1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 4652:2012Rubber compoundingingredients Carbon black Determination of specificsurface area by nitrogenadsorption methods Single-point proceduresBS ISO 4652:2012 BRITISH STA
2、NDARDNational forewordThis British Standard is the UK implementation of ISO 4652:2012. It supersedes BS 5293-11:1995 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/50, Rubber - Raw, natural and synthetic, including latex and carbon black.A list of
3、 organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2012. Published by BSI Standards Limi
4、ted 2012ISBN 978 0 580 69690 9 ICS 83.040.20 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 July 2012.Amendments issued since publicationDate Text affectedBS
5、 ISO 4652:2012 ISO 2012Rubber compounding ingredients Carbon black Determination of specific surface area by nitrogen adsorption methods Single-point proceduresIngrdients de mlange du caoutchouc Noir de carbone Dtermination de la surface spcifique par mthodes par adsorption dazote Modes opratoires u
6、n point de mesureINTERNATIONAL STANDARDISO4652Second edition2012-06-15Reference numberISO 4652:2012(E)BS ISO 4652:2012ISO 4652:2012(E)ii ISO 2012 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2012All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or
7、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 ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax
8、+ 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 4652:2012ISO 4652:2012(E) ISO 2012 All rights reserved iiiContents PageForeword iv1 Scope 12 Normative references . 13 Method A, using Ni-Count-1 apparatus . 13.1 Principle . 13.2 Reagents 23.3 Apparatus 23.4 Prepa
9、ration of the sample . 53.5 Test conditions . 53.6 Procedure 63.7 Expression of results . 113.8 Test report .124 Method B, using an Areameter apparatus 124.1 Principle .124.2 Reagents 124.3 Apparatus 124.4 Preparation of the test portion .144.5 Test conditions .154.6 Procedure 154.7 Expression of re
10、sults .164.8 Test report .175 Method C, using gas chromatography 185.1 Principle .185.2 Reagents 185.3 Apparatus 185.4 Test conditions .195.5 Procedure 195.6 Expression of results .205.7 Test report .206 Method D, using a Monosorb surface-area analyser .216.1 Principle .216.2 Reagents 216.3 Apparatu
11、s 216.4 Initial installation .226.5 Test conditions .226.6 Calibration .226.7 Procedure 226.8 Expression of results .256.9 Test report .25Annex A (normative) Preparation of Areameter .27BS ISO 4652:2012ISO 4652:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide fe
12、deration 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 com
13、mittee. 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 accorda
14、nce 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
15、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 4652 was prepared by Technical Commi
16、ttee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.This second edition of ISO 4652 cancels and replaces ISO 4652-1:1994, which has been technically revised. The revision includes the following changes: The number of the stand
