Professional Documents
Culture Documents
R. T.
977
Environment Environnement
Canada Canada
Rapports Techniques
Le rapports techniques ont des documents de recherche qui revetent une assez
grande importance pour etre con erves mais qui, pour une raison ou pour une autre,
ne conviennent pas a une publication scientifique prioritaire. Pour toute demande
de renseignements concernant un rapport particulier, il faut s'adresser au service
responsable.
Department of Fisheries and the Environment Ministere des Peches et de l'Environnement
(Numbers 1-456 in this series were issued (Les numeros 1-456 dans cette serie furent
Research Board of Canada. The series des recherches sur les pecheries du Canada.
name was changed with Les nom de la serie fut change avec Ie
by
1977
iii
TABLE OF CONTENTS
Introduction 1
Surface Samples 5
Subsurface Samples 8
Filtration 10
Sources of Error 11
Sediments 23
Page
Standard Preparation 26
Stock Standards 26
LIST OF TABLES
,
..l. Sediment classification 3
LIST OF FIGURES
ABSTRACT
(Si, AI, Ti, Fe, Mn, Mg, Ca, Na, and K) and the trace elements
(Zn, Hg, Cu, Pb, Co, Ni, Cr, V, Li, Be, Bar Rb, and Sr) in
SOMMAIRE
INTRODUCTION
Lahey 1963, 1965, Nota and Loring 1964, Loring and Nota 1966, 1968,
report has also been prepared for this region (Loring and Nota
ion (Loring 1975, 1976 a, b). The data have also been used
or leave f system.
size determination, the major elements (Si, AI, Ti, Fe, Mn, Ca, K,
Na, Mg) and trace elements (Hg, Zn, Cu, Pb, Co, Ni, Cr, V, , Be,
matter.
Table 1
SEDIMENT ClASSIFICATION
"If two components represent more than 30% each, the finer grained
component is indicated by its noun, the other with an adjective with
the adverb "vcr/He.g. very sandy pelite and not very pelitic sand. The
term calcipclite is also extended to include calclpelitic petite,
eters between 2 and 0.05 rom (sometimes subdivided into coarse sand
(2~O.5 rom), medium sand (0.5-0.25 rom), fine sand (0.25-.125 mm),
or very fine sand (.125-0.05 rom). For material smaller than 0.05
sil.t particles between 0.05 rom and 0.002 rom, and cl.ay particles
less than 0.002 rom in diameter. The term cal.carenite is calcareous
Most f the colors are estimated when the samples are fresh and wet,
Collect Observations
re col ted from the sea floor and from the water column using
is of substrate or water
Surface Samples
by a modified Van Veen grab sampler. The Van Veen grab sampler
2
used in our studies takes a sample of the sea floor of about O.lm
sea surface and the deck will result in erroneous grain size
For gravel size material (>2 mm diameter) and sands (2-0.5 mm)
date, time) waxed ice cream containers and stored onboard until
so, the grab is opened slowly, and the water drained off so as
not to wash the sample unduly. Once the top of the sediment is
After the surface layer has been sampled, the grab is opened
the surface and subsurface material and the other of the subsurface
Subsurface Sampling
conditions with time. They are usually taken in areas having fine
grained sediments. We have used two types: the gravity corer which
free-falls from the ship and penetrates the sea floor by gravity,
and the piston corer which is dropped from a set distance above the
sucked into the core barrel by an upward moving piston as the core
plastic core 1 are placed inside the core barrels. After the
corer is brought on board, the liners are capped at the bottom, the
until. all the water inside the liner has risen to the top. The
core liner is then cut off at the sediment water interface, capped
ruise No., S~.No. ,depth, time) along with core length, general
piston corers with weights of 160 kg and 545 kg; plastic 1 1/2"
the core liners with diameters greater than 2" are satisfactory for
Samples are taken with 12 litre Niskin bottles which have been
Filtration
between the top of the rack and the top end-cap of the Niskin
7\ih~itl bo r rle
""ilara''''
FIG. 1 Equipment for pressure filtration.
