1、BRITISH STANDARD BS 3993:1966 Specification for Hydrochloric acid commercial Types1and2BS3993:1966 This British Standard, having been approved by the Chemicals Industry Standards Committee and endorsed by the Chairman ofthe Chemical Divisional Council, was published under theauthority of the General
2、 Council on 7March1966 BSI 04-2000 The following BSI references relate to the work on this standard: Committee reference CIC/20 Draft for comment D63/11306 ISBN 0 580 35807 0 Co-operating organizations The Chemicals Industry Standards Committee, under whose supervision this British Standard was prep
3、ared, consists of representatives from the following Government departments and industrial organizations: Board of Trade British Iron and Steel Federation Chemical Industries Association* Fertilizer Manufacturers Association Gas Council* Institute of Vitreous Enamellers Institution of Gas Engineers
4、Ministry of Defence, Army Department* Ministry of Health National Sulphuric Acid Association* Royal Institute of Public Health & Hygiene The Government department and industrial organizations marked with an asterisk in the above list, together with the following, were directly represented on the com
5、mittee entrusted with the preparation of this BritishStandard: Royal Institute of Chemistry Amendments issued since publication Amd. No. Date CommentsBS3993:1966 BSI 04-2000 i Contents Page Co-operating organizations Inside front cover Foreword ii 1 Scope 1 2 Description 1 3 Requirements 1 4 Samplin
6、g and size of sample 1 5 Packaging and marking 1 Appendix A Method for the determination of residue on evaporation 3 Appendix B Method for the determination of sulphated residue on ignition 3 Appendix C Method for the determination of total sulphate content 3 Appendix D Method for the determination
7、of total sulphate content 4 Appendix E Method for the determination of iron content 5 Appendix F Method for the determination of arsenic content 6 Appendix G Method for the determination of lead content 8 Appendix H Method for the determination of copper content 9 Appendix J Method for the determina
8、tion of mercury content 11 Appendix K Method for the determination of oxidizing and reducing substances 13 Figure 1 Convenient form of apparatus for the determination of minute quantities of sulphate 15 Figure 2 Apparatus for use in the determination of arsenic 16BS3993:1966 ii BSI 04-2000 Foreword
9、This standard makes reference to the following British Standards: BS 506, Methanol. BS 612, Nessler cylinders. BS 846, Burettes and bulb burettes. BS 976, Density composition tables for aqueous solutions of hydrochloric acid. BS 1647, pH scale. BS 1752, Laboratory sintered or fritted filters. BS 179
10、2, One-mark volumetric flasks. BS 3218, Test tubes and boiling tubes. BS 3591, Industrial methylated spirits. The preparation of this British Standard was authorized by the Chemicals Industry Standards Committee in order to provide specifications for hydrochloric acid. The importance of the impuriti
11、es that may be present in hydrochloric acid depends to some extent on the use to which the material is to be put. This standard specifics those impurities that are commonly of importance to users who may, however, wish to supplement them with requirements in respect of such matters as extraneous odo
12、ur and organic impurities. 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. Summary of pag
13、es This document comprises a front cover, an inside front cover, pages i and ii, pages1 to 16 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.BS3993:1966 BSI 04-200
14、0 1 1 Scope This British Standard specifies two types of hydrochloric acid. 2 Description The material shall consist essentially of an aqueous solution of hydrogen chloride, HCl. It shall be clear, ranging in colour from colourless to pale yellow. 3 Requirements The material shall comply with the re
15、quirements as shown in the following table when tested by the appropriate method given in Column 4: 4 Sampling and size of sample For the purpose of examination in accordance with this specification a representative sample of the material measuring not less than2litres shall be taken from the bulk.
