LS-32003 Solid Liquid Extraction 80415

LS-32 003 SOLID LIQUID EXTRACTOR

LS-32 003 SOLIQ LIQUID EXTRACTOR

II

This is an authorized copy of the Experimental & Operations Manual. Copyright Notice © Lotus Scientific (M) Sdn. Bhd. All rights reserved. No part of this publication may be copied, reproduced, translated, stored in a re-trieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording or otherwise, in whole or in part without prior permission of Lotus Scientific (M) Sdn. Bhd. Limit of liability/disclaimer of warranty While the publisher and author have used their best efforts in preparing this manual, they make no representations or warranties with respect to the accuracy or completeness of the contents of this manual and specifically disclaim any implied warranties of merchantability or fitness for a particular purpose or those arising by law, statute, usage of trade, course of dealing or otherwise. Neither Lo-tus Scientific (M) Sdn. Bhd. nor its dealers or suppliers shall have any liability to you or any other person or entity for any indirect, incidental, special, or consequential damages whatsoever, includ-ing, but not limited to, loss of revenue or profit, lost or damaged data or other commercial or eco-nomic loss, even if we have been advised of the possibility of such damages, or they are foresee-able. Proudly Manufactured in MALAYSIA Product Serial Number : LS-32 003 Date of Production : April 2008 Manual Serial Number : 80415 Date of Print : 9th september Project Manager : Chan. W. K Authorized by : Lee. Y. W

COPYRIGHT


III

1. Safety Instructions ............................................................................... 1

2. Description .......................................................................................... 2

3. Theory ................................................................................................. 5

4. Setup ................................................................................................. 10

5. Experiments ...................................................................................... 12

6. Manufacturer’s data .......................................................................... 18

7. Components List ............................................................................... 27

CONTENT


1

READ INSTRUCTIONS COMPLETELY BEFORE STARTING EXPERIMENT Normal operation of the equipment is not considered hazardous. However, the RECOMMENDED PROCEDURES SHOULD BE FOLLOWED to be sure that the classroom instruction is performed under the safest possible conditions. If the student knows and understands the principle and opera-tion of the parts in the system, it will help him/her to operate the equipment safely. THE STUDENT SHOULD ALWAYS BE ALERT to experimental procedures which may be a hazard to the operator or be injurious to the equipment. Every control device and switch has a specific op-erational application. Be certain that all connections and control settings are carefully managed. NO SETTINGS SHOULD BE MADE INDISCRIMINATELY. STUDENTS PERFORMING THE EXPERIMENTS SHOULD BE SUPERVISED. Even the most ex-perienced student should never be allowed to operate it while alone. Always have good lighting and ventilation when performing the experiments. Instruments used in testing, while durable, are sensitive to abuse. When connecting an electrical instrument into a circuit, make sure that the instrument and its settings are within the voltage and current range to be applied to the instrument. This will protect the supervisor, the student and the equipment. Use extreme CAUTION when making electrical measurements. Remember, it is too late to learn that a circuit is live after one has touched it. Be certain that the STUDENT knows if the instrument is on or off at all times. Never handle live circuits when in contact with pipes, other wires, or damp floors. Keep the floor clean of debris – oil, water, or other slippery material. An electrical short across a ring or wristwatch can cause a severe burn. It is best to remove all watches and jewelry when working on electrical equipment. DISCONNECT the electrical power source before isolating any component from the instrument. Lock the switches open to prevent someone from closing them during demonstration or test proce-dure. Hands-on experience is an important teaching tool. However, most accidents are the result of CARELESSNESS - when students are concentrating on their lessons, they tend to momentarily ne-glect safety. Therefore, like the service technicians, the students must train themselves to do things safely. They must study the job for its safety problems before starting and think about safety aspects before each step. Refer all repairs to qualified personnel.

