LA-920

Instruction Manual Overview

Chapter 1 1.1

Overview

The measurement of particle size distribution is used for fundamental studies and quality control in production process in a many diverse fields such as fine ceramics, cement, pharmaceuticals, metal powders, industrial minerals and ores, coatings and adhesives, pigments and dyes, carbon black and other mineral additives and fillers used in the rubber plastics and paper industries, explosives, solid fules, food, drugs and beauty care emulsions, micelles, polymers- and others. Particle sizes ranging from 0.02 to 2000 microns are divided into 85 sectors, and the full range is measured at one time with no adjustments. Measurement time is adjustable, but usually 20 seconds is used. Many options such as a batch type cell holder, an auto-sampler, and a dispersion diluter are available. Note: Any sample cell other than those for the LA-920 cannot be used.

1.2

Configuration The sample carrying liquid is circulated The computer screen is used for displaying and

The LA-920 is configured as shown below. by the centrifugal circulation pump.

setting the conditions for both 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 a blue(405 nm) monochromed tungsten lamp. The light emitted from the laser and the tungsten lamp is radiated on the particles suspended in the liquid. After the laser beam has been dispersed and scattered by the particles in the flow cell, it passes through the condenser lens and is focused on the forward ring silicon diode array , comprised of 75 separate detection elements. to 138 from the forward direction. The scattered light from the tungsten lamp is sensed by 6 wide-angle silicon diode detectors, ranging in angles up The intensity of this scattered light from both the laser and tungsten lamp is converted into electrical signals, which are then used to calculate the size distribution of the particles.

Fig 1-1 Configuration of LA-920 System Chapter 2 2.2 1. Installation

Unpacking Unpack the packing case. Check them

The standard accessories are included in the upper section of the case. with Table 1 below. Table 1 LA-920 Accessory kit Name Power cable RS-232C cable Instruction Manual Program Manual Fuse Phillips screwdriver System program disk (software) LA-920 software disk Drain hose Drain hose 1m 1m 3.5 2HD type 13.5/9.5mm 9.5/6.5mm 2 1 8 3.5 2HD type 3.15A Time Lag Operation Qty 1 1 1 1 For connecting PC Remark

Hose end and socket Small hose band Large hose band Cotton swabs Tungsten lamp

1 ea. 2 2 1 carton 1 100 pcs./carton 50W, for mounting to main unit Be sure to use more

Caution: The main unit weighs approximately 55 kg (129lb). than one person to lift or carry it. 2.

Be sure to raise the LA-920 with a minimum of two persons holding the slots on

each side of the internal carton. The carton is made up as shown in Fig. 2-1. unit as a dust-cover after installing the unit. the vinyl cover. 3. Be sure to place the unit on the installation mount with a minimum of two Use the vinyl cover wrapped over the Also remove the desiccant pack from

persons holding both sides of the unit. Fig. 2-1 Unpacking Names and Functions Pre-treatment section lid

Chapter 3 3.1

Front and Top Views of Main Unit

Power Indicator Pre-treatment section lid

Fig. 3-1

Front view

Sample dispersion chamber lid of the centrifugal pump recirculation system. Power Indicator

Pre-treatment section lid

Sample chamber lid

Fig. 3-2 Sample dispersion chamber lid Sample cell chamber lid Lid Lid for sample chamber 3.2 Right Side View of Main Unit

Top view

Drain outlet

Fig. 3-3 Right side view Drain outlets, used to connect to the drain hoses. Autofill pump inlet, used to connect to customer dispersion liquid supply line or reservoir. Auto-diluter inlet, used to connect to auto-diluter dispersion reservoir. 3.3 Rear Panel of Main Unit

Connectors for options

Power switch Fuses

RS-232C connector Reset switch

AC connector Vents for fan

Fig. 3-4 Power switch Used to turn on the LA-920. AC connector Used to connect the power cable to. Fuses Fuses for the LA-920. Vents for fan

Rear panel

Their ratings are 3.15A Time lag.

Vents for the fan which is used to cool the power source. RS-232C connector Used to connect the RS-232C cable from the PC to. Reset switch Pressing this switch resets the unit.

Never block them.

Connectors for options These connectors are used for the optional auto-sampler and reservoir.

