I
nte
rna
t
io
na
l J
o
urna
l o
f
Adv
a
nces in Applie
d Science
s
(
I
J
AAS)
Vo
l.
1
3
,
No
.
4
,
Dec
em
b
er
2
0
2
4
,
p
p
.
9
8
5
~
9
90
I
SS
N:
2252
-
8
8
1
4
,
DOI
:
1
0
.
1
1
5
9
1
/ijaas
.
v
1
3
.
i
4
.
pp
985
-
9
90
985
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:
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p
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ts.
Ho
m
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n
e
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ty
re
su
lt
s
p
ro
v
e
d
t
h
a
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th
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m
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c
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p
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with
th
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m
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h
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f
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m
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teria
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s
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with
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a
l
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s
will
su
p
p
o
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g
u
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b
o
d
ies
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e
n
v
iro
n
m
e
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tal
p
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tec
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a
g
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n
c
ie
s,
a
n
d
tes
ti
n
g
lab
o
ra
to
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h
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ir
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in
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g
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latio
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K
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w
o
r
d
s
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B
T
E
X
C
er
tifie
d
r
ef
er
en
ce
m
ate
r
ial
C
h
lo
r
o
b
en
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n
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Ma
s
s
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alan
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ap
p
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Valu
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ass
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n
m
en
t
T
h
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s
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c
c
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u
n
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e
CC B
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SA
li
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se
.
C
o
r
r
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s
p
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A
uth
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r
:
I
b
r
ah
im
F.
T
a
h
o
u
n
Or
g
an
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An
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L
ab
o
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ato
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C
h
em
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Me
tr
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lo
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Div
is
io
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Natio
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I
n
s
titu
te
o
f
Stan
d
a
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s
Mo
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am
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An
war
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l Sad
at
St.
(
T
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,
E
l H
ar
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Giza
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E
g
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p
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ail: T
ah
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c
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b
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im
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T
ah
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n
is
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s
ci.
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1.
I
NT
RO
D
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I
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N
Me
asu
r
em
en
t
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esu
lts
ar
e
u
s
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tr
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b
y
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g
u
lato
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o
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s
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h
u
s
,
th
e
n
ee
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f
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r
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iab
le
an
d
ac
cu
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ate
m
ea
s
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r
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ts
o
f
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o
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lled
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s
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b
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ce
s
h
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d
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ly
.
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en
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d
its
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g
b
en
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to
lu
en
e
,
eth
y
lb
en
ze
n
e,
an
d
x
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len
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(
B
T
E
X
)
an
d
ch
lo
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b
e
n
ze
n
es
ar
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am
o
n
g
th
e
m
o
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t
co
m
m
o
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ly
wo
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ld
wid
e
r
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u
lated
p
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ll
u
tan
ts
.
T
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co
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p
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d
s
ar
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tili
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lv
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r
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m
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t
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s
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d
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e
n
t,
r
esin
,
an
d
p
esti
cid
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[
1
]
,
[
2
]
.
T
h
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lar
g
e
u
s
e
o
f
t
h
ese
s
u
b
s
tan
ce
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th
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waste
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in
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n
ex
p
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s
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[
3
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,
[
4
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.
H
u
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x
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to
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ca
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ca
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s
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lo
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d
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s
,
ca
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r
,
a
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d
h
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to
th
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k
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y
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ea
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t,
liv
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r
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s
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y
s
tem
,
am
o
n
g
o
th
er
s
id
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ef
f
ec
ts
[
5
]
,
[
6
]
.
T
h
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ef
o
r
e,
th
e
ef
f
ec
tiv
e
m
o
n
it
o
r
in
g
o
f
B
T
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X
an
d
c
h
lo
r
o
b
en
ze
n
es
in
e
n
v
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o
n
m
en
tal
s
y
s
tem
s
is
a
s
s
u
m
ed
to
b
e
o
f
p
r
im
e
im
p
o
r
tan
ce
in
co
n
t
r
o
llin
g
th
e
a
d
v
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s
e
ef
f
ec
ts
o
f
t
h
ese
p
o
llu
tan
ts
o
n
h
u
m
an
a
n
d
an
im
al
h
ea
lth
.
B
u
t
th
er
e
ar
e
m
an
y
ch
allen
g
es
af
f
ec
tin
g
th
e
ac
cu
r
ac
y
an
d
p
r
ec
i
s
io
n
o
f
B
T
E
X
an
d
ch
lo
r
o
b
e
n
ze
n
es
m
ea
s
u
r
em
en
t
r
esu
lts
in
clu
d
in
g
th
eir
l
o
w
co
n
ce
n
tr
atio
n
in
th
e
en
v
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o
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m
e
n
tal
s
am
p
les
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av
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o
f
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Evaluation Warning : The document was created with Spire.PDF for Python.
I
SS
N
:
2252
-
8
8
1
4
I
n
t J Ad
v
Ap
p
l Sci
,
Vo
l.
1
3
,
No
.
4
,
Dec
em
b
er
2
0
2
4
:
985
-
9
90
986
r
ef
er
en
ce
m
ater
ials
(
C
R
Ms)
n
ee
d
e
d
f
o
r
ca
lib
r
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d
p
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f
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an
c
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ch
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k
o
f
m
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r
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m
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ts
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v
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eth
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s
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ter
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d
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ter
lab
o
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ato
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co
m
p
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r
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s
[
7
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–
[
1
2
]
.
C
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tifie
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m
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lu
d
in
g
wate
r
co
n
ten
t
as
well
as
o
r
g
an
ic
im
p
u
r
ities
[
1
3
]
–
[
1
5
]
.
T
h
e
r
ef
er
e
n
ce
m
ater
ial
was
f
o
r
m
u
lated
g
r
a
v
im
etr
ically
an
d
ce
r
tifie
d
v
al
u
es
wer
e
ca
lcu
lated
b
ased
o
n
th
e
m
ass
o
f
ea
ch
co
m
p
o
n
en
t.
Ad
d
itio
n
ally
,
v
al
u
e
ass
ig
n
m
en
t,
h
o
m
o
g
en
eity
,
an
d
s
tab
ili
ty
ev
alu
atio
n
o
f
th
e
p
r
ep
ar
ed
r
e
f
er
en
ce
m
ater
ial
wer
e
also
h
ig
h
lig
h
ted
.
2.
RE
S
E
ARCH
M
E
T
H
O
D
2
.
1
.