SAFETY

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PRODUCT DESCRIPTION


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DESCRIPTION

DESCRIPTION The Solid-Liquid Extractor enables the extraction of soluble components in a solid mixture. When running on a continuous 3-stage mode, the pure solvent (water) is first delivered to a nozzle from a tank using a feed pump. The solvent is then distributed over the solid mixture, dissolving the soluble components and carrying them into the collecting segment. Then, the enriched solvent is carried to the nozzle of the next stage. The solvent, after passing through the last stage, is collected in the extract tank. A feed mechanism continuously delivers ex-traction material into the cells of the rotating extractor. The extraction material composes of a mix-ture of potassium bicarbonate and special carrier material. The solvent and extraction material trav-els in counter-current flow, with the depleted extraction residue dropping into a tank after one rota-tion of the extractor. The extractor can be set to run on either 1, 2 or 3-stage continuous mode by regulating the control valves. A continuous mode is also possible by stopping the carousel. Three pumps with adjustable flow rate are supplied for delivering the solvent to each stage. Each stage is also equipped with PID temperature control with temperature display as well as conductivity meters for monitoring the sepa-ration process. All measured parameters are displayed on digital meters. EXPERIMENTAL CAPABILITIES • To perform solid-liquid extraction as a continuous or discontinuous process • To investigate 1, 2 and 3-stage separation processes • To determine the effects of revolving speed and extraction material feed rate on the separation

process • To determine the influence of temperature and solvent flow rate on the extraction process


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DESCRIPTION

TECHNICAL SPECIFICATIONS Revolving extractor for operating continuous or discontinuous solid-liquid extraction • Extraction material feed rate : 0 - 3 L/hr • Extractor speed : 0 - 4 rev/hr 1, 2 or 3-stage modes; each stage includes • Solvent feed pump with adjustable flow rate : 0 - 20 L/hr • PID temperature control for solvent, up to 50°C • Temperature and conductivity measurement at stage inlet and outlet Four separate process tanks • Feed tank • Extraction residue tank • Solvent tank • Extract tank Extraction material : Potassium bicarbonate with special carrier component Solvent : Distilled water The unit can be connected to our Lotus dedicated Data Acquisition System with necessary interfac-ing hardware and Lotus software for data capture and analysis as well as graph plots. A branded desktop PC with latest Pentium processor shall be provided. All measured signal values are dis-played on the software interface with process flow diagram. Colored copy of Operations and Experimental manual in English with test data, sample calculation and student’s experimental sheet is provided. ELECTRICAL REQUIREMENT: 230 VAC Single phase 50 Hz OVERALL DIMENSIONS: 1200 x 700 x 1700 mm (L x W x H) GROSS WEIGHT: 100 kg ORIGIN: Made in MALAYSIA Note: Due to our continuous research & development program, we reserve the right to improve upon the above specifications and design without prior notice.

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THEORY


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THEORY INTRODUCTION A solid-liquid extraction is also called as Leaching. The principle for leaching is that the soluble com-pounds of a soli of matter, existing of an inert and the active agent, are extracted by a solvent. The extract can be included in the extraction matter in solid or liquid form. It can be included in cells like in oil in oil seeds or as fine dispersion on the solid matter like caffeine in coffee. The extraction material is no homogeneous substance but exits of a lot of capillaries. The solvent enter the capillaries and solutes the extract, then produce a high concentration solution. Because of diffusion a concentration change between the solution in the extraction material and the solution sur-rounding the solid particles take place. At the end of extraction, the extracted substance still contain a small amount of solvent. Therefore it is no complete extraction possible practically. The solution remain in the solid material has the same concentration on active compound as the extract. For equilibrium, the whole amount of active compound is assumed dissolved in the solvent. In solid-liquid extraction, sufficient solvent is provided to dissolve all the solute in the entering solid and there is no adsorption of solute by the solid, equilibrium is attained when the solute is com-pletely dissolved and the concentration of the solution formed is uniform. In equilibrium system, the concentration retained by the solid leaving any stage is the same as that of the liquid overflow from the same stage. The equilibrium relationship is simply

