BSEN196-6-1992水泥的试验方法.细度的测定.pdf

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Methods of testing cement —

Part 6: Determination of fineness

BRITISH STANDARD

BS EN 196-6:1992

The European Standard EN 196-6:1989 has the status of a British Standard

NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW

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Cooperating organizations

The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national standards organizations of the following countries:

Austria Oesterreichisches Normungsinstitut

Belgium Institut belge de normalisation

Denmark Dansk Standardiseringsraad

Finland Suomen Standardisoimisliito, r.y.

France Association française de normalisation

Germany Deutsches Institut für Normung e.V.

Greece Hellenic Organization for Standardization

Iceland Technological Institute of Iceland

Ireland National Standards Authority of Ireland

Italy Ente Nazionale Italiano di Unificazione

Luxembourg Inspection du Travail et des Mines

Netherlands Nederlands Normalisatie-instituut

Norway Norges Standardiseringsforbund

Portugal Instituto Portuguès da Qualidade

Spain Asociación Española de Normalización y Certificación

Sweden Standardiseringskommissionen i Sverige

Switzerland Association suisse de normalisation

United KingdomBritish Standards Institution

This British Standard, having
been prepared under the
direction of the Technical
Sector Board for Building
and Civil Engineering, was
published under the
authority of the Standards
Board and comes into
effect on
15 June 1992

© BSI01-2000

The following BSI references relate to the work on this standard: Committee reference B/516 Draft for comment 86/14805 DC

ISBN 0 580 20670 X

Amendments issued since publication

Amd. No.DateComments

BS EN 196-6:1992

Contents

Page
Cooperating organizations Inside front cover
National foreword ii
Brief history 22
Foreword
Text of EN 196-6 3
National annex NA (informative) Material for checking
the sieve 10
National annex NB (informative) Method for testing
the “absolute” specific surface of a reference cement 10
National annex NC (informative) Method of testing cement
for density 15
National annex ND (informative) Reporting of results for
density and specific surface 17
National annex NE (informative) Committees responsible 17
National annex NF (informative) Cross-references Inside back cover

BS EN 196-6:1992

© BSI 01-2000

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National foreword

This British Standard has been prepared under the direction of the Technical Sector Board for Building and Civil Engineering. It is the English language version of EN 196-6:1989 “Methods of testing cement; Determination of fineness”, published by the European Committee for Standardization (CEN). EN 196-6 was drawn up by CEN Technical Committee 51, Cement and building limes, as Part 6 of a series on testing cement which was accepted by CEN

on 3 October 1989. The UK gave a negative vote at the final voting stage but, under the CEN Rules now in force, is bound to abide by the majority decision and to implement this Part. This British Standard supersedes BS 4550-3.2:1978 and Section 3.3:1978 which are withdrawn.

The European Standard specifies the use of a “reference material of known sieve residue” for checking the sieve in the sieving method (clause 3). National annex NA gives a suitable reference material for the UK.

The European Standard furthermore specifies the use of a “reference cement of known specific surface” for the determination of the “apparatus constant” in the air permeability method (Blaine method) (clause 4). National annex NB retains the principle of the procedure which was given in BS 4550-3.3:1978, but using a porosity of 0.500, for measuring the “absolute” specific surface of a possible, future reference cement, ideally sourced within Europe, for use with this European Standard as a replacement for the material at present available from the National Institute of Standards and Technology (formerly the National Bureau of Standards), USA.

The European Standard includes in 4.5.3 only the principle of the method of determination of density which is required for the air permeability methods. National annex NC therefore describes in full the procedure which was given in BS 4550-3.2:1978.

National annex ND indicates UK preferred methods for the reporting of the results.

National annex NE gives the committees responsible for the UK participation in the preparation of this standard.

National annex NF gives details of corresponding British Standards for International Standards referred to in the European Standard.

During preparation of EN 196-6 an error has occurred in 3.4.2. CEN have been informed and a corrigendum is in preparation which will give the following information.

“In 3.4.2, paragraph 1, line 1, delete “sample of cement” and substitute “reference material”.

In 3.4.2, paragraph 1, line 4, delete “cement” and substitute “material”.

A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards 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, pages i and ii, the EN title page, pages 2 to 18, an inside back cover and a back cover.

This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.