3.4

Sample Cell Chamber

Tube for circulation

Sample cell holder

Retaining screws

Fig. 3-5

Sample Chamber

Sample cell holder A unit to hold the sample cell. Tube for sample recirculation A tube used to recirculate the sample through the cell. Retaining screws Screws used to retain the cell holder to the mount on the main unit. Lid Lid for sample chamber Chapter 4 4.1 Maintenance

Daily Care

At start-up 1) While warming up the unit, circulate dispersant fluid for a minimum of 30 minutes. 2) When the analyzer has been warmed up, drain off the dispersant fluid, inject a fresh supply of dispersant fluid, and circulate it briefly (for about 30 seconds) and drain it off again. At shutdown Drain off the fluid in the cell, rinse, inject fresh dispersant fluid again, circulate for 3 minutes and drain off. If a water soluble-solution is used as the dispersant fluid, the (Do not inject excessive detergent as this will hinder circulation system can be cleaned more easily by injecting in 1-2 drops of a natural or weak alkaline liquid detergent. the rinsing operation.) *If the outer surfaces of the analyzer are dirty, clean them with a dry cloth or wipe off with a gauze dampened with a neutral detergent. *Clean the sample cell. 4.2 1. Cleaning the Cell After making sure that there is no dispersant in the cell, loosen the four retaining Do this once again with another fresh supply of dispersant fluid.

screws holding the top sample cell transition piece on the cell holder, and remove the top transition piece. 2. Clean the cell and the O-ring with the dispersant.

Use a cotton applicator or soft cloth for this purpose. Caution: Since the outside cell surface is coated so as to prevent any reflection of light, take care that it is not exposed to detergent or chemical agent when cleaning the cell. 3. 4. Use a cotton applicator to clean the O-ring slits in the holder, top and bottom. Fit the O-ring and the cell to the cell holder. Place the top transition piece on

the cell holder and then turn the retaining screws clockwise to retain the cell. Caution : *If samples that adhere to the cell were measured, clean the cell, and also make sure that the sample does not adhere to the wet part of the cell. *If there is too much sample adheres, remove it from each part using sponge or a plastic scraper.

*The outside surface of the cell should be cleaned with a cotton applicator or soft cloth. Never scrub it, nor touch it with anything hard.

4.3

Replacing the Fuses

If the fuses are blown, replace them with those delivered with the LA-920. 1. 2. 3. Turn off the power switch. Disconnect the power cable. Replace the fuses. Fig. 3-4. 4. 5. 6. There are two fuses. The locations of the fuses are shown in

Never use any fuse that is not specified.

Connect the power cable. Turn on the power switch. Check to see that the LA-920 operates normally. Never

Caution: If the fuses are still blown after the replacement, immediately turn off the power switch, disconnect the power cable, and then contact a service center. use any fuse other than those specified. 4.8 Storage

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

carefully. The analyzer must be stored where it will not be exposed to temperatures exceeding a range of 5(40F) - 40C(104F). If the unit has been stored for a long time, be sure to carry out all the appropriate steps described above before attempting to conduct measurements.

Appendix A. Specifications

Principles of measurement Based on Mie scattering theory Range of particle size displayed 0.02 to 2000m Measurement time Approx. 20 seconds, normally from start of measurement to display of data (max. 3 min). Amount of sample liquid required for measurement 10 mg to 1 g per measurement, about 200 ml of dispersant fluid when using the flow cell - This figure depends on the sample. Optical system Light source: 632.8 mm He-Ne laser, 1 mW Tungsten halogen lamp, 50 W Photo-cell detector: 75-division, ring shaped silicon photo-diode array Silicon photo-diode x 12 Sample recirculation system Ultrasonic chamber 30 W, 22.5 kHz. Circulation pump Centrifugal pump, discharge volume 8 l/min (in case of distilled water), 15-step selection, teflon-tubing

Sample flow cell Tempaxglass Power 100/110 to 200/220 to 240 VAC, selectable, 50/60 Hz approx. 300 VA Communications RS-232C Proper operation temperature and humidity 10(50F) to 35C (95F) less than 85% RH (no condensation) Dimensions 690 (W) x 525 (D) x 355 (H) mm 17.2(W) x 20.6 (D) x 14(H) inch Weight Approx. 55 kg, 121 lb. Options Reservoir Unit (for automatic concentration adjustment and rinsing) Auto Sampler (automatic injection and measurement of up to 24 samples) Fraction cell holder with magnetic stirrer *Fraction cell Dry Aerosol Feeder

B.

Principles of Measurement

This analyzer measures the particle size distribution by angular light scattering technique. The light scattered intensity of particles at the photo-cell detector is shown below. When light goes into a spherical particle of radius r, the following three types of light will be emitted, as shown in Fig.B-1. 1. 2. Light which reflects at the outer surface of the particle Light which passes through the inside of the particle and then reflects at the inner surface of the particle

3.

