BS 6043-2 3-1997 Methods of sampling and test for carbonaceous materials used in aluminium manufacture - Electrode coke - Determination of trace elements in green and calcined coke.pdf

1、BRITISH STANDARD BS6043-2.3: 1997 ISO8658:1997 Methods of sampling and test for carbonaceous materials used in aluminium manufacture Part 2: Electrode coke Section2.3 Determination of trace elements in green and calcined coke by flame atomic absorption spectroscopy ICS71.100.10; 75.160.10BS6043-2.3:

2、1997 This British Standard, having been prepared under the directionof the Sector Board forMaterials and Chemicals, waspublished under the authorityof the Standards Boardand comes into effect on 15September1997 BSI09-1999 ISBN 0 580 28009 8 Amendments issued since publication Amd. No. Date CommentsB

3、S6043-2.3:1997 BSI 09-1999 i Contents Page National foreword ii Foreword iii Text of ISO8658 1BS6043-2.3:1997 ii BSI 09-1999 National foreword This British Standard is a revision of BS6043-2.3 and is the UK implementation of ISO8658:1997. It supersedes the1989 edition which is withdrawn. The UK part

4、icipation in its preparation was entrusted to Technical Committee CII/24, Raw materials for the aluminium industry, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for

5、 change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Part2 of BS6043 provides methods of test for electrode coke as follow

6、s: Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards El

7、ectronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. SectionSubject 2.1 Sa

8、mpling ISO6375 2.2 Ash content of green and calcined cokes ISO8005 2.3 Ash analysis by flame atomic absorption spectroscopy ISO8658 2.4 Ash analysis by X-ray fluorescence spectroscopy ISO12980 a 2.5 Apparent density and porosity a 2.6 Density (xylene method) ISO8004 2.7 Oil content (gravimetric meth

9、od) ISO6997 2.8 Oil content (extraction method) ISO8723 2.9 Sieve analysis a 2.10 Electrical resistivity of calcined coke granules ISO10143 2.11 Volatile matter content ISO9406 2.12 Particle size distribution of fine coke (laser diffraction method) No equivalent International Standard 2.13 Determina

10、tion of tapped bulk density of green and calcined coke ISO10236 2.14 Determination of bulk density after vibration a 2.15 Determination of grain stability of calcined coke using alaboratory vibration mill ISO10142 a In preparation Summary of pages This document comprises a front cover, an inside fro

11、nt cover, pagesi andii, theISO title page, pagesii toiv, pages1 to6 andabackcover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS 6043-2.3:1997 ii BSI 09-1999 Contents Page Forew

12、ord iii 1 Scope 1 2 Normative references 1 3 Principle 1 4 Reagents 1 5 Apparatus 3 6 Sampling 3 7 Procedure 3 8 Calculation and expression of results 6 9 Precision 6 10 Test report 6 Table 1 Composition of calibration solutions A 4 Table 2 Concentrations of elements in calibration solutions A 4 Tab

13、le 3 Composition of calibration solutions B 4 Table 4 Conditions for spectrophotometric measurements 5 Descriptors: Extractive metallurgy, aluminium, carbon electrodes, carbonaceous materials, coke, ashes, chemical analysis, determination of content, trace elements, flame photometric analysis, atomi

14、c absorption spectrometric method.BS 6043-2.3:1997 BSI 09-1999 iii Foreword 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

15、 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 non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with

16、 the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. 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 least75% of the

17、member bodies casting a vote. International Standard ISO8658 was prepared by the British Standards Institution (BSI) (as BS6043-2.3:1989) and was adopted, under a special “fast-track procedure”, by Technical Committee ISO/TC47, Chemistry in parallel with its approval by the ISO member bodies.iv blan

18、kBS 6043-2.3:1997 BSI 09-1999 1 1 Scope This International Standard describes a method for the determination of trace elements in green and calcined coke with an ash content of not greater than1%(m/m) and with individual concentrations not greater than the following: NOTEA method for the determinati

19、on of ash of cokes is given in ISO8005:1984, Carbonaceous materials used in the production of aluminium Green and calcined coke Determination of ash. However, it is essential that the ash produced by that method not be used in the procedure of this International Standard because of the risk of conta

20、mination by trace elements. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. Allstandards are subject to revision, and parties

21、to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO385-1:1984, Laboratory glassware Burettes P

22、art1: General requirements. ISO835-1:1981, Laboratory glassware Graduated pipettes Part1: General requirements. ISO1042:1983, Laboratory glassware One-mark volumetric flasks. ISO3696:1987, Water for laboratory use Specification and test methods. ISO6375:1980, Carbonaceous materials for the productio

