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Chapter V

Evaporation of Underground and Sea brines using Artificial Pans

5.1 Introduction

101

The process of obtaining common salt and other marine chemicals, which are

dissolved in sea water or natural brine is entirely by gradual evaporation and fractional

separation of solids at different densities. The method by which common salt is

produced by solar evaporation is very much practiced in our country even before the

chemistry of salt was established. This method is utilized to different brines, depending

upon the prevailing climatic conditions, the geographical location of the sources and

the advancement of technical knowledge and its application. In western hemisphere,

where prolonged dry weather is uncommon, solar evaporation of either sea brine or

underground brine is not so feasible and salt is produced by mining of salt deposits or

by the artificial evaporation of the brines. In tropical countries like India, where long

dry weather exists, manufacture of salt by solar evaporation is followed and salt of very

good quality and quantity has been produced. 85

Evaporation is the chief operation involved in the manufacture of salt. A

number of factors are known which affect evaporation, both meteorological and

physical. They are the quantity of the dissolved substance or substances, radiation,

temperature, humidity, rainfall, wind, depth of water mass etc. Because of the

complicated relationship between these various factors, it is difficult to assess the

relative importance of each individual factor and therefore the combined effect of the

influencing factors on the rate of evaporation is only taken into consideration.86

(a) Dissolved substances

Since the solubility of sodium chloride is little affected with increase in

temperature, it crystallizes from brines on evaporation. The rate of evaporation and

consequently the concentration of a solution depends on4he quantities of substance or

102

substances dissolved in it. More the quantities of the dissolved substances, lesser is the

rate of evaporation. 87 Evaporation decreases by about one percent for every one percent

increase in salinity under identical conditions.

(b) Radiation

The change in the state of water from liquid to gas involves an utilization of

approximately 590 calories per gram of water. Solar radiation therefore plays a

considerable role and governs the main variations in the rate of evaporation

(c) Temperature

The air and water temperatures are largely dependent on solar radiation. Since,

the temperature of water surface governs the rate at which the water molecules leave

the surface and enter into overlaying air, evaporation rate increases at higher

temperatures. The ideal range of temperature is between a minimum of 20°C and a

maximum of 45°C. Evaporation rate falls appreciably when the air temperature drops

13

below 10°C.

(d) Wind velocity

Wind helps in the removal of air saturated with water vapour from the surface

of the evaporating body and bringing in contact with it fresh unsaturated layer of the

atmosphere thus increasing evaporation. A desirable range of wind speed which aids

evaporation is in excess of 1.34 m/s. 88 Evaporation rate can be correlated with wind

velocity only by having a weather station, which can record atleast for a period of one

year. Then only an approximation can be made on the wind velocity and effect on the

103

rate of evaporation. 89 Usually, wind blowing from northeast and northwest directions

in India is very much useful in enhancing the rate of evaporation.

(e) Humidity

With an increase in relative humidity, the capacity of the atmosphere to take up

more water vapour from the evaporating body decreases. Evaporation particularly

ceases to take place, when the relative humidity exceeds eighty percent. A strong

relationship exists between solar energy, radiation, humidity and evaporation go

(1) Rainfall

The net evaporation rate in a particular area depends on the total rainfall during

a year. Excessive rainfall makes solar salt production in many sites impractical. In

calculating the net evaporation, the following expression is used i.e., (gross evaporation

x evaporation factor) minus rainfall=net evaporation. 90 The occurrence of rainfall

frequently during the evaporation process, interferes by diluting the brine and reducing

the evaporation.

In the present study, which involved the evaporation of underground and sea

brines using artificial pans, all the above parameters except rainfall played a vital role.

The study was carried out approximately for a period of one month, especially in the

premonsoon period, thereby avoiding the interference of rainfall.

5.1.1 Study area

For the study of evaporation of underground (subsoil) and sea brines using

artificial pans, samples were collected from two different sources, viz., the salt-pans at

Sal L

pJ&TE -IZ. ARTIFICIAL PANS

'-S

PJ- 7 -/3 CRYSTALLIZATION OF SODIUM CHLORIDE FROM UNDERGROUND AND SEA BRINES OF ARTIFICIAL PANS

P1-A 7-6-/1 SODIUM CHLORIDE COLLECTED FROM ARTIFICIAL PANS

PL4TL-/r GYPSUM COLLECTED FROM ARTIFICIAL PANS

104

Puthalam, where underground (subsoil) brine is used and from the salt-pans at

Kovalam, where sea brine is used.

