TESTING PROGRAM OF LIGHTWEIGHT CONCRETE In order to study the behavior of lightweight concrete, normal concrete testing was done

to determine the material and structural properties of each type of lightweight concrete and how will these properties differ according to a different type of mixture and its composition. Once concrete has hardened it can be subjected to a wide range of tests to prove its ability to perform as planned or to discover its characteristics. For new concrete this usually involves casting specimens from fresh concrete and testing them for various properties as the concrete matures. 3.2 COMPRESSIVE STRENGTH Compressive strength is the primary physical property of concrete (others are generally defined from it), and is the one most used in design. It is one of the fundamental properties used for quality control for lightweight concrete. Compressive strength may be defined as the measured maximum resistance of a concrete specimen to axial loading. It is found by measuring the highest compression stress that a test cylinder or cube will support. There are three type of test that can be use to determine compressive strength; cube, cylinder, or prism test. The concrete cube test' is the most familiar test and is used as the standard method of measuring compressive strength for quality control purposes (Neville, 1994). Please refer appendix 1 for details. APPENDIX 1 CUBE TEST Objective: -To determine the compressive strength of a lightweight concrete sample. Apparatus: - Standard cube size 100mm^3 - Steel rod measured 25x25 mm^2 General note: - Compressive strength will be determined at the age of 7 and 28 days. - 3 samples for each age will be prepare - Average result will be taken Procedure: 1. Prepare the mould; apply lubricant oil in a thin layer to the inner surface of the mould to prevent any bonding reaction between the mould and the sample (A.M Neville, 1994) 2. Overfill each mould with sample in three layers (Standard Method: BS 1881: Part 3: 1970) 3. Fill 1/3 of the mould with sample. This would be the first layer 4. Compact sample with at least 35 strokes using steel rod. Compaction should be done continuously 5. Fill 2/3 of the mould; second layer. Repeat step 4. 6. Continue with the third layer and repeat the same compaction step 7. After compaction has been completed, smooth off by drawing the flat side of the trowel (with the leading edge slightly raised) once across the top of each cube 8. Cut the mortar off flush with the top of the mould by drawing the edge of the trowel (held perpendicular to the mould) with a sawing motion over the mould 9. Tag the specimen, giving party number, and specimen identification 10. Store cube in moist closet (temperature; 18C - 24C) for 24 hours 11. Open mould and preserved cube in water (temperature; 19C - 21C) BS 1881; Part 3: 1970 12. Test cube for 7 days and 28 days accordingly 13. Placed cube on the testing machine: cube position should be perpendicular with its pouring position ( A.M. Neville, 1994) 14. Without using any capping material, apply an initial load ( at any convenient

rate) up to one-half of the expected maximum load (G.E. Troxell, 1956) 15. Loading should be increased at a uniform increment; 15 MPa/min (2200 Psi/min) BS 1881: Part 4: 1970. Since that certain sample are expected to have lower compressive strength, some adjustment will be made; loading will be increased with the increment of 5% of the expected maximum compressive strength 16. When it comes nearer to the expected maximum strength, loading increment will be lessen little by little ( A.M. Neville, 1994)

WATER ABSORPTION These properties are particularly important in concrete, as well as being important for durability. (J.H Bungey, 1996). It can be used to predict concrete durability to resist corrosion. Absorption capacity is a measure of the porosity of an aggregates; it is also used as a correlation factor in determination of free moisture by oven-drying method (G.E Troxell, 1956). The absorption capacity is determined by finding the weight of surface-dry sample after it has been soaked for 24 hr and again finding the weight after the sample has been dried in an oven; the difference in weight, expressed as a percentage of the dry sample weight, is the absorption capacity (G.E Troxell, 1956). Absorption capacity can be determine using BS absorption test. The test is intended as a durability quality control check and the specified age is 28-32 days (S.G Millard). Test procedure as been describe by BS 1881: Part 122 is as listed in the appendix 2. APPENDIX 2 BS Absorption Test Objective: - To determine the absorption capacity of lightweight concrete sample Apparatus: - A balance - An air tight vessel - A container of water - An oven General note: - Test will be carried out on 75 mm diameter ( 3mm) specimens - Specified test age is 28-32 days. - 3 samples for each age will be prepare - Average result will be taken Procedure: 1. Dry the specimens in an oven at 105C 5C for 72 2 hr. 2. Cooled specimen for 24 1/2 hr in an airtight vessel 3. Weight the specimen 4. Immersed horizontally in the tank of water at 20C 1C with 25 5 mm water over the top surface 5. Immersed for 30 minutes 6. Removed specimen 7. Shaken and dried quickly with a cloth to remove free surface water 8. Weight the specimen again Calculation: Absorption capacity can be calculate using the formula given below: (Result will be expressed to the nearest 0.1%) Absorption Capacity = Increased In Weight (kg) 100% Weight of Dry Specimen (kg)

