Fieldwork Report (Done 2007)

FIELDWORK REPORT

AT

PT. TOBA PULP LESTARI, Tbk

Desa Sosorladang Kecamatan Porsea Kabupaten Toba Samosir

North Sumatera

By

Arifista S.W. Harefa (408231012)

Astuti N. Sinambela (408231013)

Edwin H.P. Rumahorbo (408231022)

Sintong P. Sihombing (408231044)

CHEMISTRY DEPARTEMENT

FACULTY OF MATHEMATIC AND NATURAL SCIENCES

STATE UNIVERSITY OF MEDAN

2012

VALIDATION SHEET

FIELDWORK REPORT

AT

PT. TOBA PULP LESTARI, Tbk

Desa Sosorladang Kecamatan Porsea Kabupaten Toba Samosir, North Sumatera

By

Arifista S W Harefa (408231012)

Astuti N Sinambela (408231013)

Edwin H P Rumahorbo (408231022)

Sintong P Sihombing (408231044)

Approved by :

L & D Section Head Fieldwork Consultant, Fieldwork Course Lecturer,

Irwan Kelana Putra Arlodis Nainggolan Dr.Marham Sitorus M.Si

NIK 89-0498 NIP.196301011989031004

Known by :

1st Assistant of Dean Chairman of Chemistry

Drs. P.M.Silitonga, M.Si Dr.Marham Sitorus M.Si

NIP.195909071985031003 NIP.196301011989031004

R e p o r t o f F i e l d w o r k | v

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PREFACE

The goal of this fieldwork report is to know the exact pulping process which is done

on PT. TOBA PULP LESTARI, Tbk. and the chemical analysis on its laboratory. Writers

have spent three weeks to study about the chemical process and analysis. In fact, there are

four section on laboratory. They are Complete Analysis; Chemical Plant Analysis;

Recausticizing Analysis; and Bleaching Analysis. But, writers were given a chance only at

the Bleaching and Recausticizing Analysis by the company.

The material on this report is presented on five chapters. The first chapter describes

about introduction related to the some reasons which are explaining why writers choose PT.

TOBA PULP LESTARI,Tbk for fieldwork course. Chapter 2 explains profile of PT. TOBA

PULP LESTARI, Tbk. The third chapter delas with the pulping process happens on PT.

TOBA PULP LESTARI, Tbk. There reader can find a flowchart that is showing the whole

process too. As writers has told that writers only have a chance on the Bleacing and

Recausticizing section, writers are devoted Chapter 4 to discuss them. Reader can find the

procedure for analysing samples on those section. And the last chapter is conclusion and

sugestion.

Finally, writers hope this report will help any reader to find information about PT.

TOBA PULP LESTARI, Tbk and its pulping procedure.

Writers

Sosorladang, Porsea-Indonesia


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ACKNOWLEDGEMENT

Above all writers thanking to Jesus Christ for His blessing that writers have got

through three weeks fieldwork course on PT. TOBA PULP LESTARI, Tbk. Writers are

feeling so blessed because writers could find such skillful persons on PT. TOBA PULP

LESTARI, Tbk who have helped us for three weeks fieldwork course. Writers would like to

thank to Mr. Gustimar at Uniplaza office who has helped us from the first writers applied our

fieldwork proposal. To whole staff at Learning and Development Center especially Mr. Chris

Fandi Tarigan writers would like to say thank you. Mr. Arlodis Nainggolan as the Lab QA

Section Head. The nice welcome from Mr. Maxwell Simanjuntak, writers would like to thank

for that because you showed us the flowchart of pulping process.

Writers had no personal safety tools at the first time we arrived at complex. So,

writers would like to thank to Mr. Sofyan Siagian because he has lent us those tools. Either

Mr. Marudin Pasaribu or Ms. Ida Farida Ginting, writers are really proud to know you both

because you show us how to work on lab with agile. Writers would like to say a big thank to

Mr. Suhunan Manurung because you have made us knew whole samples on Recausticizing

section clearly. And writers want to insert a thank you for your invitation to your sweet home

so that writers could watch the “Tom and Jerry” there. For Mr. Bantu Nadeak, writers thank

cause you taught us the oxidation-reduction reaction on the determination of Kappa Number.

To Bang Muslim Nababan, writers would like to say thank you because you took us, Edwin

and Sintong, to effluent. Writers would like to thank you to another analyst; Mrs. Ribka

Tarigan; Mr. Sabam Simatupang; Mr. Poltak Sibuea; Mr. Sahat Marpaung; Mr. Jerry; Mr.

Yanhara Sitompul; Mr. Ilham Nasution; Mr. Yudi; Mr. Pendi Manurung; Mrs. Nelvi; Mrs.

Mega Samosir. To employees on R-1 we’d like to say thank you to you; Kak Karmanta; Kak

Bertha Simarmata; and Kak Nova.

Last but not least our beloved sisters Kak Mutiara Simatupang and Mita Gultom at

once became the partner for us. Writers are really blessed to meet you both on lab “Aloooo”.


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INDEX

PREFACE .................................................................................................................................. I

ACKNOWLEDGEMENT ........................................................................................................ II

INDEX ..................................................................................................................................... III

INDEX OF APPENDIX .......................................................................................................... IV

INDEX OF TABLE .................................................................................................................. V

CHAPTER 1 INTRODUCTION ............................................................................................... 1

1.1 Background ..................................................................................................................... 1

1.2 Objectives of Fieldwork Practice Course ....................................................................... 1

1.3 Objectives of The Fieldwork Report............................................................................... 2

1.4 Fieldwork Practice Course Result Significance .............................................................. 2

CHAPTER 2 COMPANY PROFILE ........................................................................................ 3

2.1 History of Company ........................................................................................................ 3

2.2 Profile .............................................................................................................................. 3

2.3 Performance .................................................................................................................... 4

2.4 Management Organisation Structure .............................................................................. 6

a. Fiber Management Organisation Structure .................................................................... 6

b. Mill Management Organisation Structure ...................................................................... 7

CHAPTER 3 PROCESS OVERVIEW ...................................................................................... 8

CHAPTER 4 TIMETABLE AND PROCEDURE .................................................................. 15

4.1 Timetable ...................................................................................................................... 15


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4.2 Procedure ...................................................................................................................... 17

4.2.1 Bleaching Section..................................................................................................................... 17

4.2.1.1 Viscosity Of Pulp.................................................................................................. 21

4.2.1.2 Pulp Brightness ..................................................................................................... 26

4.2.1.3 pH Testing ............................................................................................................ 27

4.2.1.3 Brown Stock Soda Loss ........................................................................................ 27

4.2.2 Recausticizing Section ............................................................................................................ 28

4.2.2.1 Lime Mud Analysis .............................................................................................. 29

4.2.2.2 Reburned Lime Analysis (Available CaO) ........................................................... 32

4.2.2.3 Reburned Lime Analysis (Residual CaCO3) ........................................................ 32

4.2.2.4 Acid Insolubles In White Liquor .......................................................................... 33

4.2.2.5 Reduction Efficiency (Green Liquor & Smelt) .................................................... 34

4.2.2.6 Density of Heavy Black Liquor ............................................................................ 35

4.2.2.7 T.A.A., T.T.A. & Na2CO3 IN WBL, HBL & SOAP SKIMMING ...................... 36

CHAPTER 5 CONCLUSION AND SUGESSTION .............................................................. 40

5.1 Conclusion .................................................................................................................... 40

5.2 Suggestion ..................................................................................................................... 40

REFERENCES ........................................................................................................................ 41


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INDEX OF APPENDIX

APPENDIX (Fibre Line Quality Plan Matrix-Toba Cell Eucalyptus Pulp Process) ............... 42

APPENDIX (Fibre Line Quality Plan Matrix-Toba Cell Eucalyptus Pulp Process) ............... 43

APPENDIX (Recauseting And Lime Kiln Quality Plan Matrix) ............................................ 44

APPENDIX (Bleaching And Recousting Analysis) ................................................................ 46


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INDEX OF TABLE

Table 1. Schedule Of Laboratory Analysis Bleaching Sector ............................................................ 15

Table 2. Schedule Of Laboratory Analysis Recausting Sector .......................................................... 16

Table 3. Scan Viscosity [Ml/G] ....................................................................................................................... 24

Table 4. Viscosity Conversion From 0.5% Ced To 1% Cuprammonium ....................................... 25

Table 5. Spgr Temperature (°C)Correction For Hbl ................................................................................ 36

R e p o r t o f F i e l d w o r k | 1

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CHAPTER 1

INTRODUCTION

1.1 Background

Chemistry is (the part of science which studies) the basic characteristics of substances and

the different ways in which they react or combine with other substances. In university,

students study the theory and practice it through laboratory activities. But even so, students

need a real experience before finishing their learning on university and an asset to compete

with another graduate. As writers are students at State University of Medan, writers have 150

credits to finish until writers will get the Bachelor degree and it includes the Fieldwork

Practice course which has three credits. This course is aiming to give the chance to student in

apllying their knowledge on the real field. Writers have studied chemical on the campus

laboratory for about three years, but writers realized that knowledge from campus was not

enough. Meanwhile, PT. TOBA PULP LESTARI, Tbk is a factory which has chemical

process and reaction on it.

