SIST ISO 2137:2008
(Main)Petroleum products and lubricants - Determination of cone penetration of lubricating greases and petrolatum
Petroleum products and lubricants - Determination of cone penetration of lubricating greases and petrolatum
This International Standard specifies several methods for the empirical estimation of the consistency of lubricating greases and petrolatum by measuring the penetration of a standardized cone. The National Lubricating Grease Institute (NLGI) classifies greases according to their consistency, as measured by the 60 strokes worked penetration. The NLGI classification includes nine consistency numbers or grades, each grade corresponding to a given range of worked penetration. The NLGI classification is given in ISO 6743-99. Clause 7 of this International Standard specifies four procedures for determining the consistency of lubricating greases by measuring the penetration of a full-scale cone. These procedures cover the measurement of unworked, worked, prolonged worked, and block penetrations. Penetrations up to 500 units can be measured. Clause 8 of this International Standard specifies methods for determining the consistency of lubricating greases when only small samples are available, by the use of cones a half-scale or quarter-scale of that used in Clause 7. The methods are applicable to greases having penetrations of 175 units to 385 units with the fullscale cone and are intended for use only if the size of the test sample prevents the use of cones described in Clause 7. They are not intended to replace the full-scale penetration as described in Clause 7, although a conversion to full-scale penetration is given in 10.2. See 8.1 for the limitations on the use of one-quarter-scale cones due to the poor precision.
Produits pétroliers et lubrifiants — Détermination de la pénétrabilité au cône des graisses lubrifiantes et des pétrolatums
L'ISO 2137:2007 sp�cifie les m�thodes suivantes, destin�es � une estimation empirique de la consistance des graisses lubrifiantes et des p�trolatums, par d�termination de la p�n�trabilit� d'un c�ne normalis�: quatre m�thodes de d�termination de la consistance des graisses lubrifiantes, par la mesure de la profondeur de p�n�tration d'un c�ne entier, recouvrant la mesure des profondeurs de p�n�tration du c�ne dans des graisses travaill�es, des graisses non travaill�es, des graisses travaill�es de fa�on prolong�e et des graisses en pain, pouvant �tre utilis�es pour mesurer des p�n�trabilit�s inf�rieures ou �gales � 500 unit�s; et des m�thodes permettant de d�terminer la consistance des graisses lubrifiantes quand on ne dispose que de petits �chantillons, gr�ce � l'utilisation de c�nes � l'�chelle 1/2 ou � l'�chelle 1/4 par rapport aux m�thodes pr�c�dentes, applicables aux graisses ayant des p�n�trabilit�s au c�ne entier allant de 175 unit�s � 385 unit�s.
Naftni proizvodi in maziva - Določevanje penetracije s stožcem za mazalne masti in vazeline
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.YD]HOLQHPetroleum products and lubricants - Determination of cone penetration of lubricating greases and petrolatum75.100MazivaLubricants, industrial oils and related products75.080Naftni proizvodi na splošnoPetroleum products in generalICS:Ta slovenski standard je istoveten z:ISO 2137:2007SIST ISO 2137:2008en01-april-2008SIST ISO 2137:2008SLOVENSKI
STANDARDSIST ISO 2137:19961DGRPHãþD
SIST ISO 2137:2008
Reference numberISO 2137:2007(E)© ISO 2007
INTERNATIONAL STANDARD ISO2137Third edition2007-12-01Petroleum products and lubricants — Determination of cone penetration of lubricating greases and petrolatum Produits pétroliers et lubrifiants — Détermination de la pénétrabilité au cône des graisses lubrifiantes et des pétrolatums
SIST ISO 2137:2008
ISO 2137:2007(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
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ISO 2007 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO's member body in the country of the requester. ISO copyright office Case postale 56 • CH-1211 Geneva 20 Tel.
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ii © ISO 2007 – All rights reserved
SIST ISO 2137:2008
ISO 2137:2007(E) © ISO 2007 – All rights reserved iiiContents Page Foreword.iv Introduction.v 1 Scope.1 2 Normative references.2 3 Terms and definitions.2 4 Principle.2 5 Apparatus.3 6 Sampling.5 7 Procedures for determining the cone penetration of lubricating grease —
Full-scale methods.14 7.1 Procedure for unworked penetration.14 7.2 Procedure for worked penetration.15 7.3 Procedure for prolonged worked penetration.16 7.4 Procedure for block penetration.16 8 Procedures for determining the cone penetration of lubricating grease —
Half- and quarter-scale cone method.17 8.1 General.17 8.2 Procedure for unworked penetration.17 8.3 Procedure for worked penetration.18 9 Procedure for determining the cone penetration of petrolatum.18 9.1 Preparation of the test portion.18 9.2 Penetration measurement.19 10 Calculation.19 10.1 Calculation of full-scale penetration.19 10.2 Conversion to full-scale penetration for the half- and quarter-scale cones.19 11 Expression of results.19 12 Precision.20 12.1 General.20 12.2 Repeatability.20 12.3 Reproducibility.20 13 Test report.21 Bibliography.22
SIST ISO 2137:2008
ISO 2137:2007(E) iv © ISO 2007 – All rights reserved Foreword SO (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 ISO 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 closely 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. Draft 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 document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 2137 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants. This third edition cancels and replaces the second edition (ISO 2137:1985), which has been technically revised. SIST ISO 2137:2008
ISO 2137:2007(E) © ISO 2007 – All rights reserved vIntroduction ISO 2137 was first published in 1972. A second edition was issued in 1985. This third edition cancels and replaces the first two editions, of which it constitutes a technical revision. The revision mainly concerns the dimensional tolerances of the various cones, to better fit with what is available from laboratory equipment suppliers. This revision is necessary because of all the quality plans and data integrity programmes established by numerous laboratories to comply with the various ISO quality standards. These quality standards require the total compliance of the cones with the dimensions indicated in ISO 2137. Unfortunately, most of the cones available do not conform to ISO 2137:1985 and users were obliged to establish waivers, which was difficult to justify to quality auditors. In the present edition of ISO 2137, the dimensional tolerances have been enlarged to allow most of the cones to fulfil the new requirements. A round-robin test has been performed with cones conforming to these new requirements and has demonstrated that the precision of the method is not altered by this change in the tolerances. Tolerances have been retained only on the characteristics where it has been established that they have a direct impact on the penetration determination, i.e. tip angle, tip height, tip top thickness, tip base diameter, cone angle, total mass of cone plus movable attachments.
