Building Materials

Building Materials - Chemical and Structural Properties
Dnu T. BABOR
Daniel COVATARIU
BUILDING MATERIALS
Chemical and Structural Properties
Matei-Teiu Botez Academic Society Publishing House Iai 2004

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Descrierea CIP a Bibliotecii Naionale a Romniei

BABOR, DNU T. Building materials: chemical and structural properties / Dnu T. Babor, Daniel Covatariu. - Iai : Editura Societii Academice "Matei-Teiu Botez", 2004 Bibliogr. ISBN 973-7962-52-4 I. Covatariu, Daniel 691(075.8)
Scientific reviewers: eng. Radu HARIGA, Ph.D., Idg scientific researcher National Institute of Testing, Iai branch Head of Building Materials Laboratory eng. Mircea RUJANU, Ph.D., associate professor Faculty of Construction Gh. Asachi Technical University of Iai
Computerised edited, photos and cover: eng. Daniel COVATARIU
FOREWORD
Any material is subjected, by natural laws, to physical or performance decay. Every material reacts entropically to the stimulation of certain external or internal agents. Very often, it reacts even synergically, thus affecting the service life of materials. So, the basics notions about physical and chemical properties and, also, the testing method involved to determine those characteristics are the base of the construction engineers knowledge.
Authors
CONTENTS
1. MEASURES AND MEASURING INSTRUMENTS ........................ 7 2. CHEMISTRY CONCEPTS ......................................................... 21 Chemical measurements, solution concentration 3. LIQUID SOLUTIONS (I) ........................................................ 26 The pH and its applications 4. LIQUID SOLUTIONS (II) ...................................................... Liquid solutions preparation 5. WATER ANALYSIS ................................................................ Identification of some ions, water hardness 6. MATERIALS DENSITIES ....................................................... 34 40 50
7. THE APPARENT DENSITY OF MATERIALS .............................. 57 8. CHARACTERISTICS OF BULKING MATERIALS ........................ 65 Bulk density, holes volume 9. STRUCTURAL CHARACTERISTICS .......................................... 70 Compactness, humidity, water absorption, porosity, bulking of sand 10. GRANULARITY .................................................................... 79 Granularity; Modules of fineness 11. MIXTURES OF BULKED MATERIALS ..................................... 87 12. MECHANICAL TESTS (I) ...................................................... 95 Compression Tests 13. MECHANICAL TESTS (II) .................................................... 100 The Flexural Test; The Cleaving Extensions Test Bibliography ............................................................................ 104
MEASURES AND MEASURING INSTRUMENTS

A laboratory determinations, suppose effectuation of measurements, the sizes and we obtain parameters of calculus for the characteristics which we have to determinate. To make those measurements we need the instruments / measuring instruments. The construction materials will be examined in different modes: looking up the physic-mechanical characteristics when we effectuate a determination; looking up the structural constituents, chemicals, impurity when we effectuate an analysis;
1.1
General rules to effectuate and express the measurements

The instruments and the measuring instruments are
typified by their measurement capacity and precision. the measurement capacity express the maximal value of the size which we can be measured from a single application (for example, with a ruler of 0,50 m the maximal size which can be measured is of 50 cm; the sizes which are bigger can be measure if we implement the ruler more then once); the precision express the minimal variation of the size variation which can be determinate and it usually is the minimal size which is marked on the instrument scale;
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The capacity and the precision of a measuring instrument are in correlation because a smaller capacity permits a better precision because the constructional system of the instrument can be more sensible and it can intimate smaller sizes. For the measuring precision and the instruments precision we must know the following rules: the instrument / measurement instrument must be prepared: keying, balanced, calibrated (after case); we must ensure the environment conditions (temperature, humidity, pressure) and the instrument will be acclimated just before we make the measurements; we handle the instrument without touching the indicator because if we move it the results obtained can be wrong; we must choose the instrument with the proper capacity of measuring, because: - if we overload an apparatus we deteriorate his constructional system; - a bigger capacity goes to a smaller precision; - a smaller capacity impose that we must make the measurement by enforcing the instrument more then once. The sizes are expressed in the measurement units from the international system (Appendix 1.1). The unit expressed in multiples or submultiple is admitted to avoid the calculus with big values or many decimals. If the measuring instruments are in units from other systems, is necessary to transform them in the units from the international system.
In every case is necessary to express the technical characteristics determinates in the measurement units provided by the specific technical norms.
1.2. Dimensions measurement (length)

The measurement unit for length is meter m; but until we determinate the last value we can use its submultiples: centimeter cm, millimeter mm. Ruler, meter and the measuring tape (Figure 1.1) allow measurements with a precision of 10-3 m.
Figure 1.1 - Dimension measuring instruments The measurements are executed through instrument
overlap on the dimension we must measure, with the mark 0 (zero) at the left limit and we read the mark from the right which coincide with the right limit of the dimension. If we use flexible instruments it must be well outspread on the surface we must measure. The caliper (Figure 1.2.) allows measurements with a precision of 10-4m.
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The measurement is executed through the comprehension of the material between the calipers measuring-jaw and the determination of the dimension through the addition of the next values. the number of the undivided millimeters which starts from the mark zero of the vernier; the number of the mark from the vernier which coincides with the one from the calipers rule, as tenths of millimeter. The dimensions which are measured with the clipper are expressed in millimeters.
Figure 1.2 - The Caliper The micrometer (Figure 1.3) allows measurements with a precision of 10-5mm. The measurement is executed through the comprehension of the material between the micrometer measuring-jaw, and the determination of the dimension through the addition of the next values.
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the number of undivided millimeters, marked with oblique signs, which are left-over the barrel; 0,5 mm if between the last oblique sign and the barrel limit we have a vertical sign; the number of the sign from the barrel scale which coincide with the horizontal line from the micrometer scale, as hundredth of millimeters.
the
approximation
of
thousandth
of
millimeter,
if
the
horizontal line from the micrometers scale is between the signs from the barrel. The dimensions which were measured with the micrometer are express in millimeters. To use the micrometer we must comprehend the sample between the measuring-jaws with the help of the operating button; if not, if is actioned by the barrel the micrometer screw will be destroyed by the advancement of the mobile-jaw.
Figure 1.3 The Micrometer The micro-comparator (Figure 1.4) permits to measure a dimension and has precision of 10-5m.
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This apparatus transform the translational motion of the feeling-bar, through a system of interchangeable gears into an angular motion of the pointer. To determinate the dimension, we fix the micro-comparator into a yoke in which is introduced a measured prism. We make the reading on micro-comparator, and after that we introduce the sample which must be measured and we make a new reading. We calculate measured the algebraic and sum the between the dimension of the Figure 1.4 Micro-comparator prism difference between 2 readings.
In the case when we follow up the length variation we repeat the measurements, and we obtain the variation through the difference between the readings or through the lengths difference that we determinate.
1.3. Volumes measurement

The measurement unit for volume is m3, but in laboratory technique the small volumes are expressed in cm3. In order to measure the volumes of liquids we use glass instruments with a calibrated volume or with continuous scale of volume. To effectuate the measurements must be respected the following rules: the liquid and the apparatus must have the standard temperature dilatation;
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to
avoid
the
errors
from
the
thermal
the scale of every apparatus will be analyzed to determinate the measurement accuracy, because it depends by cross section of every apparatus, thats why the scales can be different. the reading of the liquids level will be made perpendicular on the scale, in the tangent plan to the meniscus which is formed at the liquid surface owing to the phenomena of lyophilize or lyophobize; The apparatus must have a vertical position to be sure that the meniscus is perfectly horizontal.
The graduated cylinders (Figure 1.5.b and 1.5.c) and the calibrated pipettes are used for dosage of liquids with floating but predetermined volumes; the volume is measured on scale and is totally transverses. The bubble pipettes and the calibrated flaks (Figure 1.5.a) accept dosages only for the volumes for which are calibrated, by filing them until the stamp.
a calibrated flask b graduated cylinder c graduated cylinder (small) d Bersellius vessel e Erlenmeyer vessel
a)
b)
c)
d)
e)
Figure 1.5 The instruments for liquids volumes measuring

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The
burette
(Figure
1.6)
permits
continuous dosage of the liquids. The mark 0 is at the superior part of the burette, so we can read the volume of past liquid from the burette. For the bulked materials the volume is measured with the help of some volumetric flasks with cylindrical form, sometimes like prism, made up by clad sheet steel thick enough to keep its form. The filler neck attached by the flask permits to over fill the flask, which after we remove it and the excess of material, the entire volume of the flask to be correctly filled with material.
1.4. Masses measuring

The material mass represents the quantity of substance and is expressed in kilograms (kg). For smaller quantities and when we need a higher precision the masses are expressed in grams (g). The instruments for the mass determination compare the gravitational forces which are developing over the quantity of material, respectively over some measured masses (called avoirdupois or etalon masses).
Figure 1.7 Instruments for masses measuring

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The (Figure
technical is made
balance by two
1.7.a)
balance pan which are hanged at lever terminals with equal arms. On one of the balance pan we put the material and on the other we put the avoirdupois until we equilibrate it. The mass is calculated doing the addition of the avoirdupois (etalon masses) masses which were used. The automatic weighing machine (Figure 1.7.b) has two balances pan but also a system of interior levers which make the measurement on the dial scale. In the case when the material mass is bigger than the capacity which is indicated on the scale, on the left balance pan we can put avoirdupois, the total mass being calculated like the amount between the avoirdupois and the indicated weight from the scale. The weigh-meter (Figure 1.7.c) is fated for measurements with big masses (50 100 kg) and has only a balance pan, for the material, the weight being red on the scale. The analytical balance is fated for measurements with small masses (200 g) and a measuring precision of 10-3 g. It is
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made after the model of technical balance but the avoirdupois which is very small, like some rings of fine wire, operate through buttons and are hanged on the balance lever.
1.5. The temperatures measurement

The measurement unit for temperatures in I.S. is Kelvin (K), but we also use the Celsius degree (C). To measure the temperatures we use lab thermometers.
When we use the thermometer is necessary to keep the tank in the environment where we make the temperature measurement, because the thermometer capillary doesnt have contractions on its area to maintain the column of mercury or alcohol at the maximal registered value.
1.6. The forces measurement

The measurement unit for forces in I.S. is Newton (N). In the lab the samples of material are put on trial at presses. The hydraulic presses are operable on the Pascal principle, like a force multiplier. After this principle in a system of communicating vessels, with the sections S1 and S2 different like size (S1 << S2), covered with an air tight pistons, if we press with a force F1 over the smaller piston with the section S1, in the liquid will appear a pressure p which will be transmitted on the surface of the piston with a bigger section (S2). The total force (F2) which is exerted by the liquid over the piston (S2) is computed helping with following formula:
F S F2 = p S2 = 1 S2 = 2 F1 S1 S1
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[1.1]
If the ratio between the two sections is bigger, than the ratio of force multiplication will be bigger too. Force F2 can be read on the attached manometer which is calibrated in units of force. In the structure of a hydraulic press (Figure 1.8 and 1.8) the piston with a smaller section is replaced by a hydraulic pump, and the piston with the big section is considered the mobile balance pan of the press. Setting a sample on the mobile balance pan and clogging its movement with a fix balance pan, the force F2 will be transmitted to the sample.
Figure 1.8 Hydraulic press a) Main group

