Stable Particles

The sample can be irradiated with ultrasonic energy from the internal ultrasonic probe in the flowThe sample can be irradiated with ultrasonic energy from the internal ultrasonic probe in the flowloop, and the agglomerated particles are thus dispersed.loop, and the agglomerated particles are thus dispersed.

The ultrasonic time depends on the sample. However, 10 seconds to 1 minute is normally ad-The ultrasonic time depends on the sample. However, 10 seconds to 1 minute is normally ad-equate. If vibration is carried out for too long, the particles may coagulate or be damaged. How-equate. If vibration is carried out for too long, the particles may coagulate or be damaged. How-ever, the ideal ultrasonic time must be experimentally determined for each sample in order toever, the ideal ultrasonic time must be experimentally determined for each sample in order tothoroughly disperse the particles.thoroughly disperse the particles.

The LA-930 allows an ultrasonic time of up to 30 minutes to be set. The LA-930 allows the powerThe LA-930 allows an ultrasonic time of up to 30 minutes to be set. The LA-930 allows the powerto the ultrasonic probe to be adjusted also. The higher the power setting, the more ultrasonicto the ultrasonic probe to be adjusted also. The higher the power setting, the more ultrasonicvibration is employed and the more the particles are dispersed. The power setting can be variedvibration is employed and the more the particles are dispersed. The power setting can be variedfrom a low setting of 1 to a high of 7.from a low setting of 1 to a high of 7.

Samples with Unstable (Fragile) ParticlesSamples with Unstable (Fragile) Particles

When measuring such particles using the flow cell, do not apply ultrasonic vibration.When measuring such particles using the flow cell, do not apply ultrasonic vibration.If even normal centrifugal pumping damages the sample, conduct the measurement by placing aIf even normal centrifugal pumping damages the sample, conduct the measurement by placing asample that has been dispersed manually in the Fraction cell.sample that has been dispersed manually in the Fraction cell.

Selecting the DispersantSelecting the Dispersant

It is important that the dispersant properly “wets” the sample powder. The dispersant must be oneIt is important that the dispersant properly “wets” the sample powder. The dispersant must be onethat does not cause coagulation, dissolution, swelling or chemical reaction.that does not cause coagulation, dissolution, swelling or chemical reaction.

Water is used in most cases. However, in some cases, measurement may be carried out usingWater is used in most cases. However, in some cases, measurement may be carried out usingorganic fluids such as ethanol or ethylene glycol.organic fluids such as ethanol or ethylene glycol.

APPENDIX: SAMPLING & DISPERSIONAPPENDIX: SAMPLING & DISPERSION

APP-20APP-20

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APP-21APP-21

APPENDIX: SAMPLING & DISPERSIONAPPENDIX: SAMPLING & DISPERSION

Effect and Type of DispersantEffect and Type of Dispersant

Powder samples are generally charged, and may coagulate or may not be sufficiently dispersedPowder samples are generally charged, and may coagulate or may not be sufficiently disperseddue to the interaction with the dispersion fluid. The role of the dispersant is to increase thisdue to the interaction with the dispersion fluid. The role of the dispersant is to increase thisinteraction and to disperse each and every one of the particles. Widely used dispersants areinteraction and to disperse each and every one of the particles. Widely used dispersants aresodium polymetaphosphate and sodium pyrophosphate. Surfactants are also used for hydro-sodium polymetaphosphate and sodium pyrophosphate. Surfactants are also used for hydro-phobic (preferentially wet by oil or air) or lipophilic (preferentially wet by oil) particles.phobic (preferentially wet by oil or air) or lipophilic (preferentially wet by oil) particles.

However, if there is an excessive amount of surfactant, it might form micelles and agglomerate.However, if there is an excessive amount of surfactant, it might form micelles and agglomerate.Therefore, care must be taken regarding the concentration and the type of dispersant to be used.Therefore, care must be taken regarding the concentration and the type of dispersant to be used.The concentration of the dispersant depends on the type of dispersant. A concentration of aboutThe concentration of the dispersant depends on the type of dispersant. A concentration of about0.1-0.2% is widely used.0.1-0.2% is widely used.