The process and reaction on PT. TOBA PULP LESTARI, Tbk are a common thing on

the chemical field. Beside it, writers have ever learnt about the reaction on some courses at

campus. In addition, State University of Medan has no chemical laboratory instrument as

complete as PT. TOBA PULP LESTARI, Tbk has on its laboratory. Because of these

reasons, writers were atrracted to choose PT. TOBA PULP LESTARI, Tbk as the factory for

Fieldwork Practice course.

By following the Fieldwork Practice on PT. TOBA PULP LESTARI, Tbk writers

hoped that writers would get more knowledge on the real field and build writers’ character

before entering the same field.

1.2 Objectives of Fieldwork Practice Course

Fieldwork Practice is a compulsary course on writers campus. It means that this program

has some objectives that writers must achieve. As a common objective, writers were being

expected to finish the course at PT. TOBA PULP LESTARI, Tbk, while the factory will give

mark to writers after finishing the course related to writers’ attendance; dicipline; skill;

initiation; autonomy; and report. While the particular objective of this course are to increase

writers’ self-confidence; to apply the chemistry which writers’ got from campus; and to wide

writers’ insight related to chemical job field.


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1.3 Objectives of The Fieldwork Report

Writers were required to write a report after fininshing the course at PT. TOBA PULP

LESTARI, Tbk. This rule was made by the State University of Medan for each student who

takes the Fieldwork Practice course. Objectives of this writing are:

1. One of requirements for State University of Medan graduate student before

completing their learning.

2. Being used as an evidence that writers have taken the course at PT. TOBA PULP

LESTARI, Tbk and appraisal after finishing the course.

3. To improve the writers’ abilty in writing scientific report.

1.4 Fieldwork Practice Course Result Significance

The result significance of this course are to train writers’ skill; dicipline; responsibility;

cooperation, and to help writers’ in improving abilty to work profesionally.


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CHAPTER 2

COMPANY PROFILE

2.1 History of Company

PT. TOBA PULP LESTARI, Tbk. produces only pulp sector.The exact date that PT.

TOBA PULP LESTARI, Tbk was esrablished on January 29 20031.

2.2 Profile

Toba Pulp Lestari is a leading manufacturer of high quality paper grade pulp and

dissolving pulp produced from suitanable plantation that have some of the best growth rates

in the world. At their operation located in the pictureque Lake Toba at Porsea, they have

developed environmentally sound management processes to esnsure their long-term

viability.2 Their forestry operations follow operating procedures certified under the ISO

14001 Enviromental Management System that helps ensure their sustainability for the long-

term future.

Vision:

1. Customers choose us for for the value we create for them

2. We attract investor for the value we create

3. Our emplyees are proud to work with us

4. We strive for excellence in the market place in the community

5. We seek to attract and motivate the most competent professionals

6. We create value for our share holders

Mission of PT. TOBA PULP LESTARI, Tbk is to produce high quality pulp from

renewable fibre that is grown is a manner which promore sustainabilty and enviromental care.

While maintaning harmonious relationship with the surrounding communities and

contributing to their overall well-being values. Last, this company values are commitment to

enviromental protection; a sense of social responsibility; and ambition to improve inovate and

the lead.

1 Romeyko, Thomas. ”The Analysis of Training and Development of Employees at PT. TOBA PULP LESTARI, Tbk.”

University of Colombus, Medan (2006) 2 Toba Pulp Lestari. “Company Profile” PT. TOBA PULP LESTARI, Tbk., Porsea


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2.3 Performance

The company performance is starting from nursery and ending with its effluent activity.

The Seedlings are grown in their own nursery from clones they have selected and developed

for best growth rate, natural disease resistance and basic density. Each clone comes from

hand selected mother trees, is propagated and nurtured until it is sound and ready to plant in

the open land. Everyday they produce 20,000 clones at the Porsea nursery. The Forest

Replanting Program follows the harvesting phase. Once cleared weeding takes place and

the seedling are hand planted to produce a new forest in just seven years. The warm and wet

Sumatra climate spurs these seedlings to growth rates of 2cm per day. Harvesting and

Transport are also designed to minimize soil erosion. Labour intensive methods ensure

minimum wastage of wood. Their harvesting and transport techniques follow standard

operating procedures described in their ISO 14001 Enviromental Management System. Over

7000 subcontractors are involved in the feeling, harvesting, transport, and reforestation of

their concession area.

Incoming Wood is supplied in small logs to minimise the size of machinery used and

therefore soil disturbance. The Logs are aged debarked in a rotary debarking drum and then

chipped. The Kraft Pulping Process uses a mixture of caustic soda and sodium sulphate to

produce high quality paper grade pulp and dissolving pulp that are suitable for manufacturing

different types of paper products or rayon fibers respectively. The Kraft process is highly

efficient and uses the least energy of any pulping processes available. Batch Digester change

the chips to a pulp slurry which is washed and then bleached. The Bleaching sequence is

elemental chlorine-free and results in high quality bright white pulp. The pulp is produced in

sheets,cut and baled, then wrapped before dispatch via road to the sea port of Belawan just

outside Medan. A Chemical Recovery furnace burns the wood resins and spent chemicals,

returning the chemicals for rhe reprocessing while at the same time producing steam and

pressure for the plant’s internal energy requirements. Supplementary Energy is provided

from a Multifuel fluidized bed boiler which utilizes the bark and wood waste plus other

biofuels such as palm shell husks, peat or coal. Solid waste collected in the effluent treatment

system is also combusted in this unit. The high pressure steam is reduced through two turbine

generators making the mill totally self-suficient in steam and electricity. The Entire Process

is Quality-Controlled and Verified by a well-equipped laboratory and testing facility on

site. All operating parameters are checked and verified by random sampling techniques and

laboratory tests during every operating shift. The Mill is located on the Asahan river which


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flows out of Lake Toba. This river provides a significant supply of high quality water. Less

than 1% of the river’s normal flow is required to support the mill and, after appropriate

treatment, the water is returned to the Asahan downstream of the lake. Their Effluent is

treated and controlled to very strict parameters. While the downstream location of their mill

means it is impossible to have any effect on Lake Toba, they are also very careful that their

operations are not detrimental to the Asahan River which drains the lake. Primary

clarification followed by aeration and secondary clarification brings waste products within

the required specifications for return to the river system. Pilot Demonstration Farms show

we can grow fish, rice, and other crops in the treated effluent.


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2.4 Management Organisation Structure

a. Fiber Management Organisation Structure


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b. Mill Management Organisation Structure


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CHAPTER 3

PROCESS OVERVIEW

The basic raw material for pulp and paper and rayon fibre making is cellulose in

fibrous form.3 It is available in plant material such as wood, bamboo, straw, etc. Plant mateial

can be converted into pulp either by chemical process, mechanical process or by the

combination of these two processes, depending upon the end product desired. PT. Toba Polp

Lestari is Kraft Pulp Mill located near Porsea which is approximately 220 km from Medan

on the island of Sumatera, Indonesia. This company uses the Kraft Process to produce the

pulp. Kraft is the germanic/swedish word for strong. Kraft process is also known as sulphate

process. Kraft process is the modification of soda process (soda process utilizes sodium

hydroxide). In the Kraft process, a mixture of sodium sulphide and sodium hydroxide is used

to pulp the wood. Sodium sulphate itself is incapable of pulping wood, yet the method came

to be called the sulphate process because this salt has generally been used as a make-up to

replace any chamical losses.4 The sodium sulphate is reduced to sodium sulpide in the

recovery furnace. Advantages of kraft process are:

1. Produces highest strength pulp

2. Pulping chemical can be effectively recovered

3. Handles a wide variety of species

In the Kraft process a mixture of sodium sulphide and sodium hydroxide is used to the

pulp wood. The liquor containing the active cooking chemical is termed as white liquor. The

satandard Kraft pulping terms are described below:

1. Total Alkali

Total of all “viable” sodium alkali compounds, i.e. NaOH + Na2S + Na2SO4 +

Na2S2O3 + Na2SO3 (does not include NaCl).

Expressed in g/l as Na2O.

2. Total Titrable Alkali (TTA)

Total of NaOH + Na2S + Na2CO3, expressed in g/l as Na2O.

3. Active Alkali (AA)

Total of NaOH + Na2S, expressed in g/l as Na2O.

3 Toba Pulp Lestari, “Digester Training Manual” PT. TOBA PULP LESTARI, Tbk., Porsea 4 Rydholm, Sven A., “Pulping Processes” John Wiley & Sons, Ltd, Great Britain (1965)


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4. Effective Alkali (EA)

Total of NaOH + ½ Na2S, expressed in g/l as Na2O.

5. Activity

The percentage ratio of active alkali to total alkali expressed as %.

6. Causticity

The percentage ratio of NaOH, expressed as Na2O to active alkali , expressed as %.

7. Sulphidity

The percentage ratio of Na2S, expressed as Na2O to active alkali , expressed as %.

