EPA R2-72-039
 August 1972               Environmental Protection Technology Series
 The Appearance  and Visibility
 of Thin Oil  Films on  Water

                                    National Environmental Research Center
                                    Office of Research and Monitoring
                                    U.S. Environmental Protection Agency
                                    Cincinnati, Ohio 45268

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             RESEARCH REPORTING SERIES
Research reports of the Office of Research and
Monitoring, Environmental Protection Agency, have
been grouped into five series. These five broad
categories were established to facilitate further
development and application of environmental
technology. Elimination of traditional grouping
was consciously planned to foster technology
transfer and a maximum interface in related
fields. The five series are:

    1. Environmental Health Effects Research
    2. Environmental Protection Technology
    3. Ecological Research
    4. Environmental Monitoring
    5. Socioeconomic Environmental Studies

This report has been assigned to the ENVIRONMENTAL
PROTECTION TECHNOLOGY series. This series describes
research performed to develop and demonstrate
instrumentation, equipment and methodology to
repair or prevent environmental degradation from
point and nonpoint sources of pollution. This work
provides the new or improved technology required
for the control and treatment of pollution sources
to meet environmental quality standards.

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                                           EPA-R2-72-039
                                           August 1972
    THE APPEARANCE AND VISIBILITY OF

          THIN OIL FILMS ON WATER
             Bernard Horstein
Edison  Water Quality Research Laboratory
         Edison,  New Jersey   08817
          Program  Element 1B2041
 NATIONAL ENVIRONMENTAL RESEARCH CENTER
    OFFICE OF RESEARCH AND  MONITORING
  U.S.  ENVIRONMENTAL PROTECTION AGENCY
          CINCINNATI,  OHIO ^5268

      a U. S. GOVERNMENT PRINTING OFFICE :  1972 O - 477-049
For sale by the Superintendent of Documents, U.S. Government Printing Office
            Washington, D.r. 204D2 - Price $2.50
               Stock Number 5501-00420

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                          ABSTRACT
When oil films of controlled thickness (up to 3000 nanometers)
were formed upon water surfaces in the laboratory, an inherent
and orderly thickness-appearance relationship was confirmed —
a relationship that is independent of oil  type and water type.
The laboratory studies also investigated the effects of viewing
conditions upon the ase with which these thin films were visible.

Out-of-doors observations were made; these and the observations
reported by other sources corresponded with the laboratory re-
sults.  The visibility of a thin oil film depends not only upon
its thickness-dependent inherent appearance, but also upon con-
ditions external to the film:  the nature of illumination and sky
conditions, sun angle, color and depth of water, color of bottom,
and viewing angle.

Color photographs illustrate the points discussed.
                              iii

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                          CONTENTS


Section                                                 Page

   1.   CONCLUSIONS                                        1

   2.   INTRODUCTION                                       3

       2.1  Reasons for this Investigation                3
       2.2  Background and Approach                       6

   3.   THEORY                                            11

       3.1  Applicable Phenomena                         11
       3.2  Reflectivity                                 11
       3.3  Interference                                 13
       3.4  Fluorescence not Significant                 19

   4.   EXPERIMENTAL                                      21

       4.1  General                                      21
       4.2  Physical Procedure                           22
       4.3  Photographic Procedure                       27

   5.   RESULTS                                           31

       5.1  General                                      31
       5.2  Spreading on Different Waters                31
       5.3  Photographs of Laboratory Oil Films          31
       5.4  Field Observations                           37

   6.   DISCUSSION                                        87

       6.1  Inherent Optical Properties and Visibility   87
       6.2  Results are General, not Unique              87
       6.3  Field Application of Results                 89
       6.4  A Modified Thickness-Appearance Table        90

   7.  GLOSSARY                                          93

   8.  REFERENCES                                        95

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                               FIGURES
                                                                       Page
 1.    Relative Sensitivity of the  Human  Eye  to  Light  of  Various           5
        Wavelengths
 2.    Oil  Film Appearance  and Effective  Thickness  vs.  Coverage           10
 3.    Reflection and Refraction of Light by  a Thin Film                  12
 4.    Arrangement for Photographing Oil  Film in Tray                     28
 5.    Light Arabian  Crude  (1  yl).   Thickness is 15 nm.                   41
 6.    Light Arabian  Crude  (2.5 yl).  Thickness  is  38  nm.                 43
 7.    Light Arabian  Crude  (5  yl).   Thickness is 75 nm.                   45
 8.    Light Arabian  Crude  (10 yl).  Thickness is  150  nm.                 47
 9.    Light Arabian  Crude  (20 yl).  Thickness is  300  nm.                 49
10.    Light Arabian  Crude  (50 yl).  Thickness is  750  nm.                 51
11.    Light Arabian  Crude  (100 yl).  Thickness  is  1500 nm.               53
12a.  Light Arabian  Crude  (200 yl).  Thickness  is  3000 nm.               55
12b.  Light Arabian  Crude  - Enlarged view of 3000  nm  film,
        second from  top of Figure  12a.                                   57
13.    South Louisiana Crude (1 yl).  Thickness  would  be  15  nm
        for full coverage.                                              59
14.    South Louisiana Crude (2.5 yl).  Thickness  is 38 nm.               61
15.    South Louisiana Crude (5 yl).  Thickness  is  75  nm.                 63
16.    South Louisiana Crude (10 yl).  Thickness is 150 nm.               65
17.    South Louisiana Crude (20 yl).  Thickness is 300 nm.               67
18.    No.  2 Fuel Oil (1 yl).   Thickness  would be  15 nm with
        full coverage.                                                   69
19.    No.  2 Fuel Oil (10 yl).  Thickness is  150 nm.                     71
                                  VI

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                                                                       Page


20.   Agha Jari Crude (1  yl).   Thickness is 15 nm.                       73

21.   Agha Jari Crude (10 yl).   Thickness is 150 nm.                     75

22.   Effect of Background Brightness of Visibility (a),  (b),
        (c):  Bright and Medium Background,  (d):   Dark Back-
        ground.                                                         77

23.   No. 2 Diesel  Fuel  on Ran'tan River                                79

24.   No. 2 Diesel  Fuel  on Ran tan River (iridescence)                   79

25.   No. 2 Diesel  Fuel, with  bare water exposed.                        79

26.   No. 2 Fuel Oil on  Arthur Kill (iridescence)                        79

27.   Diminishing visibility as viewing angle departs from
        vertical.                                                       81

28.   Visibility of 50 gpm,  100 ppm oil-water discharge,  from
        the surface (a)  and  from the air (b).                           83

29.   Visibility of 25 gpm,  10 ppm discharge, from the  surface
        (a) and from the air (b).                                       83

30.   Undimini shed visibility of driveway oil film in low
        intensity light.                                                85

31.   Reduced visibility in  direct sunlight compared to shadow.          85

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                             TABLES



                                                                   Page




  IA     Oil  Film Thickness  vs.  Visible  Color                        7





  IB     Oil  Film Thickness  vs.  Surface  Coverage                     8





 II      Theoretically Implied Color vs.  Wavelength                  16





III      Wavelengths Subject to Interference vs. Thickness           18





 IV      Comparison of Oil  Spread on Sea Water and Distilled Water  32





  V      Schematic Basis  for Thickness-Appearance Relationship      91
                              vm

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                       1.   CONCLUSIONS


1.  Oil  films up to approximately 3000 nanometers  (3 microns)
    thick show characteristic inherent color effects that  are
    governed by interference phenomena.

2.  Within this range (up  to 3000 nanometers),  these inherent
    color effects have, in theory and in fact,  an  orderly  re-
    lationship to film thickness and are independent of the
    type of oil forming the film.

3.  A table such as that published by the American Petroleum
    Institute and included in this report or an equivalent
    table assembled from the EPA tray photographs, reliably
    indicates film thickness in this range.

4.  The visibility of an oil film is not constant  but depends
    upon conditions of observation as well as upon its inherent
    characteristics.  Optimum conditions include the absence of
    direct sunlight, a white overcast, a high viewing angle
    (approaching vertical), and low background brightness  from
    the underlying water.

5.  As viewing conditions  deviate from the optimum, the visi-
    bility of a given film is lessened.

6.  Under sufficiently adverse conditions, visibility becomes
    low or nil for films less than 3 microns thick.

7.  For films too thin to show color, an adjacent  area of  bare
    water for comparison is usually necessary to discern the
    higher reflectivity of the film.  This is not  usually  re-
    quired for films that show definite color.

8.  For films too thin to show color, waves or chop tend to
    obscure the higher reflectivity of the film.

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                      2.   INTRODUCTION

2.1      Reasons for this  Investigation

        Present Federal  regulations (Ref.  1)  prohibit harmful
        discharges of oil.  Harmful discharges are stated by
        the regulation to be those which:

                 11	cause a film or sheen upon or
                 discoloration of the surface of the
                 water	"

        The prohibition applies not only to oil per se, but also
        to oil mixed with water.  The latter includes, for ex-
        ample, oily ballast or bilge water from a vessel, and
        waste water from an offshore drilling platform.

        The term "sheen" is defined in the regulation as:

                 "an iridescent appearance on the surface
                 of the water",

        and the American Heritage Dictionary definition of
        "iridescence" is:

                 "producing a display of lustrous,
                 rainbow-like colors".

