NASA-CR-193481

""

DETERMINATION IN TRIGLYCINE GRANT NO.

OF TRACE SULFATE NAG08-204

ELEMENTS SOLUTIONS

r /

_ J

TECHNICAL

FINAL

REPORT

SUBMITTED

TO

NATIONAL MARSHALL

AERONAUTICS AND SPACE SPACE FLIGHT CENTER,

ADMINISTRATION ALABAMA 35762

SUBMITTED

BY

SHAWKY July

H. TADROS 31, 1993

Shawky Project

H. Tadros, Manager

Ph.D. VP,Reseach and Development

N94-I3048 (NASA-CR-193481) TRACE ELEMENTS IN SULFATE SOLUTIONS Report (Alabama A DETERMINATION TRIGLYCINE Final Technical & M Univ.) OF

Uncl 14 p

as

G3/25

0177366

DETERMINATION IN TRIGLYCINE GRANT NO.

OF

TRACE

ELEMENTS SOLUTIONS

SULFATE NAG08-204

TECHNICAL

FINAL

REPORT

SUBMITTED

TO

NATIONAL MARSHALL

AERONAUTICS AND SPACE SPACE FLIGHT CENTER,

ADMINISTRATION ALABAMA 35762

SUBMITTED

BY

SHAWKY H. July 31,

TADROS 1993

Shawky Project

H. Tadros, Manager

Ph.D.

Jeanette VP,Reseach

Jones,Ph.D. and Development

CONTENTS

Acknowledgement

Abstract

Objectives

Introduction

Research

Plan 4

Periodical first group

measurements

of the elements in the

Periodic

measurements

of the elements in the

second group

Elements

behaviour

in a mixture

Electrochemical

series

Extension

of

the project I0

References

,}

oo

Acknowledgement

Appreciation monitor guidance to for My Dr. his student at

is

extended

to

Dr.

Donald

Frazier, for thank

the his also

technical invaluable is extented

NASA-MSFC, running A. Evans,

Huntsville, the project.

Alabama, Our at his the

during Richard helpful

f

Chairman and also

Chemistry

Department,

suggestion Hanley

fruitful as a

discussion. dependable

Sean

served

competant,

assistant.

ABSTRACT Ten elements first group were divided iron, into nickel, 2 groups. The elements manganese, included in the copper,

included

Chromium,

and gold,. cobalt, Five triglycine 1-naphthyl 1-naphthyl the filtrates

The elements lead,

in the second group

zinc,

Cadmium, and gold. in each group was spiked Glycine in a I%

ppm of each element sulfate isocyanate isocyanate

(TGS)solution. in ether glycine

was removed with derivative and

medium.The glycine

was removed by filtration, for the different elements. by using the

were analyzed of these elements Absorption

Analysis Pekin-Elmer The result

was performed

5100

Atomic

Spectrophotometer. was the observation of chromium of glycine. the concentration These of that there which

of these in the

experiments concentration

was a decrease was interpreted by the derivative

and gold,

to be due to the chelation 1-naphthyl is isocyanate

these

elements

Further other

research

needed to determine sulfate

elements will

in triglycine include lithium, barium,

(TGS) solutions.

elements calcium,

sodium, rubidium, aluminum, and silicon. in

magnesium,

strontium,

These are the acid

most likely

elements

to be found

the sulfuric

used in manufacturing we will formula extend of

the TGS crystal. our research colored to investigate chelated the

Moreover, structural which

the violet

compounds,

had been formed by interaction isocyanate chromium. 1 glycine with

of the derivative the different elements,

1-naphthyl

such as gold,

Title: Determination Objectives: I. To spike a triglycine the elements sulfate Fe, Ni, (TGS) solution Cr, with 5 ppm of Trace Elements in Triglycine sulfate solutions.

of each of
Cd, 2. To and remove Au.

Mn, Cu, Zn, Co, Pb,

glycine the the

from above

the

TGS

solution, in can the be

followed filtrate. chelated by

by

determining 3. To recognize

elements that

elements

the

derivative

1-naphthyl

isocyanate

glycine.

Introduction: Triglycine has received of sulfate (TGS) is an infrared as a A in detector good space the material candidate lab 3 that for experiment

considerable microgravity the growth crystal of

attention crystal a TGS

studies performed System TGS

growth. crystal The trace of

fluid

experiment on the impurities in others and the

(FES) consistently TGS the

growth

cell. that

extensive metals initial the the result TGS the lined of and

background contaminate component of metals

indicates solution impurities acid of used

saturated Some the are FES A of

regardless are to probably synthesize

sulfuric as a result

crystal; solution with gold

interaction which ongoing quality is

between usually definition control, of

chamber vital part

itself, of the

foil.

crystal

growth optimization analyses in

dynamics, depends TGS

solution largely o%

hardware metals

the

accuracy

trace

solutions.

Research Two of Au. Pb, Five groups iron, The

plan: of Fe, second metals nickel, group Cd, each sulfate polyethylene solution in I the it first and were Ni, studied. chromium, of Au. of each group The flask like of before each group in was spiked was up in a I% in the a mark. The Cr, zinc, first copper, Zn, group Cu, composed and Co, gold, lead,

composed gold,

cobalt,

cadmium, ppm of

element (TGS)

triglycine 100-ml A The control TGS

solution.

mixture and filled but was

put to

volumetric was made

without removed

TGS. by

bottle

reacting

with

1-naphthyl

isocyanate

ether 0
fi

medium.

