Remediation of chromium residual

contaminated sites
BY
ANKITA TAMTA
MAYANK RATHURI
D.PRASHANTH
A. CHAKRAVARTHI
V.VINILA
B.HARSHA
SHIVA KUMAR
 CONTENTS

 INTRODUCTION

 CONTEXT TO THE PROBLEM

 IMPORTANCE OF THE PROBLEM

 PRESENT PRACTICES

 STATUS OF RESEARCH

 CHALLENGES + INDIAN SECENARIO

 WHAT NEXT IN THE CONTEXT OF CHALLENGES

 CASE STUDY
 INTRODUCTION: REMEDIATION

 Environmental Restoration is a matter of national concern as contamination is reaching crisis

 It deals with the removal of contaminants from environmental media such as soil, groundwater, sediment, or surface water

 Environmental Restoration involves different approaches & technologies depending on the requirements of the situation. It
involves huge quantities of resources, heavy sums of money, equipment and man-hours (as spent effort)

 To maintain sustainability, Remediation of heavy-metal contaminated sites must be prioritized

 INTRODUCTION: CHROMIUM

 Chromium is one of the most frequently used metal contaminants and one of the top 20 contaminants on the list of
hazardous substances.

 Chromium is highly toxic non-essential metal for microorganisms and plants.

 Important for industries for manufacturing of many diverse products including alloys, chemicals, refractories, wood
preservation, cement, ink and dyes manufacture and tanneries.

 Chromium exists in several oxidation states, ranging from Cr+2 to Cr+6

 CHROMIUM: EFFECTS, USES

• The trivalent chromium (Cr3+) can be sourced from many foods.

• Involved in normal insulin function (storage of carbohydrates, lipids,
Human beings and proteins )
• Cr6+ is toxic and Carcinogen

• Effects on plant physiological processes such as photosynthesis, water

relations & mineral nutrition.
Plants • Direct & indirect effect on enzymes or by its ability to generate reactive
oxygen species which may cause oxidative stress

• Important for industries.

Industries • Alloys, chemicals, electroplating, refractory material, wood
preservation, cement, ink and dyes manufacture and tanneries.
CHROMIUM FOR INDUSTRIAL USE
 INTRODUCTION: CHROMIUM CHEMISTRY

 The most stable and common forms are Trivalent, Cr(III) and Hexavalent, Cr(VI) species (Fendrof, 1995), which display quite
different chemical properties and affect organisms in different ways

Cr (VI) Cr (III)

Water soluble Soluble Insoluble

Toxicity Known Carcinogen Less toxic

pH range Above 8 4-8

Source Ore restoration Chromite ore

Causes Skin cancer allergic ,dermatitis.

Density, g/cm3 (*Based on USEPA 2.52-2.74+ 5.2

Screening Level Tables of risk) (when present as Na2CrO4)
 Eh-pH diagram for the system Cr-O2-H2O
(assuming that the concentration of ΣCr = 10−6 mol kg−1 at solid/liquid boundaries)
 INTRODUCTION: CHROMIUM OCCURANCE

 Metallic chromium does not occur in the native state, it’s extracted from chromite ore.

 Chromite ore = Exclusive feedstock for commercial production of several Cr compounds.

 India ranks second worldwide in chromium output and also stands second globally in production of leather by using chrome
tanning.
 CONTEXT OF THE PROBLEM

Location of the 320 probably contaminated sites in India Distribution of contaminants at 320 sites
 INTRODUCTION: CHROMIUM

Identification of optimal remedial strategies requires understanding processes affecting the migration, transformation and
chemical state of chromium

Physical Processes Chemical Processes

Advection Red-ox reactions

Chemical speciation
Dispersion
Adsorption/Desorption

Diffusion Precipitation/Dissolution

11
 INTRODUCTION: Cr CONTAMINATION

 Chromite ore = Exclusive feedstock for commercial production of several Cr compounds

