SAE J 2975-2015 Measurement of Copper and Other Elements in Brake Friction Materials.pdf

1、 SURFACE VEHICLE RECOMMENDED PRACTICE J2975 MAY2015 Issued 2011-12 Revised 2015-05 Superseding J2975 DEC2013 Measurement of Copper and Other Elements in Brake Friction Materials RATIONALE The states of Washington and California passed laws in 2011 restricting the amount of cadmium, copper, hexavalen

2、t chromium, lead and mercury their compounds in brake friction materials. As part of the legislation, brake friction materials are required to be analyzed to confirm the levels of the restricted elements are below the values stated in the legislation. The SAE J2975 provides a method on how to genera

3、te samples of brake friction material for analysis, how to prepare the samples for analysis and how to analyze the samples. This revision expands the applicability of EPA method 3051A and EPA method 6010C (used in tandem) for mercury detection and measurement. These two methods combined eliminate th

4、e possible interference from copper and sulfides, which are common in friction materials. The revision also allows EPA method 6020A to be used for detection restricted substances. TABLE OF CONTENTS 1. SCOPE . 2 1.1 Purpose 2 2. REFERENCES . 2 2.1 Applicable Documents . 2 3. DEFINITIONS 3 3.1 SYMBOLS

5、 AND ABBREVIATIONS . 3 4. SAMPLE PREPARATION 3 4.1 Preparation of Brake Friction Material . 3 4.2 Friction Material Sample Processing for Chemical Analysis 5 4.3 Chemical Analysis of Brake Friction Material Sample . 5 4.4 Presentation of Results 6 5. NOTES . 7 5.1 Marginal Indicia 7 _ SAE Technical

6、Standards Board Rules provide that: “This report is published by SAE to advance the state of technical and engineering sciences. The use of this report is entirely voluntary, and its applicability and suitability for any particular use, including any patent infringement arising therefrom, is the sol

7、e responsibility of the user.” SAE reviews each technical report at least every five years at which time it may be revised, reaffirmed, stabilized, or cancelled. SAE invites your written comments and suggestions. Copyright 2015 SAE International All rights reserved. No part of this publication may b

8、e reproduced, stored in a retrieval system or transmitted, in any form or by any means, electronic, mechanical, photocopying, recording, or otherwise, without the prior written permission of SAE. TO PLACE A DOCUMENT ORDER: Tel: 877-606-7323 (inside USA and Canada) Tel: +1 724-776-4970 (outside USA)

9、Fax: 724-776-0790 Email: CustomerServicesae.org SAE WEB ADDRESS: http:/www.sae.org SAE values your input. To provide feedback on this Technical Report, please visit http:/www.sae.org/technical/standards/J2975_201505 SAE INTERNATIONAL J2975 Revised MAY2015 Page 2 of 8 APPENDIX A Publically Disclosed

10、Friction Formulations Used during the Interlaboratory Study to Establish this Recommended Practice . 8 Figure 1 Measurement of friction material thickness 3 Figure 2 Setting the drill press stop at the friction material thickness 4 Figure 3 A schematic representation of a disc pad and lining showing

11、 the area that can be used for sample collection (gray shaded). 4 Figure 4 The difference in drill turning morphologies that results from varying the drill plunge rates . 5 1. SCOPE This procedure describes a method for generating, preparing and analyzing samples of new and unused brake friction mat

12、erials for their chemical constituents. 1.1 Purpose This recommended test practice is intended to establish a standardized and repeatable method for analyzing the amount of specific chemical elements in a new and unused brake friction material. Results from this test practice provide the basis to de

13、termine the appropriate environmental marking per SAE J866. 2. REFERENCES 2.1 Applicable Documents The following publications form a part of this specification to the extent specified herein. Unless otherwise indicated, the latest issue of SAE publications shall apply. 2.1.1 SAE Publications Availab

14、le from SAE International, 400 Commonwealth Drive, Warrendale, PA 15096-0001, Tel: 877-606-7323 (inside USA and Canada) or +1 724-776-4970 (outside USA), www.sae.org. SAE J866 Friction Coefficient Identification and Environmental Marking System for Brake Linings 2.1.2 EPA Publications Available from

15、 the United States Environmental Protection Agency (EPA), http:/www.epa.gov. EPA Method 245.5 Mercury in Sediments (Manual Cold Vapor Technique) EPA Method 3050B Acid Digestion of Sediments, Sludges and Soils EPA Method 3051A Microwave Assisted Acid Digestion of Sediments, Sludges, Soils and Oils EP

16、A Method 6010C Inductively Coupled Plasma - Atomic Emission Spectrometry EPA Method 6020A Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) EPA Method 7471B Mercury in Solid or Semisolid Waste (Manual Cold-Vapor Technique) EPA Method 3060A Alkaline Digestion for Hexavalent Chromium EPA Method 71

