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Introduction Where a specific standard is lacking, it is common practice for laboratories offering petrographic services to work in accordance with an in-house test procedure, which adapts accepted standards from the nearest material in terms of similarity. the hand specimen, such as scratch testing to assess relative hardness (Moh's scale), or acid drop testing (with dilute hydrochloric acid) to determine if carbonate minerals are present. Colour is usually assessed visually in the hand specimen by comparison with standard colour charts such as the Munsell rock colour chart (Geological Society of America, 1991) or the Munsell soil colour chart (Munsell, 1994). The hand specimen is then examined using a low-power stereo-zoom microscope (2) at magnifications of typically up to 50. In certain circumstances a slice of the sample may be finely ground on one surface to aid the low-power microscopical examination. In addition to being an observational tool, the visual and low-power microscopical examinations are used to determine the most appropriate location for thin section specimens and/or highly polished specimens to be taken for further, more detailed high-power microscopical examination. Specimen preparation is discussed in Sampling and sample preparation, p. 15. High-power microscopical examination is conducted using a polarizing microscope capable of magnifications up to 600 (3). Thin section specimens are examined in plane-polarized or cross-polarized transmitted light. In addition, various compensator plates may be inserted into the light path to determine different optical properties of minerals. The most commonly used compensator is the gypsum plate (sensitive tint plate) which is used for determining the directions of fast and slow rays in crystals, which is particularly useful for identifying feldspars. Figures 46 provide a comparison

Petrographic techniques showing the same view of a rock sample in planepolarized light, cross-polarized light, and cross-polarized light with the gypsum plate inserted. Fluorescent dyes may be added to the consolidating resin during sample preparation to aid the examination of cracks and pore structures when the specimen is viewed in combination with a strong light source and an excitation filter.

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PETROGRAPHIC TECHNIQUES VISUAL AND LIGHT MICROSCOPICAL EXAMINATION

Light microscopy (also called optical microscopy) is at the heart of petrography and, combined with visual examination, it forms the basis of commercial petrographic examinations. The main suppliers of highquality light microscopes and their accessories are listed in Appendix A. If required, light microscopy can be supplemented with a range of complementary techniques to achieve the objectives of the petrographic examination. These are discussed in Complementary techniques, p. 13. Following arrival in the laboratory, samples of geomaterials are first examined in the as-received condition using the unaided eye. At this stage a few simple physical and chemical tests may be performed on

46 Thin section specimen of dolerite viewed in plane-polarized transmitted light (4), cross-polarized transmitted light (5), and in cross-polarized transmitted light with the gypsum plate inserted into the light path (6); 35.

2 A stereozoom lowpower microscope for examining samples in hand specimen. (Courtesy of Leica Microsystems UK Ltd.)

3 A polarizing microscope set up for combined transmitted light, reflected light, and fluorescence microscopy of thin sections and highly polished specimens. With attached digital image capture system. (Courtesy of Leica Microsystems UK Ltd.)

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Introduction 7 This is termed fluorescence microscopy and Figures 7 and 8 show a comparison between a rock sample in cross-polarized light and fluorescent light, illustrating how the fluorescence view defines porous areas. Sometimes highly polished specimens are prepared for examination in reflected light (brightfield and darkfield). Reflected light is particularly useful for examination of opaque minerals and cements. Figures 9 and 10 show a comparison of ore minerals shown in transmitted light and reflected light. Each of the plate captions in this book includes an abbreviation to show the viewing light of the photomicrograph as follows: Applied light Abbreviation Plane-polarized transmitted PPT Cross-polarized transmitted XPT Plane-polarized reflected PPR Cross-polarized reflected XPR Normal reflected NR Reflected fluorescence UV Each photomicrograph caption also includes the viewing magnification which correspond to the following fields of view: Magnification Approximate field of view (mm) 35 4.5 75 2.5 100 1.8 150 1.0 200 0.8 300 0.5 600 0.2

Petrographic techniques

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PHOTOMICROGRAPHY AND IMAGE ANALYSIS