23、n of aluminium Coke for electrodes Sampling. 3 Principle A test portion sample is heated in a muffle furnace at700 C for10h and the ash produced is fused with a mixture of sodium carbonate and orthoboric acid. The melt is dissolved in dilute hydrochloric acid and the trace metal content is analysed

24、by flame atomic absorption spectrometry. 4 Reagents Unless otherwise stated, use only reagents of recognized analytical grade and water complying with grade2 of ISO3696. 4.1 Sodium carbonate, anhydrous. 4.2 Orthoboric acid 4.3 Hydrochloric acid, concentrated, c(HCl)=36%(m/m), =1,16g/ml. 4.4 Lanthanu

25、m chloride solution, 100mg La/ml, atomic absorption grade, c(LaCl 3 7H 2 O)=267g/l. 4.5 Standard calcium solution, 0,1mg/Cal. Dry calcium carbonate (reagent grade) at110 C 5 C for1h and cool in a desiccator containing diphosphorus pentoxide. Weigh2,497g 0,001g into a250ml beaker. Add50ml of water, t

26、hen, a little at a time,50ml of concentrated hydrochloric acid(4.3). When the solution is clear, transfer quantitatively to a1000ml one-mark volumetric flask(5.6). Dilute to the mark with water and mix. Store in a polythene bottle. Using a one-mark pipette(5.8), transfer10ml of this solution to a100

27、ml one-mark volumetric flask(5.6). Add approximately20ml of water and5ml of hydrochloric acid(4.3). Dilute to the mark with water and mix. 4.6 Standard chromium solution, 0,1mg Cr/ml. Wash, by decantation, approximately1,2g of chromium metal of minimum purity99,9%(m/m) with dilute hydrochloric acidc

28、(HCl)=1mol/l, then wash with water and dry in an air-circulating oven maintained at110 C 5 C for10min. Weigh1g 0,001gof the dried chromium into a250ml beaker containing about50ml of water. Slowly add50ml of concentrated hydrochloric acid(4.3). After dissolution, transfer quantitatively to a1000ml on

29、e-mark volumetric flask(5.6). Dilute to the mark with water and mix. Store in a polythene bottle. Using a one-mark pipette(5.8), transfer10ml of this solution to a100ml one-mark volumetric flask(5.6). Add approximately20ml of water and5ml of concentrated hydrochloric acid. Dilute to the mark with wa

30、ter and mix. Store in a polythene bottle. Calcium 0,025%(m/m) Chromium 0,005%(m/m) Copper 0,025%(m/m) Iron 0,030%(m/m) Lead 0,010%(m/m) Magnesium 0,010%(m/m) Manganese 0,001% (m/m) Nickel 0,050%(m/m) Silicon 0,100%(m/m) Vanadium 0,100%(m/m) Zinc 0,004%(m/m)BS 6043-2.3:1997 2 BSI 09-1999 4.7 Standard

31、 copper solution, 1mg Cu/ml. Wash, by decantation, approximately1,2g of copper metal of minimum purity99,9%(m/m) with dilute nitric acidc(HNO 3 )=2mol/l, then wash with water and dry in an air-circulating oven maintained at110 C 5 C for10min. Weigh1g 0,001gof the dried copper into a250ml beaker cont

32、aining about25ml of water. Slowly add35ml of concentrated nitric acid( =1,42g/ml). After dissolution, transfer quantitatively to a1000ml one-mark volumetric flask(5.6). Dilute to the mark with water and mix. Store in a polythene bottle. 4.8 Standard iron solution, 1mg Fe/ml. Weigh1g 0,001g of iron o

33、f minimum purity99,9%(m/m) into a250ml beaker and add25ml of water. Carefully add50ml of concentrated hydrochloric acid(4.3). After dissolution, transfer quantitatively to a1000ml one-mark volumetric flask(5.6). Dilute to the mark with water and mix. Store in a polythene bottle. 4.9 Standard magnesi

34、um solution, 0,01mg Mg/ml. Weigh1g 0,001g of magnesium of minimum purity99,9%(m/m) into a250ml beaker and add50ml of water. Carefully add50ml of concentrated hydrochloric acid(4.3). After dissolution, transfer quantitatively to a1000ml one-mark volumetric flask(5.6). Dilute to the mark with water an

35、d mix. Store in a polythene bottle. Using a one-mark pipette(5.8), transfer10ml of this solution to a1000ml one-mark volumetric flask(5.6). Add approximately50ml of water and45ml of concentrated hydrochloric acid(4.3). Dilute to the mark with water and mix. 4.10 Standard manganese solution, 0,1mg Mn

