1H ABSORV ’05 SPECTRA VF
8CD" DIS'7L1-ONATE LN

Thesis 5°C)“ the Degree of M. a.

.‘MCHIGAN STATE COLLEGE.
Alexanderm
I939

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CD EQUAL/lbw Xh-BLLV‘LJHLILQIMULfi UBBIA It‘s

NICK; SULFATi SLLLTICnS

I: 7

Alexander killer 1—,.- . 2"

1

Suemitted in partial fulfilment of the requirements
for tLe degree of master of Science in tie
Graduate behool, Licnigen state College,
Degertuent of Cnemistry
June, 1939

A? E CIATICA

1

‘~ g . A 1 “...." 1 - .. "' 1 --~' v. ~ ,r '51-er r 3).“ . ‘\F\ 1
Tee writer aeei es heresy «.o acnecmleite “cur... em. llx'l-Ct-

.

eQnees to 3r. D. T. Ewrn; fer .is nelgful eugreeticre and

’-

éuiience duri;; tLe course cf this work.
To Ar. J. L. Vandenbelt, Sincere aygreciation for gis valu-
able cccre"etion and assistance in the develotuent of tnis

v
0

me thOd.

121506

LlCKiL SJLFATn.EQLLTIU“5
Introduction

Tne application of sgeotroknonetry to tne Huantita-
tive determination of constituents by means of absorition

ssectrum nae been recognized since 1573 by Vierordt (1).

This tater describes an acclication of tne soectrc-e
2'... La.
gnotoneter to tne quantitative deternination of sodium m-

benzeredisulfonate in nickel sulfate solutions. Data are
given snowin; tnat small quantities of sod‘un n-benzenedi—

O

sulfonate 1n nickel sulfate solution have a distinct and

characteristic absorntion egectra in the ultra violet re-

gion with maximum absorition at gooO A? and 2750 A9, \itn
assorstion extendin; from about 2/50 s? to EVCC A9. Takin;

'5

;dventa e of these two maximum absorition toints, and en-
;loyinb tn ex incticn coefficients, one is able to comgute
quantitatively tne concentration of sodium n-benzenedisul-
fonate. With carefully controlled workinb conditions, tne
extinction coefficient was found to be retroducable witn a
high degree of accuracy.

Sodium m-benzenedisulfcnate is used for a brightener
in nickel plating solutions, and uncn an estimation of
concentration is desired, tLe usua netnod of determination

is oy a Lrevinetric analysis as barium sulfate, union is

lo 5 and involves consideracle true and worn. Tne advan-

F4;

tabs c tne sgeotIOQnotonetric netnod is tnat it is ‘acid
and convenient.

Tne nrocedure for tnis netnod of analysis is based
ugon tne grincigal tnat tne .eroentaze transnittency of
light at a certain wave lengtn is a function of the concen-
tration of tne desired substance in tne solution. In re—
cert years sucn a method of measuring a constituent s;ec-
tropnotonetrically nas been anglied by nehli; to the deter-
ninetion of manganese in steel (2), iron in ores (3); to

1 . . ., _ . ..
conzer (4); to Vitamins and nornonee cy mCItOH (3); and

also to dyestuffs, by Erode (6) and Eolnes (7).

emcloye

a .- . ‘- ' ’
:L‘DiiF-l‘r' 31-9 {TIT 393C871-

transnittancy measurements

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In the nevrlejmcnt of tie nctréd, 9: files of sadiun n
b nzfinelieulfcr'te 1"ere accrrhtcly veigled out Fa” dissolved
in a xe;9“red voluen O; ECi nickel r“lfate wter cclution.
After tie solution 'ne tee solvent cell. have been lilled
(for preprrcticn sue belon‘, they are filled rith the re-
syective solution, nlaced on the suectrog Run, and the ab—

sorptiin snectrn at vrrisus shutter readings recorded on
the photogrnfihic flute. After develonnent, the siting are
vcsn=d one—half .our in runnin; rate , dried at room tex—
perature, and the absorption indicated on the slate by
means of ink dots at the points r"rem "iso-dlnsity rever—
sals" occu The resultin' curve may he fraphed, or, in
the Cit—terminatingr of en unknour can ls, the Hc"*rt itsnect—

-.o, -- .,
ed -r eruluzt
salts are ercr
ner went.

forei"n urterirl. Befdre this wrecuution was

0 neiterable vrriitio‘ "ts f‘unn in the re ultc
:dvisrrle to use tie crdirsry orgnnic solvents

these cells, as they dissolVe the cement which

cell together. It was faurd necessary to clean
by an initirl rinsir With tfic rat’r to runare

then several czreiul rirsin's vith distilled we

6:

n of tee cores
sed he fiercent

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2300 2h00 2500 2600 2700 2800
Wave lengths in Angstroms

Fig. I Absorption Curve of
Sodium m-berzenedisulfonate in Kickel Sulfate Solution

