1、BSI Standards Publication BS ISO 9599:2015 Copper, lead, zinc and nickel sulfide concentrates Determination of hygroscopic moisture content of the analysis sample Gravimetric methodBS ISO 9599:2015 BRITISH STANDARD National foreword This British Standard is the UK implementation of ISO 9599:2015. Th
2、e UK 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
3、of a contract. Users are responsible for its correct application. The British Standards Institution 2015. Published by BSI Standards Limited 2015 ISBN 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
4、 under the authority of the Standards Policy and Strategy Committee on 31 October 2015. Amendments issued since publication Date T e x t a f f e c t e dBS ISO 9599:2015 ISO 2015 Copper, lead, zinc and nickel sulfide concentrates Determination of hygroscopic moisture content of the analysis sample Gr
5、avimetric method lment concentrs sulfurs de cuivre, de plomb et de zinc Dtermination de lhumidit hygroscopique dans lchantillon pour analyse Mthode gravimtrique INTERNATIONAL STANDARD ISO 9599 Second edition 2015-10-01 Reference number ISO 9599:2015(E)BS ISO 9599:2015ISO 9599:2015(E)ii ISO 2015 All
6、rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in Switzerland All 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 intern
7、et or an intranet, without 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 office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 c
8、opyrightiso.org www.iso.orgBS ISO 9599:2015ISO 9599:2015(E)Foreword iv 1 Scope . 1 2 Normative references 1 3 Principle 1 4 Reagents 1 5 Apparatus . 1 6 Sampling and samples 2 6.1 General . 2 6.2 Laboratory sample . 2 6.3 Preparation of the test sample 2 7 Procedure. 2 7.1 Preparation of the weighin
9、g vessel . 2 7.2 Test portion 2 7.3 Determination . 2 8 Expression of results 3 9 Test report (for internal laboratory use only) . 3 Annex A (normative) Method for samples susceptible to oxidation Drying in nitrogen 4 ISO 2015 All rights reserved iii Contents PageBS ISO 9599:2015ISO 9599:2015(E) For
10、eword 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 tech
11、nical 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
12、 electrotechnical standardization. The procedures 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
13、 was drafted in accordance with the editorial rules 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
14、patent rights. Details of any patent rights identified 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
15、not constitute an endorsement. For an explanation on 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 informat
16、ion ISO 9599 was prepared by Technical Committee ISO/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 ST ANDARD ISO
17、9599:2015(E) Copper, lead, zinc and nickel sulfide concentrates Determination of hygroscopic moisture content of the analysis sample Gravimetric method WARNING Any chemical-reagent waste must be disposed of in an environmentally sound manner that does not injure the health or welfare of the environm
18、ent, people, animals, vegetation, etc. 1 Scope This International 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,
19、 and nickel sulfide concentrates free from volatile organic 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 ba
20、sis. NOTE The result of the determination of hygroscopic moisture 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 de
21、termination of hygroscopic moisture content and the determination 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 concentra
22、tes that are susceptible to oxidation (see 6.3, note 2). Annex A sets out a modified procedure, which can be used for sulfide concentrates that are susceptible to oxidation. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated re
23、ferences, only the edition cited applies. For undated references, 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 drying ISO 12743, Copper, lead, zinc and nickel con
24、centrates Sampling procedures for determination of metal and moisture content 3 Principle Drying 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 Reagents 4.1 Desiccant, such as self-indicating silica gel
25、or anhydrous magnesium perchlorate. 5 Apparatus Ordinary laboratory equipment, 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, s
26、hallow, of glass or silica or corrosion-resistant metal, with an externally fitting air-tight cover of approximately 50 mm diameter. 5.4 Flat dish, or tray. 6 Sampling and samples 6.1 General Sampling and sample preparation shall be according to ISO 12743. 6.2 Laboratory sample Use a sample of minus
27、 150 m particle size. 6.3 Preparation of the test sample Take a sufficient mass of 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 pro