36、/ml. Wash, by decantation, approximately1,2g of manganese metal of minimum purity99,9%(m/m) with dilute nitric acidc(HNO 3 )=2mol/l, then wash with water and dry in an air-circulating oven maintained at110 C 5 C for10min. Weigh1g 0,001gof the dried manganese into a250ml beaker containing about25ml o

37、f water. Slowly add35ml of concentrated nitric acid( =1,42g/ml). After dissolution, transfer quantitatively to a1000ml one-mark volumetric flask(5.6). Dilute to the mark with water and mix. Store in a polythene bottle. Using a one-mark pipette(5.8), transfer10ml of this solution to a100ml one-mark v

38、olumetric flask(5.6). Add approximately50ml of water and3ml of concentrated nitric acid( =1,42g/ml). Dilute to the mark with water and mix. 4.11 Standard nickel solution, 1mg Ni/ml. Weigh1g 0,001g of iron of minimum purity99,9%(m/m) into a250ml beaker and add25ml of water. Carefully add35ml of conce

39、ntrated nitric acid( =1,42g/ml), and heat to dissolve. After dissolution, transfer quantitatively to a1000ml one-mark volumetric flask(5.6). Dilute to the mark with water and mix. Store in a polythene bottle. 4.12 Standard lead solution,1mg Pb/ml. Weigh1g 0,001g of lead of minimum purity99,9%(m/m) i

40、nto a250ml beaker and add25ml of water. Carefully add35ml of concentrated nitric acid( =1,42g/ml), and heat to dissolve. After dissolution, transfer quantitatively to a1000ml one-mark volumetric flask(5.6). Dilute to the mark with water and mix. Store in a polythene bottle. 4.13 Standard silicon sol

41、ution, 1mg Si/ml. Into a platinum dish or large platinum crucible, weigh2,139g of silica of minimum purity99,9%(m/m) and6g of anhydrous sodium carbonate(4.1), and mix well with a platinum spatula. Carefully fuse the mixture over a flame until a transparent melt is obtained. Allow to cool, add warm w

42、ater, heat gently until completely dissolved and transfer quantitatively to a400ml PTFE beaker. Allow to cool. Dilute the solution to about300ml with water, transfer quantitatively to a1000ml one-mark volumetric flask(5.6), dilute to the mark with water and mix. Immediately transfer this solution to

43、 a screw-cap polythene bottle. Discard this solution after one month. 4.14 Standard vanadium solution,1mg V/ml. Heat vanadium(V) oxide of minimum purity99,9%(m/m) in a covered platinum crucible(5.9) at500 C 10 C for30min and cool in a desiccator. Weigh1,785g of the dried material and dissolve in a s

44、light excess of sodium hydroxide solutionc(NaOH)=1mol/l in a PTFE beaker, then dilute to about250ml with water. Carefully add, a little at a time, concentrated sulfuric acid c(0,5H 2 SO 4 )=9mol/l, until the solution is just acid to litmus paper, then add a further5ml. Cool to room temperature, tran

45、sfer to a1000ml one-mark volumetric flask(5.6), dilute to the mark with water and mix.BS 6043-2.3:1997 BSI 09-1999 3 4.15 Standard zinc solution, 0,1mg Zn/ml. Weigh1g 0,001g of zinc of minimum purity99,9%(m/m) into a100ml beaker and add25ml of water. Carefully add25ml of concentrated hydrochloric ac

46、id(4.3) and heat to dissolve. After dissolution, transfer the solution quantitatively to a1000ml one-mark volumetric flask(5.6), dilute to the mark with water and mix. Using a one-mark pipette(5.8), transfer10ml of this solution to a100ml one-mark volumetric flask(5.6), add about20ml water and5ml of

47、 concentrated hydrochloric acid(4.3). Dilute to the mark with water and mix. 5 Apparatus Ordinary laboratory apparatus and the following are required. All glass and plastics apparatus shall be cleaned before use by washing in concentrated hydrochloric acid(4.3) and rinsing with water (seeclause4, in

48、troductory paragraph). 5.1 Spectrometer, atomic absorption type, fitted with a burner fed from cylinders of acetylene, dinitrogen oxide (nitrous oxide) and compressed air. The emission wavelength and slit width shall be variable. 5.2 Electric muffle furnace, capable of being maintained at700 C 10 C.

49、 5.3 Meker burner 5.4 Sieve, with a polythene frame and polyester mesh having an aperture size in the range5004m to10004m. 5.5 Pestle and mortar, made from sintered alumina or from ferrous metal with a tungsten carbide liner. NOTEPestles and mortars made from other materials are not suitable. 5.6 One-mark volumetric flasks, complying with ISO1042, class A. 5.7 Burettes, 25ml, complying with ISO385-1, classA. 5.8 One-mark pipettes, complying with ISO835-1, class A. 5.9 Platinum cru