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BRITISH STANDARD BS EN
196-7:1992
Methods of testing
cement —
Part 7: Methods of taking and preparing
samples of cement
Cooperating organizations
Contents
Page
Cooperating organizations Inside front cover
National foreword ii
Brief history 2
Foreword 2
Text of EN 196-7 3
National annex NA (informative) BS EN 196-7 sampling report 15
National annex NB (informative) Sampling for acceptance inspection
at delivery 16
National annex NC (informative) Committees responsible 16
National annex ND (informative) Cross-references 17
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 196-7:1989 “Methods of testing cement; Methods of taking and
preparing samples of cement”, published by the European Committee for
Standardization (CEN). EN 196-7 was drawn up by Technical Committee 51,
Cement and building limes, as Part 7 of a series on testing cement which was
accepted by CEN on 3 October 1989. The UK gave a positive vote at the final
voting stage and, thus, the European test procedure has been introduced into
the 1991 revisions of British Standards for cement BS 12, BS 146, BS 4027,
BS 4246, BS 6588 and BS 6610. This British Standard supersedes BS 4550-1
which is withdrawn.
The European Standard includes important definitions relating to the various
types of samples associated with the assessment of the quality of cements and
provides details of how these samples are required to be taken.
The European Standard also covers the preparation and storage of laboratory
samples for subsequent testing. Representative samples for the various tests
which may be required are obtained by means of a sample divider or by
quartering.
A suitable form for the sampling report specified in clause 10 is given in national
annex NA.
Since the draft European Prestandard for cement, ENV 197-1, does not deal with
acceptance inspection at delivery, EN 196-7 does not specify the relationship
between sample size/type and the size of the lot sampled. In consequence national
annex NB retains the UK conditions relating to acceptance inspection.
National annex NC gives the committees responsible for the UK participation in
the preparation of this standard.
National annex ND gives details of corresponding British Standards for
international standards referred to in the European Standard.
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.
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Summary of pages
This document comprises a front cover, an inside front cover, pages i and ii,
the EN title page, pages 2 to 16, 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.
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UDC 666.94:691.54:620.11
English version
Méthodes d’essais des ciments; Méthodes de Prüfverfahren für Zement; Verfahren für die
prélèvement et d’échantillonnage du ciment Probenahme und Probenauswahl von Zement
CEN
European Committee for Standardization
Comité Européen de Normalisation
Europäisches Komitee für Normung
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Germany, Greece, Iceland, Ireland, Italy, 4 General 4
Luxembourg, Netherlands, Norway, Portugal, 5 Sampling equipment 4
Spain, Sweden, Switzerland and United Kingdom.
6 Procedures for taking samples and
Foreword precautions to be taken depending on the
procedures adopted 5
The standard EN 196 on methods of testing cement 7 Frequency at which samples are taken and
consists of the following Parts: choice of sample type 5
— Part 1: Determination of strength; 8 Size and preparation of samples 5
— Part 2: Chemical analysis of cement; 9 Packaging and storage 7
— Part 3: Determination of setting time and 10 Sampling report 7
soundness; Annex A Typical examples of sampling
— Part 4: Quantitative determination of equipment normally used 9
constituents; Figure 1 — Make up of laboratory samples 8
— Part 5: Pozzolanicity test for pozzolanic Figure 2 — Sampling tube 9
cements;
Figure 3 — Typical ladle 10
— Part 6: Determination of fineness;
Figure 4 — Typical mechanical screw sampler
— Part 7: Methods of taking and preparing (overall length approximately 200 cm) 11
samples of cement;
Figure 5 — Typical permanently installed
— Part 21: Determination of the chloride, carbon mechanical screw sampler 12
dioxide and alkali content of cement.
Figure 6 — Sampling equipment 13
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1)
The requirements of this standard can also, by agreement between the parties, be followed for acceptance inspections for all
non-standardized hydraulic binders.
2)
At present at the draft stage.
3
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3)
However, cleaning is not necessary between the taking of successive increments from the same cement which are intended for
making up the sample.
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6.2 Sampling from bags, drums and containers present at the sampling operation. The necessary
of comparable size quantity prescribed in the second paragraph of 8.1
shall then be collected in a clean and dry container.
