1、BSI Standards PublicationBS ISO 9599:2015Copper, lead, zinc and nickel sulfide concentrates Determination of hygroscopic moisture content of the analysis sample Gravimetric methodBS ISO 9599:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 9599:2015.The UK
2、participation in its preparation was entrusted to Technical Committee NFE/36, Copper lead and zinc ores and concentrates.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 co
3、ntract. Users are responsible for its correct application. The British Standards Institution 2015. Published by BSI Standards Limited 2015ISBN 978 0 580 87931 9 ICS 73.060.99 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under th
4、e authority of the Standards Policy and Strategy Committee on 31 October 2015.Amendments issued since publicationDate T e x t a f f e c t e dBS ISO 9599:2015 ISO 2015Copper, lead, zinc and nickel sulfide concentrates Determination of hygroscopic moisture content of the analysis sample Gravimetric me
5、thodlment concentrs sulfurs de cuivre, de plomb et de zinc Dtermination de lhumidit hygroscopique dans lchantillon pour analyse Mthode gravimtriqueINTERNATIONAL STANDARDISO9599Second edition2015-10-01Reference numberISO 9599:2015(E)BS ISO 9599:2015ISO 9599:2015(E)ii ISO 2015 All rights reservedCOPYR
6、IGHT PROTECTED DOCUMENT ISO 2015, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, wit
7、hout prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS
8、 ISO 9599:2015ISO 9599:2015(E)Foreword iv1 Scope . 12 Normative references 13 Principle 14 Reagents 15 Apparatus . 16 Sampling and samples 26.1 General . 26.2 Laboratory sample . 26.3 Preparation of the test sample 27 Procedure. 27.1 Preparation of the weighing vessel . 27.2 Test portion 27.3 Determ
9、ination . 28 Expression of results 39 Test report (for internal laboratory use only) . 3Annex A (normative) Method for samples susceptible to oxidation Drying in nitrogen 4 ISO 2015 All rights reserved iiiContents PageBS ISO 9599:2015ISO 9599:2015(E)ForewordISO (the International Organization for St
10、andardization) 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 rig
11、ht 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.The procedures
12、 used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rul
13、es of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).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. Details of any patent rights identi
14、fied during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on
15、 the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationISO 9599 was prepared by Technical Committee ISO/
16、TC 183, Copper, lead, zinc and nickel ores and concentrates.This second edition cancels and replaces the first edition (ISO 9599:1991), which has been technically revised.iv ISO 2015 All rights reservedBS ISO 9599:2015INTERNATIONAL STANDARD ISO 9599:2015(E)Copper, lead, zinc and nickel sulfide conce
17、ntrates Determination of hygroscopic moisture content of the analysis sample Gravimetric methodWARNING Any chemical-reagent waste must be disposed of in an environmentally sound manner that does not injure the health or welfare of the environment, people, animals, vegetation, etc.1 ScopeThis Interna
18、tional Standard specifies a gravimetric loss-in-mass method for the determination of the hygroscopic moisture content in analysis samples of copper, lead, zinc, and nickel sulfide concentrates.The method is applicable to copper, lead, zinc, and nickel sulfide concentrates free from volatile organic
19、flotation reagents, for example kerosene, and with hygroscopic moisture contents between 0,05 % (m/m) and 2 % (m/m). The hygroscopic moisture content is used to correct the analysis results from the equilibrated moisture level to the dry basis.NOTE The result of the determination of hygroscopic mois
20、ture content using this International Standard should not be reported as part of the analysis of a concentrate sample. Whenever the bulk moisture content of a commercial shipment of concentrate is required, ISO 10251 should be used. The determination of hygroscopic moisture content and the determina
21、tion of bulk moisture content are connected with each other. In both determinations, the same state of dryness has to be achieved, in order to ascertain the correct metal content of a lot.This method is not applicable to sulfide concentrates that are susceptible to oxidation (see 6.3, note 2). Annex
