ISO 777:2005
(Main)Paper, board and pulp — Determination of acid-soluble calcium
Paper, board and pulp — Determination of acid-soluble calcium
ISO 777:2005 specifies the procedure for the determination of acid-soluble calcium by atomic absorption spectrometry or by plasma emission spectrometry. It is applicable to all kinds of paper, board and pulp. It specifies a method to determine the acid-soluble part of the incineration residue, i.e. that part of the ignition residue obtained after incineration that is soluble in hydrochloric acid. If the residue is completely soluble, the result obtained by the procedure specified in ISO 777:2005 is taken as the total amount of calcium in the sample.
Papier, carton et pâte — Détermination de la teneur en calcium soluble dans l'acide
L'ISO 777:2005 spécifie une méthode de détermination de la teneur en calcium soluble dans l'acide par spectrométrie d'absorption atomique ou par spectrométrie d'émission de plasma. Elle est applicable à tous les types de papier, de carton et de pâte. Elle spécifie une méthode de détermination de la partie soluble dans l'acide des résidus d'incinération, à savoir la partie des cendres qui est soluble dans l'acide chlorhydrique. Si le résidu est complètement soluble, le résultat obtenu, en utilisant la procédure spécifiée dans l'ISO 777:2005, correspond à la quantité totale de calcium dans l'échantillon.
Papir, karton, lepenka in vlaknine - Določevanje kalcija, topnega v kislini
Ta mednarodni standard opredeljuje postopek za določevanje kalcija, topnega v kislini, z atomsko absorpcijsko spektrometrijo ali s plazemsko emisijsko spektroskopijo. Velja za vse vrste papirja, kartona, lepenke in vlaknin. Opredeljuje metodo za določevanje dela ostanka po žarjenju, ki je topen v kislini, tj. tisti del ostanka po žarjenju, ki je topen v klorovodikovi kislini. Če je ostanek popolnoma topen, rezultat, ki ga pridobimo s postopkom, opredeljenim v tem mednarodnem standardu, predstavlja celotno količino kalcija v vzorcu.
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МЕЖДУНАРОДНЫЙ ISO
СТАНДАРТ 777
Третье издание
2005-05-01
Бумага, картон и целлюлоза.
Определение содержания кальция,
растворимого в кислоте
Paper, board and pulp – Determination of acid-soluble calcium
Ответственность за подготовку русской версии несёт GOST R
(Российская Федерация) в соответствии со статьёй 18.1 Устава ISO
Ссылочный номер
ISO 777:2005(R)
©
ISO 2005
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ISO 777:2005(R)
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ii © ISO 2005 – Все права сохраняются
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ISO 777:2005(R)
Предисловие
Международная организация по стандартизации (ISO) является всемирной федерацией национальных
организаций по стандартизации (комитетов-членов ISO). Разработка международных стандартов
обычно осуществляется техническими комитетами ISO. Каждый комитет-член, заинтересованный в
деятельности, для которой был создан технический комитет, имеет право быть представленным в этом
комитете. Международные правительственные и неправительственные организации, имеющие связи с
ISO, также принимают участие в работах. Что касается стандартизации в области электротехники, то
ISO работает в тесном сотрудничестве с Международной электротехнической комиссией (IEC).
Проекты международных стандартов разрабатываются в соответствии с правилами Директив ISO/IEC,
Часть 2.
Основная задача технических комитетов заключается в подготовке международных стандартов.
Проекты международных стандартов, принятые техническими комитетами, рассылаются комитетам-
членам на голосование. Их опубликование в качестве международных стандартов требует одобрения
не менее 75 % комитетов-членов, принимающих участие в голосовании.
Следует иметь в виду, что некоторые элементы настоящего международного стандарта могут быть
объектом патентных прав. ISO не может нести ответственность за идентификацию какого-либо одного
или всех патентных прав.
Документ ISO 777 подготовлен Техническим комитетом ISO/TC 6, Бумага, картон и целлюлоза.
Настоящее третье издание отменяет и замещает второе издание (ISO 777:2001) после его некоторого
пересмотра. Не считая незначительные редакторские правки, изменен заголовок, чтобы не
противоречить ISO 1830:2005 и различать от стандарта ISO 17812 (планируемого к изданию), который
задает метод определения общей массовой доли кальция, марганца, железа и меди.
