Arsenic. Occurrence, Toxicity and Speciation Techniques

ARSENIC: OCCURRENCE, TOXICITY AND SPECIATION

TECHNIQUES

C. K. JAIN* and I. ALI

National Institute of Hydrology, Jal Vigyan Bhawan, Roorkee 247 667, India

(First received 1 January 1998; accepted in revised form 17 February 2000)

AbstractÐThe occurrence of arsenic in natural water has received signi®cant attention during recentyears. Arsenic exists in the environment in a number of valency states. The valency state of arsenicplays an important role for its behavior and toxicity in the aqueous system. The toxicity andbioavailability of arsenic can only be determined if all its forms can be identi®ed and quanti®ed.Therefore, the aim of this article is to provide a general description of the occurrence of arsenic in theenvironment, its toxicity, health hazards, and measurement techniques for speciation analysis. Di�erenttechniques used for speciation of arsenic, viz., spectrometric, chromatographic, electrochemical, etc.have been discussed. 7 2000 Elsevier Science Ltd. All rights reserved

Key wordsÐarsenic, toxicity, occurrence, speciation techniques, spectrometric, chromatographic, elec-

trochemical

INTRODUCTION

Arsenic contamination in natural water is a world

wide problem and has become a challenge for theworld scientists. It has been reported in recent yearsfrom several parts of the world, like USA, China,Chile, Bangladesh, Taiwan, Mexico, Argentina,

Poland, Canada, Hungary, Japan, and India(Robertson, 1986, 1989; Moncure et al., 1992;Schlottmann and Breit, 1992; Frost et al., 1993;

Das et al., 1994, 1995; Chatterjee et al., 1995). Her-ing and Elimelech (1995) have reviewed the inter-national perspective and treatment strategies on the

problem of arsenic contamination in ground water.There is a growing awareness that the toxicity of

heavy metals is strongly dependent on their chemi-

cal form, resulting in increasing interests in thequantitative determination of individual species(Craig, 1986). Speciation of arsenic in environmen-tal samples is gaining increasing importance, as the

toxic e�ects of arsenic are related to its oxidationstate. Many metallic ions are found in the environ-ment in a variety of forms, that are di�erentiated

not only by their physical and chemical forms, butalso by their diverse toxic activities with respect toliving organisms (Craig, 1986). Changes in the

degree of oxidation of an element also have an im-portant e�ect on the degree of bioavailability andtoxicity (Stoeppler, 1992).

The elements occur in the environment in di�er-ent oxidation states and form various species, e.g.,As as As(V), As(III), As(0) and As (-III); Sb as

Sb(V), Sb(III), Sb(0), and Sb(-III); and Se asSe(VI), Se(IV), Se(0) and Se(-II). In oxidized en-vironment As, Sb and Se appear mostly as oxya-

nions (Cutter, 1992). The valency state of anelement plays an important role for the behavior ofthe element in the aqueous system. For example,toxicity of As(III) and Sb(III) is higher than that of

their pentavalent species (Berman, 1980; Gesamp,1986). Similarly Cr(III) is an essential element whileCr(VI) is highly toxic. The valency state of an el-

ement also determines the sorption behavior andconsequently the mobility in the aquatic environ-ment.

Many metals occur in natural waters in di�erentphysico-chemical forms. Among them simplehydrated metal ions are considered to be the mosttoxic, while strong complexes and species associated

with colloidal particles are usually assumed to beless toxic (Russeva, 1995). Organometallic com-pounds of tin, mercury and lead (particularly simple

methylated species) are more toxic than the corre-sponding inorganic species. Organoarsenic com-pounds represent an exception in this series (Prange

and Jantzen, 1995). Current interest in the determi-nation of di�erent species of arsenic in naturalwaters is caused due the fact that physiological and

toxic e�ects of arsenic are connected with its chemi-cal forms. The toxicity of di�erent arsenic speciesvaries in the order: arsenite > arsenate > mono-methylarsonate (MMA) > dimethylarsinate (DMA)

Wat. Res. Vol. 34, No. 17, pp. 4304±4312, 20007 2000 Elsevier Science Ltd. All rights reserved

Printed in Great Britain0043-1354/00/$ - see front matter

4304

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PII: S0043-1354(00)00182-2

*Author to whom all correspondence should be addressed.Tel.: +91-1332-72906, Ext. 249; fax: +91-1332-72123;e-mail: [email protected]

(Penrose, 1974; Lewis and Tatken, 1978; Stugeronet al., 1989). The concentration of arsenic in natural

waters depends on the geological composition andthe degree of pollution of the environment. Theconcentration of As(III) to As(V) varies widely

depending on the redox conditions in the geologicalenvironment (Braman and Foreback, 1973;Andreae, 1977; Shaikh and Tallman, 1978).