22、 A sets out a modified procedure, which can be used for sulfide concentrates that are susceptible to oxidation.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references
23、, the latest edition of the referenced document (including any amendments) applies.ISO 10251, Copper, lead, zinc and nickel concentrates Determination of mass loss of bulk material on dryingISO 12743, Copper, lead, zinc and nickel concentrates Sampling procedures for determination of metal and moist
24、ure content3 PrincipleDrying of a weighed test portion in air in an oven maintained at 105 C 5 C and calculation of the percentage moisture content from the loss in mass.4 Reagents4.1 Desiccant, such as self-indicating silica gel or anhydrous magnesium perchlorate.5 ApparatusOrdinary laboratory equi
25、pment, and the following. ISO 2015 All rights reserved 1BS ISO 9599:2015ISO 9599:2015(E)5.1 Analytical balance, sensitive to 0,1 mg.5.2 Laboratory oven, capable of maintaining a temperature of 105 C 5 C.5.3 Weighing vessel, shallow, of glass or silica or corrosion-resistant metal, with an externally
26、 fitting air-tight cover of approximately 50 mm diameter.5.4 Flat dish, or tray.6 Sampling and samples6.1 GeneralSampling and sample preparation shall be according to ISO 12743.6.2 Laboratory sampleUse a sample of minus 150 m particle size.6.3 Preparation of the test sampleTake a sufficient mass of
27、the laboratory sample for the required chemical analysis and moisture determination and transfer to a flat dish or tray (5.4). Spread the sample evenly into a thin layer about 3 mm to 5 mm thick. Cover the dish to protect the sample from dust, but allowing a free flow of air across the top of the sa
28、mple. Allow the test sample to equilibrate with the laboratory atmosphere for 2 h or for long enough to achieve equilibration.Equilibration is achieved whenever the change in mass of the test sample over a 2 h period of exposure is less than 0,1 %.7 Procedure7.1 Preparation of the weighing vesselDry
29、 a weighing vessel and cover (5.3) by heating in the laboratory oven (5.2) at 105 C 5 C for 1 h. Transfer the weighing vessel and cover to a desiccator containing a suitable fresh desiccant (4.1), and allow to cool to ambient temperature. Remove the weighing vessel and cover from the desiccator and
30、weigh to the nearest 0,1 mg (mass m1), after slightly lifting the weighing vessel cover and quickly replacing it.7.2 Test portionTransfer approximately 10 g of the equilibrated test sample (6.2) directly to the dried and tared weighing vessel (7.1), spreading in an even layer about 3 mm to 5 mm thic
31、k. Record the mass of the weighing vessel and cover plus test portion to the nearest 0,1 mg (mass m2). Within the following 5 min, also weigh the test portions required for the determination of constituents for which correction of the analytical values to a dry basis is required and transfer such te
32、st portions to the appropriate receptacles required for subsequent testing.7.3 DeterminationTransfer the uncovered weighing vessel containing the test portion and the vessel cover to the laboratory oven (5.2) and dry at 105 C 5 C for 2 h. After the 2 h period, remove the weighing vessel containing t
33、he dry test portion from the oven, replace the cover and allow cooling to ambient temperature in the desiccator. Whenever cool, remove the weighing vessel containing the dry test portion and the vessel 2 ISO 2015 All rights reservedBS ISO 9599:2015ISO 9599:2015(E)cover from the desiccator and reweig
34、h to the nearest 0,1 mg, after slightly lifting the weighing vessel cover and quickly replacing it.Repeat the drying at 105 C 5 C for another 2 h, cool to ambient temperature in the desiccator and weigh to determine if constant mass ( 1 mg) has been achieved. If constant mass has not been achieved,
35、repeat the drying and weighing steps described above. Record the constant mass (m3).NOTE If constant mass ( 1 mg) is not achieved after three drying periods of 2 h, then the method specified in Annex A should be used.8 Expression of resultsThe hygroscopic moisture content, H, expressed as a percenta