8. Causticizing Efficiency

In white liquor, the percentage ratio of NaOH to NaOH + Na2CO3, Both items being

expressed as Na2O and being corrected for NaOH content of the original green liquor

in order to represent only the NaOH produced in the actual causticizing reaction.

Expressed as %.

9. Residual Alkali (Black Liqour)

Alakali concentration determined by acid titration.

Expressed in g/l Na2O.

10. Reduction Efficiency (Green Liqour)

The percentage ratio of Na2S to Na2SO4 +Na2S + any other soda sulphur compounds,

all expressed as Na2O.

Expressed as %.

11. Make up chemical consumption

The amount of Na2SO4 or other sodium compounds expressed as Na2SO4, added as

new chemical per ton of air dry pulp produced.

12. Chemical Recovery

The percentage ratio of total chemical to the digesters, less the total chemical in new

chemical, to the total chemical to the digesters.

13. Chemical Logs

a. Total : The percentage ratio of total chemical in new chemical to total

chemical to the digesters.

b. Loss in cooking and pulp washing : The percentage ratio of total chemical

to the digesters, less the total chemical to the evaporators, to the total chemical

to the digesters.


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c. Loss in evaporators and furnaces : The percentage ratio of total chemical

to the evaporators plus total chemical in new chemical and minus total

chemical in the green liquor, to the total chemical to the digesters.

d. Loss in recausticizing and mud washing : The percentage ratio of total

chemical in the green liquor, minus the total chemical in the white liquor, to

the total chemical to the digesters.

14. White Liqour

The name applied to the cooking liquor used in the digesters. It is made by

causticizing green liquor.

15. Black Liqour

The name applied to liquor recovered from the digesters, up to the point of their

incineration in the recovery plant.

16. Green Liqour

The name applied to liquor made by dissolving the recovered chemicals in water and

weak liquor, preparatory to causticizing.


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Figure 1. Pulping Process


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Initially the main fiber source for the mill will be Pinus Merkusi and mixed tropical

hardwoods, and it is envisanged to use Eucalyptus at a later stage. The company’s forestly

department is planning of man made plantations of eucalyptus tress over lage acreages which

will mature in about seven to eight years.

Basically two grades of pulp, using an Alkaline Sulphate process, are to be produced:

a. Pre-Hydrolized Kraft Pulp (NDKP and LDKP) at 330 T/D

b. Fully-Bleached Kraft paper pulp (NBKP and LBKP) at 515 T/D

LDKP : Prehydrolised kraft pulp from short fiber sources (hardwoods and

eucalyptus)

NDKP : Prehydrolosed kraft pulp from long fiber sources (Pinus-Merkusii)

LBKP : Fully bleached kraft paper pulp from short fiber sources (tropical

hardwoods and eucalyptus)

NBKP : Fully bleached kraft paper pulp from long fiber sources (Pinus Merkusii)

The components that are present generally in woods can be classified chemically in

the following way; carbohydrates; phenolic substance; terpenes; aliphatic acids; alcohols;

inorganic constituents; and may other organic substance.5 Wood is delivered to the mill site

by logging trucks from the company forest concession and are unloaded by a large Goliath

crane in the wood yard which also feeds the logs to the wood room on a “first in-first used”

basis. The logs are debarked, chipped into chips, screened and stored in chip piles-separate

for hardwoods and softwoods. The wood chips are fed to the batch digesters by a belt

conveyor system. The design is for 6 batch digesters to be used on B.K.P and 8 digesters on

D.K.P. After the cooking cycle is over, the pulp is blown to the blow tank.

The stock from the blow tank is pumped through the pressure knotters to a three stage

washing system, then on to a screening system and thereafter to the 4th

brown stock washer.

The unbleached pulp after the 4th

washer is stored in a high density unbleached storage tower

at 12% consistency.

5 Browning, Bertie Lee, “The Chemistry Of Wood” Krieger Drive, Florida (1963)


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The bleach plan operation consists of four stages. The first two stages for both BKP

and DKP are the same. The first stages is the treatment of pulp with chlorine / chlorine

dioxide followed by caustic extraction/ oxygen in the second stage. The third bleaching stage

for BKP is sodium hypochloride (hypo) treatment followed by chlorine dioxide in the fourth

stage. Where as for DKP, the third stage is the chlorine dioxide chlorine treatment followed

by hypo in the last stage.

The pulp from the bleaching section is stored in the bleach high density storage tower

at 12% consistency. The pulp is then subjected to screening and centriccleaning operation

before being made into a sheet form in the sheeting machine and dried in an airbone Flakt

drier. There after, the sheet is cut, weighed, pressed, baled, wrapped, wired and labeled and

stored in a ware house.

The Chemicals plant manufactures are the bleaching chemicals that are required. This

plant is partially an integrated one. From the starting raw material, raw salt (sodium chloride)

the following chemicals are produced caustic, chlorine, hydrochloric acid, and sodium

hypochlorite by the membrane electrocity cells. The chlorine dioxide plan is an the integrated

one using the HCl ( modified Munich process) for producing chlorine dioxide from salt via

sodium chlorate electrolytic cells. Sulphur dioxide is produced from raw sulphur. Oxygen(

liquid) and Nitrogen (liquid) are generated in the chemical plant by the PSA system. Chilled

water production also forms a part of this section.

The weak black liquor from the brown stock washers is concentrated by a set of

falling film plate type evaporators and concentrators. This concentrated liquor (65%) is fired

in a recovery boiler. The high pressure steam produced by burning the organic present in the

liquor, is used the generating electricity in a turbo generator and the extracted steam utilized

for heating purposes in the process. The inorganic recovered chemicals, in the form of the

fused mass known as “smelt”, is then dissolved in the dissolver ( Green Liquor) and pumped

to the recausticizing section.

The green liquor is then clarified and slake with burnt lime to produced white liquor.

The white liquor thus produced is used as a cooking chemicals in the digesters. The lime

sludge from the clarifier is thickened and calcined along with make up lime stone in a rotary

lime kiln to produce burnt lime which is used for caustisicizing the green liquor.


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A power boiler that operates on wood bark and oil generates the extra steam required

to run the mill. Power for the mill is supplied by a double extraction condensing turbine with

a designed rated capacity of 33 megawatts.

The water for the mill is pumped from the Asahan river to a water treatment plant

where in the suspended impurities are settled and then filtered through Gravity Filters prior

to being used in the mill, as clarified or filtered water as needed.

The water that in to be used in the boilers is treated separately in order to remove all

the minerals constituents present in them by passing it through ion exchange resins. The

resultant water known as demineralized water is then used in the boiler to produce high

pressure steam.

The effluent from the mill is treated to remove all the harmfull impurities before it is

discharged back into the Asahan river, downstream of the mill water intake, by passing

through settling ponds and then to an aeration lagoon, to the established parameters of the

government of Indonesia in terms of BOD and suspended matters.


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CHAPTER 4

TIMETABLE AND PROCEDURE

4.1 Timetable

The fieldwork course was held on PT. TOBA PULP LESTARI, Tbk, started from

February 3, 2012 and ended on February 18, 2012. Below, the timetable and activities are

shown.

Table 1. Schedule of Laboratory Analysis Bleaching Sector

No. Date of Activity Time of Pulp

Analyzing

Laboratory Analyzing

Bleaching Dissolving

Pulp Quality Analysis

Digester and

Washing

Dissolving Pulp

Quality Analysis

1 February 7, 2012 09.00 am

11.00 am

1.00 pm

3.00 pm

- Viscosity Pulp

- Brightness Pulp

- Residual of Peroxide

- PH Pulp

- Viscosity Pulp

- Brightness Pulp

- PH Pulp

- Viscosity Pulp

- Brightness Pulp

- PH Pulp

- Viscosity Pulp

- Brightness Pulp

- PH Pulp

- Kappa Number

- Soda Loss

- Kappa Number

- Kappa Number

- Kappa Number

The schedule of laboratory analyzing was held from Monday – Saturday ( at Saturday until

12.00 am) start from February 3 –March 3, 2012. And the activity were regularly same daily.


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Table 2. Schedule of Laboratory Analysis Recausting Sector

No. Date of

Activity

Time of Pulp

Analyzing

Laboratory Analyzing

Evaporator

and Recovery

Quality

Analysis

Digester and

Washing

Tobacell

Eucalyptus

Pulp Quality

Analysis

Recausticizing

and Lime Kiln

Quality Analysis

1 February 7,

2012

08.00 am

09.00 am

12.00 am

-

- WBL

- IBL

- HBL-1

- HBL-2

- HBL-P

- Ash Boiler

- Green

Liquor

- White

Liquor

- Lime Mud

- WWL

- GL ( GL

Clarifier/GLC,

Slaker ,

Causticizer)

- WL Storage

- Clarifier

- Eco Filter

- RB (TTA)

- SC

The schedule of laboratory analyzing was held from Monday – Saturday ( at Saturday until

12.00 am) start from February 3 – March 3, 2012. And the activity were regularly same daily.


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4.2 Procedure

4.2.1 Bleaching Section

Pulp fibers, as they are obtained from chemical digestion as well as mechanical

pulping, are distinctly colored. Depending on the type of wood from which they originate and

the defibering process applied this color maybe anywhere from a dark brown to creamiest

white.

