NBSIR 73-416

Report on Meeting of ISO/TC 6/SC 5

Testing Metliods and Quality

Specifications for Pulp

William K. Wilson.* John H. Schulz.** C. Edwin Brandon,*** Joseph L. Borstelniann,*=*

*National Bureau of Standards

**Continental Can Company. Inc. ***Miami University, Oxford. Ohio

****Technical Association of the Pulp and Paper Industry

November 16. 1973

Meeting Held in Madrid. Spam

November 2-8. 1973

U. S DEPARTMEIMT OF COMMERCE, Frederick B. Dent, Secretary

IMATIONAL BUREAU OF STANDARDS, Richard W Roberts Director

NBSIR 73-416

REPORT ON MEETING OF ISO/TC 6/SC 5 TESTING METHODS AND QUALITY

SPECIFICATIONS FOR PULP

William K. Wilson,* John H. Schulz.** C. Edwin Brandon,*** Joseph L. Borstelmann,****

*National Bureau of Standards

*Continental Can Company, Inc. *Miami University, Oxford, Ohio

*Technical Association of the Pulp and Paper Industry

November 16, 1973

Meeting Held in Madrid, Spain

November 2-8, 1973

U. S. DEPARTMENT OF COMMERCE, Frederick B. Dent, Secretary

NATIONAL BUREAU OF STANDARDS, Richard W. Roberts, Director

TAElLE OF CONTENTS

Page

1. STATEMENT OF RESULTS 1

2. BACKGROUND 2

3. GENERAL IMPRESSIONS 6

4. RECOMT^ENDATIONS 8

5. REPORT ON MEETING OF WORKING GROUP 1,

SALEABLE MASS OF PULP

.

10

5.1 Agenda of Meeting 10

5.2 Secretariat Memorandum of September 1973 ... 11

5.3 Discussion at Working Group Meeting 12

6 . REPORT ON MEETING OF WORKING GROUP 6

,

AQUEOUS EXTRACTS 14

6.1 ^igenda of Meeting 14

b.2 Secretariat Memorandum of September 1973 ... 16

6.3 Discussion at Working Group Meeting 17

7. REPORT ON MEETING OF WORKING GROUP 8,

PREPARATION OF LABORATORY SHEETS FOR ' PHYSICAL

TESTING 19

7.1 Agenda of Meeting 19

7.2 Secretariat Memorandum of September 1973 ... 20

7.3 Discussion at Working Group Meeting 21

8. REPORT ON MEETING OF WORKING GROUP 1 OF SC 2

,

OPTICAL PROPERTIES OF PAPER, BOARD, AND PULP .... 23

8.1 Agenda of Meeting 23

8.2 Secretariat Memorandum of September 197 3 ... 24

8.3 Discussion at Working Group Meeting 25

9. REPORT ON TECHNICAL SESSION OF SC 5 27

9.1 Opening of the Meeting 27

9.2 Saleable Mass, in Lots, of Pulp 28

9.3 Disintegration for Tests on Unbeaten Pulps . . 29
Page

9.4 Laboratory Beating of Pulp 30

9.5 Preparation of Laboratory Sheets 31

9.6 Testing of Physical Properties of Pulp ... 33

9.7 Viscosity of Pulp. 34

9.8 Aqueous Extracts of Paper and Pulp 35

9.9 Dirt and Shives in Pulp 36

9.10 Determination of Total Sulphur Content ... 37

9.11 Optical Properties of Pulp 38

9.12 Revision of ISO Recommendations 39

9.13 Canadian Standard Freeness 40

9.14 Schopper Riegler Freeness ... 41

9.15 Accelerated Aging of Pulp . 42

10. DRAFT RESOLUTIONS 43

11. PROGRAM FOR FUTURE WORK 49

12. TIME AND PLACE OF NEXT MEETING 50

13. SPECIAL EVENTS 51

14. APPENDIX .... . , 52

14.1 Agenda of Meeting of SC 5 52

14.2 Delegates to Meeting of SC 5 55

14.3 Delegates to Eighth Meeting of WG 1,

Saleable Mass of Pulp ........... 56

14.4 Delegates to Second Meeting of WG 6,

Aqueous Extracts 57

14.5 Delegates to Meeting of WG 8,

Preparation of Laboratory Sheets ...... 58

14.6 Delegates to Meeting of WG 1 of SC 2,

Optical Properties of Paper, Board, and Pulp 59

14.7 List of Working Groups 60

14.8 ISO Recommendations From SC 5 ....... 62

14.9 6/5 N 416, Comparison of Methods for

Sulphate Ion Determination 63
1. STATEMENT OF RESULTS^

Over 30 delegates from Canada, Finland, France, Germany,

Norway, Poland, Portugal ^ Spain, Sweden, United Kingdom, and

the USA attended a meeting in Madrid of the Subcommittee of

the International Organization for Standardization (ISO)

dealing with testing methods and quality specifications for

pulps used for papermaking and other purposes; an observer

from the customs cooperation council was also present.

Methods were agreed upon for the determination of

saleable mass of flash-djried pulps, for disintegration of

pulp, laboratory beating of pulp, preparation of laboratory

sheets, and measurement of ISO brightness of pulps.

It was also agreed to revise current ISO Recommendations

for determination of saleable mass of pulp in lots (R 801)

,

determination of dry matter content (R 638) , and calcium,

copper, iron, and manganese content of pulp (R 777, 778, 779,

and 1830)

.

Many other items were discussed. Plans were made to continue studies of methods for the determination of viscosity,

aqueous extraction, dirt and shives, total sulphur content,

saleable mass of unitized lots of pulp, statistical evaluation

of number of sample bales, preparation of laboratory sheets

by the Rapid-Kothen method, and fiber classification and drainability.

T'he Subcommittee met from 6th to 8th November 1973

inclusive, under the chairmanship of Professor Waldemar

Jensen (Finland)

.

^Statement prepared for the press by the Editing Coimnittee,

with minor changes.
2

2 . BACKGROUND

The International Organization for Standardization was

established in 1947 for the development of standard methods

of evaluation and specifications that would be useful in

international trade. TC 6, Paper, was organized in 1947,

and France has held the Secretariat continuously since that

time. SC 5, Testing Methods and Quality Specifications for

Pulp, was organized in 1961 and the Secretariat was entrusted

to Finland. Dr. Waldemar Jensen, Managing Director of the

Finnish Pulp and Paper Research Institute, has assumed the

responsibility for this work. His Institute is responsible

for five of the eight working groups, and for those efforts

for which working groups do not exist.

The first meeting

the second in Paris in

fourth in Stockholm in

in 1967, the sixth in 0

London, England in 197

The U.S. did not partic

was represented by one

Stockholm, by seven del

in Oslo, and by four in

of SC 5 was held in Helsinki in 1961,

196 2, the third in Rome in 196 3, the

1965, the fifth in Montreal, Canada

slo, Norway in 1969, the seventh in

0, and the eighth in Berlin in 1972.

ipate in the first two meetings, but

delegate in Rome, by two delegates in

egates in Montreal, by three delegates

London, and by three in Berlin*.

The following countries are participating members of

SC 5 (P members)

:

Australia

Belgium

Bulgaria

Canada

Colombia

Czechoslovakia

Ethiopia

Finland (Secretariat)

France

Germany

Israel

Italy

Netherlands

New Zealand

Norway

Poland

Portugal

Rumania

Spain

Sweden

United Arab Republic

United Kingdom

USA

USSR

Participating members may contribute to the work of the

Subcommittee and are entitled to vote on documents as they

are processed through channels.

*A special meeting of SC 5 was held in Helsinki in August

1968 to discuss questions relating to the laboratory beating

of pulp.
3

A country with observer status receives all communications but cannot vote. The following countries are listed

as observer members (O members):

Member countries operate through their national standardizing organizations. In the U.S. this is the American National

Standards Institute. Members of working groups may communicate

directly with each other.

Liaison organizations with SC 5 include the following:

1. Customs Cooperation Council

2. Secretariat of TC 6/SC 2, Test Methods for Paper

and Paperboard

3. Secretariat of TC 38, Textiles, SC 16, Chemical

Testing

.

4. lEC (International Electrotechnical Commission)/

rc 15, Insulating Materials

Methods and specifications are developed in SC 5 specifically for use in the buying and selling of pulps. Therefore,

purely empirical methods may be very useful, but the tendency

is to keep the methods as close to current scientific developments as possible. Process control methods are not considered.

Most of the effort on standards, both national and international, in Europe is through research institutes which may

also act as standardizing bodies. Research on materials, the

development of test methods, the writing of specifications,

and the promulgation of standards are all within one organization. Thus, it is possible to make the most of whatever

funds are available. Funds usually come from both industry

and government, as in Sweden. The Norwegian Pulp and Paper

Research Institute is supported entirely by industry.

The European members of SC 5 have contributed a large

part of the effort. The Scandinavian countries in particular

are strong in SC 5, and are responsible for all of the eight

working groups. The U.S. participates in all of the working

groups

.

Austria

Cuba

Denmark

India

J apan

Peru

Republic of South Africa

Switzerland

Yugoslavia
There is no accepted procedure for determining the

relative level of effort that might be expected of a country

participating in the work of ISO/TC 6/SC 5. As ISO test

methods are designed to assist in the buying and selling of

pulp, the sum of a country's imports and exports as a percentage of the total imports and exports of the countries

participating in SC 5 might be used as a rough guide. These

data for 1972 are given in Table 1. According to this formul

the U.S. should be contributing about 20 percent of the total

effort of SC 5.

An organization called the Commission European de

Normalisation (CEN) has been in existence for many years,

but has not been particularly active until the past two years

CEN is the European response to ISO. It is a standardizing

organization for the European Economic Community (EEC) and

the European Free Trade Association (EFTA) . Most European

countries that dD not be!|.ong to the EEC belong to EFTA.

CEN standards are obligatory on the EEC and EFTA

countries six months after adoption.
5

Table 1. Pulp imports and exports fo^: 1972^ of the

countries participating in JSO/TC 6/SC 5.

% of

Imports Exports To:al Grand Total

thousands of metric tons

Australia 273 11 284 1.0

Belgium 358 126 4 84 1.7

Bulgaria 80 16 96 . 3

Canada 96 5 , 536 5,p32 20 .

