1、INTERNATIONAL STANDARD ISO 10307-2 Second edition 2009-02-01 Reference number ISO 10307-2:2009(E) ISO 2009 Petroleum products Total sediment in residual fuel oils Part 2: Determination using standard procedures for ageing Produits ptroliers Insolubles existants dans les fuel-oils rsiduels Partie 2:
2、Dtermination laide de mthodes de vieillissement de rfrenceISO 10307-2:2009(E) ii ISO 2009 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which
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7、 Published in SwitzerlandISO 10307-2:2009(E) ISO 2009 All rights reserved iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through IS
8、O technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates c
9、losely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. D
10、raft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this do
11、cument may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 10307-2 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants. This second edition cancels and replaces the first edition (ISO 10307-2:1993), wh
12、ich has been technically revised. ISO 10307 consists of the following parts, under the general title Petroleum products Total sediment in residual fuel oils: Part 1: Determination by hot filtration Part 2: Determination using standard procedures for ageingISO 10307-2:2009(E) iv ISO 2009 All rights r
13、eserved Introduction Experience has shown that the precipitation of asphaltenes from a residual fuel oil in the form of sediment can occur during storage and handling. Such sediment can cause severe difficulties, and in extreme cases can render the fuel unfit for use. Once out of solution, it is ext
14、remely difficult to repeptize the asphaltenes into their original state. Fuel pre-treatment designed to accelerate the ageing/sedimentation process, followed by filtration, is a well- established technique for testing whether sediment from residual fuel oils will precipitate during storage and handl
15、ing. This could involve thermal ageing (heating to a specified temperature for a specified time) or chemical ageing (addition of a specified amount of a normal alkane to test whether the balance between the required aromaticity of the asphaltenes and the available aromaticity of the oil phase is dis
16、turbed to the extent that asphaltene precipitation occurs). A means of predicting the presence of a reserve of stability to sedimentation in residual fuel oil during storage and handling is thus a useful tool in the petroleum products industry.INTERNATIONAL STANDARD ISO 10307-2:2009(E) ISO 2009 All
17、rights reserved 1 Petroleum products Total sediment in residual fuel oils Part 2: Determination using standard procedures for ageing WARNING The use of this part of ISO 10307 could involve hazardous materials, operations and equipment. The document does not purport to address all of the safety probl
18、ems associated with its use. It is the responsibility of the user of this part of ISO 10307 to establish appropriate safety and health practices, and determine the applicability of regulatory limitations prior to use. 1S c o p e This part of ISO 10307 specifies two procedures A (thermal) and B (chem
19、ical) for the accelerated ageing of residual fuel oils. When combined with the hot filtration method specified in ISO 10307-1, these procedures permit the prediction of fuel oil stability, as affected by sedimentation, during storage and handling of the fuel oils. NOTE For the purposes of this Inter
20、national Standard, the terms “ ” and “ ” are used to represent mass and volume fractions of a material, respectively. These expressions are deprecated under the International System and according to ISO 31-0, Quantities and units Part 0: General principles, which specifies that mass and volume fract
21、ions be expressed as “mass fraction of xx %” (symbol ) and “volume fraction of xx %” (symbol ). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest e
22、dition of the referenced document (including any amendments) applies. ISO 1773:1997, Laboratory glassware Narrow-necked boiling flasks ISO 10307-1:2009, Petroleum products Total sediment in residual fuel oils Part 1: Determination by hot filtration 3 Terms and definitions For the purposes of this do
