1、March 1991 UDC 621 392.2 : 665.765 : 620.1 : 542.93 DEUTSCHE NORM Determination of water separation ability of lubricating oils and low-flammability fluids after contact with steam DIN 51589 Part 1 Prfung von Schmierstoffen und verwandten Erzeugnissen; Bestimmung des Wasserabscheidevermgens nach Dam
2、pfbehandlung; Prfung von Schmierlen und schwerentflammbaren Flssigkeiten Supersedes August 1987 edition. Beuth Verlag GmbH. Berlin, has the exclusive right of sale for German Standards (DIN-Normen). 04.93 DIN 51 589 Engl. Price group 6 Sales No. O106 In keeping with current practice in standards pub
3、lished by the International Organization for Standardization (ISO), a comma has been used throughout as the decimal marker. Dimensions in mm 1 Scope and field of application This standard describes methods that serve to determine the water separation ability of a) lubricating oils of viscosity class
4、es up to and including IS0 VG 100 as specified in DIN 51 519, with a density of no more than 0,900 gim3 at 15 OC (method A), and to b) HFD fluids (anhydrous fluids; cf. DIN 51 502) of viscosity classes up to and including IS0 VG 46 as specified in DIN 51 519, with a density of more than 1 g/cm3 at 1
5、5 OC (method El), which may come into contact with steam and hot condensation water and are required to separate from the water quickly. 2 Concept For the purposes of this standard, water separation ability is the ability of lubricating oils or low-flammability fluids to separate from the condensate
6、 formed after steam treatment. 3 Unit The unit in which the water separation ability (settling time) is expressed is the second (s). 4 Principle The sample to be examined is placed in a cylindrical vessel and emulsified by a constant flow of steam, the latter being produced in a steam generator and
7、measured after condensation in a graduated cylinder connected to the cylindrical vessel. The settling time of the aqueous phase (method A) or the separation time of both phases (method 6) is then determi ned. Continued on pages 2 to 6 Page 2 DIN 51 589 Part 1 5 Apparatus The following apparatus shal
8、l be used. a) Emulsifier, equipped with steam generator, as shown in figure 1 ). b) Thermostat, capable of being maintained at (65f5) “C. c) Stopwatch. d) Oven, as specified in DIN 50011 Part 12, rated for temperatures of not less than 110 OC. e) Measuring ring, as shown in ligure 2 (method A). f) M
9、easuring ring, as shown in figure 3 (method E). DIN *) Cf. Explanatory notes. Figure 1. Emulsifier equipped with steam generator (cf. parts list for details) DIN 51 589 Part 1 Page 3 Table 1. Parts list for flgure 1 No. of items 1 - 1 1 1 1 1 - Notes DIN 12264 - A S 19 connector l) (with spherical g
10、round joint) Steam delivery tube made from DIN 12217 - 11 x 1 glass tube, with 2 connectors l) (with spherical ground joint) DIN 12264- BS 19 Emulsifying cylinder with connector 1 and with hook and fused-in DIN 12217 - 11 x 1 glass tube with connector (with spherical ground joint) DIN 12249- E 29/32
11、 DIN 12264 - A S 19 ) Ring mark on emulsifying cylinder at 100 mL Steam delivery tube with ground bevel end. Steam discharge attachment made of 35 X 1.25 tube with connector l) and with steam discharge tube made of DIN 12217 - 11 x 1 glass tube with connector l) (with spherical ground joint) DIN 12
12、249 - B 29/32 DIN 12264- BS 19 Allihn condenser 200 connector l) (with spherical ground joint) With DIN 12264-A S 19 DIN 12680- ME 250 graduated cylinder I I) The specified dimensions are mandatory and new apparatusshall becheckedforcomplianceon supply. 6 Reagents The following reagents shall be use
13、d. a) Toluene. b) Acetone. c) Concentrated sulfuric acid, H2SO4 *). d) Distilled or deionized water (referred to below as water for short). 7 Preparation Cf. figure 1 for Set-up of emulsifying apparatus. Pour 2 1 of water into the steam generator and mark the level reached. After each determination.