17、ard has been changed from ISO 4652-1 to ISO 4652, since there were no other parts. The title has been modified accordingly. A statement has been added to the scope that the multipoint method specified in ISO 18852 is the preferred method. The normative references in Clause 2 have been updated. The N
18、i-Count-1 apparatus used in method A is no longer available from the manufacturer. However, it has been decided to keep method A for those still using this apparatus. A note has been added at the beginning of Clause 3 to explain this.iv ISO 2012 All rights reservedBS ISO 4652:2012INTERNATIONAL STAND
19、ARD ISO 4652:2012(E)Rubber compounding ingredients Carbon black Determination of specific surface area by nitrogen adsorption methods Single-point proceduresWARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address
20、 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 four methods for the determination of
21、the specific surface area of types and grades of carbon black for use in the rubber industry: method A using the Ni-Count-1 apparatus (Clause 3); method B using the Areameter apparatus (Clause 4); method C using gas chromatography (Clause 5); method D using the Monosorb surface-area analyser (Clause
22、 6).Somewhat different results might be obtained from the four methods. The degassing procedure used differs from method to method, and it is important to investigate the possibility of correcting the results by using standard reference blacks.The results might also differ from those obtained using
23、the multipoint method specified in ISO 18852, which is the preferred method.2 Normative referencesThe 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 referen
24、ced document (including any amendments) applies.ISO 1126, Rubber compounding ingredients Carbon black Determination of loss on heatingISO 18852, Rubber compounding ingredients Determination of multipoint nitrogen surface area (NSA) and statistical thickness surface area (STSA)3 Method A, using Ni-Co
25、unt-1 apparatusNOTE Although the Ni-Count-1 apparatus is no longer being produced by the manufacturer, E.G. then resume evacuation.3.6.2.9 Close the vacuum valve and observe the leak detector to determine whether gases are still evolving from the test portion. If the test portion is properly degasse
26、d, the leak indicator should not show a change of pressure greater than 0,1 kPa (1 mmHg) over 5 min.3.6.2.10 Isolate the degassed test portion from the vacuum manifold by closing the valve. Remove the heater.3.6.2.11 If the pressure in the purged nitrogen reservoir is above 65,7 kPa (493 mmHg) at 23
27、 C or above 66,7 kPa (500 mmHg) at 27 C, evacuate to a lower pressure. Complete evacuation is not necessary unless air has been permitted to enter.Fill the purged reservoir gauge and manifold with nitrogen gas to a pressure of 65,7 kPa (493 mmHg) if the temperature is 23 C, or to 66,7 kPa (500 mmHg)
28、 if the temperature is 27 C. For each degree respectively above or below the indicated temperatures, add or subtract 0,222 kPa (1,67 mmHg) from the specified pressures.3.6.2.12 Open the valve from the nitrogen reservoir to the sample tube by rotating it through three complete turns.3.6.2.13 Place th