SIST ISO 2137:2008
SIST ISO 2137:2008
INTERNATIONAL STANDARD ISO 2137:2007(E) © ISO 2007 – All rights reserved 1Petroleum products and lubricants — Determination of cone penetration of lubricating greases and petrolatum WARNING — The use of this International Standard can involve hazardous materials, operations and equipment. This International Standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this International Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1 Scope This International Standard specifies several methods for the empirical estimation of the consistency of lubricating greases and petrolatum by measuring the penetration of a standardized cone. The National Lubricating Grease Institute (NLGI) classifies greases according to their consistency, as measured by the 60 strokes worked penetration. The NLGI classification includes nine consistency numbers or grades, each grade corresponding to a given range of worked penetration. The NLGI classification is given in ISO 6743-99. Clause 7 of this International Standard specifies four procedures for determining the consistency of lubricating greases by measuring the penetration of a full-scale cone. These procedures cover the measurement of unworked, worked, prolonged worked, and block penetrations. Penetrations up to 500 units can be measured. Clause 8 of this International Standard specifies methods for determining the consistency of lubricating greases when only small samples are available, by the use of cones a half-scale or quarter-scale of that used in Clause 7. The methods are applicable to greases having penetrations of 175 units to 385 units with the full-scale cone and are intended for use only if the size of the test sample prevents the use of cones described in Clause 7. They are not intended to replace the full-scale penetration as described in Clause 7, although a conversion to full-scale penetration is given in 10.2. See 8.1 for the limitations on the use of one-quarter-scale cones due to the poor precision. NOTE 1 Unworked penetrations do not generally represent the consistency of greases in use as effectively as do worked penetrations. The latter are usually preferred for inspecting lubricating greases. NOTE 2 Penetration of block greases can be obtained on those products that are sufficiently hard to hold their shape. These greases generally have penetrations below 85 units. Clause 9 of this International Standard specifies a method for the determination of the consistency of petrolatum by measurement of the penetration of a full-scale cone, having penetrations up to 300 units. This method can also be used to estimate the consistency of slack waxes. SIST ISO 2137:2008
ISO 2137:2007(E) 2 © ISO 2007 – All rights reserved 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 edition of the referenced document (including any amendments) applies. ASTM D 4057, Standard Practice for Manual Sampling of Petroleum and Petroleum Products 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 cone penetration distance that a standardized cone penetrates into a test portion under standardized conditions of load, time, and temperature NOTE 1 The cone penetration is expressed in units of 0,1 mm. NOTE 2 Adapted from ISO 1998-2:1998, 2.80.001. 3.2 working subjecting a lubricating grease to the shearing action of a grease worker 3.3 unworked penetration cone penetration of a test portion that has received only minimum disturbance in transfer from the sample container to the cup of the grease worker 3.4 worked penetration cone penetration of a test portion after it has been subjected to a defined number of strokes in a grease worker 3.5 prolonged worked penetration cone penetration of a test portion which has been worked more than the defined number of strokes in worked penetration (see 3.4) 3.6 block penetration cone penetration determined on a test portion which is sufficiently hard to hold its shape without a container 4 Principle The cone penetration of lubricating grease is determined at 25 °C by releasing the cone assembly from the penetrometer and allowing the cone to drop for 5 s, and measuring the extent of the penetration. Unworked penetrations are determined on test portions transferred with a minimum of disturbance to a container suitable for test purposes. Worked penetrations are determined immediately after working the test portion for 60 double strokes in a standard grease worker. Prolonged worked penetrations are determined on test portions worked more than 60 double strokes. SIST ISO 2137:2008
ISO 2137:2007(E) © ISO 2007 – All rights reserved 3Block penetrations are determined on a freshly prepared face of a cube cut from a block of grease with a standard cutter. The cone penetration of petrolatum is determined by first melting and cooling a test sample under specified conditions, and then measuring the penetration as for lubricating grease. 5 Apparatus 5.1 Penetrometer, similar to that shown in Figure 1, capable of measuring, in tenths of a millimetre, the penetration of a cone in a material. The cone assembly or the table of the penetrometer shall be adjustable to enable accurate placement of the tip of the cone on the level surface of the material while maintaining a “zero” reading on the indicator. The cone shall fall, when released, without appreciable friction for at least 62 mm. The tip of the cone shall not hit the bottom of the sample container. The instrument shall be provided with level jig screws and a spirit level to maintain the cone shaft in a vertical position. NOTE The measurement of the penetration depth is performed using either mechanical devices (mechanical indicator) or electronic devices (digital indicator). 5.2 Cones 5.2.1 Full-scale cone, consisting of a conical body of magnesium or other suitable material with a detachable, hardened steel tip. Dimensions and tolerances shall be as shown in Figure 2. The total mass of the cone shall be 102,50 g ± 0,05 g and that of its movable attachments shall be 47,50 g ± 0,05 g. The attachments consist of a rigid shaft having a stop at its upper end and a suitable means at its lower end for engaging the cone. The interior construction may be modified to achieve the specified mass, provided that the general contour and mass distribution are not altered. The outer surface shall be polished to a very smooth finish. NOTE For penetrations up to 400 units, the optional cone as shown in Figure 3 can be used. 5.2.2 One-half-scale cone and shaft, made of steel, stainless steel or brass with a hardened steel tip of 45 Rockwell C hardness to 50 Rockwell C hardness, and constructed to conform to the dimensions and tolerances shown in Figure 4. The shaft may be made of stainless steel. The total mass of the cone and its movable attachments shall be 37,50 g ± 0,05 g. The mass of the cone shall be 22,500 g ± 0,025 g. The mass of the movable attachments shall be 15,000 g ± 0,025 g. 5.2.3 One-quarter-scale cone and shaft, consisting of a conical body of plastics or other low-density material with a hardened steel tip of 45 Rockwell C hardness to 50 Rockwell C hardness, and constructed to conform to the dimensions and tolerances shown in Figure 5. The shaft may be constructed of magnesium alloy. The total mass of the cone and its movable attachments shall be 9,380 g ± 0,025 g. The total mass of the cone and its movable attachments may be adjusted by adding small shot to the cavity of the shaft. 5.3 Grease workers 5.3.1 Full-scale grease worker, conforming to the dimensions shown in Figure 6. The sizes of non-dimensioned parts are not critical and may be varied according to individual requirements. Other methods of fastening the cover and securing the worker may be used. The grease worker may be constructed for either manual or mechanical operation. The design shall be such that a rate of 60 strokes per minute ± 10 strokes per minute, with a minimum length of 63 mm, can be maintained. A suitable thermometer, standardized at 25 °C, shall be provided for insertion through the vent valve. SIST ISO 2137:2008
ISO 2137:2007(E) 4 © ISO 2007 – All rights reserved 5.3.2 One-half-scale grease worker, conforming to the dimensions given in Figure 7. Other methods of fastening the cover and securing the worker may be used. The worker may be constructed for either manual or mechanical operation. The design shall be such that a rate of 60 strokes per minute ± 10 strokes per minute, with a minimum length of 35 mm, can be maintained. 5.3.3 One-quarter-scale grease worker, conforming to the dimensions given in Figure 8. Other methods of fastening the cover and securing the worker may be used. The worker may be constructed for either manual or mechanical operation. The design shall be such that a rate of 60 strokes per minute ± 10 strokes per minute, with a minimum length of 14 mm, can be maintained. 5.3.4 Overflow-ring (optional), conforming in principle to the illustration shown in Figure 6. This is a useful aid for returning displaced grease to the grease worker cup. The overflow ring shall be positioned at least 13 mm below the rim of the cup while making a penetration measurement. A rim 13 mm high is helpful. 5.4 Grease cutter, having a sharp, rigidly mounted, bevelled blade, essentially as shown in Figure 9. It is necessary that the blade be straight and sharpened as shown. 5.5 Water bath, capable of being maintained at 25,0 °C ± 0,5 °C and holding the assembled grease worker. If the bath is to be used for samples for unworked penetrations, a means shall be provided for protecting the grease surface from water. A cover shall also be provided to maintain the air temperature above the sample at 25 °C. An air bath, maintained at 25,0 °C ± 0,5 °C, is required for determining block penetration; a tightly sealed container placed in the water bath will suffice. NOTE A constant-temperature test room or an air bath can be used instead of a water bath. 5.6 Thermometer, calibrated at 25 °C, for the water bath or air bath. 5.7 Oven, capable of maintaining a temperature of 85 °C ± 2 °C, for melting the petrolatum samples. 5.8 Spatula, corrosion-resistant, square-ended, with a stiff blade approximately 32 mm wide and at least 150 mm long; for tests with half- and quarter-scale cones, the width should be approximately 13 mm. 5.9 Timer, graduated in 0,1 s. 5.10 Test-portion containers (for petrolatum), cylindrical, having a flat bottom 100 mm ± 5 mm in diameter and 65 mm or more in depth, constructed of metal at least 1,6 mm thick and, if necessary, each provided with a well-fitting watertight cover (see 9.1.3). Containers of the “ointment box” type having somewhat flexible sides should not be used, for these permit slight working of the petrolatum, due to flexing of the sides in handling. SIST ISO 2137:2008
ISO 2137:2007(E) © ISO 2007 – All rights reserved 56 Sampling Unless otherwise specified in a commodity specification, samples shall be drawn in accordance with ASTM D 4057. The samples shall be examined for any sign of non-homogeneity such as oil separation, phase changes or gross contamination. If any abnormal conditions are found, a new sample shall be drawn. The size of the sample shall be large enough to fill the requested number of cups.
