I_                   Surveillance & Analysis Division
   337 5                   Region V
        UNITED STATES          230 South Dearborn St.
        ENVIRONMENTAL PROTECTION AGENCY Chicago, Illinois 60604	June - December, 1£



•        /_                      001R77100
      v
      \
        AMBIENT MONITORING
        NEAR THE LAND DISPOSAL SITE
|       FOR TACONITE TAILINGS
I       Reserve Mining Company
I       Silver Bay, Minnesota

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INTERIM REPORT OF SURVEY FOR THE IKS, ENVIRONMENTAL
PROTECTION AGENCY'S AMBIENT MONITORING NEAR THE LAND
DISPOSAL SITE FOR TACONITE TAILINGS, RESERVE MINING
           COMPANY, SILVER BAY, MINNESOTA
       U»S, ENVIRONMENTAL PROTECTION AGENCY
                     REGION V
        SURVEILLANCE AND ANALYSIS DIVISION
                 CHICAGO, ILLINOIS
                  JUNE - DECEMBER
                       1977
                                                         "-•y

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DISCLAIMER
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             Mention of trade names or commercial products does not constitute endorse-
 _           ment or recommendations for use by EPA.

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                                ABSTRACT
An ambient air monitoring survey for amphibole fibers and suspended
particulate was conducted near the Reserve Mining Company taconite
beneficiation process, Silver Bay, Minnesota, during the period
June 17, 1977 - June 23, 1978.  The objectives of the study were to
establish background levels of amphibole fibers and particulate,
monitor the levels of these pollutants as the beneficiation plant is
brought back into production and assess the impact of the construction
of the tailings basin (Milepost 7) on the populated areas.  During the
period of the survey, the plant was not in production from June 26, 1977-
December 6, 1977 except for one day, July 31, 1977.  This interim report
is concerned only with the period that the plant was shut down.  The back-
ground levels of particulate as measured at the six sampling stations
were low in comparison to the air quality standards.  It appears that the
construction activity at the tailings basin has little impact on the
populated areas.  Levels of amphibole fibers, as determined by X-ray
diffraction .analysis and electron microscopy for selected samples, were
also relatively low.  Conclusions are as follows:

1.   Suspended Particulates

     a.   Background levels of suspended particulate are very low in
          comparison to the air quality standards.

     b.   As measured at Sites 1 and 2, the background level of parti-
          culate in Silver Bay is 16 ug/m3.  Near the tailings basin,
          Milepost 7, the background level is 10 ug/m-\

     c.   Construction at Milepost 7 had minimal impact on the levels of
          particulate during the period of the background study.

2.   Amphibole Fibers

     a.   Background levels of amphibole fibers are low, at or near the
          detection limit of the X-ray diffraction analytical technique.

     b.   As measured at Sites 1 and 2 and considering the error of + 50%
          inherent in electron microscropy, the background level of amphibole
          fibers in Silver Bay is 7,5000 fibers/m^.  Near the tailings basin,
          Milepost 7, the background level is estimated at 3,000 fibers/m3.
          Second maximum 72 hour average background levels of fibers are
          estimated as 60,000 fibers/m3 in Silver Bay and 15,000 fibers/m3
          near the tailings basin.

     c.   Present techniques in X-ray diffraction analysis are not sufficiently
          sensitive to be used as a surrogate for electron microscope analysis
          of amphibole fibers when the Reserve Mining Company beneficiation
          plant is not operating.  However, the presence of low mass concentra-
          tion as measured by X-ray diffraction does indicate that the levels
          of fibers are correspondingly low.

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TABLE OF CONTENTS
ABSTRACT
1 . INTRODUCTION
2. OBJECTIVES
3. AIR QUALITY STANDARDS
a. Federal and State of Minnesota Ambient Air Quality
b. Minnesota Air Pollution Control Regulations
4 . BACKGROUND
a. Participating Agencies
b . Previous Survey
c . Period of Current Survey
d. Sampling Network
(1) Sampling Methods
(2) Sampling Frequencies
(3) Analytical Technique
(4) Quality Assurance
(5) Data Analysis
5. DISCUSSION
a. Ambient Monitoring
(1) Sampling Network
(2) Quality Assurance
b. Laboratory Analysis
(1) X-Ray Diffraction
(a) Sample Preparation
(b) External Standard
(2) Electron Microscope
(a) Sample Preparation
(b) Sample Analysis
c. Data Analysis
(1) Statistical Methods
(a) Statistical Analysis System (SAS)
(b) Additional Analyses
(2) Wind Data





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                                       TABLE OF CONTENTS (CONT'D)
•                                                                             PAGE
•           6 .  FINDINGS                                                        19
                 a.  Ambient Monitoring                                          19
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    (1)  Suspended Particulate                                 19
    (2)  Amphibole Fibers                                      21
•               b.  Analysis of Variance (ANOVA)