29、e Dewar flask (3.3.4) filled with liquid nitrogen (3.2.2) around the sample tube. ISO 2012 All rights reserved 7BS ISO 4652:2012ISO 4652:2012(E)Table 2 Liquid-nitrogen temperature-correction factorNitrogen vapour pressureCorrection factorNitrogen vapour pressureCorrection factorNitrogen vapour press
30、ureCorrection factorNitrogen vapour pressureCorrection factorpNB pNB pNB pNBmmHg kPa mmHg kPa mmHg kPa mmHg kPa 660 88,0 0,954 16 695 92,7 0,974 22 730 97,3 0,994 27 765 102,0 1,014 32661 88,1 0,954 73 696 92,8 0,974 79 731 97,5 0,994 84 766 102,1 1,014 90662 88,3 0,955 31 697 92,9 0,975 36 732 97,6
31、 0,995 42 767 102,3 1,015 47663 88,4 0,955 88 698 93,1 0,975 93 733 97,7 0,995 99 768 102,4 1,016 04664 88,5 0,956 45 699 93,2 0,976 51 734 97,9 0,996 56 769 102,5 1,016 62665 88,7 0,957 03 700 93,3 0,977 08 735 98,0 0,997 14 770 102,7 1,017 19666 88,8 0,957 60 701 93,5 0,977 65 736 98,1 0,997 71 77
32、1 102,8 1,017 76667 88,9 0,958 17 702 93,6 0,978 23 737 98,3 0,998 28 772 102,9 1,018 34668 89,1 0,958 74 703 93,7 0,978 80 738 98,4 0,998 85 773 103,1 1,018 91669 89,2 0,959 32 704 93,9 0,979 37 739 98,5 0,999 43 774 103,2 1,019 48670 89,3 0,959 89 705 94,0 0,979 95 740 98,7 1,000 00 775 103,3 1,02
33、0 05671 89,5 0,960 46 706 94,1 0,980 52 741 98,8 1,000 57 776 103,5 1,020 63672 89,6 0,961 04 707 94,3 0,981 09 742 98,9 1,001 15 777 103,6 1,021 20673 89,7 0,961 61 708 94,4 0,981 66 743 99,1 1,001 72 778 103,7 1,021 77674 89,9 0,962 18 709 94,5 0,982 24 744 99,2 1,002 29 779 103,9 1,022 35675 90,0
34、 0,962 76 710 94,7 0,982 81 745 99,3 1,002 86 780 104,0 1,022 92676 90,1 0,963 33 711 94,8 0,983 38 746 99,5 1,003 44 781 104,1 1,023 49677 90,3 0,963 90 712 94,9 0,983 96 747 99,6 1,004 01 782 104,3 1,024 07678 90,4 0,964 47 713 95,1 0,984 53 748 99,7 1,004 58 783 104,4 1,024 64679 90,5 0,965 05 71
35、4 95,2 0,985 10 749 99,9 1,005 16 784 104,5 1,025 21680 90,7 0,965 62 715 95,3 0,985 68 750 100,0 1,005 73 785 104,7 1,025 78681 90,8 0,966 19 716 95,5 0,986 25 751 100,1 1,006 30 786 104,8 1,026 36682 90,9 0,966 77 717 95,6 0,986 82 752 100,3 1,006 88 787 104,9 1,026 93683 91,1 0,967 34 718 95,7 0,
36、987 39 753 100,4 1,007 45 788 105,1 1,027 50684 91,2 0,967 91 719 95,9 0,987 97 754 100,5 1,008 02 789 105,2 1,028 08685 91,3 0,968 49 720 96,0 0,988 54 755 100,7 1,008 59 790 105,3 1,028 65686 91,5 0,969 06 721 96,1 0,989 11 756 100,8 1,009 17 791 105,5 1,029 22687 91,6 0,969 63 722 96,3 0,989 69 7
37、57 100,9 1,009 74 792 105,6 1,029 80688 91,7 0,970 20 723 96,4 0,990 26 758 101,1 1,010 31 793 105,7 1,030 37689 91,9 0,970 78 724 96,5 0,990 83 759 101,2 1,010 89 794 105,9 1,030 94690 92,0 0,971 35 725 96,7 0,991 41 760 101,3 1,011 46 795 106,0 1,031 51691 92,1 0,971 92 726 96,8 0,991 98 761 101,5
38、 1,012 03 796 106,1 1,032 09692 92,3 0,972 50 727 96,9 0,992 55 762 101,6 1,012 61 797 106,3 1,032 66693 92,4 0,973 07 728 97,1 0,993 12 763 101,7 1,013 18 798 106,4 1,033 23694 92,5 0,973 64 729 97,2 0,993 70 764 101,9 1,013 75 799 106,5 1,033 81NOTE The liquid-nitrogen temperature-correction facto
39、r B is derived from the formula 1 + 0,057 3 (pN 98,7)/13,3,wherepNis the vapour pressure, in kilopascals, of pure nitrogen at the nitrogen adsorption temperature, measured by means of the nitrogen vapour pressure thermometer (3.3.5);98,7 is the barometric pressure, in kilopascals, during calibration