Первое издание настоящего международного стандарта включает метод титрования, а также
процедуру на основе атомно-абсорбционной спектроскопии. Во втором издании метод титрования
исключен, так как в настоящее время этот метод используется редко, а область применения стандарта
расширена, чтобы охватить бумагу и картон в дополнение к целлюлозе.
© ISO 2005 – Все права сохраняются iii
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ISO 777:2005(R)
Введение
[1] [2]
Настоящий международный стандарт соответствует ISO 778 и ISO 779 , чтобы сделать возможным
конечное измерение содержания всех трех элементов путем анализа одного и того же раствора.
iv © ISO 2005 – Все права сохраняются
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МЕЖДУНАРОДНЫЙ СТАНДАРТ ISO 777:2005(R)
Бумага, картон и целлюлоза. Определение содержания
кальция, растворимого в кислоте
ПРЕДУПРЕЖДЕНИЕ — Метод, заданный в настоящем международном стандарте связан с
использованием опасных химикатов и газов, которые могут составлять с воздухом
взрывчатые смеси. Необходимо позаботиться об обеспечении соблюдения соответствующих
мер предосторожности.
1 Область применения
Настоящий международный стандарт задает метод для определения содержания кальция,
растворимого в кислоте, на основе атомной абсорбционной или плазменной эмиссионной
спектрометрии.
Он применяется ко всем видам бумаги, картона и целлюлозы.
Этот стандарт задает метод, чтобы определять растворимый в кислоте зольный остаток после
сжигании, т.е. золы, полученной после прокаливания и растворенной в соляной кислоте. Если остаток
является полностью растворимым, то результат, полученный методом, который задан в настоящем
международном стандарте, берется в качестве общего количества кальция в образце для анализа.
2 Нормативные ссылки
Следующие нормативные документы являются обязательными для применения с настоящим
международным стандартом. Для жестких ссылок применяются только указанное по тексту издание.
Для плавающих ссылок необходимо использовать самое последнее издание нормативного ссылочного
документа (включая любые изменения).
ISO 186, Бумага и картон. Отбор образцов для определения среднего качества
ISO 287, Бумага и картон. Определение содержания влаги. Метод высушивания в печи
ISO 638, Целлюлоза. Определение содержания сухого вещества
ISO 1762, Бумага, картон и целлюлоза. Определение остатка (золы) при прокаливании при 525 °C
ISO 7213, Целлюлоза. Отбор образцов для испытаний
3 Термины и определения
В настоящем документе применяются следующие термины и определения.
3.1
массовая доля кальция
mass fraction of calcium
количество элементарного кальция в растворе, полученном после прокаливания образца при 525 °C и
обработки зольного остатка соляной кислотой с концентрацией 6 моль/л, как задано в настоящем
международном стандарте
© ISO 2005 – Все права сохраняются 1
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ISO 777:2005(R)
4 Принцип
Часть образца для анализа прокаливается при 525 °C и полученный зольный остаток обрабатывается
соляной кислотой с концентрацией 6 моль/л. Анализируемая проба вводится в пламя ацетилен/закись
азота или ацетилен/воздух, а массовая доля кальция устанавливается одним из следующих методов:
— измерение поглощения по атомному спектру на длине волны 422,7 нм при излучении на кальций
спектральной лампы с полым катодом; или
— измерение поглощения на длине волны 422,7 нм путем плазменной эмиссионной спектрометрии.
5 Реактивы и материалы
Используйте химические реактивы признанного аналитического качества и только дистиллированную
или деионизированную воду.
5.1 Соляная кислота, концентрация около 6 моль/л
Разбавьте 500 мл соляной кислоты (плотностью 1,19 г/мл) в 500 мл воды.
5.2 Запас раствора кальция, 500 мг/л кальция.
Взвесьте 1,249 ± 0,001 г карбоната кальция, высушенного до постоянной массы при температуре не
выше 200 °C, в мерной колбе вместимостью 1000 мл. Добавьте 50 мл воды. Добавьте минимальный
объем соляной кислоты (5.1), капля за каплей (приблизительно 10 мл), чтобы осуществить полное
растворение карбоната кальция. Разбавьте водой до отметки и перемешайте.
1 мл этого запасного раствора содержит 0,500 мг кальция (Ca).
