BS ISO 1126-2015 Rubber compounding ingredients Carbon black Determination of loss on heating《橡胶配合剂 炭黑 加热损失的测定》.pdf

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1、BSI Standards PublicationBS ISO 1126:2015Rubber compoundingingredients Carbon black Determination of loss onheatingBS ISO 1126:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 1126:2015. Itsupersedes BS ISO 1126:2006 which is withdrawn.The UK participation

2、in its preparation was entrusted to TechnicalCommittee PRI/50, Rubber - Raw, natural and synthetic, includinglatex and carbon black.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovision

3、s of a contract. Users are responsible for its correctapplication. The British Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 89096 3ICS 83.040.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published unde

4、r the authority of theStandards Policy and Strategy Committee on 30 September 2015.Amendments issued since publicationDate Text affectedBS ISO 1126:2015 ISO 2015Rubber compounding ingredients Carbon black Determination of loss on heatingIngrdients de mlange du caoutchouc Noir de carbone Dtermination

5、 de la perte la chaleurINTERNATIONAL STANDARDISO1126Fifth edition2015-09-15Reference numberISO 1126:2015(E)BS ISO 1126:2015ISO 1126:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this pu

6、blication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the co

7、untry of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 1126:2015ISO 1126:2015(E)Foreword iv1 Scope . 12 Method 1: Gravity-convection oven method 12.1 Principle 12.2 Apparatus

8、12.3 Procedure 22.3.1 Precautions . 22.3.2 Determination 22.4 Expression of results 23 Method 2: Moisture balance method . 23.1 Principle 23.2 Apparatus 23.3 Procedure 33.4 Calculation 34 Method 3: Infrared irradiation method (rapid method) 34.1 Principle 34.2 Apparatus 34.3 Procedure 45 Differences

9、 between method 2 and method 3 . 56 Precision . 57 Test report . 5Annex A (informative) Precision . 6 ISO 2015 All rights reserved iiiContents PageBS ISO 1126:2015ISO 1126:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (

10、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, go

11、vernmental 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.The procedures used to develop this document and those intended for its further maint

12、enance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Atten

13、tion 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. Details of any patent rights identified during the development of the document will be in the Introduction

14、 and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformit

15、y assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (

16、including latex) for use in the rubber industry.This fifth edition cancels and replaces the fourth edition (ISO 1126:2006), of which it constitutes a minor revision with the following changes: method 1 is stated as the preferred method in the scope; precision data were moved in an informative annex.

17、iv ISO 2015 All rights reservedBS ISO 1126:2015INTERNATIONAL STANDARD ISO 1126:2015(E)Rubber compounding ingredients Carbon black Determination of loss on heatingWARNING Persons using this International Standard should be familiar with normal laboratory practice. This International Standard does not

18、 purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.1 ScopeThis International Standard specifies methods for determi

19、ning the loss on heating of carbon black for use in the rubber industry. This loss on heating is due primarily to loss of moisture, but traces of other volatile materials may also be lost.These methods are not applicable to treated carbon blacks which contain added volatile materials.One of the foll

20、owing three methods is used: method 1: gravity-convection oven method; method 2: moisture balance method; method 3: infrared irradiation method (rapid method).Method 1 is the preferred method.2 Method 1: Gravity-convection oven method2.1 PrincipleA test portion of carbon black is heated for 1 h at a

21、 temperature of 125 C in a weighing bottle. The weighing bottle plus contents is allowed to cool in a desiccator to room temperature and weighed, and the percentage loss on heating calculated.Apparatus equivalent to that specified may be used provided the same results are obtained.2.2 Apparatus2.2.1

22、 Oven, gravity-convection type, the temperature of which can be regulated to within 1 C at 125 C and the temperature uniformity of which is 5 C or better.2.2.2 Weighing bottle, squat-form, 30 mm in height and 60 mm in diameter, fitted with a ground-glass stopper.When larger samples are required for

23、other tests, use an open vessel of dimensions such that the depth of the black is not greater than 10 mm during conditioning.2.2.3 Analytical balance, accurate to 0,1 mg.2.2.4 Desiccator. ISO 2015 All rights reserved 1BS ISO 1126:2015ISO 1126:2015(E)2.3 Procedure2.3.1 Precautions2.3.1.1 Take the sam