(From Sundby 1974)
The samples are f tered through Nuclepore filters (47 rom
weighed.
Source of Error
suspended matter.
13.
volumes greater than 2.0 1 and to to. OIl for 2.0 I and
Initial Sample t
litre (MSE LR-6) was used to make the samples salt free and to
Sedimentological Analyses
and air dried for 24 hours, after which, sufficient sample material
gravel samples, about 300 pebbles are set aside for petrographic
ana s. Sand and mud samples for grain size analysis are sorted,
separating the mater 1 >2 rom from the finer material. Material
>2 rom is set aside for petrological analyses. The analyses for
Chemical Analyses
At least two separate samples are taken and dried under diff-
Soluble sea salts are removed from samples required for the
elements des under the Ocean Dumping Act and the Env 1
Contaminants Act.
intact and does not attack the resistant iron and manganese oxide
minerals.
Procedure:
The evaporating dish is covered and let stand in the fume hood for
f sk. The sediment in the teflon dish is now free from acetic acid
the last washing the supernatant does not become clear a few
drops of 25% acetic acid should be added and recentrifuged. The non-
ating dish and dried in the oven at 110C. Care must be exercised
that none of the sediment is lost at any time. When dry, the dish
plus sample is weighed and the weight of the acetic acid soluble
19.
It has been found (Loring and Nota 1973) that the elemental
size. This occurs because the host minerals of the elements and
Procedure:
53-37]J
l 37]J sieve
<2]J
C <2]J centrif.
I
16-2]J <16]J Atterberg
I Cylinder
I
37-16]J >16]J Atterberg
f Cylinder
through 500~, 53~ and 37~ sieves in sequence with the aid of H20
and light brushing. The fractions are collected from each sieve
110oe, and weighed. The dry > 500~ fraction is passed through a
2 mm sieve to remove rock fragments > 2 mm. The < 37~ fraction is
(Tanner and Jackson 1947) and the < 2~ material is syphoned off and
and we
The 37-2~ fraction is transferred from the bottle into an
made up to mark with 0.16N NH shaken and let stand for the
40H,
i time derived from Table 2.
21.
Table 2
+:
TEMP C 5 em 5 em 10 em 30 em 30 em 30 em
21 3 54 58~ 29 16 1 28 21 57 5 29
5
22 3 49 57 28 31 1 25 21 24 5 21
23 3 44 55~ 27 46 20 51 5 13
24 3 39 54 27 01 20 18 5 05
The syphon tube is then unclamped and the 2-16 ~ fraction collected
1 Co Ni Pb are to determined.
Sample Decomposition
Sediments
Boric acid is used to complex the fluorides which also makes the
for major elements, but a larger 1.0 g sample is required for trace
elements.
Reagents:
Decomposition procedure:
for 1 hr. Care should be taken that the vessels remain immersed
vessels should immediately be removed from the water bath and placed
in cold water. The water level should not reach the threaded cover.
vessel may be heated on the hot plate or in the drying oven located
the fume hood. After cooling, the contents are washed into a
decomposed.
sary to use high purity Ultrex grade HCI, HN0 and HF. The reagent
3
grade acids contain large amounts of silicon and iron. For some
Reagents:
Procedure:
Standard Preparation
Stock Standards
water.
Standards: Sed s
llg/ml
Al
'7 c:;
I .,J
1
.J..
J:;
..J V
n ':l
..JeVV
nn 4.50 6.00 12.00
Ba standard
Si standard
Sr standard
of 0.1 - 1.0 ppm Sr. Add KCl to each standard so that the final
2~10 ppm Ti. Add KCl to each standard so that the final
si blank matrix.
30.
Be standard
Cr standard
Rb standard
to the samples.
of the sample matched to the standards. For fast, but less accurate
V standard
BCR-l, G-2 and GSP-l and Canadian Certified Reference rock standards
TABLE 3
1
AGV-1 BCR-l 1 G-2 1
GSP-l 1 MRG-1 2 SY-2 2
IFlanagan (1973)
2Abbey et aL (19'75)
32.