5.3 Эталонный раствор кальция, 50 мг/k Ca
Перенесите 100 мл раствора (5.2) в мерную колбу на 1 000 мл, разбавьте водой до отметки и
перемешайте.
1 мл этого эталонного раствора содержит 0,05 мг Ca.
Можно использовать сертифицированные эталонные растворы, доступные для приобретения.
5.4 Раствор лантана, 50 г/л лантана (La)
Смочите водой 59 г оксида лантана (La O ). Медленно и осторожно добавьте 250 г соляной кислоты
2 3
(плотностью 1,19 г/мл), чтобы растворить оксид лан
...
INTERNATIONAL ISO
STANDARD 777
Third edition
2005-05-01
Paper, board and pulp — Determination
of acid-soluble calcium
Papier, carton et pâte — Détermination de la teneur en calcium soluble
dans l'acide
Reference number
ISO 777:2005(E)
©
ISO 2005
---------------------- Page: 1 ----------------------
ISO 777:2005(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2005
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2005 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 777:2005(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 777 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps.
This third edition cancels and replaces the second edition (ISO 777:2001), of which it constitutes a minor
revision. Apart from minor editorial modifications, only the title has been changed, to be consistent with
ISO 1830:2005, and to make a distinction with ISO 17812 (to be published) which specifies the method to
determine the total mass fraction of calcium, manganese, iron and copper.
The first edition of this International Standard included the titrimetric procedure as well as the procedure
based on atomic absorption spectroscopy. In the second edition, the titrimetric procedure was deleted, as it is
now seldom used, and the scope was enlarged to include paper and board in addition to pulp.
© ISO 2005 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 777:2005(E)
Introduction
[1] [2]
This International Standard corresponds to ISO 778 and ISO 779 in order to make it possible to perform
the final measurement of all three elements on the same solution.
iv © ISO 2005 – All rights reserved
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INTERNATIONAL STANDARD ISO 777:2005(E)
Paper, board and pulp — Determination of acid-soluble calcium
WARNING — The method specified in this International Standard involves the use of some hazardous
chemicals and of gases that can form explosive mixtures with air. Care must be taken to ensure that
the relevant precautions are observed.
1 Scope
This International Standard specifies the procedure for the determination of acid-soluble calcium by atomic
absorption spectrometry or by plasma emission spectrometry.
It is applicable to all kinds of paper, board and pulp.
It specifies a method to determine the acid-soluble part of the incineration residue, i.e. that part of the ignition
residue obtained after incineration that is soluble in hydrochloric acid. If the residue is completely soluble, the
result obtained by the procedure specified in this International Standard is taken as the total amount of
calcium in the sample.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 186, Paper and board — Sampling to determine average quality
ISO 287, Paper and board — Determination of moisture content — Oven-drying method
ISO 638, Pulps — Determination of dry matter content
ISO 1762, Paper, board and pulps — Determination of residue (ash) on ignition at 525 °C
ISO 7213, Pulps — Sampling for testing
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
mass fraction of calcium
amount of the element calcium in the solution obtained after incineration of the specimen at 525 °C and
treating the residue with 6 mol/l hydrochloric acid, as specified in this International Standard
© ISO 2005 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO 777:2005(E)
4 Principle
A test portion is incinerated at 525 °C and the residue is treated with 6 mol/l hydrochloric acid. The test
solution is aspirated into an acetylene/dinitrogen monoxide or acetylene/air flame and the mass fraction of
calcium is determined by one of the following procedures:
measurement of the absorption of the 422,7 nm line emitted by a calcium hollow-cathode lamp, or
measurement of the absorption of the 422,7 nm line emitted by plasma emission spectrometry.
5 Reagents and materials
Use only chemicals of recognized analytical grade and only distilled or deionized water.
5.1 Hydrochloric acid, about 6 mol/l.
Dilute 500 ml of hydrochloric acid (density 1,19 g/ml) in 500 ml of water.
5.2 Calcium stock solution, 500 mg/l of Ca.
Weigh 1,249 g ± 0,001 g of calcium carbonate, dried to constant mass at a temperature not exceeding 200 °C,
into a 1 000 ml volumetric flask. Add 50 ml of water. Add a minimum volume of hydrochloric acid (5.1)
(approximately 10 ml), drop by drop, to effect the complete dissolution of the calcium carbonate. Dilute with
water to the mark and mix.