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b) Control panel
Figure 1.8 Hydraulic press a) Main group The (Figure mechanical 1.9 presses are b) Control panel
principle)
operable on the principle of the weigh-meter. The displacement from the screw, of the fixed balance pan and implicit of the sample, to the mobile balance pan, through a feeling mechanical system make the pendulum with the weight G to rotate. If the rotate angle of the pendulum is increasing than the couple G x D is increasing and that implicit means that the force F from the couple F x d is growing. The pressess scale is divided in units of force, which corresponds to the rotation angle
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of the pendulum and to the attached weight G. The dynamometric collars permit the determination of the forces with the help of micro-comparators which measures the loading deformation. It is executed from special steels and calibrated according to the registered lever deformation, systems, and we determinate on the corresponding force from the calibrated graphic. The force. permits attempts samples relatively small, at a lower intensity with multiplications for the
Figure 1.10 Frhling Michaelis apparatus Figure 1.10 presents, for exemplification, the apparatus Frhling-Michaelis, composed from a system of levers which can multiply for 10 times or 50 times, the force G which is enforced by loading the recipient with some plumb grits from the bunker. When the sample is broken, the grits flowing is stopped, and the force G is determinate by weighing the recipient and implicating the relation oh transforming from mass in force.
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G=kmg in which:
[1.2.]
k is the multiplication ratio of levers system; m is the mass of recipient when its containing grits (kg); g is the gravitational acceleration (9,8 m/s2). Some lab instruments, apparatus and equipments, which
are older, can be calibrated in other force units kilogram-force (kgf) -tones-force (tf), for transformation we must consider the equivalence: 1 kgf = 1 daN = 10 N
Appendix 1.1 Size I.Fundamental units length mass time amperage temperature quantity of substance II. Derivated units area volume density frequency force pressure energy, quantity of heath power quantity of electricity electrical resistance temperature activity of the radionuclide thermal conductivity thermal capacity Designation meter kilogram second ampere Kelvin mol square meter cube meter kilogram on cube meter hertz Newton Pascal joule watt coulomb ohm grade Celsius Becquerel watt on meter Kelvin joule on kilogram
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[1.3]
Symbol m kg s A K mol m2 m3 kg/m3 Hz N Pa J W C O C Bq J/kg
The expression in units I.S.
s-1 m kg s-2 N/m2(m-1 kg s-2) m2 kg s-2 m2 kg s-3 JA V/A 273,05 T s-1 w m-1 K-1 m2 kg s-2 K-1
CHEMISTRY CONCEPTS
chemical measurements, solution concentration
2.1. Units of measurement used in chemistry
The atoms and the molecules, being material particles, have mass. To express the absolute masses (in grams) is difficult for calculus, and because of this in chemistry we express the relative masses (in atomic units of mass u.a.m) which represent the twelfth part from the absolute mass of Definitions: The atomic mass (relative) of a chemical element is expressed like the ratio between the absolute mass of the atom and the twelfth part from the absolute mass of The molecular mass (relative) of
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C isotope.
C isotope. a substance is
expressed like the ration between the absolute mass of a molecule of a substance and the twelfth part from the absolute mass of
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C isotope.
Practically, the molecular mass is calculated doing the amount of the atomic masses of the atoms from which that molecule is composed. To express in grams the quantities of substances, we define: The gram-atom of a chemical element represents the quantity expressed in grams, numerical equal with the atomic mass of that element. The gram-molecule (mole) of substance, which represents the quantity expressed in grams, numerical equal with molecular mass (relative) of that substance.
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The gram-equivalent the quantity from a substance expressed in grams, numerical equal with the chemical equivalent of that substance. The chemical equivalent (Ech) represents the quantity from an element from a radical or a substance, which is combining / is substituting to an atom of hydrogen. In the case of some reactions when the substances doesnt change their chemical valence, the chemical equivalents are calculating with the following rations:
atomic mass valence
molecular mass basic capacity
for the chemical elements for acids
Ech= Ech=
[2.1.] [2.2.]
the basic capacity of the acid is the number of protons H+ contained by the molecule of the acid; for alkalis the alkali acidity is the number Ech=
molecular mass acidity
[2.3.]
of the oxidril groups (OH-)
contained by the molecule of the alkali; for salts Ech=

molecular mass [2.4.] nb. of metalic ions the electric ch arg e of the metallic ions
2.2. Solutions concentration Solutions concentration represents the ratio between the number of solute parts and the number of solution parts, sometimes of solvent. According to our necessities, the parts can be expressed in
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mass units, in volume units, moles or vals and according to these we define the molar, molal and valar percentage concentration. The percentage concentration C % indicate the number of parts of solute dissolved in 100 solution parts, and it could be expressed like: mass units (C% g/g) units of volume (C% v/v) combination of units (C% g/v; C% v/g) A variant for the percentage concentration, when its values are too small is the (C) concentration. Molar concentration (molarity) Cm represents the number of gram, molecules (moles) of solute, which is found in 1 litre (1000ml) of solution. When 1 litre of solution contains 1 mol of solute substance, the solution is called molar solution, its concentration being notated m or 1m. Molarities submultiples and multiples are notated with decimals (0.1m 0.01m) or split fractions (m/10 m/100), respective 10m; 100m. Molal concentration or molality represents the number of gram molecules (moles) of solute substance in one litre of solvent. Normal concentration (valar) or normality Cn represents the number of grams equivalents (vales) of solute substance in one liter of solution. Similar to molarity, the normality is denoted: 0,01n; 0,1n; 1n; 10n; 100n and the solution which have the concentration 1n is called normal solution. The titre of a solution T represents the quantity of substance expressed in grams, contained in 1 ml solution.
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Inside of the practical work, based on the dates from the Table 2.1 we made the necessary calculus to fill the Table 2.2. The elements we calculate will be use in the futures laboratory works. Table 2.1 Chemical element Valence Atomic mass H C O Na Mg Cl k Ca P S
1 4 2 1 2 1 1 5 5 6 1.01 12.1 16.00 22.99 24.30 35.46 39.10 40.1 40.08 32.07
2.3. Concentration calculus of solutions mixtures

If two or more solutions of the same solute substance, but with different concentrations, are mixed, the concentration of the new solution will be contained between the concentrations of the two mixed solutions. So, if Vi and Cni, represent the volumes and respective the solutions concentrations, the concentration which was obtained is calculated as it follows: (Vi Cni) = C Vi [2.5.] formula which results by the fact that every solution will introduce, in the final solution a quantity of solute substance, which corresponds to their volume an concentration. The formula 2.5. can be applied for: - concentration calculus which results in a mixture of solutions (n) is:
1
C=
i=1
(Vi Ci )
i=1
Vi
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[2.6.]
- volume calculus necessary from a solution (n), the other volumes (n-1) being imposed.
n
i=1
n1 (Vi Ci ) + Vn Cn = C Vi + Vn i=1
[2.7.]
and
C
n1 i=1
Vn=
Vi
n1 i=1
(Vi Ci)
Cn C
[2.8.]
No. crt. 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Solute
Moleculary Quantity of CONCENTRATIONS Chemical mass disolvated equivalent Percentage Molarity Normality solute (u.a.m.)
HCl H2SO4 (COOH)2 H2O NaOH Ca(OH)2 CaCO3 CaSO4 CACl2 MgCl2 Ca(HCO3)2 Mg(HCO3)2 Na2CO3 CaO
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LIQUID SOLUTIONS (I)

The pH and its applications
3.1. Solutions pH
Thanks to the neutral character, basic and acid (polar molecule), the water can brake up chemical connections which will be dissolved, this phenomenon is called electrolytic dissociation and which can be described schematically by this relation. AB (A+) + (B-) Electrolytic dissociation is a reversible [3.1.] process that
devolves in accordance whit mass actions: the speed which is caused in a chemical transformation at a certain temperature is in proportion to the mass product, so implicit, of substance concentration that will suffer the process of transformation. The phenomenon will be produced such: in the sense of dissociation with the speed V1=k1 [AB] speed V2=k2 [A+] [B-] in which: k1 and k2 are constants of proportionality that are depending of the system temperature.
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[3.2.]
in the sense of recomposition of the substance, with the [3.3.]
[AB],[A] and [B] are molar concentration of the system in the substance AB and ions like A+, and B-. At the dynamical equilibrium (V1=V2), that means that: k1 [AB] = k2 [A+] [B-] and K =
k [A + ] [B ] = [3.4.] k2 [AB]
The
constant
is
named
electrolytic
dissociation
constant and can be defined by measuring the electrolytic conductivity of the solution and, in function of that, the substances can be classified as: hard electrolytes, which in watery solutions are dissociating completely (HCl; H2SO4; HNO3; Ca(OH)2;NaCl; Na2SO4) medium electrolytes (H3PO4; H2SO3) weak electrolytes (H2S; H2SiO3; H2CO3)
(Pure water suffers electrolytic dissociation, having the constant K=1,810-16) The water molarity is 55,5 and the concentrations of the resulted ions (H+ and OH-) are equal we can say that: K = 1,8 10-16 = and
[H+ ] [OH ] [H2O]
[H+]2 = K [H2O] = 1,8 10-16 55,5 = 10-14

1)
[3.5.] [3.6.]
from which results : [H+]=[OH-]=10-7
For an easy express, we appeal at the common logarithm value, with changed sign, of H+ protons concentration, resulted after the electrolytic dissociation, value named power or activity exponent of hydrogen ions. pH=-lg[H+]
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[3.7.]
For pH=7, the case of pure water results that solutions are neutral because [H+] = [OH-] When an electrolyte is dissolved in water, the electrolytic dissociation schemes: acid + HOH H3O+ + base base + HOH OH- + acid In diluted watery solutions H3O+ is the strongest acid, and HO- is the strongest base, that, adequate the modification of the ratio between the concentration of hydrogen protons and hydroxyl groups, the value of the pH number is changing. for pH < 7, [H+] > [OH-], the solution will take an acid character; for pH > 7, [H+] < [OH-], the solution will take a basic character. is produced in accordance whit the fallowing
3.2. Determination of the pHs solutions

Solutions pH can be determined by the calorimetrical methods, using the pH indicators, or by electrical methods. The indicators are organic substances which, changes their colour after structural changes and ionization processes. The changing of colour take place in pH specifically domains of value of the indicator named domains of banking or transition space.
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Table 3.1 - The main pH indicators Colour in average: pH indicator Acid Basic Phenolphthalein colourless red Cudbear red blue Bromtimol blue yellow blue Methyl red red yellow Methyl-orange red yellow Violet methyl green violet
The pHs domain of banking 8-10 5-8 6-8 4-6 3-4,5 0-2
Indicators can be used under the shape of solutions, ordinarily alcoholic ones, and is underlayed in small amounts (13) drops, in the solution which must be analyzed, or under shape of impregnate filter paper, which will be introduced in solution that must be analyzed. The valour of the pH number is established by comparing the colour which is indicated in the solution whit the etalon scale of colours of the indicator which we used. Determination of the pH number by electrical methods, named also potentiometrical methods, is based on the measuring of the electromotive tension of an galvanic cell (primary cell) formed, in the solution which must be analyzed, from a reference electrode (with a known potential) and a potential electrode with a potential variation in action whit the concentration of H+ ions from the solution which must be analyzed. The potential electrode is formed from a semi-transparent balloon flask which contains a well known concentrated solution and a contact metal electrode. The electromotive tension that appears as a result of the potential unbalance between electrodes, leading through the balloon wall the hydrogen ions H+, caused by the equalization bearing of solution concentration,
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amplified by the electronic system of the device, is measured on the calibrated scale in pH units. In this case, it will be used as indicator electrode, the glass electrode (fig.3.1) and as reference electrode the calomel one. In principle, a glass electrode is made of a small balloon (1), with very thin walls, made of a special composition with roll by semi-permeable membrane; in interior is introduced a solution (2) with a known pH (ex. HCl 0,1m) and an electrode (3) which assure the electric contact electrode (ex. Ag / AgCl, HCl). When we introduce the electrode of glass in a solution, the potential that appears at interfaces glass mean broom- solution is determined almost exclusively, by the ions of hydrogen concentration from the solution. The using of the glass electrode as measure electrode of the pH, because of equalization tendency of the H+ ions concentration from the solution of unknown pH in which this is introduced. For measuring of the pH its made the galvanic cell:
1. Reference electrode 2. Glass electrode 3. Solution of unknown pH
Fig.3.1 Glass electrode
The determination of the pH with this cell is made with the help pH meter apparatus which uses amplification electronic circuits because the glass electrode has a very big resistance (1200 M); pH-meter offers the possibility of direct reading of the pH, their scale being graduated in pH units.
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3.3. Applications of solutions pH number. Titration