Figure 1: ideal equilibrium

yx e =


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TYPE OF EXTRACTOR Hildebrandt extractor Figure 2 shows the Hildebrandt extractor. The solid material is extracted according to the immersion method. Screw converyors are installed in the extractor for transporting the solid material. Again the solvent flows countercurrent to the solid materials through the extractor. Bonotto extractor The Bonotto extractor is operate in countercurrent extraction following the immersion method. The solid material is transported by the mixer on the tray until it reaches the open sector where the solid material falls down on the next tray, the screw conveyor at the outlet withdraws the extracted solid material and prevent the flowing out of the solution from the extractor.

Figure 2: Hildebrandt extractor

Figure 3: Bonotto extractor


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Moving bed leaching Figure 4 showing a typical Rotocell or Carousel extractor. This type of extractor is a continuous sys-tem. This extractor consists of a fixed tray and a rotating star wheel, which produces the single ex-traction chamber. The tray rotates slowly about a vertical axis. Solids are admitted to each compart-ment at he feed point; the compartments then successively pass a number of solvent sprays, a drainage section, and a discharge point at which the floor of the compartment opens to discharge the extracted solids. To give countercurrent extraction, the fresh solvent is fed only to the last com-partment before the discharge point, and the solids in each preceding compartment are washed with effluent from the succeeding one.

Figure 4: Rotocel extractor

Figure 5: structure of Rotocel extractor


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The extraction system comprises of the following compound • Pure solvent, B • Inert material (exclude extractable substance), A • Extractable material, C The equilibrium is given in the triangle diagram as shown in figure 6. Solvent B and extractable sol-vent are completely miscible and therefore it is a system with two mixing gaps. The connodes have to go through point A because extract and solution in the solid particles have the same composition so that the ration C/B is constant The minimum amount of solvent is the coming closer of the mixing point to the binodal curve be-cause all connodes cross in point A.

Figure 6: equilibrium in the triangle diagram for solid-liquid extraction.

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SETUP


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LEGEND A = solid hopper B = rotary cell C = solvent pumps D = control panel E = solvent tanks F = product tanks

SETUP

A

B

C

D

E

F


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SAFETY / PRECAUTION 1. Do not touch the solvent tanks when conducting the experiment. 2. Do not touch the rotary cell when conducting the experiment. 3. Be careful when connecting the heat socket to the power source. 4. Do not attempt to change the setting of the digital power meter. SETUP 1. Place the LS-32003 Solid liquid extractor on floor. 2. Plug the 3 pin plug to the 240VAC main power supply. Turn ON the power supply. 3. Switch ON the power supply unit in front of the control panel. 4. Switch ON the rotary cell by turning ON the rotary cell ON/OFF switch. Try to regulate the rotary

cell speed by turning the regulator . 5. Pour some solid into hopper, then switch On the hopper ON/OFF switch, try to regulate the feed

screw speed by turning the speed regulator. 6. Fill in the tanks with water, then turn ON the heater with the ON/OFF switch, set the heater tem-

perature by pressing the UP/DOWN button. Keep an eye on the temperature meter and conduc-tivity meter.

7. The apparatus is ready to use if all the parts and components are working in order. MAINTENANCE 1. Please check the Rotary cell, heaters, thermocouple, and all other parts from time to time. En-

sure all of them are working properly. 2. Kindly seek the assistance from the manufacturer if necessary.

SETUP

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EXPERIMENTS


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EXPERIMENTS

LEGEND A = solid hopper B = rotary cell C = solvent pumps D = control panel E = solvent tanks F = product tanks

A

B

C

D

E

F


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EXPERIMENTS

PREPARATION Accessories 1. beaker 2. Balance 3. Potassium bicarbonate 4. 200ml water 5. Handheld conductivity meter Method to calibrate conductivity: Conductivity versus molarity graph used to determine the concentration of the solute in the final product. The graph can be obtained by simple experiment as stated below: 1. Prepare 200ml of water in a beaker, and dissolve 0.2g of potassium bicarbonate in the water.