1 ml of this stock solution contains 0,500 mg of Ca.
5.3 Calcium standard solution, 50 mg/l of Ca.
Transfer 100 ml of the stock solution (5.2) to a 1 000 ml volumetric flask, dilute with water to the mark and mix.
1 ml of this standard solution contains 0,05 mg of Ca.
Commercially available, certified standard solutions may be used.
5.4 Lanthanum solution, 50 g/l of La.
Moisten 59 g of lanthanum oxide (La O ) with water. Slowly and cautiously, add 250 ml of hydrochloric acid
2 3
(density 1,19 g/ml) to dissolve the lanthanum oxide. Dilute to the m
...
SLOVENSKI STANDARD
SIST ISO 777:2011
01-maj-2011
3DSLUNDUWRQOHSHQNDLQYODNQLQH'RORþHYDQMHNDOFLMDWRSQHJDYNLVOLQL
Paper, board and pulp -- Determination of acid-soluble calcium
Papier, carton et pâte -- Détermination de la teneur en calcium soluble dans l'acide
Ta slovenski standard je istoveten z: ISO 777:2005
ICS:
85.040 Vlaknine Pulps
85.060 Papir, karton in lepenka Paper and board
SIST ISO 777:2011 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST ISO 777:2011
---------------------- Page: 2 ----------------------
SIST ISO 777:2011
INTERNATIONAL ISO
STANDARD 777
Third edition
2005-05-01
Paper, board and pulp — Determination
of acid-soluble calcium
Papier, carton et pâte — Détermination de la teneur en calcium soluble
dans l'acide
Reference number
ISO 777:2005(E)
©
ISO 2005
---------------------- Page: 3 ----------------------
SIST ISO 777:2011
ISO 777:2005(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2005
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2005 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 777:2011
ISO 777:2005(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 777 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps.
This third edition cancels and replaces the second edition (ISO 777:2001), of which it constitutes a minor
revision. Apart from minor editorial modifications, only the title has been changed, to be consistent with
ISO 1830:2005, and to make a distinction with ISO 17812 (to be published) which specifies the method to
determine the total mass fraction of calcium, manganese, iron and copper.
The first edition of this International Standard included the titrimetric procedure as well as the procedure
based on atomic absorption spectroscopy. In the second edition, the titrimetric procedure was deleted, as it is
now seldom used, and the scope was enlarged to include paper and board in addition to pulp.
© ISO 2005 – All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 777:2011
ISO 777:2005(E)
Introduction
[1] [2]
This International Standard corresponds to ISO 778 and ISO 779 in order to make it possible to perform
the final measurement of all three elements on the same solution.
iv © ISO 2005 – All rights reserved
---------------------- Page: 6 ----------------------
SIST ISO 777:2011
INTERNATIONAL STANDARD ISO 777:2005(E)
Paper, board and pulp — Determination of acid-soluble calcium
WARNING — The method specified in this International Standard involves the use of some hazardous
chemicals and of gases that can form explosive mixtures with air. Care must be taken to ensure that
the relevant precautions are observed.
1 Scope
This International Standard specifies the procedure for the determination of acid-soluble calcium by atomic
absorption spectrometry or by plasma emission spectrometry.
It is applicable to all kinds of paper, board and pulp.
It specifies a method to determine the acid-soluble part of the incineration residue, i.e. that part of the ignition
residue obtained after incineration that is soluble in hydrochloric acid. If the residue is completely soluble, the
result obtained by the procedure specified in this International Standard is taken as the total amount of
calcium in the sample.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 186, Paper and board — Sampling to determine average quality
ISO 287, Paper and board — Determination of moisture content — Oven-drying method
ISO 638, Pulps — Determination of dry matter content
ISO 1762, Paper, board and pulps — Determination of residue (ash) on ignition at 525 °C
ISO 7213, Pulps — Sampling for testing
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
mass fraction of calcium
amount of the element calcium in the solution obtained after incineration of the specimen at 525 °C and
treating the residue with 6 mol/l hydrochloric acid, as specified in this International Standard
© ISO 2005 – All rights reserved 1
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SIST ISO 777:2011
ISO 777:2005(E)
4 Principle
A test portion is incinerated at 525 °C and the residue is treated with 6 mol/l hydrochloric acid. The test
solution is aspirated into an acetylene/dinitrogen monoxide or acetylene/air flame and the mass fraction of
calcium is determined by one of the following procedures:
measurement of the absorption of the 422,7 nm line emitted by a calcium hollow-cathode lamp, or
measurement of the absorption of the 422,7 nm line emitted by plasma emission spectrometry.