OCCURRENCE

Arsenic rarely occurs in free state, it is largelyfound in combination with sulphur, oxygen andiron (Brewstar, 1994; Chatterjee, 1994). Arsenic

occurs in the environment as a result of severalinputs that contain this element as organic andinorganic forms (Rubio et al., 1992). The presence

of arsenic in natural water is related to the processof leaching from the arsenic containing sourcerocks and sediments (Robertson, 1989; Hering and

Elimelech, 1995). In¯ux of arsenic from variousanthropogenically-induced sources may also con-taminate both soils and ground water especiallyunder anoxic conditions (Bhattacharya et al., 1996,

1997).The presence of arsenic in natural water is gener-

ally associated with the geochemical environments

such as basin-®ll deposits of alluvial-lacustrine ori-gin, volcanic deposits, inputs from geothermalsources, mining wastes and land®lls (Welch et al.,

1988; Korte and Fernando, 1991). Occurrence ofarsenic in natural water depends on the local ge-ology, hydrology and geochemical characteristics of

the aquifer materials (Bhattacharya et al., 1997).Furthermore, the geochemical characteristics of theaquifer material and their interactions with the aqu-eous media also play an important role in control-

ling retention and/or mobility of arsenic within thesubsurface environment (Bhattacharya et al.,1995a). Uncontrolled anthropogenic activities such

as smelting of metal ores, use of arsenical pesticidesand wood preservatives agents may also releasearsenic directly to the environment (Bhattacharya et

al., 1995b).The redox conditions in the subsurface environ-

ment also play an important role in determining themobility of arsenic (Robertson, 1986). The oxi-

dation of di�erent mineral species causes arsenic tobecome soluble and enter into the surrounding en-vironment through drainage water. Any phenomena

which a�ect the redox conditions such as pumpingrate and the land use pattern is of interest in ascer-taining the primary mechanisms responsible for the

excess arsenic content in ground water. Robertson(1989) has further reported that occurrence and ori-gin of arsenic in ground water depends on several

factors such as adsorption-desorption, precipitation-dissolution, oxidation-reduction, ion-exchange,grain size, organic contents, biological activity andaquifer characteristics. For example, Mok and Wai

(1989) studied the distribution and mobilization ofarsenic species in creek waters around the Blackbird

mining district, Idaho, and reported that the releaseof arsenic was pH dependent and was related to thetotal iron and free iron oxides in the sediments.

Leaching under a nitrogen atmosphere resulted inan increased release of arsenic, which may be dueto the reduction of ferric-arsenate compounds to

the more soluble ferrous-arsenate forms.The knowledge of the geographic distribution of

di�erent arsenic species in natural water systems is

important for environmental consideration of thegeochemical and biological cycling of the element.Furthermore, this will also provide insight into thegeochemical process responsible for elevated arsenic

concentrations in di�erent hydrogeological environ-ments.

TOXICITY

The toxicology of arsenic is a complex phenom-enon as arsenic is considered to be an essential el-ement also. Two types of toxicity, viz., acute andsub-acute are known from long time. The acute

arsenic poisoning requiring prompt medical atten-tion usually occurs through ingestion of contami-nated food or drink. The major early manifestation

due to acute arsenic poisoning include burning anddryness of the mouth and throat, dysphasia, colickyabnormal pain, projectile vomiting, profuse diar-

rhea, and hematuria. The muscular cramps, facialedema and cardiac abnormalities, shock candevelop rapidly as a result of dehydration (Done

and Peart, 1971).Sub-acute arsenic toxicity mainly involves the res-

piratory, gastro-intestinal, cardio-vascular, nervousand haematopoietic systems. It may cause loss of

appetite, nausea and some vomiting, dry throat,shooting pains, diarrhea, nervous weakness, tinglingof the hands and feet, jaundice and erythema.