Rea
g
ent
a
nd
chem
ica
ls
T
h
e
s
tar
tin
g
m
ater
ials
f
o
r
th
e
C
R
M
s
wer
e
p
u
r
ch
ased
f
r
o
m
Me
r
ck
(
Ger
m
an
y
)
in
clu
d
in
g
h
ig
h
p
u
r
e
b
en
ze
n
e,
to
lu
en
e
,
c
h
lo
r
o
b
en
z
en
e,
eth
y
lb
en
ze
n
e
,
o
,
m
,
p
-
x
y
len
e,
1
,
2
-
d
ich
lo
r
o
b
e
n
ze
n
e,
1
,
3
-
d
ich
lo
r
o
b
e
n
ze
n
e
,
an
d
1
,
4
-
d
ich
lo
r
o
b
en
ze
n
e
wer
e
p
u
r
ch
ased
f
r
o
m
Me
r
c
k
(
Ge
r
m
an
y
)
.
Hig
h
-
p
er
f
o
r
m
an
ce
liq
u
id
ch
r
o
m
ato
g
r
ap
h
y
(
HPLC
)
g
r
ad
e
s
o
lv
e
n
ts
,
an
d
m
eth
an
o
l
w
er
e
p
u
r
ch
ased
f
r
o
m
Sig
m
a
-
Ald
r
ich
(
Ger
m
a
n
y
)
.
Kar
l
Fis
h
er
r
ea
g
en
ts
wer
e
p
u
r
c
h
ased
f
r
o
m
Sch
ar
la
u
(
Sp
ain
)
.
No
a
d
d
itio
n
al
p
u
r
if
icatio
n
was
r
eq
u
ir
e
d
f
o
r
o
r
g
a
n
ic
s
o
lv
en
ts
u
s
ed
in
all
p
r
o
ce
s
se
s
.
2
.
2
.
I
dentit
y
a
nd
o
rg
a
nic im
pu
rit
ies det
er
m
ina
t
io
n
Ag
ilen
t
6
8
9
0
N
g
as
ch
r
o
m
ato
g
r
ap
h
y
co
n
s
is
ts
o
f
a
f
lam
e
io
n
izatio
n
d
etec
to
r
(
FID
)
,
a
5
9
7
5
in
er
t
XL
m
ass
s
elec
tiv
e
d
etec
to
r
,
an
d
a
n
au
to
m
ated
i
n
jecto
r
(
7
6
8
3
B
)
.
T
h
e
s
u
s
p
ec
ted
o
r
g
an
ic
im
p
u
r
i
ties
wer
e
s
ep
ar
ated
u
s
in
g
a
DB
-
VR
X
co
lu
m
n
,
(
6
0
m
,
I
D
0
.
2
5
m
m
,
a
n
d
0
.
2
5
µ
m
f
ilm
t
h
ick
n
ess
)
f
r
o
m
J
&
W
Scien
tific
(
USA)
.
Heliu
m
was
u
s
ed
as
a
ca
r
r
ier
g
as
at
co
n
s
tan
t
f
lo
w
(
1
.
0
m
L
/
m
in
)
.
T
h
e
o
v
en
tem
p
er
atu
r
e
was
p
r
o
g
r
am
m
e
d
as
f
o
llo
ws:
5
0
℃
f
o
r
5
m
in
in
cr
ea
s
ed
b
y
5
℃/m
in
to
2
4
0
℃
with
a
fin
al
h
o
ld
f
o
r
5
m
in
.
T
h
e
in
jecto
r
,
FID
d
etec
to
r
,
a
n
d
m
ass
s
p
ec
tr
o
m
e
ter
(
MS
)
i
n
ter
f
ac
e
te
m
p
er
atu
r
es
wer
e
h
eld
co
n
s
tan
t
at
2
5
0
,
3
0
0
,
a
n
d
2
9
0
℃,
r
esp
ec
tiv
ely
.
T
h
e
m
ass
s
p
ec
tr
o
m
eter
was
u
s
ed
at
d
ef
au
lt
o
p
er
atin
g
co
n
d
itio
n
s
f
o
r
th
e
io
n
s
o
u
r
ce
,
q
u
ad
r
u
p
le.
T
h
r
ee
s
am
p
les
f
r
o
m
ea
c
h
m
a
ter
ial
wer
e
in
jecte
d
d
ir
ec
t
ly
in
to
g
as
c
h
r
o
m
ato
g
r
ap
h
y
(
GC
)
-
MS
w
ith
o
u
t
a
n
y
f
u
r
th
er
tr
ea
tm
e
n
ts
.
Ag
ilen
t
C
h
em
s
tatio
n
s
o
f
twar
e
was
u
s
ed
f
o
r
p
r
o
ce
s
s
in
g
an
d
an
aly
s
is
o
f
ch
r
o
m
at
o
g
r
a
p
h
ic
d
ata
.
2
.
3
.
Wa
t
er
co
nte
nt
det
er
m
ina
t
io
n
T
h
e
wate
r
co
n
ten
t
o
f
ea
ch
s
tar
tin
g
m
ater
ial
was
d
eter
m
in
ed
u
s
in
g
a
Me
tr
o
h
m
8
5
2
T
itra
n
d
o
co
u
lo
m
etr
ic
KF
s
y
s
tem
;
th
e
s
am
p
les
wer
e
t
r
an
s
f
er
r
e
d
t
o
a
titra
tio
n
ce
ll
f
o
r
m
ea
s
u
r
em
en
t
with
o
u
t
an
y
ad
d
itio
n
al
p
r
ep
a
r
atio
n
s
.
Fiv
e
s
am
p
les
f
r
o
m
ea
ch
m
ater
ial
wer
e
an
aly
z
ed
an
d
th
e
m
ea
n
v
a
lu
e
was
u
s
ed
as
an
in
d
icato
r
o
f
wate
r
co
n
te
n
t.
2
.
4
.
B
lend
ing
a
nd
prepa
ra
t
io
n o
f
m
a
t
er
i
a
l
T
h
e
to
tal
am
o
u
n
t
o
f
all
s
u
b
s
ta
n
ce
s
in
a
s
am
p
le
is
eq
u
al
t
o
th
e
m
ass
f
r
ac
tio
n
o
f
th
e
tar
g
et
c
o
m
p
o
n
en
t
p
lu
s
th
e
m
ass
f
r
ac
tio
n
s
o
f
all
i
m
p
u
r
ities
.