        For convenience, this regulation will be referred to as
        the "sheen regulation".
2.1.1   Visibility as a Criterion

        The sheen regulation, if read literally, prohibits the
        existence of an oil film, sheen, or discoloration; proof
        of existence depends upon detectability.  In the absence
        of devices on the water surface for chemical or physical
        sampling and analysis, potential detection is by remote
        sensing devices.  These devices usually respond to the
        electromagnetic spectrum, from the ultraviolet through
        the visible and infrared, and into the microwave region.

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        In this  context,  the  human  eye  is  a  remote  sensing
        device,  responding  to the visible  spectrum  in  the
        400 nanometer (nm)  to 750 nm  wavelength  band  (Fig.l).
        Compared with other presently developed  remote sensing
        systems, the eye  has  greater  sensitivity, it  is  stan-
        dard equipment with observers,  and it  is served  by  a
        data processing center which  interprets  and correlates
        the eye's output  with excellent reliability and  repro-
        ducibility.

        These attributes, together  with the  fact that  the
        definition of "sheen" invokes the  visible spectrum,
        leads to the stipulation that detection  by  eye,  or
        visibility,  is the  primary  criterion for the  exis-
        tence of a film,  sheen, etc.  Accordingly,  this
        report is concerned with visual  properties  of  thin
        oil films and with  the visibility  of oil films.

2.1.2   Problem and Scope

        Limiting cases of visibility  involve very thin films
        which produce rainbow-like  colors  and  films which are
        even thinner and  show no color.  Films too  thick to
        show bright color are assumed readily  visible  either
        by virtue of their self-color (browns  and blacks for
        crudes and residuals) or by virtue of  their calming of
        the water.  These thin films  range in  thickness  from
        about 15 nm, about 1/30 the wavelength of visible light,
        to about 3000 nm  (3 microns), about  6  times the  wave-
        length of visible light.

        The following questions developed  in our examination of
        the sheen regulation:

        (a)  Once thin oil  films have been formed,  what  are
             their inherent optical characteristics and
             what are the corresponding inherent visual
             effects?

        (b)  Do these inherent visual effects  imply an
             inherent, or constant, visibility or are
             there other  factors that make visibility
             variable?   Factors to consider include
             oil type, illumination,  and viewing position.

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    100 i-
     50
>
t—
<
         400
                         500
                                        600
                                                        700
                       WAVELENGTHS IN NANOMETERS (nm)
Figure 1.   Relative sensitivity of the human  eye to light  of

             various wavelengths (from Ref.  7).

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        (c)   If we  can  establish  relationships  concerning
             the visibility  of oil  films  per  se,  can we
             also establish  relationships  between the  con-
             ditions  of oily water  discharge  and  the for-
             mation of  surface films?

        (d)   Can we then relate conditions of oily water
             discharge  and their  consequent visibility?

        We undertook  a  two-part study.  This  report addresses  itself
        to the first  two questions  that concern the oil film per  se.
        The  second  part, concerning the latter  two questions,  is  the
        subject of  a  separate report.
2.2     Background and Approach

2.2.1   Background Information

        With the exception of some crude oils  and processed products
        that form discrete "lenses" on the water's surface, most
        crudes and products spread spontaneously because of surface-
        active components (Ref. 2).  This spreading can continue
        until extremely thin films are formed.  The American Petro-
        leum Institute (API) (Ref. 3) indicates  a relationship be-
        tween film thickness and visual  effect.   Table I contains
        this information, with thickness values  in various metric
        units added for convenience.

        In Table I, a film 38 nm thick is listed as "barely visible
        under most favorable light conditions".   This  suggests that
        there is a limiting thickness below which a film is not
        visible.  It also suggests that this limiting  thickness can
        vary with lighting conditions.  The other entries indicate
        an orderly trend between appearance and  thickness, in three
        main groupings:

                  Up to 150 nm  - colorless film

                  300 - 1000 nm  - rainbow effects
                                  (iridescence)

                  Greater than 1000 nm  - progressively re-
                                         duced iridescence.

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                                   TABLE IA *



                     OIL FILM THICKNESS VS. VISIBLE COLOR
Appearance
Barely visible under most favorable light
conditions
Visible as a silvery sheen on surface
First trace of color may be observed
Bright bands of color are visible
Colors begin to turn dull
Collors are much darker
Film Thickness

1.



1
in.
5xlO-6

3xlO-6
6x10-6
2x10-6
40x10-6
80x1 0~b

3

7
1
3
1
2
cm
.8x10-6

.6x10-6
.5xlO-5
.IxlO-5
.OxlO-4
.OxlO-4

3.

7.
1.
3.
1.
2.
V
8x1

6x1
5x1
1x1
0
0

0-2

0-?
o-1
o-i



3.

7.
1.
3.
1.
2.
nm
8x1 01

6x1 01
5x1 02,
1x10^
Oxl O3
Oxl O3
u
Angstrom
3

7
1
3
1
2
.8xl02

.6xl02
.5xl03
.IxlO3
.OxlO4.
.OxlO4
*Tables IA and IB are based upon Ref.  3

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                                                 TABLE IB



                                   OIL FILM THICKNESS VS. SURFACE COVERAGE
00
Film Thickness, nm
3.8xlO]
7.6xlO]
1.5x10?
S.lxlO2
1.0x103
2.0xl03
Coverage
gal/acre
0.04
0.08
0.16
0.32
1.08
2.16
gal/mile2
25
50
100
200
666
1332
mg/m2 *
38
76
150
310
1000 (1 gm)
2000 (2 gm)
                                *Computed values assuming film specific gravity =1.0

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        The API report (Ref.  3)  does  not  indicate  the  type  or
        types of oil  used or  the range  of lighting investigated.
        The General  Research  Corporation  (Ref.  4)  reports an
        appearance -  thickness  relationship  (Fig.  2) based  upon
        a Santa Barbara crude that agrees substantially  with the
        API data.   This agreement suggests,  but does not estab-
        lish, that appearance is not  dependent  upon the  type of
        oil.

        Neither set of data mentions  the  effect of other variables
        such as water depth,  bottom characteristics, or  viewing
        angle upon visibility.   Experience,  however, has shown
        that visibility is best under an  overcast  sky  (Ref. 5 and
        6).  We thus  start out  with the central notion that ap-
        pearance is  related to  thickness, but not  oil  type, and
        that visibility is variable.   The identity and influence
        of other factors affecting visibility was  not  known.

        Additionally, we found  that the existing verbal  descriptions
        used in the appearance  relationships were  vague  enough that
        different observers could classify the  same film into dif-
        ferent appearance categories.
2.2.2   Approach
        In view of the foregoing, we set out to form oil  films  of
        known thickness under laboratory conditions  and to vary
        factors of interest in a controlled manner.   These factors,
        besides film thickness, included type of oil, surface state
        of the water, water salinity, water opacity  and character
        of bottom.  Along with these controlled experiments, random
        or contrived observations out-of-doors were  made  to corre-
        late the laboratory observations with those  in the outdoor
        environment.

        To avoid the inescapable difficulty of describing in words
        the complicated visual effects, color photography was se-
        lected for primary documentation.

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   1x10
      -3
          — 3000
          — 2000
          — 1000
o

>
   1x10
      -5 .
             300
             200
             100
             50
    1x10
       -6
        0.001
                                                             DULL GRAY/BROWN
                                                          IRIDESCENCE
                                        SILVERY SHEEN
                          -I—I  I  I  I
                                            OIL SAMPLED, gm/ff'
                                                                            DULL IRIDESCENCE

                                                                         WITH BROWN STREAKS
                                                                                              1.0
Figure 2.
                     Oil  film  appearance  and effective thickness  vs. coverage
                                      (from  Ref. 4).
                                            10

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                          3.   THEORY

3.1      Applicable Phenomena

        The appearance of a thin oil film on  water is  associated
        with that part of the incident light  that is  reflected
        from the water-air interface or from  the  oil -air and  oil-
        water interfaces.  Where the oil  film displays colors,
        these colors are the  result of interference between re-
        flections from the two oil  interfaces.

3.2      Reflectivity

        Reflectivity is defined as  that fraction  of light (inten-
        sity) incident upon a surface that is reflected.  Re-
        flectivity is a function of the angle of  incidence (from
        the normal) and the refractive indices of the media.

        The Fresnel equation  applies to reflection from the sur-
        face of a transparent medium in air:
                R = u
                                        tan(i+r)
        In this equation, the relationship between i  and r is ex-
        pressed by Snell's Law:
                sin r  =  y-j

        In these equations:

                 R  =  light reflected
                       light incident

                 i  = angle of incidence (see Fig. 3)

                 r  = angle of refraction (see Fig. 3)

                 y. = refractive index of air, taken as 1.0

                 y  = refractive index of denser transparent
                      medium
                             11

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       FROM SOURCE
TO EYE
                                                             OIL FILM
                                                            WATER
Figure 3.  Reflection and refraction  of light by a thin film (from Ref. 7)
                                  12

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        We  calculated  the  values of  reflectivity from equation  (1),
        noting  that  angle  of  incidence  is measured from the normal
        and using  the  standard  value of y for water of 1.33 and an
        average value  for  oil of 1.5.

                                               R(water)

                                                0.021

                                                0.060

                                                0.21
                                        film  should  be  distin-
             guishable from a  water surface because  of  its  higher
             reflectivity if it is  observed at  a  near vertical
             viewing angle.