5 Reagents and materials
Use only chemicals of recognized analytical grade and only distilled or deionized water.
5.1 Hydrochloric acid, about 6 mol/l.
Dilute 500 ml of hydrochloric acid (density 1,19 g/ml) in 500 ml of water.
5.2 Calcium stock solution, 500 mg/l of Ca.
Weigh 1,249 g ± 0,001 g of calcium carbonate, dried to constant mass at a temperature not exceeding 200 °C,
into a 1 000 ml volumetric flask. Add 50 ml of water. Add a minimum volume of hydrochloric acid (5.1)
(approximately 10 ml), drop by drop, to effect the complete dissolution of the calcium carbonate. Dilute with
water to the mark and mix.
1 ml of this stock solution contains 0,500 mg of Ca.
5.3 Calcium standard solution, 50 mg/l of Ca.
Transfer 100 ml of the stoc
...
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Papier, carton et pâte -- Détermination de la teneur en calcium soluble dans l'acidePaper, board and pulp -- Determination of acid-soluble calcium85.060Papir, karton in lepenkaPaper and board85.040VlakninePulpsICS:Ta slovenski standard je istoveten z:ISO 777:2005oSIST ISO 777:2011en01-marec-2011oSIST ISO 777:2011SLOVENSKI
STANDARD
oSIST ISO 777:2011
Reference numberISO 777:2005(E)© ISO 2005
INTERNATIONAL STANDARD ISO777Third edition2005-05-01Paper, board and pulp — Determination of acid-soluble calcium Papier, carton et pâte — Détermination de la teneur en calcium soluble dans l'acide
oSIST ISO 777:2011
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ii © ISO 2005 – All rights reserved
oSIST ISO 777:2011
ISO 777:2005(E) © ISO 2005 – All rights reserved iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 777 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps. This third edition cancels and replaces the second edition (ISO 777:2001), of which it constitutes a minor revision. Apart from minor editorial modifications, only the title has been changed, to be consistent with ISO 1830:2005, and to make a distinction with ISO 17812 (to be published) which specifies the method to determine the total mass fraction of calcium, manganese, iron and copper. The first edition of this International Standard included the titrimetric procedure as well as the procedure based on atomic absorption spectroscopy. In the second edition, the titrimetric procedure was deleted, as it is now seldom used, and the scope was enlarged to include paper and board in addition to pulp. oSIST ISO 777:2011
ISO 777:2005(E) iv © ISO 2005 – All rights reserved Introduction This International Standard corresponds to ISO 778 [1] and ISO 779 [2] in order to make it possible to perform the final measurement of all three elements on the same solution.
oSIST ISO 777:2011
INTERNATIONAL STANDARD ISO 777:2005(E) © ISO 2005 – All rights reserved 1 Paper, board and pulp — Determination of acid-soluble calcium WARNING — The method specified in this International Standard involves the use of some hazardous chemicals and of gases that can form explosive mixtures with air. Care must be taken to ensure that the relevant precautions are observed. 1 Scope This International Standard specifies the procedure for the determination of acid-soluble calcium by atomic absorption spectrometry or by plasma emission spectrometry. It is applicable to all kinds of paper, board and pulp. It specifies a method to determine the acid-soluble part of the incineration residue, i.e. that part of the ignition residue obtained after incineration that is soluble in hydrochloric acid. If the residue is completely soluble, the result obtained by the procedure specified in this International Standard is taken as the total amount of calcium in the sample. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 186, Paper and board — Sampling to determine average quality ISO 287, Paper and board — Determination of moisture content — Oven-drying method ISO 638, Pulps — Determination of dry matter content ISO 1762, Paper, board and pulps — Determination of residue (ash) on ignition at 525 °C ISO 7213, Pulps — Sampling for testing 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 mass fraction of calcium amount of the element calcium in the solution obtained after incineration of the specimen at 525 °C and treating the residue with 6 mol/l hydrochloric acid, as specified in this International Standard oSIST ISO 777:2011