 The mineral has a spinel structure with a general formula: AB2O4

 A is a divalent cation (Fe, Mg), and

 B is a trivalent cation (Cr, Fe, Al)

 Tathavadkar et al. (2004) investigated 8 chromite ore samples from 5 countries and found Cr contents between 30% and 35% by
weight

 Basic chromium sulfate (BCS) is a widely used leather tanning agent, and is produced from the relatively unreactive ore in a
12
soluble form, based on high temperature alkaline oxidation
Basic Chromium Sulphate
Tanneries using BCS
13
14
 INTRODUCTION: COPR SOURCE

Lime + Soda ash

Drying & Crushing Drying & Crushing
Ore
Ore Ore

100-mesh screen

Sodium Salts Al(OH)3

Rotary Kiln
Crystallizer Salt Removal pH Control
(1100-1200oC)

Chromate Salts & COPR

Liquor (2-7% Cr+6 Remaining)

15
 INTRODUCTION: COPR SOURCE

High Temperature Alkaline Oxidation

1. Conversion of insoluble chromite ore into water-soluble CrO42–.

Roasted at 1100oC (45 Min)

Lime + Soda ash
2. The Na2CrO4 produced is extracted in water, and the residue, the so called Chromite Ore Processing Residue (COPR), is
discarded. Sodium chromate is then converted into sodium dichromate by reaction with sulfuric acid

3. The addition of molasses and the following reduction of Na2Cr2O7 lead to the formation of BCS

(Molasses)
BCS Leather Tanning
16
 MAJOR SITES WITH COPR CONTAMINATION

(15 sites;
1830-1968)

(1931-1972)
(>140 sites;
2-3 Mil. T;
1905-1971)

17
 INTRODUCTION: COPR WASTE

 In general, COPR contains Un-reacted chromite ore as well as Un-extracted CrO42–

 China + India = generate > 6 million tons COPR/year (Du et al., 2012).

 After deposition, COPR is not stable and undergoes weathering reactions,

o where dissolution of Cr(VI)-bearing minerals is the main source of contamination (Chrysochoou et al., 2010; Geelhoed et
al., 2002; Geelhoed et al., 2001)

18
 INTRODUCTION: COPR COMPOSITION

The mineral composition of the COPR can be categorized into 3 groups based on the processing step

(I)

Un-reacted feedstock ore,

which contains 60-70% Cr(III)

Phases produced during

( II )
the high temperatures
of Cr extraction

( III )

Minerals formed under

subsequent weathering
conditions on the disposal sites
19
 INTRODUCTION: COPR LEACHING CHARACTERISTICS

 Two of the dominant factors that impacted leaching were the soil pH and ambient temperature

 Hillier et al. (2007) emphasized the exceptional importance of hydrogarnet as a Cr(VI)-host phase in COPR, in which up to 50%
of the total Cr(VI) was recorded

 For COPR residues with high brownmillerite and periclase content, leaching can occur months to even years after treatment

20
 COPR Pathways
(Matern et al, 2016) 21
22
 INTRODUCTION: REMEDIATION

Metal removal from soils can be achieved through different strategies:

a. In-situ treatment: Instead of removing the contaminated soil, contaminants are extracted and/or treated within their

geological environment

b. Ex-situ treatment:

 Off-site treatment: Involves excavation of the polluted soil and the subsequent treatment in a controlled waste dump or

soil-cleaning installation;

 On-site treatment: As above, with the difference that the soil-cleaning installation would be situated on location;

23
CLASSIFICATION OF REMEDIATION TECHNOLOGIES BY PROCESS

24
 TREATMENT OF COPR

 The buffering capacity of COPR is very large, thus pH adjustments and addition of organic matter are not feasible or cost effective
for in situ applications

 Farmer et al. (2006) that a minimum of ~13 mol H/kg dry COPR would be required to decrease pH to 7.5. Immediately after, the
pH would increase again due to the alkalinity of the COPR