Hen
ce
,
th
e
s
u
m
o
f
t
h
e
m
ea
s
u
r
e
d
m
ass
f
r
ac
tio
n
s
o
f
wate
r
an
d
o
r
g
a
n
ic
im
p
u
r
ities
is
u
s
ed
to
esti
m
ate
t
h
e
p
u
r
ity
o
f
th
e
c
o
m
p
o
u
n
d
s
b
y
s
u
b
tr
ac
tin
g
it
f
r
o
m
1
0
0
%.
T
h
e
co
r
r
ec
ted
weig
h
t
o
f
ea
ch
co
m
p
o
u
n
d
was c
alcu
lated
an
d
th
e
m
ix
t
u
r
e
f
o
r
ea
ch
o
f
th
e
ten
co
m
p
o
u
n
d
s
w
as
fill
e
d
g
r
av
im
etr
ically
in
th
e
o
r
d
er
o
f
d
ec
r
ea
s
in
g
d
en
s
ity
as
f
o
llo
w
s
:
eth
y
lb
e
n
ze
n
e,
1
,
2
-
d
ich
lo
r
o
b
en
ze
n
e,
1
,
3
-
d
ic
h
lo
r
o
b
e
n
ze
n
e,
1
,
4
-
d
ich
lo
r
o
b
en
ze
n
e,
c
h
lo
r
o
b
en
ze
n
e
,
b
en
ze
n
e
,
to
lu
en
e,
o
,
m
,
an
d
p
-
x
y
le
n
e.
T
h
e
m
ix
t
u
r
e
was h
o
m
o
g
e
n
i
z
ed
f
o
r
6
h
b
ef
o
r
e
b
o
ttli
n
g
in
t
h
e
f
in
al
f
o
r
m
.
T
h
e
m
ate
r
ial
was
p
ac
k
ed
in
2
m
L
b
r
o
wn
g
lass
am
p
o
u
les
u
n
d
er
p
r
ec
is
ely
r
eg
u
lated
co
n
d
itio
n
s
to
av
o
id
an
y
lo
s
s
o
f
m
ater
ial
d
u
e
to
th
e
v
o
latilit
y
o
f
th
e
s
o
lu
tio
n
.
T
h
e
p
r
ep
ar
e
d
b
atc
h
co
n
s
is
ted
o
f
ap
p
r
o
x
im
ately
1
0
0
am
p
o
u
les,
wh
ich
wer
e
g
r
o
u
p
ed
i
n
to
ten
g
r
o
u
p
s
an
d
ass
ig
n
ed
u
n
iq
u
e
co
d
e
s
b
ased
o
n
t
h
e
o
r
d
er
o
f
f
illi
n
g
.
E
ac
h
g
r
o
u
p
co
n
tain
e
d
ten
am
p
o
u
les.
All
am
p
u
les
wer
e
s
to
r
ed
at
a
c
o
n
tr
o
lled
tem
p
er
atu
r
e
o
f
ab
o
u
t 4
°C
f
o
r
f
u
r
th
er
s
tu
d
ies.
2
.
5
.
H
o
m
o
g
eneit
y
t
esting
I
n
o
r
d
er
t
o
d
eter
m
in
e
th
e
h
eter
o
g
en
eity
o
f
t
h
e
p
r
ep
ar
ed
r
ef
er
en
ce
m
ater
ial,
th
e
h
o
m
o
g
en
eit
y
ex
p
er
im
en
t
was
d
esig
n
ed
i
n
c
o
m
p
lian
ce
with
I
SO
3
3
4
0
5
:2
0
2
4
.
T
h
is
s
tan
d
ar
d
r
ec
o
m
m
e
n
d
s
s
elec
tin
g
ten
u
n
its
f
o
r
ev
al
u
atin
g
b
o
th
with
in
a
n
d
b
etwe
en
am
p
u
les
h
o
m
o
g
e
n
eity
o
f
s
m
all
b
atc
h
es.
T
h
u
s
,
1
0
am
p
u
les
wer
e
s
elec
ted
in
a
r
an
d
o
m
o
r
d
er
tak
in
g
in
to
ac
co
u
n
t
th
e
f
illi
n
g
s
eq
u
en
ce
in
clu
d
in
g
th
e
f
ir
s
t
an
d
last
f
illed
am
p
o
u
le,
s
elec
ted
am
p
u
les
wer
e
d
iv
id
e
d
in
to
th
r
ee
s
u
b
-
s
am
p
les
an
d
th
en
an
aly
z
e
d
b
y
g
as
ch
r
o
m
at
o
g
r
ap
h
th
r
ee
tim
es
Evaluation Warning : The document was created with Spire.PDF for Python.
I
n
t J Ad
v
Ap
p
l Sci
I
SS
N:
2252
-
8
8
1
4
Dev
elo
p
men
t o
f a
p
r
ima
r
y
r
ef
eren
ce
ma
teri
a
l fo
r
th
e
a
n
a
lys
is
o
f B
TEX
…
(
I
b
r
a
h
im
F
.
Ta
h
o
u
n
)
987
with
th
e
s
am
e
co
n
d
itio
n
s
.
Sa
m
p
les
wer
e
r
an
d
o
m
ly
test
ed
to
ev
alu
ate
th
e
ef
f
ec
t
o
f
t
h
e
f
illi
n
g
o
r
d
e
r
o
f
t
h
e
am
p
u
les.
An
aly
s
is
o
f
v
a
r
ian
c
e
(
ANOVA
)
was
u
s
ed
to
e
v
al
u
ate
th
e
d
ata
i
n
o
r
d
er
to
esti
m
ate
th
e
u
n
ce
r
tain
t
y
r
esu
ltin
g
f
r
o
m
th
e
h
eter
o
g
en
ei
ty
ef
f
ec
t a
n
d
ass
ess
s
am
p
le
h
o
m
o
g
en
eity
.
2
.
6
.
Sta
bil
it
y
t
esting
T
h
e
r
esu
ltin
g
m
ix
tu
r
e
was
s
u
b
jecte
d
to
is
o
ch
r
o
n
o
u
s
s
tab
ilit
y
s
tu
d
ies
in
o
r
d
er
to
ass
ess
th
e
m
ater
ials
'
s
tab
ilit
y
d
u
r
in
g
tr
a
n
s
p
o
r
tatio
n
an
d
s
to
r
ag
e.
