BS 6376-2-1984 Reagents for chemical analysis - Specifications (first series)《化学分析试剂 第2部分 规范(第1系列)》.pdf

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1、BS 6376: Part 2 : 1984ISO 6353/2-1983UDC 543-4 ; 543.06 British Standards Institution. No partof this publication may be photocopiedor otherwise reproduced without theprior permission in writing of BSI.British StandardReagents for chemical analysisPart 2. Specifications (first series)ISO title: Reag

2、ents for chemical analysis - Part 2 : Specifications - First seriesReactifs pour analyse chimiquePartie 2. Specifications (premiere serielReagenzien fur die chemische AnalyseTeil 2. Anforderungen (erste ReihelBritish Standards InstitutionBS 6376 : Part 2 : 1984ContentsSpecifications1. Scope and fiel

3、d of application2. Reagents (abbreviation: R), Specifications -First series 1R 1. Acetic acid 2R 2. Acetone 3R 3. Ammonia solution 4R 4. Ammonium acetate 6R 6. Ammonium chloride 7R 6. Barium chloride dihydrate 8R 7. Chloroform 9R 8. Citric acid monohydrate 10R 9. Copper(lI) sulfate pentahydrate 12R

4、10. Cyclohexane 13R 11. Ethanol 14R 12. (Ethylenedinitrilo)tetraacetic acid, disodiumsalt dihydrate 16R 13. Hydrochloric acid 17R 14. Hydrogen peroxide 19R 16. Hydroxylammonium chloride 21R 16. MagnesIum chloride hexahydrate 22R 17. Magnesium oxide 23R 18. Methanol 25National forewordCommittees resp

5、onsiblePageInside front coverBack coverR 19. Nitric acidR 20. Oxalic acid dihydrateR 21. Perchloric acidR 22. Phosphoric acidR 23. Potassium dichromateR 24. Potassium hydroxideR 25. Potassium iodideR 26. Potassium permanganateR 27. Potassium sodium tartrate tetrahydrateR 28. Silver nitrateR 29. Sodi

6、um acetate trihydrateR 30. Sodium carbonate anhydrousR 31. Sodium carbonate decahydrateR 32. Sodium chlorideR 33. Disodium hydrogenphosphate dodecahydrateR34. Sodium hydroxideR 35. Sodium sulfate, anhydrousR 36. Sodium thiosulfate pentahydrateR 37. Sulfuric acidR 38. Tin(ll) chloride dihydrateR 39.

7、TolueneR 40. ZincFigureApparatus for the determination of the arseniccontent of zincPage2627283031323436373839414345474850515254555667National forewordI This British Standard has been prepared under the direction of the Chemicals Standards Committee and is identical withII ISO 6363/21983 Reagents fo

8、r J;bemical analysis - Part2Q.ecifjcations- First serie!, including Addendum 2.-i5U5Tishe(fbY1heTntonaT,Organization for Standardization (1501. .1Part 1 of this British Standard is identical with I.SO,6353/1_ndspecifsgeneral tllstmethdsowhich references are _made inespecificationIn Part2:.art3 of-1S

9、0633L!erisingspecifications for further reagents, is in course ofpreparatiol and, subject to committee approval, it is intended that the completed. -“ISO 6353/3 will be implemented as Part 3 of as 6376:Terminology and conventions. The text of the international standard has been approved as suitable

10、for pUblication as aBritish Standard without deviation. Some terminology and certain conventions 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 British Standards it is current practice to use a ful

11、l point on the baselineas the decimal marker.Where the words this part of I.SO 6353 appear, referring to this standard, they should be read as this Part of BS 6376.Cross-referenceIntarnat/onal standardISO 6363/1-1982Corresponding British StandardBS 6376 Reagents for chemical analysisPart 1 : 1983 Me

12、thods of test(I dentical)Additional informationAssay ofcoppedll) sulfate pentahydrate. In the method described in R 9.3.1, it is recommended that a small amount ofpotassium thiocyanate be added just before the end of the titration to enhance the sharpness of the end-point.Identification ofreagents.