Cellulose and hemi cellulose are inherently white and do not contribute to color. It is

generally agreed that “Chromoporic groups” on the lignin are principally responsible for

color. Oxidizing chemicals may either destroy these groups or degrade lignin so as to

brighten the pulp.6

Heavy metal ions like iron and copper as well as extractive also contribute to the

color. Bleaching of chemical pulp is, in a sense, the continuation of digestion. The bleaching

process must be carried out in such a way that strength characteristic and other paper making

properties are preserved.

Common Bleaching Sequence

Modern bleaching is usually carried out in a step wise sequence utilizing different

chemicals and condition in each stage. The commonly used chemical treatments and the

“Short Hand” designations are listed as follows:

Chlorination (C) : Reaction with elemental chlorine in an acidic medium.

Alkaline extraction (E) : Dissolution of reaction products with NaOH.

Hypochlorite (H) : Reaction with ClO2 in acidic medium.

Peroxide (P) : Reaction with peroxide in alkaline medium.

Oxygen (O) : Reaction with elemental oxygen at high pressure in alkaline

medium.

C/D : admixture of chlorine and chlorine dioxide.

6 PT. Toba Pulp Lestary, Tbk., “Introduction to Pulping Technology Training Manual “ Porsea (1991)


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In the chlorination stage, lignin is chlorinated to chloro lignin which gets solubilised

in the extraction stage. Thus delignification takes place. Brightness development through the

CE sequence is very little. Oxygen is also been used in the extraction stage (Eo) and is used

primarily for delignification.

To achieve a “full bleach” brightness level of 89 to 90, bleaching is usually carried

out in five stage, employing C E H E D or C E D E D.

In the hypochlorite bleaching, the chromophoric groups of lignin are destroyed. Brightness

development is very high in this stage. Calcium or sodium hypochlorite may be used. One

disadvantage of this treatment is that the cellulose is also attacked by hypochlorite and hence

the conditions during the treatment are to be strictly monitored to avoid cellulose degradation.

Peroxide are used in the bleaching of chemical pulps. When used under relatively

mild conditions (35 to 55oC), peroxide is an effective lignin preserving bleaching agent,

improving the brightness without significant yield loss.

First Stage – Chlorination

Unbleach pulp in the HD tower is diluted to 3.5% consistency with chlorination stage

filtrate and fresh water and brought to the up-flow chlorination tower. Cl2 and ClO2 are mixed

into the stock by a RCM mixer. The dosage of Cl2 chemicals is controlled by a polarax meter

which is a linear measurement of ORP, based on residual chlorine concentration. The

temperature of the chlorination stage, 45-50oC is regulated by means of the mutual relation of

the dilution waters used on the HD – tower bottom. After the reaction, the Cl2 tower over

flow is deluted to 1.2% and wash on vacuum washer (Diameter 4000 x 6500 mm face

length). The mat consistency is 12%. The reaction pH of the chlorination stage should be to

2.2 – 2.5 range.

Chlorine charge depends upon the Permanganate or Kappa number of pulp. It is usually in the

range of 6-8% on pulp for softwood kraft, and 3-4% for hardwood kraft pulp. Maintaining a

small chlorine residual at the end of the chlorination is utilized as the basis of feedback

control.


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For effective chlorination, pH plays an important role. In Cl2 – H2O system, chlorine

exists in different forms depending upon the pH. In acid medium, the following equilibrium

exists.

1. Cl2 + H2O → HOCl + H+ Cl

-

when a base is present, a different aquilibriumexist:

2. HOCl + OH- → OCl

- + H2O

The proportion of Cl2, HOCl and HClO ions solution depends on pH. Each forms of

chlorine has different properties and attacks lignin and cellulose in a different manner.

Hyprochlorite acid is generally regarded as destructive to cellulose and therefore bleaching

within the pH range of 2 to 9 is usually avoided. At pH below 2, chlorine exists in molecular

chlorine form.

Of late, it has also became a practice to use a small portion of ClO2 in the chlorination

stage. The advantages are:

Minimize cellulose degradation

Better brightness stability

Higher final brightness

Reduced effluent color

The reaction tower used for chlorination is usually an up flow pump through tower. After

the extraction is over, the pulp is then washed in the washer in order to remove the residual

chemicals and also to thicken the pulp to be carried to the next stage.

Extraction (Second Stage)

The alkali stage control takes place with pH-measuring. On the discharge side of the

chlorination washer, the alkali amount set by the pH-valve is sprayed into the stock. The O2

dosage takes place with regard to the stock amount. To accelerate reaction, LP-steam is

brought into the MC pump pumping tank to raise the temperature to 70oC. from the preceding

washer, the stock is pumped by MC pump to the bottom of the bottom of the extraction

tower. O2 is brought to the ROM mixer after the MC pump. Alkali extraction stage pH should


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be 9.8-10.2. The dilution of in feed stock takes place in the tower launder. On the washer

(Dia.4000 x 6500 mm face length), for first wash showers, hot water is used and for the

others, Dioxide/hypo filtrate. The alkali washer filtrate is used for washer pre-dilution, tower

dilution, as spray for the Cl2 washer and for the wire washing.

Hypochlorite / Chlorine Dioxide (Third Stage)

NDKP Chlorine Dioxide

The dioxide stage control is based on the kappa number of stock after the alkali stage

and on the residual content in the D-tower top part as well as on the target brightness. The

dioxide solution is heated with alkali stage filtrate to about 35-40oC before it is fed to the MC

pump. The heating takes place in the lamella type heat exchanger.

The end pH has to be within the right range (4.0-5.5) in which case the dioxide

influence is the most effective. Alkali needed for pH control is added to the discharge side of

the alkali washer. The temperature of this stage is on the same level as the alkali stage 1.e

70oC. If heating is needed, steam is used at the MC pump, pumping tank. The tower is

furnished with an upflow pre-reaction tube and the tower is a down flow tower.

NBKP Sodium Hypochlorite Stage

Hypochlorite for BPK is dosed according to kappa number after the alkali extraction

stage. At the discharge end of alkali filter, the temperature is maintained at 40oC. The pH of

the stock should be 9-9.5. Washing is performed using fresh water, hot water (depending on

the temperature of the last stage) and filtrate from the last stage. Washer filtrates are led to the

chlorination filtrate tank for neutralization.

Hypochlorite / Dioxide (Fourth Stage)

Sodium hypochlorite is used for DKP pulp bleaching and chlorine dioxide for BKP

pulp. The tower is furnished with an up flow preretention tube and the tower itself is a down

flow tower. Otherwise, the retention time for DKP hypo would be too long and the pulp

would become degraded, stock is pumped to the bottom of the upflow tube.

On the washer (Dia. 4000 x 6500 mm face length), white water from the pulp

machine is used for BKP and demineralization water is used for DKP. SO2 is used as anti


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chlor and dosed to the stock based on residual chlorine. Stock is pumped by MC pump to the

bleached HD tower.

The filtrate from this stage is used for the dilutions, wire washing and third stage wash

waters. The excess amount is fed to the either the alkali filtrate tank (NDKP) or third tank

(NBKP).

NDKP Hypochlorite Stage

This is the stage where the viscosity of the pulp is controlled. The incoming stock

from the third stage should have the maximum brightness possible as that the hypo dosage

will be minimum.

The hypo dosage takes place on the basic viscosity of dioxide treated pulp. If

considerable disturbance occur in the viscosity of the stock coloring to the bleach plant, there

is a provision to add hypochlorite to the second stage (along with alkali). The solution feed

will then take place at the chlorination stage filter. The tower temperature is kept at about

40oC. The temperature can be changed, if chemicals residue occur, alternatively, the dosage

can be decreased.

NBKP Dioxide Stage

In this stage maximum brightness development takes place without effecting the

viscosity, pH is set by the alkali to be added at the preceding washer discharge side. The Cl2O

coming from the dioxide heat exchanger is fed to the MC pump, which takes care of mixing

and heating at the same time.

Water Gas Treatment

The exhaust gases from toers, washer, filtrate tanks and MC pumps are scrubbed with

alkali filtrate and SO2 water. The purified gases are discharged in to the sewer.

4.2.1.1 Viscosity Of Pulp

1.0. Purpose

This method describes the procedur of determining the viscosity of 0.5% cellulose

solutions, using 0.5M Cuperiethylenediamine (CED) as a solvent and a “Cannon-

Fenske” capillary viscometer, then converting viscosity following the conversion

table #2 attached to this procedure.


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2.0. Apparatus

1. Constant temperature bath maintained at 25.00 C ± 0.1

0 C.

2. Viscometer “Cannon-Fenske” capillary tipe, size chosen according to expected

viscosity range in compliance with the following characteristics.

Size Number Viscosity Range, mPaS (Cp)

50 0.8 – 3.2

100 3.0 – 11.0

150 7.0 – 27.0

200 19.0 – 76.0

300 48.0 – 90.0

3.0 Sampling

1. Tear 5-7 gram of pulp sheet sample or approximately 25-35 grams pf pulp slurry

from the washer vat. (make consistency 0.5%).