Longer exposure resulted in dry, falling hair, brittleloose nails, eczema, darken skin exfoliation and ahormy condition of the palms and soles (Holmquist,

1951; Pinto and Mcgill, 1953). The toxicities of var-ious arsenic compounds to man and animals havebeen studied by various workers (Sullivan, 1969;USEPA (United States Environmental Protection

Agency), 1971; Fairchild et al., 1977). Chatterjee(1994) has discussed the toxicity of arsenic to di�er-ent organs.

Biologically, As(III) is considered more toxicthan As(V) (NAS (National Academy of Sciences),1977). Data on the di�erences in toxicity between

As(III) and As(V) on human beings are very lim-ited. Trivalent arsenic is about 60 times more toxicthan oxidized pentavalent state (Ferguson and

Gavis, 1972). Inorganic arsenic compounds areabout 100 times more toxic than organic arseniccompounds (DMMA and MMAA) (Nagy andKorom, 1983). Methylation of inorganic arsenic in

Arsenic: occurrence, toxicity and speciation techniques 4305

the body is a detoxi®cation process, which reducesthe a�nity of the compound for tissue (Vahter and

Marafante, 1988).The assessment of arsenic pollution in soils and

plants is also important from the toxicity point of

view. Several studies have been conducted concern-ing arsenic and associated metals in stream sedi-ments, soils, and crop plants. The Wolfson

Geochemical Atlas of England and Wales clearlydelineates the major arsenic province in Devon andCornwall (Webb et al., 1978). Subsequent studies

comparing the distribution patters of arsenic instream sediments and soils have con®rmed extensivesoil contamination throughout southwest England(Colbourne et al., 1975; Abrahams and Thornton,

1987). The majority of this area is under agricul-tural use for arable and vegetable crop productionand for livestock farming. Thoresby and Thornton

(1979) have reported uptake of arsenic by pastureherbage grown on a soil contaminated with arsenic.The same ®ndings were also reported by Abrahams

(1983). However there is little evidence of signi®cantarsenic uptake into locally grown farm, horticul-tural and home garden crops. It can be concluded

that arsenic in these soils is present in forms thatare relatively insoluble and thus of low bioavailabil-ity (Thornton, 1995).Esser (1996) has studied the concentration of

arsenic in di�erent soils and plant samples in agri-cultural regions of Norway and reported that soilcultivation in¯uences the relative concentration of

arsenic in the topsoil. Distribution of arsenic insoils formed in the Indiana dunes has also been stu-died with respect to particle size, mineralogy, soil

depth, soil age (Esser et al., 1991a) and e�ect ofaerosol inputs with respect to distance from the pol-lution source, topography, vegetation and organicmatter (Esser et al., 1991b). There is obviously a

need for a multi-disciplinary study concerning en-vironmental pathways, food chain transfer ofarsenic and possible health e�ects due to consump-

tion of contaminated foods.

HEALTH HAZARDS

The results of clinical ®ndings for arsenic poison-ing from drinking arsenic contaminated water show

the presence of almost all the stages of arsenic clini-cal manifestation (Hotta, 1989). After the intake ofarsenic into the human body, approximately 50%

of the arsenic is excreted in the urine (Das, 1995;Das et al., 1995), with small portions through thefaeces, skin, hair, nails and lungs. Arsenic in urine,

faeces, skin, hair, nails and lungs has been used asan indicator of the arsenic hazard to the population(Borgono and Greiber, 1971; Goldsmith et al.,

1972; Yamamura and Yamauchi, 1980).People drinking arsenic contaminated water gen-

erally show arsenical skin lesions, which are a latemanifestation of arsenic toxicity. Long term ex-

posure to arsenic contaminated water may lead tovarious diseases such as conjunctivitis, hyperkerato-

sis, hyperpigmentation, cardiovascular diseases, dis-turbance in the peripheral vascular and nervoussystems, skin cancer, gangrene, leucomelonisis, non

pitting swelling, hepatomegaly and splenomegaly(Kiping, 1977; WHO (World Health Organisation),1981; Pershagen, 1983). The e�ects on the lungs,

uterus, genitourinary tract and other parts of thebody have been detected in the advance stages ofarsenic toxicity. Besides, high concentrations of

