BS EN 993-17-1999 Methods of test for dense shaped refractory products - Determination of bulk density of granular materials by the mercury method with vacuum《成形密实耐火制品的试验方法 真空汞法对颗粒.pdf

1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 993-17:1999 The Eur

2、opean Standard EN 993-17:1998 has the status of a British Standard ICS 81.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Methods of test for dense shaped refractory products Part 17: Determination of bulk density of granular materials by the mercury method with vacuumThis

3、 British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 May 1999 BSI 05-1999 ISBN 0 580 32321 8 BS EN 993-17:1999 Amendments issued since publication Amd.

4、 No. Date Text affected National foreword This British Standard is the English language version of EN 993-17:1998. It supersedes BS 1902-3.6:1984, which is withdrawn. The UK participation in its preparation was entrusted by Technical Committee RPI/1, Refractory products and materials, to Subcommitte

5、e RPI/1/1, Sampling and physical testing of refractory products, which has the responsibility to: aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related inte

6、rnational and European developments and promulgate them in the UK. A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be f

7、ound in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standa

8、rds are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 7, and a back cover.CEN European Committee for

9、 Standardization Comite Europe en de Normalisation Europa isches Komitee fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. 993-17:1998 E EUROPEAN STANDARD EN 993

10、-17 NORME EUROPE ENNE EUROPA ISCHE NORM December 1998 ICS Descriptors: refractory materials, shaped refractories, dense shaped refractory products, tests, determination, measurements, density (mass/volume), bulk density, granular materials, pycnometric analysis, mercury, procedures English version M

11、ethods of test for dense shaped refractory products Part 17: Determination of bulk density of granular materials by the mercury method with vacuum Me thodes dessai pour produits re fractaires faonne s denses Partie 17: De termination de la masse volumique apparente des mate riaux en grains par la me

12、 thode au mercure sous vide Pru fverfahren fu r dichte geformte feuerfeste Erzeugnisse Teil 17: Bestimmung der Rohdichte an ko rnigem Gut nach dem Quecksilber-Verdra ngungsverfahren unter Vakuum This European Standard was approved by CEN on 28 November 1998. CEN members are bound to comply with the

13、CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or

14、to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versio

15、ns. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.Page 2 EN 993-17:1998 BSI 05-1999 Foreword This European

16、 Standard has been prepared by Technical Committee CEN/TC 187, Refractory products and materials, the Secretariat of which is held by BSI. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by June 1999

17、, and conflicting national standards shall be withdrawn at the latest by June 1999. EN 993, Methods of test for dense shaped refractory products, consists of 18 parts: Part 1: Determination of bulk density, apparent porosity and true porosity; Part 2: Determination of true density; Part 3: Test meth

18、ods for carbon-containing refractories; Part 4: Determination of permeability to gases; Part 5: Determination of cold crushing strength; Part 6: Determination of modulus of rupture at ambient temperature; Part 7: Determination of modulus of rupture at elevated temperatures; Part 8: Determination of

19、refractoriness- under-load; Part 9: Determination of creep in compression; Part 10: Determination of permanent change in dimensions on heating; Part 11: Determination of resistance to thermal shock (ENV); Part 12: Determination of pyrometric cone equivalent (refractoriness); Part 13: Specification f

20、or pyrometric reference cones for laboratory use; Part 14: Determination of thermal conductivity by the hot-wire (cross-array) method; Part 15: Determination of thermal conductivity by the hot-wire (parallel) method; Part 16: Determination of resistance to sulfuric acids; Part 17: Determination of b

21、ulk density of granular materials by the mercury method with vacuum; Part 18: Determination of bulk density of granular materials by the water method with vacuum. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement

22、 this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Contents Page Foreword 2 1 Scope 3 2 Normative references 3 3 Definitions 3 4 P

23、rinciple 3 5 Apparatus 3 6 Test samples 3 7 Procedure 3 8 Calculation of results 6 9 Test report 7 Annex A (informative) Bibliography 7Page 3 EN 993-17:1998 BSI 05-1999 1 Scope This European Standard specifies the determination of the bulk density of granular refractory materials (grain bulk density

24、) having a grain size greater than 2 mm, by the mercury method with vacuum. NOTE 1 This method is intended as the reference method because of its reproducibility and simplicity in use. However, mercury is known to be a hazardous substance, and therefore the determination of bulk density of granular

25、materials can be carried out according to prEN 993-18. This standard, which defines a method by water with vacuum, is recommended for all routine purposes. Nevertheless, depending on the nature of the material tested, the two methods can give different results. NOTE 2 Under test conditions, applying

26、 a mercury pressure of 26,5 kPa, round pores with a diameter$ 55mm and elongated pores with a width$ 27,5mm are penetrated by mercury. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at

27、 the appropriate places in the text and the publications listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references, the latest edition of the

28、 publication referred to applies. ISO 383, Laboratory glassware Interchangeable conical ground joints. ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings. 3 Definitions For the purposes of this European Standard, the following definitions

29、apply. 3.1 bulk density of a granular material grain bulk density ratio of the mass of a quantity of the material to the total volume of its grains, including the volume of any closed pores within the grains 3.2 closed pores pores that are not penetrated under the conditions of this test when grains

30、 are immersed in mercury 4 Principle The measurement of the mass of a test sample previously crushed to the required grain size, and the determination of its volume by the mercury displacement method with vacuum below 3 000 Pa residual pressure and preferably with a residual pressure of 133 Pa. 5 Ap

