1、INTERNATIONALSTANDARDISO18753First edition2004-08-15Reference numberISO 18753:2004(E) ISO 2004Fine ceramics (advanced ceramics, advanced technical ceramics) Determination of absolute density of ceramic powders by pyknometerCramiques techniques Dtermination de la masse volumique absolue des poudres c
2、ramiques laide dun pycnomtreCopyright International Organization for Standardization Reproduced by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-ISO 18753:2004(E)ii ISO 2004 All rights reservedPDF disclaimerThis PDF file may contain embed
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8、-,-ISO 18753:2004(E) ISO 2004 All rights reserved iiiForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies(ISO member bodies). The work of preparing International Standards is normally carried out through ISOtechnical committees. Each
9、 member body interested in a subject for which a technical committee has beenestablished has the right to be represented on that committee. International organizations, governmental andnon-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the InternationalE
10、lectrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standardsadopt
11、ed by the technical committees are circulated to the member bodies for voting. Publication as anInternational Standard requires 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 patentr
12、ights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 18753 was prepared by Technical Committee ISO/TC 206, Fine ceramics.Copyright International Organization for Standardization Reproduced by IHS under license with ISO Not for ResaleNo reproduction or networking
13、 permitted without license from IHS-,-.ivCopyright International Organization for Standardization Reproduced by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-INTERNATIONAL STANDARD ISO 18753:2004(E) ISO 2004 All rights reserved 1Fine cera
14、mics (advanced ceramics, advanced technical ceramics) Determination of absolute density of ceramic powders by pyknometer1ScopeThis International Standard specifies a method for determining the particle density of fine ceramic powdersusing liquid pyknometry.2 Normative referencesThe following referen
15、ced documents are indispensable for the application of this document. For datedreferences, only the edition cited applies. For undated references, the latest edition of the referenced document(including any amendments) applies.ISO 758, Liquid chemical products for industrial use Determination of den
16、sity at 20 CISO 3507, Laboratory glassware PyknometersISO 6353-2, Reagents for chemical analysis Part 2: Specifications First seriesISO 6353-3, Reagents for chemical analysis Part 3: Specifications Second seriesISO 8213, Chemical products for industrial use Sampling techniques Solid chemical product
17、s in the formof particles varying from powders to coarse lumps3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1 particle densitydensity of an individual particle of powderNOTE When an enclosed space occurs inside the particle, the space is consid
18、ered to be part of the individual particle.3.2 pyknometrymethod of measuring particle density using a pyknometer4 Preparation of measurement4.1 SamplingA representative sample for analysis shall be taken in accordance with ISO 8213.Copyright International Organization for Standardization Reproduced
19、by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-ISO 18753:2004(E)2 ISO 2004 All rights reserved4.2 Drying of sampleThe selected sample is thoroughly dried in an air bath at approximately , and then cooled in a desiccatorto room temperatu
20、re. In the case of powders requiring a long drying time, the sample is thoroughly spread, andstirred lightly once or twice midway through the drying process.NOTE 1 When the material is not stable at the heating temperature, the sample should be dried under reduced pressureinstead of heating.NOTE 2 I
21、f necessary, it is recommended to record the mass loss as a function of time to ensure that the sample hasreached equilibrium. 4.3 Preparation of immersion liquidThe immersion liquid used for pyknometry shall not be reactive and shall not dissolve the sample. A liquid withgood wetting properties and
22、 a low evaporation rate under vacuum conditions shall be selected.The standard liquid for immersion shall be xylene, as specified in ISO 6353-3. When this liquid is not suitable,due to reaction or dissolution of the powders, distilled water, ethanol (e.g. purity by volume fraction) asspecified in IS
23、O 6353-2, or 1-butanol as specified in ISO 6353-3 may be used.The absolute density of the immersion liquid at the measured temperature shall be determined usingpyknometry, in accordance with ISO 758. Ethanol purity is not important. Content of ethanol is given as anexample.5 Apparatus5.1 Pyknometer,
24、 Gay-Lussac type made of glass, of capacity or (see Figure 1), as specified inISO 3507, or other suitable type of pyknometer.5.2 Vacuum container, having an integrated pyknometer with a structure wherein internal conditions of thepyknometer can be observed. The pyknometer shall be connected to a vac
25、uum pump, which is used to createthe vacuum conditions.Figure 1 Example of Gay-Lussac type pyknometer110C95 %25 ml 50 mlCopyright International Organization for Standardization Reproduced by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-I
