Automation of the Perkin - Elmer DSC 2

Thermochimica Acta, 151 (1989) 283-288 Elsevier Science Publishers B.V., Amsterdam

-Printed

in The Netherlands

AUTOMATION

ELMER

DSC

K.-P.

OF

THE

283

PERKIN-

2*

Friihauf

Technische

PhJsik.

Uni\,ersitXt

ties

Saarlandes.

6600

Saarbrtkken.

F.R.G.

.\BS TR.\CT \\.ith help of the interface system TRIF.\CE’ \\e ace able to control and to measu~~c the heat flow without read its displayed temperature. modification. Our soft\\are aIlo\\s simultaneous measurements of all \\ell as efficient and \ersatilr data anahsis and representation. \\‘ith a digital multimeter the reproducibilit? and the resolution of the DSC hale been impro\rd.

the DSC 2. to an> hard\\are quantities as high accurac) measurements

ISDRODUCTION

. the DSC 2 is either

Sormall) puter.

Thece

arc

nual!\

supervise

ana 1~sis and hale

the

\\are

has

machine

\\ritten

and

.\UTO\I.\TION

its

calorimeter.

for lo\\

flo\\.

measurement

\\as

carried

b_~ measuring

the

wcocdec

c-ommuni~~atrs

into

~ia

system

the

into

the

are

measured

same

moment.

Elmer.

heat

an

to control

the

is spread

.\T.\RI

ST

DSC

computer

Tel;troni\’

Second!\.

To atoiti

\\ide!\.

old

corn-

it is nec’essar?

the measurements. not t)ossible.

\\hic.h

out

or

the

\\ith The

an!

to

data

disatl\antages

computer and

of

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these

control

because

interfacze Realtime

signal

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Per-kin

-

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bZor~vsII;.

’

Tektronix.

must

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be

of the

DSC

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temperature

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all

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DSC

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are

D-hf>,o3

Publishers

B.V.

Sulrbnch/Saar

of

the

2 (outbinS

;I11 three triggered

flo\\ 01’ 2 \.)

TRIF.\CE

module

temperature clock.

9.

heat 0.2

system DSC

c.omputer

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Science

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The

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B‘,,.nr\\-assrr-st,..

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of

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interface

tlispla~

the

help

measured.

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001-6031/89/$03.50

vat)ac.it>

temperature.

IEEE-Bus

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computel-.

tities

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an

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costs.

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(:onnector)

out are

system

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methods

PRINCIPLE

To measure

interface

to car-r>

- an interface

been

possibilities

manual!\

1, ith these

representations

an interface

h1trrfac.e

(controlled

pi-oblems

graphic

tleteloped

RS ?3:!

t\\o

reading quanat

the

The DSC module and cool rature

buttc>ns. limits

had

be replaced

alread:

baseline

module

as ~rll

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the

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of the

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data

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this

data

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sample

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2,

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material. storrcl

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at

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r\rl.>

0.1

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time

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as

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as

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times.

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system

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isothermal

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o

rela?

temperature.

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final

slope

the

interface

directly

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measurement

equilibrium

t-if the

thr

the

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hole.

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final

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and

starting

isot hrrma

and

wsolution

samlxlr

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best

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thermal

data

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at

the final

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the

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as outer-

switches

modules.

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the

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to swh

is identical

Ithen

to\\aI-ds

is subtracted. fits

toitage

beharinui-

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xottagcs

prwedu~~a

al-p a\eragetl

resolution

linear

isothet-ma1

offset

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isothermal

be interrupted

measurement

\\ell and

relevant

1)~ D.\-<.onxrrtar

I \\ill start

rc la\ation

as

rate

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measurements

ground

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measurement. the

heat

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or cooling sequence

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e(luilil~~iun~

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records

heating

program

determine

the

<.ontt-olIing

In the future.

s houltl

D.\-con\rrtrr

an actual

program

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and

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as the

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manualI>.

module

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rktr-onic:aI?\

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cedure. On the

mal

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measurements

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time

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select

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temprratur-r.

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heating

ltet\xeen

night

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0 and

9999

minute:

time

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isother-

time

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transition.

c\ch the

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sample In thi>

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all instruments

into

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values

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). Thp

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T,cc...ccT,. (fig.1

T:,

if the

measured

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:\t

used

to

measured take

into

286

account

a steplike

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the event

terial. the

behaliour

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transition.