Photographic images can be taken through the microscope (photomicrography) by attaching a camera on to the vertical tube of the microscope's trinocular head. Until recently 35 mm film cameras were used as standard for photomicrography. While these provided high-quality images in the form of photographic prints and slides, they had the disadvantage of having to wait for the film to be processed before one could view and utilize the images. Recent developments in digital image recording have brought rapid changes to photography and, in consequence, also to photomicrography. Film cameras have now been replaced by digital cameras that provide instantly available images, which can be readily manipulated and enhanced using computer software, to suit the required purpose. A basic guide to the practical aspects of digital light micrography is provided by Entwistle (2003b & 2004). As a result of the move towards digital information, petrographic examination reports are now sent to clients in digital format using electronic mail, in addition to the traditional paper copy sent by conventional mail services. Digital technology has reduced the report production and delivery times for petrographic investigations. Having photomicrographs in digital form also makes it easy to put them up on internet websites, either for public view, or for clients' private use in a password-protected area (Entwistle, 2002). Image analysis is being increasingly used to measure various properties of construction materials through the microscope. Measurements are obtained by analysis of digital photomicrographs using computer software, which can be highly successful. However, it should be noted that image analysis techniques are only accurate if sufficient image contrast is present to allow accurate identification of the subject being measured. Special sample preparation may be required to ensure this. Also, it must be remembered that the results are only valid if the plane of section analysed is truly representative of the sample. Applications for image analysis of construction materials currently under development include: Modal analysis of rock and building stone for mineralogical composition. Determination of textures within rock and building stone. Determination of the shape, size, and particle size distribution (grading) of aggregates. Modal analysis of fine aggregate for mineralogical composition.

Modal analysis of concrete for aggregate content, aggregate particle shape, aggregate grading, cement content, and air void content. Measurement of water/cement ratio of concrete. Modal analysis of mortars, renders, and screeds for aggregate content, aggregate particle shape, aggregate grading, binder content, and air void content. Assessment of fire damage to concrete by quantifying heat-induced colour changes.

Complementary techniques
A high-quality petrological microscope can usefully magnify up to 600 times with a maximum resolution of around 1 m (microns). Where closer examination is required scanning electron microscopy (SEM) is invaluable as it achieves significantly higher magnifications of up to 50,000 times and resolutions of around 7 nm (nanometres), by using a beam of high-energy electrons to replace the light of conventional microscopes. In addition to their high-resolution capabilities, electron microscopes have great depth of field, producing electron images that have a threedimensional effect. The on-board electron probe microanalysis system (EPM) allows inorganic bulk elemental chemical analysis of characteristic X-ray spectra emitted by samples. The EMP has two modes of operation of importance to petrographers. Spot analysis focuses on selected points of the sample such as individual crystals to give a semiquantitative elemental analysis, while elemental mapping scans along a square line raster over a larger area of the sample surface (up to 30 mm 15 mm) to allow observation of variations in element distributions. Mineralogical analysis by X-ray diffraction (XRD) can be helpful for identification of crystalline minerals and decay reaction products, when the optical properties do not allow definitive microscopical identification. XRD has the advantage of actually identifying the minerals present, although estimation of the relative amounts is at best only semiquantitative. Other spectroscopic analysis methods such as X-ray fluorescence (XRF), atomic absorption (AAS), and atomic emission (ICP-AES) give very precise determinations of elemental composition. The elemental composition data from these techniques require skilled interpretation by the analyst to identify the proportions of mineral phases present. The above techniques will only detect inorganic compounds and, to identify the presence of organic materials, infrared spectroscopy is the method of choice.

7, 8 Fluorescent yellow resin impregnated thin-section specimen of marble. Viewed in cross-polarized transmitted light (7) and in reflected fluorescent light (8); 150.

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9 Roofing slate in thin section viewed in planepolarized transmitted light. Inclusions of pyrite appear opaque (black); PPT, 75.

10 Highly polished specimen of roofing slate viewed in reflected light. Inclusions of pyrite reflect light (yellowish-white); XPR, 75.

