1、BRITISH STANDARD BS 6783-1: 1986 ISO6351:1985 Sampling and analysis of nickel, ferronickel and nickel alloys Part 1: Method for determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead and zinc in nickel by flame atomic absorption spectrometry ISO title: Nickel Determination
2、of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead and zinc contents Flame atomic absorption spectrometric method UDC 669.24+669.1524-198:543.422.062BS6783-1:1986 This British Standard, having been prepared under the directionof the Non-ferrous Metals Standards Committee, waspublishe
3、d under the authorityof the Board of BSI andcomes into effect on 31December1986 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference NFM/10 Draft for comment 84/39884 DC ISBN 0 580 15520 X Committees responsible for this British Standard The preparation o
4、f this British Standard was entrusted by the Non-ferrous Metals Standards Committee (NFM/-) to Technical Committee NFM/10, upon which the following bodies were represented: British Non-ferrous Metals Federation British Steel Industry Engineering Equipment and Materials Users Association Ministry of
5、Defence Process Plant Association Stainless Steel Fabricators Association of Great Britain Coopted members Amendments issued since publication Amd. No. Date of issue CommentsBS6783-1:1986 BSI 10-1999 i Contents Page Committees responsible Inside front cover National foreword ii 1 Scope and field of
6、application 1 2 References 1 3 Principle 1 4 Reagents 1 5 Apparatus 2 6 Sampling and samples 2 7 Procedure A 2 8 Procedure B 3 9 Expression of results 4 10 Interferences and precautions 5 11 Special cases 5 12 Test report 5 Annex A Checking of spectrometer performance parameters 6 Annex B Statistica
7、l report of interlaboratory tests 7 Table 1 Concentration ranges of elements to be determined 1 Table 2 Set of calibration solutions A 2 Table 3 Spectral lines Procedure A 3 Table 4 Alternative spectral lines Procedure A 3 Table 5 Set of calibration solutions B 4 Table 6 Spectral lines Procedure B 4
8、 Table 7 Results of statistical analysis Procedure A 9 Table 8 Results of statistical analysis Procedure B 10 Publications referred to Inside back coverBS6783-1:1986 ii BSI 10-1999 National foreword This Part of BS6783 has been prepared under the direction of the Non-ferrous Metals Standards Committ
9、ee. It is identical with ISO6351:1985 “Nickel Determination of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead and zinc contents Flame atomic absorption spectrometric method” published by the International Organization for Standardization (ISO). At present this British Standard consi
10、sts of nine Parts all concerned with analysis of nickel, ferronickel and nickel alloys. Further International Standards are in preparation on sampling and analysis of nickel, ferronickel and nickel alloys and, when available, these will be published as further Parts of this BritishStandard. Terminol
11、ogy and conventions. The text of the International Standard has been approved as suitable for publication as a British Standard without deviation. Some terminology and certain conventions are not identical with those used in British Standards; attention is drawn especially to the following. The comm
12、a has been used as a decimal marker. In British Standards it is current practice to use a full point on the baseline as the decimal marker. Wherever the words “International Standard” appear, referring to this standard, they should be read as “Part of BS6783”. In British Standards it is current prac
13、tice to use the symbol “L” for litre (and in its submultiples) rather than “l”. The Technical Committee has reviewed the provisions of ISO385-1, ISO648 and ISO6283, to which reference is made in the text, and has decided that they are acceptable for use in conjunction with this standard. ISO 385-1 i
14、s related to BS846:1985 “Specification for burettes” and ISO648 is related to BS1583:1986 “Specification for one-mark pipettes”. 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. Compli
15、ance with a British Standard does not of itself confer immunity from legal obligations. Cross-references International Standards Corresponding British Standards ISO 1042:1983 BS 1792:1982 Specification for one-mark volumetric flasks (Identical) ISO 3534:1977 BS 5532 Statistical terminology Part1:197
16、8 Glossary of terms relating to probability and general terms relating to statistics (Identical) ISO 5725:1981 BS 5497 Precision of test methods Part1:1979 Guide for the determination of repeatability and reproducibility for a standard test method (Technically equivalent) Summary of pages This docum
17、ent comprises a front cover, an inside front cover, pagesi andii, pages1 to10, an inside back cover and a back cover. 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.BS6783-1:1986 BS
18、I 10-1999 1 1 Scope and field of application This International Standard specifies a flame atomic absorption spectrometric method for the determination of the silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead and zinc contents of refined, wrought and cast nickel within the ranges speci
19、fied in Table 1. This method is applicable to the independent determination of any one or more of the elements listed without including all the elements specified in the standard solutions. Table 1 Concentration ranges of elements tobe determined The lower level for iron can be extended to less than
20、0,0025%(m/m) provided nickel containing less than0,0001%(m/m) iron is used for preparation of standard solutions; see4.1. The upper limit for the determination of cobalt and copper can be raised to2%(m/m) by a minor modification to the method; see11.1. For potential interferences, seeclause10. 2 Ref
21、erences ISO 385-1, Laboratory glassware Burettes Part1: General requirements. ISO 648, Laboratory glassware One-mark pipettes. ISO 1042, Laboratory glassware One-mark volumetric flasks. ISO 5725, Precision of test methods Determination of repeatability and reproducibility by inter-laboratory tests.
