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1.

Introduction
Concrete is the most important building material for various type of structure due to its structural
stability and strength. With nearly 420 million tonnes (MT) of cement production capacity, India
is the second largest cement producer in the world and accounts for 6.9 per cent of world’s cement
output. The cement production capacity is estimated to touch 550 MT by FY 20. [1]
Global cement production is expected to increase from 3.27 billion metric tons in 2010 to 4.83
billion metric tons in 2030. Also the average amount of energy needed to create 1 gram of Portland
cement is at least 1700 J. [2] The energy needed for cement is obtained from coal. World demand
for cement is projected to rise 4.5% per year to 5.2 billion metric tons in 2019. To meet this
growing demand, a partial replacement for cement can be introduced in concrete.
Human activities on the earth produces solid waste in considerable quantities of over 3500/MT per
year, including industrial wastes, agricultural waste and wastes from rural and urban societies.
Recent technological development has shown that these materials are valuable as inorganic and
organic resources. The use of agricultural waste product in India is an environment friendly
method of disposal of large quantities of materials. The agricultural residual products which
possess pozzolanic properties are rice husk ash, saw dust ash, waste burn clay, corn cob ash.
The agricultural residual product under this study is Wheat Husk Ash (WHA). Wheat milling
generates a byproduct known as husk. This surrounds the wheat grains. During the milling of
paddy about 78% of weight is received as wheat. The rest 22% of the weight of wheat is received
as husk. Wheat production is about 70 million tonnes per year in India and counts for
approximately 12 per cent of world production. Wheat straw is produced about 33-48 tons per acre
and crop to residue ratio is 1:1.
The waste has generally no commercial value and is locally available at a low transportation cost.
The use of Waste has traditional material in construction and hence provides practical and
economic advantages. The proper utilization of these wastes conserves the natural resources and
protects the environment. Rice husk ash and wheat straw ash (WSA) are some of the alternative
pozzolanas in the agricultural countries that were investigated recently and showed promising
capabilities.

Hasan Biricik et.al. had shown that wheat straw ash possesses pozzolanic activity. It contains
considerable amounts of silica and lime, and hence has a potential as a pozzolanic material. Due
to the pozzolonic nature of wheat husk ash, it can be used as partial replacement for cement. We
are doing study on influence of WSA on the durability of concrete.
2. LITERATURE REVIEW
2.1 Effect of wheat straw ash on mechanical properties of autoclaved mortar
Nabil M. Al-Akhras

This study investigates the effect of wheat straw ash (WSA) on the mechanical strength of
autoclaved mortar. The mechanical properties studied include compressive, tensile, and flexural
strengths of mortar. Mortar mixes were prepared using natural silica, wadi (local sand), and
crushed limestone fine aggregates at a w/c ratio of 0.6. Mortar specimens were exposed to
autoclave for 2.5 hrs at a pressure of 2 MPa. Three percentages of WSA replacement levels
(3.6%, 7.3%, and 10.9%) by weight of sand were utilized in the study. The specific gravity and
the absorption of the fine aggregates were determined according to ASTM C128. The gradation
and fineness moduli of the aggregate were determined according to ASTM C136. The mortar
was mixed in a 4730-cm 3 mixing bowl according to ASTM C305 standards. Flow table tests
were performed according to ASTM C230. The presence of silica in WSA is essential for the
pozzolanic reaction to occur and consequently to increase the strength of concrete. The study
showed that the replacement of sand by WSA increases the mechanical strength of autoclaved
mortar. Mortar specimen with 10.9% WSA replacement level showed an average increase in
compressive, tensile, and flexural strength by 87%, 67%, and 71%, respectively, compared to
control mortar specimens. SEM for autoclaved paste specimens containing 7.3% WSA
replacement revealed more hydration products (calcium silicate hydrate) compared to
control paste specimens.