16、The sample shall be placed in a clean dry air-tight glass-stoppered bottle of such a size that it is nearly filled by the sample. When it is necessary to seal the container, care shall be taken to avoid the risk of contaminating the contents in any way. 5 Packaging and marking The material shall be
17、supplied in suitable sound, clean, moisture-resistant containers which shall be marked to indicate clearly the full identity of the contents. The marking shall include the number of this British Standard, viz. BS3993, Type1, or BS3993, Type2. Type 1 Type 2 Method of test in Appendix Relative density
18、 aat 20/20 C 1.137 to 1.142 or 1.157 to 1.162 or 1.177 to 1.182 Residue on evaporation: per cent by weight, maximum 0.1 b A Sulphated residue on ignition: per cent by weight, maximum 0.05 0.2 B Total sulphate (as H 2 SO 4 ): per cent by weight, maximum 0.05 C 0.6 D Iron: parts per million by weight,
19、 maximum 5 50 E Arsenic: parts per million by weight, maximum 1 2 F Lead: parts per million by weight, maximum 1 2 G Copper: parts per million by weight, maximum 1 2 H Mercury: parts per million by weight, maximum 5 b J Oxidizing substances (as Cl 2 ): parts per million by weight, maximum 50 100 K R
20、educing substances (as SO 2 ): parts per million by weight, maximum 50 100 K NOTEThe HCl content of a sample of Type 1 acid may be obtained by reference to BS976, “Density composition tables for aqueous solutions of hydrochloric acid”. Because of the dissolved solids it may contain, the HCl content
21、of a sample of Type 2 acid may be obtained only approximately in this way. a Formerly “specific gravity” : “relative density” is the term adopted for this concept, with water as the reference substance, by the International Organization for Standardization (ISO). b Not specified.BS3993:1966 2 BSI 04
22、-2000 NOTEThe mark BS3993 on or in relation to the product is a claim by the manufacturer that it complies with the requirements of the standard. The British Standards Institution is the owner of a registered certification trade mark. This is shown below, enclosed in the words “Approved to British S
23、tandard”. This mark can be used only by manufacturers licensed under the certification mark scheme operated by the BSI. The presence of this mark on or in relation to a product is an assurance that the goods have been produced to comply with the requirements of the British Standard under a system of
24、 supervision, control and testing operated during manufacture and including periodical inspection at the manufacturers works in accordance with the certification mark scheme of the BSI. Further particulars of the terms of licence may be obtained from the Director, British Standards Institution,2Park
25、 Street, London, W.1.BS3993:1966 BSI 04-2000 3 Appendix A Method for the determination of residue on evaporation A.1 Apparatus Platinum dish, approx.2in (50mm) diameter. A.2 Procedure Transfer 100 ml of the sample in successive small portions to the weighed platinum dish and evaporate to dryness on
26、a boiling-water bath in a fume cupboard. Dry the dish and residue for30minutes in an oven at a temperature of105 1 C. Cool in a desiccator and weigh immediately. A.3 Calculation Residue on evaporation, per cent by weight = Appendix B Method for the determination of sulphated residue on ignition B.1
27、Apparatus Platinum dish, approx.2in (50mm) diameter. B.2 Reagent The reagent used shall be of a recognized analytical reagent quality. Sulphuric acid, concentrated, d=1.84. B.3 Procedure Transfer 250ml (for Type1acid) or50ml (for Type2acid) of the sample in successive small portions to the weighed p
28、latinum dish and evaporate to dryness on a boiling-water bath in a fume cupboard. Cool and cover the residue with a few drops of concentrated sulphuric acid. Heat the dish on a sand-bath or hot plate until no further fumes are evolved and finally ignite to constant weight at850 50 C. B.4 Calculation
29、 Sulphated residue on ignition, per cent by weight = Appendix C Method for the determination of total sulphate content (ForType1acid only) C.1 Outline of method The sulphate present is determined nephelometrically using a standard solution of sulphuric acid for reference purposes. C.2 Apparatus a) M
30、icroburette,5ml complying with BS846 1) . b) Two similar test tubes, 125 16mm, complying with BS3218 2) . where d =relative density, of the sample at room temperature and W 1 =weight, in grammes, of residue found. where d=relative density of the sample at room temperature, V 1 =volume, in millilitre
31、s, of sample taken and W 2 =weight, in grammes, of residue found. 1) BS846, “Burettes and bulb burettes”. 2) BS3218, “Test tubes and boiling tubes”. W 1 d - W 2 100 d V 1 -BS3993:1966 4 BSI 04-2000 C.3 Reagents The reagents used shall be of a recognized analytical reagent quality. Distilled water, o
32、r water otherwise produced of at least equal purity, shall be used throughout. a) Sodium carbonate, approximately N solution. b) Hydrochloric acid, approximately N solution. c) Sulphuric acid,0.002N solution. d) Sulphate seeding reagent. Dissolve2g of barium chloride in75ml of water, add20ml of95per