2

Colombia 58 5 63 . 2

Czechoslovakia 87 17 104 . 4

Ethiopia 4 0 4 . 1

Finland A4 1 , b 11 1 , p 1

5

c o D . O

France 1,333 150 1,483 5 . 3

Germany 1,720 100 1,820 6 . 5

Israel 55 c c

. 2

Italy 1,245 2 1,247 4 . 5

Netherlands 621 13 634 2 . 3

New Zealand 14 110 124 . 4

Norway ^ X u / O J QQy ZJ ~J5 3 6

Poland 1 Q X z 9 0 7 7

Portugal 19 380 399 1.4

Rumania 66 41 107 .4

Spain 340 16 356 1.3

Sweden 37 3,741 3,778 13.6

United Arab Republic 35 35 .1

UK 2 ,190 3 2,193 7.9

USA 3,386 2,029 5,415 19.4

USSR 265 467 732 2.6

Grand Total 27,862

^Pulp and Paper International, Review Number, July 1973.
6

3. GENERAL IMPRESSIONS

The meetings are very formal. English is the principal

language, but translations are almost always made into French.

Most of the delegates are operating outside of their native

tongue. It is desirable for the U.S. delegates to be deliberate

in their speech and to k€;ep the use of idioms to a minimum.

Rapport between the U.S. delegates and the other delegates

appears to have become much better with each meeting. This

has been possible for two reasons: (1) the delegations from

most countries are remarkably constant from year to year, and

(2) as the U.S. shows more and more interesf: in the work of

SC 5, U.S. delegates are recognized as members of the group.

The experience of this meeting confirms the experience

at the Montreal, Oslo, and London meetings of the desirability

of sending a delegation of several members. Two or more

working groups may meet simultaneously. As it is impossible

for one person to be expert in all technical areas, it is

desirable to ask that each delegate be responsible for specific

items on the agenda. This worked very well in Montreal, Oslo,

London, and Berlin, and the U.S. had at least one knowledgeable

delegate in each technical area.

Delegates should be fully prepared on the subjects for

which they are responsible. This should include a knowledge

of what is in the literature, of what the working group is

doing, including all documents from the secretariat, need

for specific methods, and economic implications .

It is unnecessary for delegates to be able to speak or

understand French, but even a mediocre command of another

language (French, German, Italian, Spanish) can be helpful

as a generator of goodwill.

When traveling to Europe, delegates should allow at

least one full day for the body to adjust to the "compression

of time." A few hours rest after checking into the hotel

usually is sufficient.

Technical progress is slow, but the goodwill generated

from sincere cooperation on an international level is of

great value. However, when international committees operate

in the same way as national standardizing committees, the

speed of action is much less. Unless some mechanism can be
7

found to accelerate ISO v^drk, the effectiveness of the

organization is likely to deteriorate. It has been pointed

out that (1) we must achieve standards in half the time if

our efforts are to be useful; (2) a good standard is better

than a best standard if it is completed in time to be used;

(3) the lifetimes of many products are shorter than the time

required to develop an ISO standard; (4) the Central

Organization must exercise more stringent control over the

technical committees; (5) ISO must rethink its objectives

and priorities or it will become obsolete.^

The Commission European de Normalisation, mentioned in

section 2, has the capacity to be a real factor in trade in

Europe. Therefore, it would appear that involvement in

ISO is of vital importance.

^Address by R. L. Hennessy, Executive Director, Standards

Council of Canada, before an ISO session, The World Going

Metric—Impact on International Standardization, Washington,

D.C., September 12, 1973.
8

4 . RECOMMENDATIONS

The U.S. should continue to consider the work of ISO/

TC 6/SC 5 important find to participate actively in the

work of this subcommittee and of its wo:pking groups.

In addition to participating actively in working groups,

the U.S. should assume responsibility for some, as new

ones are formed. This participation deinands work in

the laboratory. Contributing to a discussion at a

meeting, or responding to a questionnai.jre , cannot be

considered as active participation.

Delegates should be gent to all meetingi? of SC 5 and to

meetings of the working groups. Progress usually is

best achieved through personal contact as the mission

of a working group or indication of need for a method

can change drastical3.y during discussiop at a meeting.

Continuity of effort and continuity of delegate participation is important. Within the experience of the U.S.

delegates (7 meetings) , a hard core of delegates familiar

with the history and technology of the y^ork, has attended

from most of the countries.

If possible, comments on methods should be presented in

writina before meetings are held, and a delegate should

be present at the meeting to present the- comments in

person.

In order to implement Recommendation No. 5, ASTM and TAPPI

methods that are pertinent to the work of SC 5 should be

examined on a continuing basis and suitable methods submitted to ANSI Committee P3.

The U.S. should propose methods to the working groups as

early as possible in the development of the work. These

should be ANSI standards, although TAPPI or ASTM standards

would have adequate standing.

It is very important that methods be submitted through

the cognizant committeeman or, still better, through the

working group' representative. If a proposed method is

outside the framework of an established working group,

need for the method should be well documented and suggested

as an item on the program for future work.
9

9. In view of the increasing activity of tlie Cominission

European de Normalisation, the U.S. Committee for ISO/

TC 6 should make every effort to accelerate participation

in ISO.
10

5 . REPORT ON MEETING OF WORKING GROUP 1

,

SALEABLE MliSS OF PULP

5.1 Agenda of Meeting

. The eighth meeting of ISO/TC 6/SC 5/WG 1 was held at

Institute Nacional de Investigaciones Agrarias, Avenida de

Puerta Hierro, s/n, Madrid, Spain, on Monday, 5th November

1973, at 9 a.m.

1. Opening of meeting

2. Election of chairman

3. Approval of draft agenda

4. Statistical evaluation of number of sample bales

documents: ISO/TC ^/SC 5/WG 1 (Secretariat-17) 46

ISO/TC 6/SC 5/WG 1 (Finlapd-4) 49

ISO/TC 6/SC 5/WG 1 (USA-3) 52

ISO/TC 6/SC 5/WG 1 (Secre tariat-19 ) 53

5. Determination of saleable mass in lots of flash dried pulp

docurrent: ISO/TC 6/SC 5 (Secretariat-192 ) 410

6. Sampling of unitized bales for moisture testing

document: ISO/TC 6/SC 5/WG 1 (Secretariat-21) 55

7. Revision of ISO Recommendation R 801

document: ISO/TC 6/SC 5/WG 1 (Secretariat-22) 56

8. Program of future work

9. Other questions

10. Closing of meeting
11

5.2 Secretariat Memorandum of September 1973

(Secretariat-193) 411

Statistical evaluation of number of sample bales

The principles of the method for the evaluation of the

number of sample bales have been discussed on several occasions and based on these discussions, document 6/5/1 N 46

was drafted and submitted for comments in 1972. Later two

opposite documents concerning the number of degrees of freedom

to be used for the calculation of the confidence limits have

been presented by Finland and the USA.

In document 6/5/1 N 53 the Secretariat proposed that

Technical Committee 69, Application of Statistical Methods,

be consulted. This proposal has been seconded by France and

Norway and no objections have been made.

Determination of saleable mass in lots of flash dried pulp

At the Berlin meeting of ISO/TC 6/SC 5/WG 1 the United

Kingdom proposal, document 6/5 N 223, amended as suggested

by the United Kingdom in document 6/5/1 N 50, was agreed upon

in principle. The revised draft, document 6/5 N 410, is

being considered simultaneously by Subcommittee SC 5 and

working group 1.

Sampling of unitized bales for moisture testing

A draft based on the principle presented by Finland is

being considered by the working group.

Revision of ISO Recommendation R 801 . Comments were made during the Berlin meeting of SC 5

to the effect that the test piece drying procedure should be

revised. In addition to the proposals made in connection

with the revision of ISO Recommendation R 638 to change the

basic drying temperature, no definite suggestions for revision

have been made. Any available information would be very much

welcomed.
12

5.3 Discussion at Working Group Meeting

Statistical evaluation of number of sample bales

The development of a statistical method for the determination of saleable mass was first discussed in Montreal in

1967. The discussions were continued in Oslo in 1969, in

London in 1970, and in Berlin in 1972. A method was submitted

prior to the Berlin meeting, but some of the statistical

methods used were questioned. The United States delegates

subsequently submitted a report on this queption. This report

was presented to the meml:)ers prior to the meeting. Three

major points were discussed.

1. There was a question concerning the number of degrees

of freedom to be used in selecting the "t" value used in

calculating the confidence limits. The Secretariat is to

contact ISO/TC 69 on Application of Statistical Methods for

advice on this question.

2. The formula to be used for calculating the confidence

limits was discussed. Two formulas are available with the

choice of the formula depending upon the type of variation

present. In this method, both types of variation are present

and neither formula is correct. The formula used in this

method always gives confidence limits which are too narrow,

the other gives confidence limits which are too wide. The

decision as to which should be used was postponed until the

next meeting.

3. It was agreed that the method could not be used unless

at least 24 bales were sampled. The previous method permitted

as little as 12.

Saleable mass of flash dried pulp

The subject of testing flash dried pulp was first discussed in 1964 and has been on the agenda of every meeting

since. A special boring tool has been developed for drilling

these bales, and a method has been written around this tool.

The United States has encountered diffculty with this tool

but had nothing better to offer. Therefore, the method was

accepted after a statement was added concerning the problems

which might be encountered with certain types of pulp. A few

other editorial changes were made and the method was then

approved by the working group for submission to SC 5

.
13

Sampling unitized bales for moisture testing

A method for sampling unitized bales was submitted prior

to this meeting. It specified the sampling of three bales

from each unit sampled, with the number of units sampled to

be equal to the square root of the number of units shipped.

There was some question concerning the statistical approach

and the desirability of sampling six bales in each unit. The

United States representative on this working group is to

collaborate with the Finnish delegate in developing a satisfactory technique.

Revision of ISO Recommendation R 801, Saleable Mass of Pulp

This method had been presented to ISO member countries

for ballot to advance it to an ISO standard but had failed

to get the number of votes needed for advancement. Therefore, it was returned to SC 5 for revision.

It was agreed that the drying temperature should be

increased to 105 + 2°C. This is in accordance with the TAPPI

standard. No other changes were made. The method will now

be processed through SC 5, TC 6, and ISO member bodies. If

it is approved by a majority of the member bodies but fails

to obtain enough votes to make it an ISO standard, it will

be reissued as a revised ISO recommendation.

Canadian Method

A copy of the Canadian Method was submitted for consideration of the working group. Canada pointed out that this

method is a statistical method and suggested that it replace

R 801 and the proposed statistical option being considered for

R 801. Because it was submitted at the meeting there was very

little discussion. Comments can be submitted by mail, and it

will be discussed at the next meeting.
14

6. REPORT ON MEETING OF WORKING GROUP 6,

AQUEOUS EXTRACTS

6 . 1 Agenda of Meeting

The second meeting of ISO/TC 6/SC 5/WG 6 was held at

Institute Nacional de Investigaciones Agrarias, Avenida de

Puerta Hierro, s/n, Madrid, Spain, on Monday, 5th November

1973, at 2 p.m.

