SANS 1952-2009 Solid mineral fuels - Determination of extractable metals in dilute hydrochloric acid《固体矿物燃料 稀释盐酸中可萃取金属的测定》.pdf

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1、 Collection of SANS standards in electronic format (PDF) 1. Copyright This standard is available to staff members of companies that have subscribed to the complete collection of SANS standards in accordance with a formal copyright agreement. This document may reside on a CENTRAL FILE SERVER or INTRA

2、NET SYSTEM only. Unless specific permission has been granted, this document MAY NOT be sent or given to staff members from other companies or organizations. Doing so would constitute a VIOLATION of SABS copyright rules. 2. Indemnity The South African Bureau of Standards accepts no liability for any

3、damage whatsoever than may result from the use of this material or the information contain therein, irrespective of the cause and quantum thereof. ISBN 978-0-626-21959-8 SANS 1952:2009Edition 1ISO 1952:2008Edition 2SOUTH AFRICAN NATIONAL STANDARD Solid mineral fuels Determination of extractable meta

4、ls in dilute hydrochloric acid This national standard is the identical implementation of ISO 1952:2008 and is adopted with the permission of the International Organization for Standardization. Published by SABS Standards Division 1 Dr Lategan Road Groenkloof Private Bag X191 Pretoria 0001Tel: +27 12

5、 428 7911 Fax: +27 12 344 1568 www.sabs.co.za SABS SANS 1952:2009 Edition 1 ISO 1952:2008 Edition 2 Table of changes Change No. Date Scope Foreword This South African standard was approved by National Committee SABS SC 27B, Solid mineral fuels Test methods, in accordance with procedures of the SABS

6、Standards Division, in compliance with annex 3 of the WTO/TBT agreement. This SANS document was published in May 2009. Reference numberISO 1952:2008(E)ISO 2008INTERNATIONAL STANDARD ISO1952Second edition2008-09-01Solid mineral fuels Determination of extractable metals in dilute hydrochloric acid Com

7、bustibles minraux solides Dtermination des mtaux extractibles dans lacide chlorhydrique dilu SANS 1952:2009This s tandard may only be used and printed by approved subscription and freemailing clients of the SABS .ISO 1952:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accord

8、ance with Adobes 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 Adobes lic

9、ensing 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 printi

10、ng. 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. COPYRIGHT PROTECTED DOCUMENT ISO 2008 All rights reserved. Unless otherwise

11、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 ISOs member body in the country of the requester. ISO copyright offi

12、ce Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2008 All rights reservedSANS 1952:2009This s tandard may only be used and printed by approved subscription and freemailing clients of the SABS .IS

13、O 1952:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references . 1 3 Principle. 1 4 Reagents and materials . 1 5 Apparatus 4 6 Preparation of the test sample 4 7 Procedure 4 8 Expression of results . 5 9 Precision 6 10 Test report . 6 SANS

14、1952:2009This s tandard may only be used and printed by approved subscription and freemailing clients of the SABS .ISO 1952:2008(E) iv ISO 2008 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodi

15、es). 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

16、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, P

17、art 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 casti

18、ng 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 1952 was prepared by Technical Committee ISO/TC 27, Solid mineral fuels, Subcommittee

19、SC 5, Methods of analysis. This second edition cancels and replaces the first edition (ISO 1952:1976), which has been technically revised. SANS 1952:2009This s tandard may only be used and printed by approved subscription and freemailing clients of the SABS .ISO 1952:2008(E) ISO 2008 All rights rese

20、rved vIntroduction Sodium, potassium, calcium, iron and magnesium are commonly present in solid mineral fuel. They can contribute significantly to coal-utilization problems, such as boiler-tube fouling and ash disposal; they also affect product quality and gaseous emissions from combustion processes

21、. Research indicates that the amounts of alkaline and earth-alkaline metals extractable with dilute hydrochloric acid are more closely related to the fouling/slagging properties of solid mineral fuel than are the total amounts of the metals. SANS 1952:2009This s tandard may only be used and printed

22、by approved subscription and freemailing clients of the SABS .SANS 1952:2009This s tandard may only be used and printed by approved subscription and freemailing clients of the SABS .INTERNATIONAL STANDARD ISO 1952:2008(E) ISO 2008 All rights reserved 1Solid mineral fuels Determination of extractable