13、For claims of compliance and purchasing orders relating to a specification in this standard, it isstrongly recommended that the following form of words (using sodium hydroxide as an example) be adopted:sodium hydroxide complying with as 6376/2: R 34 (1984).Compliance with a British Standard does not

14、 of itself confer immunity from legal obligations.British StandardReagents for chemical analysisPart 2. Specifications (first series)1 Scope and field ofpplicationThis part of ISO 6353 gives specifications and indicates the testmethods to be used for checking conformity With thesespecifications for

15、a first series of reagents used in analYticalchemistry.This document should be read in conjunction with ISO 6353/1which describes the general test methods (GM) applicable tothe requirements of the reagent specifications and gives suchgeneral Information as is required for the correct use of thestand

16、ard.Particular attention is drawn to ISO 6353/1, clause 4, whichdescribes the preparati?n of- standard solutions (SS) at dilutions I, II and III;BS 6376 : Part 2 : 1984reagents solutions (RS);indicator solutions (IS).In this part of ISO 6353, asterisked clause reference numbersrefer to ISO 6353/1.2

17、Reagents (abbreviation: R).Specifications - First seriesGeneral remark - In all tests involving comparison with a stan dard matching solution, the result (for example colour inten sity) obtained on the test solution shall not be greater than thatobtained on the specified standard matching solution.B

18、S 6376 : Part 2 : 1984R 1 Acetic acidCH3COOHRelative molecular mass: 60,05R 1.1 SpecificationAssay (CHaCOOH) 99,7 % min.Density: 1,05 glmlChloride (CI) “ 0,000 1 % max.Sulfate (S04) 0,000 2 % max.Copper (Cu) . . . . . . 0,000 05 % maxIron (Fe) 0,000 1 % max.Lead (Pb) 0,000 05 % max.Dichromate-reduci

19、ng substances(expressed as 0) 0,008 % max.Residue after evaporation “ 0,003 % max.R 1.2 Preparation of test solutionTo 100 g (95 ml) of the sample, add 1 ml of sodium carbonatesolution (1 %) and evaporate to dryness on a boiling waterbath. Dissolve the residue in a little water, add 1 ml of thehydro

20、chloric acid (R 13), and dilute to 50 ml with water.R 1.3 TestsR 1.3.1 AssayWeigh, to the nearest 0,000 1 g, 2 to 3 g of the sample, dilutewith 50 ml of water and titrate with standard volumetric sodiumhydroxide solution, c(NaOH) = 1 mol/I, using the phenol phthalein (IS 4.3.9*).1,00 ml ofodiumhydro

21、xide solution, c(NaOHI = 1,000 mol/I,corresponds to 0,060 05 g of CHaCOOH.R 1.3.2 ChlorideDilute 10 g (9,5 ml) of the sample with water to 30 ml, andapply GM 2.Prepare a standard matching solution, using 10 ml of thechloride SS III (10 ml e 0,000 1 % CI).R 1,3.3 SulfateTake 12,5 ml of the test solut

22、ion (R 1.2) and apply GM 3.Prepare a standard matching solution, using 5 ml of the sulfateS5 II (5 ml e 0,000 2 % 504)2R 1.3.4 Copper and leadDetermine these elements by AA5 according to GM 29, usingthe following conditions:ConcentrationResonanceElementof solutionFlame linenmCu Test solution (R 1.2)

23、 324,7Test solution (R 1.2)Air-acetylene217,0 or 283,3PbR 1.3.5 IronTake 5 ml of the test solution (R 1.2) and apply GM 8.1.Prepare a standard matching solution, using 1 ml of the iron5S II (1 ml e 0,000 1 % Fe).R 1.3.6 Dichromate-reducing substancesTo 10,00 ml of 4,90 g/I potassium dichromate solut

24、ion In aconical flask fitted with a ground glass stopper, add cautiously,while cooling and mixing, 10 ml of the sulfuric acid (R 37) andcool to ambient temperature. .Add 10 g (9,5 mil of the sample and allow to stand for 1 hat 60 2 DC. Dilute to 50 ml with water, allow to cool to ambienttemperature,

25、 add 5 ml of potassium iodide solution (10 %) andtitrate with standard volumetric sodium thiosulfate solution,c(Na2S20a) = 0,05 mol/I, using the starch (IS 4.3.11*1.Carry out in parallel a blank test.The dichromate-reducing substances, expressed as a percen tage by mass as oxygen, are given by the f

26、ormulawhereVI is the volume, in millilitres, of standard volumetricsodium thiosulfate solution used for the determination; .V2is the volume, in millilltres, of standard volumetricsodium thiosulfate solution used for the blank test;0,000 4 is the mass, in grams, of oxygen corresponding to1,00 ml of s

27、odium thiosulfate solution, c(Na2S20a)= 0,050 mol/I.R 1.3.7 Residue after evaporationTake 50 g (48 ml) of the sample and apply GM 14.The mass of the residue shall not exceed 1,5 mg.BS 6376 : Part 2 : 1984R 2 AcetoneCH3COCH3Relative molecular mass: 58,08R 2.1 SpecificationAssay (CH3COCH3). . . . . .