1. Opening of meeting

2. Election of chairman

3. Approval of draft agenda

4. Preparation of standard extracts

• documents: ISO/TC 6/SC 5/WG 6 (Secretariat-15) 28

ISO/TC 6/SC 5/WG 6 (Secretariat-18) 35

5. Determination of pH of standard extract^

documents: ISO/TC 6/SC 5/WG 6 (Secretariat-16 ) 29

ISO/TC 6/SC 5/WG 6 (Secretariat-18) 35

6. Determination of conductivity of standard extracts

documents: ISO/TC 6/SC 5/WG 6 (Secretariat-17 ) 30

ISO/TC 6/SC 5/WG 6 (Secretariat-18) 35

7. Determination of surface pH of paper

documents: ISO/TC 6/SC 5/WG 6 (Germany-4) 31

ISO/TC 6/SC 5/WG 6 (Swede^i-l) 32

ISO/TC 6/SC 5/WG 6 (Finland-3) 34

ISO/TC 6/SC 5/WG 6 (Finland-4) 36

ISO/TC 6/SC 5/WG 6 (Secretariat-19 ) 37

8. Determination of sulphate and chloride in aqueous extracts

documents: ISO/TC 6/SC 5/WG 6 (Netherlands-1) 4

ISO/TC 6/SC 5/WG 6 (Germany-1) 10

ISO/TC 6/SC 5/WG 6 (Germany- 2) 11

ISO/TC 6/SC 5/WG 6 (United Kingdom-2) 21
15

ISO/TC 6/SC 5/WG 6 (USA-1) 22

ISO/TC 6/SC 5/WG 6 (Finland-2) 23

ISO/TC 6/SC 5/WG 6 (Secret:ariat-14

)

ISO/TC 6/SC 5/WG 6 (Swederi-2) 33

Program of future work

Other questions

Closing of meeting
16

6.2 Secretariat memorandum of September 1973

Preparation of standard extracts

A revised working draft has been prepa^ped based on

comments by the Working Group members and information from

documents of ISO/TC 91, Surface Active Agents. As instructed

by the Berlin meeting of ISO/TC 6/SC 5, the Working Group

requested to re-examine the practicability of preparing one

single standard method for the preparation of aqueous extracts.

Determination of pH and conductivity of stapdard extracts

Revised proposals have been submitted to the Working

Group members for comments and discussion at the next meeting.

Determination of surface pH of paper

As agreed by the Berlin meeting of SC 5 this method will

be considered in relation to paper and boar(3 only. Several

comments on the German proposal, document 6/5/6 N 31, have

been received and counter-proposals have been presented by

Finland and Sweden.

Determination of sulphate and chloride content

As a result of the request of the Berlin meeting of SC 5,

one comment only, by Sweden, has been presented on the applicability of the various methods for determination of sulphate

and chloride content of aqueous extracts. It is hoped that

based on the test results presented in the Swedish comments

together with those received earlier, it will be possible at

the next working group meeting to agree, on the line of progress.

Program of future work

No proposals in regard to the two items included in the

program of future work, viz., determination of acidity and

basicity have been made.

Meeting of ISO/TC 6/SC 5/WG 6

Working Group ISO/TC 6/SC 5/WG 6, Aqueous Extracts, will

meet in Madrid on November 6, 1973. The draft agenda includes

all the above items and any results of the discussions will

be reported at the Subcommittee meeting.
6.3 Discussion at Working Group Meeting

Preparation of standard €>xtracts

Document (Secretariat-15 ) 28, Paper, Board, and Pulps

Preparation of Standard Extracts, was accepted in principle.

It was agreed that both hot and cold extraction is needed

and that the weight should be expressed on an oven-dry basis.

Later in the meeting it was agreed that each method (pH,

conductivity, etc.) should be self-contained. This was

realized when it became necessary to add a plethora of notes

concerning differences in precision of measuring weight of

pulp and volume of water for the extraction procedure for

subsequent test methods.

Determination of pH of standard extracts

Document (Secretariat-16 ) 29, Paper, Board, and Pulps

Determination of pH of Standard Extracts, w^s accepted in

principle. Hot and cold extraction, based on 2 grams + 0.1 g

per 100 ml should be included in the method, but not extraction

with sodium chloride solution. An ad hoc group decided that

the method should be limited to a conductivity value of

2 X 10"'^ -^/m, below which the pH value of an extract would

not be valid. The Secretariat will revise the method and

submit it to the working group for comment.

Determination of conductivity of standard extracts

It was agreed that conductivity should be determined

only on a hot extract of 2 grams + 0.002 g/100 ml.

Alum is used during the washing of some pulps to help

eliminate pitch, and hot and cold extraction would give

different results.

Although it was not mentioned at the meeting, extraction

of anions and cations from pulp with water is almost never

complete. Therefore, a standard procedure is necessary in

order to achieve comparable results.

With respect to temperature of measurement, the method

reads, "...measure at 25° ± 0.2°C." A decision concerning a choice between measuring at 25°C and measuring at a temperature

near 25°C and converting to 25°C via tables was left to the

Secretariat

.
18

Determination of surface pH of paper

It was agreed that a method was needed for paper but

not for pulp. There was considerable resisl;ance to the

surface pH determination because of its unreliability and

lack of precision. It was pointed out, however, that this

is a matter of degree rather than kind, as most methods for

pulp and paper are empirical and subject to considerable

variability. Only recently has it become standard practice

to write precision statements into methods.

It was concluded that the personnel of three countries

(Germany, Finland, and Sv/eden) should get tpgether and

finalize a method to be forwarded to SC 2 not later than

February 1974.

Determination of water soluble sulphate and chloride

It was agreed that the Finnish method, (Finland-2) 23,

is a suitable one and that determinations o^ sulphate and

chloride should be written as separate methods and finalized.

A 5-gram sample should be used for greater precision.

The determination of chloride should not be confined to

electrical papers.

It was concluded that there is a real peed for measuring

chloride and sulphate in paper.

A table showing the range and accuracy of the proposed

methods will be distributed. Sweden will study methods for

the determination of sulphate.

Program of future work

The consideration of acidity and basicity was assigned

to WG 6 at the Oslo meeting in 1969. In view of the lack of

interest, the working group agreed to recommend to SC 5 that

acidity and basicity not be considered further. In view of

possible interest by other ISO committees, WG 6 recommends to

SC 5 that active contacts with other ISO committees interested

in this work should be maintained.
19

7. REPORT ON MEETING OF WORKING GROUP 8,

PREPARATION OF LABORATORY SHEETS FOR

PHYSICAL TESTING

7.1 Agenda of Meeting

The second meeting of ISO/TC 6/SC 5/WG 8 was held at

the Instituto Nacional de Investigaciones Agrarias, Avenida

de Puerta Hierra, s/n, Madrid, Spain on Tuesday, November 6,

1973, at 9 a.m.

Sweden is the convenor of the group, and Dr. Bethge

chaired the meeting.

1. Opening of the meeting

2. Election of chairman

3. Approval of draft agenda

4. Preparation of laboratory sheets

A report of the present status of work will be

presented at the meeting . document: ISO/TC 6/SC 5 (Secretariat-189 ) N 406

5. Testing the physical properties of laboratory sheets

(document will be distributed by post before the meeting)

6 . Future work

7. Other questions

8. Closing of meeting
20

7.2 Secretariat Memorandum of September 1973

The Secretariat of ISO/TC 6/SC 5/WG 8, Sweden, has,

following the decisions made at the Berlin meetings of the

working group and SC 5, prepared a working draft for the

method of testing the physical properties of laboratory

sheets of pulp.

The object of this method is to form a link between the

present sheet forming method, document 6/5 N 406, and the

various methods used for testing laboratory sheets.

The method does not include the various physical test

methods. In most cases, the paper testing methods can be

applied and reference is made to these methods (with exception for the light-scattering coefficient) . Only when determining tensile strength, the test piece length is reduced

from 180 mm to 100 mm.

The sheet forming method, accepted in principle by SC 5,

al].ows test sheets of different sizes and shapes, which means

that no precise instructions for cutting of test pieces can

be given. The number of test pieces to be tested is less than

recommended in paper testing. Otherwise, it would be impossible

to make a complete testing with the amount of pulp obtained

from one beating point. It should be observed that the figures

given indicate the minimum number of tests.

The instructions for reporting are less comprehensive

than In the corresponding paper testing methods. One reason

for this is, of course, that the sheets have no machine and

cross directions. Another reason is that a full report, giving

all possible details, including measures of dispersion, for a

complete pulp evaluation, would become a very complicated

document

.

For the strength properties tensile, tear, and burst,

only the breaking length and the tear and burst indexes need

to be reported.

For tear and burst the indexes should be given, not the

factors. This is in accordance with decision taken at the

Philadelphia meeting of TC 6/SC 2 in September 1972 (see

document TC 6/SC 2/N 598, Resolutions 2 and 3). This is in

line with the SI rules.
21

7.3 Discussion at Working Group Meeting

Sweden has been the convenor of this group since the

London meeting in 1970. At the Berlin meeting in 1972, a method was presented to the working group which embodied the

most important principles of uniform handsheet preparation,

while still allowing different types of equipment. The only

major type of equipment which fell outside the scope of this

general method is the Rapid-Kothen method favored by Germany.

It was agreed at Berlin that Germany would prepare a draft

of the Rapid-Kothen method for future consideration. A revised

draft of the general sheetmaking method, reviewed at Berlin,

was circulated prior to the Madrid meeting.

At the Madrid meeting the major portion of the effort

was concerned with a review of 6/5/8 N 14 , a draft proposal

for testing the physical properties of laboratory sheets.

The object of this method is to form a link between the sheet

forming method and the various methods used for testing laboratory sheets. Since the general sheetmaking method allows

sheets of different sizes and shapes to be prepared, no

detailed procedure for sample cutting is included. In general,

the method refers the user to the appropriate paper testing

method. One important difference is that fewer test replications are made, since not as much sample is available as when

testing paper. The method does not include brightness testing.

The major focus of the discussion concerned the basis of

gra'nmage; whether it should be on an air-dry or an oven-dry

basis. All of the delegations present, except Canada and the

United Kingdom, preferred the air-dry basis. Those in favor

of the air-dry basis felt that all pulps hold a characteristic

level of moisture which in part affects physical properties

and that expression on an oven-dry basis does not correct for

the moisture content. Those in favor of an oven-dry basis

felt that this method expresses the results on a uniform basis.