Light which passes through the inside of the particle, and refracts and continues to pass through the particle.

General geometrical handling of scattering phenomenon

All of these phenomena can be handled as light scattering. a strict application of Maxwells electromagnetic equation. theory is precise, but difficult to use. can be stated as:

Generally, light

scattering can be often explained by the Mie scattering theory which was obtained by The Mie scattering Therefore, a simple approximation is generally

used; i.e., relationships between the incident wavelength and the particle radius r

When the particle size is considerably less than , it is considered to be Rayleigh scattering. When the particle size is considerably greater than , it is considered as Fraunhofer diffraction. According to Fraunhofer diffraction theory, the scattered light intensity distribution of a particle, as shown in Fig. B-2, can be expressed by the following equation:

2 J ( x) I = I0 1 x

...........

5.1.1

I0: Intensity at the center of the diffractive pattern J1: Fist order spherical primary Bessel function

x=

2rs f

...........

5.1.2

r: Radius of particle s: The radial distance as measured from the optical axis : Wavelength of incident light f: Focal length of the lens According to the Mie scattering theory, when monochrome light enters a single spherical particle, the intensity, I, of scattered light in a certain direction from that particle is, as shown in Fig. B-3, determined by (A) the particle-size parameter, (= 2r/) which is defined by the ratio of the circumferential length of the sphere to the wavelength of the incident light, , and (B) the relative refractive index, m, the diagram below. ( = 2/1) See which is the ratio of the refractive index of the particle to that of the medium.

2 I = 2 2 (i1 + i2 ) 8 R
where

...........

5.1.3

: Wavelength of incident light

2n + 1 i1 = {a n n + bn n } n =1 n( n + 1)

...........
2

5.1.4

2n + 1 i2 = {bn n + a n n } n =1 n( n + 1)

where

S n ( )S n ( ) mS n ( )S n ( ) an = S n ( ) n ( ) m n ( )S n ( ) mSn ( )Sn ( ) Sn ( ) Sn ( ) bn = mSn ( ) n ( ) n ( ) Sn ( ) Sn ( ) = J 2 n + 12

 J 1 ( ) 2 ( n + 2 ) n ( ) = S n ( ) + iCn ( ) 1 n = P (1)( cos ) sin n n = P (1)( cos ) n Cn ( ) = ( 1)

J is the Bessel function and Pn(1) the associated function of Legendre, i.e.,

i = 1 m= 2 1

1 : Refractive index of light in medium 2: Refractive index of light in particle = ma

2r

The scattering intensity, I, varies depending on the direction in which light scatters from the particle, i.e., according to the scattering angle. As shown in Fig. B-4, the scattered light is classified according to the scattering angle as follows:

0 < 90 :forward scattering = 90 :side scattering 90 < < 180 :back scattering

The intensity, I , 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. If the incident wavelength is constant, when the particle size is larger than the incident wavelength, the scattered light focuses almost entirely in only the forward direction, 90, and varies depending on the particle size. the ratio of 1:1. More specifically, the relation between the particle-size distribution and the light-intensity distribution is Therefore, if the light-intensity 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 scattered light gradually shifts toward the side and rear, and finally spreads in all directions. When the particle size is smaller than 0.1 m, the absolute value of the scattered-light intensity varies much more than before. In this situation, the intensity distribution of the front scattering does not depend on the particle size, becoming almost constant.

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

C.

Principles of the optical system used in the Model LA-920

The optical system in an ordinary laser-diffraction type analyzer condenses the forward scattering from a laser beam with a condenser Fourier lens and forms an image on the ring-shaped detector located at the focal distance. Using only this method, however, it is difficult to measure the range of small particle sizes, in particular, particles under 0.1 m. beam, i.e., 632.8 nm. intensity. Very small particles cannot be measured merely by means of the forward scattering using the wavelength of a He-Ne laser To measure such particles, it is necessary to have either information from the side and back scattering or that from the polarization scattering Therefore, as shown in Fig. C-1, the new optical system in the Model The light source used for LA-920 uses three separate sets of detectors, one each for the wide angle and back scattering, and a third detector for the forward scattering. tungsten lamp, filtered at 405 nm. detecting scattered light at wide angles and back scattering in the Model LA-920 is a This means: (1) the small angle forward scattered light is conventionally given by the He-Ne laser and detected by the ring detectora array, and (2) the wide angle and back scattered light is given by the tungsten lamp and detected by individual the forward detector array. photo-diodes located at larger angles from

Fig. C-1

Measuring the side and rear scattered light of blue-colored (405 nm) light

Particle size distribution analysis Particles of various sizes exist in an actual sample solution, and their scattering light differs according to their size. Equation 5.2.1 shows the relationship between the intensity distribution of the scattering light and the particle size distribution.

g( ) =
where

K ( , D) f ( D)dD
0

...........