Put halam, is located about 8 km southwest of Nagercoil, the headquarters of

Kanyakumari district of Tamil Nadu.

Kovalam, is located 20 km south of Nagercoil and just 5 km northwest of

Kanyakumari, the southern tip of India.

5.2 Materials and Methods

10 litres each of the brine samples from Puthalam (underground brine) an

Kovalam (sea brine) were collected separately. The atmospheric temperature and the

baume degrees were noted. Then both the samples were exposed to sunlight in separate CpJodi f plastic buckets. Each bucket was labeled and the atmospheric temperature and the

baume degree of the brines were recorded daily. The decrease in volume of the two

different brines were monitored daily.

Gypsum (CaSO4.2H20) began to crystallize from 16°Be onwards and the

crystallization continued upto 25°Be. The formed gypsum of the two different brines

were collected completely, dried and weighed accurately. Similarly, from 25013e,

sodium chloride began to crystallize and it continued upto 29.5°Be. All the formed

crystals of sodium chloride from the two different brines were collected, dried and

weighed accurately.

Specimen samples of brines were separated at 10°13e, 15 013e, 20013e, 25°Be and

30°Be during the course of evaporation. Parameters such as temperature of the brine,

105

atmospheric temperature, percentage of chloride, sulphate, calcium and magnesium for

the samples were determined using standard procedures. 64 The amount of sodium and

potassium in the samples were determined using flame photometer/5'0

pH of the various samples were determined using standardized pH meter and

the electrical conductivity by Elico conductivity bridge.

5.3 Results and Discussion

The study on the evaporation of underground (subsoil) and sea brines by using

artificial pans were carried out and the various physico-chemical parameters were

determined for the above two different brines at various baume degrees. During the

course of evaporation, gypsum and sodium chloride crystallized at different range of

baume degrees were collected, dried, weighed and were compared.

During the evaporation of the two different brines, jormej gypsum formed was

collected and the amount of dry gypsum was 28.35 g for the underground brine and

33.20 g for the sea brine. It was observed that both brines contained more or less the

same amount of gypsum (Table 5a).

Similarly sodium chloride crystallized between 25°Be and 29.5°Be were also

collected, dried and weighed. The amount of sodium chloride was 310.45 g for the

underground brine, while it was 416.95 g for the sea brine (Table 5a). This indicated

that the sea brine had more sodium chloride than the underground brine, as expected.

Evaporation proceeds with a gradual decrease in the volume of brine. At the

beginning, the reduction in volume for the two different brines were around a litre a

day. As evaporation continued, the volume of brine got reduced by approximately 300-

U)

C

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w 0

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9-

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106

107

400 ml per day. At 30°Be, the volume of underground and sea brines were reduced to

0.250 ml and 0.230 ml respectively (Table 5b).

5.3.1 pH

Both underground (subsoil) and sea brine samples had the same pH initially i.e.,

7.2. Then, a gradual increase in the values were observed at l0°Be i.e., 7.6 for

underground brine and 7.3 for sea brine. But at 15 0Be, both the samples had similar

value i.e., 7.7. Then as maximum iron oxide and calcium carbonate got separated

before 20°Be, a gradual decrease in the values were observed and the minimum values

were at 30°Be. At 20°Be, the values were 7.4 and 7.6 for the under ground and sea

brines respectively. At 25°Be, the values were 7.3 for underground brine and 7.5 for

the sea brine. But at 30°Be, the values were found to be minimum i.e., 7.1 for

underground brine and 7.2 for sea brine. (Tables Sc and 5d).