22、3 Principle Dissolution of a test portion in nitric acid diluted(1+1), evaporation of excess acid and dilution of the solution to a known volume. Aspiration of the solution into the air-acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the resonance line energy f
23、rom the spectrum of each element and comparison with that of calibration solutions of the same element in a matched nickel matrix. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Nic
24、kel powder, high purity containing less than0,0005%(m/m) iron and less than0,0001%(m/m) each of silver, bismuth, cadmium, cobalt, copper, manganese, lead and zinc. 4.2 Nitric acid (HNO 3 ) 20 =1,41g/ml, diluted1+1. The same batch of nitric acid shall be used throughout the procedure. 4.3 Nitric acid
25、 (HNO 3 ) 20 =1,41g/ml, diluted1+19. The same batch of nitric acid shall be used throughout the procedure. 4.4 Mixed analyte standard solutions 4.4.1 Metal stock standard solutions, corresponding to1,000g of Ag, Bi, Cd, Co, Cu, Fe, Mn, Pb, or Zn perlitre. Prepare separately for each metal of interes
26、t. Weigh to the nearest0,001g,1,00g of silver, bismuth, cadmium, cobalt, copper, iron, manganese, lead, or zinc at least99,9%(m/m) purel, transfer to a600ml beaker and dissolve in40ml of nitric acid(4.2). Heat to complete dissolution, boil gently to expel oxides of nitrogen, cool and transfer to a10
27、00ml one-mark volumetric flask containing160ml of nitric acid(4.2). Make up to the mark with water and mix. Store in polyethylene bottles, except for silver which is stored in glass. 4.4.2 Mixed analyte standard solution A, corresponding to20mg each of Ag, Bi, Cd, Co, Cu, Fe, Mn, Pb per litre and10m
28、g of Zn per litre. Pipette20,0ml each of the silver, bismuth, cadmium, cobalt, copper, iron, manganese and lead stock standard solutions(4.4.1) and10ml of the zinc stock standard solution(4.4.1) into a1000ml one-mark volumetric flask containing160ml of nitric acid(4.2). Make up to the mark with wate
29、r and mix. Store in a glass bottle. 4.4.3 Mixed analyte standard solution B, corresponding to100mg each of Co, Cu, Fe, Mn per litre and10mg of Zn per litre. Element Concentration range, %(m/m) a Procedure A Procedure B Ag Bi Cd Co Cu Fe Mn Pb Zn 0,0002to0,01 0,0001to0,01 0,0002to0,0025 0,0010to0,01
30、0,0002to0,01 0,0025to0,01 0,0005to0,01 0,0005to0,01 0,0002to0,0025 0,01 0,01 0,01 0,001 to1,00 to1,00 to0,15 to0,20 to0,015 a For specific compositions, seeISO6283.BS6783-1:1986 2 BSI 10-1999 Pipette50,0ml each of the cobalt, copper, iron and manganese stock standard solutions(4.4.1) and5,0ml of the
31、 zinc stock standard solution(4.4.1) into a500ml one-mark volumetric flask. Make up to the mark with water and mix. Store in a polyethylene bottle. 5 Apparatus Ordinary laboratory apparatus, and 5.1 Atomic absorption spectrometer. 5.1.1 The atomic absorption spectrometer used in this method shall me
32、et the instrument performance parameters given in Annex A. 5.1.2 The instrument shall be equipped with a burner head capable of accepting a solution containing25g of Ni as nitrate per litre and suitable for an air-acetylene flame. 5.1.3 The instrument should be capable of using single element hollow
33、 cathode or electrodeless discharge lamps operated at currents recommended by the instrument manufacturer. 5.2 Burette, of capacity50ml graduated in divisions of0,1ml in accordance with ISO385-1, class A. 5.3 Pipettes, of capacities5;20;25;50; and100ml, in accordance with ISO648, class A. 5.4 Volume
34、tric flasks, of capacities200;250;500; and1000ml, in accordance with ISO1042, classA. 6 Sampling and samples 6.1 Sampling and preparation of the laboratory sample shall be carried out by normal agreed procedures or, in case of dispute, by the relevant International Standard. 6.2 The laboratory sampl
35、e normally is in the form of a powder, granules, millings or drillings and no further preparation of the sample is necessary. 6.3 If it is suspected that the laboratory sample is contaminated with oil or grease from the milling or drilling process, it shall be cleaned by washing with high purity ace
36、tone and drying in air. 6.4 If the laboratory sample contains particles or pieces of widely varying sizes, the test portion should be obtained by riffling. 7 Procedure A This procedure is applicable to0,000 5%(m/m) to0,01%(m/m) of silver, bismuth, cadmium, cobalt, copper, iron, manganese and lead, a