DENSITY The density of both fresh and hardened concrete is of interest to the parties involved for numerous reasons including its effect on durability, strength and resistance to permeability. Hardened concrete density is determined either by simple dimensional checks, followed by weighing and calculation or by weight in air/water buoyancy methods (ELE International, 1993). To determine the density of lightweight concrete sample, the simple method is preferred as listed in the appendix 3. APPENDIX 3 Simple Density Test. Objective: - To determine the density of hardened lightweight concrete sample. Apparatus: - Weighing scale - One cube sample General Note: - For more economic sample are to be taken from compression test sample; before doing the test - Three sample are going to be used and average result will be taken Procedures: 1. Weight sample using weighing scale 2. Get the average weight of those 3 samples 3. Calculate the density using the formula given below (Since a standard mould; 100 x 100 x 100 mm is used, volume of each sample can be determined according to this dimensional) Density = Average Weight Of Samples (kg) Volume of Sample (m2) Chemical Shrinkage Chemical shrinkage, the volume reduction associated with the reaction between cement and water in hydrating cement paste, was assessed using the method described by Geiker [11], which is similar to that recently employed by Tazawa et al. [12]. While the latter authors concluded that chemical shrinkage is directly proportional to degree of hydration, they further stated that chemical shrinkage is not directly related to autogenous or self-desiccation shrinkage. Conversely, Hua et al. [13,14] have recently established a model which successfully directly relates autogenous shrinkage to the capillary pressures induced by chemical shrinkage. Thus, measurements of chemical shrinkage may serve a dual purpose, quantification of hydration rates and indication of system susceptibility to selfdesiccation shrinkage. To assess chemical shrinkage, a known mass of cement paste (typically 10 g) was placed in the bottom of a small glass jar, with a diameter of 2.5 cm and a height of about 6 cm. After covering the cement paste with about 1 ml of water, the remainder of the jar was filled with an hydraulic oil. The jar was then sealed with a rubber stopper encasing a pipette graduated in 0.01 ml increments. The jar was then placed in a constant temperature water bath ( T = 25 C ) and the oil level monitored to the nearest 0.0025 ml over time. A control sample using only cement powder and oil (no water) was used to correct for minor room temperature fluctuations. By normalizing the change in volume by the mass of cement in the sample, the chemical shrinkage per gram of initial cement (ml/g cement) could be determined. In all cases, two specimens were run for each w/c ratio and cement, with the average result being reported. Chemical Shrinkage Another convenient method for monitoring hydration kinetics is via the measurement of chemical shrinkage [14]. Because the cement hydration products occupy less volume than the starting materials (cement and water), a hydrating cement paste will imbibe water in direct proportion to its ongoing hydration [14,15]. This is true except for low w/c ratio pastes (< about 0.4) where the depercolation of the capillary porosity may dramatically reduce the permeability of the cement paste and limit its imbibition rate below that required to maintain saturation during the

continuing hydration [9,14]. While no standard ASTM method exists for the measurement of chemical shrinkage, a draft standard for this test is currently being considered by ASTM C01.31 subcommittee on Volume Change. The maximum expanded uncertainty [16] in the calculated chemical shrinkage has been previously estimated [9], to be 0.001 mL/(g of cement), assuming a coverage factor of 2 [16]. Knowing the volume stoichiometry of all ongoing hydration reactions, it is straightforward to compute chemical shrinkage in the VCCTL cement hydration model. Figures 7 and 8 provide comparisons of model and experimental results for cements 135 and 141, respectively. Excellent agreement is observed between model and experimental results. The deviation between model and experimental results for cement 135 at later ages (> 40 h) is likely due to the depercolation of the capillary porosity mentioned above. Chemical shrinkage measurements appear to provide a rapid and convenient method for assessing early hydration rates and may provide a simple means for evaluating cement cracking susceptibility [17].

Figure 7: Experimentally measured (circles) and model-predicted chemical shrinkage for CCRL cement 135 (w/c=0.3, hydrated at 25 C).

