1、September 2011DEUTSCHE NORM Normenausschuss Materialprfung (NMP) im DINDIN-SprachendienstEnglish price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of
2、 sale for German Standards (DIN-Normen).ICS 75.080!$r“1927997www.din.deDDIN 51581-1Testing of petroleum products Determination of evaporation loss Part 1: Noack test,English translation of DIN 51581-1:2011-09Prfung von Minerallerzeugnissen Bestimmung des Verdampfungsverlustes Teil 1: Verfahren nach
3、Noack,Englische bersetzung von DIN 51581-1:2011-09Essais des produits ptroliers Dtermination de la perte de lvaporation Partie 1: Mthode de Noack,Traduction anglaise de DIN 51581-1:2011-09SupersedesDIN 51581-1:2003-02www.beuth.deDocument comprises 18 pages07.13 DIN 51581-1:2011-09 2 A comma is used
4、as the decimal marker. Contents Page 1 Scope . 4 2 Normative references . 4 3 Principle . 4 4 Apparatus 4 5 Reagents and materials . 14 6 Calibration of apparatus 15 7 Preparation of apparatus . 15 8 Reference measurement 16 9 Performing the measurement 17 10 Expression of result . 18 11 Precision 1
5、8 DIN 51581-1:2011-09 3 Foreword This standard has been prepared by Working Committee NA 062-06-61 AA Prfung von Schmierlen, sonstigen len und Paraffinen of the Fachausschuss Minerall- und Brennstoffnormung (Standardization of petroleum, fuels, lubricants and related products committee (FAM) of the
6、Normenauschuss Materialprfung (NMP) (Materials Testing Standards Committee). DIN 51581, Testing of petroleum products Determination of evaporation loss consists of the following parts: Part 1: Noack test Part 2: Gas chromatographic method Amendments This standard differs from DIN 51581-1:2003-02 as
7、follows: a) non-Woods metal equipment has been included; b) normative references have been updated. Previous editions DIN 51581: 1958-01, 1977-08, 1983-09 DIN 51581-1: 2003-02 DIN 51581-1:2011-09 4 1 Scope This standard specifies a method of determining the evaporation loss of lubricants using a Noa
8、ck tester. The test method relates to a given set of operating parameters, which may, however, be adapted to other conditions when required. The method specified in this standard uses Woods metal, which presents a high potential risk of danger owing to its cadmium content. Therefore, the test descri
9、bed should preferably be carried out using non-Woods metal equipment. DANGER Woods metal contains cadmium which is highly toxic and hazardous to the environment. Moreover, it is known to have a mutagenic and teratogenic effect whilst also being presumed to have a cancerogenic effect! 2 Normative ref
10、erences 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 edition of the referenced document (including any amendments) applies. DIN 1333, Presentation of numerical data
11、DIN 12785, Laboratory glassware Special purpose laboratory thermometers DIN EN 573-3, Aluminium and aluminium alloys Chemical composition and form of wrought products Part 3: Chemical composition and form of products DIN EN ISO 4259, Petroleum products Determination and application of precision data
12、 in relation to methods of test ISO 5272:1979, Toluene for industrial use Specifications 3 Principle A sample of lubricating oil is weighed into an evaporation crucible and heated at 250 C for 60 min while a constant flow of air is drawn through it. The loss in mass of the lubricating oil is measure
13、d. The reproducibility of the results depends on strictly adhering to the set-up of the equipment and following the test procedure as described. The use of automated equipment is permitted provided it complies with the requirements of this standard. 4 Apparatus 4.1 General A test apparatus as shown
14、in Figure 1 shall be used. The use of automated equipment is permitted provided it yields results equivalent to those obtained with the equipment described in this standard. All components, e.g. design of heating block, crucible, heat capacity etc. and all the glassware used shall comply with the re
15、quirements of this standard. DIN 51581-1:2011-09 5 Dimensions in millimetres Key 1 Noack tester 10 Silicone hose, 100 mm long 2 Woods metal 11 Discharge tube 3 Thermometer 12 Glass bottle of capacity 2 l 4 Contact thermometer 13 Inlet tube 5 Silicone hose, 40 mm long 14 Y-piece 6 Silicone hose, 300
16、mm long 15 Evaporation crucible 7 Manometer 16 Heating block 8 Vacuum pump 17 Bleed valve 9 T-piece, with bleed valve Figure 1 Test equipment with Noack tester 4.2 Noack tester The Noack tester consists of the following components: 4.2.1 Heating block (see Figure 2) The heating block is made of alum
17、inium alloy as in DIN EN 573-3, with jacket and base insulated against loss of heat. The heating block is heated electrically by a base and jacket heater, having a total power consumption sufficient to ensure that the test temperature is reached within three minutes of starting the test (see 8.9). I