arsenic in drinking water also result in an increasein stillbirths and spontaneous abortions (Csanadyand Straub, 1995).Arsenic contamination in ground water of Tai-

wan is well known (Lu, 1990a,b) and has resultedin arsenism and black-foot disease in people drink-ing contaminated ground water. Some cases of can-

cer are also prevalent in the endemic areas (Chemet al., 1988). In Antofagasta, over 12% of the popu-lation exhibiting dermatological manifestations re-

lated to arsenic due to consumption of high arseniccontaining drinking water (Borgono and Greiber,1972). Chronic arsenic poisoning was also reported

in some parts of North Mexico (Cebrian et al.,1983). The exposed population of the regionshowed one of the cutaneous signs of chronicarsenic poisoning. A similar incident involving

arsenic was also reported from Cardoba Province,north of Argentina (Astol® et al., 1981). Regularintake of arsenic contaminated water resulted in

skin cancer. The problem of arsenic contaminationin ground water of West Bengal, India has beenclaimed as the biggest calamity in the world (Chat-

terjee, 1994; Das et al., 1994, 1995; Chatterjee et al.,1995; Mandal et al., 1996). Other incidents invol-ving smaller population groups have been reportedin Poland, Minnesota, USA, Chile, North Mexico,

Argentina, Canada, Hungary, Japan, New Zealand,and Spain and have been compiled by Chatterjee(1994). The important ®nding in most of these cases

was the close relationship between the prevalence ofcutaneous lesions and the exposure to drinkingwater containing high levels of arsenic.

SPECIATION TECHNIQUES

The concept of speciation dates back to 1954when Goldberg (1954) introduced the concept ofspeciation to improve the understanding of the bio-

geochemical cycling of trace elements in seawater.Kinetic and thermodynamic information togetherwith analytical data made it possible to di�erentiate

between oxidized vs reduced, complexed or chelatedvs free metal ions in solution and dissolved betweenparticulate species.

Florence (1982) has de®ned the term speciationanalysis as the determination of the individual phy-sico-chemical forms of the element, which togethermake up its total concentration in a sample.

C. K. Jain and I. Ali4306

According to Lung (1990), speciation analysis

involves the use of analytical methods that can pro-vide information about the physico-chemical formsof the elements. Schroeder (1989) distinguishes

physical speciation, which involves di�erentiation ofthe physical size or the physical properties of themetal, and chemical speciation, which entails the

di�erentiation among the various chemical forms.The elements occur in the environment in di�er-

ent oxidation states and form various species.Di�erent species of the same element may havedi�erent chemical and toxicological properties.

Therefore, determination of the total concentrationof an element may not provide information aboutthe actual physico-chemical forms of the element,

required for understanding its toxicity, biotrans-formation, etc. Thus, in order to obtain information

on toxicity and biotransformation of elements inaquatic systems, quanti®cation of individual speciesof an element is needed.

The fundamental requirement in element specia-tion is the need to quantitatively determine each ofthe forms of a given element independently and

without interference from the other forms. In thisregard, an ideal element speciation method is one

that can provide the desired information withoutaltering the original sample. In the absence of sucha method, elemental speciation has relied on a com-

bination of analytical techniques and method-ologies, including spectroscopic, chromatographic,and electrochemical procedures. In many instances,

physico-chemical approaches have been employed,whereby all forms of the element of interest are

converted into one species and quanti®ed.The quanti®cation of di�erent metal species is a

rather di�cult job as the concentration of heavy

metals in the environment are generally very lowrelative to the detection limits of the available ana-lytical techniques. However, during recent years a

number of approaches have been employed to over-come this problem. In the following pages a

detailed discussion is presented on the various tech-niques available for arsenic speciation, viz., spectro-scopic, chromatographic and electrochemical

methods, etc.A number of techniques are available for specia-

tion of arsenic compounds (Irgolic et al., 1983;