28、tect the sample from dust, but allowing a free flow of air across the top of the sample. 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
29、 of exposure is less than 0,1 %. 7 Procedure 7.1 Preparation of the weighing vessel Dry 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 coo
30、l to ambient temperature. Remove the weighing vessel and cover from the desiccator and weigh to the nearest 0,1 mg (mass m 1 ), after slightly lifting the weighing vessel cover and quickly replacing it. 7.2 Test portion Transfer approximately 10 g of the equilibrated test sample (6.2) directly to th
31、e dried and tared weighing vessel (7.1), spreading 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 m 2 ). Within the following 5 min, also weigh the test portions required for the determination of constituents
32、for which correction of the analytical values to a dry basis is required and transfer such test portions to the appropriate receptacles required for subsequent testing. 7.3 Determination Transfer the uncovered weighing vessel containing the test portion and the vessel cover to the laboratory oven (5
33、.2) and dry at 105 C 5 C for 2 h. After the 2 h period, 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 dry test portion and the vessel 2 I
34、SO 2015 All rights reservedBS ISO 9599:2015ISO 9599:2015(E) cover from the desiccator and reweigh 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
35、to determine if constant mass ( 1 mg) has been achieved. If constant mass has not been achieved, repeat the drying and weighing steps described above. Record the constant mass (m 3 ). NOTE If constant mass ( 1 mg) is not achieved after three drying periods of 2 h, then the method specified in Annex
36、A should be used. 8 Expression of results The hygroscopic moisture content, H, expressed as a percentage by mass, is calculated from the formula where m 1 is the mass, in grams, of the dried weighing vessel plus cover; m 2 is the mass, in grams, of the weighing vessel plus cover plus test portion be
37、fore drying; m 3 is 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. 9 Test report (for internal laboratory use only) The test report shall contain the following information: a)
38、 identification of the sample; b) reference to this International Standard; c) hygroscopic moisture content 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
39、in nitrogen A.1 Principle Drying of a weighed test portion in oxygen-free, dry nitrogen in an oven maintained at 105 C 5 C and calculation of the percentage moisture content from the loss in mass. A.2 Reagents A.2.1 Nitrogen, dry gas containing less than 30 l of oxygen per litre. A.2.2 Desiccant, su
40、ch as self-indicating silica gel or anhydrous magnesium perchlorate. A.3 Apparatus Ordinary laboratory equipment, 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
41、 (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 Weighing 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 measur
42、ing 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, packed with anhydrous magnesium perchlorate (A.2.2) for drying the nitrogen (A.2.1). A.4 Procedure A.4.1 Preparation of the weighing vessel Raise the temperature of the oven (A.3.
43、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 weighing 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), an
44、d allow to cool to ambient temperature. Remove the weighing vessel and cover from the desiccator and weigh to the nearest 0,1 mg (mass m 1 ), 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 millime
45、tres Figure A.1 Suitable nitrogen oven A.4.2 Test portion Transfer approximately 10 g of the equilibrated test sample (5.2) directly 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
46、 test portion to the nearest 0,1 mg (mass m 2 ). A.4.3 Determination Transfer the uncovered weighing vessel containing the test portion 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
47、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 period 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
48、cooling to ambient temperature in the desiccator. Whenever cool, remove the weighing vessel containing the test portion and the vessel cover from the desiccator and reweigh to the nearest 0,1 mg (mass m 3 ), after slightly lifting the weighing vessel cover and quickly replacing it. ISO 2015 All righ
49、ts reserved 5BS ISO 9599:2015ISO 9599:2015(E) A.5 Expression of results The hygroscopic moisture content, H, expressed as a percentage by mass, is calculated from the formula where m 1 is the mass, in grams, of the dried weighing vessel plus cover; m 2 is the mass, in grams, of the weighing vessel plus cover plus test portion before drying; m 3 is the mass, in grams, of the weighing vessel plus cover plus test port