5.2.1

g() : the intensity distribution of the scatted light K(,D): response coefficient of scattered light f(D): particle size distribution coefficient D: particle diameter : scattering angle In reality, measurement is performed by n number of detectors. corresponding to equation 5.2.1 becomes equation 5.2.2. As the Mie

scattering theory is used in combination for the response function, the equation

g( N ) = K ( N , Di) f ( Di)D
i =1

...........

5.2.2

where g(N) : output of N-th detector K(N,D): response coefficient of N-th detector f(Di): Particle size distribution Di: i-th representative radius D: particle size segment number The particle size distribution f(Di) is calculated from the relationship between the output of the detector (expressed by equation 5.2.2) and the response function of the detector. f(Di) is calculated on the basis of volume.

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

Distribution by area basis =

f ( Di) Di

{ f ( Di) Di}
i =1

...........

5.2.3

Distribution by length basis =

f ( Di) Di 2

{ f ( Di)
i =1

Di

...........

5.2.4

Distribution by number basis =

f ( Di) Di 3 Di
3

{ f ( Di)
i =1

...........

5.2.5

The specific surface area is calculated by equation 5.2.6, on the assumption that the particles being measured are perfectly spherical. Specific surface area = 6 10

{ f ( Di) Di}(cm
i =1

cm3

...........

5.2.6

Di D.

representative particle diameter

Spare Parts and Options

Spare Parts Part number Fraction cell Flow cell Options *LY-201 *LY-202 *LY-203 Reservoir Autosampler Fraction cell holder U802030100 U802030000

(Please use together with Fraction-type cell)

E.

LA-920 RS-232C Specification

Transmission format The transmittance format is as follows. If the setting need to be changed, please contact HORIBA for advice and assistance. HORIBA will reset the setting as necessary. Table RS-232C Transmission format Baud rate : 9600 bps Data length : 8 bits Parity check : NONE Parity : NONE Stop bit : 1 RS-232C cable The LA-920 should be connected to the Compaq PC by the supplied cable. Connection diagram for the RS-232C cable

RS-232C Connector terminal numbers Cable end as seen from terminal side.

G.

List of the Refractive Index Values

Table of Inorganic Substances Substance Composition Sp-gr Refractive index, n1 of particle Lead white Zink flower Titanium oxide(rutile) Titanium oxide(anatase) Zinc sulfide Lead titanate Ziconium oxide Barium sulfate Barium carbonate Calcium carbonate Gypsum Alumina Iron oxide Red lead CaSO4.2H2O Al2O3 Fe2O3 Pb3O4 2.4 4.8 8.9 1.55 1.66 2.90 2.42 1.16 1.25 2.17 1.82 CaCO3 2.8 1.58 1.18 ZnS PbTiO2 ZrO BaSO4 BaCO3 4.0 7.3 5.7 4.4 4.3 2.37 2.70 2.40 1.62 1.60 1.78 2.03 1.80 1.22 1.20 TiO2 3.9 2.50 1.88 Pb3(CO3)2(OH)2 ZnO TiO2 6.8 5.6 4.2 2.02 2.00 2.75 Relative refractive index (RRI) m(n0=water) 1.51 1.50 2.06

Mercuric sulfide Lead chromate Cadmium sulfide Zinc yellow Strontium yellow Barium yellow Chrome green Emerald green Chromium oxide Cobalt green Ultra marine Prussian blue Cobalt blue Celuriene Cobalt violet Manganese violet Silver chloride Fluorite Germanium Potassium bromide Potassium chloride Lithium fluoride Magnesium oxide Silicon Quartz Rock crystal Diamond Sapphire Magnesium

HgS PbCrO4 CdS ZnCrP4 SrCrO4 BaCrO4 Cr2O3 CoO.nZnO Na7Al6Si6O24S3 Fe4[Fe(CH)6]3 CoO.nAl2O3 CoO.nSnO2 Co3(PO4)2 (NH4)2Mn2(P2O
7)2