Hydrogen ions are present in all watery agents. All chemical processes that take place in this kind of agents are influenced by those ions directly when they participate in process, or indirectly. From this point of view the pH number must be considered an important parameter in many lab processes, industrial or natural. The calorimetrical method is expeditive, the pH number of liquids is the first parameter which can notify over the impurity of the liquids and the level of chemical aggressiveness over materials. Knowing the nature of the solute and his electrolytic dissociation constant, in function of the pH number can be estimated the diluted watery solutions molarity. In lab techniques, the calorimetrical method can be applied in titration operation for the determination of a solution concentration using another solution which has a well known volume with unknown concentration in which is introduced 1-3 drops of indicator solution, then will be added drop by drop from a burette another solution (with a well known concentration). The conditions to realize the process of titration are: The solute from the titrated solution must react with the solute from the titration solution and the mixture of substances must become neutral; We must know exactly the concentration of one of the substances; It is optimal to use the indicator which turns in pH number domain; All the time during the titration process the substances must be agitated for the assurance of the reaction.
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The titration process is finished when it reaches equivalent moment, when the 2 solutes had reacted in equal proportion. This moment is marked by the appropriate colour of the pH number determined by the solution concentration in the product of the reaction of the solutes. Knowing the law of chemical equivalents, that says that substances react between them in equal number of equivalents and expressing solutions concentration by normality, in the equivalent moment next relation is verified. V1Cn1=V2Cn2 from which results Cn1=Cn2 V2
V1
[3.8.]
V1 and V2 are volumes of the mixture, in the equivalence moment; Cn1 and Cn2 are the solution normalitys (Cn1 is unknown). In the practice work we will execute:
determination, with pH indicators from the cases (table 3.2). demonstratives titrations, with solutions of NaOH, HCl and (COOH)2 with the indicated concentrations. The specific reactions of these reactions are: 2NaOH + H2C2O4 Na2C2O4 + 2H2O NaOH + HCl NaCl + H2O [3.9.] [3.10.]
Table 3.2 Practice results

SOLUTION Indicator Color Solution pH Obs.
distilled water potable water solution of NaOH solution of HCl solution of (COOH)2 lime water cement suspension
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3.4. Minimal rules for labour protection Chemical substances could be caustic, so we must follow several rules: we mustnt smell the chemical substances. we mustnt make mixture of substances, other than we have to do. the recipients which contains chemical solutions or substances will be closed and carefully used to avoid the breaking. we must avoid the contact of the chemical substances with our skin or clothes. In the case of an accidental contact well dab the contact zone with a piece of cotton fill with a dilute solution which is able to neutralize the effect of the first one, and after that we must wash with water. the solution discharge will be made only if are diluted and neutralized. After we finish our work the recipients and the apparatus must be washed with potable water.
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LIQUID SOLUTIONS (II)

Liquid solutions preparation
In laboratory technique, to prepare the solutions with an especially concentration, we must face out to the following problems: We must eliminate from the solvent the substances which can react with the solute, and which can form impurities in the solution which is prepared; The correct dosage of the solute; We must verify if the concentration of the prepared solution is the same with the exact concentration that we realized; Getting out a solution with an imposed concentration, by mixing up two solutions with different concentrations. 4.1. Solvents purification In the case of watery solutions the first problem which appears can be resolved using the distillate water like solvent. Doing the distillation we eliminate the salts and by boiling we eliminate the gasses which were dissolved. The entire apparatus which was used in the solution preparation will be washed with the potable water, and than with distillates one, and the recipient which will keep the solution, and also the apparatus which were used to dosage the solution will be washed at the end with the solution which will get. The recipients which keep the solution are tight fitting. In the case of the solvents which can not be distillated we add chemical substances which react with the impurities and
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forms new substances which, doesnt reacts with the solute, or it precipitates and it can be separated by filtration or decantation. 4.2. Solute dosage In the mater of a correct dosage of the solute, we have different cases, depending by its estate (pure or impure, solid or solution, stabile or unstable at the storage conditions). The cases which could meet can be showed, in principle with one of the fourth cases: Case I: The solute is pure and stabile at the storage conditions In this case, the necessary quantity of solute is stored more precisely (with analytical balance, with burette or with pipette) and is introduced in a smaller volume of solvent, after the total dissolution the volume of solution is completed with solvent. Case II: The solute is stabile at the storage conditions, but it presents impurities with other chemical substances The case is typified with the preparation of the oxalic acid solution in the water, with the concentration 0,1n. The oxalic acid is am organic acid with the chemical composition regranted by the formula (COOH)2. It is crystallized with two molecules of water, estate in which is stabile compared to the atmospheric gases. In the dosage estate, this solute will have this chemical formula (COOH)22H2O To prepare one litre of solution 0,1n it is necessary a quantity of 0,1 val of pure oxalic acid, and that means a quantity of 0,1 x 45,019 = 4,5019 gram.
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At the weighing of this quantity, we introduce crystal water (which will become solvent), that will make to be necessary the supplementation of crystalline solute with the quantity of crystal water, from its content. To prepare the solution we must dose the quantity of crystalline oxalic acid by:
0.1val[(COOH)2 2H2 O] = 0.1 1val(COOH)2 + 2val(H2 O) =
= 0.1(45.019 + 2 9.008) = 0.1 63.035 = 6.3035g
[4.1.]
Case III: The solute is unstable at the storage conditions This case is exemplified by preparation of a sodium hydrate solution, in water, with a concentration of 0,1n. The sodium hydrate easily reacts in water with the atmospheric equation:
2NaOH + CO2 Na2CO3 + H2O
carbon
dioxide,
and
will
carbonate
after
the
[4.2.]
Forasmuch the carbonation of the hydroxide granules is variable, we cant dosage the exactly quantity of 0,1 val (4g) of pure sodium hydrate. To solve this problem, we prepare a solution with a concentration easily higher, solution for which well determinate precisely the concentration which will be corrected by dilution until we get the needed concentration. In fact, we weighing a bigger quantity (57)g of sodium hydrate granules, which is superficial carbonated, than we wash it with distillate water (to remove the carbonated layer) and than will be dissolved in distillate water to obtain one litre of solution. The concentration of the new solution will be determinate doing the titration with oxalic acid 0,1n in the presence of phenolphthalein:
36
It is measured V1=20cm3 of oxalic acid solution, with the concentration Cn1=0,1n, and is introduced in an Erlenmeyer flask, is warmed up at a temperature of (60 70)oC, to eliminate the dissolved carbon dioxide if it exists, is cool down at 20oC and we put 2 drops of alcoholic solution of phenolphthalein 2% that the solution stays colourless, because the phenolphthalein is colourless in acid. It is filled a burette with solution of NaOH (until 0 stamp),and we must to determinate its concentration Cn2; In the solution of oxalic acid we drop the solution of NaOH, until we obtain as the colour a persistence weak-pink (equivalence moment); We read on the burette the consummated volume V2 of solution of NaOH. During titration the Erlenmeyer flask must be agitated to uniform the concentration of the reaction product. During the titration we obtain the sodium oxalate after the following reaction: 2NaOH + H2C2O4 Na2C2O4 + 2H2O [4.3.]
We calculate the normality of the NaOH solution, Cn2 with the relation: Cn2 x V2 = Cn1 x V1
Cn2 = Cn1
V1 V2
[4.4.]
To correct the normality at the value Cn=0,1 an initial solution volume (Vini) with normality Cn2 must be transformed by dilution with distillate water, at a final volume (Vfin), calculated with the formula:
37
Vini x Cn = Vfin x Cn2 Vfin = Vini where f is called solution factor.
Cn2 =Vini x f Cn
[4.5.]
The water volume (Vwater) which was used to dilute the volume of solution Vini will be: Vwater = Vfin - Vini = Vini(f-1 [4.6.]
Case IV : The solute is unstable at the storage conditions and it is in a solution with the concentration almost known. This case is exemplified by the preparation of a solution of chlorine hydride of 0,1n. The chlorine hydride is gaseous at normal temperature and pressure. To be used, it must be dissolved in water, being fabricated (like a lab reactive) in solution with a concentration of 37 % (m/m) and a density =1.19g/cm3(dates which are on the flask etiquette). The volume of solution which must be dosed, to obtain 0,1n of pure chlorine hydride, results from the next reasoning: 0,1val(HCl) = 3,65 g
(HCl gaseous)
[4.7.]
For a concentration of 37%, those 3.65g of chlorine hydride will be found in the solution mass (msol): msol =
3.65 x 100 = 8.3 cm3 37 msol 9.86 = = 8.3 cm3 sol 1.19
[4.8.]
which corresponds to a volume of solution: Vsol = [4.9.]
Forasmuch we cant count on the solution concentration, we proceed in the same way like in the case III: we prepare a solution with a concentration easily higher than the one we must find out (using a bigger volume of chlorine hydride), than we
38
determinate the exact concentration of the prepared solution (by titration) and we dilute to obtain the imposed concentration. In the case of chlorine hydride, titration is executed with a solution of sodium hydrate, in the presence of methyl orange indicator. In a Erlenmeyer flask we introduce 20 cm3 of solution of NaOH and 1-2 drops of methyl orange (the solution will become yellow); We titrate with solution of HCl, until we obtain a orange color(the color of the crust of dried onion) During the titration, we obtain the reaction of sodium chloride: NaOH + HCl NaCl + H2O [4.10.] We calculate the normality of chlorine hydride and the volume of water which is used to dilute the solution, to get it at the imposed normality, similar to case III.
39
WATER ANALYSIS
Identification of some ions, water pH, water hardness
The natural water and the industrials one are, in fact solutions because of the substances which are dissolved in it. The water which is coming from rainfall, crossing the atmosphere which is more or less polluted dissolves small quantities of gases (O2, N2, NH3, CO2, H2S, SO3, also ). Surface water as those from under the ground dissolves some components of the rocks they get in contact with and so they can get to contain chemistry salt of ( Ca, Mg, Na, K, Al, Fe ) And in helmet estate, particles of loam and sand in suspension, inclusive organic substances. Chemistry salt from the water provoke in homogeneity in many industrial processes where is used (rocks sediment in the power plant installations, the rinsing and whitening of the textures, corrosion). In constructions, the water used for making materials (mortar, reinforced concrete, clay paste) must fulfil certain quality parameters concerning the mineral and organic substances it contains. If that parameter isnt performing the proper reactions can be affected with negative effects over the conglomerates that will be obtained. Also the impure water they get in contact with the elements of constructions can provoke corrosions of the materials they are made of.
40
5.1. The water quality analyses