 Extremely high pH of COPR brings down the application scope of Bio- and/or Phytoremediation. But, still can be applied to
remediate less polluted sites

 Although some plants can tolerate chromium, phytotoxicity occurs for most vascular plants at Cr concentrations above 0.5 mg/kg,
which is significantly lower than levels reported at COPR contaminated sites (Sokol et al., 2010)

25
 TREATMENT OF COPR(Contd.)

 Chrysochoou and Dermatas provided a good description of physical entrapment with cement. However, cement based entrapments
posed several unforeseen problems. In addition, it is concluded that conventional stabilization processes only reduced the leachate
to 330 mg Cr/l

 The potential formation of ettringite is one of the reasons that treatment of COPR with cement-based materials was not widely
pursued (Li et al., 2011)

 Pyrolysis has proved to be much effective, the burning in the presence of organic carbon (e.g., carbohydrates or sewage sludge) as
a reductant for Cr(VI), can be operated at lower temperatures (Wang et al., 2007; Zhang et al., 2009).

26
The natural chromium cycle in the environment
(modified from Barlett, 1991) 27
 CHEMICAL TREATMENT (REDUCTION)

The chromium oxidation/reduction cycle in soil

(James, 1996) 28
 Applicability of physical
separation according to
liberation degree of the metal
phase for the particulate forms
Dermont et al., 2007

29
 SOIL WASHING

 Cr(VI) + [CrL6]3+ ─ To be leached out

 The performance of a soil washing system will typically be measured by the volume reduction attained

 Volume reduction is easily obtained if fine and coarse fractions are separated sequentially

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 CHEMICAL TREATMENT (REDUCTION)

WITH ‘Fe’ BASED CHEMICALS

 The key reaction with ferrous in generic form─

Site (or) Materials & Results &

Source Remarks
Sample details methods Inferences

At the high pH associated with COPR,

Although earlier batch study
COPR FeSO4 (pH~3) Fe(II) was precipitated rendering the
Geelhoed et al. had found Fe(II) to be effective
of Glasgow, Scotland used as a Cr(VI) in the column effluent to be 3
2003 at treating COPR, the column
(grain size <6 mm) reductant orders of magnitude higher than the
study was not effective
acceptable limit

COPR particle size Particle size strongly linked to More effective FeSO4-induced
Moon et al. FeSO4 as
linked to efficiency treatment effectiveness for reductive immobilization of COPR
2008 reductant
of remediation both batch and column studies with smaller the particle size
31
 CHEMICAL TREATMENT (REDUCTION)

WITH ‘S’ BASED CHEMICALS

 Goal: React Cr(VI) with sulfur compound to precipitate chromium hydroxide

 Preliminary studies focused on the use of sulfides, however the reaction was too slow for practical remediation purposes

 Velasco et al. (2012) investigated the Na2S for 250 kg COPR treated with different mass ratios of Na2S:Cr(VI). A mass ratio of 6:8
converted 97% of Cr(VI) to Cr(III)

 Most of the S-based research has been in the form of calcium polysulfides (CaSx). Graham et al. (2006) first used CaSx to address
COPR in Glasgow based on the following reaction:

33
CHALLENGES
ORGANIC PYROLYSIS

 Requires high temperatures (possible only under controlled conditions).

 Application on large scale is not applicable since it is uneconomical.
 Remediation efficiency is very high but temperatures used are high.

SOIL WASHING

 Most appropriate when soil contains 50-70% of sand, and not cost effective if fines percentage is 30-50%.
 Area constraint, requires large equipments i.e a 20 ton per hour unit occupies a half acre of land.
 Removal of soluble chromium after from wash water is another challenge and in many cases not cost effective.
 REDUCTION OF Cr WITH Fe BASED CHEMICALS

 Subsequent studies by Moon et al. in 2011-12 found that adding FeSO4•7H2O at 8 times the required stoichiometry to support Cr(VI)
reduction reduced leaching of Cr(VI) from COPR for 420 days. Unfortunately, chromium content would rebound to above regulatory
limits as the Fe(II) was scavenged by competing reactions

Need excess FeSO4

FeSO4 Interferences
(>8x stoichiometric requirement)

Dissolution of
Release of Aluminum
Brownmillerite

Ettringite
+ Generates excess SO42-
Chromate Analog of Ettringite
36
 REDUCTION OF Cr WITH Fe BASED CHEMICALS(Contd.)