2.2 Durability of wheat straw ash concrete to alkali-silica Reaction


Nabil M. Al-Akhras

This study investigated the effect of wheat straw ash on the durability of concrete to detrimental
alkali-silica reaction. Three wheat straw ash levels were considered in the study: 5, 10 and 15%
as a partial replacement of cement. The other experimental parameters investigated in the study
were: w/b ratio (0.5 and 0.6) and initial curing type (moist and autoclaving). The alkali-silica
Reaction deterioration was assessed by measuring the expansion of concrete prisms and the
reduction in compressive strength. The test specimens used in the study were prisms (7cm X 7cm
X 30cm) and cubes (10cm). The prismatic specimens were used to measure the ASR expansion
and the cubic specimens were used to measure the effect of ASR on compressive strength. Two
techniques of initial curing of concrete specimens were used in the study namely: (1) moist
curing involves immersing the concrete specimens in lime-saturated water for 90 days; and
(2) autoclave curing involves exposing the concrete specimens to high pressure steam
curing1day after demoulding using an autoclave machine for 2 h at a pressure of 2 MPa.
Two techniques were used to measure the expansion in concrete prisms due to ASR
deterioration:
1. embedded-type electrical strain gauges for the initially moist-cured concrete specimens.
2. The second technique utilised a mechanical dial strain gauge to measure the expansion for the
initially autoclaved concrete specimens.
The concrete mixtures were prepared using a tilting drum mixer of 0.04 m3 capacity according to
ASTM C192-02 (ASTM, 2002. The workability of WSA concrete was measured using the slump
test according to ASTM C143-03 (ASTM, 2003). The compressive strength reduction
(SR) was determined using the following equation: SR= (Scon -SASR)/ Scon
The ASR durability of WSA concrete to ASR deterioration increased with increasing the WSA
content from 5 to 15%. The results of studies shows 1. The durability of WSA concrete to ASR
damage increased with increasing the WSA replacement level from 5 to 15%.
2. The wheat straw ash concrete with w/b ratio of 0.5 showed higher durability to alkali-silica
reaction damage in comparison with wheat straw ash concrete with w/b ratio of 0.6.
3. The autoclaved wheat straw ash concrete showed generally similar performance to alkali-silica
reaction deterioration compared to the moist-cured wheat straw ash concrete.

2.3 Durability of wheat straw ash concrete exposed to freeze–thaw damage


Nabil M. Al-Akhras phd
This study was to investigate the influence of WSA on the durability of concrete to accelerated
cycles of FT deterioration under different experimental parameters including: WSA replacement
level (0, 5, 10 and 15%), aggregate type (basalt and pumice), water to cement ratio (0.5 and 0.7)
and maximum aggregate size (9.5 and 19 mm). The durability of WSA concrete to FT damage
was observed to be higher than that of plain concrete (without WSA replacement) and the
durability increased as the WSA replacement level was increased from 5 to 15%. Plain concrete
showed little durability to FT deterioration. The durability factor of WSA concrete increased
with increasing WSA replacement level from 15% for the plain concrete to 83% for the 15%
WSA concrete. The behaviour of increasing durability of WSA concrete to FT deterioration in
comparison with that of plain concrete may be attributed to the pozzolanic reaction and filler
action effect of WSA in the concrete mixtures which increased the durability of WSA concrete to
FT deterioration. The WSA concrete containing pumice aggregate showed higher durability to
FT deterioration in comparison with WSA concrete containing basalt aggregate. The WSA
concrete with w/b ratio of 0.5 showed greater durability to FT deterioration than WSA concrete
with a w/b ratio of 0.7. The WSA concrete with maximum aggregate size of 9.5 mm showed
greater durability to FT deterioration than WSA concrete with a maximum aggregate size of 19
mm.

2.4 Study of pozzolanic properties of wheat straw ash


Hasan Biricika, Fevziye AkoÈza, Fikret TuÈrkerb, Ilhan Berktaya

The experimental work consisted of determining wheat straw properties, such as preburning stage,
ash formation grinding, and pozzolanic properties. After the physical, morphological, and
chemical properties were defined, optimum burning temperature and time were determined in
order to obtain the ash with pozzolanic character. Physical and chemical properties of the ashes
were studied. Ashes were mixed with cement and lime according to the standards specified.
Experimental results showed that wheat straw has 8.6% ash and the silica content of the ash is
73%, both ashes burned at 570 and 6700 C have pozzolanic properties, the pozzolanic properties
obtained at 6700 C are higher than those obtained at 5700 C.
2.5 Resistance to magnesium sulfate and sodium sulfate attack of mortars
containing wheat straw ash
Hasan Biricika,*, Fevziye AkoÈza, Fikret TuÈrkerb, Ilhan Berktaya

The experimental study was carried out on mortar specimens. An ordinary PC and siliceous sand,
according to RILEM guidelines, were used for the PC mortars. WSA was used as a partially
replacing material of PC for the PC-WSA mortars.The test results showed that WSA replacement
affected beneficially compressive strength of mortars in sodium sulfate solution at 10,000 and
40,000 mg/ l. If we consider flexural strength results, performance of PC-WSA mortars is
comparatively less efficient than the PC mortar. Mortars containing WSA up to 24% of the
cement by mass generally gained compressive and flexural strengths in magnesium sulfate
solutions of 10,000 and 40,000 mg/ l during the 180 days of immersion. Mortar mixture
containing 8% WSA showed highest mass increase in water and magnesium sulfate solutions. At
higher replacement levels, mass increase was lower and decrease could be observed after 140
days in concentration of 40,000 mg/ l. Strength decrease after 56 days and mass decrease at later
days in solution at concentration of 40,000 mg/ l at the 24% replacement level can be accepted as
an indication of a negative development at later days.

