mineralogy and chemistry of urinary stones: patients from north jordan

ORIGINAL PAPER

Mineralogy and chemistry of urinary stones: patientsfrom North Jordan

Iyad Ahmed Abboud

Received: 22 June 2007 / Accepted: 16 November 2007

� Springer Science+Business Media B.V. 2007

Abstract Urinary stone diseases are increasing in

the Middle East. The majority of urinary stone cases

are found in the northern part of the country. Stone

samples taken from patients living in the Irbid area

were collected from Princess Basma Hospital. The

present study concentrates on the mineralogical and

chemical composition of the urinary stones and on

the effective environmental factors that assist in

developing the different types of urinary stones.

Using X-ray diffraction techniques, the mineralogical

composition of the urinary stones was found to be as

follows: oxalate, cholesten, and uric acid, with

cystine stones occuring more frequently than the

others. Cholesten and calcium oxalate stones are the

most dominant types of stones. Calcium oxalate is the

most common type of oxalate stone. Calcium oxalate

is represented in: whewellite, wheddellite, and cal-

cium carbonate oxalate hydrate minerals, in addition

to other minerals such as brushite, ammonium

phosphate, vaterite, valleriite, and bobierrite from

other types of stones. Bobierrite (phosphate group) is

a new mineral reported in urinary stones, and this has

not been determined in any previous study world-

wide. Apatite (calcium phosphate) is deduced using

scanning electron microscope (SEM) images. The

SEM technique determined crystal forms and

systems, shapes, morphological features, and the

names of the minerals forming urine stones, while

optical properties are studied by polarizing micro-

scope. X-ray fluorescence technique determined the

concentrations of major and some trace elements. It

revealed that Ca is the main constituent of the urinary

stones, especially those composed of calcium oxalate

and calcium phosphate. The concentration of trace

elements was Ba = 1.57, P = 3.61, Fe = 1.78,

S = 2.08, Zr = 4.63, Mo = 3.92, Cu = 1.89,

Co = 1.56, and F = 4.2% and was higher in the

urinary stones of Jordanian patients than in foreigners

in the country. Questionnaires completed by patients

suggest that the most significant factors directly

effecting the formation of stones are water, climate

conditions, food rich in protein and rich in different

chemicals. Moreover, some drugs and diseases might

also help in developing other stones.

Keywords Urinary stones � Renal stones � Kidney

stones � Calcium oxalate � Medical geochemistry �Medical geology � X-ray diffraction � X-ray

fluorescence

Introduction

Human life is not possible without renal function, but

urinary stones can quickly lead to failure of the

kidneys, which is life threatening. Urinary stones are

I. A. Abboud (&)

Institute of Earth and Environmental Sciences,

Al al-Bayt University, Al-Mafraq, Jordan

e-mail: [email protected];

[email protected]

123

Environ Geochem Health

DOI 10.1007/s10653-007-9128-7

hard masses developed from organic materials and

inorganic crystals (mainly of calcium, phosphate,

magnesium salts, oxalate, and/or uric acid) that

separate from the urine and build up on the ureter

and/or on the inner surface of the kidney. Its size

varies from that of a grain of sand to a golf ball

(Fig. 1). Bladder stones may develop a single, often

large stone or many smaller ones, even several

thousands (Fig. 1) (Encyclopedia Britannica Article

2005).

Urinary stones are formed when there is a high

concentration level of certain substances, especially

calcium, oxalate, cystine, uric acid in the urine, lack

of citrate in the urine, or insufficient water in the

kidneys to dissolve waste products. Urine normally

contains chemicals—citrate, magnesium, and pyro-

phosphate—that prevent the formation of crystals.

Crystals of urinary stones may also be formed if the

urine becomes too concentrated, too acidic, or too

alkaline (Encyclopedia Britannica Article 2005, Kid-

ney stone 2005). Low levels of the elements

mentioned previously can contribute to the formation

of kidney stones. Of these elements, citrate is thought

to be the most important. Urinary stones are usually

formed inside the kidney, but they are sometimes

found in the bladder or ureter.

Most urinary stones are formed due to dietary

factors (Finlayson 1974; Robertson et al. 1980; Sobhi

2006) such as the high intake of dairy products or

salts that increase the amount of Ca in the urine. Low

intake of water would increase the percentage of

stones in the urine (Robertson et al. 1980; Sobhi

2006). Genetic effects and intake of vitamin C may

also play a role in forming the stones (Finlayson

1974; Robertson et al. 1980; Benton et al. 1997;

Sobhi 2006). Factors that can cause changes in the

urine and stone formation include the effects of

heredity, diet, drugs, climate, lifestyle factors, and

certain medical conditions (Encyclopedia Britannica

Article 2005, Kidney stone 2005). Statistical studies

show that men (Robertson et al. 1980; Dajani et al.

1988; Lee et al. 1992; Gentle et al. 1997; Sobhi

2006) aged from 20 to 40 years (Finlayson 1974;

Robertson et al. 1980; Lee et al. 1992; Mhelan 1992;

Gentle et al. 1997; Yagisawa et al. 1999) have the

highest risk. People living in arid areas have the

highest incidence rates. The common diets in these

areas are usually vegetables and tea (Sobhi 2006).

Urinary stones may contain various combinations

of chemicals. The most common type of stones is

comprised of calcium in combination with either

oxalate (Dajani et al. 1988; Mhelan 1992; Yagisawa

et al. 1999) or phosphate. Struvite stone is a less

common type that is caused by infection in the

urinary tract. Uric acid stone, however, is much less

common than struvite stone. Cystine is a rare stone.