ISO 777:2005(E) 2 © ISO 2005 – All rights reserved 4 Principle A test portion is incinerated at 525 °C and the residue is treated with 6 mol/l hydrochloric acid. The test solution is aspirated into an acetylene/dinitrogen monoxide or acetylene/air flame and the mass fraction of calcium is determined by one of the following procedures: =measurement of the absorption of the 422,7 nm line emitted by a calcium hollow-cathode lamp, or =measurement of the absorption of the 422,7 nm line emitted by plasma emission spectrometry. 5 Reagents and materials Use only chemicals of recognized analytical grade and only distilled or deionized water. 5.1 Hydrochloric acid, about 6 mol/l. Dilute 500 ml of hydrochloric acid (density 1,19 g/ml) in 500 ml of water. 5.2 Calcium stock solution, 500 mg/l of Ca. Weigh 1,249 g ± 0,001 g of calcium carbonate, dried to constant mass at a temperature not exceeding 200 °C, into a 1 000 ml volumetric flask. Add 50 ml of water. Add a minimum volume of hydrochloric acid (5.1) (approximately 10 ml), drop by drop, to effect the complete dissolution of the calcium carbonate. Dilute with water to the mark and mix. 1 ml of this stock solution contains 0,500 mg of Ca. 5.3 Calcium standard solution, 50 mg/l of Ca. Transfer 100 ml of the stock solution (5.2) to a 1 000 ml volumetric flask, dilute
...
NORME ISO
INTERNATIONALE 777
Troisième édition
2005-05-01
Papier, carton et pâte — Détermination de
la teneur en calcium soluble dans l'acide
Paper, board and pulp — Determination of acid-soluble calcium
Numéro de référence
ISO 777:2005(F)
©
ISO 2005
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ISO 777:2005(F)
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Publié en Suisse
ii © ISO 2005 – Tous droits réservés
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ISO 777:2005(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes nationaux de
normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est en général confiée
aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude a le droit de faire partie du
comité technique créé à cet effet. Les organisations internationales, gouvernementales et non
gouvernementales, en liaison avec l'ISO participent également aux travaux. L'ISO collabore étroitement avec
la Commission électrotechnique internationale (CEI) en ce qui concerne la normalisation électrotechnique.
Les Normes internationales sont rédigées conformément aux règles données dans les Directives ISO/CEI,
Partie 2.
La tâche principale des comités techniques est d'élaborer les Normes internationales. Les projets de Normes
internationales adoptés par les comités techniques sont soumis aux comités membres pour vote. Leur
publication comme Normes internationales requiert l'approbation de 75 % au moins des comités membres
votants.
L'attention est appelée sur le fait que certains des éléments du présent document peuvent faire l'objet de
droits de propriété intellectuelle ou de droits analogues. L'ISO ne saurait être tenue pour responsable de ne
pas avoir identifié de tels droits de propriété et averti de leur existence.
L'ISO 777 a été élaborée par le comité technique ISO/TC 6, Papiers, cartons et pâtes.
Cette troisième édition annule et remplace la deuxième édition (ISO 777:2001), dont elle constitue une
révision mineure. Outre des modifications d'ordre rédactionnel, seul le titre a été modifié, afin d'assurer une
cohérence avec l'ISO 1830:2005 et une distinction avec l'ISO 17812 (à publier) qui spécifie la méthode pour
déterminer la fraction massique totale en calcium, en manganèse, en fer et en cuivre.
La première édition de la présente Norme internationale décrivait la méthode titrimétrique et la méthode
basée sur la spectrométrie d'absorption atomique. Dans la deuxième édition, la méthode titrimétrique avait été
éliminée, car elle est rarement utilisée de nos jours, et le domaine d'application avait été élargi pour inclure le
papier et le carton, en plus de la pâte.
© ISO 2005 – Tous droits réservés iii
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ISO 777:2005(F)
Introduction
[1] [2]
La présente Norme internationale correspond à l'ISO 778 et à l'ISO 779 ; il est donc possible d'obtenir
des mesures finales des trois éléments pour la même solution.
iv © ISO 2005 – Tous droits réservés
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NORME INTERNATIONALE ISO 777:2005(F)
Papier, carton et pâte — Détermination de la teneur en calcium
soluble dans l'acide
AVERTISSEMENT — La méthode spécifiée dans la présente Norme internationale prévoit l'utilisation
de produits chimiques dangereux et de gaz qui peuvent former des mélanges explosifs avec l'air.