23、cument, the following terms and definitions apply. 3.1 potential total sediment total sediment, determined by ISO 10307-1, after ageing a sample of residual fuel for at under prescribed conditions 3.2 accelerated total sediment total sediment, determined by ISO 10307-1, after dilution of a sample of
24、 residual fuel with hexadecane in the ratio of per of sample under carefully controlled conditions, followed by storage for at % (m/m) % (V/V) 24 h 100 C 1ml 10 g 1h 100 CISO 10307-2:2009(E) 2 ISO 2009 All rights reserved 4P r i n c i p l e 4.1 General The total sediment is determined after accelera
25、ted ageing in accordance with either 4.2 or 4.3, followed by hot filtration in accordance with ISO 10307-1. The ageing is carried out in duplicate (see Note to 8.1). 4.2 Thermal ageing (Procedure A) A sample of residual fuel oil is subject to ageing at for under specified conditions. 4.3 Chemical ag
26、eing (Procedure B) A sample of residual fuel oil is diluted with a specified amount of hexadecane (cetane) under carefully controlled conditions. It is then heated to for . 5 Apparatus 5.1 Ageing bath, comprising an electrically heated oil bath, capable of maintaining a temperature of , fitted with
27、air wells of inner dimension and depth , as illustrated in Figure 1. 5.2 Ageing bath temperature-measuring device, capable of measuring the temperature in the range fromto with an accuracy of (see Figure 1). 5.3 General-purpose temperature-measuring device, capable of measuring the temperature in th
28、e range from to with an accuracy of . 5.4 Air condenser, glass, of outer diameter and length . NOTE The air condenser preferably matches the conical flask (5.9). Alternatively, the air condenser can be attached by means of a cork, bored to accommodate the air condenser. 5.5 Stoppers, to provide a ti
29、ght fit in the test jar. 5.6 Microburette, of minimum capacity , graduated in subdivisions or less. 5.7 Magnetic stirrer/hotplate, capable of being controlled by a surface-temperature-measuring device, (see 5.8), and with polytetrafluoroethylene (PTFE)-coated stirring bars, length . 5.8 Surface-temp
30、erature-measuring device, capable of measuring the temperature up to . 5.9 Conical flask, capacity, narrow neck, complying with ISO 1773. 5.10 Spatula, of polypropylene, chamfered ends, long. 5.11 Stirring rod, glass or PTFE (polytetrafluoroethylene), approximately long and in diameter. 5.12 Hexadec
31、ane distribution funnel, of borosilicate glass, capacity to , outlet orificediameter. NOTE Standard funnels meeting the above criteria are available commercially. 5.13 Portable warm air blower, for heating the microburette to minimum, if required. 5.14 High-speed mixer, of any convenient type with a
32、 minimum speed of . 100 C 24 h 100 C 1h 100 C 0,5 C 55 mm 120 mm 95 C 103 C 0,5 C 0 C 100 C 0,5 C 8mm 400 mm 5ml 0,02 ml 25 mm 200 C 50 ml 200 mm 150 mm 3mm 5ml 10 ml 0,4 mm 0,02 mm 20 C 400 rev/minISO 10307-2:2009(E) ISO 2009 All rights reserved 3 6R e a g e n t 6.1 Hexadecane (cetane), commercial-
33、grade normal hexadecane of purity, minimum. As hexadecane starts to solidify at approximately , store the bulk quantity at or above , or bring to this minimum temperature before use. NOTE Portable warm air blowers and/or water baths not more than are suitable for raising the temperature of the micro
34、burette or bulk hexadecane container. Key 1 test flask 2 air condenser 3 temperature-measuring device 4 air well 5 oil bath 6 hotplate or immersion heater a For well dimensions, see 5.1. Figure 1 Ageing bath 99 % 18 C 20 C 50 CISO 10307-2:2009(E) 4 ISO 2009 All rights reserved 7 Sampling and sample
35、preparation Follow the instructions given in ISO 10307-1:2009, Clauses 7 and 8. 8 Ageing procedures 8.1 General Prepare the filters in accordance with ISO 10307-1:2009, Clause 9. Carry out the ageing procedure on duplicate aliquots. NOTE The term “duplicate” as used in ISO 10307-1 has a specific mea
36、ning. ISO 10307-1 requires that a result be reported as the average of duplicate determinations. In order to facilitate this, and in order to ensure homogeneity, two aliquots are aged using the procedure given below, and each aliquot is tested once for sediment determination by hot filtration. 8.2 P
