1、Designation: D7724 11 (Reapproved 2016)D7724 18Standard Test Method forCarbon BlackNon-Dispersible Matter by MechanicalFlushing (NDM)1This standard is issued under the fixed designation D7724; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of non-dispersible matter after mechanical water flush
3、ing of regular untreatedcarbon blacks. It may not be applicable to oil-treated carbon blacks because the oil would prevent proper wetting of the black bywater.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standa
4、rd does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.1.3 This standard does not purpo
5、rt to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability ofregulatory limitations prior to use.1.4 This international standard w
6、as developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced
7、 Documents2.1 ASTM Standards:2D1799 Practice for Carbon BlackSampling Packaged ShipmentsD1900 Practice for Carbon BlackSampling Bulk ShipmentsD4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesE11 Specification for Woven Wire Test
8、 Sieve Cloth and Test Sieves3. Summary of Test Method3.1 A sample of carbon black is mechanically flushed with water through a wire-mesh screen of a specified size until all thatremains is a non-dispersible matter of carbon black. The non-dispersible matter is dried, weighed, and the amount of resid
9、ue isexpressed as mg/kg (ppm) of the original sample.4. Significance and Use4.1 The quantity of non-dispersible matter of carbon black is important in some molded or extruded products as it may relateto the surface appearance of those products. The maximum amount of non dispersible matter and the mi
10、nimum size of the particlesto be analyzed in each application is normally determined and agreed to between the user and the producer.1 This test method is under the jurisdiction of ASTM Committee D24 on Carbon Black and is the direct responsibility of Subcommittee D24.31 on Non-Carbon BlackComponent
11、s of Carbon Black.Current edition approved June 1, 2016June 1, 2018. Published July 2016July 2018. Originally approved in 2011. Last previous edition approved in 20112016 asD7724 11.D7724 11 (2016). DOI: 10.1520/D7724-11R16.10.1520/D7724-18.2 For referencedASTM standards, visit theASTM website, www.
12、astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what
13、 changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the
14、official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Apparatus5.1 Sieve Apparatus, as shown in Fig. 1.35.2 Balance, with a sensitivity of 0.01 g.5.3 Analytical Balance, with a sensitivity of 0.1 mg.5.4 Oven, gravity-co
15、nvection type, capable of temperature regulation within 61C at 125C and temperature uniformity within65C.5.5 Sieves, diameter 100 mm, of either phosphor bronze or stainless steel.3 The sieve shall be in accordance with SpecificationE11. The sieve size to be used shall be agreed upon between the purc
16、haser and the carbon black manufacture.5.6 Weighing Dishes.6. Precautions6.1 Install the apparatus as described in the manufacturers instructions and keep it clean at all times to prevent contamination.6.2 Examine the sieves each time they are used to make sure that no cracks or holes have developed
17、.7. Sampling7.1 Samples shall be taken in accordance with Practice D1799 or Practice D1900.8. Procedure8.1 Prior to each test series adjust the water pressure to 400 6 20 kPa in accordance with the manufacturers instructions. Makesure that only the spraying nozzle is operating when pressure is adjus
18、ted.NOTE 1The pressure will drop when the cleaning nozzles are operating in addition to the spraying nozzle.8.2 Attach the sieve to the apparatus in accordance with the manufacturers instructions and push the “flush” button for at least5 s. The water is flushed through the nozzles as long as the “fl
19、ush” button is pushed.8.3 After releasing the “flush” button disassemble the sieve and examine the sieve for particles. If no particles are observedreattach the sieve.8.4 Weigh 500 6 5 g of the sample into a container and transfer the sample quantitatively into the cylinder of the test apparatus.Not