18、MPORTANT In the equipment originally used the heat transfer from the heating block to the crucible is achieved by using Woods metal. Other apparatus, where the heat transfer is ensured by a mechanical procedure, are operated without Woods metal. All procedural steps described in this standard relate
19、 to Woods metal equipment and are to be adapted correspondingly when using other equipment. DIN 51581-1:2011-09 6 There is a circular recess in the centre of the heating block designed to accommodate the evaporation crucible. The space between the heating block and the crucible is filled with Woods
20、metal. To prevent the crucible from rising in the liquid metal bath, two locking bolts are provided on the block. There are two further holes at the same distance from the centre of the block, which are designed to accommodate the thermometers. The depth of these holes should be between 45 mm and 55
21、 mm, their exact depth depending on the correct insertion of the thermometer, to be determined to an accuracy of 0,1 mm. The depth of a hole to receive the recommended thermometer will be (48 1) mm. The heating block for use with Woods metal is shown in Figure 2. The design of the heating block of n
22、on- Woods metal equipment is different. When using current equipment the contact thermometer shown is no longer needed. Dimensions in millimetres Key 1 Jacket heater 4 Hole for overheating fuse 2 Hole for contact thermometer 5 Hole for thermometer, 11 mm 45 mm to 55 mm 3 Base heater 6 Hole for lock
23、screw Figure 2 Heating block of equipment for use with Woods metal DIN 51581-1:2011-09 7 4.2.2 Evaporation crucible with screw cover (see Figure 3 to Figure 10) The evaporation crucible is made of stainless steel. A thread for the cover is located above the support ring. The cover is made of nickel-
24、plated copper zinc alloy and has an internal conical surface to provide a tight seal. Three nozzles, made of hardened steel, permit air to flow through the cover. The extraction tube, which is bent downwards, is centrically fitted to the cover by a threaded joint so as to provide a tight seal. Dimen
25、sions in millimetres Figure 3 Locking bolt for securing the evaporation crucible when using Woods metal (made from a standard screw) DIN 51581-1:2011-09 8 Dimensions in millimetres Key 1 Sample level mark Figure 4 Crucible DIN 51581-1:2011-09 9 Dimensions in millimetres Key 1 3 nozzles Figure 5 Scre
26、w cover for crucible (nickel plated copper zinc alloy) DIN 51581-1:2011-09 10 Dimensions in millimetres Figure 6 Nozzle (hardened steel) Dimensions in millimetres Figure 7 Extraction tube seal DIN 51581-1:2011-09 11 Dimensions in millimetres Key*)1 Sealing flange, soldered 2 Tube, made of stainless
27、steel 3 Circular sealing grooves (0,5 mm deep) a Detail Part 1 Figure 8 Extraction tube *)Translators note: The numbering in the German original has been corrected here. DIN 51581-1:2011-09 12 Dimensions in millimetres Figure 9 Screwed flange DIN 51581-1:2011-09 13 Key 1 Screwed flange, Figure 9 4 S
28、crew cover for crucible, Figure 5 2 Extraction tube, Figure 8 5 Crucible, Figure 4 3 Extraction tube seal, Figure 7 Figure 10 Assembly of crucible and extraction tube 4.3 Balance, capable of being read to an accuracy of 0,01 g. 4.4 Crucible clamp and spanner. 4.5 Reamer, 2-mm in diameter. 4.6 Ball,
29、bearing grade, 3,5 mm in diameter. 4.7 Thermometer (e.g. BE 1/40/260 thermometer as in DIN 12785). 4.8 Contact thermometer. DIN 51581-1:2011-09 14 4.9 Glass Y-piece (see Figure 1, item no. 14), having an internal diameter of 4 mm. The upright arms, each 45 mm long, shall form an angle such that the
30、arm connected to the crucible extraction tube and the tube form a straight line. The vertical arm shall be 60 mm long, with a 45 bevel at its end. 4.10 Various glass tubes, extending into the 2 l glass bottles and having an internal diameter of 4 mm and a 45 bevel at the ends. 4.10.1 The discharge t
31、ube shall be bent at an angle of 80. The external arm shall be 50 mm long, while the arm extending into the 2 l glass bottle shall be 100 mm long. The total length of the discharge tube measures 150 mm. 4.10.2 The inlet tube shall be bent at an angle of 100. The external arm shall be approximately 5
32、0 mm long, while the arm extending into the 2 l glass bottle shall be 210 mm long and with its end 20 mm from the bottom of the bottle. 4.10.3 The discharge tube of the second glass bottle shall be bent at an angle of 90. The external arm shall be approximately 50 mm, while the arm extending into th
33、e glass bottle shall be 100 mm long. The total length of the discharge tube measures approximately 150 mm. 4.11 Two double neck glass bottles, each having a capacity of 2 l. The body of the bottle (without neck) shall be approximately 170 mm high. The necks shall be fitted with rubber stoppers havin