2.6 Effect of Corncob, Wheat Straw, and Plane Leaf Ashes as Mineral Admixtures
on Concrete Durability
Hanifi Binici, Faruk Yucegok, Orhan Aksogan and Hasan Kaplan

In this study, the effects of the use of corncob, wheat straw, and plane leaf ashes CA, WSA, and
PLA as mineral admixtures on concrete durability were investigated. The control mixes were
modified with 2, 4, and 6% of CA, WSA, and PLA in place of fine aggregate. To establish the
durability of concrete, the compressive strengths were measured after 7, 28, 90, 180 days, and 18
months under sodium sulfate solution. In the meantime, abrasion resistance and water
penetration were investigated. The water penetration test was performed according to EN TS
10967. Sulfate solution was determined according to ASTM 1012. There was increase of
compressive strength with increasing percentages of ash additions. Specimen CA3 had the
highest compressive strength at 365 days. CA, WSA, and PLA concretes had higher potential
sulfate resistance compared to the control specimens. The CA3 specimen, in particular, had the
highest sulfate resistance among all the specimens. Specimens with CA as fine aggregate showed
greater abrasion resistance than the C(control concrete), WSA or PLA specimens. The depth of
water penetration into the CA3 specimen was considerably less than for other specimens. An
increase in the percentage of ash additives from 2 to 6% reduced water penetration significantly.
Water penetration was reduced with an increase in the CA, WSA, and PLA percentage.
Furthermore, the use of the additives resulted in excellent durability, with positive effects on
concrete formation.
3. OBJECTIVE :
1. To form idea of significance and importance of consumption of agricultural waste
material for the casting of sustainable design mix concrete for the construction.
2. To utilize locally available material and also reduce the cost of casting of design mix
concrete.
3. To prepare high strength concrete, eco-friendly and cost effective to the construction.
4. To find optimum percentage of WSA as cement replacement in concrete and mortar.
5. To investigates the Durability studies of design mix concrete with Wheat husk ash to that
of normal concrete.

4) EXPERIMENTAL METHODOLOGY:
The wheat straw ash was collected from different farms nearby. From the studies of pozzolanic
properties of wheat straw ash done previously, it is concluded that the pozzolanic activity and
when it is burnt openly and then controlled burn at 600ºC -800 ºC
Hence, the same ash to be adopted. The materials required for mortar are as follows:
Cement
Sand
WSA

Sampling Procedure:

Cement is to be replaced by WHA with 10%, 15% and 25% respectively. The cubes and bars to
be casted of different sizes and will be used for durability studies of cement mortar.
The durability studies include:
I) PHYSICAL TESTS
1) Density
2) Fineness
4) Soundness
5) Air-entrainment of mortar
6) SAI
7) Compressive strength
8) Water requirement

II) Chemical tests


1) Moisture Content
2) Loss on ignition
3) Available alkali

III) Rate of Water Absorption


IV) Sulphate attack
V) Chloride diffusion
VI) Water Sorption
VII) Accelerated Chloride Penetration

I) PHYSICAL TESTS

1)DENSITY
Determine the density of the sample in accordance with the procedure described in Test Method
C188 or Test Method C604 as modified below. For Test Method C188, follow the procedure
except use a quantity of fly ash or natural pozzolan weighed to the nearest 0.05 g, of about 50 g.
For Test Method C604 use an amount of material that is appropriate for the instrument.
Determine the density of the material as received.

2) FINENESS, AMOUNT RETAINED WHEN WET-SIEVED ON


A45-µm (NO. 325) SIEVE
1)Determine the amount of the sample retained when wet-sieved on a 45-µm (No. 325) sieve, in
accordance with Test Method C430, with the following exceptions.
Calibrate the 45-µm (No. 325) sieve using a cement standard (SRM 114). Calculate the sieve
correction factors as follows:

CF = std - obs
where:
CF = the sieve correction factor, %, (include a negative sign when appropriate),
std = the certified residue value for the SRM, %, and
obs = the observed residue value for the SRM, %
2) Calculate the fineness of the fly ash or natural pozzolan to the nearest 0.1 % as follows:

RC =RS + CF
where:
RC = corrected sieve residue, %,
RS = observed residue for the test sample, %, and
CF = the sieve correction factor, %.
If the residue retained for the test sample is equal to zero (RS = 0), then the sieve correction
factor shall not be added to the test result to calculate the corrected sieve residue. In such cases,
the corrected fineness shall be reported as zero.

3) SOUNDNESS
Conduct the soundness test in accordance with Test Method C151, except that the specimens
shall be moulded from a paste composed of 25 parts by mass of fly ash or natural pozzolan and
100 parts by mass of a Portland cement conforming to Specification C150.