2. All pulp sample disintegrate in disintegrator using 500 rotation per minute (rpm).

3. Take 100 ml for making a sheet.

4. Make hand sheets utilizing a Buchner funnel with the filter paper after cut as per

Buchner funnel diameter.

5. Dry by an re lamp.

4.0 Procedure

1. Determine the moisture content of the prepared sample sheet by oven drying

half of the sheet.

2. Weigh a pulp sample equivalent to 0.1250 grams of moisture free pulp.

3. Put the sample in a dissolving flask and utilizing a burette/pipette add 12.5

mili litres of the distilled water and several pieces of copper wire, shake gently

for approximately 30 sec.

4. Add exactly 12.50 mL of the CED solution.

5. Continue shaking for another 15 minutes.

6. Fill the viscometer by immersing its smaller-diameter leg into the solution and

drawing the liquid into the instrument by appliying suction to the other end.

7. Draw the liquid level to the second etch mark then wipe and return the

viscometer to its vertical position.


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8. Place the viscometer in a constant temperature bath of 25.00

C ± 0.10 C and

leave for at least (5) five minutes to allow the viscometer temperature to

stabilize.

9. Draw the solution up into the measuring leg of the viscometer with a suction

bulb.

10. Determine the efflux time by the drawing the liquid to the upper mark and

measuring the time required for the meniscus to pass between the two marks.

11. Repeat the measurement of the efflux time and results should be within ± 0.2

seconds.

12. Measure the efflux time for the upper line to lower line.

V = CTD

V = Viscosity of the CED at 25.00 C [Cp]

C = Viscometer Constant

T = Efflux Time [s]

D = Density of pulp solution [= 1.052]

Example:

Sample C T D V= CTD

W4 0.09559 98.34 1.052 9.88

D0 0.0925 81.72 1.052 7.95

E0 0.1022 67.59 1.052 7.26

D1 0.1022 64.91 1.052 6.97

13. Reporting:

Viscosity of dissolving Pulp reported in SCAN Unit from CED Viscosity by

Calibration Curve/Conversion Table enclosed. Report in units of mg/l.


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Table 3.SCAN VISCOSITY [mL/g]

0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9

5 346 351 355 360 364 369 374 378 383 387

6 392 397 401 406 410 415 420 424 429 433

7 438 443 447 452 456 461 466 470 475 479

8 484 489 493 498 502 507 512 516 521 525

9 530 534 539 544 548 553 557 562 567 571

10 576 580 585 590 594 599 603 608 613 617

11 622 626 631 636 640 645 649 654 659 663

12 668 672 677 682 686 691 695 700 705 709

13 714 718 723 727 732 737 741 746 750 755

14 760 764 769 773 778 783 787 792 796 801

15 806 810 815 819 824 829 833 838 842 847

16 852 856 861 865 870 875 879 884 888 893

17 898 902 907 911 916 920 925 930 934 939

18 943 948 953 957 962 966 971 976 980 985

19 989 994 999 1003 1008 1012 1017 1022 1026 1031

Viscosity = 0.5% CED [Cp]


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Table 4. Viscosity conversion from 0.5% CED to 1% CUPRAMMONIUM

0.5 % CED T-206 om 82

1% CuAm T-206 m 44

0.5 % CED T-206 om 82

1% CuAm T-206 m 44

0.5 % CED T-206 om 82

1% CuAm T-206 m 44

0.5 % CED T-206 om 82

1% CuAm T-206 m 44

0.5 % CED T-206 om 82

1% CuAm T-206 m 44

4.0 6.6 8.3 16.4 12.6 28.5 16.9 41.5 21.2 55.4

4.1 6.7 8.4 16.7 12.7 28.8 17.0 41.8 21.3 55.7

4.2 6.8 8.5 17.0 12.8 29.1 17.1 42.2 21.4 56.0

4.3 7.0 8.6 17.2 12.9 29.4 17.2 42.5 21.5 56.4

4.4 7.3 8.7 17.5 13.0 29.7 17.3 42.8 21.6 56.8

4.5 7.5 8.8 17.8 13.1 30.0 17.4 43.1 21.7 57.2

4.6 7.7 8.9 18.0 13.2 30.3 17.5 43.4 21.8 57.5

4.7 7.8 9.0 18.3 13.3 30.6 17.6 43.7 21.9 57.8

4.8 8.0 9.1 18.6 13.4 30.9 17.7 44.0 22.0 58.2

4.9 8.2 9.2 18.9 13.5 31.2 17.8 44.3 22.1 58.5

5.0 8.4 9.3 19.2 13.6 31.5 17.9 44.6 22.2 58.8

5.1 8.6 9.4 19.5 13.7 31.8 18.0 45.0 22.3 59.1

5.2 8.8 9.5 19.8 13.8 32.1 18.1 45.4 22.4 59.5

5.3 9.1 9.6 20.1 13.9 32.4 18.2 45.7 22.5 59.8

5.4 9.3 9.7 20.4 14.0 32.7 18.3 46.0 22.6 60.1

5.5 9.5 9.8 20.7 14.1 33.0 18.4 46.4 22.7 60.5

5.6 9.7 9.9 21.0 14.2 33.2 18.5 46.7 22.8 60.9

5.7 10.0 10.0 21.3 14.3 33.5 18.6 47.0 22.9 61.2

5.8 10.2 10.1 21.6 14.4 33.8 18.7 47.4 23.0 61.5

5.9 10.4 10.2 21.9 14.5 34.1 18.8 47.7 23.1 61.9

6.0 10.6 10.3 22.2 14.6 34.1 18.9 48.0 23.2 62.2

6.1 10.8 10.4 22.5 14.7 34.7 19.0 48.4 23.3 62.5

6.2 11.0 10.5 22.8 14.8 35.0 19.1 48.7 23.4 62.9

6.3 11.3 10.6 23.1 14.9 35.3 19.2 49.0 23.5 63.2

6.4 11.5 10.7 23.4 15.0 35.6 19.3 49.3 23.6 63.5

6.5 11.7 10.8 23.6 15.1 35.9 19.4 49.6 23.7 63.9

6.6 12.0 10.9 23.8 15.2 36.2 19.5 50.0 23.8 64.3

6.7 12.2 11.0 24.0 15.3 36.5 19.6 50.3 23.9 64.6

6.8 12.5 11.1 24.2 15.4 36.8 19.7 50.6 24.0 65.0

6.9 12.7 11.2 24.5 15.5 37.1 19.8 50.9 24.1 65.3

7.0 13.0 11.3 24.8 15.6 37.4 19.9 51.2 24.2 65.6

7.1 13.2 11.4 25.0 15.7 37.7 20.0 51.5 24.3 66.0

7.2 13.5 11.5 25.3 15.8 38.0 20.1 51.8 24.4 66.4

7.3 13.7 11.6 25.6 15.9 38.3 20.2 52.1 24.5 66.7

7.4 14.0 11.7 25.9 16.0 38.6 20.3 52.4 24.6 67.1

7.5 14.2 11.8 26.2 16.1 38.9 20.4 52.7 24.7 67.4

7.6 14.5 11.9 26.5 16.2 39.2 20.5 53.1 24.8 67.7

7.7 14.7 12.0 26.8 16.3 39.5 20.6 53.4 24.9 68.0

7.8 15.0 12.1 27.1 16.4 39.9 20.7 53.7 25.0 68.3

7.9 15.3 12.2 27.4 16.5 40.2 20.8 54.0 25.1 68.6

8.0 15.5 12.3 27.6 16.6 40.5 20.9 54.4 25.2 86.9

8.1 15.8 12.4 28.0 16.7 40.8 21.0 54.7 25.3 87.2

8.2 16.1 12.5 28.2 16.8 41.1 21.1 55.0 25.4 87.5


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4.2.1.2 Pulp Brightness

1.0 Sampling

a. Pulp Sheet

a. Cut the pulp sheet of about 20 x 20 cm size.

b. Clean the test specimen of cut fibres.

b. Pulp Slurry

Take approximately 300 – 1000 mL pulp slurry into a plastic container.

2.0 Procedure

a. Pulp Sheet

a.1 First Alternative

a. Put the specimen on the sample port of brightness tester.

b. Release the flash button twice and note the reading.

c. Repeat releasing the flash button twice for times at different points

on the test specimen.

d. Record each reading and take the average value.

a.2 Second Alternative

a. Put the test specimen on the sample port of brightness tester.

b. Click “Measure” and instrument will be worked.

c. Record each reading and take the average value.

b. Pulp Slurry

1. Pour the collected sample on shieves screen.

2. Rinse with demineralized water until free of residual chemical.

3. Take approximately 20 grams of the wet pulp and put into plastic beaker 300

mL.

4. Put into the beaker demineralized water to dilute the wet pulp.

5. Stir by hand separate fibres.

6. Put a filter paper on Buchner Funnel and pour the slurry into it.

7. Put another filter paper on the top and apply vacuum to suck the water.

8. Press the pulp sample to equally dewater and then cut the vacuum.

9. Take the fibre mat and dry it by means of iron.

10. Put into oven at 1050C ± 3

0 C for approximately 10 minutes.


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11. Measure the brightness by following the procedure in 1a-1d above, then record

the result.