Figure 8: Experimentally measured (circles) and model-predicted chemical shrinkage for CCRL cement 141 (w/c=0.4, hydrated at 20 C). Early-Age Cracking 1 2 By Matthew DAmbrosia and Nathaniel Mohler Early-age cracking can be a significant problem in concrete. Volume changes in concrete will drive tensile stress development when they are restrained. Cracks can develop when the tensile stress exceeds the tensile strength, which is generally only 10% of the compressive strength. At early ages, this strength is still developing while stresses are generated by volume changes. Controlling the variables that affect volume change can minimize high stresses and cracking. Mechanisms of Early-Age Volume Change The volume of concrete begins to change shortly after it is cast. Early volume changes, within 24 hours, can influence tensile stress and crack formation in hardened concrete. Chemical Shrinkage Chemical shrinkage occurs due to the reduction in absolute volume of solids and liquids in the hydrating paste. Chemical shrinkage continues to occur as long as cement hydrates. After initial set, the paste resists deformation, causing the formation of voids in the microstructure. Autogenous Shrinkage Autogenous shrinkage is the dimensional change of cement paste, mortar, or concrete caused by chemical shrinkage (Figure 1). When internal relative humidity is reduced below a given threshold (i.e., extra water is not available), self-desiccation of the paste occurs, resulting in a uniform reduction of volume.

Figure 1 Chemical shrinkage and autogenous shrinkage volume changes of fresh concrete. Not to scale. Creep Creep is the time-dependent deformation of concrete under sustained load. During early age, concrete creep is generally as much as 3-5 times higher than for mature concrete. Early load application due to construction forces or prestressing operations can therefore have a significant impact on total deformation. Furthermore, the magnitude of creep in tension is greater than in compression, and early tensile creep can be relied upon as a stress relaxation mechanism. Creep is influenced by drying or selfdessication at early age, and this synergy is often referred to as the Pickett Effect, after Gerald Pickett, a PCA researcher who discovered the phenomena in the 1940s (Pickett 1947). Swelling Concrete, mortar, and cement paste will sometimes swell when sealed or in the presence of external water. Swelling is generally caused by pore pressure, but can be accentuated by the formation of some expansive hydration products. The swelling is not significant, between 50-100 millionths at early ages; therefore, we will not be discussing swelling further. Thermal Expansion As cement hydrates, the reaction provides a significant amount of heat. In large elements, this heat is trapped and can induce significant expansion. When thermal changes are superimposed upon autogenous shrinkage at early age, cracking can occur. In particular, differential thermal stress can occur due to rapid cooling of massive concrete elements.

Testing of Early-Age Volume Changes Chemical shrinkage test Volume change due to chemical shrinkage can be estimated from the hydrated cement phases and their crystal densities or it can be determined by physical test. The physical test places a measured amount of lime-saturated water in an open pipet over a known amount of cement paste inside a closed container. The change in water level within the pipet indicates the change in volume due to chemical shrinkage (Figure 2).

Figure 2 Test for chemical shrinkage of cement paste showing flask for cement paste and pipet for absorbed water measurement. ASTM C157 - Modified for early age shrinkage The standard drying shrinkage test for concrete can be modified to capture early age volume change by elimination of the curing period (usually 7-28 days) and beginning measurements as early as possible. Prisms may also be sealed after casting to provide an estimate of autogenous shrinkage. Surfaces should be sealed as quickly as possible to eliminate loss of moisture. It should be emphasized that autogenous shrinkage depends on temperature history (maturity) and will be different in a laboratory prism when compared to a larger concrete member in service under variable ambient temperatures. As with drying shrinkage measurements, the test result will not represent the actual shrinkage in the structure. ASTM C1581 Restrained Ring Shrinkage The restrained ring shrinkage test consists of a concrete ring specimen 150 mm (6 in.) tall, 13 mm (0.5 in.) thick and 330 mm (13 in.) diameter that is cast surrounding an instrumented steel ring (Figure 3). The steel ring prevents the concrete from shrinking from the time that the concrete is first cast. Shrinkage stresses continue to grow as the concrete passes from initial set to final set and beyond. Tensile creep relaxation alleviates stress development and is considered beneficial at early age.The instrumented ring uses strain sensors to monitor the development of stress. If the shrinkage in the concrete is significant, the stresses will eventually cause cracking. The strain sensors provide an indicator of the cracking time, which is used to compare the cracking tendency between different concrete mixtures.