31、paratus 5.1 Vacuum pycnometer. A vessel as shown in Figure 1 (incorporating conical ground glass joint in accordance with ISO 383). 5.2 Test arrangement, for filling and emptying the pycnometer under a vacuum. A suitable test arrangement is shown in Figure 2. 5.3 Vacuum pump, capable of reducing the

32、 pressure to a value of not more than 3 000 Pa. 5.4 Balance, with an accuracy of 0,1 g and a graduation of 0,01 g. 5.5 Desiccator. 5.6 Oven, capable of being controlled to 1108C 58C. 5.7 Sieves, with nominal aperture of 2 mm and 5,6 mm in accordance with ISO 565. 6 Test samples 6.1 Preparation of te

33、st samples The material to be tested shall consist of fractions or groups of fractions of grains. However, laboratory samples shall be produced from these fractions by sieving and comminution to obtain a grain size of between 2 mm and 5,6 mm. NOTE Any dust or loose particles adhering to the grains s

34、hould be removed before testing, by washing or, with materials sensitive to moisture or humidity, by air blowing. 6.2 Number of test samples Take at least three test samples from the laboratory sample and carry out one determination of bulk density on each test sample. 6.3 Mass of test samples The m

35、ass of the test samples depends on the grain size and homogeneity of the material being tested. A mass of 100 g is recommended. NOTE For inhomogeneous samples, the mass of the test sample may be increased to 200 g. Dry the test sample to constant mass in the drying oven maintained at 1108C 58C, and

36、allow it to cool to ambient temperature in the desiccator. Weigh the test sample to the nearest 0,1 g on the balance. This gives the mass, in grams, of the dried test sample (m P ). 7 Procedure 7.1 Measurement of ambient temperature The temperature at which the test is carried out shall be measured

37、before and after the series of sample determinations. NOTE Operational details of the test arrangement described below refer to Figure 2. 7.2 Determination of the volume of the test sample (V R ) 7.2.1 Determination of mass of empty vacuum pycnometer (m L ) Clean and dry the empty vacuum pycnometer

38、(see 5.1) and weigh it to the nearest 0,1 g. This gives the mass in grams of the empty pycnometer (m L ). NOTE This weighing can be omitted if all the determinations are carried out at a temperature which does not vary by more than 28C.Page 4 EN 993-17:1998 BSI 05-1999 Figure 1 Vacuum pycnometerPage

39、 5 EN 993-17:1998 BSI 05-1999 1 2 3 4 5 6 7 8 Dish for mercury Stopcock 2 Pycnometer lower part Glass seal with holes (diameter1mm) Stopcock 5 Pycnometer upper part Capillary and overflow tube Pycnometer vacuum connection 9 10 11 12 13 14 15 16 Vacuum tubing Mercury extraction bush Mercury reservoir

40、 Three-way tap Vacuum manometer Wolfs bottle (to collect any mercury accidentally carried over) Vacuum pump Stopcock Figure 2 Schematic representation of the test arrangement 7.2.2 Determination of mass of pycnometer filled with mercury (m G ) Fill the mercury dish (1) with sufficient mercury from t

41、he reservoir (11) to fill the pycnometer. With stopcock (2) closed and stopcock (5) and tap (12) open, evacuate the pycnometer to a residual pressure of below 3 000 Pa, as indicated by the manometer (13). Open stopcock (2) and allow the pycnometer to fill with mercury until mercury emerges from the

42、capillary tube (7). Close stopcocks (2) and (5) in that order and remove the pycnometer from the test arrangement. Pour off the surplus of mercury that has come out of the capillary tube, and remove the mercury remaining in the suction tube below stopcock (2) and in the capillary above stopcock (5)

43、using a steel wire. Weigh the pycnometer to the nearest 0,1 g. This gives the mass, in grams, of the pycnometer filled with mercury (m G ). NOTE If all the determinations are carried out at a temperature which does not vary by more than 28C, this weighing needs to be carried out only once per series

44、 of sample determinations. 7.2.3 Determination of mass of pycnometer containing test sample and filled with mercury (m T ) Empty and dry the pycnometer. NOTE 1 This can be achieved quickly by fitting the pycnometer to the mercury extraction bush (10) and evacuating the mercury reservoir (11). Transf

45、er the dried and weighed test sample (see 6.3), without loss, into the pycnometer. and fill the pycnometer, under vacuum, as specified in 7.2.2. This will give an average pressure on the grains of about 26,5 kPa. Remove the pycnometer from the test arrangement, again as specified in 7.2.2, and weigh

46、 the pycnometer and contents to the nearest 0,1 g. This gives the mass of the pycnometer containing the test sample and filled with mercury (m T ).Page 6 EN 993-17:1998 BSI 05-1999 Fit the pycnometer to the extraction bush (10), close stopcock (16) and evacuate the mercury reservoir (11). Open stopc

47、ock (2) and remove the mercury from the pycnometer while under a pressure not exceeding 3 000 Pa. Close stopcock (2), remove the pycnometer and, by gently shaking, remove any mercury adhering to the test sample. Open stopcock (5) and allow the pycnometer to return to atmospheric pressure. Remove the

48、 test sample from the pycnometer. Determine the amount of mercury remaining in the test sample, by weighing it and finding the difference from its original mass. If the mass of mercury remaining in the test sample is over 5 % of the original mass of the sample, this amount, expressed as a percentage

49、 by mass, shall be stated in the test report. NOTE 2 The stopcocks (2) and (5) should be closed in the order stated and while the pycnometer vessel is still connected to the vacuum system. Closing stopcock (5) after the apparatus has been disconnected from the vacuum system, or reopening stopcock (5) and thereby subjecting the contents to atmospheric pressure, will give an increased impregnation of the grain porosity with mercury and thus a high erroneous result. This situation