1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 12830:2011Paper, board and pulps Determination of acid-soluble magnesium, calcium,manganese, iron, copper,sodium and potassiumBS ISO 12830:2011 BRITISH STANDARDNational fo
2、rewordThis British Standard is the UK implementation of ISO 12830:2011. It supersedes BS ISO 1830:2005, BS ISO 777:2005, BS ISO 778:2005 and BS ISO 779:2005 which are withdrawnThe UK participation in its preparation was entrusted to Technical Committee PAI/11, Methods of test for paper, board and pu
3、lps.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. BSI 2011 ISBN 978 0 580 66815 9 ICS 85.040; 85.060 Complia
4、nce with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 December 2011.Amendments issued since publicationDate T e x t a f f e c t e dBS ISO 12830:2011Paper, board and pulps
5、Determination of acid-soluble magnesium, calcium, manganese, iron, copper, sodium and potassiumPapiers, cartons et ptes Dtermination de la teneur en magnsium, calcium, manganse, fer, cuivre, sodium et potassium soluble dans lacide ISO 2011Reference numberISO 12830:2011(E)First edition2011-11-15ISO12
6、830INTERNATIONAL STANDARDBS ISO 12830:2011ISO 12830:2011(E)COPYRIGHT PROTECTED DOCUMENT ISO 2011All 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, with
7、out permission in writing from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in Switzerlandii ISO 2011 All rights rese
8、rvedBS ISO 12830:2011ISO 12830:2011(E) ISO 2011 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope 12 Normative references .13 Principle .14 Reagents and materials .15 Apparatus and equipment .36 Sampling and preparation of sample .37 Procedure 37.1 General .37.2 Incineration of th
9、e test portion 37.3 Dissolution of the residue .48 Preparation of calibration solutions .48.1 Atomic absorption spectrometry (AAS) 48.2 Plasma emission spectrometry (ICP/ES) 49 Blank solution 510 Determination .511 Calculation 612 Test report .6Annex A (informative) Precision .7Bibliography .12BS IS
10、O 12830:2011ForewordISO (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 fo
11、r 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
12、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
13、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 resp
14、onsible for identifying any or all such patent rights.ISO 12830 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps.This first edition of ISO 12830 cancels and replaces ISO 777:2005, ISO 778:2005, ISO 779:2005, ISO 1830:2005 and ISO 9668:1990. ISO 12830:2011(E)iv ISO 2011 All rights
15、 reservedBS ISO 12830:2011IntroductionThis International Standard combines the determination of the acid-soluble part of magnesium (Mg), calcium (Ca), manganese (Mn), iron (Fe), copper (Cu), sodium (Na) and potassium (K) into a single standard. The scope of this International Standard covers only th
16、e acid-soluble part of the elements. ISO 17812 specifies the procedure for the determination of total magnesium, total calcium, total manganese, total iron and total copper by atomic absorption spectrometry or by plasma emission spectrometry.ISO 12830:2011(E) ISO 2011 All rights reserved vBS ISO 128
17、30:2011BS ISO 12830:2011INTERNATIONAL STANDARD ISO 12830:2011(E)Paper, board and pulps Determination of acid-soluble magnesium, calcium, manganese, iron, copper, sodium and potassiumWARNING The method specified in this International Standard involves the use of some hazardous chemicals and of gases
18、that may form explosive mixtures with air. Care should be taken to ensure that the relevant precautions are observed.1 ScopeThis International Standard specifies the procedure for the determination of acid-soluble magnesium, calcium, manganese, iron, copper, sodium and potassium by atomic absorption
19、 spectrometry or by plasma emission spectrometry. The acid-soluble element comprises the acid-soluble part of the incineration residue, i.e. that part of the ignition residue obtained after incineration which is soluble in hydrochloric acid. In the case where the residue is completely soluble, the r
20、esult obtained by the procedure specified in this International Standard is a measure of the total amount of each element in the sample.This International Standard is applicable to all types of paper, board and pulps.The limit of determination depends on the element and on the instrument used.2 Norm