Figure 3 Restrained ring shrinkage test setup. (Courtesy of CTLGroup)

ASTM C512 - Compressive Creep The standard creep test consists of a frame and hydraulic loading system to apply constant stress to 150X300 mm (6x12 in.) cylindrical specimens (Figure 4). Deformation is monitored periodically over time and compard to compansion unloaded specimens to obtain the creep strain of the concrete, which can then be used to calculate the creep compliance, or specific creep of the material. Tests are typically started at 7 or 28 days of age, but this test can be modified for early age by starting the test as early as 24 hours. Sealed tests are used to evaluate basic creep and unsealed tests incorporate the Pickett Effect, or drying creep.

Figure 4 Standard creep test frames. (Courtesy of CTLGroup) Mitigating Early-Age Cracking Optimization of aggregates to reduce total cementitious content Since volume changes are more a function of the cement paste, rather than the more volume-stable aggregates, reducing the overall cementitious content is the best way to mitigate early-age volume changes. Typical concrete mixtures have gap-graded aggregates that leave significant void space for cement paste to fill. By optimizing the aggregate gradation across the entire spectrum, as opposed to the coarse and fine aggregates individually, the amount of paste required to surround each aggregate particle and fill the void space is minimized (Figure 5); thereby minimizing the effects of early-age volume change of the paste.

Figure 5 A comparison of void space with different aggregate gradations.

Minimum w/cm ratio Autogenous shrinkage increases with a decrease in water to cementitious materials ratio (w/cm). Concrete mixtures with a w/cm of 0.30 can experience autogenous shrinkage upwards of half of the normal drying shrinkage. Using the highest w/cm that still provides adequate strength and durability can reduce the impact of autogenous shrinkage. Internal curing Internal curing is a method by which water is encapsulated within a concrete mixture for continued release during the hydration process. Typical internal curing materials include high absorption lightweight aggregate particles and super-absorbent polymers. The self-dessication of the paste draws the water out of these particles to continue the hydration of the cement particles. This is particularly helpful in mitigating autogenous shrinkage of concrete mixtures with very low w/cm (0.30 or less). Shrinkage-reducing admixtures Shrinkage-reducing admixtures (SRAs) are typically used as mitigation of cracking and curling caused by drying shrinkage; however, SRAs can be utilized to mitigate autogenous shrinkage as well. The SRA, typically propylene glycol or polyoxyalkylene alkyl ether based, alters the surface tension of the pore water and reduces the stresses developed during desiccation, whether self-induced or by evaporation. Concreting procedures Several concreting procedures can be used to minimize early-age volume changes. When autogenous shrinkage is a concern, the use of moist curing methods will help mitigate self-desiccation near the concrete surface. The use of a well-developed thermal control plan will mitigate the effects of thermalbased volume changes. References Kosmatka, Steven H.; Kerkhoff, Beatrix; and Panarese, William C.; Design and Control of Concrete Mixtures, EB001, 14th edition, Portland Cement Association, Skokie, Illinois, USA, 2002, 358 pages. Pickett, Gerald, The Effect of Change in Moisture Content on the Creep of Concrete Under a Sustained Load, Research Department Bulletin RX020, Portland Cement Association, 1947.

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X-Ray powder diffraction X-ray Powder Diffraction (XRD) Barbara L Dutrow, Louisiana State University , Christine M. Clark, Eastern Michigan University What is X-ray Powder Diffraction (XRD) X-ray powder diffraction (XRD) is a rapid analytical technique primarily used for phase identification of a crystalline material and can provide information on unit cell dimensions. The analyzed material is finely ground, homogenized, and average bulk composition is determined. Fundamental Principles of X-ray Powder Diffraction (XRD) Max von Laue, in 1912, discovered that crystalline substances act as three-dimensional diffraction gratings for X-ray wavelengths similar to the spacing of planes in a crystal lattice. X-ray diffraction is now a common technique for the study of crystal structures and atomic spacing. X-ray diffraction is based on constructive interference of monochromatic X-rays and a crystalline sample. These X-rays are generated by a cathode ray tube, filtered to produce monochromatic radiation, collimated to concentrate, and directed toward the sample. The interaction of the incident rays with the sample produces constructive interference (and a diffracted ray) when conditions satisfy Bragg's Law (n=2d sin ). This law relates the wavelength of electromagnetic radiation to the diffraction angle and the lattice spacing in a crystalline sample. These diffracted X-rays are then detected, processed and counted. By scanning the sample through a range of 2angles, all possible diffraction directions of the lattice should be attained due to the random orientation of the powdered material. Conversion of the diffraction peaks to d-spacings allows identification of the mineral because each mineral has a set of unique d-spacings. Typically, this is achieved by comparison of dspacings with standard reference patterns. All diffraction methods are based on generation of X-rays in an X-ray tube. These X-rays are directed at the sample, and the diffracted rays are collected. A key component of all diffraction is the angle between the incident and diffracted rays. Powder and single crystal diffraction vary in instrumentation beyond this. X-ray Powder Diffraction (XRD) Instrumentation - How Does It Work? X-ray diffractometers consist of three basic elements: an X-ray tube, a sample holder, and an X-ray detector.