37、rocedure A Sediment determination using thermal ageing 8.2.1 Pour a aliquot of the homogenized sample into the conical flask (5.9), attach the air condenser (5.4), and place the sample in the well of the ageing bath (5.1) at for . 8.2.2 Remove the flask from the bath, replace the air condenser with
38、the stopper (5.5), and shake vigorously until all the sludge has been uniformly suspended. To check this, invert the flask and examine the bottom and walls of the flask for any sludge deposits, after allowing the oil to drain down from the inside walls of the flask. Remove stubborn deposits from the
39、 walls or bottom of the conical flask by scraping with the spatula (5.10). Re-shake and within initiate the procedure specified in ISO 10307-1:2009, Clause 10, for sediment determination by hot filtration. 8.3 Procedure B Sediment determination using chemical ageing 8.3.1 Heat the stirrer/hotplate t
40、o a surface temperature corresponding to the temperature at which the sample under investigation has a kinematic viscosity of approximately . NOTE (Local) overheating of the sample should be avoided when placed on a hotplate. Overheating can cause sample decomposition processes. Proper sample temper
41、ature control is therefore important. Placing the flask in a metal block, which is placed on the magnetic stirrer/hotplate, is found suitable. 8.3.2 Weigh of the homogenized sample into the conical flask and add a PTFE-coated stirring bar. Place the flask in the centre of the stirrer/hotplate contro
42、lled as described in 8.3.1 (see Note above) and adjust the stirring speed to approximately . After , slowly add of hexadecane (6.1) from the microburette (5.6) to the flask at a maximum rate of , while continuously stirring. Asphaltenes that are flocculated during the addition of hexadecane owing to
43、 lack of homogeneity are not easily peptized afterwards and can produce faulty results. Therefore, it is imperative that local over-dilution does not occur during the addition step. This is dependent on the maximum rate of addition, which can be controlled by positioning the microburette above a fun
44、nel (5.12), discharging the directly into the funnel neck and allowing the hexadecane to drip into the stirred sample by gravity. Direct addition of the hexadecane from the microburette is not recommended, but if carried out it is essential that the orifice diameter of the microburette not exceed ,
45、and that the overall tip diameter not exceed . NOTE The rate of mass addition can be determined by plotting mass transferred as calculated from the volume delivered by the burette (hexadecane density at is ) against time of delivery. 8.3.3 Pour the sample and hexadecane mixture into a fresh flask an
46、d attach the air condenser. Place the flask in the well of the oil bath at . Allow the flask to remain in the bath for . 25 g1g 100 C 0,5 C 24 h 15 min 1 min 50 mm 2 /s 25 g 0,2 g 200 r/min 10 min 2,5 ml 0,02 ml 1,0 ml/min 2,5 ml 0,02 ml 1,0 mm 5,0 mm 20 C 773,4 kg/m 3 50 ml 100 C 0,5 C 60 min 2 min
47、ISO 10307-2:2009(E) ISO 2009 All rights reserved 5 8.3.4 Remove the flask from the bath, replace the air condenser with the stopper (5.5) and shake vigorously until all the sludge has been uniformly suspended. To check this, invert the flask and examine the bottom and walls of the flask for any slud
48、ge deposits, after allowing the oil to drain down from the inside walls of the flask. Remove stubborn deposits from the walls or bottom of the flask by scraping with the spatula. Re-shake and within initiate the procedure specified in ISO 10307-1:2009, Clause 10, for sediment determinations by hot f
49、iltration. 9 Expression of results 9.1 Calculate the mass percentage of total sediment for each test specimen using Equation (1): (1) where is the total sediment, expressed as percentage by mass; is the mass of the test portion, expressed in grams; is the mass of the lower filter before filtration, expressed in milligrams; is the mass of the lower filter after filtration, expressed in milligrams; is the mass of the upper filter before filtration, ex
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