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Introduction

Sampling and sample preparation investigation of bowing marble panels), detection of alkalisilica reactive aggregates, and identification of flaws in a variety of construction products. Electron microscopy is one of the main complementary techniques used in conjunction with optical microscopy hence developments in the field of electron microscopy concern the petrographer. The resolving power of the electron microscope is continually improving, with modern field emission scanning electron microscopy (FESEM) now providing magnifications of up to 550,000 times and resolutions down to 0.5 nm. One disadvantage of conventional electron microscopy is that the sample has to be viewed in a vacuum. Recent advances have allowed hydrated samples to be imaged using environmental scanning electron microscopy (ESEM) or alternatively, by soft X-ray transmission microscopy. These methods allow live examination and analysis of geomaterials undergoing reactions, for example, hydrating cement paste or carbonating lime. Also, the latest cryotransfer SEM allows sensitive hydrating specimens to be set in a stable state by quickfreezing, enabling previously impossible examinations. Advances in electron microscopy will continue to improve our understanding of geomaterials and reactions that they undergo. understand the degree of sampling bias within the sampling scheme. Ideally the petrographer should be involved in devising the investigation plan and be present during sampling operations. The actual sampling technique and the type of sample required for petrographic examination depend on the type of material being sampled, the objectives of the investigation, and if any other types of tests are to be

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Future developments
Optical microscopes have now entered the digital age and modern microscopes tend to come with a computer attached. The major microscope manufacturers now offer options for automation of their optical microscopes with a range of functions being controlled via a touch-sensitive screen. Motors automatically move the objective, substage condenser, and the image projection system; all of which is optimized quite automatically for quality of illumination, resolution, and even focus. Combined with digital image capture systems and image analysis software we now have a real possibility of automated sample examination. However, an experienced petrographer will always be required to supervise the process and check the results. Automation offers huge improvements in productivity and potentially significant reductions in the unit price of examinations. Automated modal analysis is likely to become a serious alternative for a number of standard tests that have traditionally been performed by cheaper (and arguably less accurate) chemical analysis methods. For example, the mix proportions of hardened concrete and mortars could routinely be determined by modal analysis instead of chemical analysis. Digital technology is changing the way that the findings of petrographic examinations are presented. Digital image capture allows a series of sequential micrograph frames to be animated into movies to illustrate talks and websites (Entwistle, 2003a). Digital movies demonstrating petrographic features of samples could be included within the report submitted to the client. The recent development of the birefringence imaging microscope offers the possibility of interesting applications for examination of geomaterials. The equipment consists of a motorized rotating polarizer that is fitted below the sample stage and a digital camera that fits on the trinocular microscope head, both attached to a computer. As the motorized polarizer rotates, the camera collects birefringence data at a number (between five and fifty) of different positions. The data are then processed by special computer software to produce various types of false colour image. The birefringence microscope excels at detecting strain and defects within materials. Figures 11 and 12 show examples of false colour images obtained using the birefringence microscope. Existing applications include quality control of industrial diamonds, silicon carbide abrasives, and glass, study of decomposition of biomaterials, and mapping of collagen in heart valves. Potential applications for geomaterials include investigation of rock microstructure (including the

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SAMPLING AND SAMPLE PREPARATION SAMPLING

Samples of construction materials may be obtained during the manufacturing production run or, alternatively, from structures during construction or while they are in service. The objectives of the materials investigation and details of the proposed laboratory testing should be clearly defined, before any sampling is attempted. A coordinated sampling programme should be prepared by persons experienced with the investigation of construction materials and built structures. The number of samples required to achieve the investigation objective will depend on the purpose of the investigation/testing, the size of the structure, the types of construction used, and the number of construction phases. Sampling schemes usually comprise one of two types (or a combination of both). The first is essentially a random or even spread of samples across a structure or production run, to ascertain representatively the general materials' characteristics and quality. The second scheme is more targeted to address specific issues, such as investigating suspected defects identified by visual survey. In either case, the investigator must clearly

11 Retardation (|sin |) image of a sandstone sample obtained using the birefringence microscope imaging system. This shows the relative birefringence of the different quartz grains that make up the sandstone; 150. (Courtesy of Oxford Cryosystems.)

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12 Orientation () image of a sandstone sample obtained using the birefringence microscope imaging system. The lines show the orientation of the extinction (slow axis orientation) for each of the quartz grains; 150. (Courtesy of Oxford Cryosystems.)