        (b)   As viewing angle  (angle of incidence) becomes  less
             vertical, reflectivity of oil compared  to  water  de-
             creases until  water has a higher reflectivity  than
             oil.   This latter case represents  glare.

        (c)   Except for very high angles of incidence  (approaching
             a horizontal viewing angle) only a small fraction of
             incident light is reflected. The  rest  is  transmitted
             into  the water or oil  medium.
i
30
60
75

0
0
0
The tabulated values
(a) Even
without col
R(oil)
0.041
0.090
0.16
imply that
or, an oil
3.3     Interference
        Normal  illumination, or "white"  light,  contains  all  wave-
        lengths in the visible spectrum, and each  wavelength rep-
        resents a color to the eye.   Light has  wave-like properties
        similar to an AC voltage or  current. Two  light  rays of  the
        same wavelength can reinforce each other,  cancel  each other,
        or have some intermediate additive effect, depending upon
        whether they are in phase, 180°  (h wavelength) out  of phase,
        or with an intermediate phase relationship.   Optically,  ef-
        fects from these phase relationships are termed  interference.

        Rainbow effects (iridescence) from an oil  film on water  are
        due to interference; a given film thickness  will  produce dif-
        ferent phase relationships among the various colors  contained
        in white light.  Whether a given wavelength  or color is  rein-
        forced or cancelled out depends  upon its relationship to the
        film thickness.
                             13

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Any two rays of light, of the same wavelength,  X,
emanating from the same point of a broad,  uniform
source will be in phase.  Suppose ray 1  is reflected
from the top surface, and ray 2 is reflected from  the
bottom surface of an oil film on water.   Additionally,
since the oil film has a higher refractive index than
that of water, ray 2 will undergo a phase  shift upon
reflection of 180°, or % wavelength.  Figure 3  (Ref. 7)
schematically shows the longer optical path of  light
ray 2 compared with that of ray 1.  The difference in
optical path length, AL, is

          AL  = 2t (y2- sin2i)%                         (3)

where

           t  = film thickness

           y  = refractive index of oil
               forming the film

           i  = angle of light incidence
                (the same as viewing angle)
                measured from the normal to
                the surface.

For any given wavelength of light, the interference effects
depend upon the number of wavelengths in AL, taking into
account the 180  phase change (% wavelength) that  occurs
at the oil-water interface.

          If AL contains a whole number of wave-
          lengths, maximum destructive interference
          will occur; that is ray 1 and ray 2 are
          out of phase, and will cancel  each other.
          Mathematically, this condition is,

              AL = xX    (x = 1,2,3,4, etc)             (4)

          If AL contains an odd number of half
          wavelengths, maximum constructive
          interference will occur; that is,
          ray 1 and ray 2 are in phase, and
          they reinforce each other.  Mathe-
          matically, this condition is,

              AL = x|    (x = 1,3,5,7, etc)             (5)


                      14

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         Intermediate conditions will  give
         partial interference.

Transposing equations 4 and 5 allows calculation of the
wavelengths that give maximum effects.

For destructive interference:

         X = ^           (x • 1,2,3,4, etc.)   (4a)
             /\

For constructive interference:

         X = ^-          (x = 1,3,5,7, etc.)   (5a)
              J\

Since normal illumination contains all wavelengths, a given
film thickness will selectively reinforce some wavelengths
and cancel others, changing the color composition of the total
light reaching the eye and giving the effect of visual  color.
For illustration, assume an oil film, refractive index = 1.5,
viewed at an angle of 45°.  In Table II are the calculated
wavelengths within the visible at which interference will
occur for different film thicknesses.  Wavelengths between
408 and 816 nm are considered to be in the visible, or close
enough to influence the visual effect (see Fig. 1).

The approximate resulting color, listed in Table II, is ob-
tained through the following type of reasoning; 300 nm film
is used as the example:

     Constructive Interference:  at 544 nm (yellow-green)

     Destructive Interference:   at 408 nm (violet)
                                 and at 816 nm (red)

     Net results:                Original white light plus
                                 green, and minus red and
                                 violet results in a net
                                 green light.

The color sequence deduced as a function of thickness is, in
fact, the sequence found experimentally.  Examination of the
photographs confirms this.

Thus far we have established that films thinner than 150 nm
should display no color since wavelengths subject to inter-
ference are in the ultraviolet, outside the visible.  Between
75 and 150 nm, there is some slight influence in the violet/
blue end of the visible.  As a speculation, this may contri-
bute to the "silvery sheen" effect, which we interpret as a
film that shows no distinguishable color but which does

                     15

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                  TABLE II



THEORETICALLY IMPLIED COLOR VS.  WAVELENGTH
            Constructive
Destructive    Resulting
Film
Thickness, nm
75
150
200
250
300
AL
nm
204
408
545
677
816
Interference
at nm
408
816
(none)
451
544
Interference
at nm
(none)
408
545
677
816,408
Color
Approx.
Slight bl
warm tone
purple
blue/blue
green
uish

green

                16

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have a pearl-like or metallic luster.   We  also  see  that
films in the  200-300 nm range should display  a  variety
of colors of  high purity since in this  range  there  is
only one, or  at most two wavelengths that  show  strong
constructive  interference.

As film thickness increases, a greater  and greater
number of wavelengths exhibit strong interference.
Table III is  a list of wavelengths subject to con-
structive and destructive interference  versus film
thickness.  With an increasing number of wavelengths
(colors) that are intensified or depressed by a film,
the net color becomes a blend of colors distributed
through the visible spectrum, so that the  apparent
color becomes less and less pure.  In the  extreme,
such as with  a 3000 nm film, so many colors are in-
volved that the result approaches the "whiteness"
of a complete spectrum, and the effects become  a
weakening alteration of light grey and  dark grey
bands instead of a repeating sequence of pure colors.

We can now summarize a theoretically deduced trend  of
appearance versus film thickness;

         Thickness less than 150 nm:

              no color apparent

         Thickness of 150 nm:

              warm tone apparent

         Thickness of 200 to 900 nm:

              variety of colors, including
              purple, magenta blue, green,
              yellow, showing considerable
              purity, with a net rainbow-
              like effect

         Thickness greater than 900 nm:

              colors showing progressively less
              purity, degrading toward  grey as
              thickness increases.
                      17

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                             TABLE  III
              WAVELENGTHS SUBJECT TO INTERFERENCE  VS.
                             THICKNESS
  Film            Wavelengths  for
Thickness    Constructive Interference
  (nm)                (nm)
                                Wavelengths  for
                            Destructive  Interference
                                      (nm)
   300

   600

   900

  1200

  1500

  1800


  2100


  2400


  2700


  3000
544

652,465

699,544,445

725,593,502,435

742,528,544,480,429

753,653,516,616,466,426
762,672,601,544,497,457,
423

768,687,622,568,522,484,
450,421

733,699,639,588,544,506,
474,445,420

777,710,653,604,563,526,
495,466,441,418
408,816

816,544,408

816,612,490,408

816,652,544,466,408

816,680,583,510,453,408

816,699,612,544,490,445,
408

816,714,634,571,519,476,
439,408

816,725,653,593,544,502,
466,435,408

816,734,668,612,565,525,
490,459,432,408

816,741,679,627,582,543,
509,479,453,429,408
                                 18

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3.4     Fluorescence Not Significant

        Fluorescence is the absorption  of light  at  a  wavelength
        appropriate to the structure of the  absorbing substance
        with prompt re-emission at a longer  wavelength.   Some
        components of petroleum, notably aromatic and other  ring
        species, exhibit fluorescence in the UV  and short visible.
        As a generality, absorbtion is  in the 200 to  400  nm  range,
        with re-emission in roughly the 350  to 450  nm range.

        Compared with the interference  effects,  the contribution  of
        fluorescence to the visual appearance is negligible  be-
        cause of the relatively small fraction of oil components
        affected, the low intensity of  re-emitted light,  and the
        low sensitivity of the eye in this spectral region.

        It is possible that fluorescence may contribute to (but
        not dominate) the luster of the "silvery sheen" effect.
        Fluorescence may also contribute to  photographic  re-
        cording of a thin film out-of-doors  because the photo-
        graphic emulsion has higher sensitivity  to  this spectral
        region than has the human eye.
                             19

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                      4.   EXPERIMENTAL

4.1.     General

4.1.1.  Preparing and Photographing Laboratory  Oil  Films

        The two main aspects of laboratory experimental procedure
        were physical and photographic.   Physical  procedure  in-
        cluded the equipment and techniques used to prepare  the
        oil films in small trays in the  laboratory; photographic
        procedure included equipment and lighting for producing
        the photographic record.  Although both procedures  are
        basically simple, some difficulties were encountered in
        the physical procedure.  A sufficiently detailed  account
        is given so that others who may  wish to perform similar
        or related experiments will be able to  proceed with  the
        fewest possible problems.

4.1.2.  Other Observations

        Besides photographing oil films  in the  laboratory,  a
        variety of observations were made in the laboratory
        and out-of-doors, but were not usually  photographed.
        These were done to guide and interpret  the laboratory
        procedures,  to establish the correspondence of labora-
        tory and non-laboratory effects, and to generalize
        and order  the  results.  These observations included:

         (a)   An extensive series  of small-pan  observations
              in the laboratory to verify the similarity  of
              effects produced by different oils on dis-
              tilled and sea water.