When the cement is packed in bags, drums or other
small containers, the sample indicated in the second 6.7 Sampling from bag filling machines
paragraph of 8.1 shall comprise either a single bag The quantity taken shall comprise a bag of cement
or a single container chosen at random from a obtained during the normal operation of the
sufficiently large stock. machine. It can equally comprise the equivalent
6.3 Sampling from large containers quantity (see the second paragraph of 8.1) sampled
by a mechanical device fitted in the supply hopper
Samples shall be taken while the container is being
directly above the discharge spouts. If the machine
filled or emptied taking the precautions:
is used for packing different cements, it shall be
a) not to operate in dusty or polluting completely purged of all the cement previously
atmospheres; packed until the cement from which samples are to
b) to take the number of samples necessary to be taken arrives. Depending on the type of packing
obtain the quantity prescribed in the second machine, the quantity so removed may be
paragraph of 8.1; considerable. The manufacturer’s representative
c) to transfer the collected cement into a clean, present at the sampling operation shall determine
dry and airtight container before proceeding with this quantity.
the operations described in clause 8.
7 Frequency at which samples are
6.4 Sampling from bulk transport
taken and choice of sample type
(after loading or before unloading)4)
For all equipment used, care shall be taken not to The frequency of taking samples and the type of
sample (spot sample or composite sample) depends
take material from the top or bottom layers of the
on the provisions contained:
mass of cement. The thickness of the layer to be
considered is at least 15 cm. — in the agreements between producer and
customer;
Take the same precautions as those described
in 6.3a), b) and c). — in the national, European (ENV 1975) for
example) or even international standards;
6.5 Sampling while loading into bulk
transport or silos — in the certification procedures.
Taking samples may be carried out only if suitable 8 Size and preparation of samples
equipment is available and if there is access to a
homogeneous phase of cement. Take the same 8.1 Size of sample to be taken for verification
precautions as those described in 6.3a), b) and c). of compliance
Each laboratory sample (or sample for retest or
retained sample) shall be of such a size that all the
tests specified in the contract or required by
standards indicated in the contract or the
certification procedure can be carried out twice.
Thus, unless specified to the contrary, the mass of
these samples shall be at least 5 kg (or more, if
necessary, to fill completely the container indicated
in 9.2).
4)
The equipment described in this standard (see annex A) does not allow for sample(s) to be taken during unloading.
5)
At present at the draft stage.
The total quantity (spot sample or composite Homogenization shall be considered to be obtained
sample) to be taken for verifying compliance shall be if the analysis of variance shows there to be no
greater than or at least equal to that required for significant differences between
supplying to all the laboratories concerned the the 15 micro-samples. This analysis shall be carried
samples indicated in the first paragraph above. This out as described in the literature dealing with
quantity shall be taken by the equipment specified statistical control7).
in clause 5 and in accordance with the procedures In the case of an unsatisfactory result, the mixing
stated in clause 6. In general taking a sample shall be repeated, but doubling the time of the
of 40 kg to 50 kg will suffice. mixing operation.
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8.2 Homogenization If, after this second trial, there are no significant
8.2.1 General requirements differences between the 15 micro-samples, the
method with twice the homogenization time shall be
As soon as the quantity of 40 kg to 50 kg indicated
considered valid, but, if no noticeable improvement
in the second paragraph of 8.1 has been collected, it
has been obtained in relation to the first trial, the
shall be carefully homogenized (preferably in a
chosen method shall be declared unsuitable.
laboratory) with clean dry implements not liable to
Finally, if there is no decisive improvement, it shall
react with the cement.
be decided, in view of the time required, whether it
The homogenization shall preferably be achieved is worth repeating the trial with a longer time.
using a mixing machine, the efficiency of which
shall have been previously demonstrated (see 8.2.2). 8.2.3 Choice of method
Whatever procedure is chosen, it shall be carried out The verification of the efficiency of the
as quickly as possible to minimize the exposure of homogenizing method (see 8.2.2) is only to be
the cement to the air. carried out at the time of choosing the method. This
In the absence of a homogenizer, the following choice is left to the initiative of the manufacturer,
procedure is to be adopted: but he shall be in a position to prove (for example to
an expert representing a customer or the
the quantity of cement to be distributed between certification body) that he has carried out the trial
the laboratories (see the second paragraph described above by presenting a dossier drawn up on
of 8.1) shall be tipped onto a clean dry cloth that occasion.