Being known the capacity of the water to dissociate electrochemical most of the organic chemical substances, the presence of these substances in water can be observed by detecting of some distinctive ions of them. For this the water to analyze is treated with specifically reactive that the ion we are looking for reacts with and provoke optical phenomena chemistry salt that can be observed (the appearance precipitates with different forms and colors, coloring or discoloring of the substances, emission off gasses with distinctive smells). 5.1.1. Identification of inorganically substances Ca2+ ions frequently found in natural water has a distinctive reactive the oxalic acid or soluble chemistry salt and together led to a white crystalline precipitate of calcium oxalate: COO COO Fe
3+
COO + Ca
2+
COO
Ca
[5.1.]
ions identifies with a solution of potassium sulphur-cyanide
(KSCN) with which they make complex basic ion [Fe(SCN)]2+ colored in an intensive red: Fe3++SCN [Fe(SCN)]2+ [5.2.] NH4 ions identifies with an alkaline solution of double iodide of Hg and K (Nessler reactive) with which it makes an amorphous precipitate , red-brown of mercury and ammonia iodide. NH4 + KOH NH3 +K+ + H2O Hg NH3+2K2HgI4+3KOH O Hg
41
[5.3.] NH2I + 7KI + 2H2O [5.4.]
Pb2+ ions identifies with solutions of chromium-plated or bichrome of sodium or potassium which precipitates the lead chemistry salt in yellow chromium-plated lead . Pb2+ +CrO4 2 PbCrO4 2Pb
2+
[5.5.]
+
+ HOH + Cr2O7 2 PbCrO4 + 2H
[5.6.]
Cl identifies with the silver nitrate ( AgNO 3 ) with which it forms an white-cheesy precipitate: Cl + Ag+ AgCl an white crystalline precipitate of barium sulphate. SO4 2 + Ba 2+ BaSO4 [5.8.] [5.7.] SO4 2 ion identifies with barium chloride (BaCl 2 ) with which it
Nitrite ions (NO2) identificates with potassium iodide (KI) witch colors in brown the water witch is easily carbonated with cloric acid (HCl) , because of the releasing of the iodine. 2NO2 +2KI+4HCl I2+2NO+ 4Cl +2k++2H2O [5.8.] If after we treat the water with a few drops of carbon tetrachloride (CCl 4 ) , iodine dissolves and the water gets a violet colour. 5.1.2. Organical substances identification The presence of the organic substances in the water is showed with indirect methods, based on the reduction action of them over the potassium permanganate (KMnO4), acid environment. 2KMnO4+3H2SO4 K2SO4+2MnSO4+3H2O+5O
42
[5.9.]
The atomic oxygen resulted will oxidize strongly the
organic substance. Presuming the existence of oxalic acid, this substance will be decomposed like that: COOH 5 COOH If followed the by water the we have of to analyze contains ion organic Mn 2+ substances the mentioned reactions will happen and it will be changing permanganic into uncoloured, and the solution will discolour itself. If not the mentioned transformation will not happen, and the solution will remain coloured in violet. For small quantities of organic substances it is necessary for the water which is too analyzed, to be heated. In order to identify the organical substances, there are introduce 2 3 ml of analysed water in a test tube, and also some drops from the specific reactant solution. If the searched ions are find, it will be produce a well-known reaction. The quality analysis data will be noted in the Table 5.1. Table 5.1. Quality analysis data The searched ion The specific reactant The identification reaction The ions presence +5O 10CO2 + 5H2O [5.10.]
43
5.2. Determination of waters pH

The determination is making in no more 4 hours after harvest tests. Usually are used the indicators (solutions as paper band). In order to select the indicators we must know the turning domain. In case of muddy waters, when the indicators colour may be physic influenced, we put a drop of water, an paper band and we will obtained a colour which is analysing on opposites faces of paper band. The values far of 7 value (neutrality) gives information about water contained, like chemical impurities substances, high concentrations and in this case are required to make quantitative chemical analysis. In the case of cement, concrete, a pH < 6,5 means that the water present a aggresivity type general acid.
5.3. Water hardness

Hardness represents the water concentration in calcium and magnesium chemistry salt. The main chemistry salt substances of the metals which are found dissolved in water are: Bicarbonates which dissociate in carbonates when the water is heated and which have a smaller solubility then bicarbonates , precipitates with the name of cauldron stone. Ca(HCO3)2 CaCO3 + CO2 + H2O Mg(HCO3)2 MgCO3 + CO2 + H2O remain dissolved even when the water is heated.
44
[5.11.] [5.12.]
Chlorines and sulphates (CaCl2; Caso4, MgCl2, MgSO4) which
The different reactions of those two categories of chemistry salt substances at the heat, leads to a number of two categories of hardness: temporary hardness (Dt), assigned by the bicarbonates and which disappears when the water is heated. permanent hardness (Dp), assigned by the chlorors and sulphates and which maintains when the water is heated too. Putting them together we get the total hardness (DT), of the water. DT = Dt + Dp which can have two significations: French hardness degree (dF), represents the content of chemistry salt substances equivalent with 10mg CaCO3 at 1000ml water; German hardness degree (dG) represents the content of chemistry salt substances equivalent with 10mg CaCO3 at 1000ml water. In Romania we use the german degree. 5.3.1. Temporary hardness determination Water temporary hardness can be determinate by titrating a volume of water perfectly measured, with a solution of HCl0,1n in the presence of methyl orange as indicator: it was filled a burette with a solution of HCl-o,1n (until the 0 point); in an Erlenmeyer ampoule its measured 100 ml of water for analyze and we ad 2-3 drops of orange methyl indicator. If the water contains alkaline chemistry salt substances it will become yellow;
45
[5.13.]
Water hardness is expressed in degrees of hardness (d),
titrate the content of the ampoule with acid solution from burette until the colour of the water become orange (the indicator facing); read on the burette, the volume of HCl-0,1n used in the titration. At the titration the following reaction take place: Ca(HCO3)2 + 2HCl CaCl2 + 2CO2+ 2H2O Mn(HCO3)2 + 2HCl MnCl2 + 2CO2 + 2H2O make the following reasoning: We know the specific chemical sizes of the solutions 1molHCl = 36,5g ; 1valHCl = 3,65g; 1molCaO = 56g ; 1valCaO = 28g; According to the law of masses action the substances react between them in equivalent proportions with their molecular masses; 1mol from a substance will react with 1mol from the other. Considering a ml of solution of HCl-0,1n used in the titration will react with CaO (instead of bicarbonates) . 2HCl + CaO CaCl2 + H2O is 3,65 mg following the law of masses action, it results:
36,5gCaO (1molCaO ) 28gCaO (1molCaO ) a 3,65 10 3 gHCl(a.mlHCl 0,1 ) xgCaO 3,65 10 3 28 x = a = a 28 10 3 gCaO = a 28mgCaO 36,5
react,with react,with
[5.14.] [5.15.]
In order to express the temporary hardness in degrees we
[5.16.]
Knowing the solution titer of the solution of HCl-0,1, which
[5.17.]
Because the ,,a ml of HCl have been used for titration of 100ml water and 1dG represents 10mgCaO/1000ml of water extra poling we obtain in german degrees:
46
Dt =a
2,8 1000ml = 2,8 a 10 100ml
[dG]
[5.18.]
So we can get to the conclusion that for every ml (cm3) of HCl-0,1 solution used at the titration corresponds 5,0dF . 5.3.2. Total hardness determination After titration with HCl the bicarbonates acids are of 100 cm3 water
transforming in chlorides which are added to the chlorides and sulphates which are already in the water. So the temporary hardness was transformed in permanent hardness which in fact transforms total hardness in the treated water. Determination of total hardness is made by titration with a solution which would react with the chlorides and sulphates. For these we use the solution of disodium salt of ethylenebiamino-tethraacetate acid in the presence of black eriochromiums indicator. By the name of the titration substance the method is named complexonometryc titration. The determination is executed as it follows: from the water test titration with a solution of HCl 0,1n (for the determination of temporary hardness, according to 5.2.1), are taken 50 ml and introduce its into an Erlenmeyer phial; the containing of the phial are boiled for 3 4 min in order to eliminate the CO2 existent in the water; after the cooling of the phial in the air and then in a water current, introduce a pin of spatula ( about 0,2-0,3 g ) and add 2 ml of tampon solution, for obtaining a pH of (8 10).
47
we titrate, immediately, the contain of the Erlenmeyer phial with solution of complexon III - 0,01n, from the burette until the colour turns from red to blue; read exactly the volume of solution of 0,01n used for the titration ; The calculation of the total hardness is made with the relation: DT = 2 . V . 0,5610dG in which: V the volume of solution of complexon III - 0,1n used for titration of the water test 0,561 the quantity in mg of CaO witch corresponds for 1 ml solution of complexon III - 0,1n. [5.19.] complexon III -
5.4. Permanent hardness

The permanent hardness is calculated based on the relation [5.13.], as a difference between the total hardness (permanent type) from the water titrated with HCl and the temporary hardness, determined in & 5.3.1. Table 5.2.
Probe no. Temporary hardness Probes a ml sol a 2.8 volume HCl 0.1n (ml) Probes volume (ml) Total hardness x ml 2n complexon 0.561 solution Permanent hardness Dp (d) Water category
1 2 3
100 100 100
50 50 50
48
Appendix 5.1. Conditions for the water quality used to the mortars and concrete preparation to be pure, do not contain organic or inorganic suspensions; do not have pronounced taste and smells; to correspond to the following characteristics: Characteristics H ions concentrations, pH Salt total contained [mg / dm ], (SO4 ) sulphates, (Cl ) chloride,
223 3 3 +
Admissibility conditions 5 10 maximum maximum maximum

3
2000 2000 500 1000 500 600 500

3
[mg / dm ], [mg / dm ],
-
(CO3 ) carbonates, (CO3H ) hydrocarbonates [mg / dm ] (Mg ) magnesium Alkali (Na2O)

2+
[mg / dm ], [mg / dm ],
3 3
maximum maximum maximum
Organical substances [mg / dm ],
Loses at the burning of the insoluble substances [mg/dm ]
800
49
MATERIALS DENSITIES
The real or absolute density of a material represents the unit mass (m) of material volume, named real volume (Vr), which forms that = material without pores, gas holes or other discontinuities):
m [g/cm3] Vr
[6.1.]
The density is calculated with four decimals and is expressed by rounding-off at three decimals.
6.1. Liquids density

For pure liquids, the volume which fills a space can be considerate like the real volume, without pores. Liquids purity refers to solid substances and also at liquid ones, and at the gases which can contain it in dissolved state. The elimination of solid substances or liquid which were dissolved is made by distillation. The elimination of dissolved gases is made by liquids boiling, knowing that at the boiling temperature the gases solubility, in the liquid solvent, is null. 6.1.1. Expedite methods Expedite methods can be applied with informative
character, whereas, because of the measuring errors, the results are more or less exactly.
50
Determination method of net mass of liquid which fills a calibrated flask, with the volume (VB) resides in: weighting of a calibrated flask, clean and dry (m1); filling of the calibrated flask with liquid which is to analyze, until it reaches the stamp; weighting the calibrated flask with liquid (m2); The liquid density (L) will be: L = m2 m1
VB
[g/cm3]
[6.2.]
Densimeter
(aerometer)
method
resides
in
the
immersion of the densimeter in liquid (Figure 6.1.), liquid density being read directly on the densimeter scale. Densimeter is composed by a closed tube, lested at the inferior part, that has a mass (m). When it is immersed in liquid, the densimeter will be activated by his weight (G), but also by Arhimedes force (F), equal to volumes weight of dismounted liquid. At the diving equilibrium, it can be written the forces equality. G = m g = F = mL g = VL L g from which results : L=
m VL
[6.3.]
[g/cm3]
[6.4.]
However the densimeter mass (m) is constant, it results that liquid density is linear function (inverse) by densimeter volume which was immersed in liquid in equilibrium position. The superior part of the densimeter which is smaller and
51
scaled permits a better precision, by variances intimation of the immersion volume.
reading level
A reading level for lyophilise liquid
reading level
B reading level for lyophobe liquid
Figure 6.1. Determination principle with densimeter
6.2. Solid materials density (porous)