20、e the correct weight for the calculation of the non dispersible matter.3 The sole source of supply of the apparatus known to the committee at this time is Krahnen IQS, GmbH, Paffrather Str. 1315, D-51069 Koeln, Germany. If you are awareof alternative suppliers, please provide this information toASTM
21、 International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1 which you may attend.FIG. 1 Schematic Diagram of NDA Test EquipmentD7724 1828.5 Press the “start” button and close the lid slowly while the spraying nozzle is rotating wi
22、thout any water flushing. Theflushing process will start automatically.8.6 Based on a predefined program the sample will be flushed through the sieve by the water spray nozzles. For details referto Fig. 1.8.7 Avacuum is applied periodically to keep the non dispersible particles immobilized on the si
23、eve in order to wash dispersibleproduct from the non dispersible matter. The vacuum application is also part of the automated process.8.8 The end of the test is indicated by a vacuum application without any water flowing. After that the measurement stops.8.9 Disassemble the sieve and dry in an oven
24、at a temperature of 125C for 1 h.8.10 Quantitatively transfer the non dispersible matter to a tared weighing dish and weigh to the nearest 0.1 mg using theanalytical balance.9. Calculation9.1 Calculate the non-dispersible matter to the nearest mg/kg (ppm) as follows:R 5W/S! 3106 (1)where:R = Non-dis
25、persible matter (NDM), mg/kg (ppm),W = mass of sieve residue, g, andS = mass of sample, g.10. Report10.1 Report the following information:10.1.1 Proper identification of the sample,10.1.2 Identification of the sieve size, and10.1.3 Result of the determination reported to the nearest mg/kg (ppm).11.
26、Precision and Bias11.1 Precision and bias These precision statements have not been generated.been prepared in accordance with PracticeD4483-99. Refer to this practice for terminology and other statistical details.11.2 A type 1 inter-laboratory precision program was conducted using two different siev
27、es: 45 m (No. 325 sieve) and 125 m(No. 120 sieve). In each laboratory two single tests were performed on each of two different days (total of four tests). A test resultis the value obtained from a single determination. Both repeatability and reproducibility represent short-term (daily) testingcondit
28、ions. Acceptable difference values were not measured.11.3 The precision results in this precision and bias section give an estimate of the precision of this test method with thematerials used in the particular interlaboratory program described below. The precision parameters should not be used forac
29、ceptance or rejection testing of any group of materials without documentation that they are applicable to those particularmaterials and the specific testing protocols of the test method. Any appropriate value may be used from Table 1 and Table 2.11.4 The results of the precision calculations for thi
30、s test are given in Table 1 and Table 2. In each of these tables the materialsare arranged in descending “mean level” order. The preferred precision is shown in bold text.11.5 RepeatabilityThe pooled relative repeatability, (r), of this test has been established as 33.9 % for the 45 m sieve (SieveNo
31、. 325) and as 100.4 % for the 125 m sieve (Sieve No. 120).Any other value in Table 1 and Table 2 may be used as an estimateof repeatability, as appropriate. The difference between two single test results (or determinations) found on identical test materialunder the repeatability conditions prescribe
32、d for this test will exceed the repeatability on an average of not more than once in 20TABLE 1 Precision Parameters for D7724, Carbon Black Non-Dispersible Material by Mechanical Flushing (NDM), (Type 1 Precision),45 m (Sieve No. 325)AUnits mg/kg (ppm)Material PeriodNumber ofLaboratories(M/H/L)BMean
33、 Level Sr r (r) SR R (R)A 2017 16(0/1/0) 81.2 6.66 18.85 23.2 12.40 35.10 43.2C 2017 17(0/0/0) 24.9 4.04 11.43 46.0 6.93 19.61 78.9B 2017 16(0/1/0) 9.5 1.82 5.14 54.2 5.54 15.68 165.2Average 38.5Pooled Values 4.62 13.07 33.9 8.80 24.91 64.7A Preferred precision shown in bold text.B M = number of out
34、liers for Mean; H = number of outliers for High variation; L = number of outliers for Low variation.D7724 183cases in the normal and correct operation of the method. Two single test results that differ by more than the appropriate value fromTable 1 and Table 2 must be suspected of being from differe