Ebdon et al., 1988). Spectrometric methods for thedetermination of arsenic involve the use of various

spectrometric techniques such as UV, visible,atomic absorption, atomic emission, hydride gener-ation, graphite furnace, etc. The most widely

accepted procedures for the analysis of total arsenicexploit the reduction of arsenic compounds to gas-eous arsine. This gas then either undergoes a calori-

metric reaction (Kellen and Jaselskis, 1976) or isthermally decomposed to give elemental arsenic for

atomic absorption spectrometry (Chu et al., 1972).Howard and Arbab-Zavar (1980) has developed a

spectrometric method for di�erential determination

of As(III) and As(V) species using silver diethyl-

dithiocarbamate. Spectroscopic methods based onthe formation of molybdenum blue have also beenreported for arsenic speciation (Bogdanova, 1984;

Matsubara et al., 1987; Nasu and Kan, 1988;Tamari et al., 1989; Palanivelu et al., 1992). Aggettand Aspell (1976) has developed a method in which

control of pH of sodium tetraborate(III) reductionsolution was used to di�erentiate between As(III)

and total arsenic, prior to analysis by atomicabsorption spectrometry.Hydride generation atomic absorption spec-

trometry is one of the most widely used methodsfor arsenic speciation due to its high sensitivity, lowdetection limit and high selectivity (Andreae, 1977;

Howard and Arbab-Zavar, 1981; Aggett and Haya-shi, 1987; Aggett and Boyes, 1989; Howard and

Comber, 1992). Flow injection hydride generationatomic absorption spectrometry has also been usedfor arsenic speciation in water and urine, and in

digested hair, nail and skin-scale samples (Chatter-jee et al., 1995; Das et al., 1995). Reports are alsoavailable for arsenic speciation using graphite fur-

nace (Shaikh and Tallman, 1978; Chakraborti et al.,1980, 1986, 1987; Chung et al., 1984). Howard and

Arbab-Zavar (1981) described a microprocessorbased ¯ow injection analysis system (FIAS) hydridegenerator for accurate, fast and easy experimen-

tation. Arsenic speciation by ion-exchange separ-ation followed by AAS determination has beenreported (Grabinsk, 1981; Aggett and Kadwani,

1983).Non-dispersive atomic absorption spectrometry

for hydride-forming elements has also been devel-oped. Compared to conventional dispersive AASsystems, this non-dispersive systems allow operation

of the electrodeless discharge lamp (EDL) forarsenic with high sensitivity and lower detectionlimit (Haraguchi et al., 1981). Recently, a method

has been developed for the determination of traceamounts of As(III) and total arsenic with L-cysteineas prereductant using ¯ow injection hydride gener-

ation coupled with a non-dispersive AAS device(Yin et al., 1996). Determination of arsenic by

inductively coupled plasma atomic emission spec-trometry (ICP-AES) has also been developed with adetection limit below 0.1 mg/l (Pahlavanpour et al.,

1980).Chromatographic techniques o�er excellent possi-

bilities for separation of all arsenic species. Typicalgas chromatographic methods involve conversion ofinorganic and methylated arsenic compounds into

their diethyldithiocarbamate complexes or tri-methylsilyl derivatives (Butts and Rainey, 1971;Henry and Thorpe, 1978). The approach of Berman

and co-workers (Braman and Foreback, 1973),however, involves the trapping of arsines formed byreduction with sodium tetrahydroborate, and their

subsequent sequential volatilization into an electricdischarge emission detector.


Gas chromatography with ¯ame ionization detec-

tor has been used for the speciation of arsenicspecies (Beckermann, 1982; Ballin et al. 1994) witha detection limit of 0.1 ng. Methods have also been

developed based on headspace gas chromatographyfollowing a chemical reaction and using ¯ame ioniz-ation detector. Arsenic species have also been deter-

mined by capillary gas chromatography usingmicrowave induced plasma atomic emission spec-

trometer as the detector (Lobiniski and Adams,1993).With the development of high performance liquid

chromatography (HPLC) and other chromato-graphic techniques, a variety of separation modeshave been employed to distinguish among di�erent

species, followed by calorimetric, spectroscopic, orelectrochemical detection of the separated species

(Van Loon, 1979; Eckho� et al., 1982; Nisamanee-pong et al., 1984; Haswell et al., 1985; Rauret et al.,1991; Robards et al., 1991; Hakala and Pyy, 1992;

Morita and Edmonds, 1992; Lopez et al. 1993; Leet al., 1994; Hagege et al., 1995). Where metalspecies are involved, chromatographic separation

can take place either by direct separation of metalions using ion exchange columns or by adsorption