In the case of solid materials, for density determination, the assay mass is measured when it is dried at constant mass. The solid porous materials contain in their volume pores, which have a volume that cant be determinate. In order to determinate the real volume, it is imposed the structures destruction, that the material will become powder, with grains smaller than 0.125 mm. We appreciate that at these dimensions, the material grains dont contain tight pores any more. In order to get the material in atomization form, we proceed in this way: the material (aprox. 1Kg) is triturated, as petty as we can, in the steel
52
we mix up the triturated material until it becomes homogenous and it halves its quantity, by the quarters method; we increase the detained material, in agate mortar, until the entire quantity (aprox. 0.25 Kg) passes in the gauze with holes of 0.125mm; we mix the powder until it becomes homogeneous. After drying at constant mass we bring out the determinations of the assays, constituted of 10 30g powder, for each one we determinate the volumes. 6.2.1. The burette method The burette method, for determination the volume of a powder assay, is an informative method, being expeditive, but an approaching one. Like in the liquids case, the errors come from necessity of measuring liquid volumes. The burette method resides in the following succession of operations: we weight in a calibrated flask, dry and clean (m1), having the inscribed volume (VB); we introduce in the flask a quantity of (1030) g of powder from the assay which is to analyze and we weight (m2); we calculate the difference between masses obtaining the net mass (m) of the powder from the flask (m=m2-m1); we fill in a burette until it reaches the mark 0, having the capacity at least equal
53
to the flasks volume, with reference liquid; we put the flask under the burette and we open the valve, for the reference liquid to distil in the flask, this being permanently agitated (by circular moves) to eliminate the air; when the level of the reference liquid reaches the mark of the flask, we close the burettes valve and we read the volume of the flowed liquid (VL). The powder volume (real) from the flask will result as the volume of the liquid which doesnt get into the flask because it is occupied by the powder: Vr =VB-VL [cm3] [6.5.]
The material density will be calculated applying the relation from the definition [6.1.]. 6.2.2. The pycnometer method The pycnometer method is standardized, being more exactly than the burette method; it replaces the measures of volumes with weightings (at the analytical balance) and permits the total elimination of the air (desaeration) from the system powder- reference liquid. The pycnometer is like calibrated flask, but without the volume mark, and having a thread plug. When the pycnometer is filled in with liquid and the plug is in, the access of liquid will be eliminated throw the capillary that circulates through the plug or the capillary arm, which is attached to the flask, that it will be eliminate the
54
necessity to know the volume by reading the level of the liquid at the calibrated flasks mark. The pycnometer method resides in the following succession of operations: we weight the pycnometer clean and dry (m1); we fill it in with the reference liquid, which will be used at the determination, we put the plug, we wipe on the outside with absorbent paper and we reweight it (m2); we empty the pycnometer and we dry it in the air oven, in order to be rebring it at the initial mass (m1); we introduce into the pycnometer the assay powder of (1030) g and we reweight it (m3); we fill it in, with aprox. 2/3 from the volume, the pycnometer with reference liquid, over the powder, and we put it on the sand bath and is boiled for 15 min. (for desaeration); we let the pycnometer unmoved at the air, until we got the temperature of 20C, while the powder deposits and the reference liquid becomes clearly; we complete the volume of the pycnometer with the reference liquid, by easy casting, we put the plug, we wipe it on the outside with absorbing paper and we weight it (m4). From the difference between masses an knowing the density of the reference liquid used (L) we obtain: The liquid volume that gets into the pycnometer: VL =
m2 m1 ; L

The material mass (powder) introduced in the pycnometer m=m3-m1 The liquid volume that gets into the pycnometer, over the
55
powder: V1=
m4 m3 L
The powder volume (the real volume of assay): Vr=VL-V1 All the weightings are effectuated with the analytical
balance, with the precision of 10-3 g. The material density will be calculated by applying the relation [6.1.]. In the case when we use a reference liquid that cant be boiled, for desaeration (astral oil, anhydride gasoil a.s.o.), desaeration is realized by introducing the pycnometers into the vacuum exicator from which we extract the air for reaching the pressure of 20 mmHg , until we observe the stopping of liberation of air bubbles in the exicator.
56
THE APPARENT DENSITY OF MATERIALS

The apparent density of a material (A) represents the mass the apparent unit volume, formed by the solid matter and from its a.s.o.). a=
m Va
discontinuities
(pores,
vacuums,
capillaries,
clefts,
[g/cm3; kg/dm3; t/m3]
[7.1.]
The density, in g/cm3, is calculated with four decimals and is expressed with three decimals. In order to determinate the apparent density, the assay mass (m) is always determinate, when its dry at constant mass. There are situations when, for determination of other technical properties, or for estimate the characteristic variations, we must determinate the material unit mass of volume which is at different humidity. The values which we obtain are used like estimate parameters of that characteristics, and it doesnt represents the apparent density. In order to measure the apparent volume, we can implement and other methods, depending by the form of the assays.
57
7.1. Apparent volume determination on the control cylinders and boring kernels
In the case of assays with regulate geometrical form (kernels and control cylinders), of the the simplest method and of the determination the apparent volume resides in direct measuring of characteristic dimensions geometric body application of the calculus formula of its volume. At the prosecution of measuring it must be counted the fact that the assay can have deviations from the theoretic geometrical form (deviations derived at the carving, from small defections of dies a.s.o.). Thats way, the characteristic dimensions that are introduced in the calculus formula of the volume, we adopt as arithmetic mean for other measuring, as it follows: in the case of cubic assays (Fig. 7.1.a), every characteristic dimension results as arithmetic mean of the four corresponding edges; in the case of edges, that it prismatic assays (Fig. 7.1.b), it counts will be measured the transversal the appearance of deviations from the linearity of long dimensions and at the half of the length (L); in the case of cylindrical assays (Fig. 7.1.c), on the same criteria like the prismatic assays, we measured the perpendicular diameters from the bottoms, but also from the meddle of the height (h). Thus, it results, that for application in volume calculus formula, every characteristic dimension will be calculated as a mean:
n
lj =
i =1
li
n
58
[7.2.]
b3 a3 b3 c3 a4 b2 a1 b1 b2 a2 b4 c1 c4 c2
a3 a2 c3 c1 d4 h3 h2 a4 a1 d2 b1 d3 h4 d1 h1 b4 c4 d6 d5
c2
a) cube
b) prism
c) cylinder
Figure 7.1. The characteristic dimensions of the regular shapes 7.2. The apparent volume determination on assays with irregular form In order to determinate of an assays apparent volume with irregular geometrical form it is applied the principle of dislocated liquid volume, in many other alternatives. 7.2.1. The gradated cylinder method The method is consigned, but appreciative; the obtained values could be accepted as informative character. The error source of the method resides in using of some gradated cylinder with big diameter, to aloud the liquid assays introduction. The method resides in the following operations: in a gradated cylinder we introduce a volume easily bigger then the assays volume, with reference liquid,
59
and we read volume indicated on the cylinder scale(V1); we introduce the liquid assay (it must be completely immersed) and (Figure 7.2.) we read the new indicated volume on the cylinder scale (V2); the difference between the volumes (V2-V1) will represent the dislocated liquid volume as assay.
v2 Reference liquid v1
v2-v1
Figure 7.2. The gradated cylinder method For the volume of dislocated liquid to represent the apparent volume of the assay, we have to prepared it first, that the absorption of the liquid by the material to be clogged (the apparent volume resides the material opened pores). After the assay weight when is dry and at constant mass, the preparation for immersion can be realized in two variants: the assay saturations resides in assays immersion in a bath with the liquid which will be used as reference liquid, and maintaining as this for at least four hours; the assay paraffin-covering rides in the roofing of the assay with a paraffin layer, to realize a impermeable thickness for the reference liquid. When we prepared the assay by saturation the dislocated
60
liquid volume will express directly the apparent volume of the assay. For paraffin-covering, we prepared a paraffin bath, which warmed until it melts (a higher temperature gets at big fluidity of the paraffin which gets to material penetration in the open pores). The assay which is dried and cooled off at constant mass is clamped with a laboratory plier and is immersed, for a moment, in paraffin. We wait until the paraffins adherent layer is solidified and cooled off, then we clamped it with the plier in other position and we immersed it again in paraffin. We repeat the immersion, for some times, until we realize a continuum paraffin layer, approximated as 1mm thickness. At every immersion we verify if the adherent layer of paraffin doesnt contains air checks, these must been broken with a needle which is easily warmed. At the immersion of the paraffin assay, the volume of dislocated liquid will represent the apparent volume (Va) plus the volume of the paraffin adherent layer (VP). In order to determinate the paraffin volume, we determine the mass of the adherent paraffin (mP), by weighing the paraffin assay (m1) and the difference between the mass of the assay that isnt paraffin-covered (mP=m1- m). Knowing the paraffin density which is P=0.92 g/cm3 (we work with pure paraffin), we calculate the paraffin volume (VP) from the derivate formula of the density: VP =
mP P
[cm3]
61
[7.3.]
that will be deducted from the dislocated liquid volume, to obtain the assays apparent volume. Exist an alternative for applying the method, which permits the determination on assays relative big, with a tolerant precision of the volume measures. The method resides in using a recipient with a big volume, which has a leakage too-fill. In the recipient we introduce the reference liquid and we wait, and because of the leakage, the level of the liquid to be stabilized at the too-fills level. We attach a collector recipient and we introduce the assay into the liquid. The flowed liquid throw too-fill, which is collected (Va) is measured with an instrument with a better precision than if we would use a scaled cylinder with a big diameter (corresponding with the assays dimension). 7.2.2. The hydrostatic balance method The hydrostatic balance method is standardized, being more precisely, compare to scale cylinder method, because the measures are effectuated through weighing. The hydrostatic balance (Figure 7.3.) is a technical one, with two pans, one of them being shorter, to permit the assays hanging and its immersion in a bath with reference liquid. The assay which was prepared, is weighing in air (m1) and after that we introduce the recipient with the reference liquid that the assay to be completely immersed in it. Because of the Archimedes force (F), which makes the liquid to react over the assay, the balance is unbalanced, and for equilibrating it, being necessary the (m2) mass. Knowing that the Archimedes force (F) is equal to the
62
weigh of the dislocated liquid volume (VL), results that the mass (m2), which is expressed in grams, and reported to the liquid density (L) will express this volume: F = VL L g = G = m2 and VL =
m2 L
[cm3]
The apparent volume of the assay is determined, after the way we prepared the assay, pursuant to the indications from 7.2.1.
Determination principle
Hydrostatic balances photo
Figure 7.3. The hydrostatic balance 7.2.3. Determination on assays of granular material In the case of granular materials, the apparent density is determinate, on the same principle (of the dislocated liquid volume). For being representative, the assay is analyzed after minimal necessary mass criterion, after the maximum dimension
63
of granules, so from many granules. After the drying at constant mass and determination of the mass (m), the assay is settled on a screen with holes dimensions smaller than minimal dimension of the granules and these are immersed in bath with reference liquid where is kept at least four hours. We lift up the screen and we underpin it, to permit the leakage of the waters excess. If the granules are big enough, we wipe them with wet rag, well haggard. In the case of granules with small dimensions (< 7 mm), we wait 30 min. to dry. The determination of the apparent volume is executed for all assays granules, in the way that every granule is introduced in the scale cylinder and we weigh them at the hydrostatic balance. When we use the hydrostatic balance, this will have a net wire flue with a sufficient volume, to get the entire assay. Forasmuch the mass of the flue cant be neglected in the air, at the immersion, and it must be counted when we make the weighing and the determination of the necessary mass for the apparent volume calculus.
64
CHARACTERISTICS OF BULKING MATERIALS