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Plate Cone. of Cone. of rlfl are? ”1% fivrn

nuxber disulfonnte TiSCh “‘CML‘ ”lee? "
if? T.CT 5’ 33.0 i no inflection
33h c.0637 2.M 16.0 15.7
621 0.033 30.0 13.6 16.1
aha 0.0:: 30.0 17.“ 16.2
631 “.0h0 30.0 20.6 17.7
637 0.033 30.0 20.3 1?.6
333 0.023 0.93 13.2 1n.u

 

 

r11J ~18 II
Analysis of unknown samples of Soli1. m—benzenedic1ilfcndte
in Kic :el sulfate solution

 

 

 

Plate Solution in p preserzt 5 found
r“ t‘r sclvcnt cell in solution s;cctr:cc0:i:.lly
631 r20 0.0205‘ 0.0203
637 H20 0.033 1.033
639 H20 0. 33 0.037
630 Izscn 0.030 0.033
638 £130 0.033 0.033
640 NiSOu 0.033 0.060

 

 

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The nickel sulfate solution has practically no absorp-
tion in the ultra violet (s), (0), and see Fig. II. On the
other hand, sodium m-benzenedisulfonate has no absorption
in the visible spectrum. This fact is remarkable, making
this method for the dete~hination of the disulfonate pos-
sible with no interference nor overlaping of the nickel

sulfate and the sodiun m-benzenedisulfonate absorption

bands. The disulfonate band extends from 2350 A? to 2800 A?
at 18 degrees, which the nickel sulfate band is from 3400 A?
to about 4700;?

Jones and Strong (8) in their studies on nickel sulfate
solutions indicate that the violet band for nickel sulfate
extends from 3700 A. to 4550 A.. However, the data obtained
with the instrument used by th writer, shows a wider band,
namely, from about 3400 A. to 4700 A., see Fig. II. Jones
and Strong also Show that the nickel sulfate absorption is
independent of the temperature. Extensive studies made by
Muller (9) on inorganic solutions indicate there are no de-
viations from Beer's law for nickel sulfate solutions.

In plating baths benzenedisulfonic acid is frequently
used as a brightener instead of the sodium salt, Ghosh and
Bisvas (10) have tested this acid and found the acid has

the same absorption as the sodium salt. Also in the in-
vestigation of Wright (11), the same result is confirmed.

Boric acid, which is added to a plating bath as a buffer,

 

 

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has no absorption in the region where the disulfonate absorp-
tion appears.

An interesting observation was the comparison of the
difference between the absorption curves for sodium mono-
benzenesulfonate and sodium m-benzenedisulfonate. The for-
ormer has three maxima and three minima, while the latter
has only two maxima and two minima. Incidently, the curve
of the sodium mono-benzenesulfonate is very similar to the
absorption curve of benzene, which has seven maxima and
seven minima (12). Apparently as more sulfonate groups are
attached to a benzene molecule, a greater difference in the
in the identity of the curve is obvious.

By inspection of Table III it is evident that the E
value for sodium m-benzenedisulfonate depends on the sol-
vent a:d solution. Uhen both cells cohtain nickel sulfate
(50;) solution, the 3 value is 19.0. When the solvent cell
contains ZOfl nickel sulfate and the solution cell, water,
the E Value increases from 19.0 to 20.2, making an increase
of 1.2 units, or 6.3; difference, a significant amount. It
appears from this that the presence of nickel sulfate adds
to the size of the E value. Since an increase of 1.2 units
in E value is due to absorption by nickel sulfate, and a
decrease of 5.2 units in the absence of nickel sulfate,
the difference of 2.0 units is evidently due to_the pres-

ence of nickel sulfate; 2.0 units would make a increase

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Literature Cited

f‘.

f3 '5. I ’."V "\ :1 "f- A " >‘ r "I. .~ 4— ‘
Viercrit, U18 hhnehuJLr 3.8 ..ectralon..rfiues BLT

LA;

9.
m
L:
H

Photometrie der Absorgtionagectren un

Quantitative chemiscnen Analyse. Tubigen,

 

1873

“enlig, J, P., Ind. Bab. Cgem., Anal.'2i. 7, a7 (1935)
Ibid. 7, 337 (1935)

Ibid. 9. 162 (1937)

hortcn, The Akgliczticn of Abso:;tioi Spectra to tLe

Study of Vitamins and Ecrmcnes, London, Adam

H, g - w. ; . 4 —ne finc
1

Eclues, Ina. Big, Cnem. 3, 833 (1323)

“r - n r x " Q . .-. ,-.r c .-, ,- - -r 4. ~ . -
cones, L. V. —na ytront, H. n., Curue.ie iLSthUthL

 

- N -. — 1/ ...
muller, L., Ann. Fggs, 12, 7., (13¢ )

 

Gnosh and Bisvas, Zeit. fur Elekrochemie u. angst;
LIJEVS. CPI-let“. 30, 97 (132“)

. . , _ .. // a.

ur1;nt5 Jr. Cnem. Soc. (London) 139, 009 (1%)

Ealy and Collie, Jr. Chem. SOC. (London) 67. 1332

(1905

 

 

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The absorption spectra of
sodium m-benzenedisulfonate
in nickel sulfate solutions.