4) AIR-ENTRAINMENT OF MORTAR

1)Using Portland cement conforming to the requirements for Type I or Type II of Specification
C150, prepare a test mixture in accordance with Test Method C185, using the following
proportions:

Test Mix
Portland cement, g 300
Fly ash or natural 75
pozzola
20-30 Standard sand, 1125
g
Water ,ml, sufficient Y
to give a flow of 80
to 95
Neutralised Vinsol Z
Resin solution, ml,
sufficient to produce
an air content of 18 ±
3%

2) The neutralized Vinsol resin solution used in this section on Air-Entrainment of Mortar shall
be either a commercial neutralized Vinsol resin solution or a neutralized Vinsol resin solution
prepared in accordance with Specification C226. If it is necessary to dilute either of these
solutions, use distilled or demineralized water.
3) Prepare two test mixtures with sufficient neutralized Vinsol resin to produce an air content of
15 to 18 % in the first mix and 18 to 21 % in the second mix. Then, determine by interpolation
the amount of Vinsol resin, expressed as mass percent of the cement, required to produce an air
content of 18 %.
4) Calculate the air content of the test mixtures as follows:
Air content, volume % = 100[1- (Wa/W c)]
Wa = W/400
Wc =(300+1125+75+(300*P*.01))/[(300/3.15)+(1125/2.65)+(75/D)+(300*P*.01)]

where:
Wa= actual mass per unit of volume of mortar as determined by Test Method C185, g/mL,
W = mass of the specified 400 mL of mortar (see Test Method C185), g,
Wc= theoretical mass per unit of volume, calculated on an air-free basis and using the values for
density and
quantities of the materials in the mix, g/mL,
P = percentage of mixing water plus Vinsol resin solution based on mass of cement, and
D = density of fly ash or natural pozzolan in the mixture, Mg/m3

5) STRENGTH ACTIVITY INDEX WITH PORTLAND CEMENT

Mould the specimens from a control mixture and from a test mixture in accordance with Test
Method C109/C109M. The Portland cement used in the Strength Activity Index test shall comply
with the requirements of Specification C150 and with the alkali and strength limits given in the
section on Materials. In the test mixture, replace 20 % of the mass of the amount of cement used
in the control mixture by the same mass of the test sample. Make six-cube batches as follows:

Control Mixture:
500g of Portland cement
1375g of graded standard sand
242 ml of water

Test Mixture:
400g of portland cement
100g of test sample
1375g of graded standard sand
Ml of water required for flow ± 5 of control mixture

6) COMPRESSIVE STRENGTH TEST

Determine the compressive strength, as specified in Test Method C109/C109M, of three specimens
of the control mixture and three specimens of the test mixture at ages of 7 days, or 28 days, or
both, depending upon how many specimens were molded as prescribed in the section on Number
of Specimens.

Calculation:
Calculate the strength activity index with portlandcement as follows:
Strength activity index with portland cement =(A/B) × 100 (11)
where:
A = average compressive strength of test mixture cubes, MPa (psi), and
B = average compressive strength of control mix cubes, MPa (psi)
7) WATER REQUIREMENT

Calculation
Calculate the water requirement for the Strength Activity Index with Portland Cement as
follows:
Water requirement, percentage of control = (Y/242 × 100)
where:
Y = water required for the test mixture to be 65 of control flow

II) CHEMICAL ANALYSIS:


1)MOISTURE CONTENT
Dry a weighed sample, as received, to constant mass in an oven at 110 6 5 °C [230 6 10 °F].
Calculate the percentage of moisture to the nearest 0.1 %, as follows:
Moisture content, % = (A/B)*100
where:
A = mass loss during drying, and
B = mass as received.

2) LOSS ON IGNITION
Portland Blast-Furnace Slag Cement and Slag Cement (Alternative Test Method):
This test method covers a correction for the gain in weight due to oxidation of sulphides usually
present in such cement by determining the decrease in the sulphide sulphur content during
ignition.
1)Weigh 1 g of cement in a tared platinum crucible, cover and ignite in a muffle furnace at a
temperature of 950 ± 50°C for 15 min. Cool to room temperature in a desiccator and weigh.
After weighing carefully transfer the ignited material to a 500 mL boiling flask. Break up any
lumps in the ignited cement with the flattened end of a glass rod.
2)Determine the sulphide sulphur content of the ignited sample using the procedure described in
ASTM C114 17.2.1 through 17.2.5.
3)Using the same procedure, also determine the sulphide sulphur content of a portion of the cement
that has not been ignited.
4)Calculate the percentage loss of weight occurring during ignition and add 0.8 times the
difference between the percentages of SO3 in the ignited sample and the original cement. Report
the corrected percentage, rounded in accordance with ASTM C114 Table 3, as loss on ignition.
3) AVAILABLE ALKALI
1) Weigh 5.0 g of the sample and 2.0 g of hydrated lime on a piece of weighing paper, carefully
mix using a metal spatula, and transfer to a small plastic vial of approximately 25-mL capacity.
Add 10.0 mL of water to this mixture, seal the vial by securing the cap or lid to the vial with
tape, blend by shaking until the mixture is uniform, and store at 38±2 °C.
2) Open the vial at the age of 28 days and transfer the contents to a 250-mL casserole. Break up
and grind the cake with a pestle, adding a small amount of water, if necessary, so that a uniform
slurry containing no lumps is obtained. Add sufficient water to make the total volume 200-mL.
Let stand 1 h at room temperature with frequent stirring. Filter through a medium-textured filter
paper onto a 500-mL volumetric flask. Wash thoroughly with hot water (eight to ten times).
3) Neutralize the filtrate with dilute HCl (1 + 3), using 1 to 2 drops of phenolphthalein solution as
the indicator. Add exactly 5 mL of dilute HCl (1 + 3) in excess. Cool the solution to room
temperature and fill the flask to the mark with distilled water. Determine the amount of sodium
and potassium oxides in the solution using the flame photometric procedure, described in Test
Methods ASTM C114, except that the standard solutions shall be made up to contain 8 mL of
calcium chloride (CaCl2) stock solution per litre of standard solution, and the solution as prepared
shall be used in place of the solution of cement.