23、 metals in dilute hydrochloric acid 1 Scope This International Standard describes the extraction from solid mineral fuels by dilute hydrochloric acid and determination of extractable sodium, potassium, calcium, iron and magnesium. 2 Normative references The following referenced documents are indispe

24、nsable 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 3696, Water for analytical laboratory use Specification and test methods ISO 5068-2, Brown

25、coals and lignites Determination of moisture content Part 2: Indirect gravimetric method for moisture in the analysis sample ISO 5069-2, Brown coals and lignites Principles of sampling Part 2: Sample preparation for determination of moisture content and for general analysis ISO 5725-6:1994, Accuracy

26、 (trueness and precision) of measurement methods and results Part 6: Use in practice of accuracy values ISO 11722, Solid mineral fuels Hard coal Determination of moisture in the general analysis test sample by drying in nitrogen ISO 13909-4, Hard coal and coke Mechanical sampling Part 4: Coal Prepar

27、ation of test samples 3 Principle A portion of the sample is extracted with hot, dilute hydrochloric acid after wetting of the solid mineral fuel with alcohol. All forms of sodium, potassium, magnesium, calcium, iron that are exchangeable or extractable with the hydrochloric acid are extracted from

28、the coal. After removal of the residual solid mineral fuel by filtration, the concentrations of the elements in the filtrate are determined by atomic absorption spectrometry. The concentrations of the elements may also be determined by ICP-OES if the instrument has been validated for the quantificat

29、ion in an appropriate manner. 4 Reagents and materials Use analytical reagent grade chemicals. Other grades can be used, provided it is documented that the reagent is of sufficiently high purity to permit its use without adversely affecting the accuracy of the determination. SANS 1952:2009This s tan

30、dard may only be used and printed by approved subscription and freemailing clients of the SABS .ISO 1952:2008(E) 2 ISO 2008 All rights reserved4.1 Water, high-purity deionized water as defined in ISO 3696, or as defined by the equivalent national standard. 4.2 Ethanol. 4.3 Hydrochloric acid (HCl). 4

31、.4 Hydrochloric acid, concentrated, 20= 1,19 g/ml. 4.5 Hydrochloric acid solution, prepared by mixing 1 part concentrated hydrochloric acid (4.4) with 1 part deionized water (4.1). DANGER The addition of the strong acid, HCl, to water liberates a significant amount of heat and can cause a violent re

32、action. 4.6 Nitric acid (HNO3), concentrated, 20= 1,42 g/ml. 4.7 Lanthanum oxide (La2O3). 4.8 Lanthanum solution. Dissolve 23,4 g of La2O3(4.7) in 350 mL of deionized water (4.1). Slowly add 50 mL of concentrated nitric acid. Stir until solution is completely mixed, transfer to a 1 l volumetric flas

33、k, dilute to the mark with water. DANGER The addition of the strong acid, HNO3, to water liberates a significant amount of heat and can cause a violent reaction. NOTE The lanthanum solution is used as an ionization suppressant during calcium determination. It is possible to use other commonly used i

34、onization suppressants, e.g. cesium, as a alternative. 4.9 Magnesium perchlorate, anhydrous, 2,0 mm +0,7 mm, used as a desiccant. DANGER Regeneration of magnesium perchlorate by oven drying should not be attempted because of the risk of explosion. Magnesium perchlorate is a strong oxidant, and shoul

35、d be kept away from organic materials such as oils, greases and organic solvents. 4.10 Stock solutions 4.10.1 Sodium chloride (NaCl). 4.10.2 Sodium solution, 1 000 mg/L. Dissolve 2,542 g of sodium chloride (4.10.1) (previously dried at 110 C for 1 h) in 200 mL of deionized water (4.1), stir until so

36、lution is completely mixed, transfer to a 1 l volumetric flask, dilute to the mark with water. 4.10.3 Potassium chloride (KCl). 4.10.4 Potassium solution, 1 000 mg/L. Dissolve 1,907 g of potassium chloride (4.10.3) (previously dried at 110 C for 1 h) in 200 ml of water (4.1), transfer to a 1 l volum