Four rock standards giving the expected range for each element
diluted to 25 mI. This gives standard solutions for Si, Mn, Cu and
appropriate matrix, working standards are obtained for AI, Ca, Fe,
K, Mg and Na.
rock is weighed.
TABLE 4
2500x dilution
Si Mn Cu Zn
25000x dilution
4
Ca Fe K Mg Na
MRG-l 1.80 G-2 0.56 G-2 0.74 MRG-l 0.06 G-2 0.18 MRG-l 0.21
SY-2 2.57 AGV-l 1.40 SY-2 1.77 BCR-l 0.56 AGV-l 0.37 GSP-l 0.83
G-2 3.26 BCR-l 1 98 BCR-l 3.75 AGV-l 0.96 SY-2 0.64 BCR-l 0.97
AGV-l 3.65 2.30 MRG-l 5.00 GSP-l 1.84 BCR-l 0.84 SY-2 1.30
33.
Table 5 shows the analytical scheme for the major and trace
elements in sediments.
Table 5
Sample Preparation Diagram for Silicate Rock Analyses
directly.
concentration of 1500 ppm, and these are analyzed for Ba, Sr and Ti.
34.
For the determinations of AI, Ca, Fe, Mg, and Na, a further
decomposed in the Teflon vessel and diluted to 100 mI. From this
solution Be, Co, Cr, Cu, Li, Ni, Pb, Rb, V, and Zn are determined
directly.
the ization.
Table 6
Perkin-Elmer 306
Reducing Red
Element Wavelength Setting Slit Setting Oxidant 'Flame Filter
Al 309* UV 4 N 0 .;
2
Ca 211 Vis 4 N 0
2
Fe 248* UV 3 Air
Mg 285 UV 4 N 0
2
Mn 279* UV 3 Air
Si 252* UV 3 N 0 .;
2
Ti 365* UV 3 N 0 .;
2
Ba 277 Vis 2 N 0 .;
2
Be 235 UV 4 N 0 .;
2
Co 241* UV 3 Air
Cr 358* UV 4 N2 0
Cu 325 UV 4 Air
Pb 283 UV 4 Air
Interferences
Table 7 ind tes the relative accuracy of the major and minor
element data for W-l and G-2 by the comparison of our values to
TABLE 7
Elements in U.S.G.S. Standard Rocks:
Coeff.
A B Yar.(%)
AI W-l 7.94 7.68 1.5
G-2 8.15 8.11 '1..7
Co W~l 7.83 7.83 0.7
G-2 1.39 1.40 1.9
Fe W-l 7.76 7.96 0.4
G-2 1.85 1.90 5.0
K W-l 0.53 0.56 4.1
G-2 3.74 3.62 1.2
Mg W-j 3.99 3.86 0.1
G-2 0.46 0.44 4.1
Mn W-l 0.132 0.127 1.1
G-2 0.026 0.025 4.4
No W-l 1.59 1.60 1.2
G-2 3.02 0.8
Si W-l 24.6 24.6 2.6
G-2 32.3 31.5 0.8
TI W-l 0.64 0.67 1.5
G-2 0.30 0.31 2.6
A Flanagan
B Rantala and Loring, (1975 )
3 of
38.
