1、BRITISH STANDARD BS ISO 9285:1997 Abrasive grains and crude Chemical analysis of fused aluminium oxide ICS 25.100.70BSISO9285:1997 This British Standard, having been prepared under the directionof the Engineering SectorBoard, was published underthe authority of the Standards Board and comes intoeffe
2、ct on 15 June 1997 BSI 09-1999 ISBN 0 580 27565 5 National foreword This British Standard reproduces verbatim ISO9285:1997 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee MTE/13, Grinding wheels, abrasive tools, paper and cl
3、oths and powders, 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 change, and keep the UKinterests informed; monitor related international and European development
4、s and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue u
5、nder the section entitled “International Standards Correspondence Index”, or using the “Find” facility of the BSI Standards Electronic 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 ap
6、plication. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theISO title page, pages ii to iv, pages 1 to 12 and a back cover. This standard has been updated (s
7、ee copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBSISO9285:1997 BSI 09-1999 i Contents Page National foreword Inside front cover Foreword iii Text of ISO 928
8、5 1ii blankBSISO9285:1997 ii BSI 09-1999 Contents Page Foreword iii 1 Scope 1 2 Normative references 1 3 Reagents 1 4 Apparatus 2 5 Procedure 2 6 Gain or loss on ignition 2 7 Determination of silicon dioxide 3 8 Separation of iron, titanium, magnesium and calcium from aluminium 5 9 Iron(III) oxide d
9、etermination 5 10 Titanium dioxide colorimetric determination 6 11 Calcium oxide gravimetric determination 7 12 Magnesium oxide gravimetric determination 7 13 Zirconium oxide gravimetric determination 7 14 Aluminium oxide 8 15 Analysis by atomic absorption spectrometry 9 16 Test report 11 Annex A (i
10、nformative) Other methods of analysis 12 Table 1 4 Descriptors: Tools, abrasives, metallic abrasives, aluminium oxide, chemical analysis, determination of content.BSISO9285:1997 BSI 09-1999 iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national st
11、andards 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 right to be represented on that committee. International o
12、rganizations, 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. Draft International Standards adopted by the technical committees ar
13、e circulated to the member bodies for voting. Publication as an InternationalStandard requires approval by at least75% of the member bodies casting a vote. International Standard ISO9285 was prepared by Technical Committee ISO/TC 29, Small tools, Subcommittee SC5, Grinding wheels and abrasives. Anne
14、x A of this International Standard is for information only.iv blankBSISO9285:1997 BSI 09-1999 1 1 Scope This International Standard deals with the chemical analysis of abrasive grains or crude based on fused aluminium oxide. It applies to commercially available products but not necessarily to produc
15、ts which have been altered by use. It includes the following determinations: Loss on ignition Silicon dioxide Iron oxide Titanium dioxide Calcium oxide Magnesium oxide Zirconium oxide Aluminium oxide Analysis by atomic absorption spectrometry 2 Normative references The following standards contain pr
16、ovisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the
17、 possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 6353-1:1982, Reagents for chemical analysis Part 1: General test methods. ISO 6353-2:1983, Reagents for chemical analysis Part
18、 2: Specifications First series. ISO 6353-2-Add.2:1986, Addendum 2 to ISO 6353-2:1983. ISO 6353-3:1987, Reagents for chemical analysis Part 3: Specifications Second series. ISO 9138:1993, Abrasive grains Sampling and splitting. 3 Reagents 3.1 General Unless otherwise indicated, it is intended that a
19、ll reagents shall conform to the specifications given in ISO6353-1, ISO6353-2 and ISO6353-3. Other grades may be used, provided it be first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. Unless otherwise indicated, r
20、eferences to water shall be understood to mean distilled water. Paragraphs3.2 to3.21 include those reagents common to two or more analytical procedures. Other reagents will be found in the section which deals with the particular method in which they are used. 3.2 Concentrated acids and ammonium hydr
