1、BRITISH STANDARD BS 6463-102: 2001 Quicklime, hydrated lime and natural calcium carbonate Part 102: Methods for chemical analysis ICS 91.100.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS 6463-102:2001 This British Standard, having been prepared under the direction of th
2、e Sector Policy and Strategy Committee for Building and Civil Engineering, was published under the authority of the Sector Policy and Strategy Committee on 6 November 2001 BSI 6 November 2001 First published as BS 6463-2, February 1984 Second edition as BS 6463-102, 6 November 2001 The following BSI
3、 references relate to work on this British Standard: Committee reference B/516/11 Draft for comment 99/105742 DC ISBN 0 580 33315 9 Committees responsible for this British Standard The preparation of this British Standard was entrusted by Technical Committee B/516, Cement and lime, to Subcommittee B
4、/516/11, Lime, upon which the following bodies were represented: Autoclaved Aerated Concrete Products Association British Lime Association Building Limes Forum Department of the Environment, Transport and the Regions Building Research Establishment English Heritage Mortar Industry Association Quarry
5、 Products Association Co-opted members The following bodies from the Technical Committee were also involved in the preparation of this standard: British Cement Association British Precast Concrete Federation Ltd. Cement Admixtures Association Cementitious Slag Makers Association County Surveyors Soc
6、iety Department of the Environment, Transport and the Regions Highways Agency Environment Agency Society of Chemical Industry UK Quality Ash Association Amendments issued since publication Amd. No. Date CommentsBS 6463-102:2001 BSI 6 November 2001 i Contents Page Committees responsible Inside front
7、cover Foreword ii 1S c o p e 1 2 Normative references 1 3 General requirements for testing 1 4 Determination of major and minor constituents by classical methods 2 5 Determination of minor constituents by flame atomic absorption spectroscopy 14 Bibliography 21 Figure 1 Typical apparatus for determin
8、ation of free water in hydrated lime and lime putty 8 Figure 2 Typical apparatus for determination of carbon dioxide 12 Figure 3 Determinations using atomic absorption spectrometry 14 Table 1 Densities of concentrated liquid reagents 2 Table 2 Elements, preferred wavelengths and flame types 15 Table
9、 3 Minor element concentrations in standard extracts 17 Table 4 Trace element concentrations in standard extracts 18BS 6463-102:2001 ii BSI 6 November 2001 Foreword This part of BS 6463 has been prepared by Subcommittee B/516/11, Lime, under the direction of Technical Committee B/516, Cement and lim
10、e. It supersedes BS 6463-2:1984 which is withdrawn. BS 6463-2:1984 brought together standard methods of chemical analysis for quicklime, hydrated lime and natural calcium carbonate including those for use in connection with water treatment, agriculture, steel making and chemical processing. In that
11、edition, atomic absorption methods were permitted. Since 1984 the use of atomic spectrometry has been widely used in this field of activity. These methods require special attention to calibration using reference materials. This edition describes alternative analytical methods for several elements. W
12、here available and appropriate, atomic spectrometry using atomic absorption (AAS) is recommended, although classical methods are still used by many laboratories for the determination of certain analytes and parameters. Repeatability and reproducibility for the test methods are not yet available. How
13、ever, when the necessary testing has been done, this standard will be updated accordingly. Other atomic absorption spectrometric (AAS) methods are available in BS EN 12485, and include determinations of antimony, arsenic, mercury and selenium. These methods are to be preferred over the classical met
14、hods and it is recommended that they are adopted in specifications as the reference methods. NOTE There are other atomic spectrometric methods that can give the sensitivity, precision and accuracy required by this part of BS 6463, the results of which can be calibrated against the methods described
15、in this part of BS 6463. However, if a standard specifies a reference to BS 6463-102, only methods actually given in this part of BS 6463 can be used in order to claim compliance with that standard. A number of classical chemical methods that were given in BS 6463-2:1984 have now been incorporated i
16、nto other standards, and are no longer included in this part of BS 6463. These methods, and the standards in which they are now given, are for: available lime (BS EN 459-2); silicon (BS EN 196-2); iron (BS EN 196-2); calcium (BS EN 12485); magnesium (BS EN 12485); water soluble calcium oxide and cal