24、ple of carbon black in a tightly stoppered glass bottle or friction-top can. Allow the closed container to reach ambient temperature before starting the test.2.3.1.2 To prevent loss of carbon black due to air currents, keep the weighing bottle stoppered when transferring to and from the desiccator.2

25、.3.2 Determination2.3.2.1 Dry the weighing bottle (2.2.2) and the stopper, with the stopper removed, for 30 min in the oven (2.2.1) set at 125 C. Then place the bottle and the stopper in the desiccator (2.2.4) and allow to cool to room temperature. Weigh the bottle with stopper to the nearest 0,1 mg

26、.2.3.2.2 Weigh about 2 g of carbon black to the nearest 0,1 mg into the weighing bottle.2.3.2.3 Place the weighing bottle, test portion, and stopper in the oven (2.2.1) for 1 h at 125 C, with the stopper removed.2.3.2.4 Insert the stopper and transfer the bottle and contents to the desiccator. Remov

27、e the stopper and allow to cool to ambient temperature. Re-insert the stopper in the weighing bottle and reweigh to the nearest 0,1 mg.2.4 Expression of resultsCalculate the loss on heating, expressed as a percentage by mass, to the nearest 0,1 % using Formula (1):Hmmmm=1210100 (1)whereH is the loss

28、 on heating, in %;m0is the mass, in grams, of the weighing bottle and stopper;m1is the mass, in grams, of the weighing bottle, stopper and test portion before heating;m2is the mass, in grams, of the weighing bottle, stopper and test portion after heating.3 Method 2: Moisture balance method3.1 Princi

29、pleA test portion of carbon black is heated at a temperature of not more than 125 C and the decrease in mass measured using a moisture balance.Apparatus equivalent to that specified may be used provided the same results are obtained.3.2 Apparatus3.2.1 Moisture balance, having a sensitivity of 0,1 mg

30、 and fitted with an indirect heating source.2 ISO 2015 All rights reservedBS ISO 1126:2015ISO 1126:2015(E)3.3 Procedure3.3.1 Set up the moisture balance in accordance with the manufacturers instructions. The temperature shall not exceed 125 C.3.3.2 Place approximately 2 g of carbon black into the mo

31、isture balance and determine its mass to the nearest 0,1 mg.3.3.3 Close the lid and start the machine.3.3.4 Once the mass loss, under these drying conditions, is less than 1 mg over 30 s, the test portion is considered dry and the percent mass loss shall be recorded to the nearest 0,1 %.3.4 Calculat

32、ionIf the test result is not displayed automatically by the instrument, calculate the percent loss on heating as follows:HABA=100 (2)whereH is the loss on heating, in %;A is the mass, in grams, of the test portion before heating;B is the mass, in grams, of the test portion after heating.4 Method 3:

33、Infrared irradiation method (rapid method)4.1 PrincipleA test portion of carbon black is heated by infrared irradiation from an infrared lamp and the loss on heating measured as the decrease in mass using an infrared moisture meter.Apparatus equivalent to that specified may be used provided the same

34、 results are obtained.4.2 Apparatus4.2.1 Infrared moisture meter, having a sensitivity of 1 mg.The moisture meter shall be either a distance-adjusting-type meter using a 185 W infrared lamp or a voltage-adjusting-type meter using a 250 W infrared lamp. In either case, the meter shall be equipped wit

35、h an analytical balance. Figure 1 shows an example of an infrared moisture meter.In principle, the meter used shall have a capacity of 5 g, regardless of whether it is a distance- or voltage-adjusting-type meter. A meter of different capacity may be used provided that it offers the same accuracy as

36、a 5 g capacity meter. When using a newly purchased meter, the calibrated scale of the meter shall be checked, either after a specific period of time or as deemed necessary. ISO 2015 All rights reserved 3BS ISO 1126:2015ISO 1126:2015(E)Dimensions in millimetresKey1 infrared lamp hood2 infrared lamp (

37、 100 mm 137 mm height)3 sample dish4 digital display5 grip6 moisture meterFigure 1 Example of an infrared moisture meter4.3 Procedure4.3.1 Set up the moisture meter in accordance with the manufacturers instructions.4.3.2 Weigh 5 g of the sample to the nearest 0,01 g and spread it evenly over the sam