33、cent(v/v) ethanol 3)and5ml of the 0.002N sulphuric acid solution. This reagent should be prepared fresh daily. C.4 Procedure Measure2.0ml of the sample into a small porcelain or silica basin, add 0.2ml of the N sodium carbonate solution and evaporate to dryness at 120 C. Dissolve the residue in10ml
34、of hot water and add1ml of theN hydrochloric acid solution. Filter if necessary, allow to cool to room temperature, add1ml of the sulphate seeding reagent, transfer to one of the two similar test tubes and dilute with water to20ml. Prepare a blank test in the second test tube from0.2ml of the N sodi
35、um carbonate solution,1.2ml of theN hydrochloric acid solution and 1 ml of the sulphate seeding reagent in15ml of water. Match the turbidity of the sample solution with the0.002N sulphuric acid solution added from the microburette and carrying out the final match at equal height of liquid in the two
36、 tubes. (The matching may conveniently be made using the method depicted inFigure 2.) If more than5ml of0.002N sulphuric acid solution is required to match the turbidity of the sample solution, repeat the test using a smaller volume of the sample. C.5 Calculation Total sulphate content, calculated a
37、s sulphuric acid, H 2 SO 4 , Parts per million= Appendix D Method for the determination of total sulphate content (ForType2 acid only) D.1 Outline of method The sulphate present is precipitated as barium sulphate and determined gravimetrically. D.2 Apparatus Sintered glass or porous porcelain crucib
38、le, of porosity grade No. 4 4) . D.3 Reagents The reagents used shall be of a recognized analytical reagent quality. Distilled water, or water otherwise produced of at least equal purity, shall be used throughout. a) Sodium chloride. b) Hydrochloric acid, concentrated, d=1.18. c) Barium chloride,10p
39、er cent (w/v) solution. D.4 Procedure Transfer a suitable quantity of the sample (10ml to100ml of sample according to the sulphate content) to a300ml squat-form beaker, add1g of sodium chloride and evaporate just to dryness. Moisten the residue with1ml of concentrated hydrochloric acid and add200ml
40、of boiling water. Filter, if necessary. 3) Ethanol may be replaced by methanol complying with BS506, “Methanol”. where d =relative density of the sample at room temperature, T 1 =volume, in millilitres, of 0.002N sulphuric acid solution used and V 2 =volume, in millilitres, of sample taken. 4) BS175
41、2, “Laboratory sintered or fritted filters”. 98T 1 dV 2 -BS3993:1966 BSI 04-2000 5 To the boiling solution add dropwise10ml of the barium chloride solution with constant stirring. Cover the beaker and allow to stand in a warm place for four hours. Filter through the tared sintered glass or porous po
42、rcelain crucible, wash the precipitate with hot water until the washings are free from chloride, dry at150 C. Allow to cool in a desiccator and weigh. At the same time carry out a blank test on the reagents alone. D.5 Calculation Total sulphate content, calculated as sulphuric acid, H 2 SO 4 , perce
43、ntbyweight= Appendix E Method for the determination of iron content E.1 Outline of method The iron present is reduced to the ferrous state and determined spectrophotometrically or visually using2,2-bipyridyl. E.2 Apparatus a) Photoelectric absorptiometer or Spectrophotometer with4cm cells. Alternati
44、vely Nessler cylinders, complying with BS612 5) . b) Twelve one-mark volumetric flasks 6) , 100ml capacity. c) One-mark volumetric flask 6) ,250ml capacity. E.3 Reagents The reagents used shall be of a recognized analytical reagent quality. Distilled water, or water otherwise produced of at least eq
45、ual purity, shall be used throughout. a) Hydrochloric acid, concentrated, d =1.18. b) Hydrochloric acid, approximately N solution. c) Hydroxyammonium chloride, 10per cent (w/v) solution. d) Ammonium acetate, 20per cent (w/v) solution. e) 2,2-bipyridyl,0.1per cent (w/v) solution. Dissolve0.1g of the
46、reagent in50ml of water containing2ml of N hydrochloric acid and dilute to100ml. f) Standard iron solution. Dissolve7.022g of ammonium ferrous sulphate in a mixture of600ml of water and350ml of concentrated sulphuric acid, d =1.84. Dilute to1000ml with water and further dilute10ml of the solution so
47、 obtained to1000ml with water.1ml of the resulting solution contains104g of iron. E.4 Procedure a) Preparation of colour standards. Into eleven of the100ml one-mark volumetric flasks, each containing50ml of water and2ml of the N hydrochloric acid solution, transfer amounts of the standard iron solut
48、ion, containing from0to1004g of iron increasing by stages of104g and treat each solution in the following manner: Add2ml of the hydroxyammonium chloride solution and allow to stand for one minute. Add10ml of the ammonium acetate solution and3ml of the2,2-bipyridyl solution. Dilute the contents of ea
49、ch flask to100ml and thoroughly mix. These standards are used directly for visual comparison. If an instrument is to be used measure the optical density of each solution at a wavelength of515m4 and prepare a calibration chart. where d =relative density of the sample at room temperature, V 3 =volume, in millilitres, of sample taken and W 3 =weight, in grammes, of the precipitate. 5) BS612, “Nessler cylinders”. 6) BS1792, “One-mark volumetric flasks”. 42.02W 3 V 3 d -BS399