17、96A Chromium, Hexavalent (Colorimetric) EPA Method 7199 Determination of Hexavalent Chromium in Drinking Water, Groundwater and Industrial Wastewater Effluents by Ion Chromatography EPA/600/R-93/116 Method for the Determination of Asbestos in Bulk Building Materials SAE INTERNATIONAL J2975 Revised M

18、AY2015 Page 3 of 8 3. DEFINITIONS 3.1 SYMBOLS AND ABBREVIATIONS 3.1.1 ICP-AES Inductively Coupled Plasma - Atomic Emission Spectrometry 3.1.2 ICP-MS Inductively Coupled Plasma-Mass Spectrometry 4. SAMPLE PREPARATION 4.1 Preparation of Brake Friction Material 4.1.1 Wipe entire friction assembly with

19、lint-free wipe (i.e., Kimwipe) to ensure assembly is free of any dust and foreign objects. Multiple wipes may be needed to accomplish this task. Alternatively, the assembly may be rinsed with de-ionized water and then dried with a lint free wipe. 4.1.2 Determine the thickness of the friction materia

20、l. For assemblies without any steel back or shoe assembly, simply measure the thickness. For friction assemblies, the thickness of the friction material can be measured directly as shown in Figure 1 or the total assembly can be measured and then subtract the thickness of the pressure plate / shoe st

21、eel to obtain the friction material thickness. Figure 1 - Measurement of friction material thickness 4.1.3 Place friction assembly in a heavy gage sealable plastic bag (to collect turnings). Place friction assembly on the table of the drill press in a safe manner that meets the desired safety requir

22、ements of the laboratory. Care should be taken to insure the plastic bag does not tear or become damaged during the clamping or drilling. (Some drill presses may have guarding that prohibits the effective use of a plastic bag. In this case, care should be taken to keep all grinding debris on the fri

23、ction face.) 4.1.4 Set the depth stop on the drill press such that it is at the midpoint of the friction material thickness measured in 4.1.2 as shown in Figure 2. SAE INTERNATIONAL J2975 Revised MAY2015 Page 4 of 8 Figure 2 - Setting the drill press stop at the friction material thickness 4.1.5 Set

24、 the speed of the drill such that it rotates approximately 400 100 rpm at the spindle. 4.1.6 Using a 3mm diameter solid carbide drill bit, drill numerous borings (35-40 borings to a 5mm depth yields greater than 2 grams of sample) into the friction material uniformly around the entire area to genera

25、te enough fines (2 g) for subsequent acid digestion. For larger samples of friction, a minimum of 1 hole per 2 cm2is recommended to ensure uniform sampling. To avoid any edge effects from the processing of the friction material, do not drill within 6 mm of the outer circumference of the friction mat

26、erial (Figure 3). Figure 3 - A schematic representation of a disc pad and lining showing the area that can be used for sample collection (gray shaded). Also shown (right) is a brake friction assembly in a sealable plastic bag ready for the start of sample collection SAE INTERNATIONAL J2975 Revised M

27、AY2015 Page 5 of 8 4.1.7 The morphology of the drillings is dependent on the plunge rate and drill spindle speed which is specified in section 4.15 while drilling. A plunge rate of less than 0.33 mm/sec is recommended (15 sec to drill a 5mm deep hole) to achieve a consistent and uniform granular par

28、ticulate. Slower plunge rates yield a more powdery consistency. A faster plunge rate yields a mixture of coarser turnings and granules which results in an unacceptable measurement variation of the chemical content. The different morphologies resulting from different plunge rates are shown in Figure

29、4.ferred Morphology Figure 4 - The difference in drill turning morphologies that results from varying the drill plunge rates 4.1.8 Collect drill turnings from the working face of the friction material and place in a clean sealable container. Label the sample accordingly. 4.2 Friction Material Sample

30、 Processing for Chemical Analysis 4.2.1 Either EPA Method 3050B (via hot block) or EPA Method 3051A may be used for the digesting the friction material powder collected in 4.1. If analysis of antimony is desired, follow the optional digest listed in the EPA Method 3050B section 7.5 or EPA Method 305

31、1A section 11.3.2. 4.3 Chemical Analysis of Brake Friction Material Sample 4.3.1 Using the digested sample generated in section 4.2.1, perform an analysis for the desired chemical elements following EPA Method 6010C - Inductively Coupled Plasma - Atomic Emission Spectrometry or EPA Method 6020A - In

32、ductively Coupled Plasma-Mass Spectrometry (ICP-MS). Because of the complex and heterogeneous nature of brake friction materials, it is recommended that digestion and analysis for each pad be performed in triplicate (as a minimum) and the average value be reported. Percent Relative Standard Deviatio

33、n (standard deviation / measurements average *100) should be less than 20% for the triplicate measurements. Depending on the amount of specific components in the friction materials, additional dilutions during the analysis may be necessary. 4.3.2 Chromium detection 4.3.2.1 If chromium is identified