Key 1 centring device NOTE This figure shows a combined assembly; generally, it is possible to displace vertically either the cone assembly or the plate. Figure 1 — Penetrometer SIST ISO 2137:2008
ISO 2137:2007(E) 6 © ISO 2007 – All rights reserved Dimensions in millimetres Tolerances on dimensions except where otherwise stated: ± 1 mm
Key 1 smooth and polished surface 2 hardened steel tip 3 shaft stainless steel — tight press fit a Do not round the edges. b Magnesium or any other suitable material. c ∅ 4 max., tight fit. d No shoulder. Total mass of cone: 102,50 g ± 0,05 g Total mass of movable attachments: 47,50 g ± 0,05 g Figure 2 — Cone of the penetrometer — Full-scale cone SIST ISO 2137:2008
ISO 2137:2007(E) © ISO 2007 – All rights reserved 7Dimensions in millimetres Tolerances on dimensions except where otherwise stated: ± 1 mm
Key 1 hardened steel tip 2 smooth and polished surface a Break all sharp edges. b Stainless steel. c Brass or corrosion resistant steel. d No shoulder. e ∅ 4 max., tight fit. f Machining to the required mass. Total mass of cone: 102,50 g ± 0,05 g Total mass of movable attachments: 47,50 g ± 0,05 g Figure 3 — Cone of the penetrometer — Optional cone SIST ISO 2137:2008
ISO 2137:2007(E) 8 © ISO 2007 – All rights reserved Dimensions in millimetres Tolerances on dimensions except where otherwise stated: ± 0,5 mm
Key 1 sharp corner 2 hardened steel tip a Machine this surface to give specified mass. b Polish all outside surfaces. Mass of cone: 22,500 g ± 0,025 g Mass of movable attachments: 15,000 g ± 0,025 g Total mass of cone and its movable attachments: 37,50 g ± 0,05 g Figure 4 — One-half-scale cone
SIST ISO 2137:2008
ISO 2137:2007(E) © ISO 2007 – All rights reserved 9Dimensions in millimetres Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key 1 hardened steel tip — Angle: 30° ± 30' Total mass of cone and its movable attachments: 9,380 g ± 0,025 g Figure 5 — One-quarter-scale cone SIST ISO 2137:2008
ISO 2137:2007(E) 10 © ISO 2007 – All rights reserved Dimensions in millimetres Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key 1 packing 6 vent valve 2 handle 7 adapter 3 thermometer 8 cover 4 packing nut 9 split rubber tube 5 thermometer gauge 10 overflow ring (optional) a optional, concentric to the interior of the cup, for use with the centring device. Plan of perforated plate (detail X) — circle 1 (∅ 33,35): 12 holes circle 3 (∅ 65,10): 22 holes
circle 2 (∅ 49,20): 17 holes all holes: 6,4 < ∅ < 6,53 Figure 6 — Full-scale grease worker SIST ISO 2137:2008
ISO 2137:2007(E) © ISO 2007 – All rights reserved 11Dimensions in millimetres Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key 1 base 2 grease plate 3 ring 4 shaft 5 cover 6 valve Material: stainless steel Capacity: 50 ml Figure 7 — One-half-scale grease worker SIST ISO 2137:2008
ISO 2137:2007(E) 12 © ISO 2007 – All rights reserved Dimensions in millimetres Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key 1 ring 2 cover 3 valve 4 grease plate 5 base 6 chamber: ∅ 19,0 × 17,5 height — Capacity with the plate, as shown: 4 ml Material: stainless steel Figure 8 — One-quarter-scale grease worker SIST ISO 2137:2008
ISO 2137:2007(E) © ISO 2007 – All rights reserved 13Dimensions in millimetres Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key 1 base 2 tube 3 blade 65 × 185 — Hardened steel. Grind both surfaces to 1,2 mm thick. Grind lower edge 4 plywood or hard wood, 6,4 mm thick. Grain of top perpendicular to blade Figure 9 — Grease cutter SIST ISO 2137:2008
ISO 2137:2007(E) 14 © ISO 2007 – All rights reserved 7 Procedures for determining the cone penetration of lubricating grease —
Full-scale methods 7.1 Procedure for unworked penetration 7.1.1 Preparation of test portion 7.1.1.1 Take sufficient sample (at least 0,5 kg) to overfill the cup of the grease worker (5.3.1). If the penetration is above 200 units, at least three times the amount needed to fill the cup is required. 7.1.1.2 Place the empty assembled grease worker, or metal container of equal inside dimensions, and an appropriate amount of the test sample in a metal container in the water bath (5.5) maintained at 25 °C (see the note to 5.5, and the last two paragraphs of this subclause) for sufficient time to bring the temperature of the sample to 25 °C ± 0,5 °C. Transfer from the container a test portion, preferably in one lump, to overfill the cup of the grease worker or metal container of equal inside dimensions (see below). Make this transfer in such a manner that the grease is worked as little as possible. Jar the container to drive out trapped air and pack the grease with the spatula (5.8), with as little manipulation as possible, to obtain a cupful without air pockets. Scrape off the excess grease extending above the rim, creating a flat surface, by moving the blade of the spatula, held inclined toward the direction of motion at an angle of approximately 45°, across the rim of the cup. Do not perform any further levelling or smoothing of the surface throughout the determination of unworked penetration, and carry out the measurement immediately. The penetration of soft greases is dependent upon the diameter of the container. Therefore, greases having unworked penetrations above 265 units should be tested in containers having the same diameter limitations as those of the grease worker cup. The results on greases having penetrations below 265 units are not significantly affected if the diameter of the container exceeds that of the grease worker cup. If the initial sample temperature differs from 25 °C by more than approximately 8 °C, or if an alternative method of adjusting the sample to 25 °C is used, sufficient additional time should be allowed to ensure that the test portion is at 25,0 °C ± 0,5 °C before proceeding. Also, if the sample is larger than 0,5 kg, sufficient additional time should be allowed to ensure that the test sample is at 25,0 °C ± 0,5 °C. Testing may proceed if the test portion is at a uniform temperature of 25,0 °C ± 0,5 °C. 7.1.2 Cleaning the cone and movable attachments Clean the penetrometer cone carefully before each test. Bending of the cone shaft can be avoided by holding it securely in its raised position whilst cleaning. Remove all grease or oil on the penetrometer shaft, as they can cause drag on the shaft assembly. Do not rotate the cone, as this can cause wear on the release mechanism. NOTE For penetrations up to 400 units, the optional cone as shown in Figure 3 can be used. 7.1.3 Penetration measurement 7.1.3.1 Place the cup on the penetrometer table, which shall be adjusted to a perfectly horizontal position, making certain that it cannot rock. Set the mechanism to hold the cone in the “zero” position, and adjust the apparatus carefully so that the tip of the cone just touches the surface of the test portion at the point specified in 7.1.3.2 or 7.1.3.3. Watching the shadow of the cone tip is an aid to accurate setting. For greases with penetrations over 400 units, centre the cup to within 0,3 mm of the tip of the cone. One way to centre the cup accurately is to use a centring device (see Figure 1). Release the cone shaft rapidly, allow it to drop for 5,0 s ± 0,1 s and re-clamp it in this position. The release mechanism shall not drag on the shaft. Gently depress the indicator shaft until it is stopped by the cone shaft and read the penetration from the indicator scale. 7.1.3.2 If the test portion has a penetration over 200 units, centre the cone carefully in the container. This test portion shall be used for only one test. SIST ISO 2137:2008
ISO 2137:2007(E) © ISO 2007 – All rights reserved 157.1.3.3 If the test portion has a penetration of 200 units or less, perform three tests in a single container, spacing the penetrations on three radii approximately 120° apart, and approximately midway between the centre and the side of the container, so that the cone neither strikes the side of the container nor impinges on the disturbed area made in a previous test. 7.1.3.4 Make a total of three determinations on the test portion [either in three containers (see 7.1.3.2) or in one container (see 7.1.3.3)] and record the values obtained. 7.2 P
...
INTERNATIONAL ISO
STANDARD 2137
Third edition
2007-12-01
Petroleum products and lubricants —
Determination of cone penetration of
lubricating greases and petrolatum
Produits pétroliers et lubrifiants — Détermination de la pénétrabilité au
cône des graisses lubrifiantes et des pétrolatums
Reference number
ISO 2137:2007(E)
©
ISO 2007
---------------------- Page: 1 ----------------------
ISO 2137:2007(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
COPYRIGHT PROTECTED DOCUMENT
© ISO 2007
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2007 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 2137:2007(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope .1
2 Normative references .2
3 Terms and definitions .2
4 Principle.2
5 Apparatus .3
6 Sampling.5
7 Procedures for determining the cone penetration of lubricating grease — Full-scale
methods .14
7.1 Procedure for unworked penetration.14
7.2 Procedure for worked penetration.15
7.3 Procedure for prolonged worked penetration .16
7.4 Procedure for block penetration .16
8 Procedures for determining the cone penetration of lubricating grease — Half- and
quarter-scale cone method.17
8.1 General.17
8.2 Procedure for unworked penetration.17
8.3 Procedure for worked penetration.18
9 Procedure for determining the cone penetration of petrolatum.18
9.1 Preparation of the test portion .18
9.2 Penetration measurement.19
10 Calculation.19
10.1 Calculation of full-scale penetration.19
10.2 Conversion to full-scale penetration for the half- and quarter-scale cones.19
11 Expression of results .19
12 Precision.20
12.1 General.20
12.2 Repeatability.20
12.3 Reproducibility.20
13 Test report .21
Bibliography .22
© ISO 2007 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 2137:2007(E)
Foreword
SO (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 ISO
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 closely 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. Draft 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 document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 2137 was prepared by Technical Committee ISO/TC 28, Petroleum products and lubricants.