          (b)  Daily  observation of  a weathered oil-on-water
              film in  a 4  x 6  foot  tray, out of doors, for
              several  weeks.   The  effect of  viewing angle
              and  outdoor  illumination  --  sky  and  cloud  con-
              ditions, intensity  of light,  sun  angle  --  were
              observed.

          (c)  A number of  out-of-doors  observations of small-
              pan  oil  films.   These films  were  identified!
              with those  formed in the  laboratory.  These es-
              tablished the identity of results as seen  and
              photographed with laboratory  lighting and  as
                               21

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             seen under ideal  outdoor lighting.   For  example,
             the greater brilliance  and  intensity of  irides-
             cence illuminated by white  clouds  (ideal)  was
             clearly evident when compared  with  illumination
             by clear blue sky.

        (d)  Occasional visits to nearby oil  spills.   Some
             photographs of these observations  are included
             to illustrate certain points.

4.2     Physical Procedure

        The basic setup was simple.   For each film formed, a  tray
        approximately 9 x 12 inches  was  lined with clear plastic,
        a liter of the desired water was added and allowed to  calm,
        then a measured volume of oil was expelled from a syringe
        onto the water surface.

4.2.1   Plastic Liner

        The thin, clear plastic film liner  served two purposes.
        First, it could be thrown away after  one use, and a fresh
        liner could be used for the  next oil  film. This precluded
        the need for scrupulous  cleaning of the  pan between succes-
        sive films.  Perhaps more important,  it  provided a container
        with reproducible surface properties  and avoided possible
        effects of variation in tray cleaning.   The liner was  care-
        fully handled to avoid contact with the  hands or other source
        of contamination.  To smooth the sheet into the pan,  fresh
        Kim-Wipes (lintless paper towels) were used.

        Second, the clear liner made it possible to vary the  back-
        ground brightness when white, grey  or black paper was  in-
        serted between the liner and the tray bottom  (see Section
        4.2.2.6, Background).

        Some plastic sheet materials strongly inhibited the spread-
        ing of oil.  A&P Clear Freezer Wrap was  satisfactory  from
        this standpoint.  One roll of polyethylene gave good  results.
        Other rolls (different sources)  inhibited spreading.

4.2.2   Measurement of Film Thickness

        If a known volume of oil spreads uniformly to cover a  known
        area, then the film thickness can be  computed.
                 .     volume
                 t ~
                             22

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If volume is expressed in microli
if area is expressed in square me
the oil film thickness in nanomet
         micron) is:
                  t(nm) =
                                         iters  (1  yl  =  10"   cm )  and
                                        meters  (1  m2  =  104  cm2),  then
                                   nanometers  (1  nm = 10-9m =  1Q-3
                                               (7)
                           m
4.2.2.1   Water Surface Area

         Area was deduced by measuring the depth of a known volume of
         water (1 +_ .01 liters) in the tray.  Corrections were applied
         to compensate for the sloping sides and rounded bottom edges
         of the pan.  A check was made by measuring pan dimensions at
         the water line, correcting for rounded corners.

         The two determinations checked within 5%.  Allowing for the
         fact that the plastic liner did not completely follow the
         tray contour, we estimated the total uncertainty in area at
         10%.  The surface area so determined was:

                  A = 0.068 +_ 0.0034 m2

         For convenience in computing nominal film thickness, a nominal
         area was used:
                  A = 1/15 m2  =  0.067 m2
 4.2.2.2  Oil Volume
         A Hamilton microliter syringe (25 yl capacity, 1/2 yl gradua-
         tions) was used to meter oil volumes up to 20 yl.  For larger
         volumes, up to 200 yl (0.2 ml), a normal 1 ml syringe, gradu-
         ated in 0.01 ml, was used.

         If the syringe was in continuous use with the same oil, it was
         not cleaned between successive uses.  At the end of continuous
         use, or when changing oil, the syringe was flushed several
         times with carbon tetrachloride, after which the plunger was
         removed and rinsed with acetone.  The barrel was attached to
         a vacuum line, acetone was drawn through by vacuum to rinse,
         and the barrel was then dried with air aspirated by the vacu-
         um.  A clean syringe was first flushed five or six times with
         the oil to be used.
         The estimated overall accuracy of
         0.5 yl for the 25 yl syringe, and
                                  delivered oil volume ;s +_
                                  +  10 yl for the 1 ml syrinqe
                               23

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         This takes into consideration inaccuracies in scale reading,
         dribbling, and small  droplets that occasionally remained at-
         tached to the delivery end of the needle.

4.2.2.3  Accuracy of Film Thickness

         In nearly all cases,  the oil  spread over the entire water
         surface, and thus the nominal film thickness was 15 nm per
         microliter of oil.  Uncertainties in oil film thickness
         owing to the oil volume measurement are:

         Nominal Oil Volume    Nominal Oil Thickness,    Uncertainty,
                                    nanometers           nanometers


               1-20               15  -  300             +  7.5

              50 - 200             750  - 3000             + 15.7

         Additional uncertainty owed to surface area is: +_  5%.

         Resulting total uncertainty is as follows:

         Nominal Oil Thickness     Total Absolute Error     Percent of
nanometers
15
38
300
750
300
nanometers
+ 8.3
+. 9.4
+. 22.5
+. 187.5
+ 300.0
Nominal
+ 55
+ 20.5
± 7-5
+ 15.7
+ 10.0
4.2.2.4  Oils Used
         The need to pick up and deliver oil through the fine needle
         of a microliter syringe limited the choice to low viscosity
         types.  Those used were:

                  Mediterranean Crudes (dark brown)
                       Light Arabian
                       Agha Jari (Iranian)

                  Domestic Crude (Dark brown)
                       South Louisiana
                              24

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                  Distillate (Clear with light yellow
                              to red tint)
                       No.  2 Fuel  Oil

         Samples were withdrawn from full  or nearly full  drums
         and placed in polyethylene bottles.  Small  ullage  in
         the nearly full  drums implied they had never been  or
         were infrequently  opened.  Thus,  there had been  negli-
         gible loss of volatile components, and the samples
         were representative of the parent stock.

4.2.2.5  Water Used

         Distilled water (with and without background dye:  see
         Section 4.2.2.6) and visually clean, coastal sea water
         (salinity 26 ppt)  were used as substrates for several
         hundred oil films.  Since the spreading of the test
         oils was apparently identical on  all these waters,
         no further characterization of water was  made.

         Because of this identity in behavior, distilled  water,
         with or without dye, was used for the films photographed
         for this report.  The properties  of distilled water are
         less variable then those of tap,  river, estuarian, or  sea
         water.  The advantage is clear should there be future
         need to compare results obtained  at different laboratories
         or at different times.

4.2.2.6  Background Brightness

         Background brightness was varied to represent a  range  of
         real life bottom and water conditions.  In shallow, clear
         water over a light sand bottom, most of the light incident
         on the water surface penetrates to the bottom and is  re-
         flected back through the water surface with little absorp-
         tion.  At the other extreme, the water is so deep, or  the
         bottom so dark, that almost all the incident light is  ab-
         sorbed below the water surface and the water looks almost
         black.  The former gives a high background brightness;  the
         latter, a low background brightness.

         In a shallow pan with clear water, the high brightness
         situation was simulated by white paper (or white tray  bot-
         tom) under the plastic liner.  Black paper under the liner
         gave a medium high, rather than a low, background brightness
         owing to reflection from the surface of the plastic liner
         itself.
                              25

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        Low background  brightness was obtained by dyeing the
        water.   Sheaffer Permanent  Jet  Black  ink  (2% ml per liter)
        gave an  intense dark  color  that completely obscured a
        white tray  bottom.  The  ink did not inhibit oil spreading
        on distilled water; it did  inhibit spreading on sea water.
        On undyed water, however, representing true field  condi-
        tions,  oil  spreading  on  distilled water and sea water are
        equivalent  (Section 5.2).   For  experimental reproducibility,
        distilled water is preferable  (Section 4.2.2.5).   Thus
        ink-dyed distilled water was used to  simulate  a low back-
        ground brightness.

        Other dyes  tried were unsatisfactory.  Liquid  food coloring
        gave excellent  opacity and  did  not inhibit spreading on
        either distilled or sea  water,  but gave unnatural  colors.
        RIT fabric  dye  gave excellent  opacity and good color, but
        strongly inhibited spreading on both  distilled and sea water.
4.2.2.7 Surface State
        Oil  placed on the calm water surface  spread to  form a
        static film of nearly constant thickness  and of nearly
        uniform color.  To simulate the more  realistic  condi-
        tions of an active water surface,  two things were  done.

        (a)   By blowing onto the film in the  middle of  the
             tray, a hole was formed in the film, exposing
             a circular patch of bare water.   Around the
             bare water, the oil film tapered in  thickness
             from zero at the edge to the full thickness
             away from the edge.

        (b)   The tray, containing the water and oil film,
             was agitated by a laboratory shaker  table.
             Horizontal orbital motion of the shaker table
             generated waves about %-inch to  1-inch trough-
             to-crest.

        Besides providing glittering reflections  from the  irregular
        surface, the waves produced variations in film thickness.
        The film is compressed at the crest and stretched  thin  in
        the trough, similar to the effects of sound propagation  in
        a fluid where the medium is compressed at the node and  rari-
        fied at the antinode.
                             26

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         The sequence of operations  was:

            (a)  Observe static film  as  laid on  calm water

            (b)  Observe film with hole  blown in it

            (c)  After calming, start shaker table and
                observe film

            (d)  Observe film after stopping shaker  table and
                while allowing surface  to calm.