 Ferrous sulfate addition also results in dissolution of brownmillerite from the COPR, which in turn releases aluminum

 The chromate analog of ettringite [Ca6(Al2(SO4)3(OH)12•26H2O] can also be formed which also results in heave and uncontrolled
expansion

 For COPR soils treated with excess FeSO4, the ettringite heave can be as much as 2.6 feet (Dermatas et al., 2006)

 The potential formation of ettringite is one of the reasons that treatment of COPR with cement based materials was not widely
pursued (Li et al., 2011)

 Stabilization solidification is not used for this reason.

 CHEMICAL TREATMENT(REDUCTION)

 Most of the S-based research has been in the form of calcium polysulfides (CaSx). Graham et al. (2006) first used CaSx
to address COPR in Glasgow based on the following reaction:

 Sulphide ion results in aesthetic characters results in rotten egg smell.

 MAJOR COPR SITES OF INDIA

Rania, Kanpur,
Vadodara, Uttar Pradesh
Gujarat

Howrah, West
Bengal

Ranipet, Vellore,
Tamil Nadu

39
MAJOR COPR SITES OF INDIA(Contd.)

40
Location of COPR site
near Rania, Kanpur, UP

Singh et al. 2014

41
Satellite View of Site Heaps of COPR at the site
(Google Earth; 2017) (Singh et al., 2014)
42
Groundwater Pollutant
Mapping near Kanpur
COPR Site

(Singh et al., 2013)

43
Location of COPR site
near Ranipet, Vellore,
Tamil Nadu

44
 Photos: Larry C. Price

 This chromium waste accumulated in massive mounds on the factory grounds, where
it remains today, more than 20 years after the plant closed 1995
45
What Now ?

46
 No Soil-Heavy Metal standards in Indian Context

Standards: Functions?

• Standards to ensure an equal level of protection of human health

• Standards that limit adverse effects on the ecosystem

• Standards should define the quality of land

• Standards are instruments for compliance of legal decisions

• Standards are the basis for enforcement and supervision

47
Standards and Regulations do not exist apart from each other

48
Research towards-
1) Remediation decisioning.

2) Optimization (cost, resources and time)

3) Effective scheduling and planning

4) ….

Technical Research:
• Feasibility analysis of possible and probable remediation techniques

• Development of existing treatment methods for reducing their drawbacks, such as-

a) Understanding relation between: Soil grain size – Contaminants – Treatment efficiency

b) Reducing soil heave when Fe-salts are used for treatment (by using some additives)

c) ….

49
Addressing Real-Time COPR generation

— Industrial Symbiosis

— Integrated EIPs, such as

a) Sintering and Iron-making Industry

b) Cement Industry – Mineralizer

c) Glass Manufacture – Green Colorant

d) ….

50
 Glasgow COPR Contaminated Sites

 Since 1830s, the J. J. Whites chemical works at Shawfield in

southeast Glasgow was the world’s first and largest producers
of chrome

 HTAO Operated, and COPR Disposed-off till 1967

 Chromite ore processing residues arising from the works were

used as infill and backfill material across large tracts of
south-east Glasgow

51
 Site Conditions

 For 50 years, chromates have been known to be potent

inducers of cancer in exposed personnel

 While >120 years ago, First case of adenocarcinoma of the

nose was reported by Newman (1890)* in a worker who
had previously been exposed to chrome pigments

 In 1980s, Glasgow City Council (GCC) identified 15 sites

where elevated concentrations of Cr(VI)