It was not possible at the session to reach a consensus, so

it was decided to present the problem to the SC 5 plenary

meeting

.

In other discussion, it was decided to include references

to the Rapid-Kothen method in the Scope, to delete the reference

to the measurement of light scattering coefficient, and to

modify the breaking length procedure to specify a time-tobreak rather than a rate of elongation.
22

It was agreed that the method would be revised by the

convenor and redistributed to members who would then have

six months to submit comments. The comments would be incorporated into the method and then the method submitted to SC 5.

Although not on the agenda, there was time remaining and

a desire by the group to discuss the document regarding sheet

preparation, 6/5 N 406. In this discussion, it was decided

to mention the Rapid-Kothen method in the Scope, to mention

the fact that this method does not cover the preparation of

handsheets for brightness determination, and that both pressings

shall be at 400 kPa. Further discussion of this document was

cut off for lack of time.

Finally, it was decided that members would have six months

to review and submit comments regarding 6/5 N 4 32, the RapidKothen method submitted by Germany just prior to the meeting.

It was agreed that if the comments are minor, the revised

draft would go directly to SC 5

.
23

8. REPORT ON MEETING OF WORKING GROUP 1 OF SC 2

,

OPTICAL PROPERTIES OF PAPER, BOARD, AND PULP

8.1 Agenda of Meeting

The meeting was held on 2 November 1973 at the Institute

Nacional de Investigaciones Agraria, Avenida de Puerta

Hierro, s/n , Madrid, Spain.

1. Opening of meeting

2. Approval of draft agenda

3. Discussion on the following documents

ISO/TC 6/SC 5 (Sweden-12) 417

ISO/TC 6/SC 5 (Seer. -203) 423

(These two documents are mentioned in the agenda of

the meeting of TC 6/SC 5, see item 13)

ISO/TC 6/SC 2/WG 1 (Sweden-13) 96

ISO/TC 6/SC 2/WG 1 (Seer. -43) 97

(These two documents are distributed with this

draft agenda)

4. State of "Calibration of Ref lectometers

5. Discussion of comments on 6/-/1 N 23, International

Calibration of Testing Apparatus

6. Gloss measurements

7. Other questions
24

8.2 Secretariat memorandum of Septtjmber 1973

Blue reflectance factor of pulp

Document 6/5 N 408, Determination of D:i.ffuse Blue

Reflectance Factor (ISO Brightness) of Pulp, a draft proposal

revised in accordance with the results of an interlaboratory

test, was submitted in June 1973 to the Subcommittee for

comment. In consequence of the results of --he test, the

Secretariat suggested that, for the drying of the test sheets,

the 4 hr. air-drying procedure should be adopted. Comments

on the document were requested by 1973-07-10. No comments

of significant technical importance were made, and after

certain minor adjustments, the method is now being sent to

the Secretariat of ISO/TC 6 for processing.

Sweden suggested that additional interlaboratory experiments be made to investigate the reasons foip the surprisingly

large differences in brightness values obtained from the same

sample in different laboratories. Seven laboratories in

Canada, Finland, France, Norway, South Africa, Sweden, and

the U.S. have agreed to participate in these experiments

which will be performed under the condition that no further

delay will be caused in handling of the draft proposal. Results

of this experiment are expected by October 1973.

Light scattering coefficient

A working draft has been submitted by Sweden and the

method is being considered by the working group.
25

8.3 Discussion at Working Group Meeting

This working group is part of SC 2, but also reports to

FC 5. Canada became the convenor of this group when the

chair was relinquished by the United Kingdom in 1972, and

Wolfgang Budde is the chairman.

The principal interest of SC 5 in this working group

is the determination of pulp brightness. A method for the

determination of diffuse blue reflectance factor of pulp was

submitted some years ago, but has not yet been adopted. At

the London SC 5 meeting, it was concluded that EDTA solution

should be added to all pulp suspensions and that the pH of

the suspensions should be adjusted to 4.0-5.5. At the Berlin

SC 5 meeting, Finland proposed an LiCl drying procedure, and

it was agreed to carry out laboratory tests to compare the

LiCl procedure with air drying for the preparation of brightness handsheets.

Since then two round-robin laboratory tests have been

carried out, and the United States participated in both.

The conclusion was that the LiCl method presented no advantage,

so it was decided to permit only the air drying technique for

the preparation of brightness handsheets. These tests also

showed that the Elrepho brightness tester gave reproducible

results, and that the reproducibility and repeatability of

the handsheet preparation procedure was reasonably good.

At the working group meeting the results of this work

were reviewed and considerable time was spent reviewing

document 6/5 N 408, Pulps-Determination of Diffuse Blue

Reflectance Factor. A number of minor changes were made,

mainly editorial. The most important change was to prohibit

the use of a kitchen mixer for disintegrating the pulp. Instead, the ISO recommendation for wet disintegration using

the British disintegrator will be used, although this will

give lower brightness results. The consensus was that this

technique is more reproducible. Another change in the method

was to clarify the sheet drying procedure; it will be recommended that the sheet be freely suspended in a current of air.

Considerable discussion followed regarding the need to

set up reliable "standardizing" laboratories capable of

measuring absolute reflectances. Canada and Sweden already

have this capability, and participation of the National

Bureau of Standards is desired. The standardizing laboratories
26

would then supply "authorized" laboratories with calibrated

standards of Level 2, so that the authorized laboratories

could issue standards of Level 3 to industrial concerns and

others who make brightness measurements. There seemed to

be considerable confusion as to how this mechanism would be

set up.

The group briefly discussed the measurement of gloss,

indicated its dissatisfaction with the TAPPI methods, and

requested suggestions for an improved technique. Also, the

interest of the working group in developing methods for

opacity determination and color measurement was indicated.

A document before the group regarding light scattering determination was briefly reviewed. It was agreed that the development of this method would be useful, but that it would take

time and it was concluded that this measurement should not

become part of the current SC 5/WG 8 proposal for testing

pulp handsheet properties.

The importance of setting definite dates for switching

to the absolute reflectance basis and for the change to the

pulp brightness handsheet technique was emphasized. It was

recommended that TC 6 be made aware of the need for effective

advance publicity in this regard, so that the buyers and

sellers of pulp can make the necessary adjustments.

It would seem very appropriate that a standardizing

laboratory be established in the United States equipped to

measure absolute reflectances, and the National Bureau of

Standards appears to be the proper place. The absolute

basis is certain to become the standard for reflectance

measurements, not only for paper but also for other materials

where color and brightness are important. It is very likely

that by the end of 1974, the absolute basis will be internationally adopted for reflectance measurements of paper.

This constitutes an important commercial change because it

will effectively lower brightness numbers. Therefore, the

full participation of the United States, which is the country

most involved in the buying and selling of papermaking pulp,

is important.
27

9. REPORT ON TECHNICAL SESSIONS OF SC 5

9 . 1 Opeming of the Meetirnj

The Ninth meeting ol: ISO/TC 6/SC 5, Testing Methods and

Quality Specifications for Pulp, was held November 6-8, 1973,

at Institute Nacional de Investigaciones Agrarias, Madrid,

Spain. Dr. Antonio Fernandez, speaking for the Institute

Nacional de Investigaciones Agrarias, welcomed the delegates

and gave a brief description of the pulp and paper industry

in Spain.

Prof. Waldemar Jensen of Finland, continuing chairman

of SC 5, assumed the chair and thanked the Spanish hosts for

their generous hospitality.

Working hours were set forth as follow^:

Tuesday, 13:30-17:30

Wednesday, 9:00-12:00 and 14:00-17:30

Thursday, 9:00-12:30 and 14:00-17:30

A tour of the Spanish Paper Institute was scheduled for

Wednesaay afternoon.

The secretary read the list of participating members

of SC 5 (section 2 of this report)

.

The secretary read the list of countries represented

at the meeting and the names of the delegates (section 14.2).

The draft agenda, 6/5 (Secretariat-198) 418, was approved

with the addition of several documents, and a revised agenda

is given in 14.1.

At previous meetings, brief minutes have been distributed,

but this practice was discontinued at the Madrid meeting.

Instead, draft resolutions were carefully prepared and read

at the end of each agenda item.

Mr. Hutley of the United Kingdom and Mr. Habert of

France were appointed to the editing committee.
28

9.2 Saleable Mass, in Lots, of Pulp

Action Prior to Meeting

This is summarized i.n section 5, Report on Meeting of

Working Group 5, Saleable Mass of Pulp.

Action at Meeting

Mr. Lassenius, chairman of the working group, presented

a report of the Monday meeting with the recommendations of

the working group. After some discussion, SC 5 approved

these recommendations. They can be summarised as follows:

1. The method for flash-dried pulp is to be submitted

to TC 6 after the revisions recommended by phe working group

are made

.

2. R 801, the present ISO method for saleable mass, is

to be revised by changing the drying temper&ture to lOS^'C

and is then to be submitted to TC 6 for balloting as an ISO

Standard

.

3. The working group is to study the Canadian proposal

to determine the advisability of a further revision of R 801.

4 . "i^he working group is to continue the work of developing

a statistical method to be issued as an amendment to R 801

and is to also continue its work to develop a method for

sampling unitized lots.
29

9.3 Disintegration for Tests on Unbeaten Pulps

Action Prior to Meeting

At the 1968 meeting in Helsinki, it was agreed that

each laboratory beating method should include its own method

for disintegration, but that in addition a separate method

should be prepared to describe disintegration of pulp for

other testing purposes. Since then it has been agreed that

this will be done using the British disintegrator, and there

never has been any serious consideration of any other equipment.

For some years Norway has been concerned with the conditions of disintegration for flash-dried mechanical pulp.

During the past year some laboratory work was carried out,

with the participation of the United States. The conclusion

of this work, presented in 6/5 N 412, was that a soaking time

of 10 minutes for flash-dried pulps, regardless of their pH

value, would be adequate. On that basis, document 6/5 N 359,

which first was reviewed by SC 5"^ in Berlin, was again put on

the agenda for the Madrid meeting. Several changes in 6/5 N

359, noted in the minutes of the Berlin meeting, have not yet

been implemented.

Action at Meeting

At Madrid the discussion centered on 6/5 N 359, draft

proposal on disintegration for tests on unbeaten pulps. It

was agreed that the title would be changed to "Laboratory

Wet Disintegration for Pulp," and that examples for the use

of this method would be added under Scope. Several other

editorial changes were noted, none of any real substance.

No further changes were made in the technique, equipment, or

conditions of disintegration.