37、nd0,0005% to0,005%(m/m) zinc. 7.1 Preparation of test solution Weigh, to the nearest0,01g,4,9 to5,1g of the laboratory sample and transfer to a clean unetched600ml beaker. Add sufficient water to cover the test portion and dissolve by adding60ml of nitric acid(4.2) in small portions. Heat to complet
38、e dissolution, boil gently to expel oxides of nitrogen and evaporate to a viscous syrup. Redissolve the salts by adding20ml of nitric acid(4.2) and100ml of water. Heat to complete dissolution, cool and filter, if necessary, through glass-wool washed with nitric acid(4.2) or a cellulose filter into a
39、200ml one-mark volumetric flask. Wash the filter with water. Make up to the mark with water and mix. If sample inhomogeneity is suspected, a larger test portion,10 to50g, may be taken for analysis. However, an aliquot portion to correspond to a5g test portion shall be taken from such a solution and
40、processed in accordance with the procedure given. See11.2. 7.2 Blank test The zero member of the set of calibration solutionsA(7.3) serves as the blank test since the same batch of nitric acid is used for dissolution of both the nickel reference and test samples. If it is impossible to use the same
41、batch of nitric acid a second blank test shall be prepared using the same nickel powder(4.1). This blank is then compared with the zero member and an appropriate correction made. 7.3 Preparation of the set of calibration solutions A 7.3.1 This set corresponds to0;0,2;0,5;1,0;1,5;2,0; and2,5mg each o
42、f Ag, Bi, Cd, Co, Cu, Fe, Mn and Pb per litre and0;0,1;0,25;0,5;0,75;1,0; and1,25mg of Zn per litre (seeTable 2). All the solutions contain a matrix of25g of Ni per litre. Table 2 Set of calibration solutions A No. Volume of mixed analyte standard solution A (4.4.2)(ml) Analyteconcentration(mg/l) Ag
43、, Bi, Cd, Co, Cu, Fe, Mn, Pb Zn 1 2 3 4 5 6 7 0 2,0 5,0 10,0 15,0 20,0 25,0 0 0,2 0,5 1,0 1,5 2,0 2,5 0 0,1 0,25 0,5 0,75 1,0 1,25BS6783-1:1986 BSI 10-1999 3 7.3.2 Weigh, to the nearest0,01g, seven separate5,0g portions of nickel powder(4.1) and transfer to600ml beakers. Dissolve as directed in7.1.
44、7.3.3 Add, using a burette,0;2,0;5,0;10,0;15,0;20,0; and25,0ml respectively of the mixed analyte standard solutionA(4.4.2) to the200ml flasks. Make up to the mark with water and mix. 7.3.4 The solution with no analyte added is the zero member, which also serves as the blank test (see7.2). 7.4 Calibr
45、ation and determination 7.4.1 Spectrometric measurements 7.4.1.1 The spectral lines specified in Table 3 should be used in the analysis. Table 3 Spectral lines Procedure A 7.4.1.2 The alternative less sensitive spectral lines specified in Table 4 may be used. Table 4 Alternative spectral lines Proce
46、dure A 7.4.1.3 Set the required instrument parameters according to the manufacturers instructions. Light the burner and aspirate nitric acid diluted(1+19)(4.3) until thermal equilibrium is reached. A fuel-lean air-acetylene flame shall be used. 7.4.1.4 Ensure that the instrument meets the performanc
47、e requirements given in Annex A. NOTEOptimum settings for the operating parameters vary from instrument to instrument. Scale expansion may have to be used to obtain the required readability. 7.4.1.5 Ensure that the test solution(7.1) and the set of calibration solutions A(7.3) are within1 C of the s
48、ame temperature. 7.4.1.6 Aspirate nitric acid diluted1+19 and zero the instrument. 7.4.1.7 Aspirate the test solution(s) and note the reading to determine its place within the set of calibration solutions A. 7.4.1.8 Aspirate nitric acid diluted1+19 until the initial reading is obtained. Zero the ins
49、trument if necessary. 7.4.1.9 Aspirate the set of calibration solutions A(7.3) and the test solution(s) in the order of increasing instrument response, starting with the zero member. When a stable response is obtained, record the reading. Flush the system by aspirating nitric acid diluted1+19 between each test or calibration solution. NOTEAvoid aspirating solutions with a high concentration of nickel for long periods without flushing, otherwise the burner may tend to clog. 7.4.1.10 Repeat the measureme
