BS 6376-1-1983 Reagents for chemical analysis - Methods of test《化学分析试剂 第1部分 试验方法》.pdf

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1、BRITISH STANDARD BS6376-1: 1983 ISO6353-1: 1982 Reagents for chemical analysis Part1: Methods of test ISO title: Reagents for chemical analysis Part1: General test methods UDC 543-4:543.06BS6376-1:1983 This BritishStandard, having been prepared under the directionof the Chemicals Standards Committee

2、, was published under the authority ofthe Board of BSI and comes intoeffect on 31May1983 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference CIC/26 Draft for comment80/52715DC ISBN 0 580 11995 5 Committees responsible for this BritishStandard This Britis

3、hStandard was published under the direction of the Chemicals Standards Committee CIC/-. Its preparation was entrusted to Technical Committee CIC/26 upon which the following bodies were represented: British Pharmacopoeia Commission Chemical Industries Association Institute of Petroleum Milk Marketing

4、 Board Ministry of Defence Royal Society of Chemistry Society of Glass Technology Textile Institute Amendments issued since publication Amd. No. Date of issue CommentsBS6376-1:1983 BSI 12-1999 i Contents Page Committees responsible Inside front cover National foreword ii 1 Scope and field of applica

5、tion 1 2 References 1 3 General information 1 4 Solutions for use in test methods 2 5 General test methods (GM) 5 Figure Absorption apparatus for use in arsenic test 7 Table 1 Preparations of stock standard solutions 3 Table 2 Preparation of standard matching solutions 8 Table 3 pH values 13 Table 4

6、 Typical titration end-point 14 Publications referred to Inside back coverBS6376-1:1983 ii BSI 12-1999 National foreword This BritishStandard has been prepared under the direction of the Chemicals Standards Committee. Part1 is identical with ISO6353-1 “Reagents for chemical analysis Part1: General t

7、est methods”, published in 1982 by the International Organization for Standardization (ISO). Further parts of this International Standard are to be published which will comprise specifications for a series of laboratory reagents and which will make appropriate reference to the methods specified in p

8、art1. Subject to their approval by the UK, they will be published as further Parts of this BritishStandard. Terminology and conventions. The text of the International Standard has been approved as suitable for publication as a BritishStandard without deviation. Some terminology and certain conventio

9、ns are not identical with those used in BritishStandards; attention is drawn especially to the following. The comma has been used as a decimal marker. In BritishStandards it is current practice to use a full point on the baseline as the decimal marker. Wherever the words “International Standard” and

10、 “this part of ISO6353” appear, referring to this standard, they should be read as “BritishStandard” and “this Part of BS6376” respectively. ISO918, the revision of ISO/R918 (to which BS4591 is technically equivalent), and to which reference is made in5.2.5.1, is in course of preparation. Subject to

11、 the acceptability of the revised text, it is expected that ISO918 will be published, without alteration, as the revision of BS4591. The Technical Committee has reviewed the provisions of ISO760, to which reference is made in5.12, ISO1392, to which reference is made in5.25.3 and ISO2718 to which ref

12、erence is made in5.34, and has decided that they are acceptable for use in conjunction with this standard. Related BritishStandards for ISO760, ISO1392 and ISO2718 are BS2511 “Methods for the determination of water (Karl Fischer method)”, BS4633 “Method for the determination of crystallizing point”

13、and BS5443 “Recommendations for a standard layout for methods of chemical analysis by gas chromatography”, respectively. Additional information Water. Unless otherwise stated, water complying with the requirements of these determinations is specified in BS3978 “Water for laboratory use”. Cross-refer

14、ences International Standard Corresponding BritishStandard ISO31 BS5775 Specification for quantities, units and symbols (Identical) ISO758:1976 BS4522:1970 Method for the determination of density of liquids at20 C (Technically equivalent) ISO759:1981 BS4524:1983 Method for determination of residue o

15、n evaporation on a water bath (Identical) ISO2211:1973 BS5339:1976 Method of measurement of colour in Hazen units (platinum-cobalt scale) of liquid chemical products (Identical) ISO6685:1982 BS6337 General methods of chemical analysis Part3:1983 Method for determination of iron content(1,10-phenanth

16、roline spectrophotometric method) (Identical)BS6376-1:1983 BSI 12-1999 iii Ethanol. The ethanol used in these determinations may be replaced for these purposes by industrial methylated spirits,95% (V/V), complying with the requirements of BS3591. It should be noted that the use of industrial methyla

17、ted spirits is governed by The Methylated Spirits Regulations,1952 (S.I.1952, No2230) as amended by The Alcoholic Liquors (Amendment of Units and Methods of Measurement) Regulation1979 (S.I.1979, No1149). It is not permissible to use duty-free ethanol, received under the provisions of the Alcoholic