(0.01M potassium bicarbonate solution) 2. Measured it with conductivity meter. Note: stir the solution, ensure no participate under the

beaker and no bubble trap in the conductivity probe. 3. Dissolve another 0.2g of potassium bicarbonate in the previous beaker. Obtain the conductivity

reading. 4. Repeat the procedure above while keep adding 0.2g of potassium bicarbonate until the concen-

tration of the liquid reach 2.0M.

Molarity Mass of KHCO3 Amount of H2O Conductivity (µS) 0.01 0.2 200ml 0.02 0.4 200ml

0.03 0.6 200ml 0.04 0.8 200ml 0.05 1.0 200ml 0.06 1.2 200ml 0.07 1.4 200ml 0.08 1.6 200ml 0.09 1.8 200ml 0.1 2.0 200ml 0.11 2.2 200ml 0.12 2.4 200ml 0.13 2.6 200ml 0.14 2.8 200ml 0.15 3.0 200ml 0.16 3.2 200ml 0.17 3.4 200ml 0.18 3.6 200ml 0.19 3.8 200ml 2.0 4.0 200ml

Table 1: Characteristic of conductivity on different concentration


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EXPERIMENTS

Preparation Method to prepare ceramic for experiment: 1. Wash the ceramic ball and allow the ceramic ball to dry in atmospheric temperature. 2. Dissolve 125.15g of potassium bicarbonate in 500ml of distillate water. 3. Put 1kg of clean ceramic ball into the solution. 4. After 2 hour, spread the ceramic ball on a flat tray. 5. allow the ceramic ball to dry in the oven ( Note: dry the ceramic balls at 50ºC for 30min.) 6. Weight the ceramic ball and note down the weight increase. 7. After the ceramic ball dried, keep it away from moisture surrounding. The ceramic ball can be prepared in different concentration by adding more potassium bicarbonate.


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EXPERIMENT 1 SAFETY / PRECAUTION 1. Do not touch the solvent tanks when conducting the experiment. 2. Do not touch the rotary cell when conducting the experiment. 3. Be careful when connecting the heat socket to the power source. 4. Do not attempt to change the setting of the digital power meter. PRE-EXPERIMENT PROCEDURE 1. Read the safety instruction given before conducting the experiment. 2. Read and understand the theory for solid liquid extraction (leaching) before lab session. 3. Prepare the specimen needed for the experiment. OBJECTIVE • Demonstration of solid liquid extraction. • Investigate the effect of solvent flow rates to extraction efficiency. ACCESSORIES 1. LS-32003 solid liquid extractor 2. Ceramic balls with chemicals EXPERIMENT PROCEDURE 1. Weight 1kg of ceramic balls. 2. Pour the ceramic balls into solid hopper. 3. Fill in solvent tank 1 with 7L of distilled water. 4. Set the heater temperature to 50°C. 5. Record down the initial conductivity. 6. Set the feed rate of solvent pump 10L/hr. 7. Switch on the rotary cell by the ON/OFF switch and set it to maximum rotation speed. 8. Switch on the solvent pump 1 by the ON/OFF switch . 9. When the liquid proceeds to the second solvent tank switch off the rotary cell. 10. Record the conductivity and repeat step 5 to step 8 for solvent pump2 and solvent pump 3. 11. Drain out the product tank water, and measure its volume and weight its mass. 12. Repeat the same procedure for the entire experiment with a higher solvent feed rate( 15L/hr).