5.3.2 Electrical conductivity (dsm')

Both underground (subsoil) and sea brines had almost similar values of

electrical conductivity in the beginning i.e., 52 dsm' for underground brine and 67

dsm' for the sea brine. As the baume degree increased, electrical conductivity also

increased steadily. At lO°Be, the values were 81 and 91 dsm for the underground and

sea brines respectively. But at 15°Be, the values were exactly similar i.e., 102 dsm for

both the different brines, and at 20°Be, the values were almost similar i.e., 103 dsm1

for underground brine and 104 dsm' for sea brine. At 25°Be, the values were 105 and

106 dsm for underground and sea brines respectively. This steady increase in the

electrical conductivity revealed that as evaporation proceeded, the concentration of

Table - 5b

108

Evaporation rate of Underground (Subsoil) and Sea brines

UNDERGROUND BRINE (PUTHALAM)

Brine Density

Volume (lit) °Be

SEA BRINE

(KOVALAM)

Brine Density

Volume (lit) *Be

10.000

6.00

4.00

10.000

5.00

9.200

6.50

9.100

5.25

8.665

7.00

8.710

5.50

8.210

7.25

8.300

6.00

7.520

8.00

7.620

6.50

6.800

8.50

6.950

7.00

6.275

9.50

6.460

7.50

5.725

10.00

5.940

8.50

5.150

11.25

5.375

9.25

4.800

12.00

5.000

10.00

4.400

12.75

4.625

10.75

4.075

13.50

4.325

11.75

3.725

14.25

4.000

12.25

3.650

15.00

3.850

14.00

3.000

15.50

3.725

15.50

2.550

16.50

3.350

17.50

2.200

18.00

2.975

20.00

1.870

20.00

2.625

22.50

1.575

22.00

2.300

25.00

1.350

25.50

1.820

26.50

1.050

26.00

1.570

27.50

0.760

26.50

1.320

29.00

0.475

27.00

1.000

30.00

0.250

27.50

0.770

 

29.00

0.470

30.00

0.230

109

5.1.a Evaporation rate of Underground (subsoil) Brine

12.0(

10.0c

8.0(

6.0(

4. OC

2.0(

[tJsI•IsI

 

'III]

12.000

10.000

8.000

6.000

> 4.000

2.000

0.000

I

I

6.00

Brine density (*Be)

5.2.a Evaporation rate of Sea Brine

I

I

7.25

I

I

I

9.50

I

I

I

12.00

I

I

I

14.25

I

I

16.50

Brine density (*Be)

111111

22.00

26.50

29.00

110

vious ions increased. But at 30°Be, a drop in the values was observed i.e., 101 dsm'

for underground brine and 102 dsm' for sea brine. This low value of electrical

conductivity at 30°Be was due to the removal of about 70% of sodium chloride before

30°Be (Tables 5c and 54)

5.3.3 Chloride (%)

A gradual increase in the percentage of chloride was observed for both

underground (subsoil) and sea brines and the values were maximum at 30°Be. Initially,

the percentage of chloride was 3.0% for underground and 4.0% for sea brines. At

10°Be, the values were 5.8% and 6.5% for the underground and sea brines respectively.

The values were 9.7% for the underground brine and 10.5% for the sea brine at 15°Be.

At 20°Be, the values were 14.6% and 15.0% for the underground and sea brines

respectively. At 25°Be, the values were 18.4% for underground brine and 18.8% for

sea brine. But at 30°Be, the underground brine had the maximum value of 22.7% while

the sea brine had 19.0%.

The low percentage of chloride at 30°Be for sea brine was due to the fact that it

had comparatively minimum amount of magnesium chloride than the underground

brine had. Moreover, sea brine had comparatively more sodium chloride and as

maximum amount got separated before 30°Be, the value is minimum at 30°Be for the

sea brine (Tables Sc and 5d).

5.3.4 Sulphate (%)

There was a gradual increase in the percentage of sulphate as baume degrees

increased for both the underground (subsoil) and sea brines and the maximum values

III

were observed at 30°Be. Though calcium sulphate was separated in the earlier level,

the maximum values of sulphate was due to the presence of magnesium sulphate and

potassium sulphate, as they got separated only after 30°Be. Initially the values were

0.40% and 0.74% for the underground and sea brines respectively. At I 0°Be, the

values were 0.56% for underground brine and 1.28% for sea brine. The values were

0.92% for underground brine and 1.70% for the sea brine at 15°Be. At 20 013e, the

values were 1.16% and 2.11% for the underground and sea brines respectively. At

25°Be, the values were 1.64% and 2.41% and at 30°Be, the values were maximum for

both the brines i.e., 3.86 % for underground brine and 4.92% for sea brine.