A
s
tr
atif
ied
r
a
n
d
o
m
s
am
p
lin
g
ap
p
r
o
ac
h
wa
s
ap
p
lied
to
s
elec
t
s
ev
en
teen
am
p
u
les
f
r
o
m
th
e
p
r
ep
ar
e
d
p
atch
,
th
e
am
p
u
les
wer
e
d
iv
id
ed
in
to
eig
h
t
g
r
o
u
p
s
.
T
wo
g
r
o
u
p
s
wer
e
k
ep
t
at
4
an
d
4
0
°C
,
wh
ile
o
n
e
am
p
u
le
was
k
e
p
t
at
th
e
r
ef
er
e
n
ce
tem
p
er
atu
r
e
o
f
-
2
0
°C
.
On
e
am
p
o
u
le
in
ea
c
h
g
r
o
u
p
was
r
el
o
ca
ted
to
th
e
r
ef
er
en
ce
tem
p
er
atu
r
e
at
th
e
two
-
s
to
r
ag
e
tem
p
er
atu
r
e
af
ter
3
,
6
,
9
,
an
d
1
2
m
o
n
th
s
f
o
r
th
e
lo
n
g
-
ter
m
s
tab
ilit
y
s
t
u
d
y
.
Six
s
am
p
les
wer
e
s
to
r
e
d
at
4
0
℃
f
o
r
th
e
s
h
o
r
t
-
t
er
m
s
tab
ilit
y
s
tu
d
y
,
th
e
am
p
o
u
les
wer
e
tr
an
s
f
er
r
ed
t
o
r
ef
er
e
n
ce
tem
p
er
atu
r
e
af
ter
1
,
2
,
3
,
4
,
5
,
a
n
d
6
wee
k
s
.
T
h
e
am
p
u
les
u
s
ed
to
e
s
tim
ate
th
e
in
itial
v
alu
e
f
o
r
t
=
0
wer
e
in
itially
k
e
p
t
at
t
h
e
r
e
f
er
en
ce
tem
p
er
atu
r
e
(
-
2
0
℃)
.
Af
ter
th
e
s
tu
d
y
wa
s
co
m
p
leted
,
al
l
am
p
u
les
wer
e
test
ed
u
n
d
er
r
ep
ea
ta
b
ilit
y
co
n
d
itio
n
s
in
o
n
e
b
atch
.
T
h
e
d
at
a
wer
e
s
tatis
tically
an
aly
z
ed
to
esti
m
ate
s
h
elf
life
an
d
u
n
ce
r
tain
ty
d
u
e
to
th
e
in
s
tab
ilit
y
o
f
m
ater
ials
.
3.
RE
SU
L
T
S AN
D
D
I
SCU
SS
I
O
N
3
.
1
.
Cha
ra
ct
er
iza
t
io
n o
f
m
a
t
er
ia
l
s
T
h
e
id
en
tity
an
d
p
u
r
ity
o
f
th
e
s
tar
tin
g
m
ater
ials
wer
e
co
n
f
ir
m
e
d
b
y
th
eir
m
ass
an
d
ar
ea
n
o
r
m
aliza
tio
n
m
eth
o
d
s
u
s
in
g
GC
-
MS
an
d
GC
-
FID
,
r
e
s
p
ec
tiv
ely
.
T
h
e
ch
r
o
m
ato
g
r
a
p
h
ic
s
ep
ar
atio
n
o
f
s
u
s
p
ec
ted
o
r
g
an
ic
im
p
u
r
ities
was
ac
h
iev
ed
with
a
n
o
n
p
o
lar
DB
-
VR
X
co
lu
m
n
.
T
h
e
p
ea
k
s
o
f
tar
g
e
t
co
m
p
o
u
n
d
s
wer
e
well
r
eso
lv
e
d
with
o
u
t
in
ter
f
e
r
en
ce
s
b
y
im
p
u
r
ities
with
b
aselin
e
r
eso
lu
ti
o
n
h
ig
h
er
th
a
n
1
.
5
ex
ce
p
t
f
o
r
m
an
d
p
-
x
y
len
es.
T
h
e
q
u
a
n
tific
atio
n
o
f
d
etec
ted
o
r
g
an
ic
im
p
u
r
ities
was
esti
m
ated
b
ased
o
n
a
n
ap
p
r
o
p
r
iate
ap
p
r
o
x
im
atio
n
o
f
th
eir
p
ea
k
ar
ea
s
th
e
to
tal
c
h
r
o
m
ato
g
r
am
p
ea
k
s
a
r
ea
s
.
T
h
e
p
u
r
ities
o
f
b
en
ze
n
e,
to
lu
en
e,
ch
lo
r
o
b
en
z
e
n
e,
eth
y
lb
en
ze
n
e,
o
-
x
y
len
e,
1
,
2
-
d
i
ch
lo
r
o
b
e
n
ze
n
e,
1
,
3
-
d
ic
h
lo
r
o
b
en
ze
n
e
,
an
d
1
,
4
-
d
ich
lo
r
o
b
en
ze
n
e,
m
,
an
d
p
-
x
y
len
e
u
s
ed
f
o
r
t
h
e
p
r
ep
ar
atio
n
o
f
r
e
f
er
en
ce
m
ater
i
al
wer
e
b
ased
o
n
c
h
r
o
m
ato
g
r
ap
h
ic
p
u
r
ities
in
c
o
m
b
in
atio
n
with
wate
r
co
n
te
n
t
b
y
co
u
lo
m
etr
ic
Kar
l
Fis
ch
er
titra
tio
n
m
eth
o
d
.
T
h
e
weig
h
t
o
f
ea
ch
c
o
m
p
o
u
n
d
was
ca
lcu
lated
an
d
th
e
m
ix
tu
r
e
f
o
r
ea
ch
o
f
th
e
te
n
co
m
p
o
u
n
d
s
was
fill
ed
g
r
av
im
etr
ically
in
th
e
o
r
d
er
o
f
d
ec
r
ea
s
in
g
d
e
n
s
ity
to
av
o
id
lo
s
s
o
f
a
n
aly
tes
b
y
ev
ap
o
r
atio
n
.
