x-ray diffraction – bruxer axs, d8 advance

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The basic version i.e. the x-ray powder diffraction is an analytical technique widely used to identify the crystalline phases contained in various materials. It is mainly adopted for research and quality control and ca be used alone or with other techniques to identify the constituents of simple and complex mixtures in various areas, such as: stone processing industry; production of binders; control formulations for mortar, plaster, stucco; brick production; control of metallic and non-metallic minerals, etc. X-RAY DIFFRACTION– Bruxer AXS, D8 Advance M A R M O diLA ZZA R O (g rig io) 2 6-0 9 19 (C) - Ha lite, p o tass ian , syn - K0.4 Na 0 .6Cl- Y: 1 4.5 8 % - d x b y: 1 . - W L: 1 .5 4 0 6 - Cu bic - a 8 9-1 4 77 (C) - An o rth ite , an ne a led - (Ca0.98Na 0 .02 )(Al1 .98 Si0.0 2 )Si2O8 - Y: 8 .3 3 % - d x by: 1 . - W L 4 2-1 4 14 (D) - Bio tite-1 IT M RG - K(Mg,Fe + 2)3 (Al,Fe+3)Si3O10(OH,F )2 - Y: 4 .17 % - d x b y: 1. - W L: 4 1-1 4 80 (I) - Albite , calcia n, o rde re d - (Na,Ca )Al(Si,Al)3O8 - Y: 8 .33 % - d x b y:1 . - W L : 1 .5 4 0 6 - T ric 8 6-1 6 28 (C) - Qu a rtz low - SiO2 - Y: 8 3.3 3 % - d x b y: 1 . - W L: 1 .5 40 6 - Hexagonal- a 4.90210 - b 4 . 8 3-2 4 66 (A) - Qu a rtz , syn - SiO2 - Y: 87 .5 0 % - d x by : 1 . - W L: 1 .5 40 6 - Hexagonal- a 4.89120 - b 4 8 9-1 3 04 (C) - Ma g ne s ium ca lcite , syn - (Mg 0.0 3 Ca0.97)(CO3 ) - Y: 1 8 .7 5 % - d x b y:1 . - W L : 1.5 4 06 Ope ra tio n s: Im p ort M ARMO d iL AZZARO (g rig io ) - File : MARMO diL AZZARO (g rigio ).ra w - T yp e : 2 T h /T h lo cke d - Start: Lin (C ounts) 0 1000 2000 3000 4000 5000 6000 2-Theta - Scale 5 10 20 30 40 50 60 X-ray Spectrum with quantitative indication of phase processing with Rietveld method Simple XRD spectrum with qualitative indication of present phases Images relating to examples of application of the XRD technique View of instrument and the management console

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X-RAY DIFFRACTION – Bruxer AXS, D8 Advance. The basic version i.e. the x-ray powder diffraction is an analytical technique widely used to identify the crystalline phases contained in various materials. - PowerPoint PPT Presentation

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Page 1: X-RAY DIFFRACTION –  Bruxer AXS, D8 Advance

The basic version i.e. the x-ray powder diffraction is an analytical technique widely used to identify the crystalline phases contained in various materials. It is mainly adopted for research and quality control and ca be used alone or with other techniques to identify the constituents of simple and complex mixtures in various areas, such as: stone processing industry; production of binders; control formulations for mortar, plaster, stucco; brick production; control of metallic and non-metallic minerals, etc.

X-RAY DIFFRACTION– Bruxer AXS, D8 Advance

MARMO di LAZZARO (grigio)

26-0919 (C) - Halite, potassian, syn - K0.4Na0.6Cl - Y: 14.58 % - d x by: 1. - WL: 1.5406 - Cubic - a

89-1477 (C) - Anorthite, annealed - (Ca0.98Na0.02)(Al1.98Si0.02)Si2O8 - Y: 8.33 % - d x by: 1. - WL42-1414 (D) - Biotite-1 ITM RG - K(Mg,Fe+2)3(Al,Fe+3)Si3O10(OH,F)2 - Y: 4.17 % - d x by: 1. - WL: 41-1480 (I) - Albite, calcian, ordered - (Na,Ca)Al(Si,Al)3O8 - Y: 8.33 % - d x by: 1. - WL: 1.5406 - Tric86-1628 (C) - Quartz low - SiO2 - Y: 83.33 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 4.90210 - b 4.83-2466 (A) - Quartz, syn - SiO2 - Y: 87.50 % - d x by: 1. - WL: 1.5406 - Hexagonal - a 4.89120 - b 489-1304 (C) - Magnesium calcite, syn - (Mg0.03Ca0.97)(CO3) - Y: 18.75 % - d x by: 1. - WL: 1.5406 Operations: ImportMARMO di LAZZARO (grigio) - File: MARMO di LAZZARO (grigio).raw - Type: 2Th/Th locked - Start:

Lin

(C

ou

nts

)

0

1000

2000

3000

4000

5000

6000

2-Theta - Scale

5 10 20 30 40 50 60

X-ray Spectrum with quantitative indication of phase processing with Rietveld method

Simple XRD spectrum with qualitative indication of present phases

Images relating to examples of application of the XRD technique

View of instrument and the management console

Page 2: X-RAY DIFFRACTION –  Bruxer AXS, D8 Advance

The elemental chemical analysis using x-ray fluorescence (XRF) is a technique that allows elemental analysis (in general, from sodium to uranium) for a wide range of materials with a sufficient level of accuracy and precision, especially for high concentrations.The strength of this kind of analysis is the capability to analyze both conductive materials (metals) and non-conductive materials (oxides, glass, ceramics, plastics, cement, etc.), and also liquids (oil, water, hydrocarbons, etc.). The analysis can be used for process control and for research in various fields, in particular in the environmental fields.

