BS-5711-11-1979.pdf
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1、BRITISH STANDARD CONFIRMED OCTOBER 1989 BS 5711-11: 1979 Methods of Sampling and test for glycerol Part 11: Determination of propane-1,3-diol content: gas chromatographic method NOTEIt is recommended that this Part of BS 5711 be read in conjunction with the general information given in BS 5711-0 “Ge
2、neral introduction”, issued separately. UDC 661.188.1:547.426.1:543.062:547.424.12 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:10:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5711-11:1979 This British Standard, having been prepared under the direction of the Chemicals Standards Com
3、mittee, was published under the authority of the Executive Board and comes into effect on 30 November 1979 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference CIC/6 Draft for comment 75/53579 DC ISBN 0 580 10992 5 A British Standard does not purport to i
4、nclude 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 pages This document comprises a front cover, an inside front cover, pa
5、ges i and ii, pages 1 and 2, 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 table on the inside front cover. Amendments issued since publication Amd. No.Date of issueComments
6、 Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:10:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5711-11:1979 BSI 12-1999i Contents Page 0Introduction1 1Scope and field of application1 2References1 3Principle1 4Materials1 5Apparatus1 6Sampling1 7Procedure1 8Calculation2 9Test report2 P
7、ublications referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:10:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:10:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5711-11:1979 BSI 12-19991 0 Intro
8、duction As propane-1,3-diol and glycerol differ in polarity and have widely different vapour pressures at a given temperature, they are easily and directly separated by gas chromatography. A column packing which minimizes tailing is necessary and, for this purpose, either a polar stationary phase on
9、 an inert support or a porous polymer packing may be used. 1 Scope and field of application This British Standard describes a method for the determination of propane-1,3-diol in soap lye crude and hydrolyser crude glycerols. 2 References The titles of the publications referred to in this standard ar
10、e listed on the inside back cover. 3 Principle Separation of propane-1,3-diol and glycerol by gas chromatography. 4 Materials 4.1 Carrier and auxiliary gases 4.1.1 Carrier gas. Nitrogen, argon and helium are all suitable. 4.1.2 Auxiliary gases. Hydrogen and air are required for use with a flame ioni
11、zation detector. 4.2 Reagents. The reagents used shall be of a recognized analytical grade. 4.2.1 Ethanol, absolute, complying with the requirements of BS 507 or industrial methylated spirits, complying with the requirements of BS 3591. 4.2.2 Dodecan-1-ol, or diethylene glycol, internal standard. 4.
12、2.3 Propane-1,3-diol, calibration standard. 4.3 Column packing materials 4.3.1 Stationary phase. Polyethylene glycol polymers of average molar mass 20 000 or similar materials are suitable1). Polyesters such as polyethyleneglycol adipate (PEGA), have been used but are less satisfactory. 4.3.2 Suppor
13、t, diatomaceous earth, particle size 85 4m to 106 4m. NOTEA porous polymer may be used as an alternative to a stationary phase on a support. Chromosorb 102, for example, has been found suitable. 5 Apparatus 5.1 Gas chromatographic apparatus. A flame ionization detector is preferred. Care should be t
14、aken that, under the conditions of the analysis, both the detector and the amplifier are operating within their linear range. 5.1.1 Injection heater. A method of heating the injection zone to a temperature above that of the column shall be available. It is recommended that a glass liner should be us
15、ed. 5.2 Micro-pipette or micro syringe, complying with the requirements of BS 1428-D5. 5.3 Column and packing 5.3.1 Column. The column may be of glass or metal. For rapid analyses, a column 25 cm to 30 cm long is suitable but, for the maintenance of adequate resolution over an extended period, a col
16、umn length of at least 1 m is recommended. 5.3.2 Packing. Either a packing consisting of 9 parts by mass of the support (4.3.2) and 1 part by mass of the stationary phase (4.3.1) or the porous polymer (see note to 4.3.2). NOTEThe porous polymer is more suitable for repeated measurements on soap lye
17、glycerol or other glycerols with high water contents. 5.3.3 Preparation of the packed column. Any suitable method of packing may be used. The final column should have an efficiency of about 200 theoretical plates, measured using the internal standard at the temperature of operation. Test the column
18、with an approximately 0.5 % (m/m) solution of propane-1,3-diol in ethanol and ensure that, when using a test portion size and amplifier attenuation sufficient to give a propane-1,3-diol peak height of about 50 % full scale, there is no overlap between the ethanol peak and the propane-1,3-diol peak.
19、6 Sampling Prepare the laboratory sample as described in Part 2 of this British Standard. 7 Procedure It is not practicable to provide complete details of the operating procedure for every type of instrument which might be used, but the following generalizations may be made. 7.1 Injector temperature
20、: 175 C to 250 C. The temperature should be slightly higher than the column temperature. 1) Carbowax 20 M and Carbowax 20 M/TPA have been found suitable. Licensed Copy: sheffieldun sheffieldun, na, Mon Dec 04 15:10:50 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 5711-11:1979 2 BSI 12-1999 7.2 Colum
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