BS EN 196-6:1992

ii

© BSI 01-2000

UDC 666.94:691.54:620.1:539.215

Descriptors: Cement, determination, fineness, tests, sieving, air, permeability

English version

Methods of testing cement; Determination of fineness

Méthodes d’essai des ciments; Détermination de la finesse

Prüfverfahren für Zement; Bestimmung der Mahlfeinheit

This European Standard was approved by CEN on 1989-06-16. CEN members are bound to comply with the 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 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 versions.

CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.

CEN

European Committee for Standardization Comité Européen de Normalisation Europäisches Komitee für Normung

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM

EN 196-6

December 1989

Central Secretariat: rue de Stassart 36, B-1050 Brussels

© CEN 1989 Copyright reserved to all CEN members

Ref. No. EN 196-6:1989 E

Brief history

This European Standard was drawn up by the Technical Committee CEN/TC 51 “Cement" the Secretariat of which is held by IBN.

In accordance with the Common CEN/CENELEC Rules, the following countries are bound to implement this European Standard:

Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.

Foreword

The standard EN 196 on methods of testing cement consists of the following Parts:

— Part 1: Determination of strength;

— Part 2: Chemical analysis of cement;

— Part 3: Determination of setting time and soundness;

— Part 4: Quantitative determination of constituents;

— Part 5: Pozzolanicity test for pozzolanic cements;

— Part 6: Determination of fineness;

— Part 7: Methods of taking and preparing samples of cement;

— Part 21: Determination of the chloride, carbon dioxide and alkali content of cement

Contents

Page
Brief history 2233333334
Foreword
1 Object and field of application
2 References
3 Sieving method
3.1 Principle
3.2 Apparatus
3.3 Material for checking the sieve
3.4 Procedure
3.5 Expression of results
4 Air permeability method
(Blaine method) 444
4.1 Principle
4.2 Apparatus
4.3 Materials 6
4.4 Test conditions 6
4.5 Compacted cement bed 6
4.6 Air permeability test 7
4.7 Calibration of apparatus 7
4.8 Special cements 8
4.9 Simplification of the calculations 8
4.10 Expression of results 9
Figure 1 — Blaine permeability
apparatus 5
Figure NB.1 — Details of typical
permeability cell 11
Figure NB.2 — Typical permeability
apparatus with manometer and flowmeter 12
Table 1 — Density of mercury ρí, viscosity
of air η and√0,1nη as function of the
temperatures 9
Table NB.1 — Mass of cement (in g)
required to form a bed 25.00 mm in
diameter and 10.00 mm deep having a
porosity of 0.500, over density
range 2 500 kg/m³ to 3 290 kg/m³ 14
Table NB.2 — Mass of cement (in g)
required to form a bed 25.40 mm in
diameter and 10.00 mm deep having a
porosity of 0.500, over density
range 2 500 kg/m³ to 3 290 kg/m³ 14
Table NC.1 — Density of pure water, Pw 16

EN 196-6:1989

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© BSI 01-2000

1 Object and field of application

This European Standard describes two methods of determining the fineness of cement.

The sieving method serves only to demonstrate the presence of coarse cement particles. This method is primarily suited to checking and controlling the production process.

With the air permeability method (Blaine) the specific surface (mass related surface) is measured by comparison with a reference cement sample.The determination of the specific surface serves primarily to check the consistency of the grinding process of one and the same plant. This method only allows a limited assessment to be made of the properties of the cement in use.1)

The methods are applicable to all the cements defined in ENV 1972).

2 References

ENV 197, Cement: Composition, specifications and conformity criteria²).

ISO 383:1976, Laboratory glassware Interchangeable conical ground joints.

ISO 565:1983, Test sieves — Woven metal wire cloth, perforated plate and electroformed sheet —Nominal sizes of openings.

ISO 3310-1:1982, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth.

ISO 4803:1978, Laboratory glassware — Borosilicate glass tubing.

3 Sieving method

3.1 Principle

The fineness of cement is measured by sieving it on standard sieves. The proportion of cement of which the grain sizes are larger than the specified mesh size is thus determined.

A reference sample having a known proportion of material coarser than the specified mesh size is used for checking the specified sieve.