bulk density, holes volume
Bulking materials can form structures which are like some lattice of granules, in layers or piles. If the granules are covered by a binder, it will bind them forming artificial conglomerates (common mortar, concretes). To determinate the characteristics of those lattice, we consider that the bulking material is forming a pile. However we cant form a pile with a perfect geometric form, for which we can calculate the volume with the knowing mathematical formulas, for all the specific characteristics of bulking materials we must calculate the bulk volume, by filing up a volumetric flask. The dimension of the volumetric flask is chose after the maxim dimension of the granules, so that the assays volume to be big enough to represent the entire bulking material (table 8.1.). Tab.8.1. Volumetric flask for g determination Granulator > mm mm mm Vmin flask (dm3) 1 5 10 Interior dimensions (mm) Diameter Height 108 109 185 234 186 233
The setting way in the space of the granules differs after the rate of ramming of the granules in the flask, so because of
65
this we have two conventional states (reproducible) of the material in pile: the refine state, when we considerate the volume of the holes between the granules to be maxim; the ramming state, when we considerate the volume of the holes between the granules to be minim. In order to obtain the refine state, follows the procedure: we introduce the bulking material (Figure 8.1. a, b), in the flask with a ladle lip by free falling, maintaining permanently the height of falling from about 10cm; when the flask is filled up, the material in excess is removed through scraping with a metallic ruler supported by the flask-wall and moved in a beveledmotion (Figure 8.1. c); it is clean the flask on the outside, by material. the bulking
c)
Figure 8.1. Setting up the bulked material In this time we mustnt move or clap the flask, because we risk provoking the ramming of the bulking material. It must be done the scrapping of the excess material from one single move, fast enough, because we mustnt provoke shocks over the flask.
66
In
order
to
obtain
the
ramming
state,
follows
the
procedure: we attach the extension collar at the volumetric flask; we fill the flask with bulking material and we sat it on the vibrating table and we shake it for 3 minutes, completing in this time the volume with material, if is necessary; we remove the extension of the flask and we scrap the excess of material with the metal ruler; we clean the flask, on the outside, by the material. If we dont have a vibrating table, the bulking material is introduced, in the flask, in three rounds of aprox. 1/3 from his height, every round being followed by 50 knocks of the flask by a wood table, by free fall from about 5 cm. 8.1. The bulk density Bulk density is a physical characteristic specific to granular materials (aggregates, powders, etc.) defined by the ratio between the weight and the total volume occupied by a certain amount of material (the volume of voids between granules included).
g =
m Vv
[kg / m3; kg / dm3; g/cm3 ]
[8.1.]
The method contains in determination of the dead weight (m) of the bulking material, which gets into a volumetric flask with a known volume (VV), which is filled after the imposed refine state.
67
Flask volume expresses the volume (Vg) from 8.1 formula. The determination consists in the following operations: it is dried at constant mass an assay of bulking material with a volume bigger then the volume of the flask which will be used; it is weighted the volumetric flask when is empty, clean and dry (m1); it is filled the flask with bulking material and we weight it (m2); it is calculated the dead weight of the bulking material (m), making the difference m2-m1. 8.2. The voids volume The voids volume (Vvoid) expresses the proportion in which the bulk volume, of a bulking material in refine state, is made by the voids between the granules. Vvoid =
Vvoids 100 Vga
[%]
[8.2.]
The principle of the method of determination contains in the estimation of the voids volume between the granules (Vvoids), through the measurement of the reference liquid (VL) which is in a volumetric flask with a known volume (Vga), where we also put the bulking material through the specific procedure of the refine state. Like in the case of the apparent density the bulking material must be prepared to avoid the absorption of the measured liquid by the granules.
68
The bulking material which has a volume bigger then the volume of the flask which will be used is sat on a classifying screen with the dimensions of the voids smaller then the minimal dimension of the granules and inserted in a reference liquid bath for 4 hours. We raise the classifying screen, to let-of the water excess and the granules to dry, for 30 minutes. The determination consists in the following operations: the assay of bulking material is introduced in the volumetric flask in order to obtain the refine state; it is scraped the material excess (with the metallic ruler), we introduce the reference liquid with a measured volume (with a calibrated flask), until we fill the flask with liquid. Another method for determination of the liquid volume if we know the reference liquid density (L), the volumetric flask, filled with the bulking material is weighted before we introduce the liquid (m1) and after we fill it with liquid (m2), the volume of the liquid being calculated with the formula: VL =
m2 m1 L
[8.3.]
The volume of the voids can be estimated, by calculus, if we know the bulk density in refine state (ga) and the apparent density (a) of the bulking material.
Vgol = Vga Va Vga m ga Va a 100 [%] =1 =1 =1 m Vga a ga
[8.4.]
where m is the assay mass, the same for the same assay.
69
STRUCTURAL CHARACTERISTICS
Compactness, humidity, water absorption, porosity, bulking of sand
The structural characteristic refers to the repartition mode of the matter and of the pores in the material apparent volume (in the structures of a material). Because, we cant determinate all of them making measurements in the material structure, one of them are calculated using the technical characteristics.
9.1. Compactness
Compactness (C) represents the degree of a solid matter volume (Vr), filing of the samples apparent volume (Va). C=
Vr 100 Va
[%]
[9.1.]
Because the real volume (Vr) can be calculated only by destroying the materials structure, we can calculate the compactness using the following formula:
m V = a 100 [%] C= r = m Va a
[9.2.]

a = the material apparent density, determinates in accordance with = Laboratory work no. 7; the material density, determinates in accordance
with Laboratory work no.6.

70
9.2. Humidity
Humidity (W) represents a relative quantity of water (A) which is in the material content at a given moment. W= in which: mw = the mass of the humid material, at the given moment; m = the mass of the dry material, at a constant mass; it is weighed immediately the assay (mw); if we cant weigh it the sample must be protected to keep its initial humidity (we introduce it in a polyethylene bag, good tied and closed); it is dried the sample at constant mass and we weigh it (m); it is calculated the humidity with the relation [9.3.].
A mw m = 100 m m
[9.3.]
9.3. Water absorption

Water absorption (al) represents the maximum relative quantity of water (A) which a material may absorb (in the pores which communicates with the exterior, named open pores) at the given conditions (expressed by the characteristic factor l). The materials state when it contains the maximum quantity of water is called saturated state, and the relation of its definition is: al =
m m A x L = sal x L H2O m H2O m
71
100
[9.4.]

msat = the mass of the saturated sample, at the given conditions l; m L = the mass of the dry sample at constant mass; = the density of the reference liquid (if we use
water L = water =1g/cm3). The conditions of saturation are assigned in the table 9.1 and are satisfied as follows: For the saturation from condition I = 1, we put the samples on a tray in which will introduce the reference liquid, in 3 stages at every 24 hours (until of the samples height; until of the samples. We repeat the stages of holding them into the water bath, of weighing and wiping, until the mass that we obtain at the last weigh doesnt differs by previous one with more than 0,05%from it (the material is saturated). For the conditions from I =2 to saturate the samples we introduce them into a vessel with water (at normal temperature), and which is warmed up so that the boiling will start after 30 minutes and will last 3 hours. After the boiling the samples are left into the water to cool up. For the conditions from I =3 to saturate the samples we introduce them in a water bath, which is into a vacuum exicator, from which we extract air until we get a pressure of 20mmHg. When the liberation of air bubbles is stopped, we shut off the vacuum pump and open up the exicator to get again the normal pressure. For the conditions from I =4 to saturate the samples we introduce them in a water bath, which is in a steel recipient in which we pomp air to obtain a pressure of 15 N/mm2.
72
Tab.9.1. Conditions of saturation height; minimal 2 cm over the samples) at every stage we overthrow the samples in the tray. After the last stage, at every 24 hours we take out the samples we wipe up it with Characteristic factor l 1 2 3 4 a humid rag and we weigh, after that we Conditions for saturation pressure Atmospheric Atmospheric 20 mm Hg 15 N/mm
2
introduce them into the bath. temperature 20C Boiling 20C 20C
To determinate the water absorption we must follow the next operations: 1. the sample is dried at constant mass and we weigh (m) 2. than is saturated in the conditions from I = 1 and we weigh (msa1); if the condition s are other (I =24) the sample is saturated after the index in ascending order, we make the weigh for every state of saturation (msal). 3. it is calculated the water absorption using the relation [9.4.] The water absorption represents the highest value of humidity which the material can have.
9.4.
Porosity
9.4.1. Total porosity

The total porosity (Pt) represents the proportion in which the volume of pores (Vp) forms the apparent volume (Va) of the material.
73
Pt =
Vp Va
100
[%]
[9.5.]
Because the pores volume (Vp) can not be measured, the total porosity (Pt) is calculated with the following relation:
m Va Vr Vr Pt = =1 - C 100 [%] = = 1 = 1 m Va Va Va a Vp
[9.6.]
We must observe that total porosity (Pt), calculated like a complementary amount of the compactness, express the volume of pores (Vp) unconcerned of their type (closed or opened). 9.4.2. Apparent porosity (open) The character of the pores has a big influence over the material properties, especially in the case of durability; through the open pore (which communicates with the exterior) can get in the material structure, gasses, liquids, or liquid solutions which can produce phenomenon of expansion corrosion at freezing. Thats why is necessary to determinate the porosity which is formed from the open pores, called open porosity or apparent porosity (Pa). The apparent porosity (Pa) represents the proportion in which the volume of the open pores (Vpo) forms the apparent volume (Va) of the material: Pa = in which: Vpo=the volume of the open pores; Va = the sample apparent volume;
74
Vpd Va
msa m m m L = = sa Va Va L
100
[9.7.]
m L the
= the sample mass at constant mass and dry state; = the density of the reference liquid; of porosity provokes: the absorption of
ma = the mass of the saturated sample with condition I-1; In order to determinate, we apply the phenomenon which phenomenon reference liquid in the open pores. The determination resides in the following succession of operations: the material sample is died at constant mass and we weigh (m); the sample is saturated in the conditions from I =1and we weigh (msa); it is determinates the apparent volume (Va) using the method of hydrostatic balance; it is calculated the apparent porosity with the relation [9.7.]. The apparent porosity can be calculated using the water absorption (a1) and the apparent density (a) of the material, because: Pa =
m m m msa m m 1 = (msa m) = sa = a1 a [%] m VA m Va Va
[9.8.]
9.4.3. Closed porosity Closed porosity represents (Pt) represents the proportion in which the volume of closed pores (Vpc) forms the apparent volume (Va) of the material. Closed porosity is calculated doing the difference between the total porosity (Pt) and the apparent porosity (Pa), because: Pc =
Vpc Va = Vp Vpo Vp Vpd = Pt - Pa = Va Va Va
75
[%]
[9.9]
9.5. Bulking of sand