T
h
e
g
r
av
im
etr
ically
p
r
e
p
ar
ed
co
n
ce
n
tr
atio
n
s
o
f
b
en
ze
n
e,
to
lu
e
n
e,
ch
lo
r
o
b
en
ze
n
e
,
eth
y
lb
en
z
en
e,
o
-
x
y
len
e,
1
,
2
-
d
ich
lo
r
o
b
en
ze
n
e,
1
,
3
-
d
ic
h
lo
r
o
b
en
ze
n
e
,
an
d
1
,
4
-
d
ic
h
lo
r
o
b
en
ze
n
e
wer
e
co
n
f
i
r
m
ed
b
y
GC
-
MS
as
illu
s
tr
ated
in
Fig
u
r
e
1
,
wh
er
ea
s
t
h
e
co
n
ce
n
tr
atio
n
o
f
m
an
d
p
-
x
y
le
n
e
was
n
o
t
co
n
f
ir
m
ed
d
u
e
to
d
i
f
f
icu
lties
in
ch
r
o
m
ato
g
r
ap
h
ic
s
ep
ar
atio
n
a
n
d
p
r
esen
te
d
as a
r
ef
er
e
n
ce
v
a
lu
e.
Fig
u
r
e
1
.
Gas c
h
r
o
m
ato
g
r
ap
h
i
c
ch
r
o
m
ato
g
r
am
o
f
B
T
E
X
an
d
c
h
lo
r
o
b
en
ze
n
es b
y
DB
-
VR
X
co
lu
m
n
a
n
d
m
ass
s
elec
tiv
e
d
etec
tio
n
Evaluation Warning : The document was created with Spire.PDF for Python.
I
SS
N
:
2252
-
8
8
1
4
I
n
t J Ad
v
Ap
p
l Sci
,
Vo
l.
1
3
,
No
.
4
,
Dec
em
b
er
2
0
2
4
:
985
-
9
90
988
3
.
2
.
Det
er
m
ina
t
io
n o
f
w
a
t
er
co
nt
ent
Usi
n
g
a
co
u
lo
m
etr
ic
Kar
l
Fis
ch
er
titra
to
r
with
a
d
ia
p
h
r
a
g
m
e
d
ce
ll
g
en
er
ato
r
an
d
1
0
µA
p
o
lar
izatio
n
cu
r
r
en
t,
th
e
wate
r
co
n
ten
t
o
f
t
h
e
r
aw
m
ater
ials
was m
ea
s
u
r
ed
.
T
h
e
en
d
p
o
i
n
t w
as a
u
to
m
atica
lly
d
etec
ted
at
lo
w
s
to
p
d
r
if
t
(
1
0
µg
/m
i
n
)
f
o
r
ac
cu
r
ate
d
eter
m
in
atio
n
o
f
wate
r
m
ass
f
r
ac
tio
n
.
On
e
g
r
am
of
ea
ch
m
ater
ial
was
p
r
ec
is
ely
weig
h
ed
an
d
ad
d
e
d
t
o
th
e
titra
tio
n
ch
am
b
er
.
E
ac
h
m
ater
ial
was
m
ea
s
u
r
ed
th
r
ee
t
im
es,
an
d
th
e
m
ea
n
v
alu
es
wer
e
ca
lcu
lated
an
d
u
s
ed
to
co
r
r
ec
t
th
e
tar
g
et
v
alu
e
o
f
ea
c
h
m
ate
r
ial.
I
n
all
m
a
ter
ial
s
,
th
e
h
ig
h
est
im
p
u
r
ity
co
n
ten
t is r
ep
r
esen
te
d
b
y
th
e
wate
r
co
n
te
n
t.
3
.
3
.
H
o
m
o
g
eneit
y
s
t
ud
y
T
en
am
p
o
u
les
wer
e
test
ed
t
o
d
eter
m
in
e
th
e
h
o
m
o
g
en
eity
o
f
th
e
p
r
e
p
ar
ed
b
atch
;
t
h
r
ee
s
u
b
s
am
p
les
f
r
o
m
ea
ch
am
p
o
u
le
wer
e
s
u
b
jecte
d
to
GC
-
FID
an
aly
s
i
s
u
n
d
er
r
ep
ea
tab
ilit
y
c
o
n
d
itio
n
s
.
Gr
u
b
b
'
s
test
was
u
s
ed
to
ex
am
in
e
th
e
h
o
m
o
g
e
n
eity
s
tu
d
y
d
ata
f
o
r
o
u
tlier
s
an
d
ANOV
A
s
tatis
tical
to
o
l
was
u
s
ed
to
ev
alu
ate
s
ig
n
if
ican
t
v
ar
iatio
n
s
i
n
b
len
d
ed
m
ass
f
r
ac
tio
n
s
.
T
h
e
ca
lc
u
lated
F
v
alu
e
was
co
m
p
ar
e
d
to
t
h
e
tab
u
lated
v
alu
e
f
o
r
ea
c
h
an
aly
t
e
at
a
c
o
n
f
id
e
n
ce
lev
el
o
f
ap
p
r
o
x
im
ately
9
5
%.
T
h
e
P
-
v
alu
e
was
d
ee
m
e
d
to
b
e
s
tatis
tically
s
ig
n
ifican
t
wh
en
P
-
v
alu
e
<0
.
0
5
[
1
6
]
–
[
1
8
]
.
B
ased
o
n
th
e
P
-
va
lu
e
an
d
F
test
,
n
o
s
tatis
tically
s
ig
n
if
ican
t
v
ar
iab
ilit
y
was
d
etec
ted
b
etwe
en
th
e
am
p
u
les,
as
in
d
icate
d
b
y
th
e
r
esu
lts
o
f
th
e
h
o
m
o
g
e
n
eity
test
s
h
o
wn
in
T
ab
le
1
.
Fo
r
all
an
al
y
tes,
th
e
F
-
d
is
tr
ib
u
tio
n
is
s
m
aller
th
an
t
h
e
F
-
c
r
itical
v
alu
e
an
d
th
e
P
-
v
alu
e
is
g
r
ea
ter
t
h
an
0
.
0
5
.
T
h
e
v
alu
e
o
f
u
n
ce
r
tai
n
ty
r
esu
ltin
g
f
r
o
m
m
ater
ial
h
et
er
o
g
en
eity
(
u
bb
)
f
o
r
ea
ch
an
a
ly
te
was
m
ea
s
u
r
ed
u
s
in
g
th
e
m
ea
n
s
q
u
ar
es
MS
between
a
nd
MS
within
f
r
o
m
AN
OVA
tab
les.