EXPERIMENTS

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MANUFACTURER’S DATA


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0

2000

4000

6000

8000

10000

12000

14000

16000

18000

20000

22000

24000

26000

0 0.02 0.04 0.06 0.08 0.1 0.12 0.14 0.16 0.18 0.2

The above is a sample calibration curve for a dilute potassium bicarbonate solution. The horizontal axis shows the molarities of potassium bicarbonate while the vertical axis is the conductivity of the solution. To determine the concentration of a solution, the conductivity value is first measured using the con-ductivity meter. Then, read off the appropriate curve to determine the concentration. Example: For a potassium bicarbonate solution, the conductivity value was found to be 12000µS. The concen-tration of solution is then approximately 0.862M. † This calibration curve is valid for the manufacturer’s in-house conductivity meter only. ‡ Temperature has a major effect on conductivity value ensure that the values obtained for each point is at the

same temperature and volume.

Figure 7: conductivity versus molarity of potassium bicarbonate

MANUFACTURER’S DATA C

ondu

ctiv

ity (μ

S)

Molarity of potassium bicarbonate solution

Conductivity versus Molarity of Potassium Bicarbonate


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solvent feed rate 10L/hr 12L/hr

conductivity conductivity (KHCO3 basis) conductivity

conductivity (KHCO3 basis)

solvent tank 1 101 ‐ 101 ‐ solvent tank 2 303 202 318 218 solvent tank 3 376 275 393 292 product tank 405 304 427 326

EXPERIMENT 1 Result:

Solvent tank 1

Solvent tank 2

Solvent tank 3

Product tank

Con

duct

ivity

The effect of solvent feed rate to conductivity


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Experiment result: Sample calculation Initial weight of ceramic balls is 1kg. After preparation steps, the weight increase by 0.03kg. Hence, the mass fraction is Example : mass fraction of potassium bicarbonate is From the figure 7, determine the respective concentration on each conductivity. Set the initial feed (tank 1) conductivity as reference. Example: the initial conductivity shows is 101µS. Hence, Given the molecular weight of potassium bicarbonate is 100.11g/mol. Calculate the mass composition of potassium bicarbonate after the process. Example for tank 1: Therefore , approximately 0.4625g of potassium bicarbonate is dissolve into the water after process.

Ceramic ball Potassium bicarbonate

1000 30

Mass (g)

Mass fraction (%) 97.087% 2.913%

%100301000

30×

+=

gggm

%913.2=m

Initial conductivity (µS)

Final conductivity (µS)

Initial concentration (M)

0 202 0

202 275 0.000066

275 304 0.00116

Final concentration (M)

0.00066

0.00116

0.00138

Tank 1

Tank2

Tank 3

gKHCOofmol

gwaterfeedofLL

mol 4625.011.100700066.03 =××

concentration change(M) Mass of KHCO3 removed (g)

0.00066 0.4625

0.00116 0.8129

0.00138 0.9671


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Sample calculation: Amount of water collected in the product tank is 6950ml which is equivalent to 6950g. The final com-ponent in the product tank consist of water and potassium bicarbonate. The mass fraction of the component is present in the table below. Amount of KHCO3 in product tank is 0.9671g. Therefore the water amount is The fraction of KHCO3 in extract stream is The component exits in the underflow stream is : water, ceramic balls and potassium bicarbonate. The potassium bicarbonate remain in the ceramic balls is calculated as: The amount of water No losses for the amount of ceramics ball


Ceramic ball Potassium bicarbonate

1000 29.03

Mass (g)

Mass fraction (%) 92.59 2.69

water

51

4.72

Water , wt% Potassium bicarbonate, wt%

Mass fraction (wt%) 0.9998 0.0139

mass 6949 0.9671

ggg 69499671.06950 =−

%0139.0%1006950

9671.0 wtgg

=×

ggg 03.299671.030 =−

ggg 5169497000 =−


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Result is tabulated in the ternary diagram below:

F S

E

U



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MASS BALANCE (THEORETICALLY)

Figure about shown the flow diagram of the experiment. 1,2 and 3, represent the 3 compartments in the rotary cell. The Feed is the ceramic balls consist of potassium bicarbonate, Solvent is heated water used as the solvent to extract potassium bicarbonate out from the ceramic balls. Extracted is the water with potassium bicarbonate after the extraction process. Underflow is the retain ceramic balls after experiment. Overall balance Balance for compound A (ceramic balls), With the feed concentration And no solid particles are included in solvent, so

.