The higher percentage of sulphate in sea brine at 30°Be, indicated that it had

more sulphates of magnesium and potassium than underground brine had (Tables 5c

and 5d).

5.3.5 Calcium (%)

The percentage of calcium was found to increase upto 1 5°Be for both the

underground (subsoil) and sea brine samples. Since gypsum being collected before

20°Be, there was a gradual decrease in the percentage of calcium from 20°Be and the

minimum value was observed at 30°Be.

Initially, the values were 0.065% for underground (subsoil) brine and 0.046%

for sea brine. At 10°Be, the values were 0.120% and 0.058% for the underground and

sea brines respectively. The values were maximum at I 5°Be i.e., 0.182% and 0.099%.

Then before 20°Be, as 80% of calcium sulphate being removed, the value got reduced

at 20°Be i.e., 0.099% for underground brine and 0.074% for sea brine. At higher

112

baume degrees, the values were almost similar i.e., at 25 013e, the values were 0.077%

and 0.065% and at 30°Be, they were 0.068% and 0.062% for the underground and sea

brines respectively. This indicated that despite sea brine had lower initial

concentration, both the brine samples had almost similar percentage of calcium at

various baume degrees after the separation of calcium sulphate [Tables Sc and Sd].

5.3.6 Magnesium (%)

Initially the percentage of magnesium in both the underground (subsoil) and sea

brines were 0.32% and 0.25% respectively. At l0°Be, the values were 0.60% for

underground brine and 0.41 % for sea brine. The values were 0.96% and 0.59% for the

underground and sea brines respectively at I 5°Be. But at 20°Be, the values were

1.5 1% and 0.78% and at 25°Be, they were 1.85% and 1.08%. Both underground brine

and sea brine had the maximum value at 30°Be i.e., 3.90% and 2.99% respectively.

This clearly showed that underground brine had maximum magnesium chloride than

sea brine [Tables Sc and Sd].

5.3.7 Sodium (%)

Considering the percentage of sodium, as expected, the sea brine was richer

than the underground (subsoil) brine. Initially, it was 0.78% for underground brine and

0.95% for sea brine. At 10°Be, the values were 1.17% and 1.37%. At 15°Be, the

values were 1.48% and 1.70% and at 20°Be, it was 1.65% and 1.75%. But at 25013e,

the values were 1.82% for underground brine and 1.83% for sea brine. Then, there was

a drop in the values at 30°Be for both samples, because nearly 70% of crystallized

sodium chloride was separated before 30°Be and the values were 1.41% for

underground brine and 1.43% for sea brine. The high value in the two different bittern

113

samples revealed that some sodium chloride continued to remain with the samples even

at 30°Be [Table 5c and 5d].

5.3.8 Potassium (%)

As there was no separation of potassium salts until 30°Be, the values of the

percentage of potassium went on increasing for both underground (subsoil) and sea

brine samples and reached the maximum at 30°Be. This was evident from the fact that

potassium chloride and potassium sulphate get crystallized only between 32°Be and

38°Be.

The underground (subsoil) and sea brine samples had almost similar values at

all the different baume degrees. Initially, the values were 0.032% for underground

brine and 0.033% for the sea brine. At 10°Be, the values were exactly similar for both

samples and was 0.038%. At I 5°Be, the values were 0.044% and 0.045% and at

20°Be, it was 0.055% and 0.054%. The values were exactly similar at 25°Be for both

the brines i.e., 0.068%. But at 30°Be, the values differed marginally and were 0.080%

and 0.081% for the underground and sea brines respectively. This indicated that both

underground and sea brine samples had almost similar percentage of potassium salts at

different baume degrees. [Tables Sc and 5d].