Physicians do not always know what causes a

stone to form. Certain food may promote stone

formation in people who are susceptible (Sobhi

2006). Scientists do not believe that eating any

specific food causes stones to form in people who are

not susceptible. A person with a family history of

kidney stones may be more likely to develop stones

(Encyclopedia Britannica Article 2005, Kidney stone

2005).

Urinary stones have become increasingly common

in most parts of the world (Anderson 1969; Hodgkin-

son and Marshall 1975; Hodgkinson 1977). Countries

in the Middle East (especially Jordan) are categorized

in the Afro-Asian stone belt and fall within the tropical

Fig. 1 Ideal size of two

representative samples of

urinary stones, ranging from

the size of sand particles to

golf balls


123

and subtropical regions that (Robertson et al. 1980;

Sobhi 2006) have consistently reported a high inci-

dence of urolithiasis (Rizvi et al. 2002) with a high

incidence among children (Freundlich et al. 1982;

Dajani et al. 1988). A specific problem of the Middle

East region is the neglected asymptomatic large and

staghorn calculi that present with renal failure (Gupta

et al. 1985; Husain et al. 1995). Although much has

been published on this subject, very little information

has emerged from this area (Remzi 1980; Remzi et al.

1984; Tellaloglu and Ander 1984). Calculus disease of

the urinary tract is common in the Arabian Gulf States

(Sjovall 1986; Sobhi 2006), but reports on the disease

are scarce. Several studies have examined the factors

predisposing to the formation of urinary and kidney

stones (Hesse et al. 1976; Oka et al. 1989; Grases et al.

1990; Martin et al. 1992; Pierratos et al. 1994). The

analysis of urinary calculi by chemical methods only is

rather unsatisfactory (Prien et al. 1947).

Stone disease is two to three times more common

in males than in females (Dajani et al. 1988; Hassan

and Dubbagh 1988; Andrew and Chandru 2001). It

occurs more often in adults than in elderly people and

more often in elderly people than in children (Dajani

et al. 1988). Whites are affected more often than

persons of Asian ethnicity, who are affected more

often than blacks. In addition, urolithiasis occurs

more frequently in hot, arid areas than in temperate

regions (Andrew and Chandru 2001). Decreased fluid

intake and consequent urine concentration are among

the most important factors influencing stone forma-

tion. Dietary oxalate is another possible cause, but the

role of dietary calcium is less clear, and calcium

restriction is no longer universally recommended

(Curhan et al. 1993).

Epidemiological data in Jordan lack any informa-

tion about urinary stone disease. Very few

biochemical studies have been carried out on this

disease, and the contributions of metabolic factors

have not been investigated. These studies were

mostly limited to clinical and chemical analysis of

stones collected from the patients (Dajani et al. 1981,

1988; Mhelan 1992). The increasing frequency of

stones in north Jordan, with different epidemiological

factors and diseases, and different effects depend on

water quality and high-amount intakes of protein

from green leaf plants, eggs, milk, red and white

meats, etc. All of these reasons prompted us to carry

out a mineralogical and chemical analysis of urinary

stones. This study demonstrates the role of mineral-

ogy and chemistry (type and concentration of

elements) in our stones and therefore the reasons

for the formation of urinary stones in the patients

from north Jordan.

Materials and methods

Field work

Ninety urinary stone samples of different types

(renal, bladder, and ureter) were collected from 135

patients (69 males and 66 females). Their ages varied

from 18 to 75 years with an average age of 30 years.

Samples of stones were taken from patients under-

going surgery for urinary stone removal from patients

at the Princess Basma Hospital (PBH) of Irbid City,

Jordan, from 1 September 2004 to 31 December

2005. All stones removed during surgery were placed

in polyethylene air dry bottles and transferred to be

studied in the labs of Al al-Bayt University. All

polyethylene bottles were labeled with the name, sex,

age, weight, and marital status of the patient and the

date of surgery.

Synchronized with collecting samples, question-

naires were filled out to collect information about

patients infected with stones of different types, such

as their age, weight, and other social information.

Laboratory work

Mineralogical identification

The mineralogical composition of different types of

urinary stones was determined by polarizing micro-

scope (PM).

With polarizing microscope, it was possible to

establish the presence of crystalline and amorphous

materials and obtain optical constants that are

helpful in identifying and differentiating these

materials. Some optical properties that could be

determined are crystal form, optical sign, type of

extinction, interference color, and the presence of

birefringence.

The objective of polarizing microscopy study is to

visualize the nucleus, the crystal system and structure

and to describe the order of component deposition.


123

The true nucleus is always invisible and altered

because it is the first material to aggregate and to

precipitate from urine solution (Joost and Tessadri

1983; Fru et al. 2004; Sobhi 2006). The nucleus is

either a region from which crystalline forms radiate

or a geometric center surrounded by concentric

laminations. Nucleus forms from the precipitation

of crystals from supersaturated urine, from micro-

scopic debris in urine, from drugs, from foreign

bodies, or from calcium plaques in the renal papillae

(Sobhi 2006). Finding any of these components gives

a clue to the petrogenesis of the urinary stones. All

stone specimens were first examined for shape, habit,

size, and color. They were classified as cholesterol,

black, or brown-pigmented stones and were exam-

ined under a polarized microscope.