4.2.1.3 pH Testing

1.0 Sampling

a. Pulp sheet

Tear approximately 10 grams of pulp sheet by hand into small pieces.

b. Pulp Slurry

Take about 500 mL of pulp slurry sample.

2.0 Procedure

a. Pulp Sheet

1. Perform pH meter standardization following the steps in the attachment.

2. Put the sample into disintegrator and add one (1) litre of demineralized water.

3. Desintegrate for approximately one (1) minute.

4. Dip the electrode into the pulp slurry and read the pH value.

b. Pulp Slurry

1. Perform pH meter standardization following the note below.

2. Dip the electrode and read the pH value.

4.2.1.3 Brown Stock Soda Loss

1.0 Purpose

Brown stock soda loss is defoned as the amount of Kraft Liquor carried over with

the pulp after the washing stage and is expressed as Kilograms of Sodim Sulphate

[Na2SO4] per ton of pulp.

2.0 Sampling

1. Obtain pulp sample from (3) three different points across the washer drum

face.

2. Mix the (3) three samples together to obtain a composite sample.

3.0 Procedure

1. Place 500 mL of 600 C distilled water into a 1000 mL beaker.


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2. Adjust the distilled water pH with the addition of 0.1 N Hydrochloric Acid

[HCL] to obtain a pH of 4.3.

3. Add 1-2 grams of oven dry pulp sample to the beaker of warm distilled water

and agitate with magnetic stirrer.

4. Titrate with 0.1 N Hydrochloric Acid [HCL] until the pH of the sample

solution resches pH 4.3, record the volume [mL] 0.1 N Hydrochloric Acid

[HCL] consumed.

5. Filter out the fibre and dry until moisture free.

6. Weigh the dry pulp.

4.0 Calculation

A = Volume [mL] of 0.1 N Hydrochloric Acid [HCL] used.

N = Normality of 0.1 N Hydrochloric Acid used.

W = Weigh (in grams) of the moisture free pulp sample.

Soda Loss [Kg/Tonne of Pulp] = 𝐀×𝐍×𝟕𝟏

𝐖

Example:

A = 7.6 mL

N = 0.1

W = 1.9060 gram

Soda Loss [Kg/Tonne of Pulp] = 1.5 𝑥 0.1 𝑥 71

1.9060

= 5.6

4.2.2 Recausticizing Section

The recausticizing process produces cookng liquor for the digester from recycled

inorganic chemicals generated in the recovery boiler and lime kiln. The process involves one

very simple chemicals reaction followed by process steps utilizing various types of liquid

solid separation equipments.

Cooking liquor (white liquor) for the kraft process is produced from smelt generated in

the recovery boiler. Quick lime is slaked in the smelt solution (green liquor) producing white

liquor and calcium carbonate (lime mud). The calcium carbonate is calcined in the lime kiln

to produce quick lime. The lime mud is washed to reduced it’s chemicals contents before it is


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fed into the lime kiln and the wash liquor (weak wash) generated in recycled to dissolve the

smelt to produce green liquor.

Green liquor + Lime = Lime mud + White liquor

Na2CO3 + H2O + CaO = CaCO3 + 2NaOH

Sodium + Water + Calcium = Calcium + Sodium Carbonate Oxide Carbonate

Hydroxide.

The green liquor obtained by dissolving the smelt in weak white liquor normally

contains in soluble impurities known as dregs. Dregs are remove in the green liquor clarifier

(Diameters 17 m I.D x 10.8 m height ; single compartment unit type). The dregs which settle

to the bottom the clarifier are removed from the clarifier and are washed and filtered (

precoat-rotary type filter with 1.83 m diameters x 1.83 m length). The clean liquor from the

dreg washer is weak liquor and it is used to dilute the lime mud a head of lime washer. The

dregs from the dregs filter are transported to a dregs trailer. These dregs are dumped in a

“garbage area”.

The clarified green liquor is pumped to the slaker (size 3. 65 m diameters x 2.845 m

height), where it is reacted with lime. Lime is fed by a table feeder ( rotary disc type) from

the lime storage bin. In the slaker, the burnt lime slakes when it comes contact with the green

liquor and initial causticizing reaction takes place. The chemicals reaction is as follows :

Na2CO3 + Ca (OH)2 CaCO3 + 2 NaOH

Lime mud is then pumped to a vacuum filter (type : precoat rotary drum with diameters

3048 mm x 4880 mm width ) for final washing.

4.2.2.1 Lime Mud Analysis

Note: Lime Mud is defined as the lime residu [CaCO3] left after the slaking of Quick

lime.

1.0 Sampling

a. A composite grab is taken from across the width of the Mud Filter doctor blade.

b. Place the composite mud sample in a sealed container to prevent moisture loss.

c. Cool the Lime Mud sample before analyzing.

d. The sample can be obtained from the Lime Mud Washes, Filter, Storage and ECO

Filter.


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2.0 Procedure

2.1 Lime Mud Consistency

a. Stir the sample homogeniusly

b. Accurately weigh 50 grams to the nearest 0.1 gram of lime mud into a previously tared

evaporating disk, record the total weight, to the nearest 0.1 gram, as (A).

c. Place evaporating disk with sample under infra red lamp until nearly dry.

d. Place evaporating disk with sample into an oven at 1050 C ± 3

0 C until completely dry.

e. Cool in a desiccator and weigh to the nearest 0.01 gram, record result as (B).

2.2 Calculation

A = weight of wet sample [grams]

B = weight of oven dry sample less weight of evaporating

[grams]

Consistency (Cy) [%] = (𝐁)

𝐀 𝐱 𝟏𝟎𝟎%

Example:

Sample A B (Cy) [%] = (𝐁)

𝐀 𝐱 𝟏𝟎𝟎%

C 20.0693 11.1054 55.3

W 18.6511 8.3604 44.8

St 16.3044 7.5777 46.5

F1 12.4110 8.4997 68.5

F2 12.5733 8.5328 67.9

3.0 Soda Content In Lime Mud ( Lime Mud Washer, Storage and ECO Filter)

a. Obtain a Lime Mud sample and shake well.

b. Weigh 2-3 grams, to the nearest 0.01 gram, and place in an Erlenmeyer flask.

c. Add ± 100 mL of hot water to the flask, shake well, and let stand for (5) five minutes.

d. Filter sample utilizing a Buchner Funnel and vacuum pump, rinse with approximately

50mL of hot water until clean.


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e. Add few drops of Methyl Orange indicator and titrate with 0.5N Hydrochloric acid

[HCl] to a reddish end point, record as (A) the volume of 0.5N Hydrochloric acid

consumed.

3.1 Calculation

A = volume of 0.5N HCl consumed [mL]

W = weight of sample [grams]

Cy = Consistency

T.T.A. [%] = 𝑨 𝒙 𝟎.𝟓 𝒙 𝟑𝟏 𝒙 𝟏𝟎

𝑾 𝒙 𝑪𝒚

4.0 Soda Content In Lime Mud [Lime Mud Filter]

a. Weigh 5 grams, to the nearest 0.01 gram, off oven dry lime mud and place in a

beaker.

b. Add ± 100 mL of hot destilled water and agitate.

c. Filter the mud solution through a filter paper into a flask and rinse beaker with ± 100

mL of hot distilled water.

d. Add few drops of Methyl Orange indicator to the filtrate and titrate with 0.1N

Hydrochloric acid [HCl] to a reddish end point, record as (A) the volume of 0.1N

HCl consumed.

4.1. Calculation

A = Volume of 0.5N HCl consumed [mL];

W = Weight of sample [grams]

Cy = Consistency

T.T.A. [%} = 𝐀 𝐱 𝐍 𝐱 𝟑𝟏 𝐱 𝟏𝟎

𝐖 𝐱 𝐂𝐲

Example:

Sample W Cy A T.T.A. [%]= 𝑨 𝒙 𝟎.𝟓 𝒙 𝟑𝟏 𝒙 𝟏𝟎

𝑾 𝒙 𝑪𝒚

C 4.9522 55.3 22.18 12.55

W 5.0124 44.8 4.38 3.02

St 3.9470 46.5 3.41 2.88

F1 3.1829 68.5 1.37 0.97

F2 2.8845 67.9 1.56 1.23


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4.2.2.2 Reburned Lime Analysis (Available CaO)

1.0 Sampling

Obtain a lime sample and place in a sealed container.

2.0 Procedure

a. Grind the sample to a powder and thoroughly mix.

b. Screen the powder utilizing a 100 mesh sieve.

c. Regrind the material that would not pass through the 100 mesh sieve.

d. Thoroughly mix the resulting powder.

e. Weigh a 0.5 gram sample to the nearest 0.01 gram.

f. Add 20 mL destilled free CO2 (boil), shake well and again add 150 mL distilled free

CO2, shake well.

g. Heat to boiling and boil the lossy stoppered flask for 2 (two) minutes.

h. Add 15 gram sucrose (sugar). Shake well and boiling again until all sugar dissolve.

i. Keep it for 45 minutes ± 15 minutes for cooling or cooled it with tape filter water.

j. Add a few drops of PP indicator to the filtrate and titrate with 0.5N Hydrochloric acid

[HCl} to a reddish end point, record as (A) the volume of 0.5N Hydrochloric acid

consumed.

