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1、BRITISH STANDARD BS 2000-182:2006 IP 182:2006 Methods of test for petroleum and its products Part 182: Determination of inorganic acidity of petroleum products Colour indicator titration method (Identical with IP 182:2006) ICS 75.080 ? BS 2000-182:2006 This British Standard was published under the a
2、uthority of the Standards Policy and Strategy Committee on 24 January 2006 BSI 24 January 2006 ISBN 0 580 47592 1 National foreword This British Standard reproduces verbatim IP 182:2006 and implements it as the UK national standard. It supersedes BS 2000-182:2005 which is withdrawn. The UK participa
3、tion in its preparation was entrusted to Technical Committee PTI/13, Petroleum testing and terminology, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Energy Institute, under the brand of IP publishes and sells all
4、parts of BS 2000, and all BS EN petroleum test methods that would be part of BS 2000, both in its annual publication “Standard methods for analysis and testing of petroleum and related products and British Standard 2000 parts” and individually. Further information is available from: Energy Institute
5、, 61 New Cavendish Street, London W1G 7AR. Tel: 020 7467 7110. Fax: 020 7255 1472. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index
6、”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confe
7、r immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate th
8、em in the UK. Summary of pages This document comprises a front cover, an inside front cover, pages 1 to 4, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments
9、 182.1 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. IP 182/06 BS 2000-18
10、2 : 2006 Determination of inorganic acidity of petroleum products Colour indicator titration method 1Scope This standard specifies a method for determining the water soluble inorganic (strong) acid content of used and unused lubricating oils, fuel oils, and petrolatum. NOTE 1 - Oils containing addit
11、ives that can be extracted with water may give erroneous results. NOTE 2 - The results may not be numerically identical with those obtained when other colour indicators or techniques are used. 2Normative references The following standards contain provisions which, through reference in this text, con
12、stitute provisions of this Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated be
13、low. ISO 3696, Water for analytical laboratory use Specification and test methods 3Principle The inorganic acids in the oil are extracted with boiling water in a specified apparatus. After separation of the aqueous and oil layers an extract of the aqueous layer is titrated with standardized alkali u
14、sing bromophenyl blue indicator. 4Reagents and materials Use only chemicals and reagents of recognised analytical grade and water conforming to grade 3 of ISO 3696. 4.1Potassium hydrogen phthalate 4.2Potassium hydroxide solution 0,1 mol/l Either prepare a solution in accordance with 4.2.1 or use a c
15、ommercially available potassium hydroxide solution of equivalent concentration and purity. 4.2.1 Dissolve 6 g potassium hydroxide in 1 l in water and standardize using potassium hydrogen phthalate in accordance with 4.2.2. The reagent shall be protected against carbon dioxide absorption and restanda
16、rdized frequently enough to detect concentration changes of 0,0005 mol/l. 4.2.2 Dry a quantity of potassium hydrogen phthalate (4.1) in an oven at approximately 120 C for approximately 2 h. Place in a desiccator and allow to cool. Weigh between 0,1 g to 0,2 g to the nearest 0,1 mg into a 250 ml flas
17、k and record this mass. Add approximately 50 ml of carbon dioxide free water and swirl to dissolve. Add 2 drops of bromophenol blue solution (4.3) and titrate to neutral end point with the potassium hydroxide solution (4.2). Carry out a blank determination using the same volume of carbon dioxide fre
18、e water. Calculate the concentration C, in moles per litre, of the potassium hydroxide solution from the equation: C = 1 000 m 204,23 (V1 - V0) where m is the mass of potassium hydrogen phthalate; V1 is the volume of potassium hydroxide solution for the titration; V0 is the volume of potassium hydro
19、xide used for the blank. INORGANIC ACIDITY - COLOUR INDICATOR, IP 182 182.2 4.3 Bromophenol Blue 0,04% solution Dissolve 0,4 g bromophenol blue in 200 ml 95% ethanol (4.4). Add 6 ml 0,1 mol/l potassium hydroxide solution (4.2) and make up to 1 l with water. 4.4Ethanol, approximately 95% V/V 4.5Tolue
20、ne, general purpose reagent grade. 4.6Water, carbon dioxide free, see note 3. NOTE 3 - A suitable way of preparing carbon dioxide free water is to place approximately 100 ml of water (conforming to ISO 3696 Grade 3) in a 250 ml conical flask (5.3), heat to boiling on either a hot plate or gas burner
21、 and boil for 2 min to 3 min. Remove the flask and its contents from the heat and insert a guard tube (5.7) filled with soda lime (4.7) and cool to ambient temperature before use. 4.7Soda lime, for the guard tube. 5Apparatus 5.1Extraction apparatus, made glass, con- forming to the dimensions given i
22、n Figure 1, and consisting of the following component parts: 5.1.1 Boiling flask, capacity approximately 500 ml. 5.1.2 Hopkins reflux condenser, having a vapour outlet connected by a rubber tube to an outside vent or to a suction hood. 5.1.3 Thistle tube, capacity approximately 70 ml, with a line in
23、dicating the approximate 50 ml level. 5.1.4 Heating tube, containing a chimney for increasing convection in the liquid. 5.1.5 Heating coil, 250 W, consisting of a suitable gauge of nichrome wire. 5.1.6 Rheostat, of suitable resistance and capacity, for regulating the heater. 5.2 Measuring cylinder,
24、100 ml capacity. 5.3 Conical flask x 3, glass stoppered approximately 250 ml capacity. 5.4 Filter paper, course filtration grade, approximately 125 mm diameter. 5.5 Filter funnel 5.6 Burette, 10 ml capacity 5.7Glass guard tube, with ground glass joint to fit the conical flask (5.3). 6Procedure 6.1Us
25、ing the measuring cylinder (5.2) place 100 ml distilled water into the extraction apparatus switch on and bring to the boil. Switch off the heater. 6.2Weigh 25g 0,1 g of the test material into a conical flask (5.3) and add approximately 75 ml toluene (4.5) and swill until dissolved. 6.3 Add the tolu
26、ene solution to the water in the extraction apparatus. Switch on and bring to the boil. Using the rheostat adjust the heater such that the mixture boils vigorously. After 15 min turn off the heater and allow the mixture to cool and to separate. 6.4 Place the filter funnel (5.5) fitted with a filter
27、paper (5.4) into a 250 ml flask (5.3) and locate beneath the stopcock of the extraction apparatus. 6.5 Undo the stopcock and run off the separated aqueous layer through the filter paper into the 250 ml flask. 6.6 Using the measuring cylinder (5.2) measure 50 ml of the filtrate into a clean dry 250 m
28、l flask. NOTE 4 - If separation of the oil and water mixture is poor and the stipulated volume of extract is not obtainable a smaller volume may be used for the titration, though results may be less precise. 6.7 Add 2 drops of bromophenol blue indicator (4.3) and using the burette (5.6) titrate with
29、 standard potassium hydroxide solution (4.2) to a neutral end point. Record the volume of potassium hydroxide solution used. 7Calculation 7.1Calculate the inorganic acidity of the sample using the following equation: Inorganic acidity (mg KOH/g) = 4,5 M T where M is the molarity of potassium hydroxi
30、de solution; INORGANIC ACIDITY - COLOUR INDICATOR, IP 182 182.3 3 2 DIA 5 3 5 30 - 32 BEADS (1 DIA b) the type and complete identification of the product tested; c) the result of the test (see clause 8); d) any deviation, by agreement or otherwise, from the standard procedures specified; e) the date
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