Show caption X-rays are generated in a cathode ray tube by heating a filament to produce electrons, accelerating the electrons toward a target by applying a voltage, and bombarding the target material with electrons. When electrons have sufficient energy to dislodge inner shell electrons of the target material, characteristic X-ray spectra are produced. These spectra consist of several components, the most common being K and K. K consists, in part, of K1 and K2. K1 has a slightly shorter wavelength and twice the intensity as K 2. The specific wavelengths are characteristic of the target material (Cu, Fe, Mo, Cr). Filtering, by foils or crystal monochrometers, is required to produce monochromatic X-rays needed for diffraction. K1and K2 are sufficiently close in wavelength such that a weighted average of the two is used. Copper is the most common target material for single-crystal diffraction, with CuK radiation = 1.5418. These X-rays are collimated and directed onto the sample. As the sample and detector are rotated, the intensity of the reflected X-rays is recorded. When the geometry of the incident X-rays impinging the sample satisfies the Bragg Equation, constructive interference occurs and a peak in intensity occurs. A detector records and processes this X-ray signal and converts the signal to a count rate which is then output to a device such as a printer or computer monitor.

Show caption The geometry of an X-ray diffractometer is such that the sample rotates in the path of the collimated X-ray beam at an angle while the X-ray detector is mounted on an arm to collect the diffracted X-rays and rotates at an angle of 2. The instrument used to maintain the angle and rotate the sample is termed a goniometer. For typical powder patterns, data is collected at 2from ~5 to 70, angles that are preset in the X-ray scan. Applications

X-ray powder diffraction is most widely used for the identification of unknown crystalline materials (e.g. minerals, inorganic compounds). Determination of unknown solids is critical to studies in geology, environmental science, material science, engineering and biology. Other applications include: characterization of crystalline materials identification of fine-grained minerals such as clays and mixed layer clays that are difficult to determine optically determination of unit cell dimensions measurement of sample purity With specialized techniques, XRD can be used to: determine crystal structures using Rietveld refinement determine of modal amounts of minerals (quantitative analysis) characterize thin films samples by: o determining lattice mismatch between film and substrate and o o o to inferring stress and strain determining dislocation density and quality of the film by rocking curve measurements measuring superlattices in multilayered epitaxial structures determining the thickness, roughness and density of the film using glancing incidence X-ray reflectivity measurements make textural measurements, such as the orientation of grains, in a polycrystalline sample

Strengths and Limitations of X-ray Powder Diffraction (XRD)? Strengths Powerful and rapid (< 20 min) technique for identification of an unknown mineral In most cases, it provides an unambiguous mineral determination Minimal sample preparation is required XRD units are widely available Data interpretation is relatively straight forward Limitations Homogeneous and single phase material is best for identification of an unknown Must have access to a standard reference file of inorganic compounds (d-spacings, hkls) Requires tenths of a gram of material which must be ground into a powder For mixed materials, detection limit is ~ 2% of sample For unit cell determinations, indexing of patterns for nonisometric crystal systems is complicated

Peak overlay may occur and worsens for high angle 'reflections'

Scanning Electron Microscopy (SEM) Susan Swapp, University of Wyoming What is Scanning Electron Microscopy (SEM)

