1、BRITISH STANDARD BS 6376-3: 1989 Reagents for chemical analysis Part 3: Specifications (second series) UDC 543 4:543.06:006.3/.8BS6376-3:1989 This British Standard, having been prepared under the directionof the Chemicals Standards Policy Committee, waspublished under the authorityof the Board of BS
2、Iandcomes into effect on 30March1990 BSI 01-2000 The following BSI references relate to the work on this standard: Committee reference CIC/26 Draft for comment 84/53731 DC ISBN 0 580 17516 2 Committees responsible for this BritishStandard The preparation of this British Standard was entrusted by the
3、 Chemicals Standards Policy Committee (CIC/-) to Technical Committee CIC/26, upon which the following bodies were represented: British Pharmacopoeia Commission Chemical Industries Association Institute of Petroleum Milk Marketing Board Royal Society of Chemistry Society of Glass Technology Amendment
4、s issued since publication Amd. No. Date of issue CommentsBS6376-3:1989 BSI 01-2000 i Contents Page Committees responsible Inside front cover National foreword iii 1 Scope 1 2 Reagents (abbreviation: R), Specifications Second series 1 R 41 Acetic anhydride 2 R 42 Ammonium iron(II) sulfate hexahydrat
5、e 4 R 43 Ammonium iron(III) sulfate dodecahydrate 6 R 44 Ammonium nitrate 8 R 45 Ammonium sulfate 10 R 46 Ammonium thiocyanate 12 R 47 Barium hydroxide octahydrate 14 R 48 Benzene 15 R 49 2,2-Bipyridyl 17 R 50 Boric acid 18 R 51 Bromine 20 R 52 1-Butanol, Butyl alcohol 22 R 53 Calcium carbonate 24 R
6、 54 Carbon tetrachloride 26 R 55 Cobalt(II) chloride hexahydrate 28 R 56 Diammonium oxalate monohydrate 29 R 57 Dichloromethane 31 R 58 Diethyl ether 33 R 59 Dimethylformamide 35 R 60 1,4-Dioxane 37 R 61 Disodium tetraborate decahydrate 38 R 62 Ethyl acetate 39 R 63 Formaldehyde solution 41 R 64 Gly
7、cerol 43 R 65 Hexaammonium heptamolybdate tetrahydrate 46 R 66 Hydrobromic acid 48 R 67 Hydrofluoric acid 50 R 68 Iodine 52 R 69 Iron(II) sulfate heptahydrate 53 R 70 L-Ascorbic acid 55 R 71 Lead(II) acetate trihydrate 56 R 72 Mercury(II) chloride 58 R 73 Petroleum spirit 40/60 60 R 74 Phosphorus(V)
8、 oxide 61 R 75 Potassium bromate 62 R 76 Potassium carbonate 64 R 77 Potassium chloride 66 R 78 Potassium cyanide 68 R 79 Potassium dihydrogen phosphate 70 R 80 Potassium hexacyanoferrate(II) trihydrate 72 R 81 Potassium hexacyanoferrate(III) 73 R 82 Potassium hydrogen phthalate 74 R 83 Potassium io
9、date 75 R 84 Potassium nitrate 77BS6376-3:1989 ii BSI 01-2000 Page R 85 Potassium sulfate 79 R 86 Potassium thiocyanate 81 R 87 2-Propanol 83 R 88 Sodium fluoride 85 R 89 Sodium hydrogen carbonate 87 R 90 Sodium nitrate 89 R 91 Sodium peroxide 91 R 92 Starch, soluble 93 R 93 (+)-Tartaric acid 94 R 9
10、4 Trisodium citrate dihydrate 95 R 95 Xylene 97 R 96 Zinc chloride 99 R 97 Zinc sulfate heptahydrate 101 Publications referred to Inside back coverBS6376-3:1989 BSI 01-2000 iii National foreword This Part of BS6376 has been prepared under the direction of the Chemicals Standards Policy Committee. Pa
11、rt 1 of this British Standard is identical with ISO6353-1:1982 “Reagents for chemical analysis Part1: General test methods” published by the International Organization for Standardization (ISO), and it specifies general test methods to which references are made in the specifications in Part2 and Par
12、t3. Part2 of this British Standard is identical with ISO6353-2:1983 “Reagents for chemical analysis Part2: Specifications First series” and comprises a series of specifications for41 reagents. This Part of BS6376 is based on ISO6353-3:1987 but the final text of the International Standard has been am