34、in section 4.3.1, at a level exceeding the criteria of 0.1% by weight, use EPA Method 3060A, followed by either EPA Method 7196A or EPA Method 7199, to determine the hexavalent chromium content. 1 mm/s 0.25 mm/s 0.15 mm/s Preferred Morphology SAE INTERNATIONAL J2975 Revised MAY2015 Page 6 of 8 4.3.2

35、.2 If the sample spike recovery during EPA Method 3060A is below 80%, it may indicate the presence of common sulfide-based compounds (S2-) or raw materials, such as antimony trisulfide, copper sulfide, molybdenum disulfide, metal alloys or others. Some of these materials and their reactions with oth

36、er constituents may mask the total amount of hexavalent chromium present in the formulation. In this event, conduct tests in triplicate for hexavalent chromium on all the individual chromium-based raw materials as declared by the manufacturer. 4.3.2.3 If the content of hexavalent chromium in all raw

37、 materials is below 0.1% by weight, the friction material composition can be certified as containing less than 0.1% of Cr(VI). If hexavalent chromium was at level exceeding 0.1% in at least one raw material proceed to point 4.3.2.4 4.3.2.4 In order to calculate the total hexavalent chromium present

38、in a given formulation, the supplier needs to identify the corresponding material content in percent-by-weight in the total formulation being tested. NOTE: As the actual contribution of hexavalent chromium is a function of the friction material formulation, it is the responsibility of the manufactur

39、er to demonstrate (through the product registration process) the actual contribution of hexavalent chromium to the total formulation, and to demonstrate compliance to any specific rule, regulation, or requirement applicable to the product. 4.3.3 If chromium is identified in section 4.3.1 at a level

40、exceeding the criteria of 0.1% by weight, then use either EPA Method 7196A - Chromium, Hexavalent (Colorimetric) or EPA Method 3060A - Alkaline Digestion for Hexavalent Chromium followed by EPA Method 7199 - Determination of Hexavalent Chromium in Drinking Water, Groundwater and Industrial Wastewate

41、r Effluents by Ion Chromatography to determine the hexavalent chromium content. 4.3.4 To determine the mercury contents, use one of the following methods: a. EPA Method 7471B b. EPA Method 245.5 c. EPA method 3051A and EPA method 6010C in tandem d. EPA method 3051A and EPA method 6020A in tandem NOT

42、E: The laboratory must ensure there is minimal loss of Mercury using a monitoring process of the sample matrix. For example, the laboratory should show minimal loss in matrix spike samples and not rely only on the Laboratory Control Sample (also known as Blank Spike Sample). Apply such controls to a

43、ll tested friction materials. 4.3.5 For asbestos fiber analysis, follow EPA/600/R-93/116 Method for the Determination of Asbestos in Bulk Building Materials. 4.4 Presentation of Results 4.4.1 At a minimum, the presentation of the results is to contain: Client Project Project Number Laboratory Name S

44、ample Identification - Manufacturer, Edge Code, etc. Sample Type - friction pad, friction block, etc. Laboratory Sample Number Matrix SAE INTERNATIONAL J2975 Revised MAY2015 Page 7 of 8 Sample Collection Date Sample Preparation Date Analysis Date Batch ID Preparation Method Code Preparation Method N

45、ame Analysis Method Number Code Analyte Name Result Detection Limit Reporting Limit Reporting Units Result Qualifier Basis (dry/wet) Dilution Spike Level % Recovery Upper Control Limit Lower Control Limit Relative Percent Difference (RPD) Sample Comments Result Comments 5. NOTES 5.1 Marginal Indicia

46、 A change bar (l) located in the left margin is for the convenience of the user in locating areas where technical revisions, not editorial changes, have been made to the previous issue of this document. An (R) symbol to the left of the document title indicates a complete revision of the document, in

47、cluding technical revisions. Change bars and (R) are not used in original publications, nor in documents that contain editorial changes only. PREPARED BY BRAKE LININGS STANDARDS COMMITTEE SAE INTERNATIONAL J2975 Revised MAY2015 Page 8 of 8 APPENDIX A - PUBLICALLY DISCLOSED FRICTION FORMULATIONS USED

48、 DURING THE INTERLABORATORY STUDY TO ESTABLISH THIS RECOMMENDED PRACTICE Chemical Supplier Material 1 Material 2 Material 3 Material 4 Material 5 Material 6 Phenolic Resin (straight) 9.50 9.50 9.50 9.50 9.50 9.50 Aramid Fiber DuPont 1F538 3.40 3.40 3.40 3.40 3.40 3.40 Graphite (synthetic) 20x100 8.70 8.70 8.70 8.70 8.70 8.70 Cashew Particle Brown 40 mesh 5.40 5.40 5.40 5.40 5.40 5.40 Nitrile Rubber Powder Zeon Chemicals Nipol 1411 2.60 2.60 2.60 2.60 2.60 2.60 Potassium Hexatitanate Kubota TXAX-MA 19.50 19.50 19.50 19.50 19.50 19.50 Zirconium Silicate Trebol 200 mesh 7.80 7.80 7.80 7.80