17、cium hydroxide (BS EN 12485); water insoluble constituents (BS EN 12485).BS 6463-102:2001 BSI 6 November 2001 iii This revision of BS 6463 is published in three parts, as follows: Part 101: Methods for preparing samples for testing; Part 102: Methods for chemical analysis; Part 103: Methods for phys
18、ical testing. Part 101 gives methods for sampling powdered, granular and lump quicklime and natural calcium carbonate, and of powdered hydrated lime, milk of lime and lime putty. Part 103 gives the physical tests for quicklime, hydrated lime, lime putty and natural calcium carbonate, of which the te
19、sts for quicklime, hydrated lime and lime putty were previously included in BS 6463-3 and BS 6463-4. A British Standard does not purport to include all necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard doe
20、s not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i to iv, pages 1 to 21 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.iv blankBS 6463-102:20
21、01 BSI 6 November 2001 1 1 Scope This part of BS 6463 describes methods for the chemical analysis of quicklime, hydrated lime and natural calcium carbonate. It describes both classical methods and methods which use atomic absorption spectrometry (AAS). It gives classical chemical methods for: fluori
22、ne, matter insoluble in acetic acid, matter insoluble in hydrochloric acid; loss on ignition, neutralizing value; free water in hydrated lime and also in lime putty; total sulfur; carbon dioxide in carbonate. It gives flame atomic absorption spectrometric (AAS) methods for aluminium, cadmium, chromi
23、um, cobalt, copper, iron, lead, magnesium, manganese, nickel, silicon, silver and zinc. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of this British Standard. For dated references, subsequent ame
24、ndments to, or revisions of, any of these publications do not apply. For undated references, the latest edition of the publication referred to applies. BS 1752:1983, Specification for laboratory sintered or fritted filters including porosity grading. BS 5898:1980, Specification for principles of des
25、ign and construction of volumetric glassware for laboratory use. BS 6463-101:1996, Quicklime, hydrated lime and natural calcium carbonate Part 101: Methods for preparing samples for testing. BS EN 12485, Chemicals used for treatment of water intended for human consumption Calcium carbonate, high-cal
26、cium lime and half-burnt dolomite Test methods. BS EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods. BS ISO 3534-1:1993, Statistics Vocabulary and symbols Part 1: Probability and general statistical terms. 3 General requirements for testing 3.1 Number of tests For
27、 each of the determinations in clauses 4 and 5, carry out two tests. 3.2 Reagents Water shall conform to grade 2 of BS EN ISO 3696. All reagents shall be of an analytical grade suitable for the method being used. For instrumental analysis, the instructions of the equipment manufacturer shall be obse
28、rved. The content of the elements to be determined in the water or reagents used shall be negligible compared with the lowest concentration to be determined. If commercially available AAS solutions are used as stock solutions, they shall be prepared for the purposes of analysis in accordance with th
29、e manufacturers instructions. The concentrated liquid reagents used in this standard shall have the densities shown in Table 1.BS 6463-102:2001 2 BSI 6 November 2001 Table 1 Densities of concentrated liquid reagents NOTE The degree of dilution is always given as a volumetric sum, e.g. “dilute hydroc
30、hloric acid 1 + 2” means that 1 volume of concentrated hydrochloric acid is to be mixed with 2 volumes of water. 3.3 Volumetric glassware Volumetric glassware shall be of class B as specified in BS 5898. 3.4 Preparation of the sample Prepare the laboratory sample as described in BS 6463-101. Carry o
31、ut all operations as quickly as possible to ensure that the sample is exposed to ambient air only for the minimum time that is necessary. Store the sample in an air-tight container of such a volume that the sample fills the container as completely as possible. 3.5 Expression of results Express the r
32、esults as the mean of two determinations. Express results of value not less than 1.00 % to three significant figures. Express results of value less than 1.00 % to two significant figures. If the value of the result is less than 0.10 % express it to two significant figures where feasible. 4 Determina
33、tion of major and minor constituents by classical methods 4.1 Determination of hydrochloric acid extractable fluoride 4.1.1 Principle The sample is stirred with concentrated hydrochloric acid and the extracted fluorine is determined using a specific fluoride ion electrode which develops a potential
