1、BRITISH STANDARD BS 5443:1977 Incorporating Amendment No. 1 Recommendations for A standard layout for methods of chemical analysis by gas chromatography UDC 001.818:543.544.25BS5443:1977 This British Standard, having been prepared under the directionof the Chemical Divisional Council, was publishedu
2、nder the authority ofthe Executive Board on 30November1977 BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference C/40/-/3 Draft for comment 72/52259 DC ISBN 0 580 09409 X Cooperating organizations The panel responsible for the preparation of this British S
3、tandard, which has been working under the direction of the Chemical Divisional Council, consists of representatives from the following Government departments and scientific and industrial organizations: British Gas Corporation British Pharmacopoeia Commission Chemical Industries Association Ltd Depa
4、rtment of Energy Department of Industry Laboratory of the Government Chemist Electricity Supply Industry in England and Wales Institute of Fuel Institute of Petroleum Institution of Gas Engineers Ministry of Defence National Coal Board Scientific Instruments Manufacturers Association SIRA Institute
5、Standardization of Tar Products Tests Committee Amendments issued since publication Amd. No. Date of issue Comments 7605 May 1993 Indicated by a sideline in the marginBS5443:1977 BSI 10-1999 i Contents Page Cooperating organizations Inside front cover Foreword ii Section 0. General 1 0.1 Scope 1 0.2
6、 References 2 Section 1. Recommended standard layout 1 Section 2. Notes on the application of the recommended standard layout 1 1 Scope and field of application 1 2 References 2 3 Definitions 2 4 Principle 2 5 Materials required 2 6 Apparatus 2 7 Sample 5 8 Procedure 5 9 Expression of results 9 10 N
7、otes on procedure, particularly with reference to hazards 10 11 Test report 10 12 Bibliographical references 10 13 Appendices 10 Section 3. Calculation formulae depending on the method of calibration used 11 1 Internal normalizations method 11 2 Internal standard method 11 3 External standard method
8、 11 4 Absolute method 11 5 Addition method 12 Section 4. Typical example of use of recommended standard layout 12 Introduction 12 1 Scope and field of application 12 2 Principle 12 3 Materials required 12 4 Apparatus 13 5 Sample 14 6 Procedure 14 7 Expression of results 17 8 Hazards 18 9 Test report
9、 19 10 Bibliographical references 19 Figure 1 Determination of styrene in polystyrene; typical chromatogram (not to scale) 18 Figure 2 Precision of test results 19 Table 1 Conditions of application of methods of calibration 7 Publications referred to Inside back coverBS5443:1977 ii BSI 10-1999 Forew
10、ord This British Standard, prepared under the direction of the Chemical Divisional Council, gives recommendations for a standard layout for methods of chemical analysis by gas chromatography. These recommendations have been compiled, in view of the diversity of apparatus and working methods availabl
11、e, to enable methods to be drafted in such a way as to ensure a stated reproducibility in results. It is recognized that such a standard cannot be regarded as exhaustive in its treatment. Users should therefore include any parameter not specifically mentioned therein, but known to affect the precisi
12、on of the method under consideration, in the most appropriate part of the recommended layout. On the other hand, items in the recommendations, if not applicable, should be omitted. The clauses and subclauses in such a document should be numbered consecutively in accordance with a point system. Altho
13、ugh based on recommendations given in ISO 2718, the content of this standard is different in that a) it has been essentially aligned, for uniformity, with the more general recommendations given in the more recently published ISO 78-2 and in BS 0-3; b) it gives more detailed guidance on the implement
14、ation of the recommendations; c) it contains an example of a gas chromatographic method of analysis drafted in accordance with the recommendations. (It is emphasized, however, that this example serves only to illustrate the use of the recommendations and does not constitute a British Standard method
15、 for the determination of styrene in polystyrene by gas chromatography.) This standard should be used in conjunction with BS 3282, BS 0-3. NOTEThe clause numbering of section 2 of this standard is to some extent duplicated in section 4. Care should therefore be taken, when making reference to this s
16、tandard, to give both the section and clause numbering. 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 lega
17、l obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages1 to 20, 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 tab
18、le on the inside front cover.BS5443:1977 BSI 10-1999 1 Section 0. General 0.1 Scope This British Standard gives recommendations for the layout for methods of chemical analysis by gas chromatography. 0.2 References The titles of the publications referred to in this standard are listed on the inside b