The composition of the urinary stone grains was

determined by X-ray diffraction (XRD) as described

previously. The percentage of cholesterol, oxalate

minerals, calcium carbonate, phosphate minerals, and

amorphous materials was determined. XRD analyses

were carried out in Al al-Bayt University labs, where

30 selected large urinary stone samples were prepared

for determination of minerals using X-Pert Pro XRD

systems. The urinary stone samples were pretreated

with H2O2 to leach and remove remains of organic

matter. Each sample was washed with distilled water,

then heated to 100�C overnight. After that, samples

were exposed to crushing in an an agate mortar and

made into a fine powder, then pellet stups were made

for analysis. All stones were analyzed routinely by X-

ray diffraction using Philips X-ray diffraction with a

nickel-filtered Cu Ka-beam with a generator voltage

of 40 kV and generator current of 45 mA. The

scanning speed of the goniometer was 2�/min and the

angle range (2h) between 3� and 60�, after which the

mineralogical composition was determined semi-

quantitatively by X-ray powder diffraction. Oxalate,

cholesten, uric acid, and cystine were detected in 17

renal, 11 bladder, and 2 ureter urinary stone samples

(Table 1). Calcium (vaterite and fluorite) and oxalate

stones (calcium oxalate: whewellite, weddellite and

calcium carbonate oxalate hydrate) were identified by

means of Ca; calcium phosphate (brushite, ammo-

nium calcium phosphate and calcium glycerol

phosphate oxalate) by Ca + P; magnesium phosphate

(bobierrite) by Mg + P; cholesten by C–H–O com-

pounds; cystine by S and uric acid by C–H–O–N

compounds (Table 2).

Some samples were selected to represent all the

collected stones and were analyzed by scanning

electron microscope (SEM; Philips XL-600 ESEM)

located at the Institute of Earth and Environmental

Sciences, Al al-Bayt University; this analysis was

made to identify the morphology of stones, crystal

form, and mineral type of urinary stones.

Chemical analyses

Thirty-four urinary stone samples of different types

were washed several times with de-ionized water

until they became free from urine and blood debris,

and finally they were washed in distilled water. Then,

they were dried, ground in agate mortar and homog-

enized chemically, and then they were made into

pellet stups pressed at 200 Kn pressure and analyzed

using X-ray fluorescence instrument-model Philips

Magix PW2424. Major and some trace elements were

measured as oxide in weight percentage (wt%) (see

Tables 5 and 6).

For some trace metal analysis, 30 mg of the

homogenized powder stones were dissolved in 1 ml

of concentrated boiling nitric acid (98%, Analar, BDH

Chemicals Ltd., Poole, UK). Digested aliquots were

diluted to volume and stored in polyethylene bottles

for subsequent analysis by Atomic Absorption Spec-

trophotometer (Perkin–Elmer, Model 703 & HGA-

500, Analytical Instruments, Al al-Bayt University)

with background correction. Seven major elements

(Na, Mg, Al, Si, Ca, K, and Fe) and 16 trace elements

(Ba, Mn, P, S, Zr, Mo, Cl, Sr, Ni, Zn, Cr, Co, F, Pb,

Cd, and As) were determined. Lead, cadmium and

arsenic concentrations were found to be below the

detection limit in all studied samples. Therefore, these

elements were not considered further. Details of all

procedure employed are described elsewhere (Even-

son and Warren 1975; Foote and Delves 1982).

Results

Mineralogy

The results of polarizing microscope study show that

the mineralogical components of the urinary stones

collected from patients from north Jordan can be


123

divided into the following types: oxalate stones and

brown color, dense and varied in shape from sub-

spherical to irregular shape. Oxalate stones show

moderately developed concentric and radiating lam-

inea texture with alternative brown to pale brown to

colorless whewellite laminae (Fig. 2). The alternative

laminea are concentrated around dark brown amor-

phous nuclei, and the stage of crystallization

increases toward the stones rim. Phosphate stones

were light to dull in tone building alternating

colorless to brownish zoned texture layers. Layers

of stones are built up around non-crystalline nuclei,

while the colorless layers are well crystalline radial

crystals of Ca-phosphate (Brushite and/or Bobierrite).

The bobierrite phosphate mineral has not been

determined in any previous study worldwide. The

pale brown layers are mainly ammonium phosphate

as seen from X-ray diffraction examination.

The mineral components of the urinary stones as

determined by the two techniques (XRD patterns and

then confirmed by SEM images) are presented in

Table 1. In Table 3 the type and percentages of all

Table 1 The mineralogical

composition results of

investigated urinary stone

analysis by X-ray

diffraction and scanning

electron microscope images

(SEM)

Sample type X-ray diffraction SEM (mineral image)

Oxalate Cholesten Uric acid Cystine

Renal X – – – Ca-oxalate monohydrate

Renal X – – – Ca-oxalate monohydrate

Renal X – – – Ca-oxalate, whewellite

Renal X – – – Wheddellite

Renal X – – – Wheddellite

Renal X – – – Whewellite

Renal X – – –

Renal X – – –

Renal X X – X

Renal X – X – Ca-oxalate and uric acid crystal

Renal – X – – Cholesten crystals

Renal – X – – Cholesten crystals

Renal – X – –

Renal – X – –

Renal – X X – Ca-carbonate (vaterite)

Renal – X X –

Renal – X X –

Bladder X X X –

Bladder X X X –

Bladder X X X –

Bladder X – X – Calcium phosphate

Bladder X – X – Calcium phosphate

Bladder X X – – Ca–P (brushite)

Bladder X X – – Mg–P (bobierrite)

Bladder X X – – Ca-oxalate, cholesten crystals

Bladder – X X –

Bladder – X X –

Bladder – – X – Uric acid crystals

Ureter – – X – Uric acid crystals

Ureter – X – X Cystine crystals


123

minerals detected by X-ray diffraction technique are

tabulated. The results indicate the following minerals:

calcium oxalate minerals (whewellite and weddelite)

that were identified by means of Ca (Table 2).

Calcium oxalate minerals are the chief constituent

in renal samples. However, it should be mentioned

that it was not detected in bladder stone samples as

shown in X-ray diffraction (Figs. 3–8). The SEM

image shows that calcium oxalate minerals are

characterized by a monoclinic system and platy-like

morphology, mainly with well-formed euhedral crys-

tal shape (Figs. 9, 10).