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                                                               24

c.  Wind Data                                                  25

CONCLUSIONS                                                    25

RECOMMENDATIONS                                                27
             •APPENDIX A.  Minnesota Pollution Control Agency, Suspended          28
                           Particulate Data Analysis Procedure
                      B.  Operation and Service of the Network                   36
                      C.  Production Rates                                       42
                      ID.  Total Suspended Particulate Data Sheets                45
                      E.  X-Ray Diffraction Analysis, Amphibole Mass             47
                           Concentration (ug/m^)
                      IF.  Electron Microscope Analysis, Amphibole Fibers         55
                           (fibers/m3)
                      G.  Problem Samples                                        58
•                    H.  Wind Frequency Distribution, Reserve Office            60


                                         LIST OF FIGURES

•           Figure No. 1.  Air Monitoring Network                                5
                        2.  Typical X-Ray Diffraction Pattern of Filtered
•                           Solids                                              12
                        3.  Preparation of Electron Microscope Grids             14
                        4.  Wind Rose, Reserve Mining Company                    26

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                                TABLE OF CONTENTS (CONT'D)


                                                                       PAGE


TABLE No. 1.  Randomized Fiber Samples                                   6
          2.  Performance Audits                                         9
          3.  Statistical Analysis System Functions                     15
          4.  Statistical Symbols                                       16
          5.  Suspended Particulate Summary Statistics, ug/m^           19
          6.  Projected Annual Statistics, ug/m-*                        20
          7.  Precision of Noncontinuous Sampling                       20
          8.  Amphibole Mass Summary Statistics, ug/m^                  22
          9.  Amphibole Fiber Summary Statistics, fibers/m              22
         10.  Projected Annual Statistics, Amphibole Fibers             23
         11.  Correlation Between the Amphibole Mass and Fibers Data    24
         12.  Summary of ANOVA                                          24

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     INTERIM REPORT OF SURVEY  FOR THE  U.S.  ENVIRONMENTAL  PROTECTION
       AGENCY'S AMBIENT MONITORING NEAR THE LAND DISPOSAL SITE FOR

     TACONITE TAILINGS, RESERVE MINING COMPANY,  SILVER BAY,  MINNESOTA
1.    INTRODUCTION


     During the summer of 1976,  ambient  air  monitoring for  amphibole
     fibers was completed by the University  of Minnesota, Duluth
     under contract with the Surveillance  and  Analysis Division,
     Region V,  U.S. Environmental Protection Agency (EPA).   At  that
     time, this study was the latest  of  a  series  of studies completed
     by the EPA, the State of Minnesota  or Reserve Mining Company
     beginning  in the early 1970s.   The  1976 study was undertaken to
     assess levels of fibers in  Silver Bay,  Minnesota during the period
     of the annual shutdown of the  Reserve Mining Company's beneficia-
     tion plant.  This occurs during the month of July.  In the spring
     of 1977,  it was once again  determined to  gather background levels
     of fibers  during the shutdown.  However,  regulatory agency re-
     sources were to be used to  complete the monitoring. As a  result,
     a network  was established on June 17, 1977.   The ambient air
     monitoring included suspended  particulate in addition  to the
     amphibole  fibers.  The Air  Surveillance Branch, Region V,  had
     responsibility for installation and service  of the network.
     Laboratory analysis for suspended particulate was completed by

     the Minnesota Pollution Control  Agency.  Analysis of amphibole
     fibers was completed by the Lake Superior Basin Studies Center,
     University of Minnesota, Duluth under contract with the Environ-
     mental Research Laboratory, EPA, Duluth,  Minnesota. This  interim
     report is  concerned with the period of  the extended shutdown
     of the beneficiation plant  from July  to December, 1977.


2.    OBJECTIVES


     a.   Establish background levels of amphibole fibers and suspended
     particulate in Silver Bay,  Minnesota  during the shutdown of the
     beneficiation plant.


     b.   Monitor levels of amphibole fibers and  suspended  particulate
     as the beneficiation plant  is  brought into full production.


     c.   Monitor levels of fibers  and suspended  particulate near the
     boundary of Milepost 7 and  assess the impact of the construction
     work on the populated areas.

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                                   -2-


3.   AIR QUALITY STANDARDS


     No air quality standard for amphibole fibers has been promulgated;
     however, the Eighth Circuit Court in its decision of March 14, 1975,
     mandated that the fiber count be reduced to the level ordinarily
     found in the ambient air of a control city such as St. Paul (7000
     fibers/cubic meter).  Existing standards for suspended particulate
     are defined below.


     a.   Federal and State of Minnesota Ambient Air Quality


          (1)  Primary Standards - annual geometric mean of 75 ug/m^ not
               to be exceeded.


                                 - 260 ug/m^ maximum 24-hour average con-
               centration not to be exceeded more than one day per year.