14、 top the water up to this level. After a total of ten determinations, empty the steam generator and, after cleaning, refill it with water. Prior to each determination, clean the emulsifying cylinder together with the steam discharge attachment by rinsing with toluene, then with acetone, concentrated
15、 sulfuric acid *) and water. Dry the cleaned apparatus in an oven at (105f2)OC. After cooling to an ambient temperature of 18 to 28 OC, fill the dry emulsifying cylinder with (100f 1) ml of sample at ambient temperature, taking care not to wet the wall of the cylinder above the level of the sample.
16、Heat the cylinder for not less than 15 minutes in a bath at (65f 5) “C. 8 Procedure Heat the water in the steam generator to boiling and pass steam through the delivery tube for two minutes. Remove the emulsifying cylinder from the bath and place it vertically in the apparatus with steam flowing thr
17、ough it. Allow the steam to act for a period of 20 minutes, measured with the stopwatch from the time of placing the emulsifying cylinder in the apparatus. Check the volume of condensate entering the graduated cylinder at five-minute intervals in order to verify whether the steam flow is constant. A
18、fter 20 minutes, thevolume of condensate shall be (205*5) mland the steam generator shall be adjusted to achieve this. Method A Just before the end of steam injection, push the measuring ring shown in figure 2 over the emulsifying cylinder. After 20 minutes, stop the flow of steam by simultaneously
19、opening the straight bore stopcock on the steam generator and switching off the heater. Set the zero mark of the measuring ring to the emulsioniair interface no more than two seconds after stopping the steam injection and start the stopwatch. Observe the drop in the oiliwater phase boundary and read
20、 the time on the stopwatch when it reaches the 55 mm mark. Discontinue the measurement if the observation time exceeds 1800seconds. To facilitate observation of the settling process and to illuminate the apparatus, it is recommended that a lamp be used that is placed to the side in front of or behin
21、d the emulsiying cylinder. Method B Just before the end of steam injection. push the measuring ring shown in figure 3 over the emulsifying cylinder so that its base touches the base of the emulsifying cylinder. Afler 20 minutes, stop the flow of steam by simultaneously opening the straight bore stop
22、cock on the vent tube and switching off the heater. Start the stopwatch and observe the rise in the aqueous phase in the sample. When the waterlsample phase boundary reaches the 65 mm mark, read off the time on the stopwatch. Discontinue the measurement if the observation time exceeds 1800 sec- onds
23、. To facilitate observation of the separation process and to illuminate the measurement zone, it is advisable to use a lamp fitted to the side in front of or behind the emulsifying cylinder. 9 Expression of results The water separation ability, .e. the time required for the settling or separation pr
24、ocess expressed in seconds, shall be reported to the nearest second, reference being made to this standard. If the water separation ability is less than 30 seconds, the result shall be reported as less than 30 seconds; if it exceeds 1800 seconds, it shall be reported as greater than 1800 seconds. Fo
25、r *), see page 2. Page 4 DIN 51 589 Part 1 DIN 439 -A M3 - 11H Spring, 5 mm long CulZn alloy washer, as specified in DIN 125 Part 1 DN 84 - M3 x 25 - 5.8 cheese head screw Material: DIN 1751 sheet made from CuZn37 F37 (material no.: 2.0321.26) as specified in DIN 17 670 Part 1 Figure 2. Measuring ri
26、ng for testing lubricating oils (method A) Other details as shown in Figure 3. Measuring ring for testing low-flammability fluids (method B) DIN 51 589 Part 1 Page 5 Absolute, in s 30 If the lubricating oil is filtered before being tested by method A, the filtration method used shall be stated along
27、 with the result. DIN 1333 Part 2 shall be taken into account when rounding to the last significant place. Relative, as a percentage of mean result - 10 Precision (Cf. DIN 51 848 Part 1) The following criteria shall be used in assessing the re- Repeatability (same operator, same apparatus) If two re