T
h
e
u
n
ce
r
tain
t
y
d
u
e
to
m
ater
ials
h
eter
o
g
en
eity
was
co
m
b
in
e
d
with
u
n
ce
r
tain
ties
f
r
o
m
s
tab
ilit
y
an
d
ch
ar
ac
ter
izatio
n
to
esti
m
ate
ex
p
an
d
ed
u
n
ce
r
tain
ty
ass
o
c
iated
with
e
ac
h
ce
r
tifie
d
v
alu
e
[
1
6
]
–
[
1
8
]
.
A
r
em
a
r
k
ab
le
d
eg
r
ee
o
f
c
o
n
co
r
d
an
ce
am
o
n
g
th
e
p
r
ep
ar
e
d
am
p
u
les
was
d
em
o
n
s
tr
ated
b
y
th
e
s
m
all
v
al
u
es
o
f
u
n
ce
r
tain
ty
d
u
e
t
o
m
ater
ials
h
eter
o
g
en
eity
(
u
bb
)
.
T
h
e
b
atch
th
at
was
b
ein
g
ce
r
t
if
ied
was
d
ee
m
ed
s
u
f
f
icien
tly
h
o
m
o
g
e
n
o
u
s
s
in
ce
th
er
e
was
a
g
o
o
d
ag
r
ee
m
en
t
am
o
n
g
s
t a
m
p
u
les f
o
r
all
an
al
y
tes.
T
ab
le
1
.
Su
m
m
a
r
y
o
f
h
o
m
o
g
e
n
eity
,
s
tab
ilit
y
,
ce
r
tifie
d
v
al
u
e
s
,
an
d
ex
p
a
n
d
ed
u
n
ce
r
tain
ties
o
f
B
T
E
X
an
d
ch
lo
r
o
b
e
n
ze
n
es r
ef
e
r
en
ce
m
at
er
ial
H
o
mo
g
e
n
e
i
t
y
R
e
s
u
l
t
s
S
t
a
b
i
l
i
t
y
R
e
s
u
l
t
s
C
h
a
r
a
c
t
e
r
i
z
a
t
i
o
n
R
e
s
u
l
t
s
A
n
a
l
y
t
e
MS
b
e
t
w
e
e
n
MS
w
i
t
hi
n
F
P
-
v
a
l
u
e
F
c
r
i
t
i
c
a
l
u
bb
u
st
u
ch
C
o
n
c
e
n
t
r
a
t
i
o
n
(
µ
g
/
g
)
U
e
xp
(
µ
g
/
g
)
B
e
n
z
e
n
e
1
.
5
8
E+
1
0
1
.
1
0
E+
1
0
1
.
4
3
0
.
2
4
2
.
3
9
0
.
0
0
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5
0
.
0
0
0
7
9
.
9
9
9
9
9
.
2
1
9
.
9
9
To
l
u
e
n
e
6
.
6
7
E+
1
0
5
.
2
6
E+
1
0
1
.
2
7
0
.
3
1
2
.
3
9
0
.
0
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.
0
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3
9
.
9
9
9
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6
6
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9
9
C
h
l
o
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o
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e
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1
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1
1
E+
1
0
9
.
7
3
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0
9
1
.
1
4
0
.
3
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2
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3
9
0
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0
0
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0
9
9
9
.
8
2
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Et
h
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l
b
e
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z
e
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2
.
6
0
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f
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atch
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b
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s
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t
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ter
m
s
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T
h
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m
p
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e
s
to
r
ed
at
4
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d
4
0
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f
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r
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k
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d
twelv
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m
o
n
th
s
,
r
esp
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tiv
ely
,
wh
er
ea
s
r
ef
er
en
c
e
am
p
u
les
wer
e
k
ep
t
at
r
ef
e
r
en
ce
tem
p
er
at
u
r
e
(
-
2
0
℃)
.
Af
ter
a
y
ea
r
,
all
s
am
p
les
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test
ed
s
im
u
ltan
eo
u
s
ly
in
d
u
p
licates
with
th
e
s
am
e
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n
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itio
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s
in
a
s
in
g
le
b
atch
.
T
h
is
d
esig
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e
d
u
ce
d
th
e
p
o
s
s
ib
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o
f
v
a
r
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s
in
th
e
GC
-
FID
r
e
s
p
o
n
s
e.
T
h
e
Gr
u
b
b
s
test
was
u
s
ed
at
9
5
an
d
9
9
%
co
n
f
id
en
ce
lev
els
to
s
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t
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ata
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t
tim
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an
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t
-
test
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s
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cs
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s
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eter
m
in
e
wh
eth
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e
r
eg
r
ess
io
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lin
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s
h
o
w
ed
an
y
s
ig
n
if
ican
t
tr
en
d
s
.
All
m
ater
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d
id
n
o
t
s
ig
n
if
ican
tly
d
eg
r
ad
e
at
4
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ac
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r
d
in
g
to
th
e
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b
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t
at
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s
o
m
e
m
ater
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d
id
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ican
tly
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As a
r
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lt,
th
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m
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ce
r
tific
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th
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t
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m
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ig
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t
d
eter
io
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atio
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o
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tr
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s
p
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tatio
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at
4
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d
4
0
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Alth
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u
g
h
t
h
e
m
ater
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n
b
e
tr
an
s
p
o
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ted
at
b
o
t
h
c
o
n
d
itio
n
s
,
it
was
ad
v
is
ed
to
d
is
p
atch
an
d
tr
a
n
s
p
o
r
t
m
ater
ia
l
at
≤
4
°
C
f
o
r
m
ate
r
ial
p
r
o
tect
io
n
.
T
h
e
ca
lcu
latio
n
o
f
s
h
elf
l
if
e
an
d
u
n
ce
r
t
ain
ty
r
esu
ltin
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f
r
o
m
m
ater
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in
s
tab
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was
d
o
n
e
u
s
in
g
r
eg
r
ess
io
n
r
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lts
f
r
o
m
a
lo
n
g
-
ter
m
s
tab
ilit
y
s
tu
d
y
[
1
6
]
–
[
1
9
]
.
E
s
tim
ated
u
n
ce
r
tain
t
y
w
as
in
clu
d
ed
in
t
h
e
co
m
b
in
ed
e
x
p
an
d
e
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u
n
ce
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tain
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o
f
th
e
ass
ig
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al
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e
o
f
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ac
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aly
te.
T
h
e
a
s
s
ig
n
ed
v
alu
e'
s
co
m
b
in
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n
ce
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tain
t
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clu
d
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th
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esti
m
ated
u
n
ce
r
tain
t
y
.