This method is handled directly by the SC 5 Secretariat,

and no working group is involved. It was agreed that the

Secretariat would prepare a revised draft and submit it to

the members. If approved, it would be submitted directly to

TC 6 without waiting for the next SC 5 meeting.
30

9 . 4 Laboratory Beating of Pulp

Action Prior to Meeting

In Helsinki in 1968, four ad hoc working groups were

formed to prepare methods for the laboratory beating of

pulp. These four groups were to deal with the Lampen mill,

the Jockro mill, the Valley beater, and the PFI mill, respectively. At the Berlin meeting, it was decided to drop

futher consideration of the Lampen mill. The methods for

the PFI and Jockro mills have been completed for some time,

and only additional work on the Valley beater was required

after the Berlin meeting. At Berlin, the Secretariat was

asked to prepare a revised draft on the Valley beater method

and to submit it to SC 5 members by mail.

Action at Meeting

There was very little substantial discussion. Sweden

had presented some comments regarding the Valley beater in

6/5 N 434, and these were reviewed and generally adopted, but

they were mainly editorial in nature.

At the Berlin meeting it had been decided to add a note

to all the beater methods indicating some superiority to the

PFI mj.ll. The value of this note was discussed, and Canada

indicated that it felt it constituted an advertisement for

the device. After some deliberation, it was agreed to retain

the note

.

There was little or no comment regarding the other mills.

The Secretariat was instructed to prepare revised drafts and

forward them to TC 6

.
31

9.5 Preparation of Laboratory Sheets

Action Prior to Meeting

This work has been under the jurisdiction of Working

Group 8, Preparation of Laboratory Handsheets for Physical

Testing, with Sweden as the convenor. The goal of the group

is to develop a single sheet forming method which can be

adapted to most sheet-forming equipment. The problem has

been that a general sheetmaking procedure developed by the

group will not work with the Rapid-Kothen method, and Germany

has insisted that the Rapid-Kothen method be included. At

Berlin, it was agreed that a separate method would be prepared

for the Rapid-Kothen technique, but that it would be used

only when the pulp is beaten with a Jokro mill. Further,

at Berlin, it was agreed that if two sheet forming methods

are approved with the above stipulation, then both methods

would be equally considered anew if the Jokro method is

dropped as an ISO recommended method some time in the future.

The general sheetmaking procedure under consideration

in document 6/5 N 406, circulated prior to the Madrid meeting,

stipulates that there shall be no sheet shrinkage during

drying, and that the sheets will dry to equilibrium with the

conditions at which they will be tested. The method encompasses

the British sheetmaking technique commonly used in the United

States. TVie document was briefly discussed at the working

group meeting reported in section 7 of this report. However,

there was not sufficient time at the WG m.eeting for a complete

review and discussion.

Immediately prior to the SC 5 meeting, Germany circulated

6/5 N 432, a draft proposal for the Rapid-Kothen method. This

was the method they had promised at the Berlin session to

prepare. There was no discussion of this method at the WG

level, except it was indicated that members should submit

their comments within six months. If the comments are minor,

the document will be forwarded directly to SC 5.

Action at Meeting

At the meeting an attempt was made to review document

6/5 N 406, a draft proposal for the preparation of laboratory

sheets. However, because of lack of time and the great

interest in this subject, an ad hoc committee was set up to

handle this task. This group consisted of representatives of
32

Finland, Sweden, Germany, United Kingdom, United States, and

Portugal, and it met soor^ after formation for about six hours.

It agreed, in addition to the points mentioned in section 7

of this report, to modify the scope to indicate that brightness measurements cannot be made on these sheets; to indicate

in Field of Application that the method is not suitable for

long-fibered pulps; to add the British mesh description in

section 4.1 (c) ; to mention under Equipment the need for a

means to release vacuum under the septum; to amplify the

blotter specification; to indicate that the drying plates

should be flat; and to largely rewrite the section on drying

and conditioning to clarify the essential points. In addition,

several other smaller editorial changes were made.

The ad hoc group reported back to SC 5, and its report

was accepted without further comment. A new draft of 6/5 N

406 will be prepared by SC 5 and submitted directly to TC 6.
33

9.6 Testing of Physical Properties of Pulp

Action Prior to ^feeting

This work comes under the responsibility of WG 8,

Preparation of Laboratory Handsheets for Physical Testing.

This working group held a meeting just prior to the SC 5

plenary session, and the actions taken at that meeting are

described in section 7 of this report. In brief, at the

working group session, considerable time was spent reviewing

document 6/5/8 N 14, a draft proposal for testing the

physical properties of pulp.

Action at Meeting

The report of the working group was accepted without

significant comment. The WG indicated that it had not been

able to resolve the grammage calculation, as reported in

section 7, and asked the Secretariat for guidance. Canada

and the United Kingdom, the only two countries wanting an

oven-dry basis, indicated that they would not insist to the

extent of slowing the adoption of the method, and in this

way a consensus was. reached. The method again is in the

hands of the working group. The convenor of the WG will

prepare a revised draft and submit it to the WG members.

If no important comments are received within six months,

the method will then be submitted to SC 5.
34

9.7 Viscosity of Pulp

Action prior to meeting

The Secretariat of ISO/TC 6/SC 5/WG 4, Viscosity of

Pulp, had prepared for comment of the members of the working

group a revised working draft for the determination of viscosity

by the CUEN method. The members also were :requested to consider whether two alternative methods of determination of

viscosity should be recommended, viz., the CUEN and the EWNN

methods.

These two methods, together with a report on the work

of ISO/TC 6/SC 5/WG 4, were discussed at the Paris meeting

of ISO/TC 38/SC 16, Textiles/Chemical Testing, in February 1973.

They agreed that further experiments would ^e necessary before

any choice was possible.

lEC/TC 15, Insulating Materials, is considering a method

for the determination of intrinsic viscosity of papers for

electrical purposes. This method, a CUEN method, is very

similar to that considered by ISO/TC 6/SC 5/WG 4.

Action at Meeting

?s very little has been done since the last meeting,

the U.S. suggested that action was urgently needed. The

group agreed, and the urgency resolution (No. 10) proposed

by the U.K. was adopted.
35

9 . 8 Aqueous Extracts of Paper and Pulp

Action Prior to Meeting

This is summarized in section 6, Report on Meeting of

Working Group 6, Aqueous Extracts.

Action at Meeting

Mr. Lassenius reported on the meeting of the working

group, and this report was accepted.

Sweden suggested that the working group should act as

soon as possible, along the lines mentioned in the report,

and Resolution No. 11 covering this suggestion was approved.
36

9.9 Dirt and Shives in Pulp

Action Prior to Meeting

Experiments have been made in Finland in order to

determine whether changes occur in the dirt and shives content

of pulp during the sheet making procedure. Under the conditions prescribed in the proposed method, changes were not

observed. In addition to the standard sheet making procedure

described in 6/5 N 406, fully satisfactory test sheets can be

made using a very simple sheet making device.

A revised working draft is now being considered by WG 7.

The revised draft takes into account the various amendments

agreed upon at the Berlin meeting. Comments were requested

by 1973-11-04.

Action at Meeting

Finland reported that a proposal was not yet forthcoming

from the working group, and suggested that action not be taken

at this time. The problem vas left to the working group.
37

9.10 Determination of Total Sulphur Content

Action Prior to Meeting

At the last meeting of SC 5, the determination of total

sulphur content of pulps was discussed. The subject had been

raised by Sweden who had, for information, submitted a method,

6/5 N 332, based on the Schoninger burning technique. Sulphate

ions are determined indirectly by precipitation with barium

chloride and conductometric titration of excess reagent with

lithium sulphate solution.

The Subcommittee agreed in principle that a method for

the determination of total sulphur content was necessary.

Attention was, however, drawn to the risk of explosion when

using the method presented by Sweden.

The Secretariat was instructed to contact other committees

dealing with total sulphur determination, such as TC 47,

Chemistry. Contact has been made, but no information has

been received.

Sweden had submitted a report, 6/5 N 416, on the comparison of various methods for determination of sulphate ion,

and this is reproduced in section 14. Appendix.

Action at Meeting

It was agreed that the draft proposed by Sweden, 6/5 N

332, was the best, but instructions must be given for avoiding

explosions.

Sweden was invited to submit a revised proposal

(Resolution No. 22)

.
I 38

9.11 Optical Properties of Pulp

Action Prior to Meeting

Working group 1 of SC 2, dealing with optical properties

of pulp, paper, and board, also reports to SC 5. This working

group met in Madrid prior to the SC 5 meeting, and a report

of its deliberations are found in section 8

,

The main interest of SC 5 in optical properties concerns

the measurement of the brightness of pulp. At Berlin a

technique for brightness pad preparation wag considered which

allowed either air drying or an LiCl drying technique. Since

there was considerable discussion about these alternatives, it

was agreed that a series of comparative laboratory tests would

be run. Two series of such tests were made^ both with the

participation of the United States. The conclusion was that

the LiCl technique holds no advantage, so only the air drying

method will be allowed. '

The delegations of SC 5 have supported the move initiated

by SC 2 to put reflectance measurements, such as brightness,

on an absolute basis. Attention has been d^awn repeatedly

at SC 5 meetings to the need to publicize the date of change

to the absolute basis. The change will alter the magnitude

of brightness numbers and a considerable quantity of pulp is

priced according to brightness. Therefore, the change should

take place all over the world at the same time, and the change

should be understood by buyers and sellers. There has been

considerable confusion about how this change should be organized

and when the date of change will be.

Action at Meeting

Mr. Budde , chairman of the working group, reported the

results of the WG meeting to the SC 5 session » He noted that

a revised draft of 6/5 N 408, concerning the determination of

diffuse blue reflectance factor of pulp, would be prepared by

the working group with the object of recommending to SC 5 that

it be submitted to TC 6 without delay.

The importance of adequate publicity regarding the change

to absolute reflectance values was treated at some length.

The working group target date of July 1, 1974, was accepted

by the SC 5 session as being suitable, and the Secretariat was

asked to try to work out a procedure with TC 6 to properly

implement the change, with all urgency.
39

9.12 Revision of ISO Recommendations

Action Prior to Meeting

It is now the established policy of ISO to revise all

ISO recommendations every five years and to advance ISO

recommendations to ISO standards whenever possible. Four

methods were due for five year revision at this meeting.

The method for saleable mass of pulp has already been reported.

The other three are discussed below.