8.0 6.0 4.4 3.5 4.4 4.1 3.2 5.1 2.4 1.8 3.8 -

2.95 2.40 2.42 1.87 1.96 1.63 2.40 1.97 2.50 1.97 1.57 1.56 1.74 1.84 1.72 1.70 2.08 1.43 4.10 1.58 1.80 1.39 1.76 3.50 1.45 1.54 2.41 1.76 1.37

2.21 1.80 1.81 1.40 1.47 1.22 1.80 1.48 1.88 1.48 1.18 1.17 1.31 1.38 1.29 1.28 1.56 1.07 3.07 1.16* 1.32* 1.04 1.32 2.63 1.09 1.16 1.81 1.32 1.03

AgCl CaF Ge KBr KCl LiF MgO Si SiO2 SiO2 Al2O3 MgF2

fluoride Mica Kal2(AlSi3O10)( OH)2 BaCa2(C3H5O2)6 Barium fluochloride Barium fluoride Barium phosphate Barium sulfide Calcium alminate Calcium borate Carbon Chromium oxide Copper oxide Copper sulfate Magnesium orthoborate Potassium carbonate Potassium hydrogencarbo nate Potassium cyanide Potassium chlorate Sodium bromide Sodium cyanide Sodium metasilicate Sodium sulfate Strontium Na2SO4 SrCr2O7.3H2O 1.55 1.71 1.28 1.08 Na2SiO3 1.52 1.14 NaCN 1.45 1.12 NaBr 1.64 1.06 KClO3 1.62 1.20 KCN 1.41 1.22 KHCO3 1.48 1.04 K2CO3 1.50 1.09 Cu2O CuSO4 3MgO.B2O3 2.71 1.73 1.65 1.27 1.24 1.10 CaO.B2O3 C Cr2O3 1.60 1.92-0.522 2.50 1.20 1.88 2.03 BaS Ca3Al2O3 2.16 1.71 1.59 1.28 BaHPO4 1.62 1.22 BaF2 1.47 1.10 BaC12.BaF2 1.45 1.64 1.09 1.23 1.59 1.19

dichromate Strontium fluoride Strontium sulfide Zinc metasilicate Iron Zinc Gold Silver Copper Aluminum Antimony Magnesium Manganese Nickel Platinum Fe Zn Au Ag Cu Al Sb Mg Mn Ni Pt 2.4-1.4i 2.4-5.5i 0.34-3.2i 0.19-3.4i 0.6-3.6i 1.6-5.4i 3.2-5.0i 0.4-4.6i 2.5-4.0i 1.8-3.6i 2.9-4.5i ZnSiO3 1.62 SrS 2.11 1.22 SrF2 1.44 1.58

Taken from 1) Handbook of chemistry and physics., C.R.C. Press, 2)American Institute of Handbook., MaGraw-Hill and 3) The Merck Index., MERCK & Co., Inc. n0 of this value is methanol.

Table of Organic Substances Substance Composition Sp-gr Refracti n1 Asphalt Ebonite Opal Canadian balsam Amber Ivory Vinyl chloride resin Vinyliden chloride -1.63 1.66 1.44 1.52 1.54 1.54 1.54 1.61 Relative index refraction m(n0=water) 1.22 1.25 1.08 1.14 1.16 1.16 1.16 1.21

ve index, of

resin Vinyl acetate resin Silicon oil Tetrafluoroethylene resin Nylon Polyethylene Polystyrene Methylmethacrylic acid resin Melamine resin 1.60 1.20 1.53 1.53 1.60 1.49 1.15 1.15 1.20 1.12 1.46 1.40 1.35 1.10 1.05 1.01

Taken from 1)Handbook of chemistry and physics ., C.R.C. Press, 2) American Institute of Handbook, MaGraw-Hill and 3) The Merck Index., MERCK & Co., Inc.

H. Sampling and Dispersion 1. Sampling Methods This measurement sample must,

A representative sample is required in order to measure the particle size distribution of powders or particles suspended in a liquid. therefore, have the same particle size distribution as the overall sample. Obviously, when extracting measurement samples from a large reaction vessel, sample drawn from the top will have a different particle size distribution from samples drawn from the bottom. Small and heavy particles collect at the bottom of the vessel. segregation. This is called

Taking samples from the upper and lower levels of the vessel is

appropriate if the degree of particle settling is to be measured, but for particle size distribution measurements, meaningless, unreproducible data will be obtained unless suitable sampling techniques are employed. Sampling methods for powders 1. Take samples of equal weight from throughout the material. 2. Use a twin divider or rotary splitter. 3. Use the conical quartering or flow division method. (see Figs. H-1 and H-2.) 4. Disperse a large amount of the sample in a 215-315 ml dispersion medium.