4.3      Photographic Procedure

         No special photographic equipment was  needed except
         supplementary devices for critical focusing at object:
         image ratios of about 6:1.   The  lighting was arranged
         to give optimum conditions  --  a  bright white uniform
         source with an area large enough so that  its image,
         reflected by the water surface into the lens, would
         substantially fill the negative  area.   This simulated
         illumination by a uniform white  sky.

         A schematic, Figure 4, shows the general  arrangement used.
         Details are in the following sections.

4.3.1    Camera and Objective

         A 35 mm Leica Ilib body was mounted on the rear plate of
         a Leica sliding focusing attachment.  A 9-cm Leica Elmar
         f:4 objective with lens shade  was mounted  on the  front
         plate.  The sliding focusing attachment provided  ground
         glass viewing and critical  focusing with  a 10X magnifier.
         The attachment added 11.8 mm to  the normal lens flange to
         focal plane distance, acting as  an extension tube or bel-
         lows for closer-than-normal focusing.   The 9-cm focal
         length, compared to the normal 5-cm objective, increased the
         object-lens distance to about 60 cm (24 in.) for more con-
         venient working at the reduction ratio of 6 or 7 to 1.

4.3.2    Lighting

         A  No. 2 photoflood lamp  (color temperature 3400 K) or a
         500 watt  3200K lamp  (color temperature 3200  K) in a 12-inch
         aluminum  reflector with diffusing  screen provided good il-
         lumination.   For maximum light and to fill the negative
         area with  its image, the diffuser was close to the water
                              27

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Figure 4.   Arrangement for photography oil  film in tray.
                        28

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        surface, about 12 inches.   The  "earth  from space"  effect
        in the photographs clearly illustrates  the lamp  placement;
        the circular light source  covers  the  height of the photo-
        graph, but does not quite  cover the  full  width of  the
        format.

        Illumination at the water  surface varied  from about 4000
        lumen/ft^at the center to  about 3000  at the edges. In-
        tensity at the center was  about half  that of a normal sun-
        lit outdoor scene; variation over the  field represented
        a one-half stop exposure variation.

4.3.3.1 Film and Exposure

        For the laboratory photographs, High  Speed Ektachrome
        (ASA 125 with 3200K lamp)  was used at  first; later on,
        Kodachrome II Professional, Type A (ASA 40 with  3400K
        lamp) was adopted.  The higher  contrast and greater ap-
        parent saturation gave transparencies  that seemed  closer
        to the visual impression.   Most of the  out-of-door photo-
        graphs were on High Speed  Ektachrome,  daylight type.

        Exposure for the tray photographs, as  indicated  by an inci-
        dent light exposure meter, was  1/100  sec. at a marked aper-
        ture of F:6.3.  Effective  aperture (correction for close-up
        focusing) was f:8.

4.3.3.2 Processing

        The exposed film was given to a local  dealer for normal
        processing by Kodak.  There were no  special arrangements.
        Results were satisfactory.  Slight variations in overall
        tone were found (slight green cast vs.  slight blue cast)
        among rolls processed at different times, but these dif-
        ferences were insignificant for the  purpose at hand.
                             29

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                          5.  RESULTS
5.1      General
         This section presents the results obtained from laboratory
         observations and includes photographs of oil  films formed
         in small trays.  Additional  photographs of oil  films taken
         in the field are included to show the correspondence be-
         tween effects in the laboratory and in the field.

5.2      Spreading on Different Waters

         The degree of spreading between films of Arabian and No. 2
         Fuel Oil on sea water and distilled water, in 1/15 m2 trays,
         was compared (Table IV).

         Although in the thinnest films there are differences in
         spreading tendency between different oils, the spread of
         each oil is nearly identical for sea water and distilled
         water.  This fact allowed the use of dyed distilled water
         as a controlled substrate for experimental purposes.

         Photographs of water-to-water comparisons are not included
         in this report.

5.3      Photographs of Laboratory Oil Films

         In the color photographs, the oil films range from 15 to
         3000 nm (nominal) thick  (Figs. 5 thru 21).  Films of Light
         Arabian represent the entire range.  Films of South Louisi-
         ana represent the range 15 to 300 nm (nominal).  Agha Jari
         and No. 2 Fuel Oil represent two thicknesses each:  15 and
         150 nm.  This series used dyed water for a dark background
         and shows nearly pure optical effects from the surface film
         alone, undegraded by extraneous light from glare or back-
         ground.

         The four photographs in Figure 22 show the effects of back-
         ground brightness on visibility.

         Figures 5 through 21 each have three or four different photo-
         graphs of the same oil film  (one film per figure), with each
         photograph representing a different surface state.  The arrange-
         ment of photographs is a consistent vertical sequence from top
         to bottom:

                        Film as formed
                        Hole blown in film
                        Shaker table  in operation
                        At rest after shaker table

                              31

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                           TABLE IV

     COMPARISON OF OIL SPREAD ON SEA WATER AND DISTILLED WATER
             Oil/Water
                          Fraction of Surface Covered
                         	oil ,  yl*	
Light Arabian
 Sea Water, undyed
 Distilled water, undyed
 Distilled water, dyed
                                    1
                                                   10
0.8
0.8
0.8
1.0
0.9
1.0
1.0
1.0
1.0
No. 2 Fuel
 Sea water
 Distilled
Oil
 undyed
water, dyed
0.5
0.5
0.8
            *Film thickness = ylx!5 for coverage - 1.0
0.9
1.0
                             32

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         If one of the spaces within the sequence  is  blank,  there
         is no photograph of that particular surface  state.

5.3.1    Effect of Film Thickness

         Figures 5 through 12 record the changing  appearance of
         Light Arabian oil films as thickness increases  from 15 nm
         to 3000 nm.  The main points are:

         (a)  Films less than about 150 nm show no color,  but
              are brighter when compared with bare water because
              of the higher reflectivity of the oil  film.   There
              is no color for these thicknesses because  inter-
              ference occurs only at wavelengths shorter than
              those in the visible spectrum.

         (b)  At about 150 nm, a bronze tint is seen  in  the
              calm film, as laid.  Surface activity introduces
              an additional purple tint owing to local thick-
              ening.

         (c)  From 300 to 750 nm, strong color and brilliant
              rainbow coloring  (iridescence) prevails, the
              latter when surface activity causes  thickness
              variations.

         (d)  At 1500 nm, brilliance is lost from the rainbow,
              and at 3000 nm, considerable dulling is evident.
              As film thickness increases beyond this, irides-
              cence will disappear completely except where there
              is pronounced local thinning, and the film will
              assume the color of the bulk oil.

5.3.2    Effect of Oil Type

         Figures 13 through 17 similarly show the appearance of
         South Louisiana films from 15 nm to 300 nm.   Once nearly
         complete coverage is obtained at 38 nm (2.5 ul),  the ap-
         pearance of these films is nearly identical  with  their
         Arabian counterparts.  As a further comparison, 150 nm
         films of Agha Jari and No. 2 Fuel Oil  (Figs. 19 and
         21) are similar in appearance to the Arabian and South
         Louisiana.

         Differences are found  in the thinnest  films, formed by
         1 yl of oil.  Arabian and Agha Jari spread uniformly to
         give thin films, about 15 nm thick, with reflectivity
         somewhat higher than that of the water.

                               33

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         The  South  Louisiana  and  No.  2  Fuel  Oil  (1 yl)  (Figures
         13 and 18) give  incomplete films with a  Swiss  cheese ap-
         pearance of decidedly  higher reflectivity than  do the
         other two  oils.   Note, however, that the greater reflec-
         tivity is  associated with a  lower  surface coverage  and,
         thus, a film thickness greather than that obtained  with full
         coverage.   In fact,  these films of low  coverage do  indeed
         appear similar in brightness to the 38  or 75 nm films of
         Arabian.

         Thus, even when  spreading characteristics of an oil do
         vary, owing to type, composition,  or other  factors, the
         appearance of the film,  in terms of brightness  or color,
         is appropriate to the  actual local  thickness,  in accord
         with theory.

5.3.3    Effect of  Surface State

5.3.3.1   Blown Holes (Films with  tapered edges)

         The  main purpose in  exposing the bare water was to  demon-
         strate that even very  thin films,  15 and 38 nm, displayed
         a reflectivity greater than  water.  In  fact, comparing
         these photographs with those of the fully spread films
         (Arabian and Agha Jari,  Figs.  6 and 20), it is evident  that
         the  detection, or visibility,  of thin  colorless films de-
         pends on the ability to  make such  a comparision.  The eye
         is unable  to make quantitative estimates of brightness  with-
         out  comparing an unknown to  a  reference or  standard.  This
         is a significant aspect  of visibility  and detectability.

         With films thick enough  to show iridescence,  300 nm and
         thicker, the tapered edges show the sequence of the inter-
         ference colors as thickness  increases.   This sequence is
         bronze, purple,  blue and green; as the  film becomes thicker,
         the  sequence repeats (Figures  10,  11,  and 12.).