19、ack cover. Section 1. Recommended standard layout The following standard layout is recommended for methods of chemical analysis by gas chromatography. Title 1 Scope and field of application 2 References 3 Definitions 4 Principle 5 Materials required 6 Apparatus 7 Sample 8 Procedure 9 Expression of r
20、esults 10 Notes on procedure, particularly with reference to hazards 11 Test report 12 Bibliographical references 13 Appendices Guidance on the use of this layout is given in section 2 of this standard. Section 2. Notes on the application of the recommended standard layout NOTEThe numbering of the c
21、lauses and subclauses in this section refers to those used in the recommended standard layout (seesection 1). Title The title of the publication or standard should express its contents concisely and unambiguously, mentioning briefly the products concerned and the nature of the analysis. The title sh
22、ould always contain the words “by gas chromatography” and should be phrased either “Determination of . in . by gas chromatography”, or “The analysis of . by gas chromatography”. The phrase “the purity of” should not be used. 1 Scope and field of application This clause should contain precise details
23、 of the subject of the standard. The field of application, particularly, should be fully described and should contain the following information: a) the determination to be made; b) the products for which the method is suitable, in sufficient detail to prevent ambiguity; c) the physical state of the
24、sample unless clearly defined by b); d) the range(s) of concentration covered by the method; e) known limitations or interference in the method, arising from the state of the sample; f) any other special features of the method. To avoid repetition, where many substances are to be determined, a) and
25、d) may be more conveniently tabulated with retention times or other practical data elsewhere in the standard. Clause 1 then need only include a reference to the clause containing the table.BS5443:1977 2 BSI 10-1999 2 References This clause should list, or make reference to, all other standards that
26、are indispensable for the application of the method. 3 Definitions If it is necessary, for clarity, to give definitions of certain terms used in the standard, these definitions should be given in this clause. 4 Principle This clause should give a concise summary of the method used, from receipt of t
27、he original sample to the calculation and reporting of results, and the statement should be suitable for use as an abstract in other documents. It should make particular reference to the following: a) the method of obtaining a suitable chromatogram (including preparation of sample); b) features of t
28、he apparatus or technique; c) the method by which results are calculated. 5 Materials required The purpose of this clause is to ensure that all materials used are sufficiently defined for selection. Hazards should be indicated where they exist and, in these circumstances, reference should be made to
29、 clause 10 of the standard layout. The materials used should be listed as given in 5.1 to 5.3. 5.1 Carrier gas and auxiliary gases. The carrier gas and auxiliary gases should be named, together with the supply pressure requirements. The purity of the gases should be specified if necessary to the pro
30、per functioning of the method. Reference should be made, where appropriate, to established methods for determining the purity of the gases and for purifying them. 5.2 Materials for use in calibration and sample treatment. The materials to be used for calibration purposes or as sample diluents, sampl
31、e solvents or internal standards should be named and limits for the impurities given; suitable criteria should be given for the specific limits of peaks that interfere, by reference to 8.2. 5.3 Materials for the preparation of columns. The materials used to prepare the column, including, if relevant
32、, any solvent used to disperse the stationary phase, should be specified. Details of how to pack the column should, however, be specified in 6.3. 6 Apparatus This clause should specify the apparatus and facilities necessary to perform within the stated reproducibility of the method. The details give
33、n in 6.1 to 6.7 are intended for guidance. The efficiency of the column and of the recording apparatus should always be stated, preferably by reference to 6.3.4 and8.3.3 respectively. NOTEA British Standard specification for gas chromatographic equipment is in course of preparation. When available i
34、ts use is recommended, where appropriate, in specifying the components of the apparatus. 6.1 General description 6.1.1 Gas chromatographic system. The chromatographic system required should be briefly described, e.g.”Dual flame ionization detector, temperature-programmed chromatograph with heated in