21、oxide Concentrated acids and ammonium hydroxide having the following approximate volumetric masses , in grams per millilitre or concentrations, in percentage by mass will be required: 3.3 Dilute acids and ammonium hydroxide The dilute acids and ammonium hydroxide referred to have varying concentrati
22、ons. They shall be made up by mixing proportional volumes of the concentrated reagent and water. The dilute sulphuric acid mixtures shall be made up by slowly adding the acid to the water and stirring continuously. These dilutions are designated in the test procedures as (1 + 5), (1 + 8), etc., exce
23、pt for the very dilute solutions which are characterized by the percentage of reagent added. The designations in parentheses indicate the volume of the reagent added to the volume of water; for example H 2 SO 4(1 + 9) contains 10% (V/V) of H 2 SO 4( = 1,84 g/ml). 3.4 Ammonium acetate, 300 g/l soluti
24、on. Dissolve300 g of NH 4 C 2 H 3 O 2in water. Fill to the1 l mark with water. 3.5 Ammonium chloride (NH 4 Cl). 3.6 Ammonium oxalate(NH 4 ) 2 C 2 O 4 , saturated solution. 3.7 Diammonium hydrophosphate, 100 g/l solution. Dissolve10 g of (NH 4 ) 2 HPO 4in100 ml of water. 3.8 Barium diphenylamine sulp
25、honate, 2 g/l solution. Dissolve0,5 g of the salt in250 ml of H 2 SO 4 . 3.9 Hydrogen peroxide, 30 g/l solution. 3.10 Hydrogen sulfide gas(H 2 S) 3.11 Hydroxylamine hydrochloride or hydroxylammonium chloride, 100 g/l solution. Dissolve50 g of ClNH 3 OH in500 ml of water. Filter if necessary. 3.12 Me
26、rcuric chloride (HgCl 2 ), saturated solution. Hydrochloric acid (HCl): = 1,18 g/ml Nitric acid (HNO 3 ): = 1,42 g/ml Sulphuric acid (H 2 SO 4 ): = 1,84 g/ml Hydrofluoric acid (HF): 40% (m/m) Phosphoric acid (H 3 PO 4 ): 85% (m/m) Ammonium hydroxide (NH 4 OH): = 0,90 g/mlBSISO9285:1997 2 BSI 09-1999
27、 3.13 Methyl red indicator, 1 g/l solution. Dissolve0,1 g methyl red in100 ml of methanol. 3.14 o-Phenanthroline (1,10-phenanthroline), 1 g/l solution. Dissolve1 g o-phenanthroline monohydrate in15ml of ethanol (95%). Dilute to1 l with water. 3.15 Potassium dichromate (K2Cr 2 O 7 ), 0,01 mol/l solut
28、ion. Dissolve2,9424 g of K 2 Cr 2 O 7in water. Make up the solution to the1 l mark of a volumetric flask. Standardize the solution against a sample with a certified iron content. 3.16 Potassium permanganate (KMnO 4 ), standardized solution, c (1/5 KMnO 4 ) = 0,01 mol/l. Dissolve1,5800g of KMnO 4in50
29、0 ml of water. Allow to stand for1 d-2 d. Filter through an asbestos mat and dilute to the1 l mark of a volumetric flask with water. Standardize against sodium oxalate. 3.17 Potassium permanganate (KMnO 4 ), 50 g/l solution. Dissolve5 g KMnO 4in100 ml of water. 3.18 Potassium pyrosulfate (K 2 S 2 O
30、7 ). 3.19 Anhydrous sodium carbonate (Na 2 CO 3 ). 3.20 Sodium tetraborate (Na 2 B 4 O 7 ). 3.21 Stannous chloride (SnCl 2 ), 50 g/l solution. Dissolve50 g of SnCl 2in100 ml of HCl. Make up to the1 l mark of a volumetric flask with water. Store the solution with metallic tin in the bottle. 4 Apparat
31、us 4.1 Small jaw or roll crusher with hardened steel faces 4.2 Tool steel mortar In situations where it is vital that iron contamination be eliminated, the crushing should be carried out in a tungsten carbide mortar. 4.3 Sieve, with mesh of 150 4m aperture size. 4.4 Sieve, with 2 mm aperture size. 4
32、.5 Platinum crucible, weighed, 30 ml, with lid. 5 Procedure 5.1 Preparation of samples for analysis 5.1.1 Abrasive crude The sample, carefully obtained by means of an approved sampling method, is crushed in a small jaw or roll type crusher with hardened steel faces until it can be passed through a s
33、ieve having a mesh size of2 mm; it is then mixed and divided by coning and quartering until approximately500 g are obtained. The500 g sample is in turn mixed and divided by coning and quartering until a sample weighing between10 g and20 g is obtained. This20g sample is then pulverized in a tool stee
34、l mortar until, unless otherwise specified, it completely passes through a sieve having a mesh size of1504m; it is then mixed thoroughly and placed in a container which will ensure freedom from contamination. Precautions shall be taken in order to prevent the sample being contaminated by steel parti
35、cles from the sampling and crushing equipment. Magnetic separation of the sample shall be carried out in order to remove this iron contamination. 5.1.2 Abrasive grain The sample, carefully obtained by one of the approved methods, is thoroughly mixed and divided by coning and quartering until10 g to2