         From the discussion  of theory  and  the  application of equa-
         tion 3 (Section 3),  one  would  expect  this sequence  to re-
         peat for approximately each  300 nm increment of thickness.
         Counting sets of bands in  the  300  to  3000 nm films  shows
         this to be true, allowing  for  an occasional extra band  due
         to ripples.  In the  1500 and 3000  nm  films, one can also
         see that,  with an increase  in  thickness and in the  number
         of wavelengths subject to  interference  (Table  III)  some
         colors drop out of the sequence and the intensity or
         purity of color degrades.
                               34

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         Figure 12b is an enlargement showing  the  3000  nm film in
         greater deail.  The changing appearance with each 300 nm
         increment, although sometimes subtle, can be seen.   The
         major changes reflect the groupings  in Table  I;  the  first
         two sets of bands are bright, the next three degrade to
         brick-red and turquoise,  and ultimately color  is lost and
         the bands are light-dark.  This one  photograph in itself
         summarizes the thickness-appearance  relation.

5.3.3.2  Waves (Shaker Table)

         Where a thin, colorless film covers  the entire field of
         view, (Fig. 5 and 6) waves or chop on the water produce
         a glitter of reflected light spots that make  it hard to
         identify these films.  A difference  in reflectivity  be-
         tween a film and the adjacent bare water  can  be obscured
         by the brightness differences in the glitter  pattern.

         The relative reluctance of South Louisiana and No.  2 Fuel
         Oil to spread tends to be preserved  under wave conditions.
         Because of the incomplete coverage,  bare  water can  be seen
         and the colorless film can be discerned.   The  lower  spreading
         tendency affects the films up to 150 nm,  and  the local thick-
         ening gives the appearance of a nominally thicker film.

         The wave condition also illustrates  well  the  progressive
         dulling of iridescence as film thickness  increases  beyond
         1000 nm.

5.3.3.3  Calm After Waves

         There frequently occurs, in actuality, the condition of calm
         after waves; during the lifetime of a film it  can be exposed
         to changing weather and sea conditions.  Three effects of
         wave actions were noted in the laboratory when the surface
         came to rest after wave making on the shaker  table.

         (a)  The tendency of wave action to  work  a compressed deposit
         into a larger, thinner film is illustrated in  Figs.  13 and
         18, where the initial "Swiss cheese" films of South  Louisiana
         and No. 2 Fuel Oil have been worked into  a more continuous
         film.  This  "working out" was observed in experiments on  the
         open sea  (Ref. 8).

         (b)  A weathering effect is quite noticeable  with the 150  nm
         films.  Loss from the Arabian film,  Fig.  8, has been enough to
         decrease the apparent film thickness to about  75 nm as evidenced
         by the change from the original yellow color  to a colorless


                               35

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         reflecting  film.  The  South  Louisiana film, Fig. 16
         does  not  show  this  effect markedly.  This may be be-
         cause of  a  difference  in duration of exposure to wave
         conditions, or it may  represent a true difference owed
         to  differences in solubility and volatility of  light
         components. The Agha  Jari film, Fig. 21, shows an
         intermediate effect.   The No.  2 Fuel Oil film shows a
         notably different phenomenon.  The  loss of components
         from  the  film, and  perhaps their partial solution in the
         water, changed the  interfacial properties so as to in-
         hibit spreading.  Examination  of the original color
         slide shows that the deposit had become an array of
         small discrete flecks  of oil  separated by apparently
         open  water  that gives  the film a grainy appearance.

         In  the paragraph above, material loss from the  film was
         attributed  to  volatilization and solubility.  A third
         possibility is that some of  the oil became stuck to the
         tray  liner  during agitation; this was, in fact, observed
         with  thicker films. The behavior of No. 2 Fuel Oil, how-
         ever, substantiates that even though material loss via
         edge-sticking  may have occurred, it was not the sole
         mechanism.   The change in spreading properties  requires
         a selective loss of constituents; this indicates that
         volatility  and solubility are involved, since these pro-
         cesses are  selective with respect to molecular  weight and
         molecular structure.

         (c)  A third result of wave  action  noticed especially with
         the thicker film was the creation of apparently permanent
         or long-lasting variations in film  thickness that give  rise
         to color  variation  and streaking in the quiescent film.

5.3.3.4  Background  Brightness

         Figures  22a, 22b, and  22c show 15 nm,  105 nm, and 300 nm
         films of  Arabian oil.   In each case, one half the tray  con-
         tributes  a  high background brightness  and the other half,
         a medium  to medium-high  background  brightness.  These films
         were  gently disturbed  to develop local variations in thick-
         ness.  For  comparison, Figure 22d shows a 300 nm film over
         a dark background  (dyed  water), at  rest, after  wave-making
         on the shaker  table.

         The increased  visibility and brilliance owed to the low
         background  brightness  is evident.   Also evident in the
         trays having both  bright and medium backgrounds is the
         apparent  discontinuity at the background boundary, even
         though the  oil film is continuous over both  backgrounds.


                              36

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         Because only a  fraction  of the  incident  light  is  subject
         to interference,  the  inherent visual  effect  is  readily
         diluted by extraneous light.    If  the incident  light  is
         nearly normal to  the  surface, most of the  light will
         penetrate.  Simple measurements  with  a photographic ex-
         posure meter indicated that about  2%  to  5% of  the incident
         light is reflected by a  bare water surface,  and about 5%
         to 10% by a surface with an oil  film. This  is  as predicted
         by theory.  Of  the 90% that penetrates,  some will  be  ab-
         sorbed in the water column, some absorbed  by the  bottom,  and
         some reflected  by the bottom.   After  reflection,  and  after
         further attenuation,  this light  returns  through the oil film
         to the observer.   The amount of  returned light  depends on
         the absorbtivity  of the  water and  the bottom and  on sus-
         pended particles  that can reflect  light  directly.  This
         returned light, added to the interference  effects, dilutes
         the color effects and reduces the  interference  effects, the
         contrast, and the relative brightness between  oil-covered
         areas and bare  water  areas.

         In its extreme, a bright background can  overwhelm the opti-
         cal effects of  an oil film as shown in the photographs.
         The effect is similar to projecting a slide  or  movie  in a
         darkened room and then turning  on  the house  lights.

5.4      Field Observations

         Our own and the published results  of  other observers  substan-
         tiate the effects observed in the  laboratory and  add  further
         information that  expands upon the  laboratory results.

5.4.1     The Appearance  of Oil Films

         Comparison of relationships between film thickness and visual
         appearance shows  excellent agreement  among our laboratory
         photographs, the  API  data (Table I) and  the  General Re-
         search Corporation data  (Figure  2).

         Figures 23, 24  and 25 are of oil films formed  by  a spill  of
         No. 2 Diesel Fuel on  fresh water,  the Raritan  River.  Figure
         23, a view from  a bridge across the  river, shows  a colorless
         oil film  along the right bank;   Figure 24,  a thicker irides-
         cent  film; and Figure 25,  a film with a circle of bare water
         created by  tossing a stone.  The  effect is  similar to blow-
         ing a hole  in  the laboratory film, and  demonstrates  unequi-
         vocally the presence of the film.

          Figure 26 shows  a film of No.  2 Fuel Oil  from a  spill  on es-
          tuarian  water,  the  Arthur Kill.  The low background  brightness


                               37

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         and overcast sky produced clear color  effects  similar  to
         those in the laboratory.

5.4.2    Viewing Angle and Viewpoint

         Figure 27a,  colorless  films of an  unknown  oil  on  estuarian
         water shows  how a high viewing angle  (bottom of photograph)
         gives better visibility.   As distance  from the viewer  be-
         comes greater, and thus the viewing angle  departs more from
         the vertical, the oil  film becomes less  visible and finally
         is obscured  by the increased glare from  the surface.   A
         similar effect is apparent in Figure  27b,  a brightly iri-
         descent film of No. 2  Fuel Oil (which  can  be seen better  in
         Figure 26, taken at a  high viewing angle).

         Figure 28 shows the results of a 50 gallon per minute  sea
         water discharge (Raritan Bay) containing 100 ppm  South Loui-
         siana Crude.  In Figure 28a, taken from  the vessel and show-
         ing the discharge, it  is hard, if not  impossible, to see  the
         resulting oil film because of the poor viewing angle.   On
         the other hand, Figure 28b, taken from a helicopter at 100  ft.
         altitude, clearly reveals a film described by  the observer
         as "sheen, non-metallic, no color".

         Figure 29 illustrates  a reversed situation. The  discharge
         here is 25 gallons per minute and contains 10  ppm South Loui-
         siana.  The  oil discharge rate was too low to  yield a  large
         continuous film, and formed instead the  discontinuous  streaks
         and patches  of thin colorless film.  From the  vessel,  these
         were visible; from the helicopter, however, there was  no  vis-
         ible result  of the discharge.  In this case, a close viewpoint
         permitted the detail to be seen, whereas at a  distant view-
         point, this  detail could not visually or photographically be
         resolved.

5.4.3    Illumination, Background Brightness and  Surface States

         These factors are considered together because  it  is sometimes
         hard to separate them in a real situation.

         References 5 and 6 emphasize that an  overcast  sky gives better
         visibility than a blue sky with sun,  and our experience is
         certainly in accord.  Interestingly,  with an overcast sky,
         illumination need not be intense.   Figure 30 is a photograph
         of an iridescent patch of oil on a blacktop driveway on a
         rainy day.  Light intensity from the  overcast  sky was  450
         lumens/ft^,  about 1/60 of the intensity  on a sunny day.  The
         primary factors are the overcast sky,  giving a broad uniform
         light source, and the dark background.