TABLE a
Trace Elements in U.5.G.S. Stt:mdcnd Rocks (ppm)
AGV-l BCR-l W-l 075-1 G-2 GSP-l PCC-l
Bo (0) 1208 675 160 2.4 1870 1300 1.2
(b) 1140 630 156 <5 1970 1230 <5
Be (0) 3 1.7 0.8 2.0 1.5
(b) 2.0 2.1 0.9 <0.5 2.9 1.7 <0.5
Co (0) 14 38 41 133 5.5 0 112
(b) 18 36 41 128 7 9 109
Cr (a) 12 18 114 7 12
(b) 9 11 no not enelyzed 7 12 not analyzed
CI.I (0) 60 18 110 7 12 33 11
(b) 59 15 122 7 12 31 11
u (a) 12 13 14 2 37 32 2
(b) 12 14 14 2.7 34 30 1.7
Ni (0) 18.5 16 76 22.59 5 12.5 2339
(b) 12 <12 66 2420 <12 <12 2420
Pb (a) 35 18 8 14 31 51 13
40 16 <1:2 13 34 59 <12
Rb (a) 67 47 21 168 254
(b) 67 49 21 not analyzed 166 248 notol'lclyzed
Sf 657 330 190 0.35 479 233 0.41
(b) 698 363 194 <2 457 245 <2
V (a) 125 399 264 10 35 53 30
128 446 285 <15 42 62 23
Zn (a) 84 120 86 45 85 98 36
90 129 86 32 87 105 28
a (1973)
b Ranta and , (1975)
TABLE 9
Precision of Variation} for the
Determination of Trace Elements in
U.S.G.S. Standard Rocks (%)
W-l DrS-} G-2 GSPl PCC-T
3.2 1.1 1.4
Be 2.8 4.0 1.7 1.9
Co 14 2.4 0.9 7.9 12 0.9
Cr 5.6 0.5 6.1 1.9
Cu 4.2 3.7 4.2 4.3 4.9 5.6
u 2.6 2.2 6.4 0.8 1.5 10
Ni 4.5
Pb 4.3 15 11 8.6
Rb 2.3 1.2 4.1 2.1 0.5
Sr 2.2 2.9 5.1 1.6 3.5
V 1.2 2.4 0.7 6.0 4.3 7.5
Zn 1.3 1.6 0.7 1.5 4.1 1.0 1.8
39.
Nisken bottle were filtered. Each filter (mean SPM wt 1.99 mg)
.div.
mean
x 100) was 2.4% for Fe and 4.4% for Mn.
40.
Apparatus
Water bath
BOD bottles
Tygon tubing
Reagents
Ni c d conc low Hg
Sample P
and digest 1 hour at 60C. Remove from water bath and add
be the
42.
Standard Preparation
Procedure
rinse it with H20. After the peak falls back to the baseline
weight in grams.
the rock standards G-1 and W-l for which we obtained values
Magnetic s rrer
Reagents
85% H3P04
Solid NaP
1 liter of H2S04
45.
s 49.04 g of
water lute to 1 1
of concent
Procedure
s is a 00 ml r ask. Exac 10 ml of
is back trated
The color 11
to a bl sh-black-grey at s po
fe
46.
Calculation of Results
= 10(1-~) x F
S
S = standardization blank titration, ml ferrous solution
Standard
:::::: X
(x 100 :::: %)
a1 f o rmu I
Precision
Method
Reagents
Procedure
Calculation
P/Q x 0,200 x 100
% CaC0
3 = weight abs. dry soil
Note: Tubes filled with CaC1 2 should be stored in desiccator and
tion of 2.6%)
and 11 VA.LU,C::S as
a hydrosu
t of i to ho pH at
Na 1, effect ly serves as
fer.
Centr uge
50 ml fla
50.
Reagents
1 litre
Sodium bicarbonate. 1M
Procedure
centrifuge tube.
r di necessary to Fe
of Ferrous (FeO)
ac %)
Satura ac lut
Ceri . 5N
52.
Calculation
are made on each sample: one from the surface layer and one from the
diagram, Fig. 4). Two drops of HCl are added to each of the sediments
5
A B
1
are
4)
1'e
paper
oxygen supp
f The the
to the a
A negative ferric iron test soon becomes a positive one and shows
REFERENCES
Rep.BI R-72 7 1 p.
. Chern. 6 99- 2.
Acta 37 1
85 p.
Kothandaraman P. J. F. 1 1976.
Absorp. . 15 20-121.
56.
140: 23 p.
MS Rep. 189: 53 p.
2327-2347.
58 98 p.
Geol. 2 9 -235.
58.
97-99.
pp. 60-65.