/_-N:C:O

H2N-CH2COOH

_'_/'_'HN-C-HN-CH2COOH

l-naphthy]

isocyanate

+ glycine

l-naphthyl

isocyanate

glycine

The

derivative

1-naphthy1 and

isocyanate the filtrate

glycine was

was

removed for the

by

gravity

filtration,

analyzed

corresponding The The flame 1 and elements 5100 mode, 2.

elements. of the control atomic for analysis solution absorption purpose. The were also determined.

Perkin-Elmer was used

spectrophotometer. results are shown in tables

Table

I : Periodical measurements of the elemen_ in the first group in ppmunit.

at once wee_
on

Element
CH

two. week

three week

four week

I14 week_F24week s

W/out TGS with TGS

5.0

5.1

5.0

5.1

Cr

w/out TGS with TGS

3.1

3.1

3.0

3.0

Ni

w/out
TGS with TGS 5

3.1

5.1

5.1

Mn

w/out
TGS with TGS

5.0

5.1

5.1

5.1

Au

w/out
TGS with TGS 5 .1

3.1

3.1

.1

.I

.1

.I

.I

Fe

w/out
TGS with TGS

5.1

5.1

5.0

5.1

Table

2:

periodical measurements of the second group in

of the ppm unit.

elements

Element

at once

on wee_

two, week

three week

_een w_ r

24 week week

W/out TGS

5
with TGS

5.1

Cd w/out
TGS

5 5 5.1

with TGS

Pb w/out
TGS

5 5 5.0

with TGS

Zn w/out TGS with TGS

5
5 5 5 5

5.1

Au

w/out
TGS with TGS

Elements

Behaviour

in

Mixture:

Chromium a strong

atom, reducing in

Cr,

in agent

the

electrochemical (Table 3). be Therefore, to E 1)of atomic the

series the the =

is

considered

chemical hand (I) Chromium spectrothe derivative side:

equillibrium

eq.

(I) 4---3 ppm

will _Cr3++ 3+ Cr

shifted 3e-

right

Cr As a result, could AAS. only be

-0.744 spiked

(Tabl_ by 2 the

solution photometer, 1-naphthyl On the

detected The rest

absorption by I)

ppm

were (I-NICG)

chelated (Table 3) It is is

isocyanate other i e hand electron agent. to the gold

glycine
3+

ion seeking

Au

(Table species.

considered considered

a a in

Lewis strong eq.(2)

acid" oxidizing is

Therefore, left hand Au

the side: 3+ +

chemical

equillibrium

shifted

Au<------_ As a result, be a small by I-NICG had been

3e.I ppm 4.9 A

E Au3+of ppm were of Ist

+1.498 the spiked

(2) gold by

proportion, AAS. The rest I).

could the to The

detected

chelated Au week

derivative Zero value

(Table noticed of the

decrease the

concentrtion (Table with gold in 2). or i.

after chelated the to

structural can be

formula

compounds

chromium X-ray formula.

represented can be

by used

formula confirm

indicated this

figure

spectroscopy

structural

._-IR

.M, Oo

Proposed

Formula

for the chelated compounds

R = NH-CO-NH-CH2-COOH M = Cr, Au (Figure I)

Table 3 Electrochemical Se ries2

Red. _ Ox. Li + K+ Ca2+ Na+ Mg2 + Be 2+ AI_" .Mn2+ Zn 2+ Cr 3. Ga 3. Fe2 + Cd 2+ Co 2+ Ni 2+ Sn =+ pb 2+ 2D + 2H+ Cu 2* Ag + Hg 2+ Pd 2+ pt 2+ Au 3. + 0
_0

F-Z ,,i e_O

(.0 Z

Li _ K _ Ca _ Na _ Mg _ Be = AI _ Mn _ ZnCam) _ Cr = Ga _ Fe _: Cd _z Co ,z Ni = Sn (weiID = Pb = D2 H2 = = = = = _z = =

+ O + O + 2 G + O + 20 + 20 + 30 + 20 +2o + 30 + 30 + 2O + 2 0 + 20 + 20 + 2O + 2 O + 2 O + 2 O + + + + + + 2 O O 20 20 20 30

_ 3.04561 -- 2.925 -- 2.866 -- 2.714 -- 2.363 -- 1.847 -- 1.662 -- 1.180 -- 0.7627 -- 0.744 --0.529 -- 0.4002 --0.4029 -- 0.277 -- 0.250 --0.136 -- 0.126 -- 0.0034 0.0000 + + + + ~+ + 0.337 0.7991 0.854 0.987 1.2 1.498

u,1 t-z uJ

m z

r,4

t,--4

W e_

Cu Ag Hg Pd Pt Au

x 0

Extension Further other elements calcium, These acid are used

to

the

Project: is needed to determine (TGS) the concentration These

research in

elements will

triglycine lithium, barium, likely

sulfate sodium, aluminum; elements the TGS to

solutions.

include

rubidium, and be $ilic0n. found in

magnesium,

strontium, the in we most

the

sulfuric

manufacturing will extend of the by

crystal. to investigate chelated the the compounds,

Moreover, structural which had

our

research colored

formula been formed

violet interaction with

of the

derivative elements,

1-naphthyl such as

isocyanate gold, chromium.

glycine

different

References

I.

Mitchell, Ed.

c.

A. s F.

"Commercial son and and Wiberg, de Co.,

Organic Inc. E.

Analysis." Phyladelphia, der

Vol.

VIII p.

5th 234

Balckiston A. 80-90

1930, Anorganischen York,

2.

Holleman, Chemie." p. 202

"Lerhbuch Berlin,

Auflage,

Gryter:

New

1976,

i0