                              38

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In sunlight, best results are obtained when the area
observed is shaded from direct sunlight and illuminated
only by light from the sky.  Figure 31 is a photograph  of
a colorless film viewed from our vessel, whose shadow can
be observed in the foreground.  In the shadow, the oil  film
is readily discerned.  In the sunlit upper right portion,
the film is not detectable owing to an adverse combination
of illumination, background brightness, and surface state.

If sunlight illumination cannot be avoided, the sun should
generally be at the observers back for best visibility, or
at least not more than 90 degrees to either right or  left.
See also Reference 6.
                     39

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  Calm,  as  formed
  Hole  blown
  Waves  (shaker  table)
Figure 5.   Light Arabian Crude (1  yl).   Thickness is 15 nm.



                            41

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 Calm, as formed
  Hole  blown
  Waves  (shaker table)
Figure 6.  Light Arabian Crude (2.5 yl).   Thickness  is  38 nm.
                             43

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  Calm,  as  formed
  Hole  blown
  Waves (shaker table)
Figure 7.   Light Arabian Crude (5 yl).   Thickness is 75 nm.
                            45

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   Calm,  as  formed
   Hole  blown
   Waves (shaker table)
   Calm after waves
Figure 8.   Light Arabian Crude (10 yl).   Thickness  is  150 nm.
                             47

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   Calm,  as  formed
   Hole blown
   Waves (shaker table)
   Calm after waves
Figure 9.   Light Arabian Crude  (20 yl).   Thickness  is  300  nm.
                            49

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   Calm, as formed
    Hole  blown
    Waves  (shaker  table)
    Calm after waves
Figure 10.   Light Arabian Crude (50 yl).   Thickness  is  750  nm.
                              51

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    Calm, as formed
    Hole blown
    Waves (shaker table)
    Calm after waves
Figure 11.   Light Arabian Crude (100 yl).   Thickness  is  1500 nm.
                              53

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    Calm,  as  formed
    Hole  blown
    Waves  (shaker table)
    Calm after waves
Figure 12a.   Light Arabian Crude (200 yl).   Thickness  is  3000  nm.
                              55

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    Figure 12b.   Light Arabian  Crude.
Enlarged view of 3000 nm film (Figure  12a)
                    57

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Calm, as formed
 Waves  (shaker table)
 Calm after waves
        Figure 13.   South Louisiana Crude (1  yl),
      Thickness would be 15 nm for full  coverage,

                           59

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    Calm,  as  formed
    Hole blown
    Waves  (shaker table)
    Calm after waves
Figure 14.   South Louisiana Crude (2.5  yl).   Thickness  is  38  nm.
                              61

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  Calm,  as formed
  Hole blown
  Waves (shaker table)
  Calm after waves
Figure 15.   South Louisiana Crude  (5  yl).   Thickness  is 75 nm.
                            63

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  Calm,  as  formed
                                     '
  Hole blown
  Waves (shaker table)
  Calm after waves
Figure 16.   South Louisiana  Crude  (10  yl).  Thickness is 150 nm.
                            65

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   Calm,  as  formed
   Hole  blown
   Waves (shaker table)
   Calm after waves
Figure 17.   South Louisiana  Crude  (20  yl).   Thickness is 300 nm.
                             67

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Calm, as formed
Waves  (shaker table)
Calm after waves
           Figure  18.   No.  2  Fuel  Oil  (1 yl).
     Thickness would  be  15 nm with  full coverage,

                           69

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Calm, as formed
Hole blown
Waves (shaker table)
Calm after waves
 Figure 19.   No.  2 Fuel  Oil  (10 pi).   Thickness  is  150 nm.
                          71

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 Calm,  as  formed
 Hole blown
 Waves (shaker table)
 Calm after waves
Figure 20.   Agha Jari  Crude (1  yl).   Thickness  is  15  nm.
                           73

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Calm, as formed
Hole blown
Waves (shaker table)
Calm after waves
 Figure 21.   Agha Jari  Crude (10 yl).   Thickness  is  150  nm.
                          75

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a.  1  yl  15 nm (if full  coverage)
b.  7 yl  105 nm (if full coverage)
c.  22 yl  330 nm
d.  20 yl  300 nm
      Figure 22.  Effect of Background Brightness of Visibility.
   (a),(b),(c) Bright and Medium Background; (d) Dark Background.
                            77

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                                                              ;*•
            Figure 23.

No. 2 Diesel Fuel on Raritan River,

            Figure 24.

No. 2 Diesel Fuel on Raritan River
          (iridescence).
            Figure 25.

        No. 2 Diesel Fuel ,
     with bare water exposed.
            Figure 26.

        No. 2 Fuel Oil on
    Arthur Kill  (iridescence)
                          79

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                  a.   Unknown oil  on Arthur Kill
                 b.  No. 2 Fuel Oil on Arthur Kill
                         Figure 27.
Diminishing visibility as viewing angle departs from vertical

                             81

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             Figure 28.

    Visibility of 50 gpm, 100 ppm
    oil-water discharge, from the
  surface (a) and from the air (b).
             Figure 29.

    Visibility of 25 gpm, 10 ppm
oil-water discharge, from the surface
     (a) and from the air (b).
                              83

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                   Figure 30.
Undimini shed visibility of driveway oil  film in
             low intensity light.
                   Figure 31.
  Reduced visibility in direct sunlight compared
            with visibility in shadow.
                     85

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                        6.   DISCUSSION


6.1      Inherent Optical  Properties and Visibility

         This investigation provides direct answers to the questions
         that prompted it:

         (a)  Thin oil films have defnite optical  character-
              istics that produce inherent visual  effects
              with an orderly relationship between film
              thickness and appearance.  This relationship
              is independent of oil  type.  The most evident
              aspect of appearance is color, with  orderly
              variations in the number of colors present
              and in their purity or intensity.

         (b)  Visibility is not inherent or constant, but  is
              the product of the inherent visible  effects  and
              of the various factors external to the film  that
              can degrade or obscure the inherent  effects.
              These factors include sky conditions, sun posi-
              tion, state of the water surface, character  of
              underlying water and bottom, viewing angle,  and
              distance between observer and film.   Light in-
              tensity does not appear as a strong factor.

6.2      Results are General, not Unique

         The laboratory photographs are an internally consistent set
         of data that shows the inherent appearance of oil films and
         variations in visibility that result from viewing conditions.
         We must now establish that these results  and the  conclusions
         based upon them are completely general.  Correspondence be-
         tween laboratory results and observations in actual situations
         is just one aspect of the generality sought.

         One way to establish generality is by comparing enough obser-
         vations to show that the same effects are found in a wide
         range of circumstances.

         The appearance-thickness relationship demonstrated in our
         laboratory photographs corresponds closely if not identically
         with those of the American Petroleum  Institute and the General
         Research Corporation.  Taken as a whole, these three sets of
         data include laboratory and field observations, a minimum
         of five and probably six or more types of oil, a  minimum of
         three different observers, a minimum of two different water
         types, and an unknown number of different viewing conditions.
         The net results, with regard to the thickness relationship,
                              87

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is that inherent appearance is a function  of thickness
and is not a function of oil  type or of water type.   A
further implication is that our laboratory photographs
show the same visual  effect as do oil  films in the field.
This is further supported by our photographs of real
fi1ms.

The effect of ambient or viewing conditions upon visi-
bility also shows agreement between our laboratory re-
sults and field observations.  Photographs in this report
of real situations bear out the trends established in the
laboratory, especially with respect to background (optical
character of water and bottom) and surface condition.  Com-
ments of the Coast Guard and other observers upon sky con-
dition and sun position are the same as ours.  During the
course of studying oily water discharges (to be reported
separately), extensive observations were made from the
air.  These confirmed the trend indicated in the labora-
tory that water chop and high background brightness (be-
cause of light return from the particles in turbid water)
lessen visibility, especially for colorless films.

When comparing a range of observations, we find agreement
in all respects and an absence of contradiction and con-
clude that our photographic data and the conclusions  of-
fered can be applied to all instances of thin oil films
on water.

A second approach to assess generality is to compare  re-
sults with theory.  Two optical phenomena are involved:
the relative reflectivites of oil and water surfaces, and
the interference between light reflected from the top and
the bottom oil film surfaces.

Reflectivities of 2% to 5% for water and 4% to 10% for oil
are obtained both from theoretical calculation and measure-
ment.  Only that small fraction of the incident light
reflected by the oil film is involved in creating the
optical effects of brightness and color that we see.   With
only 10% of the light being  "processed" by the film before
reaching the eye, it follows that, if even a small fraction
of the "unprocessed" light is returned to the eye, the ef-
fects resulting from the film will be diluted and weakened.
The observed effects of background brightness and of view-
ing angle  (glare) upon visibility, even to the point of
making a film non-visible, are in complete accord with this
physical picture.
                     88

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         The  photographs  of laboratory  films were made  under ideal
         conditions;  glare  was  eliminated  by the higher viewing angle,
         and  background minimized by  dying the water.   Because of this,
         they show with high purity the inherent visual  effects pro-
         duced by the oil  film  itself.   Comparing the photographs with
         the  effects  predicted  from increasing the  thickness (Equation
         3),  one sees complete  correspondence: the  onset of color
         is at the correct  thickness; the  sequence  in which colors
         appear is correct; the reduction  in the number of colors
         with increasing  thickness is appropriate to the increasing
         number of wavelengths  in interference; the progressive
         dulling colors,  with their eventual disappearance into
         greyness, is as  expected.