40、 of the apparatus to determine area S at the equilibrium pressure (see Table 3).If the pressure is expressed in millimetres of mercury, the above formula becomes 1 + 0,057 3 (pN 740)/100.8 ISO 2012 All rights reservedBS ISO 4652:2012ISO 4652:2012(E)Table 3Equilibrium pressureCorrela- ting factorSur-
41、 face areaEquilibrium pressureCorrela- ting factorSur- face areaEquilibrium pressureCorrela- ting factorSur- face areammHg kPa F S mmHg kPa F S mmHg kPa F S100 13,3 0,006 99 255,7 140 18,6 0,010 94 213,8 180 23,9 0,015 98 176,3101 13,4 0,007 08 254,6 141 18,7 0,011 05 212,8 181 24,1 0,016 12 175,410
42、2 13,5 0,007 17 253,5 142 18,9 0,011 17 211,8 182 24,2 0,016 26 174,5103 13,7 0,007 26 252,4 143 19,0 0,011 28 210,8 183 24,3 0,016 41 173,7104 13,8 0,007 35 251,3 144 19,1 0,011 39 209,8 184 24,5 0,016 56 172,8105 13,9 0,007 44 250,2 145 19,3 0,011 51 208,8 185 24,6 0,016 70 171,9106 14,1 0,007 53
43、249,1 146 19,4 0,011 62 207,9 186 24,7 0,016 85 171,0107 14,2 0,007 62 248,0 147 19,5 0,011 73 206,9 187 24,9 0,017,00 170,2108 14,3 0,007 71 247,0 148 19,7 0,011 85 205,9 188 25,0 0,017 15 169,3109 14,5 0,007 81 245,9 149 19,8 0,011 97 204,9 189 25,1 0,017 31 168,5110 14,6 0,007 90 244,8 150 19,9 0
44、,012 08 204,0 190 25,3 0,017 46 167,6111 14,7 0,007 99 243,7 151 20,1 0,012 20 203,0 191 25,4 0,017 61 166,8112 14,9 0,008 09 241,7 152 20,2 0,012 32 202,0 192 25,5 0,017 77 165,9113 15,0 0,008 18 241,6 153 20,3 0,012 44 201,1 193 25,7 0,017 93 165,1114 15,1 0,008 28 240,5 154 20,5 0,012 56 200,1 19
45、4 25,8 0,018 08 164,2115 15,3 0,008 37 239,5 155 20,6 0,012 68 199,2 195 25,9 0,018 24 163,4116 15,4 0,008 47 238,4 156 20,7 0,012 80 198,2 196 26,1 0,018 40 162,5117 15,5 0,008 56 237,3 157 20,9 0,012 93 197,3 197 26,2 0,018 56 161,7118 15,7 0,008 66 236,3 158 21,0 0,013 05 196,3 198 26,3 0,018 73
46、160,9119 15,8 0,008 76 235,2 159 21,1 0,013 17 195,4 199 26,5 0,018 89 160,0120 15,9 0,008 86 234,2 160 21,3 0,013 30 194,5 200 26,6 0,019 05 159,2121 16,1 0,008 96 233,1 161 21,4 0,013 42 193,5 201 26,7 0,019 22 158,4122 16,2 0,009 06 232,1 162 21,5 0,013 55 192,6 202 26,9 0,019 39 157,6123 16,3 0,
47、009 16 231,0 163 21,7 0,013 68 191,7 203 27,0 0,019 56 156,8124 16,5 0,009 26 230,0 164 21,8 0,013 81 190,7 204 27,1 0,019 73 155,9125 16,6 0,009 36 229,0 165 21,9 0,013 93 189,8 205 27,3 0,019 90 155,1126 16,7 0,009 46 227,9 166 22,1 0,014 06 188,9 206 27,4 0,020 07 154,3127 16,9 0,009 56 226,9 167
48、 22,2 0,014 19 188,0 207 27,5 0,020 24 153,5128 17,0 0,009 66 225,9 168 22,3 0,014 33 187,1 208 27,7 0,020 42 152,7129 17,1 0,009 77 224,9 169 22,5 0,014046 186,1 209 27,8 0,020 59 151,9130 17,3 0,009 87 223,8 170 22,6 0,014 59 185,2 210 27,9 0,020 77 151,1131 17,4 0,009 97 222,8 171 22,7 0,014 73 1
49、84,3 211 28,1 0,020 95 150,3132 17,5 0,010 08 221,8 172 22,9 0,014 86 183,4 212 28,2 0,021 13 149,5133 17,7 0,010 19 220,8 173 23,0 0,015 00 182,5 213 28,3 0,021 31 148,7134 17,8 0,010 29 219,9 174 23,1 0,015 13 181,6 214 28,5 0,021 50 147,9135 17,9 0,010 40 218,8 175 23,3 0,015 27 180,7 215 28,6 0,021 68 147,2136 18,1 0,010 51 217,8 176 23,4 0,015 41 179,8 216 28,7 0,021 87 146,4137 18,2 0,010 61 216,8 177 23,5 0,015 55 178,9 217 28,9 0,022 06 145,6138 18,3 0,010 72 215,8 178 23,7 0,015 69 178,1 218 2
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