36、0 g are obtained. It is then crushed until, unless otherwise specified, it completely passes through a sieve having a mesh size of150 4m; it is then carefully mixed and placed in a container which will ensure freedom from contamination (see ISO9138). 5.2 Blank determination Blank determination on th
37、e reagents shall be made for each determination and the necessary corrections applied in each case. 6 Gain or loss on ignition 6.1 Procedure Weigh a1 g sample to within0,0001g and place it in a weighed platinum crucible which has been previously heated to1100 C. Record the mass of the sample and the
38、 crucible. Heat the crucible plus sample at1100 C until a constant mass is obtained. Cool the crucible in a desiccator and weigh the crucible plus sample. 6.2 Expression of results Loss on ignition, expressed as a percentage, is given by the formula m 1 m 2 () m 0 - 100BSISO9285:1997 BSI 09-1999 3 w
39、here NOTEIf the sample gains in mass, report as a gain, and use the formula: 7 Determination of silicon dioxide 7.1 Gravimetric method 7.1.1 Apparatus 7.1.1.1 Platinium crucible, with lid. 7.1.1.2 Beaker, 400 ml. 7.1.1.3 Filter paper, medium grade. 7.1.1.4 Desiccator 7.1.2 Procedure Weigh a1 g sampl
40、e to within0,0001g and place in a platinum crucible containing3g of Na 2 CO 3and3g of Na 2 B 4 O 7 . Mix the sample and fuse mixture thoroughly. Cover the crucible with a platinum lid and fuse the mixture at1000 C until the entire sample is in solution. Rotate the crucible during cooling to deposit
41、the melt in a thin layer on the side of the crucible. Place crucible and lid in a400ml beaker. Dissolve the fusion in100ml of H 2 SO 4(1 + 4). When fully dissolved, thoroughly wash crucible and lid, adding washes to main solution. Carefully evaporate the solution to fumes of SO 3and leave to cool. A
42、dd100ml of water and boil to dissolve salts. Filter using a medium grade ashless filter paper. Wash the paper and precipitate with hot H 2 SO 4(2 + 98). Retain the filtrate for the Fe 2 O 3 , TiO 2 , CaO and MgO determinations. Transfer the filter paper to a platinum crucible and char at low heat. W
43、hen fully charred ignite at1000 C. Leave the crucible to cool in a desiccator and weigh to constant mass. Moisten the solid mass with1or2drops of water, add10ml of HF acid and2or3drops ofH 2 SO 4 (1 + 1). Slowly evaporate to dryness then ignite at1000 C. Cool the crucible in a desiccator and weigh t
44、o constant mass. Evaluate the loss in mass due to HF, H 2 SO 4treatment. 7.1.3 Expression of results Silicon dioxide content, expressed as a percentage by mass, is given by the equation where 7.2 Colorimetric method 7.2.1 Reagents 7.2.1.1 Molybdic acid solution Dissolve100g of ammonium molybdate 82%
45、 (m/m) of MoO 3 in approximately600ml of water. Add70ml of H 2 SO 4( = 1,84 g/ml). Filter the solution. Dilute to1 l with water in a volumetric flask. 7.2.1.2 Reducing solution Dissolve25g of sodium hydrogen sulphite (NaHSO 3 ) in25ml of water. Dissolve2g of sodium sulphite (Na 2 SO 3 ) and0,4g of1-
46、amino-2-naphthol-4-sulphonic acid in25ml of water. Mix the two solutions and dilute to250ml with water in a volumetric flask. Note that this solution has a maximum shelf life of two weeks. 7.2.1.3 Silicon dioxide, standard solution corresponding to 0,1 mg SiO 2per millilitre. Melt0,100g of anhydrous
47、 SiO 2and1g of Na 2 CO 3in a platinum crucible. Cool the molten mass. Dissolve in water and make up to1000 ml in a volumetric flask. Transfer to a polyethylene bottle. 7.2.1.4 Tartaric acid, 100 g/l solution. Dissolve100g of tartaric acid in water. Dilute to1000ml in a volumetric flask. 7.2.1.5 Fusi
48、on mixture, comprising3parts Na 2 CO 3or1part B 2 O 3 . (Boric oxide is the preferred reagent. Salts containing boron have varying amounts of SiO 2giving high and frequently inconsistent blank values.) 7.2.1.6 Hydrofluoric acid, 2% (V/V) solution (forcleaning PTFE). 7.2.2 Apparatus 7.2.2.1 Platinum
49、crucible 7.2.2.2 PTFE beaker, 250 ml. 7.2.2.3 Magnetic stirrer 7.2.2.4 PTFE stirring bar 7.2.2.5 pH-meter 7.2.2.6 Volumetric flask, 100 ml. m 1 is the mass of the crucible plus sample before ignition, in grams; m 2 is the mass of crucible plus sample after ignition, in grams; m 0 is the mass of sample, in grams. m 1 is the mass loss due to the HF, H 2 SO 4treatment, in grams; m 0 is the mass of the sample, in grams.BSISO9285:1997 4 BSI 09-1999 7.2.2.7 Spectrophotometer 7.2.3 Procedur