This third edition cancels and replaces the second edition (ISO 2137:1985), which has been technically
revised.
iv © ISO 2007 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 2137:2007(E)
Introduction
ISO 2137 was first published in 1972. A second edition was issued in 1985. This third edition cancels and
replaces the first two editions, of which it constitutes a technical revision. The revision mainly concerns the
dimensional tolerances of the various cones, to better fit with what is available from laboratory equipment
suppliers. This revision is necessary because of all the quality plans and data integrity programmes
established by numerous laboratories to comply with the various ISO quality standards. These quality
standards require the total compliance of the cones with the dimensions indicated in ISO 2137. Unfortunately,
most of the cones available do not conform to ISO 2137:1985 and users were obliged to establish waivers,
which was difficult to justify to quality auditors. In the present edition of ISO 2137, the dimensional tolerances
have been enlarged to allow most of the cones to fulfil the new requirements. A round-robin test has been
performed with cones conforming to these new requirements and has demonstrated that the precision of the
method is not altered by this change in the tolerances. Tolerances have been retained only on the
characteristics where it has been established that they have a direct impact on the penetration determination,
i.e. tip angle, tip height, tip top thickness, tip base diameter, cone angle, total mass of cone plus movable
attachments.
© ISO 2007 – All rights reserved v
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INTERNATIONAL STANDARD ISO 2137:2007(E)
Petroleum products and lubricants — Determination of cone
penetration of lubricating greases and petrolatum
WARNING — The use of this International Standard can involve hazardous materials, operations and
equipment. This International Standard does not purport to address all of the safety problems
associated with its use. It is the responsibility of the user of this International Standard to establish
appropriate safety and health practices and determine the applicability of regulatory limitations prior
to use.
1 Scope
This International Standard specifies several methods for the empirical estimation of the consistency of
lubricating greases and petrolatum by measuring the penetration of a standardized cone.
The National Lubricating Grease Institute (NLGI) classifies greases according to their consistency, as
measured by the 60 strokes worked penetration. The NLGI classification includes nine consistency numbers
or grades, each grade corresponding to a given range of worked penetration. The NLGI classification is given
in ISO 6743-99.
Clause 7 of this International Standard specifies four procedures for determining the consistency of lubricating
greases by measuring the penetration of a full-scale cone. These procedures cover the measurement of
unworked, worked, prolonged worked, and block penetrations. Penetrations up to 500 units can be measured.
Clause 8 of this International Standard specifies methods for determining the consistency of lubricating
greases when only small samples are available, by the use of cones a half-scale or quarter-scale of that used
in Clause 7. The methods are applicable to greases having penetrations of 175 units to 385 units with the full-
scale cone and are intended for use only if the size of the test sample prevents the use of cones described in
Clause 7. They are not intended to replace the full-scale penetration as described in Clause 7, although a
conversion to full-scale penetration is given in 10.2. See 8.1 for the limitations on the use of one-quarter-scale
cones due to the poor precision.
NOTE 1 Unworked penetrations do not generally represent the consistency of greases in use as effectively as do
worked penetrations. The latter are usually preferred for inspecting lubricating greases.
NOTE 2 Penetration of block greases can be obtained on those products that are sufficiently hard to hold their shape.
These greases generally have penetrations below 85 units.
Clause 9 of this International Standard specifies a method for the determination of the consistency of
petrolatum by measurement of the penetration of a full-scale cone, having penetrations up to 300 units. This
method can also be used to estimate the consistency of slack waxes.
© ISO 2007 – All rights reserved 1
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ISO 2137:2007(E)
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 edition of the referenced
document (including any amendments) applies.
ASTM D 4057, Standard Practice for Manual Sampling of Petroleum and Petroleum Products
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
cone penetration
distance that a standardized cone penetrates into a test portion under standardized conditions of load, time,
and temperature
NOTE 1 The cone penetration is expressed in units of 0,1 mm.
NOTE 2 Adapted from ISO 1998-2:1998, 2.80.001.
3.2
working
subjecting a lubricating grease to the shearing action of a grease worker
3.3
unworked penetration
cone penetration of a test portion that has received only minimum disturbance in transfer from the sample
container to the cup of the grease worker
3.4
worked penetration
cone penetration of a test portion after it has been subjected to a defined number of strokes in a grease
worker
3.5
prolonged worked penetration
cone penetration of a test portion which has been worked more than the defined number of strokes in worked
penetration (see 3.4)
3.6
block penetration
cone penetration determined on a test portion which is sufficiently hard to hold its shape without a container
4 Principle
The cone penetration of lubricating grease is determined at 25 °C by releasing the cone assembly from the
penetrometer and allowing the cone to drop for 5 s, and measuring the extent of the penetration.
Unworked penetrations are determined on test portions transferred with a minimum of disturbance to a
container suitable for test purposes.
Worked penetrations are determined immediately after working the test portion for 60 double strokes in a
standard grease worker.
Prolonged worked penetrations are determined on test portions worked more than 60 double strokes.
2 © ISO 2007 – All rights reserved
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ISO 2137:2007(E)
Block penetrations are determined on a freshly prepared face of a cube cut from a block of grease with a
standard cutter.
The cone penetration of petrolatum is determined by first melting and cooling a test sample under specified
conditions, and then measuring the penetration as for lubricating grease.
5 Apparatus
5.1 Penetrometer, similar to that shown in Figure 1, capable of measuring, in tenths of a millimetre, the
penetration of a cone in a material.
The cone assembly or the table of the penetrometer shall be adjustable to enable accurate placement of the
tip of the cone on the level surface of the material while maintaining a “zero” reading on the indicator. The
cone shall fall, when released, without appreciable friction for at least 62 mm. The tip of the cone shall not hit
the bottom of the sample container. The instrument shall be provided with level jig screws and a spirit level to
maintain the cone shaft in a vertical position.
NOTE The measurement of the penetration depth is performed using either mechanical devices (mechanical
indicator) or electronic devices (digital indicator).
5.2 Cones
5.2.1 Full-scale cone, consisting of a conical body of magnesium or other suitable material with a
detachable, hardened steel tip.
Dimensions and tolerances shall be as shown in Figure 2. The total mass of the cone shall be
102,50 g ± 0,05 g and that of its movable attachments shall be 47,50 g ± 0,05 g. The attachments consist of a
rigid shaft having a stop at its upper end and a suitable means at its lower end for engaging the cone. The
interior construction may be modified to achieve the specified mass, provided that the general contour and
mass distribution are not altered. The outer surface shall be polished to a very smooth finish.
NOTE For penetrations up to 400 units, the optional cone as shown in Figure 3 can be used.
5.2.2 One-half-scale cone and shaft, made of steel, stainless steel or brass with a hardened steel tip of
45 Rockwell C hardness to 50 Rockwell C hardness, and constructed to conform to the dimensions and
tolerances shown in Figure 4.
The shaft may be made of stainless steel. The total mass of the cone and its movable attachments shall be
37,50 g ± 0,05 g. The mass of the cone shall be 22,500 g ± 0,025 g. The mass of the movable attachments
shall be 15,000 g ± 0,025 g.
5.2.3 One-quarter-scale cone and shaft, consisting of a conical body of plastics or other low-density
material with a hardened steel tip of 45 Rockwell C hardness to 50 Rockwell C hardness, and constructed to
conform to the dimensions and tolerances shown in Figure 5.
The shaft may be constructed of magnesium alloy. The total mass of the cone and its movable attachments
shall be 9,380 g ± 0,025 g. The total mass of the cone and its movable attachments may be adjusted by
adding small shot to the cavity of the shaft.
5.3 Grease workers
5.3.1 Full-scale grease worker, conforming to the dimensions shown in Figure 6.
The sizes of non-dimensioned parts are not critical and may be varied according to individual requirements.
Other methods of fastening the cover and securing the worker may be used. The grease worker may be
constructed for either manual or mechanical operation. The design shall be such that a rate of 60 strokes per
minute ± 10 strokes per minute, with a minimum length of 63 mm, can be maintained. A suitable thermometer,
standardized at 25 °C, shall be provided for insertion through the vent valve.
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ISO 2137:2007(E)
5.3.2 One-half-scale grease worker, conforming to the dimensions given in Figure 7.
Other methods of fastening the cover and securing the worker may be used. The worker may be constructed
for either manual or mechanical operation. The design shall be such that a rate of 60 strokes per minute
± 10 strokes per minute, with a minimum length of 35 mm, can be maintained.
5.3.3 One-quarter-scale grease worker, conforming to the dimensions given in Figure 8.
Other methods of fastening the cover and securing the worker may be used. The worker may be constructed
for either manual or mechanical operation. The design shall be such that a rate of 60 strokes per minute
± 10 strokes per minute, with a minimum length of 14 mm, can be maintained.