34、g holes to receive the inlet and discharge tubes. 4.12 Manometer, inclined form, capable of being read to an accuracy of 0,2 mm water column. 4.13 T-piece, made of glass, fitted with a bleed valve. 4.14 Vacuum pump. 4.15 Timer, capable of being read to an accuracy of 0,2 s. 4.16 Silicone hoses, cut
35、to size as shown in Figure 1, each with an internal diameter of 4 mm. 5 Reagents and materials 5.1 Woods metal, composition (indicated as percentages by mass): bismuth (50 %), lead (25 %), tin (12,5 %), cadmium (12,5 %), melting point at 70 C. 5.2 Toluene, grade 2 (as in ISO 5272:1979) or any other
36、suitable cleaning solvent. 5.3 Wad of cotton wool. 5.4 Fine corundum powder (e.g. standard corundum of particle size 240). 5.5 Protective gloves. 5.6 Cleaning brush. DIN 51581-1:2011-09 15 5.7 Reference oil for determining the evaporation loss For this determination a reference oil1)is to be used (e
37、.g. reference oil type CEC RL 208 or RL 223; each batch of these reference oils being given a serial number, e.g. RL 208/1). 6 Calibration of apparatus 6.1 Thermometers should be calibrated every six months, in accordance with standard laboratory practice. 6.2 The entire test apparatus shall be cali
38、brated at regular intervals. If in regular use, a reference measurement should be made at least after every tenth test, otherwise, before the first sample is introduced. 7 Preparation of apparatus 7.1 Owing to the emission of oil vapours, installation of the test assembly in a fume cupboard is recom
39、mended. The procedure described below is for the standard test assembly. If automated equipment is used, the manufacturers operating instructions shall be consulted in addition. 7.2 When using a test assembly with Woods metal, pour enough Woods metal into the recesses in the heating block for any ga
40、ps left after the evaporation crucible and the two thermometers are in place to be filled with molten metal. 7.3 Heat the block at full power (controller in position 3). As soon as the Woods metal melts, place the two thermometers in the holes provided so that their bulbs touch the bottom. Check the
41、 contact thermometer connections at the back of the heating block and set the block to the test temperature of (250 0,5) C by adjusting the contact thermometer and its power supply. Maintain this temperature for at least fifteen minutes with the controller in position 1 before starting a measurement
42、. 7.4 Assemble the rest of the apparatus without the crucible. 7.5 Place an empty crucible in the heating block and use the two locking bolts on the support ring to prevent the crucible from rising in the Woods metal bath. Check that the meniscus of the molten metal is flush with the upper edge of t
43、he hole. 7.6 Once the crucible is in place, the response of the manometer is checked. Set the manometer to zero with the bleed valve fully open before switching on the vacuum pump. After switching on the pump, adjust the bypass flow by slowly closing the bleed valve until the pressure reading on the
44、 scale of the manometer is 1,96 mbar. 7.7 Disconnect the hose and remove the crucible from the test assembly. Open the bleed valve again. 7.8 After switching off the vacuum pump and heating block, remove the thermometers from the molten Woods metal. 7.9 Clean the Y-piece and glass tubes to prevent b
45、uild-up of condensate. 1) Information on sources of supply is obtainable from Fachausschuss Minerall- und Brennstoffnormung (FAM), berseering 40, 22297 Hamburg, Germany. DIN 51581-1:2011-09 16 8 Reference measurement 8.1 Switch on the pump, heat up the heating block and, without the crucible in plac
46、e, check that the set-up of the test assembly is as shown in Figure 1. 8.2 Check that the crucible is clean and free of oil and carbonization residues. Thoroughly clean the crucible and its cover with solvent between consecutive measurements and dry them. NOTE Carbonization residues resistant to thi
47、s treatment may be removed by immersion in hot cleaning solution or by mechanical abrasion with extremely fine corundum powder using a wad of cotton wool impregnated with solvent. 8.3 Use the reamer to check that the three nozzles in the screw cover of the evaporation crucible are clear. 8.4 Run the
48、 ball, bearing grade, through the extraction tube to ensure that is clear. 8.5 Determine the mass of the crucible without its cover to an accuracy of 0,01 g. 8.6 Weigh (65 1) g of reference oil (see 5.7) to an accuracy of 0,01 g into the evaporation crucible without its cover. 8.7 Screw on the cover and tighten it with a spanner to ensure a tight seal. 8.8 Place the crucible in the recess in the heating block and use the two bolts on the support ring to prevent the crucib