III) Standard Test Method for Measurement of Rate of Absorption of Water


by Hydraulic- Cement Concretes
1. Obtain the specimen from molded cylinder as per Practices C31/C31M or C192/C192M
or drilled cores according to Test Method C42/C42M.
2. Saturate the specimens in accordance with the vacuum-saturation procedure in Test
Method C1202
3. Measure the mass of each test specimen to the nearest 0.01 g.
4. Place test specimens in the environmental chamber at a temperature of 50 +/- 2°C and
RH of 80 +/- 3 % for 3 days. Alternatively, place test specimens in a desiccator inside an
oven at a temperature of 50 +/- 2°C for 3 days.
5. After the 3 days, place each specimen inside a sealable container. Use a separate
container for each specimen.
6. Store the container at 23 +/- 2°C for at least 15 days before the start of the absorption
procedure.
7. Remove the specimen from the storage container and record the mass of the conditioned
specimen to the nearest 0.01 g before sealing of side surfaces.
8. Measure at least four diameters of the specimen at the surface to be exposed to water.
Measure the diameters to the nearest 0.1 mm and calculate the average diameter to the
nearest 0.1 mm.
9. Seal the side surface of each specimen with a suitable sealing material. Seal the end of
the specimen that will not be exposed to water using a loosely attached plastic sheet. The
plastic sheet can be secured using an elastic band or other equivalent system.
10. Use the procedure below to determine water absorption as a function of time. Conduct
the absorption procedure at 23 +/- 2°C with tap water conditioned to the same
temperature.
11. Measure the mass of the sealed specimen to the nearest 0.01 g and record it as the initial
mass for water absorption calculations.
12. Place the support device at the bottom of the pan and fill the pan with tap water so that
the water level is 1 to 3 mm above the top of the support device. Maintain the water level
1 to 3 mm above the top of the support device for the duration of the tests.
13. Start the timing device and immediately place the test surface of the specimen on the
support device. Record the time and date of initial contact with water.
14. Record the mass at the intervals (60s, 5min, 10min, 20min, 30min, 60min, every hour up
to 6 h, once a day up to 3 days, day 4 to 7 3 measurements 24 h apart, day 7 to 9 1 (one)
measurement) after first contact with water.
15. For each mass determination, remove the test specimen from the pan, stop the timing
device if the contact time is less than 10 min, and blot off any surface water with a
dampened paper towel or cloth. After blotting to remove excess water, invert the
specimen so that the wet surface does not come in contact with the balance pan (to avoid
having to dry the balance pan). Within 15 s of removal from the pan, measure the mass to
the nearest 0.01 g. Immediately replace the specimen on the support device and restart the
timing device.
16. The absorption is calculated as the change in mass divided by the product of the cross-
sectional area of the test specimen and the density of water.

I=mt/a*d
where:
I = the absorption,
mt = the change in specimen mass in grams, at the time t,
a = the exposed area of the specimen, in mm2, and
d = the density of the water in g/mm3.

IV) Standard Test Method for Potential Expansion of Portland-Cement


Mortars Exposed to Sulphate
Procedure:

1. Make six 25 by 25 by 285-mm [or 1 by 1 by 111⁄4-in.] test specimens, three from each of
two batches, for each cement.
2. In routine tests, 25 by 25 by 160-mm [or 1 by 1 by 61⁄4-in.] specimens may be used, but
in case of dispute, results obtained with 25 by 25 by 285-mm [or 1 by 1 by 111⁄4-in.]
specimens govern.
3. Prepare the moulds in accordance with Practice C490.
4. Use 400 g (cement plus gypsum) and 1100 g of sand for each batch. Use 194 mL of
mixing water for all non-air entraining Portland cements, and 184 mL of mixing water for
all air-entraining Portland cements.
5. Mix the mortar according to the procedure for mixing mortars of Practice C305, except
after placing the mixing water in the bowl, add the gypsum and mix at the slow speed for
15s, then stop the mixer, add the cement, and continue as prescribed in Practice C305.
6. Moulding Test Specimens: Immediately upon completion of the flow test, return the
mortar to the bowl, scrape down into the batch any mortar on the side of the bowl, and
remix at the medium speed (285±10r/min) for 15 s. Remove the paddle and the bowl
from the mixer and shake the excess mortar from the paddle into the bowl. Fill the mould
in two layers, each layer being compacted with the tamper. Work the mortar into the
corners, and along the surfaces of the mould with the tamper until a homogeneous
specimen is obtained. After the top layer has been compacted, cut the mortar off flush
with the top of the mould and smooth the surface with a few strokes of the trowel.
7. Storage of Test Specimens:
Initial Storage—Cure the specimens in the moulds in the moist closet at 23 ±2 °C [73.5
±3.5 °F] for 22 to 23 h. Then remove them from the moulds, properly identify, and place
in water at 23 ±2 °C [73.5 ±3.5 °F] for at least 30 min prior to making the initial length
measurement. Subsequent Storage—After the bars have been removed from the moulds
and measured, store them horizontally in water at 23 ±2 °C [73.5 ±3.5 °F]. Store the
specimens with at least 6-mm [1⁄4-in.] clearance on all sides except for the necessary
supports. Cover the specimens with at least 13 mm [1⁄2 in.] of water. Use a volume of
water that does not exceed 5 times the volume of the bars to prevent excessive leaching.
Replenish the water with fresh water every 7 days for the first 28 days and every 28 days
thereafter.
8. Measure the specimens for length by means of the length comparator. Remove them from
the water storage, one at a time, and wipe with a damp cloth before measuring. 11.2
Make the first reading at the age of 24 h ±15 min from the time the cement and water are
mixed together. Measure the specimen again at the age of 14 days.