13、ended to meet some of the objections raised by the United Kingdom when commenting on the draft International Standard. As a consequence, this Part of BS6376 is technically equivalent to ISO6353-3 except that the specification for 1,4-dioxane (R60) differs in the following respects. a) The requiremen
14、t and test for residue after evaporation have been omitted. b) The test for determination of iron content involves the use of a matching solution, instead of atomic absorption spectroscopy. c) The test for determination of peroxide content has been omitted. The other United Kingdom objections to the
15、 draft International Standard which were not taken into account when ISO6353-3 was finally published were more general and related to the style of presentation rather than technical content. In order to retain a high degree of equivalence between the British Standard and the International Standard,
16、these points have not been incorporated at this stage but will be raised again during subsequent reviews and revisions. For ease of production, it has been found convenient to reproduce the text of ISO6353-3, which has been amended to incorporate the differences outlined above. For claims of complia
17、nce and purchasing orders relating to a specification in this British Standard, it is strongly recommended that the following form of words (using iodine as an example) be adopted: “Iodine complying with BS6376-3: R 68 (1989)”. A British Standard does not purport to include all the necessary provisi
18、ons 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 pages This document comprises a front cover, an inside front cover, pages i to iv, pages1to 102, an in
19、side 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.iv blankBS6376-3:1989 BSI 01-2000 1 1 Scope This Part of BS6376 gives specifications and indicates t
20、he test methods to be used for checking conformity with these specifications for a second series of reagents used in analytical chemistry the numbering system of which continues the first series specified inBS6376-2. This document should be read in conjunction with BS6376-1, which describes the gene
21、ral test methods (GM) applicable to the requirements of the reagent specifications and gives such general information as is required for the correct use of the standard. Particular attention is drawn to BS6376-1, clause4, which describes the preparation of standard solutions (SS) at dilutions I, II
22、and III; reagent solutions (RS); indicator solutions (IS). In this part of BS6376, asterisked clause reference numbers refer to the1983 edition of BS6376-1. NOTEThe titles of the publications referred to in this standard are listed on the inside back cover. 2 Reagents (abbreviation: R), Specificatio
23、ns Second series General remarks 1 In all tests involving comparison with a standard matching solution, the result (for example colour intensity) obtained on the test solution shall not be greater than that obtained on the specified standard matching solution. 2 For iron determinations according to
24、BS6337-3 (GM8.1), no photometric measurement will be executed; the determinations will be carried out using a matching solution as indicated in the relevant monograph. 3 Trivial names of indicators are used in the clauses and the IUPAC names are given in footnotes.BS6376-3:1989 2 BSI 01-2000 R 41 Ac
25、etic anhydride (CH 3 CO) 2 O Relative molecular mass: 102,09 R 41.1 Specification R 41.2 Preparation of test solution Dilute37ml (40g) of the sample to200ml with water (1ml 0,2g). R 41.3 Tests R 41.3.1 Assay Pipette 50ml of morpholine methanolic solution (RS) 1)into each of two250ml glass-stoppered
