Derivatograph-QMS system in geochemical research

ThermochimicaActa, 92 (1985) 395-398 Elsevier Science Publishers B.V., Amsterdam

DERIVATOGRAPH-QMS

Gyula

SYSTEM

Kossuth

Szijar, of

RESEARCH

Department

and

Geology,

Debre-

Nuclear

Research

Hungary Institute

Sohatka, of

GEOCHEMICAL

University,

Mineralogy

ten, Sandor

IN

the

of

Hung.

Debrecen,

Aced.

of

Sci.

/ATOMKI/

Hungary

ABSTRACT A quadrupole mass spectrometer /ATOMKI, Hungary/ is coupled to The complex thermoanalytical a Derivatograph /MOM, Hungary/. method has been successfully applied in many fields of mineralogy, Some examples of the combined analysis petrology and geochemistry. are shown.

INTRODUCTION A quadrupole a Derivatograph

mass

spectrometer

[3].

The

evolved

and

sensitive

TG,

DTG and

instrument.

DTA This

conventional sulphate,

clay

materials

[2,

analysis

EGA

by

combined

TGT-EGA

the

well

and

[4]

to

organic

has to

been

carry

coupled

out

to

complex

simultaneously

known

was used

method

technique

mineral

[1,2]

possible

gas

analyses

/QMS/

QMS makes

with

the

thermoanalytical

parallel

determine

content

with

the

carbonate,

rocks

of

and building

53 . METHOD

The /MOM,

instruments Hungary/,

KI , Hungary/ in

placed establish used

and

reference gases

capillary

tion

The is.

Proceedings

and

a smell filter

about

unit 0.5

of ICTA 85,

ml/s,

be

heating from

Bratislava

was

the

flow

was

rate the

was

time

up

to is

maintained

10

200

into

50

‘C,

ms.

its The

was

‘C/min.

through

end

were to

A1203

furnace

introduced

/ATOM-

samples

sampling.

low-pressure

heated

response

He

‘C

QMS-300

/ATOMKI/.

dynamic

portion at

can

l/s

for the

type

system

200

pumped

a molecular coupling

sampling

and were

Derivatograph-1000

spectrometer,

atmosphere

inert

via

experiments:

mass

crucibles.

inert

evolved

long

the

a dynamic

platinum

pole

in

quadrupole

the

as

The

ry.

used

of

a

the

m

quadru-

the gas

1.2

capillaconsump-

QMS has

a mass

- 396 range

of

Faraday

l-300 cup.

amu and Ultimate

a sensitivity pressure

of

is

4*10m4

less

than

A/mbar

1010’~

with

mbar

without

baking.

RESULTS The the by

Pleistocene

Keszthely low

yellow

hydrous

iron

sulphate

combined

of

minerals. the

H20

as

thermoanalytical

components

ICPDS

and

complex

cemented

the

In

The

X-ray

cards

no.

copiapite(MGo rhomboclase

Minor

amounts

Uzsa

/NE

marcasite

weathered

of

locali.,ty

rhe

rock

surfaces

were

[S]

using

diffraction and

69Alo

30)

showed S and

27-245

( Fe:+56A10.44) H20. ;he

F;?H[S04j2*4

of

part

deposited

this

20-659

investigations

/Fig.l/.

at

by

activity. on

minerals

l19.7

(0%

main

hydrothermal

datp the

(s04)6

is

incrustrations

standard

indicated

gravel

Hungary/

temperature

vivid

the

fluviatile

Mts.,

H20

and

CO2

indicated

SO2

as

+

-7

OTA AT

/

f

L

DTG dm/dt TG ;:,

1 ; 0

/

u-. \

\

39.73 QMS AP 24.66 c.

11,64

.H \ .

To

Fig.

1.

200

DTA,

LOO

DTG,

curves copiapite

of

600

ml

TG and a mixture and

1000

To

r*c1

QMS-EGA of

rhomboclase

Fig.2.