Cystine by S and carbon-hydrogen-nitrogen com-

pounds [mostly uric acid, uric acid dihydrate

Table 2 Minerals of urinary stones and chemical analysis of 30 samples with their detection by X-ray diffraction

Element Name of mineral Chemical formula Frequency

Ca Whewellite CaC2O4H2O Frequent

Weddellite CaC2O4 � 2H2O Frequent

Calcium carbonate oxalate hydrate Very rare

Vaterite CaCO3 Frequent

Fluorite CaF2 Very rare

Ca + U Calcium uranium oxide CaU2O7 Rare

Ca + Si Calcium silicon fluorohydrate CaSiF6 � 2H2O Rare

Ca + B Calcium borate Ca2B2O5 Rare

Ca + Al Calcium aluminum c… Ca6Al2(CO3)3… Very rare

Calcium aluminum o… C6H6Ca3O12 � Al… Very rare

Ca + Bi Beyerite CaBi2O2(CO3)2 Very rare

Ca + Si + Au Calcium gold silica CaAu2Si2 Very rare

Ca + Mn + Mg + Fe + P Jahnsite CaMnMg2Fe2(P…) Very rare

Ca + P Brushite CaPO3(OH) � 2H2O Very rare

Ammonium calcium phosphate (NH4)2Ca3(P2…) Very rare

Calcium glycero phosphate (oxalate) C3H7CaO6P… Very rare

P Ammonium phosphate (NH4PO3)3 Frequent

Mg + P Bobierrite Mg3(PO4)2 � 8H2O Frequent

Cu + P Likasite Cu6(NO3)2(P…) Very rare

U + P Uranyl hydrogen phosphate UO2(H2PO2)2 � H2O Frequent

Cs + Fe + P Cesium iron phosphate Cs3Fe2(PO4) Very rare

U Uranium oxalate hydrate C4O8U � 2H2O Rare

Mo Molybdenum oxalate C6MoO12 Rare

Ammonium molybdenum oxide (NH4)4Mo2O6 Rare

K + Mo Potassium molybdenum oxide K4MoO5 Frequent

K + W Potassium tungsten oxide K4WO5 Frequent

Pb + Al Dundasite Pb2Al4(CO3)4… Very rare

Mn + Si Tephroite Mn2SiO4 Very rare

Th Thorium oxalate C4O8Th Rare

Ce Cerium oxalate C6CeO12 Rare

Y Yttrium oxalate hydrate C6O12Y2 � 10H2O Rare

Y + Ca + Ln Fluorite, yttrium (Ca,Y)F2 or (Ca,Ln)F2 Very rare

Cu + Mg + Al Valleriite CuFeS2(MgO(AlO)) Frequent

C + H + O Cholesten C27H46O or C27H44O2 Frequent

C + H + O + N Uric acid C5H4N4O3 Frequent

C + H + O + N + S Cystine SCH2CH(NH)2COOH Very rare


123

(uricite)] (Table 2) is recognized in most renal

samples as shown in Figs. 6, 7; SEM image shows

uric as monoclinic and having a prismatic crystal

shape (Figs. 11, 12).

In a sample of bladder stone cholesten (choles-

terol) appears as the main mineral (Fig. 8), and the

SEM images show the rhombohedral-like shape for

cholesten crystals (Figs. 13, 14).

Only some samples show phosphatic minerals

[calcium phosphate (brushite)] by Ca and P

(Table 2), where the SEM images show calcium

phosphate as spherical and semi-spherical shaped

(Figs. 15, 16).

Mineralogical results are concurrent with previous

mineralogical studies (Al-Maliki 1998; Al-Fawwaz

2006). They found the main content of renal stones to

be calcium oxalate and uric acid; however, the main

mineral present in bladder stones is cholesten

(cholesterol).

Thirty urinary stones were analyzed mineralogi-

cally by X-ray diffraction and chemically by X-ray

fluorescence to detect the type of mineral and the

percentages of different elements. Calcium stones

form the majority (8 and 26.7%), five are cholesten/

uric acid (16.7%), four samples are cholesten (13.3%),

oxalate/cholesten, oxalate/uric acid and oxalate/

cholesten/uric acid are plotted in three samples for

each stone type (10%), one sample for each oxalate/

cholesten/cystine and cholesten/cystine stones (3.3%),

and only two samples are uric acid stones (6.7%)

(Table 4).

Chemistry of stones

The results of the chemical analysis of 34 urinary

stone samples selected from different patients

depended on the size and weight of the stone.

Tables 5 and 6 show the results of major and trace

elements and their mean and average concentrations,

respectively. Calcium elements have the highest

concentration, where the content of calcium as oxide

ranges between 11.8% and 95.3% with an average

value of 70.74% (Table 5). Calcium is considered as

the main constituent of the stones of all different

types. Ca content is obviously affected by the type of

food and drinks taken by patients, e.g., diary and milk

products, eggs, tea, and hard water (Robertson et al.

1980; Sobhi 2006). Comparing the Ca content in

urinary stone samples with that of water in north

Jordan, Irbid city, it is noted that there is a strong

relationship between them. This leads the researcher

to conclude that drinking water is the main source of

Ca (Abboud 2006). Renal stones have higher Ca

concentration than those present in bladder stones.

The Mg oxide content in all stone samples ranges

from 0.21–3.67% with an average value of 1.16%

(Table 5). The presence of magnesium in urinary

stones is usually considered an indicator of an

increase in their concentration in the human body

(Deeming and Wepu 1977). Foods, drinks, drugs, and

vitamins are responsible for Mg content (Sobhi

2006). The main source of Mg is a high concentration

in water (Abboud 2006).

