1、DRAFT FOR DEVELOPMENT DD ISO/TR 16144:2002 Hydraulic fluid power Calibration of liquid automatic particle counters Procedures used to certify the standard reference material SRM 2806 ICS 23.100.60 DD ISO/TR 16144:2002 This Draft for Development, having been prepared under the direction of the Engine
2、ering Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 11 November 2002 BSI 11 November 2002 ISBN 0 580 40715 2 National foreword This Draft for Development reproduces verbatim ISO/TR 16144:2002. This publication is not to be r
3、egarded as a British Standard. It is being issued in the Draft for Development series of publications and is of a provisional nature because the technique and calibration material described are under development. It should be applied on this provisional basis, so that information and experience of i
4、ts practical application may be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the international organization responsible for the Technical Specification. A review of this publication will be initiated not later than 3 yea
5、rs after its publication by the international organization so that a decision can be taken on its status at the end of its 3-year life. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the replies received by th
6、e end of the review period, the responsible BSI Committee will decide whether to support the conversion into an international standard, to extend the life of the Technical Specification for another 3 years or to withdraw it. Comments should be sent in writing to the Secretary of BSI Subcommittee MCE
7、/18/-/6, Contamination control, at British Standards House, 389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text. A list of organizations represented on this committee can be obtained on request to i
8、ts secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue
9、or of British Standards Online. Summary of pages This document comprises a front cover, an inside front cover, the ISO/TR title page, pages ii to v, a blank page, pages 1 to 17 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments
10、 issued since publication Amd. No. Date Comments Reference number ISO/TR 16144:2002(E)TECHNICAL REPORT ISO/TR 16144 First edition 2002-09-15 Hydraulic fluid power Calibration of liquid automatic particle counters Procedures used to certify the standard reference material SRM 2806 Transmissions hydra
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16、 + 9 74 E-mial coirypthgis.oc h Web ww.wiso.ch ii DDISO/TR16144:2002 iiiContents Page Foreword iv Introduction. v 1 Scope 1 2 Equipment and material 1 2.1 Test powder . 1 2.2 Test fluid. 1 2.3 Sample preparation loop 2 2.4 Membrane preparation equipment 2 2.5 Scanning electron microscope and image a
17、nalyser .2 3 Equipment validation 3 3.1 Sample preparation validation. 3 3.2 Microscope calibration validation . 4 3.3 Membrane preparation validation 4 3.4 Membrane and SRM 2806 stability testing . 6 4 Test procedure 6 4.1 Calibration suspension preparation SRM 2806 . 6 4.2 Membrane preparation 7 4
18、.3 Membrane examination and particle counting. 7 5 Data processing 11 Bibliography 16 DDISO/TR16144:2002iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is no
19、rmally 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
20、 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 3. The main task of technical committees is to prepa
21、re 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. In exceptional circumstances, when a technica
22、l committee has collected data of a different kind from that which is normally published as an International Standard (“state of the art”, for example), it may decide by a simple majority vote of its participating members to publish a Technical Report. A Technical Report is entirely informative in n
23、ature and does not have to be reviewed until the data it provides are considered to be no longer valid or useful. Attention is drawn to the possibility that some of the elements of this Technical Report may be the subject of patent rights. ISO shall not be held responsible for identifying any or all
24、 such patent rights. ISO/TR 16144 was prepared by Technical Committee ISO/TC 131, Fluid power systems, Subcommittee SC 6, Contamination control. DDISO/TR16144:2002 vIntroduction Solid particulates are a major contributor to wear in hydraulic systems. The fluid power industry, the aerospace industry
25、and the military sector utilize optical automatic particle counter (APC) technologies to assess the level of hydraulic oil contamination by suspended particulate. The amount of contamination is often related to the integrity of the system and the usage of the fluid. APCs are also employed in various
26、 oil filter testing operations by the manufacturers and the users. The standard method ISO 4402 11)has been used for nearly 30 years to calibrate optical particle counters in terms of particle size as a function of particle concentration. The calibration material used in ISO 4402:1991 is Air Cleaner
27、 Fine Test Dust (ACFTD) produced in the past by a division of General Motors Corporation. This material consists of a polydisperse dust having the largest number of particles, as indicated in ISO 4402:1991, with the size range of 1 m to 80 m diameter (particle concentration increases with decreasing
28、 diameter). There is a low concentration of particles reported to extend out to approximately 100 m. Some problems have arisen with the use of ACFTD in such calibration procedures. Firstly, there has been ongoing concern that the particle size distribution is not accurate in the small particle size
29、regime ( 10 m) of the distribution 2, 3, 4, 5 . Many researchers have noted that there are more sub-10 m particles in ACFTD than reported by ISO 4402:1991. Secondly, but not less importantly, the production of ACFTD has been discontinued by the supplier. Thus there is a need to investigate, design a