34、proportional to the logarithm of the fluoride ion concentration in solution. The method is applicable to quicklimes and hydrated limes, with fluorine contents in the range 20 mg/kg to 500 mg/kg. It is also applicable to natural calcium carbonates which are used for the neutralization of moderately a
35、cidic solutions (pH 1). NOTE The extractable fluoride content of a natural calcium carbonate should not be used to predict the levels of extractable fluoride in quicklimes and hydrated limes. This is due partly to the effects of the calcination and hydration reactions and partly to the volatility of
36、 fluorides at elevated temperatures. 4.1.2 Reagents 4.1.2.1 Sodium fluoride, NaF, dried at (105 5) C for 1 h. 4.1.2.2 Fluoride, standard stock solution, with a concentration of fluoride ions of 500 g/ml. Dissolve (1.105 0.005) g of sodium fluoride (4.1.2.1) in water, make up to 1 000 ml in a volumet
37、ric flask and mix thoroughly. Store in a suitable container and under suitable conditions for up to 14 days if necessary (see note). NOTE All fluoride solutions may be kept for limited periods providing they are placed in a cool dark cupboard in stoppered containers made of a material which has been
38、 shown not to interfere with the determination of fluorine. Laboratory grade polyethylene or polypropylene is usually suitable. Reagent Density ( ) at 20 C g/ml Acetic acid 1.05 to 1.06 Hydrochloric acid 1.16 to 1.19 Industrial methylated spirit 0.79 Nitric acid 1.40 to 1.42 Orthophosphoric acid 1.7
39、0 to 1.75 Sulfuric acid 1.84BS 6463-102:2001 BSI 6 November 2001 3 4.1.2.3 Fluoride, dilute solution, with a concentration of fluoride ions of 50 g/ml. Pipette 50 ml of the standard stock fluoride solution (4.1.2.2) into a 500 ml volumetric flask. Make up to the mark with water and mix. NOTE This so
40、lution can be kept for up to 14 days if stored as described (see note to 4.1.2.2). 4.1.2.4 Fluoride, dilute solution, with a concentration of fluoride ions of 5 g/ml. Pipette 50 ml of fluoride solution (4.1.2.3) into a 500 ml volumetric flask. Make up to the mark with water and mix. NOTE This soluti
41、on can be kept for up to 14 days if stored as described (see note to 4.1.2.2). 4.1.2.5 Reference standard calcium carbonate, with less than 1 mg/kg of hydrochloric acid extractable fluorine. 4.1.2.6 Trisodium citrate dihydrate. 4.1.2.7 Trisodium citrate solution. Dissolve (147.0 0.1) g of trisodium
42、citrate dihydrate (4.1.2.6) in water and dilute to 1 l. 4.1.2.8 Hydrochloric acid, 1 + 19. 4.1.2.9 Fluoride standard solution, 10 g in 80 ml. Pipette 2 ml of fluoride solution (4.1.2.4) into a polyethylene beaker. Add (0.20 0.01) g of calcium carbonate (4.1.2.5), 18 ml of distilled water, 40 ml of t
43、risodium citrate solution (4.1.2.7) and 20 ml of hydrochloric acid 1 + 19 (4.1.2.8). Add a magnetic follower and stir. NOTE This solution can be kept for up to 48 h, if stored as described (see note to 4.1.2.2). 4.1.2.10 Fluoride standard solution, 100 g in 80 ml. Pipette 20 ml of fluoride solution
44、(4.1.2.4) into a polyethylene beaker. Add (0.20 0.01) g of calcium carbonate (4.1.2.5), 40 ml of trisodium citrate solution (4.1.2.7) and 20 ml of hydrochloric acid 1 + 19 (4.1.2.8). Add a magnetic follower and stir. NOTE This solution can be kept for up to 48 h, if stored as described (see note to
45、4.1.2.2). 4.1.3 Apparatus 4.1.3.1 Plastics beaker. 4.1.3.2 Magnetic follower. 4.1.3.3 Millivoltmeter, with an expandable scale and a specific ion electrode for fluorine, containing a lanthanum fluoride crystal across which a potential develops proportional to the fluoride ion concentration in soluti
46、on. This potential is measured against a calomel reference electrode. 4.1.4 Preparation of sample solution Accurately weigh (0.200 0.005) g of sample into a plastics beaker (4.1.3.1). Add 25 ml of hydrochloric acid 1 + 19 (4.1.2.8) and a magnetic follower (4.1.3.2). Stir for 15 min and add 15 ml of
47、distilled water and 40 ml of trisodium citrate solution (4.1.2.7). BS 6463-102:2001 4 BSI 6 November 2001 4.1.5 Procedure Operate the millivoltmeter (4.1.3.3), the specific fluoride ion electrode and the calomel reference electrode as described in the manufacturers instructions. Allow sample solutio
48、ns, reagents and apparatus to equilibrate at room temperature (1 C) before reading. NOTE 1 When taking readings, it is advisable to transfer solutions into small beakers (made of a material which has been shown not to interfere with the determination of fluorine) and to agitate gently, without vorte
49、x, using a magnetic stirrer. NOTE 2 The determination of fluorine in the sample should be completed within 0.5 h of preparing the sample solution (4.1.4). NOTE 3 When a series of measurements has been completed, rinse the electrodes and store them as recommended by the manufacturer. If the meter has slope and gain controls, calibrate the instrument and electrode, using the fluoride solutions as follows. a) Rinse the electrodes in distilled water and dip them into the first fluoride st