28、. . . . . 99,5 % min.Methanol (CH30HI . . . . . . . . . . . . . . . . . 0,05 % max.Density: 0,787 to 0,793 g/mlResidue after evaporation 0,001 % max.AciditY (expressed in millimoles of H +) “ 0,05/100 g max.Alkalinity(expressedinmillimolesofOH-) 0,05/100 g max.Permanganate-reducing substances(expres

29、sed as 0) 0,000 3 % max.Aldehydes (expressed as HCHO) 0,002 % max.Water “ 0,3 % max.R 2.2 TestsR 2.2.1 Assay and methanolApply GM 34, using the following conditions:Stationary phase “ 10 % Carbowax 400Support. Chromosorb G-AW-DMCS0,125 to 0,150 mm(100 to 120 mesh ASTMIColumn length. . . . . . . . .

30、. . . . . . 3 mColumn internal diameter. . . . . 2,5 mmColumn material. . . . . . . . . . Stainless steel or,preferably, glassColumn temperature . 60 DCInjection temperature. . . . . . 150 DCDetection temperature. . . . . 150 DCType of detector . . . . . . . . . . . . . . Flame IonizationCarrier gas

31、 . . . . . . . . . . . . . . . . . NitrogenFlow rate 25 ml/minTest portion . “ 0,5 ,.dR 2.2.2 DensityApply GM 24.1.R 2.2.3 Residue after evaporationTake 100 g (127 mil of the sample and apply GM 14.The mass of the residue shall not exceed 1 mg.R 2.2.4 AcidityTake 79 g (100 mil of the sample and appl

32、y GM 13.1, titratingwith standard volumetric sodium hydroxide solution,c(NaOHI = 0,01 mol/I, and using the phenolphthalein(IS 4.3.9*).The volume of titrant shall not exceed 4 ml.R 2.2.5 AlkalinityTake 79 g (100 mil of the sample and apply GM 13.1, titratingwith standard volumetric sulfuric acid solu

33、tion,c(1/2 H2S04) = 0,01 molll, and using the methyl red(IS 4.3.6*).The volume of titrant shall not exceed 4 ml.R 2.2.6 Permanganate-reduclng substancesTake 40 g (50 mil of the sample and apply GM 19.1, adding0,15 ml of 3,16 gil potassium permanganate solution. Allowthe test solution to stand at 20,

34、0 0,5 DC for 15 min.The pink colour shall not be completely discharged.R 2.2.7 AldehydesTake 2 g (2,5 mil of the sample and apply GM 20.Prepare it standard matching solution, using 4 ml of the for maldehyde 88 II (4 ml0,002 % HCHO).R 2.2.8 WaterTake 7,9 g (10 mil of the sample, dilute to 30 ml with

35、pyridineand apply GM 12.3as 6376 : Part 2 : 1984R 3 Ammonia solution (25 0/0)NH3Relative molecular mass: 17,03R 3.1 SpecificationAssay (NHa) . . . . . . . . . . . . 25 % min.llCarbonate (expressed as CO2) . . . . . 0,002 % max.Chloride (CI) . . . . . . . . . . . . . . . . . . . . . . . . 0,000 05 %

36、max.Phosphate (P04) 0,000 2 % max.Silicate (expressed as S102) “ 0,001 % max.Sulfate (S04) . . . . . 0,000 2 % max.Sulfide (S) 0,000 02 % max.Calcium (Ca) , . . . 0,000 1 % max.Copper (Cu) . . . . . . . . . . . . . . . . . . . . . . . . . . 0,000 01 % max.Iron (Fe) . 0,000 02 % max.Magnesium (Mg) .