3.2 Apparatus

3.2.1 Test sieve, comprising a firm, durable, non-corrodible, cylindrical frame of 150 mm to 200 mm nominal diameter and 40 mm to 100 mm depth, fitted with 90 μm mesh sieve cloth of woven stainless steel, or other abrasion-resisting and non-corrodible metal wire.

The sieve cloth shall comply with the requirements ofTable 1 ofISO 565:1983 and ISO 3310-1 and shall be free of visible irregularities in mesh size when inspected optically by the methods of ISO 3310-1. A tray fitting beneath the sieve frame and a lid fitting above it shall be provided to avoid loss of material during sieving.

3.2.2 Balance, capable of weighing up to 10 g to the nearest 10 mg.

3.3 Material for checking the sieve

A reference material of known sieve residue shall be provided for checking the sieve.

The material shall be stored in sealed, airtight containers to avoid changes in its characteristics due to absorption or deposition from the atmosphere. The containers shall be marked with the sieve residue of the reference material.

3.4 Procedure

3.4.1 Determination of the cement residue

Agitate the sample of cement to be tested by shaking for 2 min in a stoppered jar to disperse agglomerates. Wait 2 min. Stir the resulting powder gently using a clean dry rod in order to distribute the fines throughout the cement.

Fit the tray under the sieve. Weigh approximately 10 g of cement to the nearest 0,01 g and place it in the sieve, being careful to avoid loss. Disperse any agglomerates. Fit the lid over the sieve. Agitate the sieve by swirling, planetary and linear movements until no more fine material passes through it. Remove and weigh the residue. Express its mass as a percentage, $R _ { 1 } ,$ of the quantity first placed in the sieve to the nearest 0,1 %. Gently brush all the fine material off the base of the sieve into the tray.

Repeat the whole procedure using a fresh 10 g sample to obtain $\bar { R } _ { 2 } .$ Then calculate the residue of the cement R as the mean of $\scriptstyle { R _ { 1 } }$ and $R _ { 2 }$ as a percentage, expressed to the nearest 0,1 %.

When the results differ by more than 1 % absolute, carry out a third sieving and calculate the mean of the three values.

The sieving process is carried out manually by a skilled and experienced operator.

NOTE Alternatively a sieving machine may be used provided that it can be shown to give the same results as the manual operation.

EN 196-6:1989

  1. The air permeability method may not give significant results for cements containing ultrafine materials. 2) At present at the draft stage.

© BSI 01-2000

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3.4.2 Checking the sieve

Agitate the sample of cement to be tested by shaking for 2 min in a stoppered jar to disperse agglomerates. Wait 2 min. Stir the resulting powder gently using a clean dry rod in order to distribute the fines throughout the cement.

Fit the tray under the sieve. Weigh approximately 10 g of the reference material (3.3) to the nearest 0,01 g and place it in the sieve, being careful to avoid loss. Carry out the sieving procedure as in 3.4.1 including the repeat determination of residue to yield two values $P _ { 1 }$ and $P _ { 2 }$ expressed to the nearest 0,1 %.

The two values of $P _ { 1 }$ and $P _ { 2 }$ for a satisfactory sieve should differ by not more than 0,3 %. Their mean P characterizes the state of the sieve.

Given the known residue on the 90 μm mesh of the reference material, $\scriptstyle R _ { 0 } ,$ calculate $R _ { 0 } / P$ as the sieve factor, $F ,$ expressed to the nearest 0,01. The residue, R, determined as in 3.4.1 shall be corrected by multiplying by F, which may have a value of $1 { , } 0 0 \pm 0 { , } 2 0$

Check the sieve after every 100 sievings.

NOTE Any other checking procedure, such as the optical methods described in ISO 3310-1 may be used. All sieves will wear slowly and consequently their sieve factor, F, will slowly change.

3.5 Expression of results

Report the value of R, to the nearest 0,1 %, as the residue on the 90 μm (ISO 565) sieve for the cement tested.

The standard deviation of the repeatability is about 0,2 % and of the reproducibility is about 0,3 %.

NOTE Where there is local difficulty in obtaining ISO sieves, the same procedure can be followed with the nearest available standard sieve but the report is to state on which standard sieve mesh the cement residue has been determined.