Obtain RepresentativeObtain RepresentativeSAMPLESAMPLE

Reactivity CheckReactivity Check

Reactive in WaterReactive in Water Not ReactiveNot Reactive Reactive in WaterReactive in Waterand Organic Liquidsand Organic Liquids in Waterin Water Not Reative inNot Reative in

Organic SolventsOrganic SolventsSoluble?Soluble?

DRYDRY Water Solubility?Water Solubility? Organic Liquid CheckOrganic Liquid CheckANALYSISANALYSIS

InsolubleInsoluble Not Reactive,Not Reactive, ReactiveReactiveInsolubleInsoluble or Solubleor Soluble

SelectSelect SelectSelect DRYDRYDistilled?D.I. WaterDistilled?D.I. Water Organic LiquidOrganic Liquid ANALYSISANALYSIS

NoNoWettable?Wettable? SelectSelect

SurfactantSurfactant

YesYes

Not DispersedNot Dispersed DispersedDispersedDispersion CheckDispersion Check

DispersedDispersedUltrasonic EnergyUltrasonic Energy Dispersion CheckDispersion Check WET SLURRYWET SLURRY

TreatmentTreatment ANALYSISANALYSIS

Not DispersedNot Dispersed

Select DifferentSelect DifferentSurfactantSurfactant

Fig. H-3:Fig. H-3: Selection procedure for dispersant when the properties of the sample are unknown Selection procedure for dispersant when the properties of the sample are unknown

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SampleSample DispersantDispersant

BaCOBaCO33 EthanolEthanol

CaCOCaCO33 0.1% NaPMP*, ethanol, isopropyl alcohol0.1% NaPMP*, ethanol, isopropyl alcohol

MgCOMgCO33 EthanolEthanol

AlAl22OO 33 0.1% NaPMP0.1% NaPMP

CeOCeO22 0.1% NaPMP0.1% NaPMP

MgOMgO EthanolEthanol

SiOSiO22 0.1% NaPMP0.1% NaPMP

TiOTiO22 0.1% NaPMP0.1% NaPMP

FeFe22OO33 Ethylene glycolEthylene glycol

Al(OH)Al(OH)33 0.1% NaPMP, ethanol0.1% NaPMP, ethanol

Ca(OH)Ca(OH)22 EthanolEthanol

Mg(OH)Mg(OH)22 EthanolEthanol

SiCSiC 0.1% NaPMP0.1% NaPMP

SiSi33NN44 0.1% NaPMP0.1% NaPMP

CuCu Ethylene glycolEthylene glycol

Ceramics raw materialsCeramics raw materials 0.1% NaPMP, ethylene glycol0.1% NaPMP, ethylene glycol

ClayClay De-ionized water, 0.1% NaPMP, 0.1% surfactantDe-ionized water, 0.1% NaPMP, 0.1% surfactant

CementCement 0.1% NaPMP, ethanol0.1% NaPMP, ethanol

Coal dustCoal dust 0.1% surfactant0.1% surfactant

Fly ashFly ash 0.1% NaPMP, 0.1% surfactant0.1% NaPMP, 0.1% surfactant

TonerToner 0.1% NaPMP, ethylene glycol0.1% NaPMP, ethylene glycol

DyesDyes O-xyleneO-xylene

Carbon blackCarbon black 0.1% surfactant0.1% surfactant

GypsumGypsum EthanolEthanol

WaxWax De-ionized water, 0.1% surfactantDe-ionized water, 0.1% surfactant

LatexLatex De-ionized water, 0.1% surfactantDe-ionized water, 0.1% surfactant

Coffee, cocoaCoffee, cocoa De-ionized waterDe-ionized water

ChocolateChocolate Food oilFood oil

Powdered milkPowdered milk OctanolOctanol

PepperPepper 0.1% surfactant0.1% surfactant

PharmaceuticalPharmaceutical XyleneXylene

*NaPMP stands for sodium polymetaphosphate.*NaPMP stands for sodium polymetaphosphate.

Table H-1:Table H-1: Typical samples & dispersants Typical samples & dispersants

APPENDIX: SAMPLING & DISPERSIONAPPENDIX: SAMPLING & DISPERSION

APP-20APP-20

Table H-1 shows typical examples of samples and dispersants.Table H-1 shows typical examples of samples and dispersants.

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