5.3.4 Overflow-ring (optional), conforming in principle to the illustration shown in Figure 6.
This is a useful aid for returning displaced grease to the grease worker cup. The overflow ring shall be
positioned at least 13 mm below the rim of the cup while making a penetration measurement. A rim 13 mm
high is helpful.
5.4 Grease cutter, having a sharp, rigidly mounted, bevelled blade, essentially as shown in Figure 9.
It is necessary that the blade be straight and sharpened as shown.
5.5 Water bath, capable of being maintained at 25,0 °C ± 0,5 °C and holding the assembled grease
worker.
If the bath is to be used for samples for unworked penetrations, a means shall be provided for protecting the
grease surface from water. A cover shall also be provided to maintain the air temperature above the sample at
25 °C.
An air bath, maintained at 25,0 °C ± 0,5 °C, is required for determining block penetration; a tightly sealed
container placed in the water bath will suffice.
NOTE A constant-temperature test room or an air bath can be used instead of a water bath.
5.6 Thermometer, calibrated at 25 °C, for the water bath or air bath.
5.7 Oven, capable of maintaining a temperature of 85 °C ± 2 °C, for melting the petrolatum samples.
5.8 Spatula, corrosion-resistant, square-ended, with a stiff blade approximately 32 mm wide and at least
150 mm long; for tests with half- and quarter-scale cones, the width should be approximately 13 mm.
5.9 Timer, graduated in 0,1 s.
5.10 Test-portion containers (for petrolatum), cylindrical, having a flat bottom 100 mm ± 5 mm in diameter
and 65 mm or more in depth, constructed of metal at least 1,6 mm thick and, if necessary, each provided with
a well-fitting watertight cover (see 9.1.3).
Containers of the “ointment box” type having somewhat flexible sides should not be used, for these permit
slight working of the petrolatum, due to flexing of the sides in handling.
4 © ISO 2007 – All rights reserved
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ISO 2137:2007(E)
6 Sampling
Unless otherwise specified in a commodity specification, samples shall be drawn in accordance with
ASTM D 4057.
The samples shall be examined for any sign of non-homogeneity such as oil separation, phase changes or
gross contamination. If any abnormal conditions are found, a new sample shall be drawn.
The size of the sample shall be large enough to fill the requested number of cups.
Key
1 centring device
NOTE This figure shows a combined assembly; generally, it is possible to displace vertically either the cone
assembly or the plate.
Figure 1 — Penetrometer
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ISO 2137:2007(E)
Dimensions in millimetres
Tolerances on dimensions except where otherwise stated: ± 1 mm
Key
1 smooth and polished surface
2 hardened steel tip
3 shaft stainless steel — tight press fit
a
Do not round the edges.
b
Magnesium or any other suitable material.
c
∅ 4 max., tight fit.
d
No shoulder.
Total mass of cone: 102,50 g ± 0,05 g
Total mass of movable attachments: 47,50 g ± 0,05 g
Figure 2 — Cone of the penetrometer — Full-scale cone
6 © ISO 2007 – All rights reserved
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ISO 2137:2007(E)
Dimensions in millimetres
Tolerances on dimensions except where otherwise stated: ± 1 mm
Key
1 hardened steel tip
2 smooth and polished surface
a
Break all sharp edges.
b
Stainless steel.
c
Brass or corrosion resistant steel.
d
No shoulder.
e
∅ 4 max., tight fit.
f
Machining to the required mass.
Total mass of cone: 102,50 g ± 0,05 g
Total mass of movable attachments: 47,50 g ± 0,05 g
Figure 3 — Cone of the penetrometer — Optional cone
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ISO 2137:2007(E)
Dimensions in millimetres
Tolerances on dimensions except where otherwise stated: ± 0,5 mm
Key
1 sharp corner
2 hardened steel tip
a
Machine this surface to give specified mass.
b
Polish all outside surfaces.
Mass of cone: 22,500 g ± 0,025 g
Mass of movable attachments: 15,000 g ± 0,025 g
Total mass of cone and its movable attachments: 37,50 g ± 0,05 g
Figure 4 — One-half-scale cone
8 © ISO 2007 – All rights reserved
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ISO 2137:2007(E)
Dimensions in millimetres
Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key
1 hardened steel tip — Angle: 30° ± 30'
Total mass of cone and its movable attachments: 9,380 g ± 0,025 g
Figure 5 — One-quarter-scale cone
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ISO 2137:2007(E)
Dimensions in millimetres
Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key
1 packing 6 vent valve
2 handle 7 adapter
3 thermometer 8 cover
4 packing nut 9 split rubber tube
5 thermometer gauge 10 overflow ring (optional)
a
optional, concentric to the interior of the cup, for use with the centring device.
Plan of perforated plate (detail X) — circle 1 (∅ 33,35): 12 holes circle 3 (∅ 65,10): 22 holes
circle 2 (∅ 49,20): 17 holes all holes: 6,4 < ∅ < 6,53
Figure 6 — Full-scale grease worker
10 © ISO 2007 – All rights reserved
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ISO 2137:2007(E)
Dimensions in millimetres
Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key
1 base
2 grease plate
3 ring
4 shaft
5 cover
6 valve
Material: stainless steel
Capacity: 50 ml
Figure 7 — One-half-scale grease worker
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ISO 2137:2007(E)
Dimensions in millimetres
Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key
1 ring
2 cover
3 valve
4 grease plate
5 base
6 chamber: ∅ 19,0 × 17,5 height — Capacity with the plate, as shown: 4 ml
Material: stainless steel
Figure 8 — One-quarter-scale grease worker
12 © ISO 2007 – All rights reserved
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ISO 2137:2007(E)
Dimensions in millimetres
Tolerances on dimensions except where otherwise stated: ± 0,25 mm
Key
1 base
2 tube
3 blade 65 × 185 — Hardened steel. Grind both surfaces to 1,2 mm thick. Grind lower edge
4 plywood or hard wood, 6,4 mm thick. Grain of top perpendicular to blade
Figure 9 — Grease cutter
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ISO 2137:2007(E)
7 Procedures for determining the cone penetration of lubricating grease —
Full-scale methods
7.1 Procedure for unworked penetration
7.1.1 Preparation of test portion
7.1.1.1 Take sufficient sample (at least 0,5 kg) to overfill the cup of the grease worker (5.3.1). If the
penetration is above 200 units, at least three times the amount needed to fill the cup is required.
7.1.1.2 Place the empty assembled grease worker, or metal container of equal inside dimensions, and an
appropriate amount of the test sample in a metal container in the water bath (5.5) maintained at 25 °C (see
the note to 5.5, and the last two paragraphs of this subclause) for sufficient time to bring the temperature of
the sample to 25 °C ± 0,5 °C. Transfer from the container a test portion, preferably in one lump, to overfill the
cup of the grease worker or metal container of equal inside dimensions (see below). Make this transfer in such
a manner that the grease is worked as little as possible. Jar the container to drive out trapped air and pack the
grease with the spatula (5.8), with as little manipulation as possible, to obtain a cupful without air pockets.
Scrape off the excess grease extending above the rim, creating a flat surface, by moving the blade of the
spatula, held inclined toward the direction of motion at an angle of approximately 45°, across the rim of the
cup. Do not perform any further levelling or smoothing of the surface throughout the determination of
unworked penetration, and carry out the measurement immediately.
The penetration of soft greases is dependent upon the diameter of the container. Therefore, greases having
unworked penetrations above 265 units should be tested in containers having the same diameter limitations
as those of the grease worker cup. The results on greases having penetrations below 265 units are not
significantly affected if the diameter of the container exceeds that of the grease worker cup.
If the initial sample temperature differs from 25 °C by more than approximately 8 °C, or if an alternative
method of adjusting the sample to 25 °C is used, sufficient additional time should be allowed to ensure that
the test portion is at 25,0 °C ± 0,5 °C before proceeding. Also, if the sample is larger than 0,5 kg, sufficient
additional time should be allowed to ensure that the test sample is at 25,0 °C ± 0,5 °C. Testing may proceed if
the test portion is at a uniform temperature of 25,0 °C ± 0,5 °C.
7.1.2 Cleaning the cone and movable attachments
Clean the penetrometer cone carefully before each test. Bending of the cone shaft can be avoided by holding
it securely in its raised position whilst cleaning. Remove all grease or oil on the penetrometer shaft, as they
can cause drag on the shaft assembly. Do not rotate the cone, as this can cause wear on the release
mechanism.
NOTE For penetrations up to 400 units, the optional cone as shown in Figure 3 can be used.