4 Air permeability method (Blaine method)

4.1 Principle

The fineness of cement is measured as specific surface by observing the time taken for a fixed quantity of air to flow through a compacted cement bed of specified dimensions and porosity. Under standardized conditions the specific surface of cement is proportional to √t where t is the time for a given quantity of air to flow through the compacted cement bed. The number and size range of individual pores in the specified bed are determined by the cement particle size distribution which also determines the time for the specified air flow.

The method is comparative rather than absolute and therefore a reference sample of known specific surface is required for calibration of the apparatus.

4.2 Apparatus

4.2.1 Permeability cell. The cell shall be a rigid right cylinder of the dimensions and tolerances shown in Figure 1 a). It shall be of austenitic stainless steel or other abrasion-resisting, non-corrodible material. The top and bottom faces shall be flat and normal to the axis of the cylinder, as shall the upper surface of the ledge at the bottom of the cell. The outer surface of the cylinder shall be tapered to form an airtight fit with the conical socket of the manometer (IS0 383, Joint 19/34).

4.2.2 Perforated disc. The disc shall be of non-corrodible metal, perforated with 30 to 40 holes of 1 mm diameter, and shall have the dimensions and tolerances shown in Figure 1 b). When in position on the ledge in the cell, its plane surfaces shall be normal to the axis of the cell.

4.2.3 Plunger. The plunger is a piston, capable of sliding freely in the measuring cell by means of a clearance to be applied in such a way that, when the cap of the plunger comes to rest on the upper face of the cell cylinder, a distance of 15 ± 1 mm will be maintained between the upper face ofthe perforated disc and the lower face of the piston.

This piston shall be provided with a flat connected to an annulus around the head to enable air to escape.

The plunger shall be of austenitic stainless steel or other abrasion-resisting and non-corrodible material; it shall have the dimensions and tolerances shown in Figure 1 c). A plunger can only be used with the corresponding cell the dimensions of which match within the permitted tolerances.

4.2.4 Manometer. The manometer shall be a rigidly and vertically mounted U-tube of borosilicate glass tubing (ISO 4803) arranged as in Figure 1 d) and having the dimensions and tolerances shown in this figure.

One arm of the manometer shall be provided at the top with a conical socket (ISO 383, Joint 19/34) to form an airtight fit with the conical surface of the cell. The same arm shall also have four etched lines and a T-joint whose positions shall have the dimensions and tolerances shown in Figure 1 d). The side branch of the T-joint shall lead to an airtight stopcock beyond which shall be attached a suitable aspiration device such as the rubber tube and bulb shown in Figure 1 d).

Fill the manometer tube with the liquid (4.2.5) to wet the inner surface. Empty the tube and refill it so that the manometer liquid is level with the lowest etched line [11 in Figure 1 d)]. This manometer liquid shall be changed (or cleaned) after servicing or before a new calibration.

EN 196-6:1989

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© BSI 01-2000

NOTE Other forms of cell and plunger and other arrangements of the joint between cell and manometer may be used provided that they can be shown to give the same results as the specified apparatus.

(c) Plunger All dimensions in millimetres.)

ItemDescription
1Piston
2Flat for air vent
3Cell
4Compacted cement disc
5Filter paper disc
6Perforated disc
7Manometer
8,9,10, 11Etched lines
12Conical joint for cell
13Stopcock
14Rubber type
15Aspirator bulb

4.2.5 Manometer liquid. The manometer shall be filled to the level of the lowest etched line [11 in Figure 1 d)] with a non-volatile, non-hygroscopic liquid of low viscosity and density, such as dibutyl phthalate or light mineral oil.

(d) Manometer Figure 1 — Blaine permeability apparatus)

Recommended mmObligatory mm
A ≤ 50 $\scriptstyle B = 1 3 5$ $\boxed { G = 1 2 , 7 \pm 0 , 1 }$
$c = 2 7 5$ $\pm \nobreakspace 1 0 \nobreakspace$ $\pmb { { \cal E } } / = \mathbf { G } - 0 , 1$
D= 23 $\pm ~ 2 5$ $\pm \_ { 1 }$
J = $5 0 \quad \pm 1 5 \quad$ $H = 1 5 \quad \pm 1$
K=
$0 , 8 \ \pm \ 0 { , } 2$
L = $\begin{array} { r l } { 0 , 9 ~ \pm ~ } & { { } 0 , 1 } \end{array}$
$\scriptstyle \left| M = \right|$ $9 , 0 ~ \pm ~ 0 { , } 4$

EN 196-6:1989

© BSI 01-2000

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4.2.6 Timer, having a positive starting and stopping mechanism, readable to 0,2 s or better, and accurate to 1 % or better over time intervals up to 300 s.