3.0 Calculation

A = Volume of 0.5N HCl consumed [mL]

W = weight of sample [mg]

N = Normally of HCl

% CaO available = 𝐀 𝐱 𝐍 𝐱 𝟐𝟖

𝐖 𝐱 𝟏𝟎𝟎%

Example:

Sample W N A % CaO available = 𝐀 𝐱 𝐍 𝐱 𝟐𝟖

𝐖 𝐱 𝟏𝟎𝟎%

LK 0.5003 0.5 32.62 91.3

TF 0.5047 0.5 32.18 90.0

4.2.2.3 Reburned Lime Analysis (Residual CaCO3)

1.0 Purpose

The residual carbonate [CaCO3] should be maintained in a certain range, very low or very

high residual carbonate will cause problems in the process. The amount of residual

carbonate [CaCO3] should be maintained in the range of 0.5% ~ 3.0%.


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2.0 Sampling

Obtain a lime sample and place in a sealed container. The same sample used for the

available CaO analysis should also be utilized for the residual Carbonate analysis.

3.0 Procedure

a. Add sufficient distilled water to the leveling bottle (#88 on attached diagram) to fill

the graduated burette (#89 on attached diagram) to the zero mark when the leveling

bottle is resting on it’s shelf.

b. Add 0.4 grams of lime sample to the compartment of the mixing flask (#87 on the

attached diagram.

c. Pipette (5) five mL of 20% hydrochloric acid (HCl) into other compartment of the

mixing bottle, being carefull not to mix the acid and lime sample at this time.

d. Open tap (#16 on attached diagram), the water level in the graduated burette should

be at zero.

e. Place the rubber stopper firmly into the top of the mixing flask the close the tap (#16

on the attached diagram)

f. Tilt the mixing flask so that the Hydrochloric acid [HCl] mixes with the lime sample.

g. Insert the mixing flask into a cooling bath until the bottle reaches room temperature.

h. Record the liquid level in the graduated burette, the liquid level corresponds to the

volume of residual carbonate in the lime sample. ( a reading of 1 equals 1% residual

carbonate).

4.0 Calculation

% Residual Carbonate = mL Reading on Graduated Burette

4.2.2.4 Acid Insolubles In White Liquor

1.0 Procedure

1. After checking for suspended solids in the white liquor sample Hydrochloric acid

1:1 to the sinter glass crucible [50mL].

2. Wash the precipitate with hot destilled water until free of acid (check with Methyl

Orange indicator until colour is yellow).

3. Dry the Sinter Glass Crucible in oven at 1050 C± 2

0 C for (2) two hours then cool

in desicator and weigh, to the nearest 0.1 grams, record the weight.


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2.0 Calculations

D = Volume of Sample [mL]

B = Weight [grams] of crucible and sample (after adding HCl 1:1)

A = Weight [grams] of crucible

Acid Insolubles [ppm] = [C-A] x 1000 x 𝟏𝟎𝟎𝟎

𝑫

4.2.2.5 Reduction Efficiency (Green Liquor & Smelt)

1.0 Purpose

Green liquor and Smelt Reduction Efficiency is defined as the percentage ratio of Sodium

Sulphide [Na2S] to the totel of Sodium Sulphide [Na2S] plus Sodium Sulphate [Na2SO4]

expressed as percentage Sodium Oxide [Na2O].

2.0 Determination Of Reduction Efficiency

2.1 Sampling

i. Green Liquor

a. Obtain a green liquor sample approximately 250 mL from the dissolving tank

or the green liquor storage.

b. Run liquor from sample line for a few minutes to ensure that a fresh sample is

obtained.

ii. Smelt

a. Using the sample red obtain a smelt and put it into sample cup and

immediately closing tightly the cap.

b. Prepare approximately 500 mL of CO2 free distilled water by boiling it for

about (10) ten minutes.

c. Allow the smelt sample to cool, and when cool remove the sample container

cap.

d. Remove the hardened smelt and as rapidly as possible immerse it in the CO2

free distilled water to dissolve.

e. Boil the smelt solution for approximately (15) fifteen minutes.


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2.2 Procedure

i. Determination Of Sodium Sulphide [Na2S]

a. Pipette 5.0 mL of clesr sample liquor and let drain into a 250 mL Erlenmeyer

flask, then add 50 mL of distilled water.

b. Add 25 mL of 10% Barium Chloride [BaCl2] and few drops of

phenolphthalein indicator.

c. Stir sample and titrate with 0.5N Hydrochloric acid [HCl] until the reddish

colour turns milky white, stop the titration and record titrated volume [mL] as

(A).

d. Add 5 mL of 40% Formaldehyde and then continue to titrate until the reddish

colour again turns milky white, stop the titration and record titrated volume

[mL] as (B).

e. Add a few drops of Methyl Orange indicator and then continue to titrate until

the yellow colour again turns to an orange colour, stop the titration and record

titrated volume [mL] as (C).

4.2.2.6 Density of Heavy Black Liquor

Note: Density is defined as the weight [grams] per unit of volume [mL].

1.0 Sampling

a. Run liquor from sample line for a few minutes to ensure that e fresh sample is

obtained.

b. Obtain a heavy black liquor sample and seal the container.

2.0 Specific Gravity by Direct Weighing

a. Clean a 25 mL graduated cylinder with distilled water and dry in oven at 105oC ± 3

o

C.

b. Cool the dry graduated cylinder in desiccators and weigh.

c. Vigorously stir the heavy black liquor sample and then pour exactly 25 mL into

graduated cylinder and weigh.

3.0 Calculation

A = weigh of sample and graduated cylinder [grams].


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B = weigh of empty graduated cylinder [grams].

C = volume of sample [mL].

Density [grams/cc] = (A−B)

V

4.0 Specific Gravity by Hydrometer

a. Shake the sample in the bottle well.

b. Pour into hydrometer cyilinder or graduated measuring cylinder until it over flows.

c. Dip the hydrometer and thermometer into the cylinder.

d. Read the special gravity and temperature at the same time.

e. Use the following temperature correction table to find the special gravity.

Table 5. SpGr Temperature (oC)Correction for HBL

4.2.2.7 T.A.A., T.T.A. & Na2CO3 IN WBL, HBL & SOAP SKIMMING

1.0 Sampling

a. Run liquor from sample lines for a few minutes to ensure that a fresh sample is

obtained

b. Obtain Heavy Black Liquor sample and store in a completely filled alkali resistant

bottle.

c. Obtain Weak Black Liquor sample and store in completely filled alkali resistant

bottle.

oC 0 1 2 3 4 5 6 7 8 9

3 0.001 0.0013 0.0013 0.0020 0.0024 0.0027 0.0030 0.0033 0.0037 0.0040

4 0.0043 0.0046 0.0048 0.0051 0.0053 0.0056 0.0060 0.0064 0.0069 0.0073

5 0.0077 0.008 0.0083 0.0087 0.0090 0.0093 0.0097 0.0101 0.0105 0.0109

6 0.0013 0.0116 0.0120 0.0123 0.0127 0.0130 0.0134 0.0138 0.0142 0.0145

7 0.0150 0.0157 0.0163 0.0170 0.0176 0.0183 0.0190 0.0197 0.0204 0.0210

8 0.0217 0.0228 0.0238 0.0249 0.0259 0.0270 0.0279 0.0289 0.0229 0.0308

9 0.0317 0.0324 0.0330 0.0337 0.0343 0.0350 0.0353 0.0355 0.0358 0.0360

10 0.0363 0.0365 0.0368 0.0370 0.0373 0.0376 0.0378 0.0381 0.0383 0.0386


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2.0 Procedure

Standardize the pH meter [following the standardizing procedure] with buffer solution pH =

4.0 and pH = 7.0.

2.1 Procedure for Weak Black Liquor & Soap Skimming

a. Pipette 2.0 mL of sample liquor into a 250 mL beaker containing 100 mL of distilled

water.

b. Place the beaker with the sample on a magnetic stirrer then add 25 mL of 10% Barium

Chloride [BaCl2].

c. Insert the electrode of the pH meter into the sample then turn on the pH meter.

d. Stir sample and add 5 mL of 40% formaldehyde the immediately titrate with 0.5 N

Hydrolchloric acid [HCl] to a pH of 8.3, then immediately stop the titration and

record titrated volume [mL] as (A).

e. Continue to titrate to a pH of 4.3, then immediately stop the titration and record

titrated volume [mL] as (B).

Calculation

Note : All calculations are expressed as Grams per Litre of Sodium Oxide [Na2O]

V = volume of sample [mL]

T.A.A. [grams/litre] = A × 31 ×0.5

V

T.T.A. [grams/litre] = B × 31 ×0.5

V

Na2CO3 [grams/litre] = B−A × 31 ×0.5

V

Example:

2.2 Procedure for Heavy Black Liquor

a. Determine the density of the heavy black liquor.

b. Clean a 25 mL graduated cylinder with distilled water and dry in oven at 105oC.

c. Cool the dry graduated cylinder in desiccators and weigh.