26、SO 18753:2004(E) ISO 2004 All rights reserved 35.3 Vacuum pump, capable of obtaining a vacuum of ( ) or better.5.4 Vacuum gauge, capable of measuring from to ( to ).5.5 Balance, with a reciprocal sensitivity of .5.6 Thermometer, capable of reading to .6 ProcedureMeasurements shall be carried out acc
27、ording to the following procedure. All masses shall be measured to thenearest .a) Clean the pyknometer (5.1), thoroughly dry it, then measure the mass, .b) Transfer the powder sample to the pyknometer, filling the pyknometer to approximately one-third of itscapacity, and measure the mass, .c) Gently
28、 fill the pyknometer with immersion liquid until the powder sample is covered. It is permitted to slightlyexceed this level. When the immersion liquid is dispensed, care should be taken not to scatter the sample.d) Install the pyknometer containing the powder sample, immersed in liquid, in a vacuum
29、container (5.2),reduce pressure to ( ) or less, and implement the degassing procedure. Allow areduction of pressure to a level at which the immersion liquid cannot boil, and carry out the degassing untilbubbles cannot be generated from the sample.e) Remove the pyknometer from the vacuum container an
30、d allow it to stand until the temperature of the liquidfalls to room temperature. After thermal equilibrium is reached, record the temperature. The temperature ofthe sample/container shall be recorded and thermal equilibrium shall be reached before the mass isrecorded.f) Add the specific amount of i
31、mmersion liquid to the pyknometer, and measure the mass, .g) Remove the sample and the immersion liquid from the pyknometer. After washing and drying thepyknometer, fill with fresh immersion liquid to the specified level, and measure the mass, .h) Determine the absolute density of the immersion liqu
32、id at the measured temperature using pyknometry, inaccordance with ISO 758, and determine the absolute density of the immersion liquid to four places ofdecimals. Where distilled water is used as the immersion liquid, the absolute density for a giventemperature, listed in Table A.1, shall be used. Th
33、e permissible temperature difference for measurementstaken in steps f) to h) shall be within .7CalculationCalculate particle density by means of Equation (1) by using the values obtained from Clause 6. Foursignificant digits shall be obtained.(1)whereis the particle density in grams per cubic centim
34、etre;is the mass of the sample and the measuring container in grams;is the mass of the measuring container in grams;is the mass of the specific amount of immersion liquid and the measuring container in grams;666,5 Pa 5 mmHg0 kPa 26,66 kPa 0 mmHg 200 mmHg0,1 mg0,1C0,1 mgmp1mp213,33 kPa 100 mmHgmp3mp4
35、1C=(mp2mp1)(mp4mp1) (mp3mp2)Lmp2mp1mp4Copyright International Organization for Standardization Reproduced by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-ISO 18753:2004(E)4 ISO 2004 All rights reservedis the mass of the specific amount o
36、f sample, the immersion liquid and the measuring container ingrams;is the density of the immersion liquid at measuring temperature in grams per cubic centimetre.8 Tests in duplicateCarry out tests in duplicate on representative analysis samples. If the difference between the original andduplicate re
37、sults is greater than , repeat the procedure.9 Test reportThe test report shall contain the following information:a) date of the test;b) name of the testing establishment;c) reference to this International Standard, i.e. ISO 18753;d) description of the test material (manufacturer, type, batch or cod
38、e number);e) description of the sample pre-treatments (evacuation time and evacuator, heating temperature and period);f) pyknometer (type, capacity);g) description of the immersion liquid used and temperature of measurements;h) absolute density of the sample;i) comments concerning the test or test r
39、esults.mp3L0,03 g/cm3Copyright International Organization for Standardization Reproduced by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-ISO 18753:2004(E) ISO 2004 All rights reserved 5Annex A(normative)The reference data for absolute de
40、nsity of distilled waterTable A.1 indicates the absolute density of distilled water as a function of temperature between and1.Table A.1 Absolute density of distilled water as a functionof temperature between and Temperature Density15 0,999 116 0,999 017 0,998 818 0,998 619 0,998 420 0,998 221 0,998
41、022 0,997 823 0,997 624 0,997 325 0,997 126 0,996 827 0,996 528 0,996 329 0,996 030 0,995 715C30C15C30CC g/cm3Copyright International Organization for Standardization Reproduced by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-ISO 18753:2
42、004(E)6 ISO 2004 All rights reservedBibliography1 LANDOLT-BRNSTEIN, Zahlenwerte und Funktionen aus Physik, Chemie, Astronomie, Geophysik undTechnik, 6th Edition, II, Part 1, p. 36 (1971); IV, Part 1, p. 101 (1955), Springer-VerlagCopyright International Organization for Standardization Reproduced by
43、 IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-.7Copyright International Organization for Standardization Reproduced by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-ISO 18753:2004(E)ICS 81.060.30Price based on 6 pages ISO 2004 All rights reservedCopyright International Organization for Standardization Reproduced by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS-,-
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