4.2.7 Balance(s), capable of weighing about 3 g to the nearest 1 mg (for the cement) and about 50 g to 110 g to the nearest 10 mg (for the mercury).

4.2.8 Pyknometer, or other convenient means of determining the density of cement.

4.3 Materials

4.3.1 Mercury, of reagent grade or better.

4.3.2 Reference cement³), of known specific surface.

4.3.3 Light oil, to prevent formation of mercury amalgam on the inner surface of the cell.

4.3.4 Circular discs of filter paper, having a smooth circumference adapted to the dimensions of the cell. The filter paper is of medium porosity (mean pore diameter 7 μm).

4.3.5 Light grease, for ensuring an airtight joint between cell and manometer, and in the stopcock.

4.4 Test conditions

The laboratory in which the air permeability test is carried out shall be maintained at a temperature of $2 0 \pm 2 { } ^ { \circ } \mathrm { C }$ and a relative humidity not exceeding 65 %. All materials for test and calibration shall be at the laboratory temperature when used and shall be protected from absorption of atmospheric moisture during storage.

4.5 Compacted cement bed

4.5.1 Basis

The compacted cement bed comprises a reproducible arrangement of cement particles with a specified volume of air included between the particles. This air volume is defined as a fraction of the total volume of the bed and is termed the porosity, e.

It follows that the volume fraction occupied by the cement particles is (1 – e). If Vis the total volume of the bed, the absolute volume of cement is V(1 – e) in cm³, and the mass of cement, m is ρV(1 – e) in g where ρ is the solid density of the cement particles in g/cm³.

Thus, knowing ρ, a mass of cement can be weighed to produce a desired porosity, e, in the compacted bed of total volume V. The determination of ρ is described in 4.5.3 and that of Vin 4.7.1.

4.5.2 Preparation of the sample

Agitate the sample of cement to be tested by shaking for 2 min in a stoppered jar to disperse agglomerates. Wait 2 min. Stir the resulting powder gently using a clean dry rod in order to distribute the fines throughout the cement.

4.5.3 Determination of density

Determine the density of the cement using a device such as a pyknometer (4.2.8). Use a non-reactive liquid in the determination. The quantity of cement used will depend on the nature of the apparatus but shall be such that the value of ρ determined is accurate to 0,01 g/cm³. Verify this accuracy by a repeat determination and record the mean of the two determinations to the nearest 0,01 $\mathbf { g } / \mathbf { c m } ^ { 3 }$ as the density.

4.5.4 Formation of the bed

To give a cement bed of porosity e = 0,500 weigh a quantity of cement, $m _ { 1 } ,$ calculated from

$$ m _ { 1 } = \ 0 , 5 0 0 \rho V ( \mathbf { g } )\tag{1} $$

where

ρ is the density of the cement (g/cm³) (4.5.3);

V is the volume of the cement bed (cm³) (4.7.1).

This mass, correctly compacted, will produce a bed of porosity 0,500. Place the perforated disc (4.2.2) on the ledge at the bottom of the cell (4.2.1) and place on it a new filter paper disc (4.3.4). Ensure that the filter paper disc fully covers the perforated disc and is flat by pressing with a clean dry rod. Place the weighed quantity of cement, m,, in the cell taking care to avoid loss. Tap the cell to level the cement. Place a second new filter paper disc on the levelled cement. Insert the plunger (4.2.3) to make contact with the filter paper disc. Press the plunger gently but firmly until the lower face of the cap is in contact with the cell. Slowly withdraw the plunger about 5 mm, rotate it through 90° and gently but firmly press the bed once again until the plunger cap is in contact with the cell. The bed is now compacted and ready for the permeability test. Slowly withdraw the plunger.

NOTE Too rapid and vigorous pressing may change the particle size distribution and therefore change the specific surface of the bed. The maximum pressure should be that comfortably exerted by a thumb on the plunger.

EN 196-6:1989

  1. At present reference cements are available from:

National Bureau of Standards, Office of Standard Reference Materials, Chemistry Building, Washington DC, 20234, USA

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