(reversed- or normal-phase) liquid chromatographyif the metal species are complexed with organicligands. Irgolic et al. (1983) has described high per-

formance liquid chromatography (HPLC) in combi-nation with inductively coupled plasma atomicemission spectrometry (ICP-AES). High sensitivity

has been achieved using ICP-MS (mass spec-trometry) in combination with HPLC (Beaucheminet al., 1989; Heitkemper et al., 1989; Hansen et al.,

1992). The coupling of mass spectroscopy with ICP(Batley and Low, 1989; Rauret et al., 1991; Hakala

and Pyy, 1992; Hansen et al., 1992; Morita andEdmonds, 1992; Branch et al., 1994) is the moste�ective detector in HPLC speciation studies.

Arsenite, arsenate, DMA and MMA have been spe-ciated by HPLC using the coupling of mass spec-trometry with ICP (Beauchemin et al., 1989;

Harrison and Rapsomanikis, 1989; Krull, 1991;Rauret et al., 1991; Sheppared et al., 1992; Shum et

al., 1992; Weber, 1993; Demesmay et al., 1994; Leet al., 1994). While numerous methodologies havebeen developed employing HPLC where complexed

metals in clinical, environmental, and agriculturalsamples are separated, the main drawback of thisapproach stems from the incompatibility of com-

monly used mobile phase system with the ¯ame andplasma sources commonly used in atomic spec-trometry.

The hyphenated techniques, HPLC±HGAAS(Tye et al., 1985; Hakala and Pyy, 1992) and

HPLC±HGAES (Rauret et al., 1991) are now beingwidely used for arsenic speciation. Super criticalliquid chromatography is another development in

the ®eld of arsenic speciation (Laintz et al., 1992).A relatively new and fast growing chromato-

graphic approach that seems to overcome the limi-tations of HPLC is ion chromatography (IC). The

fundamental separation scheme involved here is ionexchange. Ion chromatography with conductivitydetection has been used for the determination of

arsenate in the presence of other ions (Hoover andYager, 1984; Hemmings and Jones, 1991). Li et al.(1995) has speciated arsenite and arsenate using ion

chromatography with electrochemical detection.The columns generally used with ion chromatog-raphy include ion exchange, ion exclusion, etc.

(BDH, 1988; Korksich, 1989). Various detectionsystems employed in ion chromatography includepotentiometric, atomic spectrometry (AAS or AES)and photometric measurements after postcolumn

derivatization of the separated species (Haddad andAlexander, 1985; Kondratyunok and Schwedt,1988). Ion chromatographic methods can be used to

separate organic and inorganic ions, complex aswell as simple ions, and neutral species. The tech-nique is particularly suitable for metal speciation in

aqueous solutions.Polarography and voltametry techniques have

also been used for the speciation of arsenic (Flor-

ence, 1986). Anodic pulse voltameter, with a detec-tion limit of 0.2 ppb, has been used to di�erentiatebetween arsenite and arsenate (Pretty et al., 1990,1992). Total arsenic concentration is determined by

anodic voltametry by reducing As(V) into As(III)using SO2 (Pretty et al., 1993). Recently capillaryelectrophoresis has been used for the speciation of

inorganic and organic species (Gareil, 1990a,b;Lopez et al., 1993). It has also been coupled withmass spectrometry (Lopez-Sanchez et al., 1994).

CONCLUSIONS

Arsenic contamination in natural water is aworld wide problem and has become a challenge

for the world scientists. The toxic e�ects of arsenicare related to its oxidation state, resulting inincreasing interests in the quantitative determi-

nation of individual species. Speciation of trace el-ements has become an important issue during thepast decade because of its impact on environmentalchemistry, eco- and clinical toxicology and food

and energy related industries. Various approacheshave been developed for speciation studies ofarsenic with its own advantages and limitations.

However, research e�orts are still needed to developinexpensive, rapid, sensitive and reproducible meth-odologies for arsenic species capable of working in

the range of drinking water limits. It is obvious toconclude that geographical distribution of arsenic,quanti®cation of di�erent species, their solubility

and bioavailability, and understanding of geochem-ical processes responsible for elevated arsenic con-centration in the environment is very much neededfor e�ective management of water resources.


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