Na and K oxide content ranges from 0.53–19.78%

and 0.0–5.57%, respectively, with an average value

of 3.33% and 1.05%, respectively (Table 5). The

main contributor to the presence of sodium and

potassium in the urinary stone samples is their

content in water (Abboud 2006) or from food

(Robertson et al. 1980; Sobhi 2006).

The element Fe is present in trace percents in most

urinary stone samples of different types. Their

contents range from 0.13–4.73% with an average

value of 1.78% (Table 5). Food and water are

responsible for the presence of Fe. Meats and beans

are considered the main source of Fe (Meranger and

Fig. 2 Stone no. 6. Concentric and radiate laminations of

whewellite mineral of calcium oxalate stone around invisible

nuclei (39)


123

Table 3 Type of samples and mineralogical composition percent results of investigated urinary stone analysis by X-ray diffraction

Sample type X-ray diffraction*

Oxalate stones

Renal CCOH (40%) + Whe (60%)

Renal CCOH (30%) + Whe (70%)

Renal CO: Wedd (30%) + Whe (70%)



Renal CO: Whe (100%)

Renal CAO&NHOH (50%)+AP&Jah (20%) + Vall (20%) + CAC&CSF (10%)

Renal CAO (80%) + PMO (20%)

Cholesten stones

Renal Ch (70%) + AP (30%)

Renal Ch (40%) + UHP (20%) + Vall (20%) + PTO (10%) + CSF (10%)

Renal Ch (30%) + AP&UHP (40%) + PMO&Tep (20%) + Bey&CSF&CB (10%)

Renal Ch (40%) + Vall (30%) + PMO (20%) + CBT (10%)

Oxalate/cholesten stones

Bladder YOH (35%) + Ch (40%) + AP&Bob&Bru (20%) + NC (5%)

Bladder CGPO (40%) + Ch (40%) + UHPH (20%)

Bladder PCO (30%) + Ch (40%) + AP (20%) + AMO&CB (10%)

Oxalate/uric acid

Renal CO (Whe) (20%)/UA (80%)

Bladder CeO (40%) + UA (40%) + PTO (20%)

Bladder CeO (50%) + UA (40%) + PTO (10%)

Oxalate/cholesten/uric acid

Bladder MO (30%) + Ch (30%) + UA (30%) + PMO (10%)

Bladder UOH (20%) + Ch (40%) + UA (20%) + Lik&CIP (10%) + PMO (5%) + Fl (5%)

Bladder TO (20%) + Ch (30%) + UA (20%) + AP&ACP (20%) + PMO (5%) + CGS&CDP (5%)

Oxalate/cholesten/cyctine

Renal YOH (20%) + Ch (40%) + Cys (30%) + AP (10%)

Urate (uric acid) stones

Bladder UA-Uricite (100%)

Ureter UA-Uricite (100%)

Cholesten/urate (uric acid) stones

Renal Ch (30%) + UA (20%) + AP&UHP (25%) + PMO (10%) + Vat (15%)

Renal Ch (30%) + UA (30%) + AP&UHP (20%) + PMO (10%) + Dun (10%)

Renal Ch (40%) + UA (30%) + Vat (30%)

Bladder Ch (40%) + UA (40%) + UHP (15%) + CUO (5%)

Bladder Ch (50%) + UA (30%) + AP (20%)

Cholesten/cystine stones

Ureter Ch (30%) + Cys (20%) + AP&UHP (30%) + Vat (20%)

CO: calcium oxalate, CCOH: calcium carbonate oxalate hydrate, Whe: whewellite, Wedd: weddellite, YOH: yttrium oxalate hydrate,

Ch: cholesten, UA: uric acid, Cys: cystine, PMO: potassium molybdenum oxide, PTO: potassium tungsten oxide, CSF: calcium

silicon fluorine, AP: ammonium phosphate, UHP: uranyl hydrogen phosphate, Vat: vaterite, Dun: dundasite, Vall: valleriite, UOH:

uranium oxalate hydrate, Lik: likasite, CIP: cesium iron phosphate, Fl: fluorite, TO: thorium oxalate, ACP: ammonium calcium

phosphate, CGS: calcium gold silica, CDP: calcium D1-Pantoth…, MO: molybdenum oxalate, CBT: calcium benzoatet…, CUO:

calcium uranium oxide, Tep: tephroite, Bey: beyerite, CB: calcium borate, Bob: bobierrite, Bru: brushite, NC: neodymium carbonate,

PCO: potassium calcium oxalate, AMO: ammonium molybdenum oxide, CGPO: calcium glycero phosphate oxalate, UHPH: uranyl

hydrogen phosphate hydrate, CAO: calcium aluminum oxalate, NHOH: neodymium hydrazin oxalate hydrate, Jah: jahnsite, CAC:

calcium aluminum carbonate

* The percentage is reached by comparing peak heights to those of pure substance (semi-quantitative)


123

Position [°2Theta]

10 20 30 40 50 60 70 80 90 100 110

Cou

nts

0

20

40

60

80 30_mesh.CAF(2).CAF

Fig. 3 X-ray diffraction

pattern of urinary sample

no. 30, containing calcium

oxalate minerals

(whewellite and weddellite)

Position [°2Theta]

10 20 30 40 50 60 70 80 90 100 110

Cou

nts

0

50

100

18_mesh.CAF



no. 18, containing

whewellite calcium oxalate

mineral

Position [°2Theta]

10 20 30 40 50 60 70 80 90 100 110

Cou

nts

0

50

100

150 sam27_1mary.CAF


pattern of urinary samples

no. 3 and 27, containing

calcium oxalate minerals

(whewellite and calcium

carbon oxalate hydrate)


123

Position [°2Theta]

10 20 30 40 50 60 70 80 90 100 110

Cou

nts

0

100

200 sample11_1m.CAF



no. 11, containing calcium

oxalate mineral

(whewellite) and uricite of

uric acid

Position [°2Theta]

10 20 30 40 50 60 70 80 90 100 110

Cou

nts

0

200

400

sam17_1mary.CAF



no. 17, containing uric acid

mineral (uricite)

Position [°2Theta]

10 20 30 40 50 60 70 80 90 100 110

Cou

nts

0

50

100

150

sam1default_1.CAF


pattern of urinary samples

no. 1 and 9, containing

cholesten mineral

(cholesterol)


123

Smith 1972). The Fe concentration in water is lower

than it is within the stones.