37、. . . . . . . . . . . . . . . . . . . . . 0,000 1 % max.Lead (Pb) . 0,000 05 % max.Potassium (K) . . . . . . . . . . . . . . . . . . . 0,000 1 % max.Sodium (Na) 0,000 5 % max.Permanganate-reducing substances(expressed as 0) . 0,000 8 % max.Residue after evaporation : . . . . . . 0,002 % max.R 3.2 Pr

38、eparation of test solutions and ofmixed indicator solutionR 3.2.1 Test solution IEvaporate 250 9 (275 ml) of the samplellto a volume of about10 mi. Acidify with the nitric acid (R 19) and dilute to 100 mlwith water.R 3.2.2 Test solution IIDissolve the residue after evaporation obtained in R 3.3.12 i

39、n0,6 ml of the hydrochloric acid (R 13) and dilute to 100 ml withwater.R 3.2.3 Mixed indicator solutionMix 1 volume of methyl red solution 0,2 % in 95 % (VI V)ethanol) with 1 volume of methylene blue solution 0,1 % in95 % (VI V) ethanol).R 3.3 TestsR 3.3.1 AssayPlace 25,00 ml of standard volumetric

40、sulfuric acid solution,el1/2 H2S04) = 1 mol/I, in a 100 ml conical flask fitted with aground glass stopper and weigh to the nearest 0,000 1 g.Add about 1,2 g of the sample and re-weigh to the nearest0,000 1 g. Add 2 drops of the mixed indicator solution (R 3.2.3)and titrate the excess of acid with s

41、tandard volumetric sodiumhydroxide solution dNaOH) = 1 moili.1,00 ml of sulfuric acid solution, cl1/2 H2S04) = 1,000 molll,corresponds to 0,017 03 g of NHa.R 3.3.2 CarbonateDilute 5 g (5,5 mil of the sample with 10 ml of carbon dioxide free water and add 5 ml of a 4 % solution of barium hydroxideoct

42、ahydrate Ba(OH)2.8H20).After 5 min, any turbidity in the test solution shall not begreater than that of a similarly prepared standard matchingsolution using 10 ml of the carbonate SS II(10 ml !:l 0,002 % CO2),R 3.3.3 ChlorideTake 20 ml of the test solution I (R 3.2.1) and apply GM 2.Prepare a standa

43、rd matching solution, using 2,5 ml of thechloride SS II (2,5 ml0,000 05 % CI).R 3.3.4 PhosphateTake 20 ml of the test solution I (R 3.2.1) and apply GM 4.Prepare a standard matching solution, using 10 ml of thephosphate 5S II (10 ml !:l 0,000 2 % P04).R 3.3.5 SilicateNeutralize 20 g (22 mil of the s

44、ample with the hydrochloric acid(R 13), dilute to approximately 60 ml and apply GM 5.1) The same qualitY is also commercially available with an NHacontent of about 30 % or 35 % and allowance should be made for this when prepar ing test .solution I.4BS 6376 : Part 2 : 1984R 3 Ammonia solution (25 %)P

45、repare a standard matching solution, using 20 ml of thesilicate 55 “ (20 ml e 0,001 % 5i021.R 3,3.6 SulfateTake 10 ml of the test solution I (R 3.2.11 and apply GM 3.Prepare a standard matching solution, using 5 ml of the sulfate55 II (5 ml e 0,000 2 % 804)R 3.3.7 SulfideTo 50 9 (55 mil of the sampl

46、e, add 0,5 ml of the lead acetate(basic) (RS 4.2.10*1.The brown coloration of the test solution shall not be moreintense than that of a similarly prepared standard matchingsolution using 1 ml of the freshly prepared sulfide 5S II(1 ml e 0,000 02 % 5).R 3.3.8 Calcium, copper, magnesium and leadDeterm

47、ine these elements by AAS according to GM 29, usingthe following conditions :ConcentrationResonanceElementof solutionFlame linenmCa 422,7CuTest solution II324,7(R 3.2.2)Air-acetyleneMg 285,2Pb 217,0 or 283,3R 3.3.9 IronEvaporate 50 g (55 mil of the sample to dryness on a boilingwater bath. Take up t

48、he residue in 0,5 ml of the hydrochloricacid (R 13) and apply GM 8.2.Prepare a standard matching solution, using 10 ml of the ironS8 III (10 ml e 0,000 02 % Fel.R 3.3.10 Potassium and sodiumDetermine these elements by FE8 according to GM 30, usingthe follOWing conditions :ElementConcentrationFlameWa

49、velengthof solution nmKTest solution II Oxygen-766,6Na(R 3.2.2) acetylene689,0R 3.3.11 Permanganate-reducing substancesTo 20 g (22 ml) of the sample, add 20 ml water, mix thoroughlyand acidify cautiously with 20 ml of sulfuric acid solution(50 %). Add 0,2 ml of 3,16 gIl potassium permanganate solu tion and boil for 5 min.The pink colour shall not be complete.ly discharged.R 3.3.12 Residue after evaporationTake 100 9 (110 mil of the sample and apply GM 14.The mass of the residue shall not exceed 2 mg.Ret