18、Liquor Duties Act1979, Section10, for purposes for which industrial methylated spirits is an acceptable alternative to ethanol. Storage of stock standard solutions. Glass bottles may be used for storage of stock standard solutions in place of the plastics bottles recommended in4.1.1, unless otherwis

19、e stated in the remainder of4.1. Textual errors. When adopting the text of the International Standard, the textual errors listed below were discovered. They have been marked in the text and have been reported to ISO in a proposal to amend the text of the International Standard. 3.10. In line10, “man

20、ufactures” should be read as “manufacturers”. 4.2.3. In line7, “soon any turbidity appears” should be read as “soon as any turbidity appears”. 4.2.6.2. In line6, “starch solutions” should be read as “starch solution”. 5.9.2. In line1, “solution using” should read “solution to”. This standard describ

21、es a method of test only and should not be referred to as a specification defining limits of purity. Reference to the standard should indicate that the method of test used is in accordance with BS6376-1. A British Standard does not purport to include all the necessary provisions of a contract. Users

22、 of British Standards are responsible for their correct application. 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, pagesi toiv, pages1to16, an inside back cover and a back c

23、over. 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.iv blankBS6376-1:1983 BSI 12-1999 1 1 Scope and field of application This part of ISO6353 specifies general test methods for ver

24、ifying the compliance of reagents for chemical analysis with the specifications given in other parts of this International Standard. 2 References ISO31, Quantities, units and symbols. ISO758, Liquid chemical products for industrial use Determination of density at20 C. ISO759, Volatile organic liquid

25、s for industrial use Determination of dry residue after evaporation on a water bath General method. ISO760, Determination of water Karl Fischer method (General method). ISO918, Volatile organic liquids for industrial use Determination of distillation characteristics General method 1) . ISO1392, Dete

26、rmination of crystallizing point General method. ISO2211, Liquid chemical products Measurement of colour in Hazen units (platinum-cobalt scale). ISO2718, Standard layout for a method of chemical analysis by gas chromatography. ISO6685, Chemical products for industrial use General method for determin

27、ation of iron content 1,10-Phenanthroline spectrophotometric method 2) . 3 General information 3.1 The nomenclature for chemical compounds used in this International Standard in general conforms to the rules published by the International Union of Pure and Applied Chemistry (IUPAC). 3.2 In all react

28、ions or operations described, use only distilled or deionized water. Carbon dioxide-free water, if required, may be prepared by boiling water of the above grade for about10min and protecting from the atmosphere during cooling and storing. 3.3 Unless otherwise stated, solutions are aqueous and, dilut

29、ions shall be made with water. 3.4 The symbol “%” indicates percentage by mass (m/m), unless otherwise stated. 3.5 The reference number of a general test method, abbreviated GM, as given in the individual tests, refers to the number of the method in clause5. 3.6 The reagents used shall conform to th

30、e specifications in ISO6353. In the absence of such a specification, reagents of suitable analytical grade be shall be used. NOTEReagents specified in this International Standard are identified R, e.g.sodium chloride is R31. 3.7 Unless otherwise stated, values for density refer to the density at20 C

31、. 3.8 Temperatures are expressed in degrees Celsius( C). 3.9 The following additional abbreviations are used in this International Standard: 3.10 Warning The physical and chemical properties of the chemicals being handled, in particular those relating to physiological effects, combustibility and exp

32、losive tendencies, may be such as to present significant health and safety hazards. Although the degree of risk is extremely variable, it should be assumed, in the absence of specific information to the contrary, that the handling of any chemical will involve hazards of this kind. The provision of e

33、xhaustive details in respect of hazards and associated safety procedures is not considered to fall within the scope of this International Standard as most manufactures 3)of chemicals are very willing to advise prospective users on the handling of their products. In addition, national regulations on

34、the packaging and labelling of hazardous chemicals should ensure that adequate information is given on the hazards associated with the use of chemicals. 1) At present at the stage of draft. (Revision of ISO/R918.) 2) At present at the stage of draft. AgDDTC silver diethyldithiocarbamate APDC ammoniu

35、m pyrrolidine-1-carbodithioate EDTA ethylenediaminetetraacetic acid, disodium salt AAS atomic absorption spectroscopy FES flame emission spectroscopy GC gas chromatography SS standard solution IS indicator solution RS reagent solution GM general test method R reagent MAS molecular absorption spectro

36、photometry 3) See national foreword, textual errors.BS6376-1:1983 2 BSI 12-1999 4 Solutions for use in test methods 4.1 Standard solutions Prepare stock standard solutions(4.1.1) and dilute standard solutions(4.1.2) as follows. 4.1.1 Stock standard solutions Dissolve the constituents indicated in co

37、lumn2 of Table 1, dilute to the mark in a1000ml one-mark volumetric flask and mix. It is recommended that all stock standard solutions of inorganic compounds be stored in bottles of suitable plastic material, unless otherwise stated. 4.1.2 Dilute standard solutions Prepare dilute standard solutionsI