5.4 Chemical Parameters of Salt Samples from Artificial Pans

During the evaporation of underground (subsoil) and sea brines using artificial

pans, the common salt crystallized were separated, dried and weighed. The salt

samples from the evaporation of underground and sea brines using artificial pans were

subjected to various studies involving the percentage of moisture, insoluble impurities,

114

Table - 5c

Physico - Chemical parameters of Underground (subsoil) brine at various baume degrees

A

B

C

D

E

F

G

H

I

J

K

4

29.0

31.0

7.2

52

3.0

0.40

0.065

0.32

0.78

0.032

10

30.5

32.0

7.6

81

5.8

0.56

0.120

0.60

1.17

0.038

15

30.0

30.5

7.7

102

9.7

0.92

0.182

0.96

1.48

0.044

20

31.5

31.0

7.4

103

14.6

1.16

0.099

1.51

1.65

0.055

25

30.0

30.5

7.3

105

18.4

1.64

0.077

1.85

1.82

0.068

30

31.0

31.0

7.1

101

22.7

3.86

0.068

3.90

1.41

0.080

Table - 5d Physico - Chemical parameters of Sea brine at various baume degrees

A

B

C

D

E

F

G

H

I

J

K

6

29.0

31.0

7.2

67

4.0

0.74

0.046

0.25

0.95

0.033

10

32.0

31.0

7.3

91

6.5

1.28

0.058

0.41

1.37

0.038

15

28.5

28.0

7.7

102

10.5

1.70

0.099

0.59

1.70

0.045

20

30.5

31.5

7.6

104

15.0

2.11

0.074

0.78

1.75

0.054

25

31.0

30.5

7.5

106

18.8

2.41

0.065

1.08

1.83

0.068

30

31.5

30.5

7.2

102

19.0

4.92

0.062

2.99

1.43

0.081

A - Brine density (° Be)

F

- Percentage of Chloride

B - Temperature of the brine (° C)

C

- Percentage of Sulphate

C - Atmospheric Temperature (° C)

H

- Percentage of Calcium

D - pH

-

Percentage of Magnesium

E - Electrical conductivity (dsm1)

J

-

Percentage of Sodium

K - Percentage of Potassium

115

calcium sulphate, magnesium sulphate, magnesium chloride and sodium chloride and

the results were compared and presented in Table 5e.

5.4.1 Moisture (%)

The percentage of moisture in the salt samples of underground (subsoil) and sea

brines were almost similar i.e., 0.93% for underground brine salt sample and 0.97% for

sea brine salt sample. This showed that despite the brine differed, there was no marked

difference in the amount of moisture in the samples.

5.4.2 Insoluble impurities (%)

The salt samples crystallized from the two different brines had almost similar

percentage of insoluble impurities i.e., 0.52% for underground brine salt sample and

0.58% for sea brine salt sample. As the experiment was carried out under similar

environment, there was no marked difference in the percentage of insoluble impurities.

5.4.3 Calcium sulphate (%)

The salt samples of the two different brines had almost similar percentage of

calcium sulphate. The sample of underground brine had a value of 1.09% , while sea

brine had 1.12%. This almost similarity in the values of percentage of calcium sulphate

revealed that both underground and sea brine had almost similar amount of calcium.

5.4.4 Magnesium sulphate (%)

The salt samples from the underground (subsoil) and sea brines had a marginal

difference in the percentage of magnesium sulphate i.e., the value was 1.14% for

underground brine salt sample and 1.21% for sea brine salt sample. This marginal

higher percentage of magnesium sulphate in sea brine salt sample indicated that the

116

sample had comparatively more amount of magnesium sulphate than underground brine

sample.

5.4.5 Magnesium chloride (%)

The salt samples crystallized from the two different brines had almost similar

percentage of magnesium chloride i.e., 1.01% for the sample of underground brine and

1.02% for that of sea brine. This similarity in the percentage of magnesium chloride

indicated that irrespective of the brines used for salt-making, it made no difference in

the magnesium chloride value.

5.4.6 Sodium chloride (%)

The percentage of sodium chloride for the salt samples of underground and sea

brines had marked difference. The salt sample of sea brine had a higher value of

93.22% while that of the underground sample had a lower value of 89.62%. This vast

difference in percentage of sodium chloride of the two different samples, indicated that

sea brine had comparatively more sodium chloride as expected.

The above various parameters clearly revealed that the salt samples from sea

brine had higher percentage of sodium chloride than underground brine sample. But

the percentage of all other parameters showed only marginal differences.

5.5 Chemical Parameters of Underground (subsoil) and Sea brine salt samples from Natural and Artificial Pans

This part involved a comparative study of the salt samples obtained from the

evaporation of underground and sea brines by artificial and by natural pans. For the

study of evaporation by artificial pans, underground (subsoil) brine from Puthalam salt-

works and sea-brine from Kovalam salt-works were used. The common salt

117

crystallized in the above two different brines were collected separately and dried.