26、flasks. For the test portion, weigh accurately1,8to2,0g of the acetic anhydride from a Lunge pipette into the first flask and swirl to effect dissolution. Reserve the second flask for the determination of the quantity of morpholine mixed with the sample. Allow the flasks to stand at room temperature
27、 for5min. Add0,20 to0,25ml of methyl yellow methylene blue mixed indicator (IS) 2)3)4) . Titrate each solution with a standard volumetric hydrochloric acid methanolic solution, c(HCl)=0,5mol/l, 1)to the end-point at which the green colour changes to amber. 1,00ml of hydrochloric acid methanolic solu
28、tion, c(HCl)=0,500mol/l, corresponds to0,05105g of (CH 3 CO) 2 O. R 41.3.2 Residue after evaporation Take50g (46ml) of the sample and apply GM14 drying the residue for30min. The mass of the residue shall not exceed1,5mg. R 41.3.3 Chloride Dilute10ml of the test solution(R41.2) to20ml with water and
29、applyGM2. Prepare a standard matching solution, using1ml of the chloride SSII (1ml 0,0005%Cl). R 41.3.4 Sulfate To 50ml of the test solution(R41.2) add1ml of sodium carbonate solution(1%) and evaporate to dryness on a boiling water bath. Dissolve the residue in10ml of water and apply GM3. Prepare a
30、standard matching solution, using5ml of the sulfate SSII (5ml 0,0005%SO 4 ). Assay (CH 3 CO) 2 O 97,0 % min. Residue after evaporation 0,003 % max. Chloride (Cl) 0,000 5 % max. Sulfate (SO 4 ) 0,000 5 % max. Copper (Cu) 0,000 1 % max. Iron (Fe) 0,000 5 % max. Lead (Pb) 0,000 1 % max. Permanganate-re
31、ducing substances (expressed as O) 0,02 % max. 1) Reagent solutions (RS) a) Hydrochloric acid, methanolic standard volumetric solution, c(HCl)=0,5mol/l. Transfer 84ml of hydrochloric acid, c(HCl)=6mol/l, to a1000ml one-mark volumetric flask and dilute to the mark with the methanol (R18). Standardize
32、 daily against a standard volumetric sodium hydroxide solution, c(NaOH)=0,5mol/l, using0,2ml of the phenolphthalein (IS4.3.9*) IUPAC name:3,3-bis(4-hydroxyphenyl)phthalide. The reagent is best handled in an automatic burette assembly. b) Morpholine, 0,5mol/l methanolic solution. Dilute 44ml of redis
33、tilled morpholene to1litre with the methanol (R18). To facilitate removal of aliquots fit the bottle with a two-hole rubber stopper and insert a50ml pipette through one hole so that the tip dips below the surface of the liquid. Through the other hole insert a short piece of glass tubing to which is
34、attached a rubber atomizer bulb. 2) Indicator solution (IS) Methyl yellow methylene blue, mixed solution. Dissolve1,0g of methyl yellow Cl11020 and0,1g of methylene blue Cl52015 in125ml of the methanol(R18). 3) IUPAC name: N,N-dimethyl-4-(phenylazo)aniline. 4) IUPAC name: 3,7-bis(dimethylamino-5 4 -
35、phenothiazin-5-ylium) chloride.BS6376-3:1989 BSI 01-2000 3 R 41.3.5 Copper, iron and lead Determine these elements by AAS according to GM29, using the following conditions: R 41.3.6 Permanganate-reducing substances To 10 ml of the test solution(R41.2) add0,5ml of potassium permanganate solution(0,32
36、%) and allow to stand for5min. The pink colour shall not disappear completely. Element Concentration of solution Flame Resonance line nm Cu Evaporate37ml (40g) of the sample, dissolve the residue with3ml of warm hydrochloric acid (R13) and dilute to20ml with water. Air-ethine 324,7 Fe 248,3 Pb 217,0
37、BS6376-3:1989 4 BSI 01-2000 R 42 Ammonium iron(II) sulfate hexahydrate (NH 4 ) 2 Fe(SO 4 ) 2 .6H 2 O Relative molecular mass: 392,14 R 42.1 Specification R 42.2 Preparation of test solution Dissolve 10 g of the sample in water with the addition of2ml of sulfuric acid solution (96%) and dilute to200m
38、l with water (the solution shall be clear). R 42.3 Tests R 42.3.1 Assay Weigh, to the nearest0,0001g, about1,5g of the sample, dissolve in water and add20ml of sulfuric acid solution(16%) and2ml of the phosphoric acid(R22). Titrate with standard volumetric potassium permanganate solution, c(1/5KMnO