A typical SEM instrument, showing the electron column, sample chamber, EDS detector, electronics console, and visual display monitors. The scanning electron microscope (SEM) uses a focused beam of high-energy electrons to generate a variety of signals at the surface of solid specimens. The signals that derive fromelectron-sample interactions reveal information about the sample including external morphology (texture), chemical composition, and crystalline structure and orientation of materials making up the sample. In most applications, data are collected over a selected area of the surface of the sample, and a 2-dimensional image is generated that displays spatial variations in these properties. Areas ranging from approximately 1 cm to 5 microns in width can be imaged in a scanning mode using conventional SEM techniques (magnification ranging from 20X to approximately 30,000X, spatial resolution of 50 to 100 nm). The SEM is also capable of performing analyses of selected point locations on the sample; this approach is especially useful in qualitatively or semi-quantitatively determining chemical compositions (using EDS), crystalline structure, and crystal orientations (using EBSD). The design and function of the SEM is very similar to the EPMA and considerable overlap in capabilities exists between the two instruments. Fundamental Principles of Scanning Electron Microscopy (SEM) Accelerated electrons in an SEM carry significant amounts of kinetic energy, and this energy is dissipated as a variety of signals produced byelectron-sample interactions when the incident electrons are decelerated in the solid sample. These signals include secondary electrons (that produce SEM images), backscattered electrons (BSE), diffracted backscattered electrons (EBSD that are used to determine crystal structures and orientations of minerals), photons (characteristic X-rays that are used for elemental analysis and continuum X-rays), visible light (cathodoluminescence--CL), and heat. Secondary electrons and backscattered electrons are commonly used for imaging samples: secondary electrons are most valuable for showing morphology and topography on samples and

backscattered electrons are most valuable for illustrating contrasts in composition in multiphase samples (i.e. for rapid phase discrimination). X-ray generation is produced by inelastic collisions of the incident electrons with electrons in discrete ortitals (shells) of atoms in the sample. As the excited electrons return to lower energy states, they yield Xrays that are of a fixed wavelength (that is related to the difference in energy levels of electrons in different shells for a given element). Thus, characteristic X-rays are produced for each element in a mineral that is "excited" by the electron beam. SEM analysis is considered to be "non-destructive"; that is, x-rays generated by electron interactions do not lead to volume loss of the sample, so it is possible to analyze the same materials repeatedly. Scanning Electron Microscopy (SEM) Instrumentation - How Does It Work?

Essential components of all SEMs include the following: Electron Source ("Gun") Electron Lenses Sample Stage Detectors for all signals of interest Display / Data output devices Infrastructure Requirements: o o o o o Power Supply Vacuum System Cooling system Vibration-free floor Room free of ambient magnetic and electric fields

SEMs always have at least one detector (usually a secondary electron detector), and most have additional detectors. The specific capabilities of a particular instrument are critically dependent on which detectors it accommodates.

Applications

The SEM is routinely used to generate high-resolution images of shapes of objects (SEI) and to show spatial variations in chemical compositions: 1) acquiring elemental maps or spot chemical analyses using EDS, 2)discrimination of phases based on mean atomic number (commonly related to relative density) using BSE, and 3) compositional maps based on differences in trace element "activitors" (typically transition metal and Rare Earth elements) using CL. The SEM is also widely used to identify phases based on qualitative chemical analysis and/or crystalline structure. Precise measurement of very small features and objects down to 50 nm in size is also accomplished using the SEM. Backescattered electron images (BSE) can be used for rapid discrimination of phases in multiphase samples. SEMs equipped with diffracted backscattered electron detectors (EBSD) can be used to examine microfabric and crystallographic orientation in many materials. Strengths and Limitations of Scanning Electron Microscopy (SEM)? Strengths There is arguably no other instrument with the breadth of applications in the study of solid materials that compares with the SEM. The SEM is critical in all fields that require characterization of solid materials. While this contribution is most concerned with geological applications, it is important to note that these applications are a very small subset of the scientific and industrial applications that exist for this instrumentation. Most SEM's are comparatively easy to operate, with user-friendly "intuitive" interfaces. Many applications require minimal sample preparation. For many applications, data acquisition is rapid (less than 5 minutes/image for SEI, BSE, spot EDS analyses.) Modern SEMs generate data in digital formats, which are highly portable. Limitations Samples must be solid and they must fit into the microscope chamber. Maximum size in horizontal dimensions is usually on the order of 10 cm, vertical dimensions are generally much more limited and rarely exceed 40 mm. For most instruments samples must be stable in a vacuum on the order of 10-5 - 10-6 torr. Samples likely to outgas at low pressures (rocks saturated with hydrocarbons, "wet" samples such as coal, organic materials or swelling clays, and samples likely to decrepitate at low pressure) are unsuitable for examination in conventional SEM's. However, "low