The hydrophilic materials can bind (through absorption) a layer of water which will act like a solid and will push on the grains between them, when are in bulk state. The phenomenon is more intense if the material is smaller and its specific surface is bigger. The thickness of waters layer grows together with the material humidity until the thickness becomes approximately of 15 m, which corresponds for a humidity of 5 8 %. At a bigger humidity the water in excess stays free, as liquid.
S S S
Sand
particles
which
absorb
water
separated and their volume will be greater than that of the dry sand. Material in this case is considered
The effect of this phenomenon can be measured after the variation of the unit mass of bulk volume, in refine state, at the humidity variation. The operations: it is formed sample with a mass m = 2000 g, from the granular material (sand), dried at constant mass and introduce it into a bowl. it is determinate the bulk density, in refine state (b); in a bowl it is introduced the material and over it we process resides in the following succession of
cast 40 cm3 of water and then well immix until the content gets a homogenous humidity; knowing that the water density (1 g/cm3), the humidity that we obtain becomes: W=
40 g 100 = 2% 2000 g
76
[9.10.]
it is determinate the unit of volume mass of the the operations are repeated, introducing the water in
granular material (gW) for this humidity; stages of 40 cm3, mixing to homogenize the sample and determination the unit of volume mass until the sample is flowed. During this operations we must take care of the sample because if we lose from material, the mass of the bulked material will be modified and the calculated humidity wrong. For every humidity that we obtain we make three parallel determinations of the unit of volume mass (Table 9.2.), and the medium values will be marked in a diagram fig. 9.1. Table 9.2. Bulking of sand
W% No. of test Mbowl [kg] gW [Kg/m3] gW med [Kg/m3] Ii [%]
0 2 4 6 8 10 12
1 2 3 1 2 3 1 2 3 1 2 3 1 2 3 1 2 3 1 2 3
77
Well follow the graphic to see if it indicates any uniform variation; if not we must repeat the last determination of gW.
1600 1500
Density
1400 1300 1200 1100 1000 2 4 6

Humidity
10
For each humidity percent, we calculate the bulking index with the relation: Ii =
ga(100 + W%) gw 100
[%]
[9.11.]
40
Bulking index
30 20 10 0 2 4 6
Humidity
78
10
GRANULARITY
Granularity; Modules of fineness
10.1 Granularity
Granularity represents the relative content of grains with different dimensions which forms a bulked material. The principle of this method resides in sieving of e certain amount of material on a series of sieves with standard holes. The amount of material sieved during one determination, which remained between the two consecutive screens /sieves, from the series of sieves is called sort. The size of the sample which must be sieved depends of the maximum dimension of the grains. Table 10.1 The maximum dimension of the grain [mm] 0.2 or 0.5 1 or 2 7.1 or 5 16 or 10 31.5 or 20 71 or 40 or 60 71 or 63 Determination of granularity is made succession of operations: The sample of material is dried at constant mass and we weigh
79
The samples weight [kg] 0.1 0.5 1 5 15 25 50 following the
(mtot). We form the series of sieves, by attaching a box (at the bottom) and oscillating the entire set we made the sieve. In proportion as we finished the sieving from every sieve from the top, we remove it from the set and we weigh the amount of material which remains in it (m1). To verify if the sieving from a sieve is finished we proceed to: take up the sieve from the set and we brought it over sheet of paper (big enough). sieve it for one minute, and after that we collect the passed bulked material and we weigh (mt). it is weighed the material which is kept by the sieve (mr). it is calculated the percent of sieved material, reported to the total mass of the kept material, before sieving. % passed =
mt 100 mt + mr
[10.1]
It is considered the sieving finished, if the calculated percent is smaller than 1%. If not, the sieving is continued until we fulfill this condition. The material passed through sieve, is introduced and sieve with the next sieve from the set and we continue the sieving with the entire set of sieves. The masses (mi) kept by the sieves, and also the mass (m0) collected in the box from the bottom of the set of sieves, is notated in table 10.2. The bulked material with dimensions smaller than 1 mm, collected in the box from the bottom must be sieved. To have an easily sieve, after homogenization, we collect a sample of
80
material of 100g, which will be sieved with the set of sieves. The sorts which are kept on every sieve are weighed (m0i) and extrapolated to mass (m0) from which they were separated. 100 g m0i m0 .Xi Xi=
m0 m0i 100
from which results [10.2.]
The calculated masses Xi are noted in table 10.2 like masses which were kept on the sieves, if we would sieved the entire quantity (m0) collected in the box from the bottom of the set of sieves. The amount of all the masses which were kept on the sieves and screens must be equal with the sample total mass (mtot), or with a minus error of 5% from (mtot). The error represents the mass of the dust which can be released when we sieved the sample. m = mtot - mi + Xi and m 0,005 mtot In the case when (m) is bigger than 0,5% the process is considered as failed and it is necessary the execution of another sieving, on other sample of corning material. The percentage calculus (Pi) of sieving of the sorts through sieves and screens (I) used in the sets of sieving, are resulted from table 10.2, with the following observations: if the loss (m) wasnt released in atmosphere, we would find it in the mass which passed through the finest sieve (in mass n0,1). the mass remained on the biggest screen, used at sieving (m71), must be null (it mustnt keep any granule) so that the passed mass (n71) to be equal to the total mass of the sample (mtot), and the passing
81
percentage (P71) to be 100%. In table 10.3. is presented a numeric example, with rounded-values to be easier to follow the calculus. Table 10.2. Granularity calculus Sieve (mm) 71 Screens 31,5 16 7,1 3,15 1 Sieves 0,2 0,1 0 Total losses Remained (g) m71 m31 m16 m7 m3 m1 X0,2 X0,1 X0 mI+xi m Sieving to sieve/screen PI(%) nI(g) n71=n31+m31 P71 n31=n16+m16 n16=n7+m7 n7=n3+m2 n3=n1+m1 n1=n0,2+x0,2 n0,2=n0,1+x0,1 n0,1=m+x0 P31 P16 P7 P3 P1 P0,2 P0,1 -
Table 10.3. Numeric examples Screen/Sieve (mm) 71 31,5 16 7,1 3.15 1 0,2 0,1 0 Total Remained (g) 0 2000 1500 1200 500 350 200 150 80 5980
82
Sieving to sieve/screen PI(%) nI(g) 6000 100 4000 2500 1300 800 450 250 100 66,67 41,67 21,67 13,33 7,50 4,17 1.67 -
Losses Granularity is
20 represented
graphically
through the
granularity curve (fig.10.1) The system of coordinates is rectangular, but the abscise scale is semi-logarithmic: until to dimension of 7,1 mm on the ordinate we mark the dimensions logarithm values, and for bigger dimensions, we mark the abscise line at the drawing scale. On the ordinate, we mark the passing percentages, the obtained points being united by lines. It can be observed the development of the granularity curve: On the abscise, between the dimensions of the finest sieve, respectively of the biggest screen, used in sieving; On the ordinate, between the passing percentage through the finest sieve used and the ordinate of 100%. The described representation permits the next
interpretations for the granularity curve. The establishment of the proportion of granules smaller than an well known dimension; (for example the material contains 41,67% granules smaller then 16 mm, 21,67% granules smaller than 7,1 mm ) The establishment of the proportion in which the sorts are forming the corning material (for example the material contains the sort 7,1 16 mm in a proportion of 41,37 21,67=20(%)).
83
Figure 10.1 Granularity curve
10.2. Modules of finesse

Granularity visualization through the granularity curve, permits us to appreciate the repartition of the component sorts, after the appreciation of the graphic curve. So, in the Figure 10.2. the graphic (1), more concave than graphic (2), will indicate a content proportional smaller for the smaller sorts than the coarse sorts; we can say that the granularity (1) more poor in finest parts or that the granularity (2) is wealthier in finest parts. To express the valor formula for the granularity curve, we calculate the modulus of finesse: m=
S S = 100 lg 2 30,1
[10.3.]
in which S = the surface, from the graphic, closed by the granularity curve, the vertical through minimal abscise (lg0,1) and the horizontal through the ordinate of 100% . In Figure 10.2 is represented the surface (S) which
84
corresponds to the granularity expressed in the graphic (2). Surface (S) is determinate doing the amount of the trapezes surface, which are formed by the segments from the graphic having as bases the differences (100 pi%) and the height equal with the distances between the segments abscises, and this impose to draw up the graphic at the following scales : Ordinate scale to have 10 cm The distance between the abscise 0,1 mm and 1 mm (in logarithmic scale) to have 10 cm; The remnant of the abscise will follow the graphic scale from the segment 0,1 1mm. Well observe that a graphic with a bigger concavity suppose a less number of finest parts, a bigger surface and implicit the modulus of finesse will have a bigger value.
The Fineness Modulus
85
Figure 10.2 Calculus of finesse modulus
86
MIXTURES OF BULKED MATERIALS

As a general rule, the bulked materials must fulfill conditions of granularity, expressed through the way in which the curve is bordered in the domain of granularity, defined through maximal percentage (Cmax) and minimal (Cmin) which corresponds to the sorts dimensions. In the Table 11.1.and the Fig.11.1 is represented one of these domains. The granularity utilizations permits to solve three types of problems, which will be explained giving numerical examples. Table 11.1. The imposed domain of granularity Curve Cmax Cmin Cmed Passes (% from mass) through screen/sieve (mm) 0,2 10 1 5,5 1 32 10 21 3,15 47 22 34,5 7,1 62 40 51 16 80 60 70 31,5 100 95 100 71 100 100 100
11.1. The achievement of a mixed material with an imposed granularity

We must form a quantity of 2000 kg of bulked material formed by the sorts: 0 3,15 / 3,15 7,1 / 7,1 16 / 16 31,5 mm which must have a granularity contented in the domain from the table 11.1. Like in every situation in which we must respect a domain, the optimal value is the dominium medium value, results that the
87
optimal granularity which we have to respect is expressed by the medium domain curve (Cmed). In first stage, after the granularity curve (Cmed), we calculate the necessary proportions of sorts, using the differences passing percentages, corresponding with the sorts limits of definition. In the second stage, using the mixture proportions, we calculate the dosage of sorts, which are necessary to realize the total mixture of 2000kg (Table 11.2. col. 03). Table 11.2. Calculus of proportions and the sorts dosage Sort 0 3,15 3,15 7,1 7,1 16 16 31,5 TOTAL Mixture proportions [%] 34,5 0,0 = 34,5 51,0 34,5 = 16,5 70,0 51,0 = 19,0 100 70,0 = 30,0 100 Doses of mixtures [Kg] 0,345 x 2000 = 690 0,165 x 2000 = 330 0,190 x 2000 = 380 0,300 x 2000 = 600 2000
Figure 11.1 Granularity domain