Action at Meeting

R 302, Kappa Number . This was the first recommendation

approved by SC 5 and in reviewing it for reaffirmation, it

had been suggested that the scope of this method be changed

to include semichemical pulps up to 70 percent yield. There

was some discussion as to whether yield should be used as a limiting factor, as the user of the pulp does not know the

yield. There were several other comments concerning the

wording of the present method. It was decided to have the

method edited by a working group and then submitted to TC 6.

The working group is also instructed to consider the advisability of preparing a method for a micro Kappa determination.

John Tasn;an of Canada is the convenor, other representatives

are to be appointed by Finland, France, Sweden, and the U.S.

R 6 38, Dry Matter in Pulp . Two changes were agreed

upon, a sample size as small as 2 g will be permitted and

the drying temperature was increased to 105°C. The Secretariat

is to prepare a revised method and submit it to TC 6.

R 777, R 778, R 779, and R 1830, Trace Metals in Pulp . It was agreed that the methods should be revised to permit

the use of atomic absorption techniques where applicable and

should then be submitted to TC 6 for ballot.
40

9.13 Canadian Standard Freeness

Action Prior to Meeting

Canada had submitted a proposal for standardizing screen

plates for the Canadian Standard Freeness tester. This recommended that the Pulp and Paper Research Institute of Canada

maintain a group of identical screen plates which shall be

recognized as the International Standard. These would be

designated as #1 standards. Level #2 screen plates would be

supplied by PPRIC to any agency which has been nominated as

an agency for calibration of screen plates. These Level #2

screen plates would be calibrated against the Level #1 screen

plates. The standardizing agency would use the Level #2

screen plates to standardize new screen plates for sale to

users. These screen plates would be designated as level #3.

Every tenth screen plate calibrated by a secondary calibrating

agency would be sent to PPRIC for checking. In addition,

any agency nominated to be a calibrating agency would be

required to send. their master instrument to PPRIC for checking

before the agency is approved.

Action at Meeting

Several countries stated that it would be impossible to

send every tenth plate to PPRIC because the plates would not

belong to them. They also objected to the requirement that

the calibrating instruments be sent to Canada. Some editorial

changes were suggested.

After some discussion of these points, an ad hoc committee

was appointed to prepare a revised proposal. The revised

proposal retained the basic system, but made optional the

submitting of every tenth plate to PPRIC for checking. A

statement that all calibrating instruments must meet all

specifications given in the ISO recommendation was substituted

for the requirement that the calibrating instrument be sent

to PPRIC for checking. This proposal v/as approved by SC 5.
41

9.14 Schopper Riegler Freeness

Action Prior to Meeting

A method for measurement of freeness using the Schopper

Riegler instrument had been submitted to letter ballot of

SC 5. Some comments concerning the calibration procedure

had been received.

Action at Meeting

It was agreed that the method should be submitted to

TC 6, but that a working group should be established to

study the calibration procedure. The United Kingdom will

serve as convenor of this working group. Other members

will be appointed by Finland, France, Germany, and Norway.

The U.S. is not participating because of the relatively

small usage of the instrument in this country. A representative can be appointed by the U.S. if this seems desirable.
42

9.15 Accelerated Aging of Pulp

Action Prior to Meeting

At a meeting of the U.S. Committee for ISO/TC 6 on

October 23, 1973, it was agreed that a suggestion be made

to the Secretariat of SC 5, that the accelerated aging of

pulp be placed on the agemda of the meeting of ISO/TC 6/

SC 5 in Madrid, November 2-8.

The accelerated aging of paper is being considered by

ISO/TC 6/SC 2,' and drafts of methods have been submitted.

As the stability of paper depends partly on the nature of

the pulp and as brightness reversion of pulp during transit

and storage is a problem for both supplier and buyer, this

subject might logically be considered by SC 5

.

The U.S. delegation has conferred informally with the

Swedish delegation and with Mr. Jack Histed, a Canadian who

is a member of the TAPPI Bleaching Committee. Mr. Histed is

prepared to write a method for brightness reversion of pulp

based on the Finnish steaming device.

Action at Meeting

Background material and a report prepared by Mr. Histed

was distributed at the meeting. The Secretariat was instructed

to send this material, 6/5 N 446, to the membership of SC 5,

and Mr. Wilson was designated to serve as a focal point for

expressions of interest (Resolution No. 21).
43

10. DRAFT RESOLUTIONS

No. 1

The delegations present instruct the Secretariat to

prepare an amended text of document 6/5 N 435, Saleable Mass

of Flash-Dried Pulps, taking into account the information in

regard to the Scandinavian texts to be provided by Norway

and the editorial comments to be made by the U.S. They also

authorize the Secretariat to submit the revised text to the

Secretariat of TC 6 for further action.

No. 2

The delegations present agree to proceed with the work

on revision of ISO Recommendation R 801, Saleable Mass, with

the object of publishing it as an International Standard.

They also instruct Working Group 1 to continue to actively

study the current Canadian proposals, 6/5/ N 60 and 61, and

any others which are relevant, with the object of replacing

ISO R 801 with one which is an improvement.

No. 3

The delegations present accept the recommendations of

TSO/TC 6/SC 5/WG 1 in document 6/5 N 4 36 regarding the sampling

of unitized bales and program of future work.

No. 4

The delegations present instruct the Secretariat to

prepare an amended text of document 6/5 N 359, Laboratory

Wet Disintegration of Pulp, taking into account document 6/5

N 411 and the comments made at the meeting. The Secretariat

is authorized to submit the revised document to the Secretariat

of TC 6 for further ISO procedure.

No. 5

The delegates present authorize the Secretariat to

prepare revised texts of documents 6/5 N 414 and 415, Laboratory Beating in the PFI mill and in the Jokro Mill, taking

into account the discussion at the meeting, and to pass the

methods to the Secretariat of ISO/TC 6 for further action.
44

No. 6

The delegations present agree that for the time being it

may be necessary, for technical reasons, to specify a wire

screen different from the current ISO recommendations, in the

International Standard for preparation of laboratory sheets

of pulp. They also advise Working Group 8, if practicable,

to continue their studies with the object of applying the

ISO specification in due course when the future International

Standard preparation of laboratory sheets will be revised.

No. 7

The delegations present advise Working Group 8 to proceed

with their studies concerning document 6/5 N 432, Preparation

of Laboratory Sheets by the Rapid-Kothen method, on the lines

suggested in document 6/5 N 445 (report of the working group

on the meeting, Madrid, November 6, 1973).

No. 8

It has been agreed that the ultimate aim of standardization of the preparation of laboratory sheets should be to

develop one test method which is internationally acceptable;

i"^ possible, one which includes the possibility of using

different sheet making apparatus.

For practical reasons it has not proved possible to

achieve this at present. Therefore, as an interim measure,

in view of the wide spread use of equipment described in

document 406 and document 432, it has been decided to provide

agreed guidance on the use of different equipment in order to

achieve consistency of results with each method.

To avoid creating too many levels of results, the method

described in document 432 (Rapid-Kothen) should preferably be

used in connection with beating according to document 415

(Jokro) only, and the method in document 406 in connection with

the beating methods in documents 413 (Valley) and 414 (PFI)

only.

The decision at the Berlin meeting was confirmed stating

that when consideration at later stage will be given to a single standard method, the two sheet forming procedures

should be given equal consideration.

These comments should be included as introduction in all

the methods for preparation of laboratory sheets and the

methods for laboratory beating.
45

No. 9

The delegations pres'.ent request Working Group 8 to

continue their studies on testing of physical properties of

pulp on the lines presented in the report on the WG 8 meeting,

document 6/5 N 445.

No. 10

The delegates present agree that SC 5 instruct Working

Group 4 to prepare draft proposals of the b^ast method or

methods for determination of intrinsic viscosity after due

consultation and to pass them to the Secretariat of the Subcommittee for forwarding to TC 6 with urgenpy.

No. 11

The delegates present instruct Working Group 6, Aqueous

Extracts of Paper and Pulp, to continue their activities on

the lines presented in document 6/5 N 443.

do. 12

The delegates present agree to authorize the Secretariat

to amend the text of document N 406, Preparation of Laboratory

Sheets, taking into account the recommendations of the

Secretariat of TC 6. At the same time, the Secretariat shall

submit the method to the members of SC 5 for information.

No. 13

The delegates present have received a report from

Working Group SC 2/1 regarding the adoption of the method

for measurement of ISO brightness of pulp, 6/5 N 437, and

their recommendation that July 1, 1974, be a target date for

adoption of the perfect reflecting diffuser as ultimate

reference (ISO Reference Standard of Level 1)

.

The delegates present recommend that urgent action be

taken by the Secretariat of SC 2, SC 5, and TC 6 (and the

new ISO body responsible to ISO Council for General International Calibration), to implement the adoption of the WG's

suggestions. Further, the delegates request urgent circulation by the WG of advance information relating to the change

of ultimate reference and its effects so that national

standards bodies may prepare advance publicity in their

countries

.
46

They stress the importance of urgent action by all

parties involved in view of the requirements of international

commercial interests regarding pulps.

No. 14

The delegations present instruct the Secretariat to

submit the method for determination of drainability by the

Schopper-Riegler method, document 6/5 N 380, to TC 6 for

further action. They also agree to create a working group,

ISO/TC 6/SC 5/WG 11, to consider the revision of the instruction for the calibration of the apparatus in particular.

Finland, France, Germany, Norway, and the United Kingdom

will nominate members of the group, and the convenor will be

appointed by the U.K.

No. 15

The delegates present note with interest that the

information they have received in regard to the work of

ISO/TC 6/SC 5/WG 7, Dirt and Shives in Pulp, and advise the

working group to continue their work on the lines presented.

No. 16

The delegations present realize that additional studies

are required before a proposal for revision of ISO R 302,

Kappa Number of Pulp, can be drafted. They instruct a group

of experts, including members from Canada, Finland, France,

Sweden, and the U.S., to prepare a preliminary draft for

consideration of the subcommittee by post and for the

document to be submitted to TC 6. They shall then consider

possibilities of preparing a report on the determination of

micro-Kappa for the consideration of the Subcommittee.

No. 17

The delegates present authorize the Secretariat to

prepare revised text of document 6/5 N 413, Laboratory

Beating of Pulp in the Valley Beater, taking into account

the discussion at the meeting and the comments presented by

Sweden in document 4 34 as well as comments presented by

Canada and U.K. to pass the method to the Secretariat of

ISO/TC 6 for further action.
47

No. 18

The delegations present instruct the Sejcretariat to

prepare a revised text of ISO Recommendation R 638, Dry

Matter in Pulp, taking into account the decisions made at

the meeting and to pass it to the Secretariat of TC 6 with

the object of publishing it as an International Standard.