vacuum" and "environmental" SEMs also exist, and many of these types of samples can be successfully examined in these specialized instruments. EDS detectors on SEM's cannot detect very light elements (H, He, and Li), and many instruments cannot detect elements with atomic numbers less than 11 (Na). Most SEMs use a solid state x-ray detector (EDS), and while these detectors are very fast and easy to utilize, they have relatively poor energy resolution and sensitivity to elements present in low abundances when compared to wavelength dispersive x-ray detectors (WDS) on most electron probe microanalyzers (EPMA). An electrically conductive coating must be applied to electrically insulating samples for study in conventional SEM's, unless the instrument is capable of operation in a low vacuum mode. User's Guide - Sample Collection and Preparation Sample preparation can be minimal or elaborate for SEM analysis, depending on the nature of the samples and the data required. Minimal preparation includes acquisition of a sample that will fit into the SEM chamber and some accommodation to prevent charge build-up on electrically insulating samples. Most electrically insulating samples are coated with a thin layer of conducting material, commonly carbon, gold, or some other metal or alloy. The choice of material for conductive coatings depends on the data to be acquired: carbon is most desirable if elemental analysis is a priority, while metal coatings are most effective for high resolution electron imaging applications. Alternatively, an electrically insulating sample can be examined without a conductive coating in an instrument capable of "low vacuum" operation. Data Collection, Results and Presentation Representative SEM images of asbestiform minerals from the USGS Denver Microbeam Laboratory

UICC Asbestos Chrysotile 'A' standard

Tremolite asbestos, Death Valley, California

Anthophyllite asbestos, Georgia

Winchite-richterite asbestos, Libby, Montana

Literature The following literature can be used to further explore Scanning Electron Microscopy (SEM) Goldstein, J. (2003) Scanning electron microscopy and x-ray microanalysis. Kluwer Adacemic/Plenum Pulbishers, 689 p. Reimer, L. (1998) Scanning electron microscopy : physics of image formation and microanalysis. Springer, 527 p. Egerton, R. F. (2005) Physical principles of electron microscopy : an introduction to TEM, SEM, and AEM. Springer, 202. Clarke, A. R. (2002) Microscopy techniques for materials science. CRC Press (electronic resource)

Nuclear magnetic resonance spectroscopy Nuclear magnetic resonance spectroscopy, most commonly known as NMR spectroscopy, is a research technique that exploits themagnetic properties of certain atomic nuclei to determine physical and chemical properties of atoms or the molecules in which they are contained. It relies on the phenomenon of nuclear magnetic resonance and can provide detailed information about the structure, dynamics, reaction state, and chemical environment of molecules. Most frequently, NMR spectroscopy is used by chemists and biochemists to investigate the properties of organic molecules, though it is applicable to any kind of sample that contains nuclei possessing spin. Suitable samples range from small compounds analyzed with 1-dimensional proton or carbon-13

NMR spectroscopy to large proteins or nucleic acids using 3 or 4-dimensional techniques. The impact of NMR spectroscopy on the sciences has been substantial because of the range of information and the diversity of samples, includingsolutions and solids.

Scanning electron microscope A scanning electron microscope (SEM) is a type of electron microscope that images a sample by scanning it with a high-energy beam ofelectrons in a raster scan pattern. The electrons interact with the atoms that make up the sample producing signals that contain information about the sample's surface topography, composition, and other properties such as electrical conductivity. The types of signals produced by an SEM include secondary electrons, back-scattered electrons (BSE), characteristic X-rays, light (cathodoluminescence), specimen current and transmitted electrons. Secondary electron detectors are common in all SEMs, but it is rare that a single machine would have detectors for all possible signals. The signals result from interactions of the electron beam with atoms at or near the surface of the sample. In the most common or standard detection mode, secondary electron imaging or SEI, the SEM can produce very high-resolution images of a sample surface, revealing details less than 1 nm in size. Due to the very narrow electron beam, SEM micrographs have a large depth of field yielding a characteristic three-dimensional appearance useful for understanding the surface structure of a sample. This is exemplified by the micrograph of pollen shown to the right. A wide range of magnifications is possible, from about 10 times (about equivalent to that of a powerful hand-lens) to more than 500,000 times, about 250 times the magnification limit of the best light microscopes. Back-scattered electrons (BSE) are beam electrons that are reflected from the sample by elastic scattering. BSE are often used in analytical SEM along with the spectra made from the characteristic X-rays. Because the intensity of the BSE signal is strongly related to the atomic number (Z) of the specimen, BSE images can provide information about the distribution of different elements in the sample. For the same reason, BSE imaging can image colloidal gold immuno-labels of 5 or 10 nm diameter, which would otherwise be difficult or impossible to detect in secondary electron images in biological specimens. Characteristic Xrays are emitted when the electron beam removes an inner shell electron from the sample, causing a higher energy electron to fill the shell and release energy. These characteristic X-rays are used to identify the composition and measure the abundance of elements in the sample.