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Introduction carried out on the sample. The various petrographic examination standards listed in Table 2 give details of sampling requirements and provide guidance on appropriate sampling procedures (Table 3). For rock and building stone, the size of sample required depends on the grain size of the rock, with coarse-grained rock requiring larger samples than fine-grained rock. Rock/stone samples may consist of lump samples, drilled cores, or sawn blocks. For aggregate products it is important to ensure that a representative number of individual aggregate particles are examined. For this reason, the required sample mass increases as the nominal maximum particle size of the aggregate increases. When sampling concrete from a structure, broken fragments are not usually acceptable for petrography, as it is difficult to differentiate between inherent concrete defects and sampling damage. Diamond drilled concrete core samples (13) are preferred and the core diameter should be at least twice, and preferably three times, the maximum size of the coarse aggregate within the concrete. For construction products that are supplied as units, for example precast concrete or clay bricks, it is normally sufficient to examine one complete representative unit. Due consideration should be given to the health and safety issues that arise from sampling activities, including safe access to the sample locations. Once obtained in the field, samples should be labelled indicating orientation details (bedding, outer surface, way up, and so on), placed into separate sealed sample bags, and each bag labelled with a unique identification reference. Concrete cores should first be wrapped in cling film to prevent carbonation. The exact sample locations should be recorded using a combination of written notes, drawings, and photography. These should include comprehensive inspection details of the location prior to sampling and an as-found record photograph. These details should be made available to the petrographer if he/she was not present during the sampling operations.

Sampling and sample preparation are soft, heat sensitive, and/or water sensitive, thin section preparation presents considerable challenges for the technician. Thin section making starts with oven-drying the sample at a temperature that will not damage heatsensitive materials (lower than 60C). Once dry the specimen is vacuum impregnated with a low viscosity epoxy. The resin is usually coloured with a dye to assist in the determination of porosity and cracking when the thin section is microscopically examined. The colour of this dye would normally be fluorescent yellow except when investigating the thaumasite form of sulfate attack (TSA) in concrete, in which case blue dye is a better choice. Following impregnation the resin is heat cured in an oven or on a hot plate, again at <60C. The cured sample block is then ground using a diamond cup wheel to expose the examination surface. At this stage the thin-sectioning machine is first used. The surface for examination is finely ground using the thin-sectioning machine, cleaned, and mounted on a glass slide using epoxy glue (either heat or ultraviolet light curing). The excess sample is then cut off using a special diamond saw with a vacuum chuck that holds the slide in place (14). All cutting and grinding must be done in oil or alcohol rather than water to avoid damage of water-sensitive materials. The thin section is then finely ground to the finished sample thickness on the thinsectioning machine and finished by gluing a thin glass cover slip over the sample.

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Table 3 Summary of sampling requirements for different geomaterials Material group Building stone Roofing slate Rock Coarse aggregate1 63 mm (75 mm) nominal maximum size 31.5 mm (37.5 mm) nominal maximum size 16 mm (19 mm) nominal maximum size 8 mm nominal maximum size <4 mm (<4.75 mm) sized From structure From production run From structure From floor From structure or production run Sample type/minimum size for petrographic examination 100 mm 100 mm 50 mm sawn block or 5 kg lump sample 1 whole slate 5 kg of lump or core samples 50 kg (180 kg) 25 kg (90 kg) 8 kg (45 kg) 2 kg 0.5 kg (23 kg) 100 mm diameter core 150 mm cube specimen 1 unit or 100 mm diameter core sample 0.5 kg intact lump sample 100 mm diameter core sample or 2 kg intact lump sample 1 unit 1 unit 100 mm 100 mm square piece From pavement From production run 150 mm diameter core sample 20 kg

THIN SECTION SPECIMEN PREPARATION

High-power microscopical examination requires the preparation of petrographic thin section specimens comprising ground slices of the sample mounted on glass slides, through which light will pass to allow microscopical observation. The thin section making technique was developed by geologists for the study of rocks. When applied to other construction materials that

Fine aggregate1 Concrete Concrete product Mortar, plaster, and render Screed Clay brick Ceramic tile Architectural glass Bituminous mixtures
1

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14

EN 932-3 requirements (with ASTM C295 requirements in brackets).

13 Obtaining a core sample from a reinforced concrete structure by diamond drilling.

14 A thin section cut-off and trim saw. (Courtesy of Logitech Materials Technologists and Engineers.)