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d. Vigorously stir the heavy black liquor sample and then pour exactly 25 mL into

graduated cylinder and weigh.

A = weigh of sample and graduated cylinder [grams].

B = weigh of empty graduated cylinder [grams].

C = volume of sample [mL].

Density [grams/cc] = 𝐀−𝐁

𝐂

e. Place approximately (± 2 ) two grams of heavy black liquor into a 250 mL beaker.

f. Add to the beaker 100 mL of distilled water.

g. Place beaker with sample on magenetic stirrer and add 25 mL of 10% Barium

Chloride [BaCl2].

h. Insert the electrode of the pH meter into the sample then turn on the pH meter.

i. Stir sample and add 5 mL of 40% formaldehyde the immediately titrate with 0.5N

Hydrochloric acid [HCl] to a pH 8.3, then immediately stop the titration and record

titrated volume [mL] as (A).

j. Continue to titrate to a Ph of 4.3, then immediately stop the titration and record

titrated volume [mL] as (B).

Note : All calculations are expressed as Grams pe Litre of Sodium Oxide [Na2O]

D = density of sample [grams/cc] = 1.41

W = weight of samplpe [grams]

T.A.A. [grams/litre] = 𝐀 ×𝟑𝟏 ×𝟎.𝟓 ×𝟏.𝟒𝟏 (𝐃)

𝐕

T.T.A. [grams/litre] = 𝐁 ×𝟑𝟏 ×𝟎.𝟓 ×𝟏.𝟒𝟏 (𝐃)

𝐕

Na2CO3 [grams/litre] = (𝐁−𝐀) ×𝟑𝟏 ×𝟎.𝟓 ×𝟏.𝟒𝟏 (𝐃)

𝐕

2.1.1 Free Lime Analysis

1.0 Purpose

This procedure is written to define the method to determine the residual Calcium

Oxide (CaO) in lime mud as an indication of causticizing efficiency.


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2.0 Sampling

Obtain lime mud cake from lime mud filter and place into a plastic bottle and cap tightly.

3.0 Procedure

a. Pour about 20 mL of distilled water, free from carbon dioxide in a 300 mL conical

flask.

b. Weigh 20 gram portion of prepared sample to the nearest 1 mg and carefully brush it

into the flask, stopper the flask immediately.

c. Disperse the sample thoroughly in the water by swirling motion.

d. Remove the stopper and place the flask on the hot plate and immediately add 150 mL

of boiling carbon dioxide free water, swirl the flask and boil actively for 1 minute to

achieve complete slaking.

e. Remove the flask from the hot plate, stopper it loosely and place it in a cold water

bath to cool it room temperature.

f. Add 15 gram sugar, stopper the flask, swirl and allow it to stand for 15 minutes to

react.

g. Swirl at 5 min intervals during the reaction period, alternatively a magnetic stirrer

may be used.

h. Remove the stopper, add 4 to 5 drops of the PP indicator solution, wash down the

stopper and the sides of the flask with carbon dioxide free water.

i. Titrate rapidly with 0.5 N standardized HCl, swirl or stirrer the solution during the

entire titration.

j. When the first complete disappearance of the pink colour is observed, read the end

point, ignore the return of the pink colour (A).

4.0 Calculation

X = 2.8 A .C

W

Where ;

X = the content of free lime (residual available CaO), %

A = Volume of titration consumed (mL)

C = Concentration of HCl (N)

W = weight of sample (grams)


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CHAPTER 5

CONCLUSION AND SUGESSTION

5.1 Conclusion

Writers conclude this report with some conclution related to the Bleaching and

Recausticizing particularly and whole process widely below:

1. PT. TOBA PULP LESTARI, Tbk uses the Alkali Active as liquid for cooking the

wood (chips) to produce pulp.The Active Alkali are NaOH and Na2S.

2. There is a relationship among Kappa number, Viscosity, Soda Loss, and Pulp

Brightness. They relate proportionally each other. A high amount of Kappa number

means that some lignins are still left on the pulp with high amount.This will increase

the number of Viscocity and Soda Loss. It is happened because a large amount of

chemical is needed to cook the wood (chips), then chemical is left on the pulp and

makes the number of Soda Loss increases. As a result, the brightness of pulp would

get lower.

3. Kraft process is applied on pulping process at PT. TOBA PULP LESTARI, Tbk.

5.2 Suggestion

Actually PT. TOBA PULP LESTARI, Tbk has shown that they has such good process

and a high quality product. But, writers suggest that the company give a chance for the

student to join either the Complete Analysis section or Chemical Plant Analysis section. For

another student who has a willing to take fieldwork on PT. TOBA PULP LESTARI, Tbk,

writers suggest to learn about the process firstly. This would help us to understand the

activity on its laboratory.


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REFERENCES

Browning, Bertie Lee, “The Chemistry Of Wood” Krieger Drive, Florida (1963)

PT. Toba Pulp Lestary, Tbk., “Introduction to Pulping Technology Training Manual “ Porsea

(1991)

Romeyko, Thomas. ”The Analysis of Training and Development of Employees at PT. TOBA

PULP LESTARI, Tbk.” University of Colombus, Medan (2006)

Rydholm, Sven A., “Pulping Processes” John Wiley & Sons, Ltd, Great Britain (1965)

Toba Pulp Lestari, “Digester Training Manual” PT. TOBA PULP LESTARI, Tbk., Porsea

Toba Pulp Lestari. “Company Profile” PT. TOBA PULP LESTARI, Tbk., Porsea


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APPENDIX


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Fibre Line Quality Plan Matrix-Toba Cell Eucalyptus Pulp Process

Number Area Department

Test Or Inspection Unit Minimum Maximum

1. Washing/ Screening (W4)

Unbleach Viscosity, CUAM

Cp 13 30

Pulp Kappa Number - 4 9

Soda Loss Kg/ton pulp

5 10

Conductivity ms/cm - 1.5

2. Bleach Plant

DO Tower Inlet pH - 1.0 2.5

Stage brightness % ISO 60 -

Stage viscosity, CUAM

Cp 12.5 27

EO Vat Washer pH - 10 11.5

Washer Brightness % ISO 75 -

Stage viscosity Cp 12 25

D1 Vat washer pH - 2.5 4.5

Stage brightness % ISO 87 -

Stage Viscosity, CUAM

Cp 11 20

D2 Vat Washer pH - 2.5 4.5

Stage brightness Cp 88 -

ISO 9001 Quality Management System


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Recauseting And Lime Kiln Quality Plan Matrix

Number Area Department Test or Inspection Unit Minimum Maximum

1. GL Clarifier NaOH gpl 13 25

Na2S gpl 18 28

Na2CO3 gpl 70 85

TAA gpl 31 53

TTA gpl 101 138

2. Slaker Outlet NaOH gpl 65 80

Na2S gpl 18 28

Na2CO3 gpl 20 30

TAA gpl 83 108

TTA gpl 103 138

Causticizing Efficiency (CE) % 65 76

Temperature 0C 100 105

3. Cauticizer Outlet NaOH gpl 75 85

Na2S gpl 18 28

Na2CO3 gpl 18 28

TAA gpl 93 113


4. WL Storage NaOH gpl 75 85

Na2S gpl 18 28

Na2CO3 gpl 18 28

TAA gpl 93 113

S % 20 29

Level % 15 -


Flow M3/hr - As per Costumer Request

4a. WL clarifier-Mud Consistency % 35 55

TTA % 11 16

Density Baume 40 50

4b. Inlet ECO filter NaOH gpl 75 85

Na2S gpl 18 28

Na2CO3 gpl 18 28

TAA gpl 93 113

S % 20 29


5. WWL TTA gpl 18 -

Flow M3/hr - As per Costumer Request

6. Lime Mud Washer

Consistency % 35 55

TTA gpl 2.3 5.0

Density Baume 40 55

6a. Lime Mud Storage

Consistency % 35 55

TTA % 2.3 5.0

7. Lime Mud Filter #1

Consistency % 40 85


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Filter #2 TTA gpl 35 1.5

8. Lime Kiln Cao Purity Lime Kiln % 76 -

Residual CaCO3 Lime Kiln % - 7

Cao Puruty Table Feeder % 70 -

Pressure Bar - 0

9. Purchase Material

Lime Stone Per Specs

Per Specs Per Specs

Burnt Lime Per Specs

Per Specs Per Specs

ISO 9001 Quality Management System


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Bleaching and Recousting Analysis

Brightness Meter Viscometer Bath Digital Burette

Hand Sheet Forming

Mch. Analytical Balance pH Meter

Oven Desiccator Shaker


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Magnetic Stirrer Viscometer Stopwatch

Vacuum Pump Pipe Ball Infrared Lamp

Bleaching Sample Soda Loss Analysis Brightness Viscosity Sampling


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Kappa Analysis Sample Washing Viscosity Analysis

Liquor Sample Total Solid Analysis Liquor Analysis

Liquor Analysis Lime Mud Sample Consistensy Analysis

Documents

Fieldwork Report (Done 2007)