It was noticed that there were no concentrations of

toxic trace element such as Pb, Cd, and As. Water

samples collected from Irbid containede no Cd or As,

whereas some very small concentrations of Pb are

noticed (Abboud 2006). Most samples of urinary

stones have no concentrations of Cu. Five samples

had low Cu content ranging from 0.0% to 0.38%,

except one sample with 13.36% (Table 6).

Green vegetables, flour, milk products, and meats

are responsible for these concentrations. Water sam-

ples collected from Irbid city have very low

concentrations of Cu. Magnesium was detected in

seven samples of different types of urinary stones that

were analyzed, and the values rangefrom 0.1–1.9%.

Figs. 9, 10 SEM micro-

graph shows monoclinic

system and platy-like

morphology of calcium

oxalate crystals

Figs. 11, 12 SEM

micrograph shows: in

Fig. 11 uric acid crystals as

monoclinic and prismatic

crystals with monoclinic

system of weddellite

calcium oxalate mineral.

Figure 12 shows a

monoclinic system of uric

acid crystals

Figs. 13, 14 SEM

micrograph shows

rhombohedral-like shape of

cholesten crystals


123

The main sources of Mn are beans, tea, and green

vegetables (Mena et al. 1969). Ba, P, S, Zr, Mo, Cl,

Sr, Ni, Zn, Cr, Co, and F were detected in a few

samples in very low concentrations (Table 6).

Discussion

Hussein et al. (1989) reported many factors that play

a role in forming urinary stone, including age, sex,

obesity, diets, multiparty, recurrent infection, and

underlying liver disease.

Tables 7–11 show the impacts of various types of

urinary stones, sex (males 69, 51.1%: females 66,

48.9%), age (93.3% more than 30 years), marital

status (single 126, 93.3%: married 9, 6.7%), and

weight (91.9% more than 60 kg), respectively, on

stone formation in different patients.

Cholesten (cholesterol) stones are more abundant

in Irbid patients than any other type of stones (bladder

stones 80, 59.3%) (Tables 1 and 7). Etiological

reasons are the basis of this abundance and distribu-

tion in different patients. In the former type of

cholesten stone, cholesterol saturation of bile may be

an important prerequisite, but is not sufficient by itself

to produce cholesterol precipitation in vivo (liver

tissues?) (Halzbach et al. 1973; Abu-Farsakh 1997).

Cholesterol is normally stabilized by mixed micelles

of bile acids and phosphates. If the amount of

cholesterol becomes abnormal in bladder solutions,

it precipitates as cholesten minerals (cholesterol) and

results in the development of cholesterol bladder

stones (Abu-Farsakh 1997). Pigment stones (renal and

ureter stones 55, 40.7%) are composed of Ca biliru-

binate, phosphate, and carbonate. The cause of their

formation is commonly found in association with

hemolysis or cirrhosis (Ros et al. 1986; Abu-Farsakh

1997; Fru et al. 2004).

To determine urinary stone composition, there are

many possibilities offered by different technologies.

As may be seen in Tables 1, 5 and 6, all major

mineral and chemical components are identified

precisely by routine X-ray diffraction analysis and

X-ray fluorescence. Some minor phases are identified

by scanning electron microscope and polarizing

microscope. The limits of X-ray diffraction are

clearly shown when phosphate minerals (brushite

and calcium phosphate oxalate) are only minor

constituents. In three cases, the crystal components

were found by scanning electron examination. The

detection limit of X-ray diffraction is generally about

5% (Joost and Tessadri 1983), but crystalline crystals

can be seen by SE images as well.

Results of scanning electron microscope of blad-

der stones bile suggest the presence of rhombohedral-

like shaped cholesten crystals (cholesterol) (Figs. 13,

14), for oxalate a monoclinic system and platy-like

shape of calcium oxalate minerals (Figs. 9, 10),

monoclinic system and prismatic shape like of uric

acid crystals (Figs. 11, 12), for phosphate the calcium

phosphate crystals as spherical and semi-spherical

shaped (Figs. 15, 16) and for vaterite large mono-

clinic crystals confirm the presence of calcium

carbonate in the bladder stones (Fig. 20) (Nakai

et al. 2001). All stones were analyzed with X-ray

diffraction where cholesterol, calcium carbonate, and

amorphous material were detected. The components

of the amorphous material (vanadyl sulphate, cellu-

lose nitrate hydrate, trona salt, and oleandrin) are not

identifiable on X-ray diffraction examinations.

Figs. 15, 16 SEM image

showing spherical calcium

phosphate aggregate

crystals (spheroliths) and

spherical and semi-

spherical crystal aggregates

in Fig. 16 image


123

Nuclear magnetic resonance and elemental instru-

ments are used to identify the type of amorphous

substance and different micro-structure and micro-

composition. Insufficient detection of phosphate

minerals in uric acid (uricite) stones leads to impor-

tant clinical consequences. Alkalization therapy

should be avoided even if there is only a small

amount of phosphate mineral in the uric acid, because

the highest precipitation rate of phosphate is reached

in the alkaline pH range. An exact urinary pH control

is important if oxalate stones have a low phosphate

mineral content, and acidification below pH 6.2

might be necessary for metaphylaxis (Joost and

Tessadri 1983).