Calculation:
Calculate the difference in length of the specimen at 24h and at 14 days to the nearest 0.001 % of
the effective gage length and report as the expansion of the specimen at that period. All
specimens remaining after 14 days must comprise a set having at least three specimens with a
permissible range depending on the number of the remaining specimens, as follows:
No. of Specimens Maximum Permissible Range, %
3 0.010
4 0.011
5 0.012
6 0.012
V) Standard Test Method for Determining the Apparent Chloride
Diffusion Coefficient of Cementitious Mixtures by Bulk Diffusion

1. Test Specimens
1. Drilled cores, moulded cylinders, or moulded cubes are acceptable test specimens. One
sample consists of at least two test specimens representative of the cementitious mixture
under test. Specimens must be free of defects such as voids or cracks visible to the
unaided eye. The minimum dimension across the finished surface of each test specimen
must be at least 75 mm, but not less than three times the nominal maximum aggregate
particle size. The specimen depth must be at least 75 mm. Unless otherwise specified,
provide 28 days of laboratory standard moist curing in accordance with Practice
C31/C31M or C192/C192M prior to sample preparation for immersion in the exposure
liquid.
2. Describe any variance from standard curing practice in the report.
3. For drilled cores obtained according to Test Method C42/C42M, prepare the test
specimen by cutting off the outermost 75 mm of the core. The test specimen thus
obtained has one face that is the original finished surface, and the other face that is a
sawn surface.
4. For specimens prepared in accordance with Practice C31/C31M or C192/C192M, the test
specimen is prepared by cutting parallel to the finished surface. The top 75 mm is used as
the test specimen.
5. From the remainder of the drilled core, or moulded specimen, cut a slice that is at least
20-mm thick. Use this slice to determine the initial chloride-ion content, Ci either by
crushing the entire slice or by grinding off a layer at least 2-mm thick. Alternately, if the
profile from the diffusion test specimen is ground deep enough such that the last 2
successive layers taken have chloride contents within 0.01 % by mass of concrete of each
other, it is permitted to extrapolate the best-fit equation of the chloride profile to obtain
the initial chloride-ion content, Ci.
6. Rinse the specimens with tap water immediately after cutting. Scrub the surface with a
stiff nylon brush, and rinse again. Prior to sealing specimen surfaces, air dry until no
moisture can be removed from the surface with a dry paper towel.
7. Exposure specimens must be surface-dry but internally moist prior to sealing. This
condition is satisfied by standard moist-cured specimens allowed to air dry for no more
than 24 h in laboratory air maintained at 23 ± 2 °C and 50 ±3 % RH.
8. Seal all sides of the exposure specimen except for the finished surface following the
procedure described in Test Method C1202.
9. Determine the initial mass of the test specimen when the coating has hardened.
10. Immerse the test specimen in the saturated calcium hydroxide water bath at 23±2°C in a
tightly closed plastic container. The container must be filled to the top to prevent
carbonation. After 24 h of immersion, remove the specimen, blot the surface dry with a
paper towel, and determine the mass of the specimen in the surface-dry condition.
11. The test specimen is immersed in a saturated calcium hydroxide water bath until the mass
does not change by more than 0.1 % in 24 h. An acceptable alternative procedure is to
vacuum saturate the specimens with saturated calcium hydroxide solution using a
vacuum chamber similar to the system described in Test Method C1202.
12. Exposure: Remove the saturated test specimen from the calcium hydroxide water bath,
immediately rinse the specimen surface with tap water, place the specimen in the
exposure container, fill the container with the exposure liquid, and then seal the
container. Place the container in a temperature-controlled chamber or room maintained at
23±2°C. Record the start date and start time to the nearest hour.
13. It is permitted to place multiple specimens in a single container as long as the specimens
are placed in the container such that the entire exposure surface is unobstructed. Maintain
the exposed surface area to exposure liquid volume ratio within the range of 50±30
cm2/L
14. The specimens must remain in the exposure liquid for at least 35 days.
15. Record the exposure time to the nearest hour.
16. Profile Grinding: Remove the test specimen from the exposure liquid, rinse with tap
water, and dry for at least 24 h in laboratory air maintained at 23±2°C and 50±3 % RH.
When grinding is to be performed longer than 48 h after removal from the exposure
solution, store the specimens in watertight resealable polyethylene bags until time of
grinding. When grinding is to be performed longer than 7 days after removal from the
exposure solution, store the bagged specimens in a freezer maintained at -15 °C (65 °C)
until time of grinding. Obtain the powder samples by grinding off material in layers’
parallel to the exposed surface. Unless the coating is removed by sawing or by using a
chisel, do not grind closer than 5 mm from the edge of the specimen to avoid edge effects
and disturbances from the coating. For the minimum exposure time of 35 days, grind off
at least eight layers in accordance with exposure times, select depth increments such that
a minimum of 6 points span the range from 1 mm below the exposed surface to a depth
with a chloride-ion content equal to, or slightly greater than, the initial chloride-ion
content.
17. The following alternate profiling procedure is permitted if the exposure time is sufficient
to allow chloride penetration deeper than 40 mm. Slice the test specimen parallel to the
exposure surface using a water-cooled diamond saw in 5- to 6- mm increments,
minimizing the time specimens are exposed to water. Dry the slices for 24 h in laboratory
air, then crush and prepare the powder sample as described in Test Method
C1152/C1152M.
18. Obtain a sample of at least 10 g of powder from each. Determine the distance from the
exposure surface to the mid-depth of each layer. For example, the layer thickness and
mid-depth are determined from measurements of the specimen before and after powder
sample collection. Calculate the depth below the exposed surface as the average of five
uniformly distributed measurements using a slide calliper.
19. Chloride Analysis: Determine the acid-soluble chloride-ion content of the powder
samples, Cx (mass %), to ±0.001 % according to Test Method C1152/C1152M.
20. Obtain the initial chloride-ion content, Ci (mass %), from the 20-mm thick slice by
crushing and prepare a powder sample as described in Test Method C1152/C1152M.
21. Record any deviations from the requirements of this method.