38、ple dish of the infrared moisture meter.4.3.3 Start the machine.4.3.4 The upper rim of the sample dish is set at a distance of 75 mm 2 mm from the central surface of the infrared lamp of the moisture meter. Infrared irradiation is then delivered to the sample.4.3.5 When the change in the meter readi

39、ng falls to 0,05 % or below per minute of irradiation, record the value given after a further 2 min have elapsed. This value is taken as the loss on heating. It is expressed as a percentage.4 ISO 2015 All rights reservedBS ISO 1126:2015ISO 1126:2015(E)5 Differences between method 2 and method 3Table

40、 1 Comparison of methods 2 and 3Method 2 Method 3Apparatus Moisture balance Infrared moisture meterSensitivity 0,1 mg 1,0 mgMeasurement method Indirect heating source Direct heating sourceDistance-adjusting-typeVoltage-adjusting-typeMeasurement tempera-tureNot to exceed 125 C Mass of test portion Ab

41、out 2 g About 5 gPoint at which reading is takenOnce the mass loss, under these drying con-ditions, is less than 1 mg over 30 s, the test portion is considered dry and the percent mass loss is recorded to the nearest 0,1 %.When the change in the meter read-ing (loss on heating) falls to 0,05 % or be

42、low per minute of irradiation, then the value given after a further 2 min have elapsed is recorded.Calculation of resultHABA=100 Automatic readout6 PrecisionSee Annex A.7 Test reportThe test report shall include the following particulars:a) a reference to this International Standard, i.e. ISO 1126;b

43、) the method used;c) all details necessary to identify the sample;d) the test result in %, expressed to the nearest 0,1 %;e) any unusual features noted during the determination;f) any operation not included in this International Standard or regarded as optional;g) the date of the determination. ISO

44、2015 All rights reserved 5BS ISO 1126:2015ISO 1126:2015(E)Annex A (informative) PrecisionA.1 GeneralMethod 1 and method 3 were compared in various laboratories using several different samples. The precision data are reported in Table A.1 and Table A.2.A.2 Precision data for method 1 using the gravit

45、y-convection oven method (drying for 1 h at 125 C)Table A.1 Precision data Loss on heating (%) by method 1Sample Mean levelWithin laboratory Between laboratoriessrr (r) sRR (R)A 0,39 0,034 0,097 25,10 0,037 0,105 27,24B 0,78 0,052 0,146 18,73 0,052 0,148 19,02C 1,36 0,065 0,183 13,47 0,065 0,183 13,

46、47D 2,40 0,091 0,258 10,76 0,105 0,296 12,33E 4,49 0,142 0,402 8,96 0,143 0,403 8,99Pooled 1,88 0,085 0,242 12,85 0,087 0,252 13,37sr= within-laboratory standard deviationr = repeatability (in measurement units)(r) = repeatability (in percent)sR= between-laboratory standard deviationR = reproducibil

47、ity (in measurement units)(R) = reproducibility (in percent)6 ISO 2015 All rights reservedBS ISO 1126:2015ISO 1126:2015(E)A.3 Precision data for method 3 using the infrared irradiation methodTable A.2 Precision data Loss on heating (%) by method 3Sample Mean levelWithin laboratory Between laboratori

48、essrr (r) sRR (R)A 0,38 0,041 0,116 30,39 0,041 0,116 30,50B 0,77 0,053 0,151 19,67 0,053 0,151 19,67C 1,24 0,066 0,186 15,01 0,066 0,186 15,01D 2,22 0,079 0,222 9,94 0,079 0,222 9,94E 4,31 0,111 0,314 7, 29 0,111 0,314 7, 29Pooled 1,78 0,074 0,209 11,71 0,074 0,209 11,71sr= within-laboratory standa

49、rd deviationr = repeatability (in measurement units)(r) = repeatability (in percent)sR= between-laboratory standard deviationR = reproducibility (in measurement units)(R) = reproducibility (in percent) ISO 2015 All rights reserved 7BS ISO 1126:2015ISO 1126:2015(E) ISO 2015 All rights reservedICS 83.040.20Price based on 7 pagesThis page deliberately left blankBSI is the national body responsible for preparing British Standards and other standards-related publications, information an