S'assurer que les mesures de sécurité nécessaires ont été prises.
1 Domaine d'application
La présente Norme internationale spécifie une méthode de détermination de la teneur en calcium soluble
dans l'acide par spectrométrie d'absorption atomique ou par spectrométrie d'émission de plasma.
Elle est applicable à tous les types de papier, de carton et de pâte.
Elle spécifie une méthode de détermination de la partie soluble dans l'acide des résidus d'incinération, à
savoir la partie des cendres qui est soluble dans l'acide chlorhydrique. Si le résidu est complètement soluble,
le résultat obtenu, en utilisant la procédure spécifiée dans la présente Norme internationale, correspond à la
quantité totale de calcium dans l'échantillon.
2 Références normatives
Les documents de référence suivants sont indispensables pour l'application du présent document. Pour les
références datées, seule l'édition citée s'applique. Pour les références non datées, la dernière édition du
document de référence s'applique (y compris les éventuels amendements).
ISO 186, Papier et carton — Échantillonnage pour déterminer la qualité moyenne
ISO 287, Papier et carton — Détermination de l'humidité — Méthode par séchage à l'étuve
ISO 638, Pâtes — Détermination de la teneur en matières sèches
ISO 1762, Papier, carton et pâtes — Détermination du résidu (cendres) après incinération à 525 °C
ISO 7213, Pâtes — Échantillonnage pour essais
3 Termes et définitions
Pour les besoins du présent document, les termes et définitions suivants s'appliquent.
3.1
fraction massique de calcium
quantité de calcium présente dans la solution après incinération de l'éprouvette à 525 °C et traitement du
résidu avec de l'acide chlorhydrique à 6 mol/l, conformément à la présente Norme internationale
© ISO 2005 – Tous droits réservés 1
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ISO 777:2005(F)
4 Principe
Incinérer une prise d'essai à 525 °C et traiter le résidu avec de l'acide chlorhydrique à 6 mol/l. Aspirer la
solution d'essai dans une flamme d'acétylène/monoxyde de diazote ou une flamme aéro-acétylénique, et
déterminer la fraction massique de calcium par l'un des deux procédés suivants:
mesure de l'absorption de la ligne de 422,7 nm émise par une lampe à cathode creuse au calcium, ou
mesure de l'absorption de la ligne de 422,7 nm émise par un spectromètre à émission de plasma.
5 Réactifs et matériaux
Utiliser uniquement des produits chimiques de qualité analytique reconnue et de l'eau distillée ou déionisée.
5.1 Acide chlorhydrique, 6 mol/l environ.
Diluer 500 ml d'acide chlorhydrique (densité de 1,19 g/ml) dans 500 ml d'eau.
5.2 Solution mère de calcium, 500 mg/l de Ca.
Peser 1,249 g ± 0,001 g de carbonate de calcium, préalablement séché à masse constante à une
température n'excédant pas 200 °C, dans une fiole jaugée de 1 000 ml. Ajouter 50 ml d'eau. Ajouter goutte à
goutte la quantité juste nécessaire d'acide chlorhydrique (5.1) (environ 10 ml), pour dissoudre complètement
le carbonate de calcium. Diluer avec de l'eau jusqu'au trait et mélanger.
1 ml de cette solution mère contient 0,500 mg de Ca.
5.3 Solution étalon de calcium, 50 mg/l de Ca.
Transférer 100 ml de la solution mère (5.2) dans une fiole jaugée de 1 000 ml, diluer avec de l'eau jusqu'au
trait et mélanger.
1 ml de cette solution étalon contient 0,05 mg de Ca.
Les solutions étalons commerciales conviennent à l'essai.
5.4 Solution de lanthane, 50 g/l de La.
Mouiller 59 g d'oxyde de lanthane (La O ) avec de l'eau. Lentement et avec précaution, ajouter 250 ml
2 3
d'acide chlorhydrique (densité de 1,19 g/ml) pour dissoudre l'oxyde de lanthane. Diluer jusqu'au trait dans une
fiole jaugée de 1 000 ml et mélanger.
Cette solution sert à éliminer l'interférence du phosphate dans
...
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