21、ative referencesThe 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
22、to determine average qualityISO 638, Paper, board and pulps Determination of dry matter content Oven-drying methodISO 1762, Paper, board and pulps Determination of residue (ash) on ignition at 525 CISO 3696, Water for analytical laboratory use Specification and test methodsISO 7213, Pulps Sampling f
23、or testing3 PrincipleA test portion is incinerated at 525 C and the residue is dissolved in 6 mol/l hydrochloric acid. The concentration of each element in the test solution is then determined by atomic absorption or plasma emission spectrometry, as specified in this International Standard.4 Reagent
24、s and materials4.1 General.All chemicals shall be of reagent grade or better unless otherwise indicated. Water shall be distilled or deionized, of grade 2 in accordance with ISO 3696. ISO 2011 All rights reserved 1BS ISO 12830:20114.2 Hydrochloric acid (HCl), 6 mol/l. Dilute 500 ml of concentrated h
25、ydrochloric acid (specific gravity 1,19 g/ml) to 1 000 ml with water.4.3 Nitric acid (HNO3), concentrated (specific gravity 1,4 g/ml).4.4 Lanthanum chloride (LaCl3), solution, (La) = 50 g/l. In a 1 000 ml volumetric flask, dissolve 59 g of lanthanum oxide (La2O3), in small portions, in 200 ml of hyd
26、rochloric acid (4.2) and dilute to 1 000 ml with water.NOTE This lanthanum solution is used to eliminate chemical interference when determining calcium and magnesium in an air/acetylene flame. The solution is not required when the nitrous oxide/acetylene flames or inductively coupled plasma techniqu
27、e (ICP technique) is used.4.5 Cesium chloride (CsCl), solution (Cs) = 50 g/l. In a 1 000 ml volumetric flask, dissolve 63,5 g of ultra-pure cesium chloride (CsCl) in water and dilute to 1 000 ml with water.NOTE This cesium solution is used to suppress ionization of sodium and potassium. It is also u
28、sed to suppress ionization of calcium in a nitrous oxide/acetylene flame. The solution is not required when the air/acetylene flame or ICP technique is used.4.6 Standard stock solutions of each element, commercially available certified atomic absorption or atomic emission standard solutions can be u
29、sed. Standard stock solutions can also be prepared as follows:4.6.1 Magnesium, 1 000 mg/l standard solution. Dissolve 1,000 g of magnesium metal ribbon in 100 ml of 1:4 nitric acid (4.3) and dilute to 1 000 ml with water.4.6.2 Calcium, 1 000 mg/l standard solution. Dissolve 2,497 g of primary standa
30、rd calcium carbonate (CaCO3) in a minimum volume of 1:4 nitric acid (4.3) and dilute to 1 000 ml with water.4.6.3 Manganese, 1 000 mg/l standard solution. Dissolve 1,000 g of manganese metal strip or wire in a minimum volume of 1:1 nitric acid (4.3) and dilute to 1 000 ml with water.4.6.4 Iron, 1 00
31、0 mg/l standard solution. Dissolve 1,000 g of iron metal strip or wire in 20 ml of hydrochloric acid (4.2) and dilute to 1 000 ml with water.4.6.5 Copper, 1 000 mg/l standard solution. Dissolve 1,000 g of copper metal strip or wire in a minimum volume of 1:1 nitric acid (4.3) and dilute to 1 000 ml
32、with water.4.6.6 Sodium, 1 000 mg/l standard solution. Ignite a portion of anhydrous sodium sulfate (Na2SO4) at 550 C in a crucible of platinum or porcelain. Allow to cool to room temperature in a desiccator. Dissolve 3,089 g of dried sodium sulfate in water and dilute to 1 000 ml with water. Store
33、in a polyethylene bottle.4.6.7 Potassium, 1 000 mg/l standard solution. Ignite a portion of anhydrous potassium sulfate (K2SO4) at 550 C in a crucible of platinum or porcelain. Allow to cool to room temperature in a desiccator. Dissolve 2,228 g of dried potassium sulfate in water and dilute to 1 000
34、 ml with water. Store in a polyethylene bottle.4.7 Acetylene gas and/or nitrogen oxide gas, of a grade suitable for atomic absorption spectrometry. Nitrous oxide is used only when measuring calcium.WARNING Acetylene gas forms explosive mixtures with air.4.8 Carrier gas, appropriate gas for the plasm
35、a emission spectrometer. Argon is usually recommended as a carrier gas.ISO 12830:2011(E)2 ISO 2011 All rights reservedBS ISO 12830:20115 Apparatus and equipment5.1 General.Ordinary laboratory equipment is used. All glassware and plastic ware shall be rinsed with 0,1 mol/l hydrochloric acid prior to