88
11.2.
Determination
of
granularity
obtained
by
mixtures of real sorts

At the verification of the available sorts, the resulted granularities for each sort are those from table 11.3. We must find out the granularity of the total aggregate, resulted from the mixtures of the sorts at the established proportions from & 11.2.1. Table 11.3. Granularity of the sorts Transition (% percentage from mass) SORT 0,2 0 3,15 3,15 7,1 7,1 16 16 31,5 12,5 2,2 0,9 0,2 1 60,6 4,1 2,9 0,3 through screen/sieve (mm) 3,15 93,4 6,3 6,4 0,5 7,1 100 95,4 7,4 0,7 16 100 100 97,3 3,6 31,5 100 100 100 96,7 71 (100) (100) (100) 100
To solve the problem we must calculate the proportions which are introduced by every sort in the total aggregate and this is made doing the multiplication between the mixture proportion and the sorts percentage of granularity (table 11.4.). Example: the sort 0 3,15mm will introduce in the total aggregate:
3,45 12,5% = 4,31% aggregate which has the dimensions 100
smaller than 0,2mm; the sort 7,1 16,5mm will introduce in the total aggregate:
89
19,0% 97,3% = 18,49 % 100
aggregate
which
has
the
dimensions smaller than 16mm. It is noticed that the necessity of introducing the transition percentage of 100% for dimensions bigger than the maximum dimension of every sort, operation which doesnt modify the granularities of the sorts because the sort is smaller than the respective dimension. The real granularity of the mixture is calculated making the amount of the proportions each sort, like in the table 11.4. Table 11.4. The mixture real granularity Transition (% percentage from mass) SORT 0,2
0 3,15 3,15 7,1 7,1 16 16 31,5 TOTAL 4,31 0,36 0,17 0.06 4,90
through screen/sieve (mm) 1

20,91 0,68 0,55 0,09 22,23
3,15
32,22 1,04 1,22 0,15 34,63
7,1
34,50 15,74 1,41 0,21 51,86
16
34,50 16,50 18,49 1,08 70,57
31,5
34,50 16,50 19,00 29,01 99,01
71
34,5 16,5 19,00 30,00 100,00
Laying out the curve of the resulted granularity (Crez) in Figure 11.1., we can observe that it doesnt match exactly over the curve we need (Cmed) but is laying into the imposed domain. 11.3. Optimal mixtures for the bulked materials In practice at a given moment we must mix different bulked materials and to obtain the maximum grade of utilization, with a granularity closed like value to the one we want. We have to bulked materials
90
(A
and
B)
with
the
granularities from the tab. 11.5 and we have to find out the characteristics of each bulked material so that, after a integral use, to obtain a mixture with a necessary granularity (N). Table 11.5. The granularities of the material and mixtures Transition (% from mass) Material 0,2 A B N 10 1 5,5 through screen/sieve (mm) 1 30 10 21 3,15 40 20 34,5 7,1 60 30 51 16 80 70 70 31,5 100 95 100 71 100 100 100 420 326 382 Amount
The proportion calculus can be made in two methods: The amount method; The method of the granularitys index.
The amount method To solve it using the amount method we must follow the following steps: We calculate the percentage amounts of transition for the two sources of bulked materials and for the necessary mixtures. This amounts will be noted SA, SB and SN: Ex: SA = 10 + 30 + 40 + 60 + 80 + 100 + 100 = 420 Notations: 1. p the proportion from material A which is necessary in the mixture; 2. q - the proportion from material B which is necessary in the mixture; 3. ni the percentage of transition, resulted from the mixture of the two materials in the proportions p and q.
91
Could be written the following relations: p+q=1 ni = pai + qbi = pai + (1 - p)bi = p(ai - bi) + bi SN =ni = p(ai - bi) + bi = p(SA - SB) + SB p=
SN SB X 100 S A SB
[%]
and
q=
S A SN 100 [%] S A SB
For granularities from the table 11.5. results:
p=
382 326 100% 420 326
and
q=
420 382 100 % 420 326
Figure 11.2 The amount method for two components The amount method of two components can be realized graphic too, using a mixture diagram (fig.11.2) with the following stages: we mark on the corresponded coordinates of the materials A and B the amounts values; knowing that the calculus relation of the amount SN represents linear function, the two ordinates are united with a line. we mark the ordinate which corresponds for the amount Sn.
92
The corresponding abscise for the intersection of the lines, express the mixture proportions for this two bulked materials. The method of the granularitys index The method of the granularity index operates with the remnant ordinates from the screens/sieves. The formula for the granularity index (Ii) is:
IA =
sieves.
1 (100 ai ) 100
where ai represents the transition percentage through screens or
For the granularities from the table 11.5.the index is:
IA =
1 (100 10) + (100 30) + (100 40) + (100 60) + (100 80) + (100 100) + (100 100) 100
1 (100 1) + (100 10) + (100 20) + (100 30) + (100 70) + (100 95) + (100 100) 100 1 IN = (1005,5) +(10021) +(10034,5) +(10051) +(10070) +(100100) +(100100) 100 IB =
Using a similar reasoning with the one we applied in the amount method, results:
I N = pI A + qI B = pI A + (1 q) I B = p ( I A I B ) + I B and, respectively
p= IN IB 100[%] I A IB
and
q=
IA IN 100[%] I A IB
There are calculated the mixtures proportions, we make the verification of the total aggregate, after the method described at point 11.2 considering that the mixture is realized between two sorts (Table 11.6.).
93
Table 11.6. Material A B Crez Transition (% from mass) through screen/sieve (mm) 0,2 5,96 0,40 6,36 1 17,87 4,04 21,91 3,15 23,83 8,09 31,91 7,1 35,74 12,13 47,87 16 47,66 28,30 75,96 31,5 59,57 38,41 97,98 71 59,57 40,43 100
Will be observed that the resulted granularity curve, doesnt match with the necessary curve (N), but is coiling up on it.
Figure 11.3 Optimal mixture graphs
94
MECHANICAL TESTS (I)

Compression Tests
This
subchapter
has
like
purpose
the
practical
demonstration of the factors which are influencing the material resistance to compression: The test rod form (cube, prism, cylinder); The size of the test rod (cube with the edge of 100mm and 200mm); Rise rate of the force intensity (high speed and slow speed); The friction from the interface between the test rod and the pan; The attempts will be executed by series of concrete test samples, with different forms and dimensions, but prepared and kept in the same conditions. The test samples will be marked and measured with a precision of 1mm. We calculate the average values of the edges and the initial diameters of the rupture sections. We calculate the characteristically section for the attempt (A0). The values of the attempt parameters, the maximum forces indicated by the press and the resulted resistances will be registered in Table 12.1., corresponding to the hypothesis oh the attempts which were programmed. The compression resistance is calculated: RC =
Fmax A0
[N/mm2]
95
[12.1.]
in which: Fmax = the maxim force registered by the press (N); A0 = the characteristically initial section of the test sample (mm2) The characteristically section (A0), on which is distributed the force of compression is calculated: For cube and prism For cylinders A0 = a b A0 = [12.2.] [12.3.]
d
4
Figure 12.1 The attempt of the tests at compression

96
The attempt speed (v) is calculated:
v=
Fmax A0 t
[12.4.]
in which t = presss pull-in time, until the test rod is break. After the cracks rising (failure) the sample (cube, cylinder, prism) will failed, as follows:
Figure 12.2 The samples shapes after the tests at compression
97
Results Table
V [N/mm2s] No crt a1 a2 a3 a4 b1 b2 b3 (d1) (d2) (d3) (d4) (d5) (d6) b4 Fmax [N] t [s] Rc [N/mm2] A0 [mm2] Slides (diameters) mm a (d) [mm] b [mm]
0 1 2 3
Aver age
6 7 8 9 10 Cube with the slide of 100 mm
11
12
13
14
15
Cube with the slide of 200 mm 1 2 3

Aver age
Prism with the slide of the base of 100mm 1 2 3

Aver age
Cylinder with the diameter by 100 mm 1 2 3

Aver age
Cube with the slide of 100mm tried at high speed 1 2 3

Aver age
Cube with the slide of 100mm tried at reduced speed 1 2 3

Aver age
98
The resistance medium values are compared with the results from the Table 12.1 and are mentioned the conclusions, as follows: Cube with the side of 100 mm and 200 mm
Cube with the side of 100 mm and a prism with a square base and the slide of 100mm
Cube with the side of 100 mm and a cylinder with the base diameter of 100mm
Prism with the side of the base of 100 mm and cylinder with the base diameter of 100 mm
Cube with the side of 100 mm
Cube with the side of 100 mm tried at different speeds
Cube with the side of 100 mm, prism with the base of 100 mm, cylinder with the base of 100 mm
99
MECHANICAL TESTS (II)

The Flexural Test The Cleaving Extensions Test
13.1. Flexural tensile resistance
The attempt from flexural tensile, is effectuated on prismatic tests rod which have a square section. The prism is settled on two supports at the distance (l) between them, called opening and the force pres straight at the half of the opening (Fig.13.1).
Figure 13.1 The test from flexural tensile

100
Flexural tensile resistance (Rti) is calculated with:

R ft = 3 Fmax l 2 b h2
[N/mm2]
[13.1.]
in which: Fmax = the maximum force registered until the rupture [N]; l = the distance between presses supports [mm]; b = the horizontal dimension of the prism section [mm]; h = the vertical dimension of the prism section [mm].
Figure 13.2 The samples shape after the flexural tensile test Table 13.1. The test through flexural extension Dimensions [mm] No. crt. b1 b2 b3 b4 h1 h2 h3 h4 1 2 3 Medium resistance Fmax [N] Averages Rft b h [N/mm2] [mm] [mm]
101
13.2. The resistance from cleaving extension

The tests through cleaving extension are effectuated on cylindrical test rods which are settled on generating lines (Fig.13.2.) and have between them and the press supports a band of board, PFL, for uniformly application of the action on the generating lines and to reduce the friction between test rod and the supports.
Figure 13.3 The test from cleaving extension The supports action will be transmitted to the test rods like a charge uniform distributed on the generating lines. The bending stress from the vertical will go to extension stress perpendicular on the plan formed by that two generating lines and which will receive the force, and the test rod will cleave after it. The resistance to rupture through cleaving is calculated with:
R ce = 2 Fmax A0
[N/mm2]
[13.2.]
in which:
102
= constant 3,141592;
A0= d h = the surface of the cleaving plan.
Figure 13.4 The samples shape after cleaving extension test Table 13.1. The test through cleaving extension Dimensions [mm] N o cr d1 d2 d3 h1 h2 t 1 2 3 Medium resistance
103
Fmax [N]
Averages
[mm] [mm]
[mm2]
A0
[N/mm2]
Rce
Bibliography
1. Bob Corneliu, Velica Paraschiva 2. Groll L. .a. - Materiale de construcii, Editura Didactic i Pedagogic, Bucureti, 1976 - Materiale de construcii; bazele fizicochimice ale studiului materialelor de construcii, editura ROTAPRINT, I.P. lai 1985 - Caiet pentru lucrri la disciplina Materiale de construcii, editura ROTAPRINT, I.P. lai 1985 - Proprietile betonului, Editura Tehnic, Bucureti, 1979 - Chimia fizic a silicailor tehnici, Editura Tehnic, Bucureti, 1968 - Materiale de construcii, Editura Tehnic - Bazele tehnologiei lianilor, Editura Tehnica, Bucureti, 1975 - Durabilitatea betonului, Editura Tehnic, Bucureti, 1982
3. Groll L., Hrhui I. .a. 4. Neville A. M. 5. Solacolu S. 6. Steopoe Al. 7. Teoreanu I. 8. Teoreanu I. .a.
9. M. Budescu, ncercarea materialelor, vol. 1 i 2, Editura I. Bliuc, Tehnic, Bucureti, 1982 A. Caracostea .a. 10. Standarde i normative n vigoare
104

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Building Materials - Chemical and Structural Properties

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