36、ge by mass, is calculated from the formulaHmmmm=2321100wherem1is the mass, in grams, of the dried weighing vessel plus cover;m2is the mass, in grams, of the weighing vessel plus cover plus test portion before drying;m3is the mass, in grams, of the weighing vessel plus cover plus test portion after d
37、rying.Calculate the hygroscopic moisture content of the sample to the second decimal place.9 Test report (for internal laboratory use only)The test report shall contain the following information:a) identification of the sample;b) reference to this International Standard;c) hygroscopic moisture conte
38、nt of the sample;d) date on which the test was carried out. ISO 2015 All rights reserved 3BS ISO 9599:2015ISO 9599:2015(E)Annex A (normative) Method for samples susceptible to oxidation Drying in nitrogenA.1 PrincipleDrying of a weighed test portion in oxygen-free, dry nitrogen in an oven maintained
39、 at 105 C 5 C and calculation of the percentage moisture content from the loss in mass.A.2 ReagentsA.2.1 Nitrogen, dry gas containing less than 30 l of oxygen per litre.A.2.2 Desiccant, such as self-indicating silica gel or anhydrous magnesium perchlorate.A.3 ApparatusOrdinary laboratory equipment,
40、and the following.A.3.1 Analytical balance, sensitive to 0,1 mg.A.3.2 Minimum-free-space oven, capable of maintaining a temperature of 105 C 5 C, with provision for pre-heated nitrogen (A.2.1) to pass through the oven at 15 to 20 oven-volumes per hour. A suitable oven is shown in Figure A.1.A.3.3 We
41、ighing vessel, shallow, of glass or silica or corrosion-resistant metal, with an externally fitting air-tight cover of approximately 50 mm diameter.A.3.4 Flowmeter, capable of measuring the rate of flow of nitrogen (A.2.1) through the oven (A.3.2).A.3.5 Drying tower, of approximately 250 ml capacity
42、, packed with anhydrous magnesium perchlorate (A.2.2) for drying the nitrogen (A.2.1).A.4 ProcedureA.4.1 Preparation of the weighing vesselRaise the temperature of the oven (A.3.2) to 105 C 5 C while passing nitrogen (A.2.1) through the oven at the rate of 15 to 20 oven-volumes per hour.Dry a weighi
43、ng vessel and cover (A.3.3) by heating in the oven at 105 C 5 C for 1 h. Transfer the weighing vessel and cover to a desiccator containing a suitable fresh desiccant (A.2.2), and allow to cool to ambient temperature. Remove the weighing vessel and cover from the desiccator and weigh to the nearest 0
44、,1 mg (mass m1), after slightly lifting the weighing vessel cover and quickly replacing it.4 ISO 2015 All rights reservedBS ISO 9599:2015ISO 9599:2015(E)Dimensions in millimetresFigure A.1 Suitable nitrogen ovenA.4.2 Test portionTransfer approximately 10 g of the equilibrated test sample (5.2) direc
45、tly into the dried and tared weighing vessel (A.4.1), spreading the sample in an even layer about 3 mm to 5 mm thick. Record the mass of the weighing vessel and cover plus test portion to the nearest 0,1 mg (mass m2).A.4.3 DeterminationTransfer the uncovered weighing vessel containing the test porti
46、on and the vessel cover to the oven (A.3.2) and dry at 105 C 5 C until constant mass ( 1 mg) is achieved (see Note).NOTE Under the conditions described above, drying should be complete in between 1,5 h and 3 h. Constancy in mass ( 1 mg) should be established by reheating at 105 C 5 C for a further p
47、eriod of 30 min, followed by cooling and weighing as described.Remove the weighing vessel containing the dry test portion from the oven, replace the cover and allow cooling to ambient temperature in the desiccator. Whenever cool, remove the weighing vessel containing the test portion and the vessel
48、cover from the desiccator and reweigh to the nearest 0,1 mg (mass m3), after slightly lifting the weighing vessel cover and quickly replacing it. ISO 2015 All rights reserved 5BS ISO 9599:2015ISO 9599:2015(E)A.5 Expression of resultsThe hygroscopic moisture content, H, expressed as a percentage by m
49、ass, is calculated from the formulaHmmmm=2321100wherem1is the mass, in grams, of the dried weighing vessel plus cover;m2is the mass, in grams, of the weighing vessel plus cover plus test portion before drying;m3is the mass, in grams, of the weighing vessel plus cover plus test portion after drying.Calculate the hygroscopic moisture content of the sample to the second decimal place.A.6 Test report (for internal laboratory use only)The test report shall contain the f
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