Lecture No.

18 Lecture Name:
Geomaterial Characterization

Sub-topics
• Necessity….. ? ?? ???
• Scarcity of the (natural resources)… ? ?? ???
– Chemical (Pore-Solution sampling)
– Biological

– Thermal
– Electrical
– Magnetic
– Radiation
 CHEMICAL CHARACTERIZATION
X-Ray Fluorescence (XRF)
Inductively Coupled Plasma (ICP/ICP-MS)
pH value
Gas Chromatography (GC-MS)
Nuclear Magnetic Resonance (NMR)
Fourier Transform Infra-Red (FTIR) Spectroscopy
Cation Exchange Capacity (CEC)
Pore-solution analysis
XRF Pallets
XRF Studies Calibration of
XRF- Setup

➢Physical Calibartion
➢Chemical Calibration

Elemental Composition (% by weight) of Materials

Material
Element CS WC IC RSS BSS FA-I FA-II C-I C-II GGBFS
Si 15.78 20.32 11.52 39.21 40.71 25.53 28.30 24.65 23.62 15.56
Al 5.75 17.77 1.67 2.65 3.29 15.95 15.92 20.70 21.92 8.59
Fe 8.23 1.09 1.19 0.50 0.94 2.51 2.31 1.38 1.81 0.25
Ti 1.53 2.88 0.03 0.22 0.14 2.12 1.45 1.15 1.02 0.37
S - - 0.1 - - 0.01 0.23 0.11 0.03 0.39
Ca 4.58 0.27 38.9 001 0.01 3.20 0.11 0.06 0.10 26.50
K 0.54 0.06 0.13 2.42 1.49 0.77 0.55 1.07 1.14 0.19
Mg 0.99 0.45 0.48 0.09 0.19 0.33 0.24 0.41 0.24 5.52
P 0.07 0.02 5.0 0.01 0.02 0.18 0.25 0.12 0.06 0.02
Sr 0.02 0.00 0.14 - - 0.06 0.07 0.08 0.05 0.08
Ba - - - - - 0.66 0.07 0.11 0.12 0.06
Na 1.49 0.13 - 0.04 - 0.09 0.04 0.08 0.02 0.05
Mn 0.12 0.04 0.01 - 0.04 0.03 0.01 0.01 0.01 0.01
Si +Al+Fe 29.76 39.18 14.39 42.35 44.94 43.98 46.54 46.74 47.35 24.41
Inductively Coupled Plasma (ICP) Atomic Absorption Spectrophotometer
(AAS)

Historic

Gas Chromatograph with high resolution Mass

Spectrometer (GC-HRMS)

Contemporary
Fourier Transform Infra-Red (FTIR) Nuclear Magnetic Resonance
Spectroscopy Spectrometer
 pH determination

Water Quality Analyzer

Glass calomel electrode is used

Soil solutions with different Liquid to solid ratios

pH
Temperature
Total Dissolved Solids
Electrical Conductivity
Chemical Oxygen demand
Biological Oxygen Demand
 Cation-exchange Capacity

 Concentration of Ca 2 + ( g/ml)  100  Vol. of extract (ml)  Material CEC(meq./100g)

CEC =  
 Equivalent weight of the cation  1000  wt.of sample (g)  CS 18.6
 
WC 5.0
IC 12.6

IS:2720 RSS 3.5

BSS 3.4
FA-I 4.5
FA-II 5.2
C-I 3.9
C-II 4.1
GGBFS Not applicable
 Pore-solution Sampling
The pore-solution sampling is identical to blood sampling
A Prerequisite to Soil-Water-Contaminant Interaction Studies

To predict transport/fate of contaminants in the soil mass

Design of suitable containment/Barrier system

Assessment of safe waste disposal limits: Quantity & Concentration

Leaching/Attenuation characteristics of soils

Intrusion of pollutants in ground water resources

Prediction of the loss of nutrients from the root zone

Detection of the microbial activity in soils

Validation of solute transport models

9
 CHEMICAL CHARACTERIZATION
(In particular for ASSESSMENT OF SOIL CONTAMINATION)

Direct methods Indirect methods

Pore-solution extraction (PME) Impedance spectroscopy
AAS (Impedance analyzer)
ICP-MS Electrical resistivity methods
Gas chromatography Electro-magnetic methods
Ion selective electrodes (TDR/FDR: Time/Frequency domain
Probes/Sensors Reflectometry)
PME: Pressure membrane extractor Dielectric constant
(GPR: Ground penetrating radar)
Limitations
Expensive instrumentation
Cumbersome methodology
Intensive & rigorous sample preparation, time consuming
Complicated procedure for calibration and analysis
Requirement of skilled and trained personnel
10
 Lysimeter (Pore Solution Collection Device)