W
h
en
s
to
r
ed
at
≤
4
℃,
Evaluation Warning : The document was created with Spire.PDF for Python.
I
n
t J Ad
v
Ap
p
l Sci
I
SS
N:
2252
-
8
8
1
4
Dev
elo
p
men
t o
f a
p
r
ima
r
y
r
ef
eren
ce
ma
teri
a
l fo
r
th
e
a
n
a
lys
is
o
f B
TEX
…
(
I
b
r
a
h
im
F
.
Ta
h
o
u
n
)
989
th
e
p
r
e
p
ar
ed
C
R
Ms
ar
e
th
o
u
g
h
t
to
b
e
s
tab
le
f
o
r
a
p
e
r
io
d
o
f
1
2
m
o
n
th
s
.
T
o
p
r
eser
v
e
co
n
f
id
en
ce
in
th
e
ce
r
tifie
d
v
alu
es,
s
tab
ilit
y
test
in
g
will b
e
ca
r
r
ied
o
u
t th
r
o
u
g
h
o
u
t th
e
d
u
r
atio
n
th
at
th
e
m
ater
ial
is
av
ail
ab
le.
3
.
5
.
Va
lue a
s
s
ig
nm
ent
a
nd
un
ce
r
t
a
inty
o
f
re
f
er
ence
v
a
lues
T
h
e
p
u
r
ity
o
f
th
e
s
tar
tin
g
m
a
ter
ials
was
est
im
ated
b
y
em
p
lo
y
in
g
th
e
m
ass
b
alan
ce
ap
p
r
o
ac
h
.
T
h
e
m
ass
f
r
ac
tio
n
s
o
f
all
f
o
u
n
d
i
m
p
u
r
ities
wer
e
co
n
v
e
r
ted
to
p
er
ce
n
tag
e
u
n
its
(
%)
an
d
s
u
m
m
ed
in
o
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d
er
to
g
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er
ate
a
s
in
g
le
q
u
an
titativ
e
esti
m
ate
f
o
r
all
im
p
u
r
ities
[
8
]
,
[
1
3
]
,
[
2
0
]
.
T
h
e
im
p
u
r
ities
esti
m
ates
wer
e
u
s
ed
to
esti
m
ate
th
e
p
u
r
ity
o
f
th
e
s
tar
tin
g
m
ater
ials
.
T
h
e
r
ef
er
e
n
ce
m
ater
ial
was p
r
ep
ar
ed
g
r
av
im
etr
ically
an
d
ce
r
tifie
d
v
alu
es
wer
e
ca
lcu
lated
b
ase
d
o
n
th
e
c
o
r
r
ec
ted
p
u
r
ity
a
n
d
m
ass
o
f
ea
ch
c
o
m
p
o
n
en
t.
E
v
e
r
y
s
tep
in
th
e
p
r
o
d
u
ctio
n
p
r
o
ce
s
s
co
n
tr
ib
u
t
es
to
th
e
ce
r
tifie
d
v
alu
es
u
n
ce
r
tain
ty
,
wh
ic
h
h
as
an
im
p
ac
t
o
n
la
b
o
r
ato
r
y
u
n
ce
r
tain
ty
b
u
d
g
ets.
Acc
o
r
d
in
g
ly
,
th
e
u
n
ce
r
tain
ty
o
f
th
e
ce
r
tifie
d
v
alu
es
was
esti
m
ated
u
s
in
g
th
e
u
n
ce
r
tain
ty
co
m
p
o
n
en
ts
r
esu
ltin
g
f
r
o
m
th
e
ch
ar
ac
ter
izatio
n
o
f
im
p
u
r
ities
(
u
ch
)
,
s
am
p
le
in
h
o
m
o
g
e
n
eity
(
u
bb
)
,
an
d
lo
n
g
-
ter
m
in
s
tab
ilit
y
(
u
lts
)
,
in
co
m
p
lian
c
e
with
I
SO
3
3
4
0
5
:2
0
2
4
an
d
GUM
[
1
6
]
,
[
2
1
]
,
[
2
2
]
.
T
h
e
m
ea
s
u
r
em
en
t
o
f
wate
r
co
n
ten
t
(
u
w
)
an
d
o
r
g
a
n
ic
im
p
u
r
ities
(
u
oi
)
was
u
s
ed
to
d
eter
m
in
e
th
e
u
n
ce
r
tain
ty
r
esu
l
tin
g
f
r
o
m
im
p
u
r
ity
ch
ar
ac
ter
izatio
n
.
T
h
e
ex
p
a
n
d
ed
u
n
ce
r
tain
t
y
(
U
EXP
)
is
ex
p
r
ess
ed
as
two
tim
es
th
e
r
o
o
t
o
f
th
e
s
u
m
o
f
th
e
s
q
u
ar
es o
f
u
ch
,
u
bb
,
a
n
d
u
lts
at
a
co
n
f
id
en
ce
lev
el
o
f
ap
p
r
o
x
im
a
tely
9
5
%
[
1
6
]
,
[
2
3
]
–
[
2
5
]
.
4.
CO
NCLU
SI
O
N
I
n
co
m
p
lian
ce
with
I
SO
1
7
0
3
4
:2
0
1
6
an
d
I
SO
3
3
4
0
5
:2
0
2
4
s
tan
d
ar
d
s
,
a
n
ew
ce
r
tifie
d
r
ef
er
en
ce
m
ater
ial
h
as
b
ee
n
ce
r
tifie
d
f
o
r
B
T
E
X
an
d
ch
lo
r
o
b
en
ze
n
e
m
ass
f
r
ac
tio
n
s
.
E
ig
h
t
an
aly
tes
in
clu
d
in
g
b
en
ze
n
e
,
to
lu
en
e,
ch
lo
r
o
b
en
ze
n
e,
eth
y
lb
en
ze
n
e,
o
-
x
y
le
n
e,
1
,
2
-
d
i
ch
lo
r
o
b
e
n
ze
n
e,
1
,
3
-
d
ic
h
lo
r
o
b
en
ze
n
e
an
d
1
,
4
-
d
ich
lo
r
o
b
en
ze
n
e
w
as
ce
r
tifie
d
with
o
u
t
m
aj
o
r
p
r
o
b
lem
s
in
in
h
o
m
o
g
en
eity
,
s
tab
ilit
y
,
an
d
ch
ar
ac
ter
izatio
n
.