5. Disperse evenly with ultrasonic energy or a stirrer. 6. Draw off a measurement sample while agitating and pour it into the cell. Particles suspended in a liquid 1. Do not dilute at once in a large amount of dispersion medium, but carry out the dilution over several smaller stages. 2. Agitate well while diluting. 3. Dilute in the same dispersion medium as the medium used in the original sample. 4. Disperse evenly with ultrasonic energy or a stirrer. 5. 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 to suit the properties of the sample, as some particles (particularly fine particles) adhere or cluster together if they are made damp by humidity. Particles in solids 1. Dilute the solid containing the particles in an appropriate solution (a) Use the diluted samples as the measurement sample. (b) Remove only the particle and measure. Clean until the dissolved solid has completely been removed and extract the particles. All further operations are the same as in (a).

Fig. H-1

Fig. H-2 2. Dispersing Methods for Samples

As the LA-920 carries out measurements with the particles in a diluted state, the dispersed state of 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 are measured and the distribution is unnatural if particles agglomerate. Alternatively, when a dispersant of the sort that dissolves the powder is used, particles are measured 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 used and the dispersion method must be chosen carefully. Dispersion Methods Samples with Stable Particles The sample can be irradiated with ultrasonic energy from the internal ultrasonic

probe in the flow loop, and the agglomerated particles are thus dispersed. The ultrasonic time depends on the sample. normally adequate. coagulate or be damaged. solution. The LA-920 allows an ultrasonic time of up to 30 minutes to be set. allows the power to the ultrasonic probe to be adjusted also. dispersed. The LA-920 However, 10 seconds to 1 minute is

If vibration is carried out for too long, the particles may However, the ideal ultrasonic time must be

experimentally determined for each sample in order to thoroughly disperse the

The higher the power

setting, the more ultrasonic vibration is employed and the more the particles are The power setting can be varied from a low setting of 1 to a high of 7.

Samples with Unstable (Fragile) Particles When measuring such particles using the flow cell, do not apply ultrasonic vibration. If even this damages the sample, conduct the measurement by placing a sample that has been dispersed manually in the small volume cell. Selecting the Dispersant It is important that the dispersant properly wets the sample powder. chemical reaction. Water is used in most cases. However, in some cases, measurement may be carried The

dispersant must be one that does not cause coagulation, dissolving, swelling or

out using organic solvents such as ethanol or ethylene glycol. Effect and Type of Dispersant Powder samples are generally charged, and may coagulate or may not be sufficiently dispersed due to the interaction with the solution. The role of the dispersant is to Widely increase this interaction and to disperse each and every one of the particles.

used dispersants are sodium hexametaphosphate and sodium pyrophosphate. Surfactants are also used for hydrophobic (preferentially wet by oil or air) or lipophilic (preferentially wet by oil) particles. However, if there is an excessive amount of dispersant, the dispersant will coagulate. 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 about 0.1-0.2% is widely used due to its stability.

Table H-1 shows typical examples of samples and dispersants. Table H-1 Sample BaCO3 CaCO3 MgCO3 Al2O3 CeO2 MgO SiO2 TiO2 Fe2O3 Al(OH)3 Ca(OH)2 Mg(OH)2 SiC Si3N4 Dispersant Ethanol 0.2% NaHMP*, ethanol, isopropyl alcohol Ethanol 0.2% NaHMP 0.2% NaHMP Ethanol 0.2% NaHMP 0.2% NaHMP Ethylene glycol 0.2% NaHMP, ethanol Ethanol Ethanol 0.2% NaHMP 0.2% NaHMP

Cu Ceramics raw materials Clay Cement Coal dust Fly ash Toner Dyes Carbon black Gypsum Wax Latex Coffee, cocoa Chocolate Powdered milk Pepper Medicine

Ethylene glycol 0.2% NaHMP, ethylene glycol De-ionized water, 0.2% NaHMP, 0.1% surfactant 0.2% NaHMP, ethanol 0.1% surfactant 0.2% NaHMP, 0.1% surfactant 0.2% NaHMP, ethylene glycol O-xylene 0.1% surfactant Ethanol De-ionized water, 0.1% surfactant De-ionized water, 0.1% surfactant De-ionized water Food oil Octanol 0.1% surfactant Xylene

NaHMP stands for sodium hexametaphosphate.