35、nt populations and some appropriate action taken.NOTE 2Appropriate action may be an investigation of the test method procedure or apparatus for faulty operation or the declaration of a significantdifference in the two materials, samples, etc., which generated the two test results.11.6 Reproducibilit
36、yThe pooled relative reproducibility, (R), of this test has been established as 64.7 % or the 45 m sieve(Sieve No. 325) and as 171.4 % for the 125 m sieve (Sieve No. 120). Any other value in Table 1 and Table 2 may be used asan estimate of reproducibility, as appropriate. The difference between two
37、single and independent test results found by twooperators working under the prescribed reproducibility conditions in different laboratories on identical test material will exceed thereproducibility on an average of not more than once in 20 cases in the normal and correct operation of the method. Two
38、 singletest results produced in different laboratories that differ by more than the appropriate value from Table 1 and Table 2 must besuspected of being from different populations and some appropriate investigative or technical/commercial action taken.11.7 BiasBias is the difference between a test v
39、alue and a reference value. However, for this test method, bias has not beendetermined.12. Keywords12.1 carbon black; non-dispersible matterAPPENDIX(Nonmandatory Information)X1. DRY CLASSIFICATION OF NON-DISPERSIBLE MATTERX1.1 IntroductionX1.1.1 As mentioned in 5.5 the sieve size to be used for the
40、determination of non-dispersible matter (NDM) shall be agreed uponbetween the purchaser and the carbon black manufacturer.X1.1.2 In some cases it can be of interest to determine NDM using more than one sieve size, for example, with a 45 m sieve(Sieve No. 325) and with a 125 m sieve (Sieve No. 120).
41、In principle this requires two independent tests with the specified sieves.X1.1.3 As an alternative, the dried residue from the determination with the finer sieve (here: 45 m) can be classified through acoarser sieve (here: 125 m) in order to obtain test results for NDM for two sieve sizes. The adva
42、ntage of such approach is thatit saves one additional NDM wet sieving test and it reduces the sample quantity required.X1.2 ApparatusX1.2.1 Sieves, of either phosphor bronze or stainless steel. The sieve shall be in accordance with Specification E11. Sieve opening125 m (Sieve No. 120), typical diame
43、ter 50 mm.X1.2.2 Weighing dish.TABLE 2 Precision Parameters for D7724, Carbon Black Non-Dispersible Material by Mechanical Flushing (NDM), (Type 1 Precision),125 m (Sieve No. 120)AUnits mg/kg (ppm)Material PeriodNumber ofLaboratories(M/H/L)BMean Level Sr r (r) SR R (R)C 2017 14(1/1/3) 3.6 1.30 3.69
44、101.4 2.23 6.30 173.1B 2017 14(0/1/3) 2.0 0.69 1.96 97.9 1.14 3.22 160.7A 2017 14(0/1/3) 2.0 0.52 1.46 73.2 0.94 2.67 133.7Average 2.5Pooled Values 0.90 2.56 100.4 1.54 4.37 171.4A Preferred precision shown in bold text.B M = number of outliers for Mean; H = number of outliers for High variation; L
45、= number of outliers for Low variation.D7724 184X1.3 ProcedureX1.3.1 Carry out the test according to ASTM D7724 using a 45 m sieve (Sieve No. 325).X1.3.2 Report the test result.X1.3.3 Do not discard the dried residue from this test.X1.3.4 Pour the dried residue on the small 125 m sieve (Sieve No. 12
46、0) and hold the sieve above a weighing dish.X1.3.5 Move the sieve gently to pass through all particles with a diameter smaller than 125 m.X1.3.6 When completed, weigh out and enter the result into the report sheet.X1.4 Test ResultsX1.4.1 This procedure has been applied as an additional method when p
47、erforming the ITP to create the precision data in Section11. The results are shown in Table X1.1.X1.5 PrecautionsX1.5.1 When comparing the test results from this “dry” determination with the ones of the regular NDM test using a 125 m sieve(Sieve No. 120), it turns out that the results are not equiva
48、lent: The dry classification leads to higher test results by a factor ofroughly 2.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the v
49、alidity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,