2. Calculation
2.1 Test Results:
Determine the values of surface concentration and apparent chloride diffusion coefficient
𝑥
C(x,t)=Cx-(Cx-Ci).erf( ) (1)
√4𝐷𝑎.𝑡
where:
C(x,t) = chloride concentration, measured at depth x and exposure time t, mass %,
Cs = projected chloride concentration at the interface between the exposure liquid
and test specimen that is determined by the regression analysis, mass %,
Ci = initial chloride-ion concentration of the cementitious mixture prior to
submersion in the exposure solution, mass %,
x = depth below the exposed surface (to the middle of a layer), m,
Da = apparent chloride diffusion coefficient, m2/s,
t = the exposure time, s, and
erf = the error function described in Eq 2.
𝑧
erf(z) =2⁄√𝜋 . ∫0 exp⁡(−𝑢2 ) 𝑑𝑢 (2)

2.2 Non-linear Regression Analysis—


Perform the regression analysis by minimizing the sum given in Eq 3.
2
S =∑𝑁 2 𝑁
𝑛=2 Δ𝐶 (𝑛) = ∑𝑛=2(𝐶𝑚 (𝑛) − 𝐶𝑐(𝑛) )
where:
S = sum of squares to be minimized, (mass %)2,
N = the number of layers ground off,
ΔC(n) = difference between the measured and calculated chloride concentration of the nth layer,
mass %,
Cm(n) = measured chloride concentration of the nth layer, mass %, and
Cc(n) = calculated chloride concentration in the middle of the nth layer, mass %.

VI) Standard Test Method for Determination of One-Point, Bulk Water


Sorption of Dried Concrete.

Designation: C1757 − 13

1. Scope
This test method covers the determination of water ingress into the bulk (mass) of a
hardened, dried concrete specimen after being submerged for 30 minutes.

2. Procedure
Test Specimens and Sampling
 Specimens cast in the laboratory shall be made and cured in accordance with Practice
C192/C192M.
 Specimens cast in the field shall be made and cured in accordance with the field-curing
procedure in Practice C31/C31M.
 Carry out Coring and cutting the specimen to length shall be in accordance with Test
Method C42/C42M.
 Drill cores according to Test Method C42/C42M
 Measure the dimensions of the specimen to the nearest millimeter in accordance with
Test Method C42/C42M.
1. Begin testing by placing the specimen in the forced-air oven so that it is at least 25 mm
from any heating surface and from another specimen. Dry the specimen at 50 +/-2ºC for
an initial period of 48+/- 2 h. After the initial period, determine the mass of the oven-
warm specimen. Return the specimen to the oven and determine subsequent oven-warm
masses every 24+/-2 hrs. Drying is complete when the specimen loses less than 0.2 % of
its previous mass during a 24+/- 2 hrs period of drying. For weekend and holiday
interruptions in this cycle, store the specimen in the airtight vessel as specified in bellow
and then begin with another 24-hour drying cycle.