         Also apparent from Equation  3  is  the fact  that the visual
         effect of an oil  film  is, for  practical purposes, inde-
         pendent of the type of oil.  Thickness and refractive index
         are  the only film properties that enter the equation.  The
         refractive indexes of  most components of oils  are between
         1.4  to 1.5 and the limits are  1.3 to 1.7.  The maximum
         variance from the  average value 1.5 is 4^13%,  which is neg-
         ligible compared with  the 200:1 ratio of thickness values
         investigated. Once again, the photographs bear this out.

         From the theoretical standpoint,  we see that:

         (a)   The two principles of reflectivity and inter-
              ference adequately explain the quantitative
              as well as  qualitative  appearance and visi-
              bility of oil films less  than 3000 nm thick.

         (b)   No other phenomena need be invoked to explain
              these findings.

         In summary, the  data from this laboratory  and  from other sources
         agree:  our data are adequately explained  by the above physical
         principles; and  these  principles  are fundamental and general.
         Therefore, the effects reported here should apply, and do  apply
         without restriction, to all  thin  oil films on  water.

6.3      Field Application  of Results

         Many of the details developed  can be useful in field observa-
         tions and may be especially  helpful to  inexperienced observers.
         Some aspects are discussed  below.
                              89

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        The thickness-appearance relationship can be used with
        complete confidence to estimate the thickness of an oil
        film.  This, together with an estimate of area, yields an
        estimate of the amount of oil in the film.  For this
        purpose, the relationship listed in Table I is conven-
        ient.  Table I is simple enough to commit to memory.  We
        suggest that thickness in nanometers be used, since the
        surface coverage in milligrams per square meter is nu-
        merically the same as thickness in nanometers.

        If observation conditions do not permit a fine judgment
        of color purity or of film brightness, a simple scale of
        "no color - bright color - dull color" still provides
        useful information on the approximate thickness.

        Conversely, if careful observation is possible, one can
        make up a table, based upon our photographs, that is more
        detailed than Table I (see Section 6.4).

        The series of laboratory photographs has proved useful in
        our laboratory as a direct illustration of actual appear-
        ance that avoids the imprecision of verbal color descrip-
        tion.  They have been useful in indoctrinating new obser-
        vers and in refining the perception of more experienced
        people.  They have been used in training courses given at
        this laboratory for field personnel of Federal and State
        organizations.

        Appreciation of the factors  affecting visibility should
        help the observer evaluate what he sees.  Although  some
        of the factors are not  under his  control  (sky  conditions
         and water  background),  to  some  extent he  may  be  able  to
         select the  most  favorable  viewing position  and angle  or  to
         otherwise  influence  the total  set of conditions  under
         which  he must  operate.

6.4      A Modified  Thickness-Appearance Table

         By using  the  guidance  provided  by theory  and  the  effects
         shown  in  the  photographs,  especially Figure  12b,  one  can
         make more  refined estimates  of  film  thickness.  In  Table  V,
         a set of  colors  is  referred  to  as being  characteristic of
         a given film  thickness; remember  that the range  of colors
         represents  a  small  range  of  thicknesses,  more  or less
         ending at  the  nominal  value  cited.
                              90

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   Appearance
                       TABLE V

SCHEMATIC BASIS FOR THICKNESS-APPEARANCE  RELATIONSHIP

    Thickness Range                            Description
     (nanometers)
Colorless Films
     Up to 150
Onset of Color
     Approx.  150
Pure Rainbow Colors     150 to 900
Dull, Impure Colors     900 to 1500
     Films reflect more light than does water, and look
brighter.  May need adjacent bare water for comparison.
Apparent brightness increases with thickness.  At about
75 nm and thicker, a pearly or metallic luster is
usually apparent.

     First color seen is a warm tone, more bronze than
yellow.
     As film thickens, deep violet or purple appears,
these colors begin the first set of rainbow bands.

     The set of bands around 300 nm are in the sequence:
bronze, purple, blue, green, in order of increasing
thickness.  These colors are pure and intense.
     The set of bands around 600 nm are slightly less
intense than at 300 nm, and have a modified color se-
quence:  yellow, magenta (reddish violet), blue, green.
They are quite pure.

     Main characteristic is reduction in number and
purity of colors.  Colors at 900 nm are a rich terra
cotta (brick red) and turquoise (rather bright blue-
green).  At 1200 nm and 1500 nm these colors are pro-
gressively duller or less pure looking.  These sets of
bands may also contain a trace of white or pale
yellow.

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                                         TABLE V (Continued)
         Appearance
Thickness Range
 (nanometers)
                     Description
      Light and Dark Bands
       with Little Color
 1500 to 3000
     Any color present is merely a tint in  the light and
dark alternating bands.
     At 1800 nm, the contrast between light and dark
bands is strong, but weakens as thickness increases.
     At 3000 nm, it is apparent that interference effects
are weak, and they will  quickly disappear as thickness
increases.
vo
ro

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                     7.   GLOSSARY
cm          centimeters
gm          gram
lumen/ft^   intensity of  illumination, same as foot-
            candle
m           meter
                         _3
mg          milligram, 10   gm
                          _3
ml          milliliter,  10   liter
              -9          -3           °
nm          10   meters,  10    micron, 10 Angstrom units
00                -1-8
A           Angstrom unit, 10  nm or  10   cm
X           wavelength in nm
                                              -4
y           refractive index; also  micron or  10  cm
yl          microliter,  10   liter  or 10~  ml
                         93

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                     8.   REFERENCES
1.   Federal  regulation,  "Part  610  -  Discharge of Oil"  issued
    under Section ll(b)  (3)  of the Federal Water Pollution
    Control  Act, as amended  (84 Stat.  92'  33 U.S.C. 1161),
    and printed in the Federal  Register,  Vol. 55,  No.  177,
    September 11, 1970.

2.   Bikerman, J.J., Surface  Chemistry, Academic Press  (New
    York) 1958 (2nd Ed.);  or other similar sources.

3.   Manual on Disposal of  Refinery Hastes: Vol. I  Haste
    Hater Containing Oil,  pg.  10,  American Petroleum  In-
    stitute, 1963 (7th Ed.).

4.   Allen, A.A., and Schlueter, R.S.,  Estimates of Surface
    Pollution Resulting  from Submarine Oil Seeps at Plat-
    form A and Coal Oil  Point, Technical  Memorandum 1230,
    November 1969, General Research  Corporation, Santa
    Barbara, California.

5.   Wobber, F.J., Imaging  Techniques for  Oil Pollution Sur-
    vey Purposes, Photographic Applications  in Science,
    Technology and Medicine, Vol.  6, No.  4 (July 1971).

6.   Orthlieb, F.L., LTJG,  USCGR, Photographic Detection of
    Ship-Generated Oil Slicks. Final Report, February 1971,
    Coast Guard Office of  Research and Development, Wash-
    ington, D.C.

7.   Short!ey, G. and Williams, D., Elements  of Physics,
    Prentice-Hall (Englewood Cliffs, New  Jersey),  1955
    (2nd Ed.); or other college physics textbooks.

8.   "Pollution in Navigable  Waters", Hearings before  the
    Committee on Rivers  and  Harbors, House of Representa-
    tives, 71st Congress,  2nd  Session on  H.R. 10625,  A Bill
    to Amend the Oil Pollution Act of 1924.  Part  I.
    May 2, 3, and 26, 1930,  p. 41-49, Washington,  U.S.
    Government Printing Office, 1930.
                       95

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SELECTED WATER
RESOURCES ABSTRACTS

INPUT TRANSACTION FORM
                  w
       THE APPEARANCE AND VISIBILITY OF THIN
       OIL FILMS ON WATER,
       Hornstein, B.
       Environmental  Protection  Agency
       Edison Water Quality Laboratory
       National  Environmental  Research Center
       Edison, New Jersey 08817
                                                                   In-House Report
        Environmental Protection Agency report
        number EPA-R2-72-039,, August 1972.
         Oil  films of controlled thickness up to 3000 nanometers, upon water
     surfaces  in the  laboratory, confirm an inherent and orderly thickness-
     appearance relationship which is independent of oil type and water type.
     These  laboratory studies also investigated the effects of viewing condi-
     tions  upon the ease of visibility of these thin films.

         Out-of-doors observations were made; these and the observations
     reported  by other sources were found to correspond with the laboratory
     results.  The visibility of a thin oil film depends not only upon its
     thickness-dependent inherent appearance, but also upon conditions ex-
     ternal  to the film.  These include nature of illumination and sky con-
     ditions,  sun angle, color and depth of water, color of bottom, and
     viewing angle.

         Color photographs are included for illustration of the points
     discussed.
          *0il-water  interfaces, *Thin  films, *0il, *Color, Theoretical analysis,
     Laboratory  tests,  On-site  investigations, Water pollution, Oil pollution,
     Water pollution  effects.
          Visibility,  Appearance,  Iridescent  films, Optical interference,
     Reflectivity.
                     05A
                                                    Send To:
                                                    WATER RESOURCES SCIENTIFIC INFORMATION CENTER
                                                    US DEPARTMENT OF THE INTERIOR
                                                    WASHINGTON, D C. 2O24O
         Bernard Hornstein
Edison Water Quality Laboratory,  NERC

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