28、sults are obtained under repeatability conditions by the same operator, both results shall be considered acceptable and in conformity with this standard if they differ by no more than the values given in table 2. Reproduel bllity (different operators, different apparatus) If two separate laboratorie
29、s each obtain a result under reproducibility conditions, both results shall be considered acceptable and in conformity with thisstandard if they differ liability of results. by no more than the values given in table 2. Table 2. Repeatability and reproducibility Water separation ability, in s Method
30、A Method B Method A Method B Repeatabi I ity Absol Ute, Relative, as a percentage of mean result - I-+- Standards referred to DIN 84 DIN 125Part1 DIN 439Part1 DIN 1333Part2 DIN 1751 DIN 12 217 DIN 12 242 Part 1 DIN 12 244 Part 1 DIN 12 249 DIN 12 24 DIN 12 541 Part 1 DIN 12 680 Part 1 DIN 17 670 Par
31、t 1 DIN 50 O11 Part 12 DIN 51 502 DIN 51 519 DIN 51 848 Part 1 Product grad A slotted cheese head screws Product grade A washers with a hardness up to 250 HV, designed for use with hexagon head bolts and nuts Unchamfered hexagon thin nuts; product grade B Presentation of numerical data: rounding Col
32、d rolled copper and wrought copper alloy sheet and sheet cut to length; dimensions Laboratory glassware; borosilicate 3,3 glass tubes of outside diameter 4 rnm to 100 mm Laboratory glassware; interchangeable conical ground joints: dimensions and tolerances Laboratory glassware; interchangeable spher
33、ical ground joints; dimensions and tolerances Laboratory glassware; connectors with conical ground joint Laboratory glassware: connectors with spherical ground joint Laboratory glassware; straight bore stopcocks Laboratory glassware; graduated cylinders Copper and wrought copper alloy plate, sheet a
34、nd strip; properties Artificial climates in technical applications; air temperature as a climatological quantity in controlled- atmosphere test installations Designation of lubricants and marking of lubricant containers, lubricating equipment and lubrlcation points IS0 viscosity classification for i
35、ndustrial liquid lubricants Testing of petroleum products; precision: general; terminology and its application to petroleum standards specifying requirements Page 6 DIN 51 589 Part 1 Other relevant documents l Thoenes, H. W. Das Wasserabscheidevermgen von Minerallen als Beitrag zu ihrer Beurteilung
36、(Assessment of 2 Thoenec, H. W. Stand der Prfung von Schmierlen nach physikalischen und chemischen Untersuchungsverfahren petroleum products on the basis of their water separation ability), Brennstoff-Chemie, 1956: 37, 336-341. (Testing of lubricating oils using physical and chemical methods), Brenn
37、stoff-Chemie, 1959: 40, 123-128. Previous editions DIN 51 589: 11.63, 09.74; DIN 51 589 Part 1 :01.78, 08.87. Amendments The following amendments have been made to the August 1987 edition. a) The diameter of the emulsifying cylinder (cf. item no. 3 in figure 1) has been changed from 40-Prnm to 45-2m
38、m. b) Method B has been included for testing low-flammability fluids. c) The standard has been editorially revised. Explanatory notes This standard has been prepared by Technical Committee 661 Prfung von Schrnierlen, sonstigen &en und Paraffinen of Fachausschu Minerall- und Brennstotnormung of the N
39、ormenausschu Materialprfung (Materials Testing Standards Com mittee). Note on clause 5 Equivalent steam generators may be used. Test apparatus conforming to the January 1978 edition of this standard may be used for a transitional period of five years. Note on clauses 6 and 7 Acid-free, effective cle
40、ansing agents) which are biodegradable may be used instead of concentrated sulfuric acid. International Patent Classification G O1 N 33/28 l) Information on sources of supply is obtainable from DIN-Bezugsquellen fr normgerechte Erzeugnisse of DIN Deutsches Institut fr Normung eV., Burggrafenstrae 6, D-1000 Berlin 30.