No. 19

The delegations present request the Secretariat to

prepare definite draft proposals for the revision of ISO

Recommendations 777-779 and 1830, Trace Metals in Pulp, in

the lines presented in document 6/5 N 425 with the object

of publishing them as International Standards. They also

agree that should ISO/TC 6/SC 2 wish to create cooperation

in this field, SC 5 would be able to assist them in their

work

.

No. 2 0

The delegates present authorized the Secretariat to

prepare a revised text of document 6/5 N 426, Calibration

of Canadian Standard Freeness Screen Plates, taking into

account the decisions of the ad hoc working group and to pass

the revised proposal to ISO/TC 6 with a request that they

should consult the new ISO body responsible to ISO Council

for General International Calibration.

No. 21

The delegations present considered that work on aging

of pulp may be required and noted the existence of ISO/TC 6/

SC 2/WG 16, Accelerated Aging. They instruct the Secretariat

to circulate document 6/5 N 446 to the members of the Subcommittee who will in due time pass their opinions as to the

need of this method to Mr. W. K. Wilson, U.S., who has undertaken to act as a focal point for this task.

No. 22

The delegates present invite Sweden to submit to the

Secretariat their revised proposal for the determination of

total sulphur in pulp; the Secretariat, to circulate the

proposal to members when it is available.
48

No. 23

The delegations present agree to constitute a working

group, ISO/TC 6/SC 5/WG 12, to undertake th<» work concerning

fiber classification of pulp. Canada, Finland, France,

Germany, Norway, and the U.S. will join the working group,

Finland accepting the task of the WG Secretariat.
49

11. PROGRAM FOR FUTURE WOR^

1. Saleable mass of pulp in lots WG-1

Statistical method

Flash dried pulp

Canadian method , Pulp in rolls

2. Disintegration of pulp WG-10

3. Drainage properties

Canadian Standard Freeness

Schopper-Riegler

4. Laboratory beating, including necessary WG-10

disintegration

5. Preparation of laboratory sheets for WG-8

physical testing

6. Testinr of physical properties of pulp WG-8

7. Dirt and shives in pulp WG-7

8. Optical properties of pulp (in cooperation SC 2/WG-l

with FC 2)

9. Intrinsic viscosity of pulp (no longer in

cooperation with TC 38)

10. Aqueous extracts of pulp (in cooperation WG-6

with SC 2)

11. Total sulphur in pulp

12. Fiber classification WG-12

13. Sampling pulp for chemical and physical

testing

14. Revision of ISO Recommendations

R 302, Kappa Number of Pulp

R 624, Extraction from Pulps of Materials

Soluble in Dichloromethane

R 6 38, Determination of Dry Matter Content

R 777-779, Trace Metals in Pulp

15. Accelerated Aging of Pulp
50

12. TIME Al^lD PLACE OF NEXT MEETING

The chairman noted that it was seldom possible to

announce the exact time and the place of th$ next meeting

at the conclusion of a meeting. The next meeting will be

held approximately two years from now. The delegates from

one country indicated privately to the Secretariat that an

invitation should be forthcoming within a few months. The

chairman indicated that he would be pleased to have an

invitation. .

t

) . .. s.
51

13. SPECIAL EVENTS

On the evening of November 6, La Association de

Investigacion Tecnica de la Industria Papelera Espanola

hosted a dinner for the delegates and their spouses at the

Los Porches restaurant in Madrid.

Lunch was served every day to the delegates. A bus

from the delegates' hotels to the meeting rooms and return

was provided daily.
52

14. APPENDIX

14.1 Agenda of Meeting of SC 5

1. Opening of the meeting

2. Approval of the draft agenda

3. Appointment of the editing committee

4. Saleable mass, in lots, of pulp

Doc. ISO/TC 6/SC 5 (Seer. -192) 410

ISO/TC 6/SC 5 (Seer. -193) 411

ISO/TC 6/SC 5 (Seer. -212) 435

5. Laboratory disintegration of pulp

Doc. ISO/TC 6/SC 5 (Seer. -173) 359

ISO/TC 6/SC 5 (Seer. -194) 412

6 . Laboratory beating of pulp

Doe. ISO/TC 6/SC 5 (Seer. -195) 413

ISO/TC 6/SC 5 (Seer. -196) 414

ISO/TC 6/SC 5 (Seer. -197) 415

ISO/TC 6/SC 5 (Sweden-13) 434

7. Preparation of laboratory sheets

Doc. ISO/TC 6/SC 5 (Seer. -189) 406

ISO/TC 6/SC 5 (Seer. -209) 429

ISO/TC 6/SC 5 (Germany-5) 432

ISO/TC 6/SC 5 (Sweden-15) 442

8. Testing of physical properties of pulp

Doc. ISO/TC 6/SC 5 (Seer. -199) 419

(The Subcommittee meeting will be preceded by a

meeting of ISO/TC 6/SC 5/WG 8, and a report on their

deliberations will be presented.)

9. Viscosity of pulp

Doc. ISO/TC 6/SC 5 (Seer. -200) 420
53

10. Aqueous extracts of paper and pulp

Doc ISO/TC 6/SC 5 (Seer. -201) 421

11. Dirt and shives in pulp

Doc. ISO/TC 6/SC 5 (Seer. -202) 422

12. Determination of total sulphur content

Doc. ISO/TC 6/SC 5 (Sweden-10) 332

ISO/TC 6/SC 5 (Seer. -181) 367

ISO/TC 6/SC 5 (Netherlands-15) 374

ISO/TC 6/SC 5 (USSR-5) 376

ISO/TC 6/SC 5 (Sweden-11) 416

ISO/TC 6/SC 5 (Sweden-14) 441

13. Optical properties of pulp

Doc. ISO/TC 6/SC 5 (Sweden-12) 417

ISO/TC 6/SC 5 (Seer. -203) 423

ISO/TC 6/SC 5 (Seer. -208) 428

ISO/TC 6/SC 5 (Seer. -210) 430

ISO/TC 6/SC 5 (Seer. -413) 437

14. Revision of published ISO Recommendations

14.1 Kappa number of pulp, ISO/R 302

Doe. ISO/TC 6/SC 5 (Canada-6) 409

14.2 Dry matter in Pulp

Doc. ISO/TC 6/SC 5 (Seer. -204) 424

14.3 Trace metals in pulp

Doc. ISO/TC 6/SC 5 (Seer. -205) 425

15. Canadian Standard Freeness

Doc. ISO/TC 6/SC 5 (Seer. -185) 379

ISO/TC 6/SC 5 (Canada-7) 426

ISO/TC 6/SC 5 (USSR-6) 431

16. Schopper-Riegler Freeness

Doc. ISO/TC 6/SC 5 (Seer. -186) 380

ISO/TC 6/SC 5 (U.K. -11) 438
54

17. Accelerated aging of pulp

Doc. ISO/TC 6/SC 5 (USA-6) 446

18. Program of future work

19. Other questions

20. Approval of the resolutions and of the statement of

results

21. Date and place of next meeting

22. Closing of the meeting
55

14.2 Delegates to Meeting of !pC 5

Chairman: Prof. W. Jensen

CANADA

Mr. J. E. Tasman (leader)

Dr. W. Budde

Mr. E. A. Sexton

FINLAND

Mr. T. Lassenius (leader)

Mr. J-E. Levlin

Mrs. Liva Vuorilehto

FRANCE

M. Garnache (leader)

M. Lonvert

M. riabert

GERMANY

Dr. 0. Toppel (leader)

Mr. L. Baumqarten

NORWAY

Mr. 0. Ellefsen

POLAND

Mr. Andrzes Winczakiewicz

Mr. Janusz Berndt

Mr. Julio Molleda

Dr. Pedro Barbadillo

Mr. Luis Bustamante

Mr. Jaime Vidal

SWEDEN

Dr. P.O. Beth<je

UNITED KINGDOM

Mr. H. R. Hutley (leader)

Mr. R. Hamer

Mr. G. Youd

UNITED STATES

Mr. W. K. Wilson (leader)

Mr. J. L. Borstelmann

Prof. C. E. Brandon

Dr. J. H. Schulz

OBSERVER: Customs Cooperation

Council: Mr. F. Lobato

Interpreter: Miss M. Girot

Secretariat: Mrs. Heidi Suonuuti

PORTUGAL

Mr. Veloso Gaio (leader)

Mr. A.F.P. de Campos

Mr. Julio Salvadore

Mr. Manuel Saraiva Santos

SPAIN

Kr . Antonio Xucla (leader)