37、etric flask, dilute to the mark with water. 4.10.5 Calcium carbonate (CaCO3). 4.10.6 Calcium carbonate solution, 1 000 mg/L. Dissolve 2,497 g of calcium carbonate (4.10.5) (previously dried at 110 C for 1 h) in a solution containing 10 ml of concentrated hydrochloric acid (4.4) and 200 ml of deioniz

38、ed water (4.1), stir until solution is SANS 1952:2009This s tandard may only be used and printed by approved subscription and freemailing clients of the SABS .ISO 1952:2008(E) ISO 2008 All rights reserved 3completely mixed. Bring to a gentle boil to remove excess carbon dioxide. Cool the solution, t

39、ransfer to a 1 l volumetric flask, dilute to the mark with water. 4.10.7 Magnesium oxide. 4.10.8 Magnesium solution, 1 000 mg/L. Place 1,658 g of magnesium oxide (4.10.7) (previously heated at 1 000 C for 1 h) in solution containing 10 ml of concentrated hydrochloric acid (4.4) and 200 ml of deioniz

40、ed water (4.1), stir until solution is completely mixed. Warm until dissolved, cool, transfer to a 1 l volumetric flask, dilute to the mark with water. 4.10.9 Iron, minimum purity 99,8 % Fe. 4.10.10 Iron solution, 1 000 mg/L. Place 1,000 g of pure iron (4.10.9) in a solution containing 20 ml of conc

41、entrated hydrochloric acid (4.4) and 20 ml of deionized water (4.1), stir until solution is completely mixed. Heat to boiling and gently simmer until dissolved. Cool, transfer to a 1 l volumetric flask, dilute to the mark with deionized water. 4.10.11 Commercial stock solutions, optional, certified

42、stock solutions with a concentration of the ion of interest of 1 000 mg/l that can be used as an alternative to preparing stock solutions. 4.11 Calibration solutions, prepared with the volumes of reagents given in Table 1. Prepare calibration solution A, by adding 40 ml of lanthanum solution (4.8) a

43、nd 32 ml of hydrochloric acid solution (4.5) to a 1 l volumetric flask. Add 1 ml of each stock solution and stir until the solution is completely mixed. Dilute to the mark with water. Prepare calibration solutions B, C, D, E and the calibration BLANK in the same way as calibration solution A using t

44、he volumes of each stock solution shown in Table 1. Additional calibration solutions within the range of those described here may be prepared in the same manner, in order to increase the number of points on the calibration graph. This can be necessary because of the wide ranges of analyte concentrat

45、ions likely to be encountered, and also because of the variations in spectrometer responses. The calibration solutions should be stored in screw-top polyethylene bottles. They should be discarded after three months. Table 1 Volumes of reagents for calibration solutions Calibration solution Concentra

46、tion of calibration solution mg/l Volume of stock solution ml Volume of lanthanum solution ml Volume of hydrochloric acid solution ml A 1 1 40 32 B 2 2 40 32 C 3 3 40 32 D 4 4 40 32 E 5 5 40 32 BLANK 0 0 40 32 4.12 Filter paper, medium-textured filter paper. SANS 1952:2009This s tandard may only be

47、used and printed by approved subscription and freemailing clients of the SABS .ISO 1952:2008(E) 4 ISO 2008 All rights reserved5 Apparatus 5.1 Dispensers for reagents, with the following capacities: 5.1.1 for ethanol 5 ml, graduated. 5.1.2 for hydrochloric acid 10 ml, graduated to fit on top of the h

48、ydrochloric acid container. 5.1.3 for lanthanum solution 10 ml. 5.2 Hotplate. 5.3 Atomic absorption spectrometer. 5.4 Desiccator, with desiccant. 5.5 Plastic bottles, polyethylene or polypropylene with screw caps, giving an airtight seal, for storage of all solutions. Condition the bottles before us

49、e, by filling with nitric acid (4.6) diluted 1 + 9. Allow to stand for at least 48 h. Rinse the bottles thoroughly with water. 5.6 Glassware, 250 ml beaker and 250 ml volumetric flask. 6 Preparation of the test sample The sample shall be the general test sample prepared in accordance with ISO 13909-4 or ISO 5069-2. 7 Procedure 7.1 Preparation of test portion Weigh approximately 1,5 g of the test sample to the nearest 2 mg into a 250 mL glass beaker. Concurrently, determine moisture in accordance wit