7.1.3 Penetration measurement
7.1.3.1 Place the cup on the penetrometer table, which shall be adjusted to a perfectly horizontal
position, making certain that it cannot rock. Set the mechanism to hold the cone in the “zero” position, and
adjust the apparatus carefully so that the tip of the cone just touches the surface of the test portion at the point
specified in 7.1.3.2 or 7.1.3.3. Watching the shadow of the cone tip is an aid to accurate setting. For greases
with penetrations over 400 units, centre the cup to within 0,3 mm of the tip of the cone. One way to centre the
cup accurately is to use a centring device (see Figure 1). Release the cone shaft rapidly, allow it to drop for
5,0 s ± 0,1 s and re-clamp it in this position. The release mechanism shall not drag on the shaft. Gently
depress the indicator shaft until it is stopped by the cone shaft and read the penetration from the indicator
scale.
7.1.3.2 If the test portion has a penetration over 200 units, centre the cone carefully in the container. This
test portion shall be used for only one test.
14 © ISO 2007 – All rights reserved
-------------
...
NORME ISO
INTERNATIONALE 2137
Troisième édition
2007-12-01
Produits pétroliers et lubrifiants —
Détermination de la pénétrabilité au cône
des graisses lubrifiantes et des
pétrolatums
Petroleum products and lubricants — Determination of cone penetration
of lubricating greases and petrolatum
Numéro de référence
ISO 2137:2007(F)
©
ISO 2007
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ISO 2137:2007(F)
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© ISO 2007
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ii © ISO 2007 – Tous droits réservés
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ISO 2137:2007(F)
Sommaire Page
Avant-propos. iv
Introduction . v
1 Domaine d'application.1
2 Références normatives .2
3 Termes et définitions.2
4 Principe.2
5 Appareillage .3
6 Échantillonnage .5
7 Modes opératoires pour déterminer la pénétrabilité au cône de la graisse lubrifiante —
Méthodes à l'échelle 1/1 .14
7.1 Mode opératoire pour les graisses non travaillées.14
7.2 Mode opératoire pour les graisses travaillées .15
7.3 Mode opératoire pour les graisses travaillées de façon prolongée.16
7.4 Mode opératoire pour les graisses en pain .17
8 Modes opératoires pour déterminer la pénétrabilité au cône de la graisse lubrifiante —
Méthode à l'échelle 1/2 ou à l'échelle 1/4 .17
8.1 Généralités .17
8.2 Mode opératoire pour les graisses non travaillées.17
8.3 Mode opératoire pour les graisses travaillées .18
9 Mode opératoire pour déterminer la pénétrabilité au cône des pétrolatums.19
9.1 Préparation de la prise d'essai.19
9.2 Mesurage de la pénétrabilité .19
10 Calculs .19
10.1 Calcul de la pénétration à l'échelle 1/1 .19
10.2 Conversion à la pénétrabilité à l'échelle 1/1 des résultats avec les cônes aux échelles 1/2
et 1/4.20
11 Expression des résultats .20
12 Fidélité .20
12.1 Généralités .20
12.2 Répétabilité.20
12.3 Reproductibilité.21
13 Rapport d'essai .21
Bibliographie .22
© ISO 2007 – Tous droits réservés iii
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ISO 2137:2007(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes nationaux de
normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est en général confiée
aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude a le droit de faire partie du
comité technique créé à cet effet. Les organisations internationales, gouvernementales et non
gouvernementales, en liaison avec l'ISO participent également aux travaux. L'ISO collabore étroitement avec
la Commission électrotechnique internationale (CEI) en ce qui concerne la normalisation électrotechnique.
Les Normes internationales sont rédigées conformément aux règles données dans les Directives ISO/CEI,
Partie 2.
La tâche principale des comités techniques est d'élaborer les Normes internationales. Les projets de Normes
internationales adoptés par les comités techniques sont soumis aux comités membres pour vote. Leur
publication comme Normes internationales requiert l'approbation de 75 % au moins des comités membres
votants.
L'attention est appelée sur le fait que certains des éléments du présent document peuvent faire l'objet de
droits de propriété intellectuelle ou de droits analogues. L'ISO ne saurait être tenue pour responsable de ne
pas avoir identifié de tels droits de propriété et averti de leur existence.
L'ISO 2137 a été élaborée par le comité technique ISO/TC 28, Produits pétroliers et lubrifiants.
Cette troisième édition annule et remplace la deuxième édition (ISO 2137:1985), qui a fait l'objet d'une
révision technique.
iv © ISO 2007 – Tous droits réservés
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ISO 2137:2007(F)
Introduction
L‘ISO 2137 a d’abord été publiée en 1972, puis une seconde édition est parue en 1985. La présente troisième
édition annule et remplace les deux premières éditions, dont elle constitue une révision technique. La révision
concerne essentiellement les tolérances sur les dimensions des différents cônes, afin de mieux coïncider
avec l'offre des fournisseurs d’équipement de laboratoire. Une telle révision était rendue nécessaire par
l’existence des plans qualité et des programmes d’exactitude des résultats mis en place par de nombreux
laboratoires selon les normes de qualité de l’ISO. Lesdites normes de qualité requièrent une conformité
absolue des cônes avec les dimensions données dans l’ISO 2137. Malheureusement, la plupart des cônes
disponibles sur le marché n’étaient pas conformes à l’ISO 2137:1985, et les utilisateurs étaient obligés
d’établir des dérogations qui étaient difficiles à justifier auprès des auditeurs qualité. Dans la présente édition
de l’ISO 2137, les tolérances sur les dimensions ont été élargies, ce qui permet à la plupart des cônes d'être
conformes aux nouvelles spécifications. Des essais interlaboratoires ont été organisés avec des cônes
respectant ces nouvelles exigences, ce qui a démontré que la fidélité de la méthode n’est pas altérée par le
changement des tolérances. Par ailleurs, des exigences de tolérance n'ont été maintenues que sur les
dimensions dont il a été prouvé qu’elles ont un impact direct sur la détermination de la pénétrabilité,
c’est-à-dire sur l’angle de la pointe, la hauteur de la pointe, l’épaisseur du bout de la pointe, le diamètre de
base de la pointe, l’angle du cône et la masse totale du cône et de ses accessoires mobiles.
© ISO 2007 – Tous droits réservés v
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NORME INTERNATIONALE ISO 2137:2007(F)
Produits pétroliers et lubrifiants — Détermination de la
pénétrabilité au cône des graisses lubrifiantes et des
pétrolatums
AVERTISSEMENT — L'utilisation de la présente Norme internationale peut impliquer l'intervention de
produits, d'opérations et d'équipements à caractère dangereux. La présente Norme internationale
n'est pas censée aborder tous les problèmes de sécurité concernés par son usage. Il est de la
responsabilité de l'utilisateur de consulter et d'établir des règles de sécurité et d'hygiène appropriées
et de déterminer l'applicabilité des restrictions réglementaires avant utilisation.
1 Domaine d'application
La présente Norme internationale spécifie des méthodes destinées à une estimation empirique de la
consistance des graisses lubrifiantes et des pétrolatums, par détermination de la pénétrabilité d’un cône
normalisé.
Le National Lubricating Grease Institute (NLGI) classifie les graisses en fonction de leur consistance, celle-ci
étant caractérisée par la pénétrabilité des graisses travaillées pendant 60 cycles. La classification NLGI
comprend neuf indices de consistance, ou grades, chaque grade correspondant à un intervalle donné de
pénétrabilité travaillée. La classification NLGI est donnée dans l'ISO 6743-99.
L’Article 7 de la présente Norme internationale spécifie quatre méthodes de détermination de la consistance
des graisses lubrifiantes, par la mesure de la profondeur de pénétration d'un cône entier. Ces méthodes
recouvrent la mesure des profondeurs de pénétration du cône dans des graisses travaillées, des graisses non
travaillées, des graisses travaillées de façon prolongée et des graisses en pain. Elles peuvent être utilisées
pour mesurer des pénétrabilités inférieures ou égales à 500 unités.
L’Article 8 de la présente Norme internationale spécifie des méthodes permettant de déterminer la
consistance des graisses lubrifiantes quand on ne dispose que de petits échantillons, grâce à l'utilisation de
cônes à l'échelle 1/2 ou à l’échelle 1/4 par rapport à ceux utilisés à l’Article 7. Ces méthodes sont applicables
aux graisses ayant des pénétrabilités au cône entier allant de 175 unités à 385 unités, et ne sont destinées
qu’aux seuls cas où les quantités de l'échantillon limitent l'utilisation des cônes décrits à l’Article 7. Elles n'ont
pas pour but de remplacer la pénétrabilité à l'échelle 1/1, selon l’Article 7, bien qu'une conversion à des
pénétrabilités à l'échelle 1/1 soit donnée en 10.2. Voir 8.1 pour les limitations de l’utilisation des cônes à
échelle 1/4 en raison de la mauvaise fidélité des mesures obtenues.