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the

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sample

degree

baseline.

procedure

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in slope

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the

I
11=320.42

3,04

2,85

-

2,66

-

heat

capacity

assumes

that

and

not

change

of the

l-2)

in literature.

clefs.

nessung :c331 MeBbereich:300 / 365 Rate/Range:5 / 0.2 TU :325.92

_ T3~326.46 # k.!

\\hich

the

of comerted

determines

procedure

of

after-

during

yet

value

the

ther-

converted and

the

maslope

Datun/Zeit:26.02.1989/10:12:56 t4ass.z Ensl:8.048 Konnentar :430/300/029.2/902 PeakflYche:l.7551 / 11=319.95 T2=323.02 T3=332.34 T4=334.22

T2=323.62 T4=327.83

and

2.1886

of

J/s

TV2

” 2,47

-

2,28

_

321

Fig. 1.

Screencq)>

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To determine Using

the

the mouse must

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so-called

perature.

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333

onset

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338

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327 T/K

the measurement

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peratures

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324

the

on the

on the

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Fig.

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.

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287

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to finish

on screen copies the

can

the

description

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can

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RES ULTS During

our

measurements

temperature

of the

used.

? some

the

In fig.

reproducibility

header.

\\cf did not block

and

the

of

One

fig. 2) and

all runs

of the

“noise”.

cal~~ulatctl

the true

specific-

heat

The

~-e~~~~oduc~il~ilit~ as

+/-

:I\\..

The

times

20

isothermal

as goo~l as the

\alucs

Messung: Saphir tleBbereich:328 Rate/Range:5 /

I

I

Fig.

2. Screencop) in one cj-cle

“noise” can

/ 468 0.2

I

sho\\ing night.

the

and

as

the

the

than

br attainrd

+/-

\\ith

2 :!\\-. this

from

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the

of

heat empt:

(Y.CI.O line in all mrasul-e-

aI\\a~s

machine

better

\alues

Iwfore

ilre

than three

automation.

Datun/Zeit:23.05.1989/22:06:42 Masse Cnsl 31.137 Konmentar :

:

I

~~r~~l-o(lLI(:it~ilit?. and line corresponds

I

I

I

I

420

the

“noise” with

450

of

is

within

specific

measurement

\\ere

390 T/K

The ~cro

he seen

measurement

“noise”

the

cooling

to demonstrate

I;. The

is subtracted

s( arming

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same

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t alibration

to control

cold

can

h: and

I

368

during

one

are

information 320

it> of saijphire

as

regulator On!\

sample

rrlc\ant

\\ith

capa~ \\rll

that

trmperature pan holders.

Iwt\\ren

is taken

I

330

done

Some tir,nr

fi\-e measurements

ments.

the

c,n a sapl)hirr

\\ere are

USC an?

surrounding

measurements

.\II measurements

capacities pans.

metal

five

one of the

measurements measurements.

CONCLLlSION \\‘ith heat

the

described

capacity

\\ith

measurements takes and

on!\

an

soft\\are

and

impro\rd

I.rl~~~~~(luc.il)ilit\ anti

require a few

transition

\erj

moments

pans.

the

pans

taken

intoaccount.

measurements h> any

laboratory

measurement

as dell

user

as the

This

the

fast

speed

The control data

heat

is obtained

analysis

measure

heat

though

and

the

automatic

the

as

it

of transition. measurement

different

is easy

be handled

specific

The

a measurement

caljac-it?.

program can

can

“noise”.

c.ompleting

e\en

material.

and ana!\sis

one

a reduc~ed .\fter

specific:

of a reference

ensuing

interface

supervision.

to calculate

temperature.

of empt! are

little

the tle\elo~~d

\\eights

to use. a routine

The

matter

assistant.

REFERESCES

1 2

\\..H. Hemminger and G. Hiihnr. \\‘rinheim-N.I.. 1079. U. Bandana. Journal of Thermal

CruntllaKrn .\nal>sis.

drr

ltilor-imetrie.

31 (1980)

lOG3-1071

I’erlag

of DSC

Chemie.