Similarly, the mean value of the various parameters of the salt samples collected from

the natural evaporation of brines from Puthalam (underground brine) and Kovalam (sea

brine) were compared with the above samples, obtained by artificial pans. The samples

were analysed for various parameters like percentage of moisture, insoluble impurities,

calcium sulphate, magnesium sulphate, magnesium chloride and sodium chloride and

the values were presented in Table 5f.

5.5.1 Moisture (%)

The percentage of moisture of sodium chloride samples crystallized from the

artificial evaporation of underground (subsoil) and sea brines were almost similar i.e.,

underground brine had the value of 0.93% and sea brine had the value of 0.97%. But

the mean value of percentage of moisture for the samples collected from the natural

pans of Puthalam (underground brine) and Kovalam (sea brine) had high values i.e.,

1.70% and 1.87% respectively. The higher value for the samples of the two different

brines of natural evaporation was due to the fact that the crystallized salt was made into

a heap and some moisture continues to reside with the salt.

5.5.2 Insoluble impurities (%)

The value of insoluble impurities of the salt samples crystallized by the

evaporation of two different brines by artificial pans were almost similar i.e., the

sample from underground brine had a value of 0.52% and that of sea brine it was

0.58%. But the mean value of the salt samples collected from the natural evaporation

of two different brines from Puthalam and Kovalam had high values of 1.39% and

1.48% respectively.

(N

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118

119

The minimum value for the samples from artificial pans of underground and sea

brines were due to evaporation being made in plastic buckets which had lesser area of

exposure. This prevented the intrusion of dust by strong winds to some extent. But in

natural pans, as the area of exposure was maximum, the brines may be contaminated by

insoluble impurities carried by strong dusty winds.

5.5.3 Calcium sulphate (%)

The percentage of calcium sulphate for the two different samples crystallized

from the artificial pans of underground and sea brines were almost similar i.e., for

underground brine sample, it was 1.09% and for that of the sea brine sample, it was

1.12%. Similarly, the mean value of percentage of calcium sulphate for the samples

obtained from natural pans of underground and sea brines were 1.11% and 1.08%

respectively.

This indicated that despite the method of salt-making differed, the samples had

no marked difference in the percentage of calcium sulphate.

5.5.4 Magnesium sulphate (%)

The salt samples crystallized from the evaporation of underground (subsoil) and

sea brines by artificial pans had almost similar percentage of magnesium sulphate i.e.,

1.14% and 1.21% respectively. The mean values of percentage of magnesium sulphate

for the salt samples of the two different brines from the natural pans were also similar

i.e., 1.14% for the sample of underground brine and 1.15% for that of the sea brine

sample.

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This indicated that despite the mode of evaporation varied, the percentage of

magnesium sulphate in the salt samples had no characteristic difference.

5.5.5 Magnesium chloride (%)

The percentage of magnesium chloride for the salt samples crystallized from the

artificial pans of underground and sea brines were also almost similar i.e., 1.01% for

the underground brine sample and 1.02% for the sea brine sample. The mean value of

the salt samples of the two different brines from natural pans were also almost similar

i.e., 0.99% for the sample of underground brine and 0.94% for that of the sea brine

sample. This near similarity in the values of salt samples crystallized from both the

artificial and natural pans, clearly indicated that though the method of evaporation

varied, there was no marked difference in the percentage of magnesium chloride.

5.5.6 Sodium chloride (%)

The salt samples crystallized from the artificial pans of underground and sea

brines had marked difference in the percentage of sodium chloride. Sea brine sample

had maximum sodium chloride, as expected i.e., 93.22% while the sample of

underground brine had lesser percentage i.e., 89.62%.

A similar trend was also observed for the samples from natural pans. The mean

value of percentage of sodium chloride of the salt samples of two different brines were

91.99% for the underground brine salt sample and 93.33% for the sea brine salt sample.

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It was clear that the percentage of moisture and insoluble impurities of the salt

samples from artificial and natural pans showed a marked difference. But the other

parameters like percentage of calcium sulphate, magnesium sulphate, magnesium

chloride and sodium chloride for the salt samples of both underground and sea brines

were almost similar, even though the salt was separated from either artificial or natural

pans.