Zero Tension Lysimeter

Collects Pore Solution From Saturated Soils

Percolating water

Control volume

Soil
Pervious fill Collection device
to Collection bottle

11
 Field Lysimeter

To collect leachate
485 mm
Percolating water
Waste rock material
40 mm thick creek sand
50 mm thick Gravel
(5-7 mm)

300 mm thick Gravel

(14mm)
Gravel (5-7 mm)

Occurrence of preferential flow

Influence of mobile colloids on contaminant mobility

Extra organic matter in soil reduced colloid release
12
Zero-tension Lysimeter

Loose fill
A O
Undisturbed soil core

Sand

Sloping bottom

A : Air inlet
O : Pore solution extraction

13
 Collection Basin Lysimeter

Clay liner

Granular Backfill
P
Flexible membrane liner
P : Perforated pipe

▪ To detect leakage from the clay liner

▪ To determine in situ hydraulic conductivity of the liners
▪ To demonstrate proper functioning of the clay liner

14
 Basic Philosophy

Rain water

Upper compartment with fill material, sensors

and moisture extraction cups

Lower compartment for leachate collection

Leachate

▪ Performance assessment of solidified radioactive waste

▪ Attenuation properties of soils

Validation of theoretical model by fitting

Mathematical model to Lysimeter data

15
 Tension Lysimeter

Collects pore-solution from “Unsaturated Soils”

To sample bottle To Vacuum pump

Ground

PVC pipe

I – Inflow of pore solution

under vacuum applied Porous ceramic cup

I I

16
 Importance of Lysimetric studies

Lysimeter Device which creates a control volume of soil

for studying various contaminant transport
mechanisms under in-situ conditions

➢ Field studies No control of boundary conditions,

cost and time intensive

➢ Laboratory studies Cannot simulate field conditions, Spatial

variability cannot be taken into account

➢ Lysimetric study Intermittent approach Simulates

In-situ conditions with
better control on
boundary conditions

Lysimeter identified as a potential tool for studying radioactive contaminant

Interaction and migration in Geoenvironment
17
R is the soil spiked
(with Cs, Co & Tritium)

18
Slurry of native soil

19
Vial for pore-solution collection

20
 To the
Flexible rubber tube vacuum
Pump

Stopper
Screw cap
Sample Collector

Perspex tube

Soil slurry

Ceramic thimble

Details of the suction sampler

21
Activities at a Glance

22
 TDR studies
0
15/06/05 20/06/05
20 05/07/05 14/07/05 18/07/05
26/7 flash floods
40 26/08/05 27/09/05
GSL
60

80
Depth(cm)

100

120

140

160

180

200
0.0 0.1 0.2 0.3 0.4 0.5


Hanumantha Rao, B, Sridhar, V., Rakesh, R.R., Singh, D.N., Narayan, P.K. and
Wattal, P.K., “Application of In-situ Lysimetric Studies for Determining Soil Hydraulic
Conductivity”, Geotechnical and Geological Engineering, 2009, DOI 10.1007/
s10706-009-9260-5. Published Online: 13 May 2009. 23
Variation of 137Cs and 60Co activity concentration with
depth in dry soils after a period of 500 days

24
 Pressure Membrane Extractor
S
PG
PG
P

PME RU

B
C
R

Pressure gauge Air inlet

Air pressure

Drain

Expelled water to the sampling bottle 25

 Chloride and Sulphite contents
determination
The chloride and sulphite contents of the soils can be obtained
on an extract of 2:1 Liquid to solid ratio.

Indion Easy test kit (Ion Exchange, India Ltd.), an ion exchange
resin, is employed

A sort of a titration

Change in color of the solution due to addition of chemicals

Soil Salinity Sensors:

Used for in situ measurement of soil salinity

Soil salinity is an indication of soil contamination

26
 Working principle of WP4

Block chamber

Works on relative humidity principle

Measuring range- 0 to 80 MPa
WP4 measures total suction of soil
Uncontaminated soil : Total suction = Matric(x) suction
Contaminated soil : Total suction = Matric(x) suction + Osmotic suction
SWCC of uncontaminated and contaminated soil of same type
would be different
The difference between SWCCs would indicate soil contamination
27