The results of whole chemical analysis by X-ray

fluorescence confirm the mineralogical results.

Table 2 shows the identification possibilities of stone

components by elemental analysis. For example, the

detection of calcium and phosphorus does not provide

absolute evidence for the presence of brushite, but the

Table 4 Frequency

distribution of the different

chemical constituents of

urinary stones collected

from adult patients

Components No. of stones

and no. of

patients

Percentage of total

no. of stones and %

of total no. of patients

1. Oxalate stones: 8 26.7

a. Calcium carbonate oxalate hydrate + whewellite 2

b. Calcium oxalate: weddellite + whewellite 3

c. Calcium oxalate: whewellite 1

d. Oxalate/phosphate/oxide 1

e. Oxalate/oxide 1

2. Cholesten stones: 4 13.3

a. Cholesten/phosphate 1

b. Cholesten/phosphate/oxide 2

c. Cholesten/oxide 1

3. Oxalate/cholesten stones: 3 10

a. Oxalate/cholesten/phosphate/carbonate 1

b. Oxalate/cholesten/phosphate 1

c. Oxalate/cholesten/phosphate/oxide 1

4. Oxalate/uric acid: 3 10

a. Calcium oxalate (whewellite)/uric acid 1

b. Oxalate/uric acid/oxide 2

5. Oxalate/cholesten/uric acid: 3 10

a. Oxalate/cholesten/uric acid/oxide 1

b. Oxalate/cholesten/uric acid/phosphate/oxide 2

6. Oxalate/cholesten/cystine: 1 3.3

a. Oxalate/cholesten/cystine/phosphate/oxide 1

7. Urate (uric acid) stones: 2 6.7

a. Uric acid/uricite 1

b. Uric acid/uricite 1

8. Cholesten/urate (uric acid) stones: 5 16.7

a. Cholesten/uric acid/phosphate/oxide 3

b. Cholesten/uric acid 1

c. Cholesten/uric acid/phosphate 1

9. Cholesten/cystine stones: 1 3.3

a. Cholesten/cystine/phosphate 1

30 100


123

rare occurrence of other Ca–P compounds make this

likely, and in addition a semi-quantitative analysis

(Ca:P ratio in the formula) is helpful.

Chemical analysis of urinary stones shows almost

very rare, frequent phosphate urinary stones (except

for ammonium phosphate, bobierrite, and uranyl

hydrogen phosphate, they are frequent), and this

indicates that the stones consist mainly of P, Ca, Mg,

and U oxides and trace amounts of Mn, Cu, Fe, and

Cs oxides with frequent C, H, and N elements

(Table 2).

Phosphate stones may belong to the non-infectious

urinary stones (Abdel-Halim et al. 1993; Sobhi

2006). Mineralogically, these stones consist of more

abundant phosphate minerals of ammonium phos-

phate, bobierrite, and uranyl hydrogen phosphate, and

some other trace minerals (Table 2).

In comparison, the oxalate urinary stones are poor

in phosphate and magnesium oxide and rich in

calcium oxide and C (Table 2). Oxalate stones may

belong to the infection stones (Abdel-Halim et al.

1993; Sobhi 2006). The cholesten, ureter and cystine

stones are rich in C, H and O, C, H, O and N and C,

H, O, N and S, respectively (Table 2). Cystine stones

occur individually with the relatively rare inherited

defect of urinary function causing cystinuria (Sobhi

2006).

SEM photos allow a morphological analysis of the

stone surfaces. Figure 17 shows a cystine crystal with

dissolution marks. The sample referring to this

patient was treated with Thiola, but litholysis was

not possible because of the bad kidney function (Joost

and Tessadri 1983). Figure 18 shows large a mono-

clinic weddellite crystal. Figure 15 shows calcium

phosphate spherolithes of about 3 lm diameter,

which seem to consist of smaller ones (Fig. 16,

0.3 lm in diameter).

Table 5 Concentration of major elements: results of different

types of urinary stone samples (wt%)

Element Concentration (%)

Bladder Renal Ureter All stones

Na Mean 2.19 5.16 3.87 3.33

Range 0.87–3.67 0.53–

19.78

1.85–5.89 0.53–19.78

Mg Mean 0.48 1.49 3.14 1.16

Range 0.21–1.56 0.33–3.67 2.83–3.45 0.21–3.67

Al Mean 1.42 3.12 12.53 2.84

Range 0.16–3.31 0.45–11.3 11.5–

13.56

0.16–13.56

Si Mean 1.15 3.96 8.85 2.60

Range 0.21–2.99 0.64–10.4 5.71–

11.98

0.21–11.98

Ca Mean 76.30 66.46 39.47 70.74

Range 47.65–

88.80

11.8–95.3 24.7–

53.24

11.80–

95.30

K Mean 0.42 1.49 0.53 1.05

Range 0.19–0.98 0.19–5.57 0.00–1.06 0.00–5.57

Fe Mean 1.33 1.12 2.25 1.78

Range 0.23–4.12 0.13–4.73 2.05–2.45 0.13–4.73

Table 6 Concentration of trace elements results of different

types of urinary stone samples (wt%)

Element Concentration (%)