36、use.5.2 Filter paper, ash free, particle retention 20 m to 25 m.5.3 Crucibles, platinum or fused silica, of minimum capacity 50 ml.5.4 Muffle furnace, capable of maintaining a temperature of 525 C null 25 C.5.5 Balance, of capacity 100 g, accurate to 0,1 mg.5.6 Atomic absorption spectrometer (AAS),
37、equipped with air/acetylene and nitrous oxide/acetylene burners and with hollow cathode lamps for Mg, Ca, Mn, Fe, Cu, Na and K.NOTE Multi-element lamps can also be used.5.7 Inductively coupled plasma/optical emission spectrometer (ICP/OES).5.8 Disposable protective gloves.6 Sampling and preparation
38、of sampleIf the analysis is being made to evaluate a lot of paper, board or pulp, the sample shall be selected in accordance with ISO 186 or ISO 7213, as relevant. If the analysis is made on another type of sample, report the source of the sample and, if possible, the sampling procedure. Select the
39、specimens so that they are representative of the sample received. A sufficient amount of sample shall be collected to allow for at least duplicate determinations. Avoid cut edges, punched holes and other parts where metallic contamination may have occurred. Disposable protective gloves (5.8) shall b
40、e worn when handling samples to avoid contamination.Prepare a test specimen by tearing at least 30 g of small pieces from various parts of the sample. This amount is sufficient for the duplicate determinations described in Clause 7.Since iron tends to be non-homogeneous in the sample, it is recommen
41、ded that a composite sample be used.7 Procedure7.1 GeneralAlthough dry ignition followed by acid treatment is described in this International Standard, other dissolution methods such as wet ignition or microwave digestion using various acid combinations can also be used, provided that the results ha
42、ve been validated.WARNING For samples with high silicon content, microwave digestion with nitric acid will give lower results for magnesium and for some other elements.7.2 Incineration of the test portionCarry out the procedure in duplicate.Air-dry the specimen in the laboratory atmosphere until it
43、reaches moisture equilibrium.ISO 12830:2011(E) ISO 2011 All rights reserved 3BS ISO 12830:2011Determine the moisture content on a separate air-dried portion, as specified in ISO 638. Weigh this portion at the same time as the test portion used for incineration. For the determination of major element
44、s, including magnesium, calcium, sodium and potassium, a 1 g to 2 g test portion (calculated as oven-dry) is recommended. For minor elements, including manganese, iron and copper, test portions of 5 g to 10 g are recommended. If trace levels of elements are needed, then use sample sizes that are lar
45、ger than 10 g.Carry out ashing of the test portion as described in ISO 1762.NOTE In order to avoid flames, cover the dish with a lid. The lid should only cover the dish partially to avoid the occurrence of reducing conditions in the dish, in which case acid-insoluble compounds might be formed. Under
46、 reducing conditions, for example, copper might be lost due to the formation of a platinum alloy.7.3 Dissolution of the residueAfter ashing, allow the crucible to cool. To avoid splattering, carefully moisten the residue of ignition with water and add cautiously, in a fume hood, 5 ml of hydrochloric
47、 acid (4.2) to the crucible. Evaporate to dryness on a boiling water bath or hotplate or using an infrared lamp. Repeat this procedure.NOTE For samples with high carbonate content, more than 10 ml of acid (2 null 5 ml) might be needed.Add 5 ml of hydrochloric acid (4.2) to the residue. If some insol
48、uble residue is visible, heat, without boiling, the crucible covered with a watch glass for a few minutes.Using the filter paper (5.2), filter the content of the crucible into a 100 ml volumetric flask. To ensure that the transfer is complete, add another portion of 5 ml of hydrochloric acid (4.2) t
49、o the crucible and heat again if necessary. Filter this last portion of acid into the main portion in the volumetric flask with the aid of some water (5.1). If required for AAS, add 4 ml of lanthanum chloride solution (4.4) or 2 ml of cesium chloride solution (4.5) to the volumetric flask. Fill up to the mark with water and mix. This is the test solution.8 Preparation of calibration solutionsIt is important that the acid concentration and the lanthanum chloride/cesium chloride concentration in the calibration solutions are