35、jection block and column back-flush facilities. 6.1.2 Flow diagram. For clarity, it is recommended that a flow diagram be incorporated in all but the simplest cases.BS5443:1977 BSI 10-1999 3 6.1.3 Characteristics of the assembly (type of oven, temperature regulation, etc.) , special devices 6.1.3.1
36、Column temperature a) Isothermal temperature control range. The upper and lower temperature limits of the method should be specified. Nominal precision of temperature control may be given if required. b) Temperature programming. The programme required for the method should be stated, together with n
37、ominal precision limits for the temperature/time relationship. c) Temperature read-out. Minimum facilities for checking the temperature should be specified. 6.1.3.2 Detector temperature. The upper and lower range of temperature limits should, and the nominal precision of temperature control may, be
38、specified and should be compatible with the required test performance. 6.1.3.3 Special devices. Specialized equipment such as precolumn reaction units and back-flush systems should be adequately described. Where appropriate, suitable diagrams should be included. 6.1.4 Devices for the control of pres
39、sure or of the flow of carrier gases and auxiliary gases. The methods used for controlling the flow of carrier gases or other gases (such as those used for flame ionization detection or for back-flushing) should be specified, e.g. control of flow rate or pressure. Where gas flow is programmed, the m
40、inimum and maximum flow rates and/or pressures should be specified, together with the precision limits for the programme profile. Suitable equipment for checking flow rates and/or pressure should normally be specified, together with the required discrimination. The units should comply with the appro
41、priate requirements of 8.1. 6.2 Injection equipment 6.2.1 Injection device. The injection device, which is not normally permanently attached to the apparatus, should be specified in respect of type, capacity and, if necessary, the manufacturers reference, e.g. “10 4l glass injection syringe” or “10
42、ml gas-tight syringe”. 6.2.2 Injection system. The injection system is normally an integral part of the chromatographic apparatus and should be specified by type, e.g. “direct on-column”, “heated injection block”, “gas sampling valve with a sample volume of20ml”. Where appropriate, the material of c
43、onstruction (including that used for the injection septa), special design features, manufacturers reference and lubricants (where used) should be stated. Where the injection system is required to be heated, the appropriate nominal range of operating temperatures should be specified. Details should p
44、referably be given of suitable temperature monitoring facilities. 6.2.3 Flow splitter. If inlet splitters are required, nominal split ratios should be stated. If it is important, materials of construction and layout should be described; if necessary, the manufacturers reference should be given. 6.3
45、Columns (and precolumn if required) 6.3.1 Number. The number of columns should be stated. 6.3.2 Column details. This subclause should specify the column system required. The following information should always be given. a) The wall material, including any special pretreatment required. b) The packed
46、 length, in metres, and nominal internal diameter, in millimetres. c) Additional relevant information such as wall thickness, the composition of any end plugs used, details of connections and requirements for sealing compounds. The form of column should be specified only when necessary. The expected
47、 life of the column should be stated, either in hours at operating conditions or as a number of injections. This subclause should also indicate such requirements for the preparation of the column as are necessary to comply with the requirements of clause 8. Column packing should be specified in 6.3.
48、3.BS5443:1977 4 BSI 10-1999 6.3.3 Packing 6.3.3.1 General. This subclause should specify such requirements for the preparation of the column packing as are necessary to comply with the requirements of clause 8. The column packing should be clearly identified and should be characterized by the retent
49、ion parameters of selected calibration compounds. If a physical or chemical property of a packing component can be correlated with the retention behaviour, this property should be included in the description. It is preferable to use commercially available materials. However, if the liquid phase or active solid is not commercially available, adequate details of preparation should be given. The method of packing, if critical to the method, should be adequately described. These details should be suitably incorporated in 6.3.3.2 to 6.3.3.6. 6.3.3.2 Support. Special tre