2. After completion of the drying, store the specimen in the airtight vessel for 24+/-1 h.
Maintain the ambient temperature around the vessel at 23+/-3ºC. After 24 h in the vessel,
determine the mass of the specimen and record it as the oven-dried mass. Within ten
minutes, place the specimen on the support rack in the immersion container with a flat
face horizontal and so that it does not contact the container walls or another specimen.
Maintain the water temperature at 23+/-3°C and the water level in the container such that
there is 25+/- 10 mm of water over the top of the specimen.

3. Then Immerse the specimen for 30+/-0.5 min. Remove the specimen; shake it to remove
the bulk of the surface water. Dry it using a damp absorbent cloth as rapidly as possible
until all visible films of water are removed and the surface appears damp. Immediately
determine the mass of the specimen and record it as the mass after immersion.
3. Calculation
Calculate the sorption of the specimen as the change in mass divided by the product of
the surface area of the test specimen and the density of water. For the purpose of this test,
the temperature dependence of the density of water is neglected and a value of 0.001
g/mm3 is used. The units of sorption is mm.

1. Sorption = ( W x D)/ (A*d)

Where:
W = mass of specimen after immersion in grams,
D = mass of oven-dried specimen in grams, and
A = the surface area of the specimen in square millimetres

A=3.14* sd*( sd/2+ sh)


Where:
sd = specimen diameter in mm,
sh = specimen height in mm, and
d = density of water (0.001) in grams per cubic millimeter
VII) CONCRETE, HARDENED: ACCELERATED CHLORIDE
PENETRATION

1. SCOPE
This Nordtest method specifies a procedure for the determination of penetration parameters
for estimating the resistance against chloride penetration into hardened concrete or other
cement-based materials.
The resistance against chloride penetration is determined by accelerated testing.
2. METHOD OF TEST
A water-saturated concrete specimen is on one plane surface exposed to water containing
sodium chloride. After a specified exposure time thin layers are ground off parallel to the
exposed face of the specimen and the chloride content of the layers, Cx, is measured. The
original (initial) chloride content of the concrete, Cj, is measured at a suitable depth below
the exposed surface. The effective chloride transport coefficient,
De, and the boundary condition of the chloride profile at the exposed surface, Cs, are
calculated. This is done by using the related values of measured depth below the exposed
surface,
x, and measured chloride content, Cx.
The penetration parameter, KCr , is calculated for a selected chloride concentration, Cr The
influence of De, Cs, Ci, and Cr is combined in the calculation of KCr, which facilitates
comparison of the results.

3. Procedure
1.Exposure liquid
An aqueous NaCl solution is prepared with a concentration of 165 g ± 1 g NaCl
per dm3 solution This exposure liquid is used for 5 weeks and then replaced by a
new pure NaCl solution.The NaCl concentration of the solution must be checked
at least before and after use.
2. Exposure temperature
The temperature of the water bath must be 21-25 °C with target average
temperature of 23 °C. The temperature must be measured at least once a day.
3. Exposure
The Ca(OH)2 solution in the container used for water saturation is replaced with
the exposure liquid and the test specimen is immersed in surface-dry condition in
the saline solution. It is important that the container is completely filled with the
exposure liquid and closed tightly. The ratio between the exposed area in sq. cm
and the volume of exposure liquid in dm3 shall be minimum 20 & maximum 80.
The container is placed in the temperature controlled cupboard during exposure.
The exposure shall last for at least 35 days, and the container is shaked once every
week. The date and time of exposure start and exposure stop is recorded.
4.Profile grinding
The chloride profile is measured immediately after the exposure by grinding off
material in layers parallel to the exposed surface. The grinding is performed within
a diameter approx.10 mm less than the full diameter of the core. This obviates the
risk of edge effects and disturbances from the coating. At least eight layers must be
ground off. The thickness of the layers must be adjusted according to the expected
chloride profile, so that minimum 6 points covers the past of the profile between
the exposed surface and the depth with a chloride content of Ci + 0.03 mass %.
However, the outermost layer must always have a thickness of minimum 1.0 mm.
It must be ensured that a sample of at least 5 gm of dry concrete dust is obtained
from each layer. For each sample of concrete dust collected, the depth below the
exposed surface is calculated as the average of five uniformly distributed
measurements using a slide caliper.
5. Chloride analysis
The acid-soluble chloride content of the samples is determined to three decimals in
accordance with NT BUILD 208 or by a similar method with the same or better
accuracy. The accuracy must be documented.
6. Initial chloride content
From the concrete slice a representative subsample of approx. 20 g is prepared, e.g.
by crushing until the material passes a 1 mm standard sieve, followed by splitting.
The acid-soluble chloride content of the subsample is determined to three decimals
by using the method described in above The measured chloride content is the initial
chloride content of the specimen, Ci.

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