(or plastics sheet) and shall then be mixed
carefully using a shovel. 8.3 Division of the quantity necessary for
verification of compliance
This procedure shall only be used if:
a) the ambient relative humidity is less After homogenization (see 8.2) of the sample made
up as specified in the second paragraph of 8.1, it
than 85 %;
shall be divided into the required number of
b) all risk of the sample being affected by wind, laboratory or retained samples either by using a
rain, snow or dust is avoided. sample divider or, after quartering the quantity to
8.2.2 Verification of the efficiency of the be distributed, by extracting with a hand scoop
homogenizing procedure selected increments of approximately 0,5 kg from each of the
Take approximately equal quantities of two cements quarters and transferring these successively into
of differing characteristics (i.e. Blaine fineness, by containers prepared for receiving the laboratory
EN 196-6, and additionally colour). Mix these using (or retained) samples. This operation shall be
one of the procedures described in 8.2.1 and note the continued until the desired mass (stated in the first
time between starting and finishing the operation. paragraph of 8.1) is obtained in each container.
Once the operation is judged to be complete, take The sequence of distributing the contents of the
fifteen “micro-samples”, each of 12 g to 20 g, from hand scoop from which each laboratory sample is
points equally distributed within the mass of which gradually made up shall be as follows.
the homogeneity is to be verified6).
Determine the Blaine fineness three times on each
of these micro-samples.
6) To
obtain initial information, the colour of these micro-samples can be compared if care has previously been taken to select two
cements of distinctly different colour.
7)
For UK purposes, a suitable method can be found in “Statistical methods in research and production” eds O.L. Davies and
P.L. Goldsmith, 1972, Oliver and Boyd, Edinburgh.
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Distribute successively to each of the laboratory To prevent aeration the containers shall as far as
containers X, Y, Z, etc. possible, be completely filled and their closure
first a scoopful from A, sealed with adhesive tape9).
then a scoopful from B, When made of plastics, containers or bags shall only
be used under the following conditions:
then a scoopful from C,
a) the period of storage shall be limited
then a scoopful from D.
to 3 months;
This represents one distribution sequence; repeat
b) the sheet from which they are made shall be at
the same sequence as many times as necessary to
least 100 µm thick;
reach the quantity prescribed in the first paragraph
of 8.1 (see Figure 1). c) the plastics material shall under no
circumstances cause the cement to become “air
Each laboratory (or retained) sample so prepared
entraining” whether by loss from this material or
shall be packaged as stated in clause 9 and
as a result of surface treatment. On this point,
despatched with the minimum delay. It is then up to
check for the absence of risk by carrying out
the receiving laboratory, to store, prepare and treat
appropriate tests where needed;
the sample in a manner appropriate to its
subsequent use.8) d) provision shall also be made to seal them
where necessary, by using suitable tape.
8.4 Foreign bodies in the sample
9.3 Storage condition
During the above operations any foreign bodies
which may appear shall, in all cases, be noted in the The samples shall preferably be stored at a
sampling report (clause 10). temperature of less than 30 °C.
If they appear to be uniformly distributed in the 9.4 Identification of samples
cement (for example, a powder other than cement, In order to identify the samples unambiguously, the
lumps) it is not possible to remove them from the containers (bags or drums) shall be clearly and
sample. Otherwise, they shall be removed and kept: indelibly marked in at least one place. When there
a) by one of the two parties (manufacturer, is only one mark, this shall be on the body of the
container and not on the lid.
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8)
At this point the work of the laboratory is usually specified in the test standards. (Principally EN 196-1 to EN 196-6 and
EN 196-21.)
9)
It has to be remembered, however, that the packaging, however air-tight, cannot in the long term prevent a certain amount of
aeration, the extent of which may vary depending on the properties of the product.
10)
At present at the draft stage.
11)
In the possible case of non-standardized binders (see note 1 on page 3) the product should be given an unequivocal mark.
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Annex A (informative)
Typical examples of sampling
equipment normally used
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Figure 4 — Typical mechanical screw sampler (overall length approximately 200 cm)
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12) In preparation.
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