NOTE 1 La pénétrabilité d'une graisse non travaillée n’est généralement pas aussi représentative de sa consistance à
l’utilisation que la pénétrabilité d'une graisse travaillée. C'est la pénétrabilité des graisses travaillées qui est généralement
utilisée pour l'examen des graisses lubrifiantes.
NOTE 2 La pénétrabilité d'une graisse en pain peut être obtenue sur les produits suffisamment durs pour conserver
leur forme. Ces graisses présentent habituellement des pénétrabilités inférieures à 85 unités.
L’Article 9 de la présente Norme internationale spécifie une méthode permettant, par la mesure de la
pénétration d'un cône entier, de déterminer la consistance d'un pétrolatum ayant une pénétrabilité inférieure
ou égale à 300 unités. Cette méthode peut aussi être utilisée pour estimer la consistance des gatsch.
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ISO 2137:2007(F)
2 Références normatives
Les documents de référence suivants sont indispensables pour l'application du présent document. Pour les
références datées, seule l'édition citée s'applique. Pour les références non datées, la dernière édition du
document de référence s'applique (y compris les éventuels amendements).
ASTM D 4057, Standard Practice for Manual Sampling of Petroleum and Petroleum Products
3 Termes et définitions
Pour les besoins du présent document, les termes et définitions suivants s'appliquent.
3.1
pénétrabilité au cône
profondeur à laquelle un cône normalisé pénètre dans une prise d’essai, dans des conditions normalisées de
charge, de temps et de température
NOTE 1 La pénétrabilité au cône est exprimée en unités de 0,1 mm.
NOTE 2 Adaptée de l’ISO 1998-2:1998, 2.80.001.
3.2
travail
soumission d’une graisse à l’action de cisaillement d’un malaxeur à graisse
3.3
pénétrabilité d’une graisse non travaillée
pénétrabilité au cône d’une prise d’essai ayant subi le minimum de manipulations lors des opérations de
transvasement du récipient porte-échantillon à la coupelle du malaxeur
3.4
pénétrabilité d’une graisse travaillée
pénétrabilité d’une prise d’essai après qu’elle a subi un nombre défini de cycles dans un malaxeur
3.5
pénétrabilité d’une graisse travaillée de façon prolongée
pénétrabilité au cône d’une prise d’essai qui a été travaillée pendant un nombre de cycles supérieur à celui
défini pour la pénétrabilité d’une graisse travaillée (voir 3.4)
3.6
pénétrabilité d’une graisse en pain
pénétrabilité déterminée sur une prise d’essai qui est suffisamment dure pour garder sa forme sans qu’elle
soit placée dans un récipient
4 Principe
La pénétrabilité au cône d'une graisse lubrifiante est déterminée à 25 °C en mesurant la profondeur de
pénétration du cône dans l'échantillon, celle-ci étant obtenue en libérant l'ensemble cône du pénétromètre et
en laissant le cône agir pendant 5 s.
La pénétrabilité au cône d'une graisse non travaillée est déterminée sur des prises d'essai transvasées avec
un minimum de perturbation dans un récipient convenant aux essais.
La pénétrabilité au cône d'une graisse travaillée est déterminée immédiatement après malaxage de la prise
d'essai pendant 60 cycles dans un malaxeur de graisse normalisé.
La pénétrabilité au cône d'une graisse travaillée de façon prolongée est déterminée sur des prises d'essai
malaxées pendant plus de 60 cycles.
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ISO 2137:2007(F)
La pénétrabilité au cône d'une graisse en pain est déterminée sur une face fraîchement préparée d'un cube
découpé dans un bloc de graisse avec un couteau normalisé.
La pénétrabilité au cône d'un pétrolatum est déterminée en mesurant, comme pour une graisse lubrifiante, la
profondeur de pénétration du cône dans l'échantillon soumis à l'essai préalablement fondu puis resolidifié par
refroidissement dans des conditions spécifiées.
5 Appareillage
5.1 Pénétromètre, analogue à celui représenté sur la Figure 1, conçu pour mesurer, en dixièmes de
millimètre, la profondeur de pénétration d'un cône dans un matériau.
L'ensemble cône, ou le plateau du pénétromètre, doit être réglable de façon à permettre un positionnement
précis de la pointe du cône sur la surface plane du matériau tout en maintenant une valeur «zéro» sur
l'indicateur. Le cône doit, quand il est libéré, tomber sur au moins 62 mm sans frottement appréciable. La
pointe du cône ne doit pas heurter le fond du récipient porte-échantillon. L'instrument doit posséder des vis de
mise à niveau et un niveau à bulle, de façon à assurer une position verticale à la tige du cône.
NOTE La mesure de la profondeur de pénétration est faite soit avec des systèmes mécaniques (indicateur
mécanique), soit avec des dispositifs électroniques (indicateur numérique).
5.2 Cônes
5.2.1 Cône entier, consistant en un corps conique, en magnésium ou un autre matériau approprié, et
possédant une pointe en acier trempé, détachable.
Les dimensions et tolérances sont indiquées sur la Figure 2. La masse totale du cône doit être de
102,50 g ± 0,05 g, et celle des accessoires mobiles doit être de 47,50 g ± 0,05 g. Les accessoires
comprennent une tige rigide portant une butée à son extrémité supérieure et un moyen approprié, à son
extrémité inférieure, de fixation au cône. On peut modifier l'intérieur du cône pour obtenir la masse spécifiée,
à condition que le contour extérieur et la répartition des masses n'en soient pas modifiés. La surface
extérieure doit être très finement polie.
NOTE Pour des pénétrabilités jusqu'à 400 unités, la variante du cône du pénétromètre représentée sur la Figure 3
peut être utilisée.
5.2.2 Cône à l'échelle 1/2 et tige, en acier, acier inoxydable ou laiton, muni d'une pointe en acier trempé
de dureté 45 Rockwell C à 50 Rockwell C et conforme aux dimensions et tolérances indiquées sur la Figure 4.
La tige peut être en acier inoxydable. La masse totale du cône et de ses accessoires mobiles doit être de
37,50 g ± 0,05 g. La masse du cône doit être de 22,500 g ± 0,025 g. La masse des accessoires mobiles doit
être de 15,000 g ± 0,025 g.
5.2.3 Cône à l'échelle 1/4 et tige, formé d'un corps conique en matière plastique ou en tout autre matériau
de faible masse volumique, muni d'une pointe en acier trempé de dureté 45 Rockwell C à 50 Rockwell C, et
construit conformément aux dimensions et tolérances indiquées sur la Figure 5.
La tige peut être en alliage de magnésium. La masse totale du cône et des accessoires mobiles doit être de
9,380 g ± 0,025 g. Cette masse totale peut être ajustée en ajoutant de la grenaille dans la cavité de l'axe.
5.3 Malaxeurs
5.3.1 Malaxeur à l'échelle 1/1, conforme aux dimensions indiquées sur la Figure 6.
Les dimensions non indiquées ne sont pas critiques et peuvent être modifiées selon des exigences
particulières. On peut utiliser d'autres méthodes de fixation du couvercle ou du dispositif proprement dit. Ce
malaxeur peut être construit pour fonctionner manuellement ou automatiquement. Il doit permettre une
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ISO 2137:2007(F)
fréquence de malaxage de 60 cycles par minute ± 10 cycles par minute, avec une course minimale de 63 mm.
Il faut prévoir un thermomètre approprié, étalonné à 25 °C, et destiné à traverser le robinet d'évent.
5.3.2 Malaxeur à l'échelle 1/2, conforme aux dimensions de la Figure 7.
On peut utiliser d'autres méthodes de fixation du couvercle et du malaxeur. Le malaxeur peut être construit
pour fonctionner manuellement ou automatiquement. Il doit permettre une fréquence de malaxage de
60 cycles par minute ± 10 cycles par minute, avec une course d'au moins 35 mm.
5.3.3 Malaxeur à l'échelle 1/4, conforme aux dimensions de la Figure 8.
On peut utiliser d'autres méthodes de fixation du couvercle ou du malaxeur. Le malaxeur peut être construit
pour fonctionner manuellement ou automatiquement. Il doit permettre une fréquence de malaxage de
60 cycles par minute ± 10 cycles par minute, avec une course d'au moins 14 mm.
5.3.4 Bague de trop-plein (facultative), conforme dans son principe à l'illustration de la Figure 6.
Cette bague est particulièrement utile pour remettre la graisse déplacée dans la coupelle du malaxeur. La
bague de trop-plein doit être positionnée lors du mesurage de la pénétrabilité à au moins 13 mm en dessous
du bord de la coupelle. Il est utile d'avoir un bord de 13 mm de haut.
