PROCEDURE:

1. SAMPLING
1.1. WEIGHT OF SAMPLE
- The sample, whether grab or composite, should weigh at least 5 kg (10 lb)
1.2. EQUIPMENT
- The sampling instrument shall be clean and dry when used.
- The sample containers shall be of such a size that they are almost completely filled by
the sample.
- The sample containers shall he sealed airtight after filling and marked with full
particulars of the material and the date of sampling.
1.3. METHOD OF SAMPLING
Take samples by any of the applicable methods:
1.3.1. SAMPLING FROM A CONVEYOR TO BULK STORAGE
- Take one grab sample in a receptacle at 6 hours intervals when the cement is
discharge from the conveyor into the bulk storage,
1.3.2. TRANSFER SAMPLING
- During transfer between storage bins take one grab sample for every 360 Mg (400
tons) of cement. Make sure to take at least two grab samples to be combined into a
composite sample.
1.3.3. OPTIONAL METHODS
- Samples may be taken by one of the following methods, depending upon the
approval of the purchaser, when neither of the mentioned sampling methods above
is not applicable.
1.3.3.1. SAMPLING FROM BULK STORAGE AT POINTS OF DISCHARGE
- If authorized by the purchaser, cement in storage may be sampled at the
discharge openings of the bin. The steps usually followed are to:
a) Take samples from the discharge openings in a steady stream.
b) Estimate the quantity of cement in Mg to be withdrawn from one
discharge opening as 0.055 d 3 x 0.2, where d is the depth in
meters of cement above the discharge opening.
c) Samples shall be taken at such intervals so that at least two grab
samples shall be secured for each 360 Mg (400 tons) in the bin or
silo.
- If a high circular silo is being sampled, take all samples from one opening.
- If a low rectangular bins are being sampled and the quantity of cement in
the bin exceeds 1100 Mg (1200 tons) when, discharge openings employed
in the sampling shall be such that for no opening shall the number of
samples represent more than one half the contents of the bin or more than
1800 Mg (2000 tons).
1.3.3.2. SAMPLING FROM BULK STORAGE AND BULK SHIPMENT BY
MEANS OF A SLOTTED TUBE SAMPLER
- When the depth of the cement to be sampled does not exceed 2.1 m (7 ft),
obtain samples using a slotted tube sampler similar to that shown in Fig. 1

FIG. 1 Slotted Tube Sampler for Bulk Cement.

- Take samples from well-distributed points and various depths of the

cement so that the samples taken will represent the cement involved.
1.3.3.3. SAMPLING FROM BAGS OR PACKAGES
- Insert the sampler, shown in Fig. 2, diagonally into the valve of the bag and place
the thumb over the air hole.
 FIG. 2 Tube Sampler for Packaged Cement

- Withdraw the sampler.