Fo
r
m
an
d
p
-
x
y
len
e,
th
e
g
r
a
v
im
etr
ically
p
r
ep
a
r
ed
c
o
n
ce
n
t
r
atio
n
is
n
o
t
co
n
f
ir
m
ed
b
y
th
e
GC
tech
n
iq
u
e
d
u
e
to
th
e
s
ep
ar
atio
n
p
r
o
b
lem
.
T
h
e
r
ef
er
en
ce
m
ater
ial
was
ch
ar
ac
ter
iz
ed
u
s
in
g
a
m
ass
b
alan
ce
ap
p
r
o
ac
h
with
d
if
f
e
r
en
t
an
aly
tical
tech
n
iq
u
es.
T
h
e
m
ass
f
r
ac
tio
n
s
o
f
all
an
aly
tes
wer
e
ass
ig
n
ed
with
a
s
m
al
l
r
elativ
e
ex
p
an
d
e
d
u
n
ce
r
tain
ty
o
f
±
1
%.
Du
e
to
t
h
e
lack
o
f
av
ailab
ilit
y
o
f
tr
ac
ea
b
le
C
R
Ms
in
th
e
m
ar
k
et
f
o
r
an
aly
s
is
o
f
B
T
E
X
an
d
ch
l
o
r
o
b
e
n
ze
n
es,
th
e
m
ate
r
ial
will
b
e
u
s
ef
u
l
f
o
r
estab
lis
h
in
g
tr
ac
ea
b
ilit
y
to
SI
u
n
its
,
q
u
ality
co
n
tr
o
l
,
a
n
d
s
u
p
p
o
r
tin
g
lab
o
r
at
o
r
ies to
d
em
o
n
s
tr
ate
th
eir
m
eth
o
d
p
r
o
f
icie
n
cy
.
ACK
NO
WL
E
DG
E
M
E
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S O
F
AUTH
O
RS
Ibra
h
im
F
.
Ta
h
o
u
n
is
a
n
As
so
c
iate
P
ro
fe
ss
o
r
o
f
An
a
ly
ti
c
a
l
Ch
e
m
istry
a
n
d
Ch
e
m
ica
l
M
e
tro
lo
g
y
a
t
th
e
C
h
e
m
ica
l
M
e
tro
lo
g
y
Div
isi
o
n
,
Na
ti
o
n
a
l
In
st
it
u
te
o
f
S
tan
d
a
rd
s
,
Eg
y
p
t.
He
re
c
e
iv
e
d
a
P
h
.
D.
d
e
g
re
e
in
a
n
a
ly
ti
c
a
l
c
h
e
m
istry
fro
m
Ca
iro
Un
i
v
e
rsity
.
His
re
se
a
rc
h
in
tere
sts
in
c
l
u
d
e
th
e
d
e
v
e
l
o
p
m
e
n
t
o
f
n
o
v
e
l
m
e
th
o
d
o
l
o
g
ies
a
n
d
p
r
o
c
e
d
u
re
s
a
s
we
ll
a
s
t
h
e
d
e
v
e
lo
p
m
e
n
t
o
f
c
e
rti
fied
re
fe
re
n
c
e
m
a
teria
ls
(CRM
s)
in
th
e
f
ield
o
f
c
h
e
m
ica
l
a
n
a
ly
sis.
Cu
rre
n
tl
y
,
h
e
is
a
n
a
c
ti
v
e
m
e
m
b
e
r
o
f
th
e
I
n
tern
a
ti
o
n
a
l
B
u
re
a
u
o
f
Weig
h
ts
a
n
d
M
e
a
su
re
s
(BIP
M
)
wo
rk
in
g
g
r
o
u
p
s
(CCQM
-
OA
WG
,
CCQM
-
IRW
G
)
a
n
d
th
e
In
tra
-
Afric
a
M
e
tro
lo
g
y
S
y
ste
m
(AFRIM
E
TS
).
He
c
a
n
b
e
c
o
n
tac
ted
a
t
e
m
a
il
:
I
b
ra
h
im.Tah
o
u
n
@n
is.sc
i.
e
g
;
Tah
o
u
n
_
n
is@y
a
h
o
o
.
c
o
m
.
Mo
h
a
m
e
d
A
d
ly
G
a
b
-
All
a
h
i
s
a
re
se
a
rc
h
e
r
a
t
th
e
Ch
e
m
ica
l
M
e
tro
lo
g
y
Div
isi
o
n
,
Na
ti
o
n
a
l
In
sti
tu
te
o
f
S
tan
d
a
rd
s
,
Eg
y
p
t
.
He
re
c
e
iv
e
d
h
is
P
h
.
D.
fro
m
th
e
Un
iv
e
rsit
y
o
f
S
c
ien
c
e
a
n
d
Tec
h
n
o
l
o
g
y
(S
o
u
t
h
Ko
re
a
)
in
2
0
2
3
u
n
d
e
r
th
e
d
irec
ti
o
n
o
f
Dr
.
By
u
n
g
j
o
o
Kim
.
Hi
s
re
se
a
rc
h
fo
c
u
se
s
o
n
d
e
v
e
lo
p
in
g
stra
teg
ies
fo
r
g
l
y
c
o
p
e
p
ti
d
e
e
n
rich
m
e
n
t
a
n
d
a
n
a
ly
sis
u
si
n
g
n
a
n
o
-
LC
-
M
S
/M
S
.
His
re
se
a
rc
h
a
lso
in
c
lu
d
e
s
th
e
d
e
v
e
lo
p
m
e
n
t
o
f
a
n
a
ly
ti
c
a
l
m
e
th
o
d
s
fo
r
t
h
e
a
n
a
ly
sis
o
f
o
rg
a
n
ic
c
o
n
tam
i
n
a
n
ts
a
n
d
n
u
tri
e
n
ts
(i.
e
.
,
m
y
c
o
to
x
in
s,
a
n
ti
b
i
o
ti
c
re
sid
u
e
s,
a
n
d
v
it
a
m
in
s)
i
n
fo
o
d
s
u
sin
g
m
u
lt
i
-
a
n
a
ly
te
m
e
th
o
d
s
(LC
-
M
S
/
M
S
).
He
c
a
n
b
e
c
o
n
tac
ted
a
t
e
m
a
il
:
m
o
h
a
m
e
d
a
d
ly
_
n
is@y
a
h
o
o
.
c
o
m
.
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