Bladder Renal Ureter All stones

Ba Mean 0.49 0.11 n.d. 1.57

Range 0.91–4.96 0.12–0.93 n.d. 0.12–4.96

Mn Mean 0.57 0.05 0.46 0.76

Range 0.23–1.90 0.10–0.16 n.d.–0.92 0.10–1.90

P Mean 4.35 2.48 2.95 3.61

Range 1.17–10.1 0.59–8.58 0.58–5.33 0.58–10.1

S Mean 1.76 2.26 3.13 2.08

Range 0.22–5.36 0.31–5.36 1.34–4.91 0.22–5.36

Zr Mean 4.61 5.10 1.98 4.63

Range 0.14–26.38 0.25–26.38 0.98–2.99 0.14–26.38

Mo Mean 1.98 4.47 10.19 3.92

Range 0.65–7.88 0.45–17.91 2.89–17.49 0.45–17.91

Cl Mean 0.56 0.73 0.64 0.93

Range 0.22–1.87 1.09–2.61 0.61–0.67 0.22–2.61

Sr Mean 0.16 n.d. n.d. 0.24

Range 0.06–0.89 n.d. n.d. 0.06–0.89

Cu Mean 1.04 n.d n.d. 1.89

Range 0.15–13.36 n.d. n.d. 0.15–13.36

Ni Mean 0.11 0.62 1.10 0.70

Range 0.09–0.44 0.02–2.03 0.99–1.20 0.02–2.03

Zn Mean 0.16 0.13 n.d. 0.30

Range 0.01–0.76 0.02–1.30 n.d. 0.01–1.30

Cr Mean 0.17 0.21 0.97 0.46

Range 0.07–0.98 0.03–1.97 n.d.–1.94 0.03–1.97

Co Mean 0.24 1.28 0.77 1.56

Range 0.19–0.90 0.11–11.06 n.d.–1.54 0.11–11.06

F Mean 0.90 0.01 7.78 4.20

Range 0.54–8.33 n.d.–0.10 n.d.–15.58 0.54–15.58


123

Interpretation of these spherolithes remains con-

troversial. Some assume that they represent only one

of the many crystalline forms of apatite. Others think

that they might be the nidus for stone formation

(Leusmann 1981; Joost and Tessadri 1983). These

spherolithes could be traced in one of our samples

only. Figures 19–24 show well crystalline brushite,

vaterite, whewellite and calcium oxalate monohy-

drate, uric acid and cystine, and cholesten, calcium

oxalate and calcium carbonate (vaterite) mineral,

respectively.

The percentage incidence of oxalate, phosphate,

and urate stones in patients from north of Jordan is

lower than that reported in Iraq (Aziz et al. 1985;

Hassan and Dabbagh 1988; Al-Maliki 1998) and in

Egypt (Hammoud et al. 1973) and similar to that

reported from the Arabian Gulf States (Sobhi 2006)

and to those from western countries (Fellstrom et al.

1986a, b).

Countries in the Mediterranean area (Jordan is a

part of this area) extend from the hot and arid climate

with high temperature in summer exceeding 40�C.

Climate with such conditions plays a major role in the

incidence of urolithiasis (Al-Naam et al. 1987; Fre-

undlich et al. 1982; Rizvi et al. 2002; Sobhi 2006).

The increase of animal protein intake and carbohy-

drate foods leads to an increase of oxalate and urate

stones in patients (Robertson et al. 1978; Robertson

and Peacock 1982; Parks et al. 1994; Sobhi 2006). In

Jordan, people normally consume diets rich in animal

meat, milk proteins, and sugar. These diets can cause

changes in the chemical composition of urine and

play a role in forming calcium oxalate and uric acid

stones.

To prevent stone formation and reduce the risk of

stones, it is highly recommended to minimize eating

foods rich in oxalate (such as: chocolate, coca,

cheese, yogurt, oranges, apples, spinach, coffee, milk,

tea, vitamin C, etc.) because more than 85% of the

135 patients eat these foods in high amounts daily. In

turn, we recommend eating natural fiber foods, flakes,

and black bread. As obvious in Table 12, more than

90% of the 135 patients drink less than 2 l daily. As a

Table 7 Type of urinary

stones and number of

patients

Sample

type

No. of patients

(stones)

Percentage of

stones

No. of stones studied

by XRF

Percentage of stones

studied by XRF

Bladder 80 59.3 20 58.8

Renal 50 37 12 35.3

Ureter 5 3.7 2 5.9

Total 135 100 34 100

Table 8 Sex of patients and frequency (135 patients)

Sex Frequency Percent (%)

Male 69 51.1

Female 66 48.9

Total 135 100

Table 9 Age of patients and frequency (135 patients)

Age (years) Frequency Percent (%)

\30 9 6.7

31–45 55 40.7

[45 71 52.6

Total 135 100

Table 10 Marital status of patients and frequency (135

patients)

Marital status Frequency Percent (%)

Single 126 93.3

Married 9 6.7

Total 135 100

Table 11 Weight of patients and frequency (135 patients)

Weight (kg) Frequency Percent (%)

\60 11 8.1

60–90 100 74.1

[90 24 17.8

Total 135 100


123

result, we recommend drinking large amounts of

mineral water to reduce the concentration and

precipitation of the Ca ions responsible for forming

calcium oxalate in the urinary system that are present

in high concentrations in the water provided by the

Water Authority.

Figs. 17, 18 SEM images.

Figure 17 shows cystine

crystals with partial

dissolution marks; Fig. 18

shows a big monoclinic

crystal of weddellite


Figure 19 shows an

aggregate of arrangement

brushite crystals (calcium

phosphate); Fig. 20 shows a

big monoclinic crystal of

vaterite (calcium carbonate)


Figure 21 shows platy-like

whewellite (calcium

oxalate); Fig. 22 shows an

arrangement crystal of

calcium oxalate

monohydrate mineral


123

Acknowledgments This research was sponsored by a grant

from Al al-Bayt University. The author highly appreciates the

efforts of Professor Dr. Nadher Al Ansari, Dr. Ali Ahmed Bani

Nasser and Mr. Musa Al-Zghoul during all stages of this

research.

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mineralogy and chemistry of urinary stones: patients from north jordan

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