Mr. Jaime Vidal

Mr. Jose L. Asenjo
56

14.3 Delegates to Eighth Meeting of WG 1,

Saleable Mass of Pulp

Chairman: Mr. Lassenius^ Finland

CANADA

Mr, John Tasman

Mr. Ernest A. Sexton

FINLAND

Mrs. Liva Vuorilehto

Mr. Jan-Erik Levlin

FRANCE - -

Mr. Hubert Garnache

Mr. Jean Lonvert

GERflANY

Mr. Heinrich L. Baumgarten

Dr. Otmar Toppel

NORWAY

Mr. 0ystein Ellefsen

POLAND

Mr. Janusz Berndt

Mr. Andre Winczakiewicz

SPAIN •

Mr. Pedro Barbadillo

SWEDEN

Dr. Per Olof Bethge

UNITED KINGDOM

UNITED STATES

Mr. J. L. Bor^telmann

Prof. C. E. Brandon

Mr. W. K. Wilson

Secretariat: Mrs. Heidi Suonuuti

Mr. H. R. Hutley

Mr . G . Youd
57

14.4 Delegates to Second Meeting of WG 6,

Aqueous Extracts

Chairman: Mr. T. Lassenius, Finland

CANADA

Mr. John Tasman

Mr. Ernest A. Sexton

FINLAND

Mrs. Liva Vuorilehto

FRANCE

Mr. Hubert Garnache

Mr. Jean Lonvert

GERMANY

Mr. Heinrich L. Baumgarten

Dr. Otmar Toppel

NORWAY

Mr. 0vsteir Ellefsen

SPAIN

Mr. J. Vidal

SWEDEN

Dr. Per Olof Bethge

UNITED KINGDOM

Mr. Ronald Hamer

Mr. H. R. Hutley

Mr. G. Youd

UNITED STATES

Mr. J. L. Borstelmann

Mr. C. E. Brandon

Mr. W. K. Wilson

Secretariat: Mrs. Heidi Suonuuti
58

14.5 Delegates to Meeting of WG 8,

Preparation of Laboratory Sheets

Chairman: Dr. P. 0. Bethge, Sweden

CANADA UNITED STATES

Mr. E. A. Sexton

Dr. W. Budde

Mr. J. E. Tasman

FINLAND

Mr. T. Lassenius

Mr. J. E. Levlin

Mrs. Liva Vuorilehto

FRANCE

M. Garnache

M. Lonvert

GERMANY

Dr. 0. Toppel -

' Mr. L. Baumgarten

NORWAY

Mr. 0. Ellefsen

PORTUGAL

Fr. Manuel Saraiva Santos

SPAIN

Mr. A. Xucla

Dr. Pedro Barbadillo

Mr. Luis Bustamente

UNITED KINGDOM

Mr. W. K. Wilson

Mr. J. L. Borstelmann

Prof. C. E. Brandon

Dr. J. H. Schulz

Mr. H. R. Hutley

Mr. R. Hamer

Mr. G. Youd
59

14.6 Delegates to Meeting of WG 1 of SC 2

,

Optical Properties of Paper, Board,

and Pulp

Chairman: Dr. W. Budde , Canada

CANADA

Mr. E. A. Sexton

FINLAND

Mr. T. Lassenius

Mr. Jan-Erik Levlin

Mrs. Heidi Suonuuti

FRANCE

Mr. Jacques L. Poujade

Mr. Robert Seve

GER^^NY

Mr. Otmar Toppel

NORWAY

Mr. ^ystein Ellefsen

SPAIN

Dr. Pedro Barbadillo

SWEDEN

Mr. Ake Stenius

UNITED STATES

Dr. J. H. Schulz
60

14.7 List of Working Groups

Saleable Weight, in Lots, of Pulp Baled in Sheet Form,

and of Flash-Dried Pulp

Secretariat: Finland; Convenor: Mr. T. Lassenius

Members: Canada, Finland, France, Germany, Italy,

Netherlands, Norway, Sweden, U.K., and

U.S.

Viscosity of Pulp

Secretariat: Finland

Members: Finland, Canada, France, Czechoslovakia,

Germany, Italy, Netherlands, Romania,

Norway, Sweden, U.K., and U.S.

Aqueous Extracts of Pulp. This group is common to SC 2

and SC 5.

Secretariat: Finland

Members: Finland, Sweden, Germany, France, U.S.,

Italy, Portugal, Australia, Belgium,

Spain, U.K., and Czechoslovakia

Dirt and Shives in Pulp

Secretariat: Finland

Members: Czechoslovakia, Finland, France, Netherlands

Norway, U.K., U.S., Sweden, and Italy

Preparation of Laboratory Handsheets for Physical Testing

Secretariat: Sweden; Convenor: Dr. Bethge

Members: Canada, Czechoslovakia, France, Germany,

Italy, Netherlands, Norway, Portugal,

Sweden, U.K., U.S., and Australia

Laboratory Beating, Including Necessary Disintegration

Secretariat: Finland

Members: Australia, Canada, Finland, France, Germany,

Italy, Norway, Poland, Portugal, Sweden,

U.K. , and U.S.
61

Fiber Classification of Pulp

Secretariat: Finland

Members: Canada, Finland, France, Germany, Norway

and U.S.

Optical Properties of Pulp

There is no independent working group under SC 5, but

joint working group exists with SC 2 which reports to

SC 2. This is WG 1 under SC 2.

Secretariat: Canada; Convenor: Wolfgang Budde

Members: (list not available)
62

14.8 ISO Recominendations From SC 5

R 302-1963 Determination of Kappa Number of Pulp

R 624-1967 Cellulose Pulps. Extraction from Pulps of

Materials Soluble in Dichloromethane

R 638-1967 Cellulose Pulps. Determination of Dry Matter

Content.

R 692-1968 Pulps. Determination of Alkali Solubility

R 699-1968 Pulps. Determination of Alkali Resistance

R 776-1968 Pulps. Determination of Acid Insoluble Ash

R 777-1968 Pulps. Determination of Calcium Content

R 778-1968 Pulps. Determination of Copper Content

R 779-1968 Pulps. Determination of Iron Content

R 801-1968 Pulps. Determination of Saleable Mass, in Lots,

of Pulp Baled in Sheet Form

R 1762-1970 Determination of Ash Content

R 1830-1970 Determination of Manganese Content

R 2144-1971 Determination of Ash Content
63

14.9 6/5 N 416, Comparison of Methods for Sulphate

Ion Determination (from Sweden)

In accordance with the decision taken at the Berlin

meeting of ISO/TC 6/SC 5, we have studied some methods for

the determination of sulphate ions in dilut<2 aqueous solutions. The primary object of the study was to establish

which methods could be recommended for analysis of the

adsorption solution obtained after combustion in oxygen

atmosphere in the determination of total sulphur in pulp.

The results are also of interest for the determination of

sulphate ions in aqueous extracts of pulp, which is studied

by ISO/TC 6/SC 5/WG 6.

Our study is not completed yet, but we think that it might

be of interest to report on the results obtained so far.

Methods Studied and Summary of Results

1. Precipitation titration with BaCl2 using Alizarine Red S

as the indicator. ISO/TC 6/SC 5 N 376.

Approximately 90% of the amount of 0.05 M BaCl2 solution

be added before the indicator is introduced. Titrate to

color change from yellow to reddish.

In our hands, the method worked less satisfactorily. The

color change was difficult to observe. A preliminary

titration is required, which is a serious drawback.

2. Precipitation titration with Ba(C104)2 using thorin as

the indicator. ISO/TC 6/SC 5 N 374, method A.

The titration is performed in 80% isopropanol at pH 2-5.

Color change from yellow to pink.

Precise results were obtained with solutions (5 ml) containing 0.33 mg S and also at higher concentrations. The

color change is somewhat difficult to observe.

3. Alkalimetric titration with sodium hydroxide using methyl

red as the indicator. ISO/TC 6/SC 5 N 374, method B.
64

The sample solution is heated to boiling, 'cooled, and

titrated with 0.01 NaOH.

Precise results were obtained down to a level of 0.1 mg

of sulphur in 5 ml. The method is, however, not specific;

chlorine in the pulp will appear as hydrochloric acid and

will be titrated in the same titration.

Precipitation titration with Ba (€104)2, using carboxyarsenazo

as the indicator. (Method by Archer, White, and Mackinson,

The Analyst 96(1971) 879-880.)

The titration is performed in 67% acetone in the presence

of pyridine. Color change from red to blue.

Precise results were obtained with 0.16 mg of sulphur in

5 ml solution. The endpoint was sharp; further experiments

are planned

.

Conductometric titration with Li2S04 after addition of

excess BaCl2. ISO/TC 6/SC 5 N 332.

Sulphate ions are precipitated from a solution containing

50% ethanol with BaCl2, the excess is titrated with Li2S04

and the titration is followed by measuring the conductivity

of the solution.

The procedure is time-consuming, and the results were less

precise

.

Spectrophotometric determination of H2S after reduction

with hydriodic acid. Method in use at the Swedish Forest

Products Research Lab.

The sample is evaporated to dryness, hydriodic acid

reduction mixture is added and hydrogen sulphide is

distilled off and adsorbed in an alkaline solution. The

H2S is determined colorimetrically as methylene blue.

The method is less precise than methods 2-4, but can be

used down to very low sulphur contents. For 0.008 mg of

sulphur in 5 ml sample solution, the results were in the

range of 0.0098-0.0077.
65

7. Spectrophotometric determination as phenantroline . Method

by Davis and Lindstroni/ Analytical Chemistry ££ (1972) . Method similar to 6, but reduction is made without previous

evaporation. The color reaction depends on reduction of

Fe3+ toFe2+, which forms an orange complex with

o-phenantroline

.

We plan to test this method at a later date.

Conclusion

The amount of pulp which conveniently can be burnt in a 1-liter oxygen flask is about 500 mg. A pulp sample containing

0.1 percent sulphur contains 0.5 mg of sulphur. For such

samples the methods 2, 3, 4 seem to be applicable. Method 3

will probably give high results due to chlorine in the pulp

especially from bleached pulps, and the endpoint is more

difficult to observe in method 2 than in method 4. It, therefore, seems as if method 4 is best suited for pulps containing

0.1 percent of vS or more.

We plan to continue the experimental work on methods 4

and 7

.

The investigations are carried out at Swedish Forest

Products Research Laboratory.

li.b. orpT. c- covM. "n. I'l. hl.iCA i ib.N' OK Riil-'OiLT NO. BIBLIOGRAPHIC DATA mdctd Ti l\c NBSIR 73-4L6

2. C>)V 1 Ac ce.-: iioa 3. Ricipierit's Accession N'o.

4. TlTLli AXn SUBTITl.lv Testing Methods and Quality Specifications

for Pulp

5. Publication Date

6. Performing Or£^ar) i?ati on Code

7. AUTIIOIUS)

WKVJilson, JHSchulz, CEBrandon, & JLBorstelmann

£. Performing Organization

NBSIR 73-416

9. PERI-ORMIXG ORGANIZATION NAME AND ADDRESS

NATIONAL BUREAU OF STANDARDS

DEPARTMENT OF COMMERCE

WASHINGTON, D.C. 20234

10. Project/Task/ Work Unit No.

11. Contract/Grant No.

12. Sponsoring Organization Name and Address 13. Type of Report & Period

Covered

Final

14. Sponsoring Agency Code

15. SUPPLEMENTARY NOTES

This report describes what happened at an ISO meeting, V7ith the exception of section 3 and section 4, opinions of the delegates are not

expressed.

16, ABSTRACT (A 200-word or less factual summary of most significant information. If document includes a significant

bibliography or literature survey, mention it here.)

The ninth meeting of ISO/TC 6, Paper, SC 5, Testing Methods for

Pulp, was held in Madrid, Spain, November 2-8, 1973. Over 30 delegates

from 11 countries discussed methods for testing of pulp and, to some

extent, paper. Methods were agreed upon for the determination of

saleable mass of flash dried pulp, disintegration of pulp, laboratory

beating of pulp, preparation of laboratory sheets, and measurement of

ISO brightness of pulp. It v/as agreed that ISO Recommendations for

determination of saleable mass of pulp in lots, determination of dry

matter content, and determination of trace metals in pulp should be

revised. Plans were made to continue studies of methods for the determination of viscosity, aqueous extraction, dirt and shives, total

sulphur content, saleable mass of unitized lots of pulp, statistical

evaluation of number of sample bales, preparation of laboratory sheets,

and fiber classification and drainability

.

17. KEY WORDS (Alphabetical order, separated by semicolons)

ISO Recommendations; pulp; pulp, testing methods; testing methods for

pulp

.

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