38、,II andIII at the time of use by diluting the stock standard solutions(4.1.1) in one-mark volumetric flasks of appropriate capacity and in the precise volume ratios1/10,1/100,1/1000, respectively. 4.2 Reagent solutions Prepare the reagent solutions as follows. 4.2.1 Ammonium metavanadate (RS) Dissol

39、ve2,5g of ammonium metavanadate in500ml of boiling water, cool, add20ml of nitric acid solution (R19), cool and dilute to1000ml. Store in a polyethylene bottle. 4.2.2 Borate standard buffer (RS) Using the carbon dioxide-free water (see3.2), dissolve3,81g of sodium tetraborate decahydrate and dilute

40、to1000ml. Store protected from atmospheric carbon dioxide. 4.2.3 Calcium hydroxide standard buffer (RS) Prepare a saturated solution at25 C. Determine the calcium hydroxide concentration by titration with standard volumetric hydrochloric acid solution, c(HCl)=0,1mol/l, using phenol red (IS4.3.10) as

41、 indicator. The concentration c1/2Ca(OH) 2 shall be between0,0400 and0,0412 mol/l. Store protected from atmospheric carbon dioxide and reject the solution as soon any turbidity appears 4) . 4.2.4 Chromic acid (RS) Dissolve100g of chromium trioxide in sulphuric acid solution(35%) and dilute to1000ml

42、with the same acid. 4.2.5 Cobalt(II) chloride (RS) 4.2.5.1 Preparation Dissolve60g of cobalt(II) chloride hexahydrate in about900ml of a mixture of25ml of hydrochloric acid solution (R13) and975ml of water and dilute to1000ml with the same mixture. Determine the concentration by the method specified

43、 in4.2.5.2 and adjust it to59,5mg of CoCl 2 .6H 2 O per millilitre using a calculated quantity of diluted hydrochloric acid solution. 4.2.5.2 Titration Place5,0ml of the solution(4.2.5.1),5ml of hydrogen peroxide solution(3%) and10ml of sodium hydroxide solution(27%) in a200ml conical flask fitted w

44、ith a ground glass stopper. With the stopper removed, boil gently for10min, allow to cool, add60ml of sulphuric acid(10%) and2g of potassium iodide (R25). Stopper the flask and dissolve the precipitate by shaking gently. Titrate the liberated iodine with standard volumetric sodium thiosulphate solut

45、ion, c(Na 2 S 2 O 3 )=0,1mol/l, adding10drops of the starch solution (IS4.3.11) towards the end of the titration. The end-point is reached when the blue colour has just been discharged. 1ml of sodium thiosulphate solution, c(Na 2 S 2 O 3 )=0,1 mol/l, corresponds to23,79mg of CoCl 2 .6H 2 O. 4) See n

46、ational foreword, textual errors.BS6376-1:1983 BSI 12-1999 3 Table 1 Preparations of stock standard solutions Reagent name Mass of substance required to prepare1000ml of solution 1ml of solution corresponds to Acetaldehyde 1,00g of CH 3 CHO 0,001g of CH 3 CHO Aluminium 17,60g of KAl(SO 4 ) 2 .12H 2

47、O+10ml H 2 SO 4 (25%) 0,001g of Al Ammonium 2,97g of NH 4 Cl (R5) 0,001g of NH 4or 0,0007766g ofN Arsenic 1,32g of As 2 O 3dissolved in3ml of NaOH solution(27%) by warming. 0,001g of As Barium 1,78g of BaCl 2 .2H 2 O (R6) 0,001g of Ba Bismuth 1,00g of Bi dissolved in6ml of HNO 3(R19), and nitrous ga

48、ses removed by boiling. 0,001g of Bi Bromate 1,31g of KBrO 3 0,001g of BrO 3 Bromide 1,49g of KBr 0,001g of Br Calcium 3,67g of CaCl 2 .2H 2 O. Alternatively,2,50g of CaCO 3dissolved in25ml of HCl(10%) solution and CO 2removed by boiling. 0,001g of Ca Carbonate 2,41g of Na 2 CO 3(R30) 0,001g of CO 2

49、or 0,00027g of C Carbonyl 10,43g of acetone (R2) corresponding to5,0g of CO, weighed into a100ml one-mark volumetric flask containing50ml of carbonyl-free methanol (RS4.2.11), diluted to the mark with the same methanol and mixed thoroughly. Take20,0ml of this solution and dilute to1000ml. Use the same methanol for all dilutions. 0,001g of CO Chlorate 1,47g of KClO 3 0,001g of ClO 3 Chloride 1,65g of NaCl (R32) 0,001g of Cl Chlorine 3,97g of Chloramine T (trihydrate) 0,001g of active chlorine Chromium 2,83g of K 2 Cr 2 O 7(R23) 0,001g of