260

DTA, curves

-1

100

‘00

DTG,

TG and

of

mellite

100

QMS-EGA

- 397 impurities H20

and

suggested of

in SO3

the

X-ray

diffraction.

by

of

and

the

The

gases.

the

rhomboclase

territory

evolved

verified

ratio

of

calculated

copiapite

This

second

one

is

of

the

weight

ratio

and

rhoqboclase

first

known

copiapite

in

the

of

occurence

present

day

Hungary.

+

$

OTA

AT OTG dm/dt

TG

Am

I,41 % I,55 % 1.!5 % 1,61

coo

200

6

0

T

IV

*do

%

4

,600

coo

IPC1

390 oc

0

Fig.3.

40

20

Thermoanalytical

and

QMS-EGA

Teresztenye-2/11.

borehole,

H20/18/,

H2S/34/

C02/44/,

continously recorded carrier

detected. at gas/.

390

‘C

100

80

60

analysis 48.25

and

02,

Ar

of

oil

numbers

mass are

I

shale

from

m,

mass

A complete /N2,

M [a mu

41.66

spectrum

impurities

were was

in

the

He

- 398 Mellite 16 /?/

/hydrated H20/

Basin

and

is

a very

occures

Transdanubia, was

alumfnium

QMS-EGA

endothermic At and

oil

sediments.

Two

while

in

produced

North

Ir

the

in

case

oil

the

are

of

shale

of

to

water

in

calcite

and

siderite

fleresztenye with lagoon

and

facies

were

pyrite

gas

facies

oxydative

in

first

/thermoanalysis,

the

gel

accumulated

DTG,

boreholes,

processes

under

the

ingression

investigations

mellite

DTA,

formula.

shallow

diagenetic

or

Carpatic

of

our in

the

Pannonian

In

the

H20

Csordakut,

Hungar.y

some

Upper

decomposed

protobitumens

content

moles

spectroscopy/. was

water

Borsod-Karst,

there

in of

loss

g-16

instrumental

material

aliphatic

of

unique

According

the

39.73

is

/?/

desposit

crystal

present.

characteristic by

chromatography, organic

The

/Fig.2/

layers

distinguished

coal

.

villages/

shale

It

brown

the

is

foreground

Sziiliisardo

have

to

records

process

the

[7]

up

Al2[Cl2012]~18

mineral.

Eocene

Hungary

controversial

TG and

rare

in

mellate,

the

circumstances, facies

reductive

typical environment

/Fig.3/.

CONCLUSION The

examples DTG,

DTA

ous

TG,

the

characterization

for

geochemical The

and

the and

in

this

QMS-EGA of

paper

demonstrate

technique

geological

is

that

a very

materials,

simultane-

helpful

it

is

a

means basic

in

method

research.

QMS completes

identifies inDTG

reported

evolved

TG evaluation

the

Derivatograph

inorganic and

and fairly

in

this

organic fast

combination: gas

compared

products, to

it helps

the

thermoprocesses.

REFERENCES

I. Berecz, S. Bohatka, 3. Gal and A. Paal, ATOMKI Kozl. 19 (1977) 123. r Berecz, S. Bohatka, G. Langer and G. Szoiir, Intern. 3. Of Mass Spectrometry and Ion Physics. 47(1983)273. Simultaneoz Thermoanalytical Paulik and F, Paulik, J. Examinations by Means of the Derivatograph, Elsevier Sci. Publ. Co, 1981. F. Paulik and M. Arnold, 3. of Thermal Anal. J. Paulik, 25 (1982) 327. x Sz68r, E. Balazs, S. Bohatka, Epit8anyag. 9(1984)274. G, SziiCjr and I. Viczian, Ann. Rep. ‘6f the Hungarian M. Kozak, Geol. Institute. /In press/ T. Weiszburg, Asvanygytijtb Figyelo, Hungary 2(1984)4.