In a typical SEM, an electron beam is thermionically emitted from an electron gun fitted with a tungsten filament cathode. Tungsten is normally used in thermionic electron guns because it has the highest melting point and lowest vapour pressure of all metals, thereby allowing it to be heated for electron emission, and because of its low cost. Other types of electron emitters include lanthanum hexaboride (LaB6) cathodes, which can be used in a standard tungsten filament SEM if the vacuum

system is upgraded and field emission guns (FEG), which may be of thecold-cathode type using tungsten single crystal emitters or the thermally assisted Schottky type, using emitters of zirconium oxide. The electron beam, which typically has an energy ranging from 0.5 keV to 40 keV, is focused by one or two condenser lenses to a spot about 0.4 nm to 5 nm in diameter. The beam passes through pairs of scanning coils or pairs of deflector plates in the electron column, typically in the final lens, which deflect the beam in the x and y axes so that it scans in a raster fashion over a rectangular area of the sample surface. When the primary electron beam interacts with the sample, the electrons lose energy by repeated random scattering and absorption within a teardrop-shaped volume of the specimen known as the interaction volume, which extends from less than 100 nm to around 5 m into the surface. The size of the interaction volume depends on the electron's landing energy, the atomic number of the specimen and the specimen's density. The energy exchange between the electron beam and the sample results in the reflection of highenergy electrons by elastic scattering, emission of secondary electrons byinelastic scattering and the emission of electromagnetic radiation, each of which can be detected by specialized detectors. The beam current absorbed by the specimen can also be detected and used to create images of the distribution of specimen current. Electronic amplifiers of various types are used to amplify the signals, which are displayed as variations in brightness on a cathode ray tube. The raster scanning of the CRT display is synchronised with that of the beam on the specimen in the microscope, and the resulting image is therefore a distribution map of the intensity of the signal being emitted from the scanned area of the specimen. The image may be captured by photography from a high-resolution cathode ray tube, but in modern machines is digitally captured and displayed on a computer monitor and saved to a computer's hard disk.

Powder diffraction Powder diffraction is a scientific technique using X-ray, neutron, or electron diffraction on powder [2] or microcrystallinesamples for structural characterization of materials.

ASTM C330 / C330M - 09 Standard Specification for Lightweight Aggregates for Structural Concrete ASTM C332 - 09 Standard Specification for Lightweight Aggregates for Insulating Concrete

Work Item: ASTM WK34078 - New Specification for Lightweight Aggregate for Internal Curing of Concrete 1. Scope 1.1 This specification covers lightweight aggregate intended to provide internal curing for concrete. It includes test methods for determining the adsorption and desorption properties of lightweight aggregate. NOTE 1-Internal curing provides an additional source of curing water to promote hydration and substantially reduce the early-age autogenous shrinkage and self-desiccation that can be significant contributors to early-age cracking. Appendix X1 provides guidance on the use of lightweight aggregates for internal curing. 1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance. Some values have only SI units because the inch-pound equivalents are not used in practice. NOTE 2-Sieve size is identified by its standard designation in Specification E11. The alternative designation given in parentheses is for information only and does not represent a different standard sieve size. 1.3 The text of this standard references notes and footnotes that provide explanatory material. These notes and footnotes (excluding those in tables and figures) shall not be considered as requirements of the standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. This is a proposed specification for lightweight aggregate for internal curing of concrete. It has been recognized for a long time that wetted lightweight aggregate can provide curing water and mitigate the effects of self-desiccation in sealed concrete. This has been shown to be very effective for high-performance concrete mixture with low w/cm. This specification proposes minimum requirements for lightweight aggregates for internal curing. It introduces the term wetted surface-dry as one of the reference moisture states, which is analogous to the SSD condition used for normal weight aggregate. The specification includes test methods for measuring absorption and desorption properties of the aggregate. This specification is needed by the industry to simplify the incorporation of lightweight aggregate into project specifications.

Keywords absorption; desorption; internal curing; lightweight aggregate; relative density; wetted surface dry