*Newman D. A case of adeno-carcinoma of the left inferior turbinated body, and perforation of the nasal
septum, in the person of a worker in chrome pigments. Glasgow Medical Journal 1890;33:469-70.
52
 Initial Remediation Push

 The investigation of remedial options was undertaken by Dames and Moore Pvt Ltd on behalf of
GCC in 1993 at Whites chemical works near Shawfield

 Observations: Cr(T)-65100 mg/kg; Cr(VI)-15600 mg/kg

 Three proprietary remedial techniques for soil were evaluated :

 In-situ physicochemical ─ Lab Scale ─ Slurrry of (unnamed reducing agent) + immobilisation agents
including combinations of specially modified ‘E-clays’, flyash, bentonite, slag and OPC

 Ex-situ physicochemical ─ Pilot Scale (Batch basis; 100 tons) ─ Molecular Bonding System (Patented
remediation method) ─ Chemical reduction

 In-situ biological ─ Pilot Scale ─ Bacterium (Shewanella alga Br-Y) ─ capable of reducing Cr(VI) to
Cr(III) ─ grown up in a fermentation process and then starved to form Ultramicrobacteria (UMB)
53
 Initial Remediation Push (Contd…)

 Dames and Moore Pvt Ltd. have also conducted a ‘baseline trial’, to examine the effectiveness of
three non-proprietary techniques
 Organic Matter ─ A mixture of horse manure and molasses to stimulate microbial activity and generate
anaerobic conditions in an attempt to reduce Cr(VI) to Cr(III);

 Sulphate Reducing Bacteria (SRB) ─ Molasses and ammonium sulphate to stimulate sulphate-reducing
bacteria to produce hydrogen sulphide which acts as a reducing agent on the Cr(VI); and

 FeSO4 ─ To treat Cr(VI) directly by chemical reduction

 Monitoring of the effects of these treatments was carried out over an 8-month period

 Result: All methods (both patented and non-proprietary) showed either insignificant remediation
effectiveness or not proved to be feasible 54
55
56
 The ANC7.5 is less than that reported by Geelhoed et al. (2002) for COPR from Glasgow
reacted with HCl (13mol H+/kg) and comparable to that of steel slag (8mol H+/kg) (Yan et al.,
1998).

 Maximum aqueous Cr(VI) concentrations were reported at pH≈8 for Glasgow-based COPR
(Geelhoed et al., 2002)
 Maximizing the soluble Cr(VI) content may lead to more efficient groundwater pump and treat
systems

Farmer et al., 2001

57
 GW Sampling points near/across clyde river
(Graham et al., 2006) (Whalley, Caroline, et al., 1999)

Whalley, Caroline, et al. "Chromium speciation in natural waters draining contaminated land, Glasgow, UK." Water, Air,
and Soil Pollution 112.3-4 (1999): 389-405. 58
Whalley, Caroline, et al., 1999
CaSx - Based Remediation

 First CaSx based remediation

 pseudo-first-order kinetics

60
Mineralogical composition of solid
phase residue

61
 Full Scale Field Remediation

 In completing preparation works for the 2014 Commonwealth Games Athletes Village in
Glasgow, VHE pvt ltd secured yet another major project

 Extensive site trials were undertaken to help establish the most effective treatment process which led
to a new form of specifically manufactured chemical reductant solution, Calcium Polysulphide
(CaSx), being selected due to its high reactivity properties

 Manufactured in Japan

 The solution was distributed to 8000 injection points, inserted on a grid pattern to help target specific
affected areas of contamination

 The injection works successfully treated around 70,000m3 of Chromium contaminated soils down to 6
metres below ground level within the saturated zone

62
63
Palumbo-Roe, Barbara, et al. "Limitations on the role of the hyporheic zone in chromium natural
64
attenuation in a contaminated urban stream." Applied Geochemistry 83 (2017): 108-120.
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THANK YOU

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