5.4 Couteau à graisse, possédant une lame effilée et en biseau, montée d'une manière rigide,
essentiellement comme représenté sur la Figure 9.
Il faut que la lame soit rectiligne et aiguisée comme indiqué.
5.5 Bain d'eau, pouvant être maintenu à 25,0 °C ± 0,5 °C et capable de contenir le dispositif pour le travail
des graisses.
Si le bain doit être utilisé pour des échantillons non travaillés, il faut prévoir un moyen protégeant la surface de
la graisse de l'eau. Prévoir aussi un couvercle pour maintenir la température de l'air se trouvant au-dessus de
l'échantillon à 25 °C.
Un bain d'air, maintenu à 25,0 °C ± 0,5 °C, est nécessaire pour déterminer la pénétrabilité d'une graisse en
pain; il suffira d'avoir un récipient fermé d'une manière étanche et placé dans le bain d'eau.
NOTE On peut utiliser, à la place du bain d'eau, un local d'essai à température constante, ou encore un bain d'air.
5.6 Thermomètre, étalonné à 25 °C, pour le bain d'eau ou pour le bain d'air.
5.7 Étuve, pouvant être maintenue à une température de 85 °C ± 2 °C, pour faire fondre les échantillons de
pétrolatum.
5.8 Spatule, résistant à la corrosion, à bout carré, possédant une lame rigide d’approximativement 32 mm
de large et d'au moins 150 mm de long; pour les essais avec les cônes à l'échelle 1/2 et à l'échelle 1/4, il
convient que la largeur soit d'environ 13 mm.
5.9 Chronomètre, gradué en 0,1 s.
5.10 Récipients pour prises d'essai, pour les pétrolatums, cylindriques, ayant un fond plat de
100 mm ± 5 mm de diamètre et une profondeur d'au moins 65 mm, en un métal d'au moins 1,6 mm
d'épaisseur et, si nécessaire, munis chacun d'un couvercle fermant hermétiquement (voir 9.1.3).
Il n'est pas recommandé d'utiliser des récipients du type «boîte à onguent», qui présentent des côtés
relativement souples, car ils agissent légèrement sur le pétrolatum, en raison de la flexion des côtés lors de
leur manipulation.
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ISO 2137:2007(F)
6 Échantillonnage
Sauf avis contraire dans les spécifications d’usage, l'échantillonnage doit être fait conformément à
l'ASTM D 4057.
Examiner les échantillons pour déceler un manque éventuel d'homogénéité, tel qu'une décantation de produit
organique, ou des changements de phase, ou une contamination flagrante. En cas d'anomalie, faire un
nouveau prélèvement.
La taille de l'échantillon doit être suffisante pour permettre de remplir le nombre nécessaire de coupelles.
Légende
1 dispositif de centrage
NOTE Il s'agit ici de la représentation d'un montage combiné: en général, on peut déplacer verticalement soit
l'ensemble cône, soit le plateau.
Figure 1 — Pénétromètre
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ISO 2137:2007(F)
Dimensions en millimètres
Tolérances sur les dimensions, sauf indication contraire: ± 1 mm
Légende
1 surface lisse et polie
2 pointe en acier trempé
3 axe en acier inoxydable — ajustement serré
a
Ne pas arrondir les angles.
b
Magnésium ou tout autre matériau approprié.
c
∅ 4 max., ajustement serré.
d
Pas d'épaulement.
Masse totale du cône: 102,50 g ± 0,05 g
Masse totale des accessoires mobiles: 47,50 g ± 0,05 g
Figure 2 — Cône du pénétromètre — Modèle entier
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ISO 2137:2007(F)
Dimensions en millimètres
Tolérances sur les dimensions, sauf indication contraire: ± 1 mm
Légende
1 pointe en acier trempé
2 surface lisse et polie
a
Abattre les arêtes vives.
b
Acier inoxydable.
c
Laiton ou acier résistant à la corrosion.
d
Pas d'épaulement.
e
∅ 4 max., ajustement serré.
f
Usinage à la masse requise.
Masse totale du cône: 102,50 g ± 0,05 g
Masse totale des accessoires mobiles: 47,50 g ± 0,05 g
Figure 3 — Cône du pénétromètre — Variante
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ISO 2137:2007(F)
Dimensions en millimètres
Tolérances sur les dimensions, sauf indication contraire: ± 0,5 mm
Légende
1 coin à arête vive
2 pointe en acier trempé
a
Usiner cette surface jusqu'à la masse prescrite.
b
Polir toutes les surfaces extérieures.
Masse du cône: 22,500 g ± 0,025 g
Masse des accessoires mobiles: 15,000 g ± 0,025 g
Masse totale du cône et de ses accessoires mobiles: 37,50 g ± 0,05 g
Figure 4 — Cône à l'échelle 1/2
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ISO 2137:2007(F)
Dimensions en millimètres
Tolérances sur les dimensions, sauf indication contraire: ± 0,25 mm
Légende
1 pointe en acier trempé – Angle: 30° ± 30'
Masse totale du cône et de ses accessoires mobiles: 9,380 g ± 0,025 g
Figure 5 — Cône à l'échelle 1/4
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ISO 2137:2007(F)
Dimensions en millimètres
Tolérances sur les dimensions, sauf indication contraire: ± 0,25 mm
Légende
1 presse-étoupe 6 robinet d'évent
2 poignée 7 raccord
3 thermomètre 8 couvercle
4 chapeau du presse-étoupe 9 tube caoutchouc fendu
5 pièce d'épaisseur du thermomètre 10 bague de trop-plein (facultative)
a
Facultatif, concentrique à l'intérieur de la coupelle, pour utilisation avec le dispositif de centrage.
Plan de la plaque perforée (détail X) — cercle 1 (∅ 33,35): 12 trous cercle 3 (∅ 65,10): 22 trous
cercle 2 (∅ 49,20): 17 trous tous les trous: 6,4 < ∅ < 6,53
Figure 6 — Malaxeur à l'échelle 1/1
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ISO 2137:2007(F)
Dimensions en millimètres
Tolérances sur les dimensions, sauf indication contraire: ± 0,25 mm
Légende
1 socle
2 plaque perforée
3 joint torique
4 axe
5 couvercle
6 robinet
Matière: acier inoxydable
Capacité: 50 ml
Figure 7 — Malaxeur à l'échelle 1/2
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ISO 2137:2007(F)
Dimensions en millimètres
Tolérances sur les dimensions, sauf indication contraire: ± 0,25 mm
Légende
1 joint torique
2 couvercle
3 robinet
4 plaque perforée
5 socle
6 chambre: ∅ 19,0 × 17,5 hauteur — Capacité avec la plaque perforée représentée: 4 ml
Matière: acier inoxydable
Figure 8 — Malaxeur à l'échelle 1/4
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ISO 2137:2007(F)
Dimensions en millimètres
Tolérances sur les dimensions, sauf indication contraire: ± 0,25 mm
Légende
1 base
2 tube
3 lame 65 × 185 — Deux faces en acier trempé rectifiées à 1,2 mm — Affûter l'arête inférieure
4 contreplaqué ou bois plein, épaisseur 6,4 mm. Veine du bois perpendiculaire à la lame
Figure 9 — Couteau à graisse
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ISO 2137:2007(F)
7 Modes opératoires pour déterminer la pénétrabilité au cône de la graisse
lubrifiante — Méthodes à l'échelle 1/1
7.1 Mode opératoire pour les graisses non travaillées
7.1.1 Préparation de la prise d'essai
7.1.1.1 Prendre un échantillon suffisamment important (au moins 0,5 kg) pour que la coupelle du
malaxeur (5.3.1) soit plus que remplie. Si la pénétrabilité est supérieure à 200 unités, il faut que la quantité
d'échantillon soit au moins égale à trois fois la prise d'essai nécessaire au remplissage de la coupelle.
7.1.1.2 Dans un bain thermostatique (5.5) maintenu à 25 °C (voir la note en 5.5 ainsi que les deux
derniers alinéas de ce paragraphe), placer le malaxeur vide, ou un récipient métallique de dimensions
internes identiques, ainsi qu'une quantité appropriée de la prise d'essai se trouvant dans un récipient
métallique, pendant un temps suffisant pour porter la température de la prise d'essai à 25,0 °C ± 0,5 °C.
Prendre de préférence en une seule fois la prise d'essai dans le récipient et en remplir, avec excès, la
coupelle du malaxeur ou le récipient métallique de mêmes dimensions intérieures (voir ci-dessous). Effectuer
ce transvasement de maniè
...
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