30、nd devise a new standard method (Hydraulic fluid power Calibration method for liquid automatic particle counters) using a new Standard Reference Material (SRM) 6 . The National Institute of Standards and Technology (NIST) was requested to develop an SRM for use by the fluid power industry. Users wil
31、l benefit from improved precision since there is a central source of only one material and increased accuracy resulting from the size characterization 7 . The new SRM, designated as SRM 2806, is composed of ISO Medium Test Dust (ISO MTD) suspended in MIL-H-5606 hydraulic fluid. The number of particl
32、es per millilitre greater than specified sizes has been determined for this material. 1) Cancelled in 1999 and replaced by ISO 11171:1999. DDISO/TR16144:2002 1Hydraulic fluid power Calibration of liquid automatic particle counters Procedures used to certify the standard reference material SRM 2806 1
33、 Scope This Technical Report describes the procedures used by the United States National Institute of Standards and Technology (NIST) for the certification of the calibration material SRM 2806, which is used in the primary calibration of liquid automatic particle counters. SRM 2806 is a suspension o
34、f ISO MTD in hydraulic fluid with a number size distribution certified using a scanning electron microscope (SEM) and image analysis techniques. 2 Equipment and material 2.1 Test powder 2.1.1 Standard reference material SRM 2806 The particulate material used is a silica powder made from Arizona dese
35、rt sand by jet milling and then air classifying to a consistent particle size distribution. Several grades with different size ranges are available and their properties are specified in ISO 12103-1 8 . The powder used to prepare SRM 2806 is an ISO 12103-A3 grade, also called ISO MTD, with supplier b
36、atch number 4390C. 2.1.2 Reference materials RM 8631 and RM 8632 Reference materials RM 8631 and RM 8632 are composed of ISO MTD and ISO ultra fine test dust lot numbers 4390C (same lot as the SRM 2806) and 4476 J, respectively. These RMs provide materials to make secondary standards used in support
37、 of ISO 11171 9and SRM 2806 10 . The RM was received in 3,6 kg bottles. This dust was dried and spin-riffled into 147 aliquots, each of 20 mg. The material was examined for homogeneity using optical particle counters after suspension in clean oil. 2.2 Test fluid Test fluid in which ISO MTD is suspen
38、ded is a hydraulic fluid widely used worldwide for filter testing. This oil is defined in American national standards as MIL-H 5606 and in French national standards as AIR 3520, and in the NATO specification H 515. Its physical-chemical properties are defined in annex A of ISO 16889:1999 11 . To eas
39、e particle dispersion, a small quantity (50 g/g) of an antistatic agent is added to the oil so that its conductivity is 1 500 pS/m 100 pS/m. DDISO/TR16144:20022 2.3 Sample preparation loop In view of supplying worldwide demand for several years with the SRM 2806 (supplied in bottles of 400 ml), it w
40、as necessary to prepare and store a great number of bottles for further sales. Because of the settling velocity of the larger silica grains, a special mixing loop was built with mechanical and hydraulic components which were used to eliminate grinding the powder in suspension. It was designed accord
41、ing to the recommendations of ISO 11943 12 . To guarantee bottle sample homogeneity, a supplementary volume of oil was necessary to allow sampling of control bottles used as described in 3.1.2. The schematic of the sample preparation loop is given in Figure 1. Key 1 Fluid reservoir (200 l) 2 Circula
42、ting pump 3 Clean-up filter 4 Sampling tap Figure 1 Schematic of calibration suspension preparation loop 2.4 Membrane preparation equipment Particles are filtered on 25 mm diameter polycarbonate membranes, 0,2 m pore diameter using the equipment commonly used for determining hydraulic fluid particul
43、ate contamination by gravimetry according to ISO 4405 13or by microscopic counting according to ISO 4407 14 . 2.5 Scanning electron microscope and image analyser The scanning electron microscope used to examine particles is a JEOL 840. The images were produced by electron backscattering and collecte
44、d on a MicroVax and analysed using LISPIX, a public domain image processing software developed at NIST. LISPIX currently runs on any computer. DDISO/TR16144:2002 33 Equipment validation 3.1 Sample preparation validation 3.1.1 General Quality assurance for both production and testing was developed by
45、 a task force composed of North American members from two filter manufacturers, a particle counter manufacturer, an independent laboratory and NIST. APC measurements were made by both the independent laboratory and NIST, with NIST performing the data analysis. 3.1.2 Homogeneity testing/batch screeni
46、ng An experimental sampling design was developed and implemented at NIST to measure the bottle-to-bottle homogeneity and, at the same time, to identify possible systematic errors in the instrumental measurements. In the production process, four bottles (a, b, c, d) were filled at any one time. There
47、 were 320 bottles per batch and bottles were numerically labelled sequentially from 1 (a, b, c, d), 2 (a, b, c, d), ., to 80 (a, b, c, d) as they were produced. Selected bottles from each batch were tested for homogeneity at both the independent laboratory and NIST using APCs with extinction sensors
48、 calibrated according to ISO 4402:1991. Four bottles (a, b, c, d) were sampled and analysed from approximately the following four points in the production cycle: 5 %, 30 %, 60 %, and 95 %. Another set of four bottles that were produced directly adjacent to the first four were then analysed. For exam
49、ple, the first 16 bottles 5 a, 5 b, 5 c, 5 d, 25 (a, b, c, d), 50 (a, b, c, d) and 75 (a, b, c, d) were analysed in that order. Then bottles 6 (a, b, c, d), 26 (a, b, c, d), 51 (a, b, c, d), and 76 (a, b, c, d) were analysed all by the same calibrated APC. With three replicates for each bottle, this totalled 96 measurements. Each batch of 320 bottles was subjected to this procedure or a modified version of this test. A batch of material wa