X-RAY FLUORESCENCE– Bruxer AXS, S2 Ranger

00

,10

,20

,30

,40

,50

,60

,70

,8

KC

ps

Zn

KA

1

Zn

KB

1

Mn

KA

1

Mn

KB

1

Ti K

A1

Ti K

B1

Fe

KA

1

Fe

KB

1

Ca

KA

1

Ca

KB

1

K

KA

1

K

KB

1

Ni K

A1

Ni K

B1

3 4 5 6 7 8 9

KeV

Formula Z

Amount% in weight

SO3 16 36,18

Fe2O3 26 23,06

Na2O 11 11,28

Al2O3 13 11,05

SiO2 14 9,401

MgO 12 5,366

CaO 20 2,293

TiO2 22 0,333

K2O 19 0,012

Fluorescence spectrum

Report of a typical XRF analysis

Tablets for fluorescence measurements

Desk instrument for X-ray

Images relating to examples of application of XRF technique

Page 3: X-RAY DIFFRACTION –  Bruxer AXS, D8 Advance

Stereomicroscope is commonly used to make observations on sections allowing to obtain detailed information about morphology, nature and composition of various layers of fragments under investigation, such as: shape of grains; type of binder; presence of layers of pigment; superficial alteration.

Optical microscope with polarized light (Olympus BX51). It is used for studing thin sections which detailed examination, allowing to obtain information about nature of clasts and matrix which constitute respectively the aggregate and the binder of various materials (stone, mortar, plaster, stucco, etc.). It is also possible to carry out studies on decay associated with reactions such as alkali-aggregate processes and sulphation black crusts.

OPTICAL MICROSCOPY

Polished section of a cocciopesto mortar

Thin section processed by computer

Desk with transmitted optical microscope with polarized light, transmitted biologicmicroscopr, stereo-binocular microscope

Images relating to examples of application of optical microscopy (OM)

Page 4: X-RAY DIFFRACTION –  Bruxer AXS, D8 Advance

This technique allows a recognition and a simultaneous determination of one or more cations or anions in aqueous solution. It is based on the separation of ions through ion exchange columns, thanks to the different affinities of analytes in solution for eluent phase and stationary phase, contained in a column chromatographic. The technique is mainly used to determine soluble salts which are the typical

constituents of salt efflorescence.

ION CHROMATOGRAPHY– Metrohm IC 761)

Chromatogram of cation

Chromatogram of anions

Ionic chromatograph

Images relating to examples of application of ion chromatography

Page 5: X-RAY DIFFRACTION –  Bruxer AXS, D8 Advance

The technique allows monitoring the behaviour of a substance under controlled regime of temperature increase. It is generally used to identify transformations of chemical and physical nature of a material, during a thermal treatment. Operating under standards, the most common and basic information that can be derived include, for example: quantification of loss in weight; determination of decomposition temperature of a chemical; temperature deidrossilation of substances containing water in its structure, and everything related to reactions involving structural changes in weight.

THERMAL ANALYSIS– Netzsh, STA 409 PC LUXX

Simple thermogram

Images relating to examples of application of thermal analysis (TA)

Thermal Analyzer

Stacking multiple thermograms

Page 6: X-RAY DIFFRACTION –  Bruxer AXS, D8 Advance

It is used for physical and environmental testing on any material. The instrument allows to evaluate the behaviour of thermo-shrinkage of a given material in the temperature range -40 to +180 °C and relative humidity (RH) +20 to +95%. If needed, it can be used either for maturation of standardized samples that will undergo mechanical tests, or for freeze-thaw cycling of stones.

CLIMATE CHAMBER– Angelantoni, Challenge 160

Performance of a pre-set cycle of treatment

Climate chamber for physical and environmental testing

Images relating to examples of application of treatment cycles

Page 7: X-RAY DIFFRACTION –  Bruxer AXS, D8 Advance

Static furnace and rotary furnace are chambers for controlled thermal treatments of various products under static and dynamic standard from room temperature up to 1600 °C and 1100 °C respectively.Jaw mill and centrifugal mill with spheres are grinding machines that reduce to powder various materials that have to undergo further processing for powder production or for laboratory analysis.Electro-mechanical-sieving machine produces a dry sieve of a pool to derive the dissolved fraction useful in composition of particle size distribution curve.

THERMAL AND PHYSICAL AND MECHANICAL TREATMENTS

Grading curve

Fractions separated using series of standard sieves

Desk with instruments for physical-mechanical treatments

Images relating to examples of application of treatment cycles

Page 8: X-RAY DIFFRACTION –  Bruxer AXS, D8 Advance

Load test machine. The instrument is set up for flexion and compression rupture tests for normalized elements with size 4.0 x4,0x16cm. The maximum load is 300kN. It is equipped with a dual channel with high sensitivity to appreciate different values of tensile strength from various tens of kN for elements made of concrete to single digits for elements made of lime and hydraulic lime.

MECHANICAL TESTS

Photo of an element, realized with gypsum, broken under compression

Typical stress-strain curve of an element tested in compression.

Compression machine

Images relating to examples of application of this machine

Page 9: X-RAY DIFFRACTION –  Bruxer AXS, D8 Advance

In support of a laboratory, focused on building materials and particularly mortars based on inorganic binders, it is necessary a range of equipments, part of which are represented by an automatic mixer, a motorized flow table, an automatic Vicat needle, a Blaine permeabilimeter, a Le Chatelier volumeter. The aim is to characterize, under the current legislation, various materials to mix and final products of compositions.

Accessory equipments for preparation of plaster elements

Motorized flow table

Automatic Mixer

Water heating bath