Hence, Balance for compound B (potassium bicarbonate), With the feed concentration And no solid particles are included in solvent, so

.

Hence,

Feed , L0

Solvent , V2

Underflow, L1

Extracted, V1

1 3 2

gggVLMVL 8030700010301120 =+=+==+

MAVALA wMwVwL ,,2,0 20=+

9709.00, =LAw

02, =VAw

MAwgg ,8030)0)(7000()9709.0)(1030( =+

1245.0, =MAw

MBVBLB wMwVwL ,,2,0 20=+

0291.00, =LBw

02, =VBw

MAwgg ,8030)0)(7000()0291.0)(1030( =+

03733.0, =MBw


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The concentration of compound C in the mixing point M can be determined either by mass balance for compound C With the feed concentration And no solid particles are included in solvent, so

.

Hence, Or by rule, that the sum of the mass percent of each compound in point M has to be 1. The concentration of underflow can be calculated as below. Solution is represent the total mass of extractable substance and solvent. Hence, The amount of the leaving flows L1 and V1 can be calculated from the mass balance for compound A. With no solid material in extracted (WA,V1=0) and WA,L1 =0.8755 With the total balance Follows

MCVCLC wMwVwL ,,2,0 20=+

12, =VCw

00, =LCw

MCwggg ,)8030()1)(7000()0)(1030( =+

8717.0, =MCw

1,,, =++ McMBMA www1)03733.0()01245.0( , =++ Mcw

8717.0, =Mcw

solventcesubseextractablmaterialinertsolutionw LA ++

=tan1,

8755.080307030

1, ==LAw

11 ,1,1, LAVAMA wLwVwM +=

ggww

MLLA

MA 11418755.01245.08030

1,

,1 =⎟

⎠⎞

⎜⎝⎛==

11 VLM +=

1.68889.1141803011 =−=−= LMV


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The concentration of compound B and C in stream V1 are calculated wit the assumption that no compound A is exclusive in the extracted stream. Where inert material is zero at stream V1

The concentration of compound B and C in stream L1 can be calculated by ,ass balance of com-pound B and C. Where, Hence Result tabulated as below:

solventmaterialeextractablmaterialinertmaterialeExtractablw VB ++

=1,

004267.07030

301, ==VBw

solventmaterialeextractablmaterialinertSolventw VC ++

=1,

99573.07030

301, ==VCw

2011 ,2,0,1,1 VBLBVBLB wVwLwVwL +=+

02, =VBw

1

,1,0,

1

1 LwVwL

w VBLBLB

o−

=

gggw LB 1141

)004267.0)(1.6888()0291.0)(1030(1,

−=

0005096.01, =LBw

A, wt% B, wt% C, wt% Feed , L0 0.9708 0.0291 0

Solvent, V2 0 0 1.000

Extracted, V1 0 0.0043 0.9957

Underflow, L1 0.8755 0.0051 0.1194

1194.0005096.08755.011, =−−=Lcw

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COMPONENTS LIST


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STORAGE CONDITION

Note : This machine may contain heat sensitive thermoplastic and

electronic components. Do not store in a place of temperature higher

than 40°C and lower than 10°C.

Any defects arising out of the improper storage condition will not be

considered a manufacturer’s defect and replacement of such af-

fected components shall be charged accordingly.

COMPONENTS LIST


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1. Rotating cell X1

2. Sieve tray X3

3. Feed tank X3

4. Product tank X3

5. Solid hopper X1

6. Conductivity probe X4

7. Conductivity meter X4

8. Feed pump X3

9. Thermocouple X3

10. Heater X3

11. Temperature meter X3

COMPONENTS LIST

LS-32003 Solid Liquid Extraction 80415

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