39、4 )=0,1mol/l, to a faint pink colour. 1,00ml of potassium permanganate solution, c(1/5KMnO 4 )=0,100mol/l, corresponds to0,039214g of (NH 4 ) 2 Fe(SO 4 ) 2 .6H 2 O. R 42.3.2 pH Determine the pH of a5% solution of the sample according to GM31.1, using a calibrated pH meter. R 42.3.3 Chloride Take 30
40、ml of the test solution (R42.2), add5ml of the nitric acid(R19), heat to boiling and after cooling apply GM2. Prepare a standard matching solution, using10ml of the test solution and1ml of the chloride SSII(1ml 0,001%Cl). R 42.3.4 Phosphate Dissolve1g of the sample in20ml of water, oxidize with4ml o
41、f the nitric acid(R19) and remove the nitrogen oxides by boiling. Cool, dilute to80ml with water and applyGM4. Prepare a standard matching solution, using2ml of the phosphateSSII (2ml 0,002%PO 4 ). Assay (NH 4 ) 2 Fe(SO 4 ) 2 .6H 2 O 99 % min. pH (5% solution) 3 to 5 Chloride (Cl) 0,001 % max. Phosp
42、hate (PO4) 0,002 % max. Calcium (Ca) 0,01 % max. Copper (Cu) 0,002 % max. Iron(III) (Fe) 0,02 % max. Lead (Pb) 0,002 % max. Magnesium (Mg) 0,01 % max. Manganese (Mn) 0,05 % max. Potassium (K) 0,01 % max. Sodium (Na) 0,01 % max. Zinc (Zn) 0,003 % max.BS6376-3:1989 BSI 01-2000 5 R 42.3.5 Calcium, copp
43、er, lead, magnesium, manganese and zinc Determine these elements by AAS according to GM29, using the following conditions: R 42.3.6 Iron(III) Dissolve0,5g of the sample in10ml of carbon dioxide-free water containing0,5ml of hydrochloric acid solution(25%). Add2ml of 5-sulfosalicylic acid solution(10
44、%) and close the test tube. After15min, the red coloration of the resulting solution shall be not more intense than that of a similarly prepared standard matching solution, using5ml of the ironSSII (5ml 0,01%Fe). R 42.3.7 Potassium and sodium Determine these elements by FES according to GM30, using
45、the following conditions: Element Concentration of solution Flame Resonance line nm Ca Test solution (R42.2) Air-ethine 422,7 Cu 324,7 Pb 217,0 or 283,3 Mg 10 ml of the test solution (R42.2) diluted to100ml 285,2 Mn 279,5 Zn Test solution (R42.2) 213,9 Element Concentration of solution Flame Wavelen
46、gth nm K Test solution(R42.2) Air-ethine 766,5 Na 589,0BS6376-3:1989 6 BSI 01-2000 R 43 Ammonium iron(III) sulfate dodecahydrate NH 4 Fe(SO 4 ) 2 .12H 2 O Relative molecular mass: 482,18 R 43.1 Specification R 43.2 Tests R 43.2.1 Assay Weigh, to the nearest0,0001g, about2g of the sample, dissolve in
47、20ml of water, add5ml of hydrochloric acid solution(15%),3g of the potassium iodide(R25) and set aside in the dark for5min. Titrate with a standard volumetric sodium thiosulfate solution, c(Na 2 S 2 O 3 )=0,1mol/l, using the starch(IS4.3.11*). 1,00 ml of sodium thiosulfate solution, c(Na 2 S 2 O 3 )
48、=0,100mol/l, corresponds to0,04822g of NH 4 Fe(SO 4 ) 2 .12H 2 O. R 43.2.2 Water-insoluble matter Take 20g of the sample and apply GM1. The mass of the residue shall not exceed1mg. R 43.2.3 Chloride Dissolve2g of the sample in50ml of water and apply GM2. Prepare a standard matching solution, using1m
49、l of the chlorideSSII(1ml 0,0005%Cl). R 43.2.4 Copper, lead, magnesium, manganese and zinc Determine these elements by AAS according to GM29, using the following conditions: R 43.2.5 Iron(II) Dissolve1,5g of the sample in30ml of water, add1ml of sulfuric acid(15%) and0,1ml of a freshly prepared solution of potassium hexacyanoferrate(III)(5%). Compare any resulting blue colour with that of a solution prepared from0,5g of the sample,30ml of water,1ml of sulfuric acid(15%),0,1ml of a freshly prepared solution of potassium hexacyanoferrate