- Take one sample from a bag in each 4.5 Mg (5 tons) or fraction thereof.
1.3.3.4. SAMPLING FROM BULK SHIPMENT OF RAIL CAR OR TRUCK
1.3.3.4.1. SINGLE SHIPMENT (only one car/truck is being loaded)
- If the loading is continuous and all from the same source, take 5
kg (10 lb) sample
- If the loading is not continuous or unknown, combine two or
more portions from different point in the load to form the test
samples.
1.3.3.4.2. MULTIPLE SHIPMENTS (several cars/trucks are being
loaded)
- Sample the shipment at the rate of one sample for each 90 Mg
(100 tons) of cement or fraction thereof. Note that not less than
two samples should be taken.
- Consider cement represented by the samples as a lot.
- Test the samples in accordance with the procedure specified.
2. PREPARATION OF SAMPLES FOR TESTING
- As soon as the sample has been obtained, it shall be carefully homogenized.
- Pass each sample through an 850-µm (No. 20) sieve,6 or any other sieve having
approximately the same size openings, in order to mix the sample, break up lumps, and
remove foreign material.
- The reduction and homogenization of the sample shall be continued until the quantity of the
cement required for the testing sample is obtained.
3. STORAGE
- Store the samples in a moisture-proof multiple-wall and airtight containers strong enough to
avoid breakage, and if they can be sealed immediately after filling in such a manner as to
eliminate excess air in the sample in order to avoid moisture absorption and aeration.
- If placed in cans, it must be filled completely and be immediately seal after.
- Take note that polyvinyl chloride sample containers, upon occasion, have been found to affect
the air-entraining potential of a cement sample. The same problem might be experienced with
containers made from other plastics.
- If the testing is to be done at the reduced rate (refer to 4.2), mix the drawn markers and draw
two to select the numbers of the samples to be tested.
4. TESTING
4.1. ESTABLISHING QUALITY HISTORY AND CONTROL CHART
4.1.1. QUALITY HISTORY
- Prepare available test results not less than 40 test samples covering at least seven
lots of cement.
 - Make pairs of consecutive test results such as two test samples from the same lot
but not individual test results from different lots.
- Several pairs from the same lot may be used where available but if desired so, it
may be reduced as follows:
a) Select a subgroup by some random method from the consecutively numbered
group of tested samples representing the entire lot.
b) List the numbers identifying the subgroup in numerical sequence, and pair in
the order of listing.
4.1.2. CRITICAL LIMIT AND CONTROL CHART OF THE RANGE
- Compute the average range for each included physical and chemical property
limited by specification requirements as follows:
Range(R)=The difference between the test results of a pair
The ∑ of ranges
Average range (ṝ )=
Total number of ranges
- Calculate the critical limit, “C”, for each included physical and chemical property
limited by a specification requirement as follows:
d=2.49 ṝ
C=specification limit – d, if the requirement has maximum specification limit
C=specification limit + d, if the requirement has minimum specification limit
- Obtain the upper control limit for the range between each consecutive pair of the
test results as follows:
upper control limit=3.267 ṝ
- Record all the calculations and make a control chart of the range wherein the
horizontal scale of the chart will be successive groups of two, and the vertical scale
of the chart will be the range.
- Critical limit may need to be recalculated if any of the following conditions applies:
a) The range chart indicates lack of control (points beyond the upper control limit.
b) The occurrence of two consecutive points beyond the upper control limit for the
range, or the occurrence of three consecutive points beyond the upper control
limit in any series of five consecutive points.
4.2. METHOD OF TESTING
- The purchaser shall specify the amount of testing when heat of hydration, alkali reactivity,
and sulfate resistance are required. All other required tests shall be made on selected
samples depending on the applicable testing method as shown in Table 1.

4.2.1. NORMAL TESTING

- Test and obtain the number of tests under the normal testing rate as shown in Table
1 if the following conditions are present:
a) Before the quality history has been established.
b) When no samples from a particular mill have been tested within a year.
c) When the quality history is based entirely on data more than two years old.
 d) When it is deemed necessary to recalculate the critical limit because of
indicated lack of control as shown by the control chart of the range.
4.2.2. REDUCED TESTING
- Test and obtain the number tests under the reduced testing rate as shown in Table 1
if the quality history has been already established
- If the results of these tests, indicated in the quality history, are within the critical
range, make additional tests (total equal to the number of tests at the normal rate as
shown in Table 1).
- However, take note that if the additional test would result into the delay in completion
of testing, it is desirable to test under the normal testing rate rather than the reduced
testing rate.
4.3. SELECTION OF SAMPLES FOR TESTING
Take samples to be tested from each lot by the method with accordance to the test to be
done.
4.3.1. NORMAL RATE
- Place a group of consecutively numbered markers equal to the number of samples
in a container and mix.
- Draw one marker at a time from the container until the number drawn is equal to the
number of samples to be tested at the normal rate.
4.3.2. REDUCED RATE
- Mix the drawn markers and draw two to select the numbers of the samples to be
tested.
4.4. TESTING-TIME REQUIREMENTS FOR THE COMPLETION OF TESTS
The testing laboratory shall provide test results not later than the indicated number of days
after sampling:

4.5. REPORTING
The cement shall be reported by indicating the following information:
4.5.1. NORMAL RATE
a) Complying with the specification requirements – if the specification requirements
are reached
b) Failing to meet the specification requirements – if at least one specification
requirement is not attained during the tests. Include in the report which
specifications it failed and its corresponding applicable limit.
4.5.2. REDUCED RATE
a) Complying with the specification requirements – if the average of the test results
is further from the specified limit than the critical limit. If the average of the results
for one or more requirements are between the critical limit and the specification
limit, test additional samples (total equal to the number of tests at the normal rate)
for that requirement
 b) Failing to meet the specification requirements – if at least one of the average test
result does not meet its respective requirement. Include in the report which
specifications it failed and its corresponding applicable limit.
4.6. NONCOMPLIANCE AND RETEST
- Any test result that fails to meet the specification requirements must be retested to confirm
noncompliance before being reported.
- Retests shall be conducted in accordance with the provisions, if given, of the applicable
specification. If no provisions are given, the following procedure shall be used:
a) Make the retest on a portion of the same sample as the initial test. Use referee
methods whenever they are provided for determination of the property requiring
retest and in such case use only the results obtained by referee methods.
b) The retest shall consist of the same number of determinations required for the initial
test, or, if a within laboratory precision statement is given which is based on a
specified number of replicates (that is, duplicate or triplicate determinations), the
number of replicates used as the basis of such precision statement.
c) If two or more determinations are required, the value reported shall be the average of
all results that are within the limits of precision of the method at the 95 % confidence
level, as stated in the applicable specification or as generally recognized.
TERMINOLOGY:
Blended hydraulic cement – a cement composed of one of five classes of hydraulic cement for
general and special applications, using slag, fly ash or other Pozzolan with Portland cement, or
Portland cement clinker with slag.
Bulk Storage – referred to a place where equipment and supplies in large quantities are stored
Composite Sample – the quantity of cement obtained by mixing together equal quantities of cement
from each of the laboratory samples representing the subgroup into which the lot has been divided.
Control chart – is a graph used to study how a process changes over time. Data are plotted in time
order. A control chart always has a central line for the average, an upper line for the upper control
limit, and a lower line for the lower control limit. These lines are determined from historical data
Conveyor – a device for moving materials; usually a continuous belt, an articulated system of
buckets, a confined screw, or a pipe through which material is moved by air or water.
Critical Limit – represents the boundaries that are used to ensure that an operation produces safe
products.
Expansive hydraulic cement – a hydraulic cement that forms a paste when mixed with water, and
increases in volume a controlled amount during the early hardening period occurring after setting.
Grab sample – the quantity of cement taken by combining together all the sample from the same
subgroup of a lot.
Hydraulic cement – a finely ground material which on addition of requisite quantity of water is
capable of hardening both under water and in air by the chemical interaction of its constituents with
water, and is also capable of binding together appropriate materials.
Lot – the quantity of cement considered as a unit from the same manufacturing unit and offered for
inspection at one time or the contents of one or more transport containers drawn from one or more
bins of material from a single production run, sequentially packaged from one or more bins, or a
group of samples secured from one of the above.
Masonry cement – a hydraulic cement manufactured for use in mortars for masonry construction or
in plasters, or both, which contains a plasticizing material and, possibly, other performance-enhancing
addition(s).
Mortar cement - a hydraulic cement manufactured for use in masonry mortar designed for specific
bond and air content criteria.
Plastic stucco cement - a hydraulic cement used in plaster or stucco–a hydraulic cement plaster
containing fine aggregate, used for coating exterior surfaces.
Polyvinyl chloride – a synthetic resin prepared by the polymerization of vinyl chloride, used in the
manufacture of nonmetallic water stops for concrete.
Portland cement – a hydraulic cement produced by pulverizing Portland-cement clinker, and usually
containing calcium sulfate.
Quality history – historical data which represent the cement from the same source as the cement to
be tested and based on data not more than 2 years old.
Retest – considered to be an additional test of the failed property. A retest may be a single
determination or a set of replicate determinations.
Sample – a quantity of cement taken at random or in accordance with a sampling plan, from a larger
quantity (silo, trucks, bags, etc.) or from a fixed lot, relating to the intended tests.
Silo – a structure used for storing bulk amount of cement.
Slotted Tube sampler – an equipment ideal for taking a large volume, cross sectional sample from a
container. It ranges between 1.5 and 1.8 m (5 and 6 ft) long and approximately 35 mm (13⁄8 in.) in
outside diameter and consist of two polished brass telescopic tubes with registering slots that are
opened or closed by rotation of the inner tube, the outer tube being provided with a sharp point to
facilitate penetration.
Subgroup – the quantity of cement in each of the parts into which a lot is divided for the purpose of
sampling.
Testing sample – the quantity of cement obtained by reducing the grab sample by following a
specified procedure for laboratory testing.