           (2) Secondary Standard - 150 ug/m-' maximum 24-hour average
               concentration not to be exceeded more than one day per
               year.


     b.   Minnesota Air Pollution Control Regulations


          (1)  APC-6 - Preventing Particulate Matter from Becoming Air
               Borne: All reasonable measures must be used to prevent
               particulate from becoming air-borne.


4.   BACKGROUND


     A meeting was held on June 2, 1977, at the Minnesota Pollution Control
     Agency to finalize plans for starting an ambient monitoring network
     near Silver Bay, Minnesota.1  Earlier, the Minnesota Supreme Court
     directed Reserve Mining Company to construct a land disposal site for
     taconite tailings at Milepost 7.  As a result, plans for monitoring
     near the land disposal site first formulated in October 1976 could be
     incorporated into the network for monitoring near Silver Bay.2  The
     network which resulted represents a modification of that originally
     intended for monitoring the land disposal site.  The important objec-
     tive of sampling in the populated areas was met.  However, boundary
     line sampling at the disposal site was not possible because of the
     lack of available power.
      1. Region V, U.S. EPA, Surveillance and Analysis Division Memorandum
      dated June 8, 1977, subject: Ambient Air Monitoring Milepost 7,
      Reserve Mining Company.


      2. Protocol for Ambient Monitoring Near the Land Disposal Site for
      Taconite Tailings, Reserve Mining Company, Region V, U.S. EPA,
      Surveillance and Analysis Division, October 8, 1976.

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                              - 3 -



a.   Participating Agencies


     The agencies represented at the meeting were as follows:


     (1)  Region V, Surveillance and Analysis Division.
     (2)  Environmental Research Laboratory, Duluth, Minnesota.
     (3)  Minnesota Pollution Control Agency.


     Certain areas of responsiblity were accepted by each agency to
     ensure gathering quality assured air monitoring data.  These
     are detailed below:


     (4)  Region V, Surveillance and Analysis Division (S&AD).
          (a)  Overall responsiblity for the air monitoring study.
          (b)  Specific responsiblity for gathering the air samples
               including site selection, installation, service and
               maintenance of the network.
          (c)  Report preparation.


     (5)  Environmental Research Laboratory, Duluth, Minnesota (ERL).
          Specific responsibility for laboratory analysis of the
          amphibole fiber samples.


     (6)  Minnesota Pollution Control Agency (MPCA).
          (a)  Specific responsiblity for supplying and analyzing the
               filters used to gather the suspended particulate data.
          (b)  Assist in site selection and installation of the network.


b.   Previous Survey


     The one previous survey designed specifically to gather back-
ground data on amphibole fibers in the Silver Bay area was that
completed by the University of Minnesota, Duluth during 1976.^  This
study was completed under contract with Region V, Surveillance and
Analysis Division.  The study was designed to include air sampling
during the time the beneficiation plant was shutdown.  At one of the
sites located in Silver Bay (The William Kelly High School), the
average amphibole fiber concentration was estimated at 311,000 fibers/in-*
including the contribution from the plant.  During the shutdown period,
the average concentration measured at the same site was estimated to be
40,700 amphibole fibers/m3.
3. D.E. Olson, Report on Air Monitoring at Silver Bay During Shutdown -
Summer of 1976, Dept. of Physics, University of Minnesota, Duluth,
EPA Contract #68-01-4193, April 1977.

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                                 - 4 -
   c.    Period of Current Survey


        As originally designed,  the survey was planned for a period
   of  90 days to include the shutdown of the beneficiation plant
   during July.  Following the resumption of the operation of the
   plant on July 31, 1977, an iron workers strike caused its immedi-
   ate shutdown on August 1, 1977.  Since this presented the opportu-
   nity to gather additional background data, the survey was continued
   through the period of the strike and for an additional six months
   following resumption of production.  The survey began June 17, 1977
   and ended June 23, 1978.


   d .    Sampling Network


        The air monitoring network is described in Figure 1.  Coverage
   was provided for Silver Bay (Stations 1 and 2), Beaver Bay (Station
   3)  and in the area of the tailings basin at Milepost 7.  Sampling
   was to be conducted for suspended particulate and amphibole fibers
   at  each location.  In addition, wind data were collected at two
   locations .


       (1)  Sampling Methods
            (a)Suspended particulate - reference method high volume
                 samplers as described in 40 CFR 50, Appendix B.


            (b)  Amphibole fibers - membrane samplers of the type used
                 historically for sampling amphibole fibers at a nominal
                 flow of four cubic feet per minute (CFM) through a
                 membrane filter with a pore size of 0.45 micron (um)
                 and 102 millimeters in diameter.^


       (2)  Sampling Frequencies


            At the recommendation of the Duluth Laboratory, a composite
            sample of amphibole fibers was collected over three days.
            This would provide sufficient mass of material for analysis
            by X-ray diffraction.  As a result, the sampling frequency
            for gathering suspended particulate data was every third day
            rather than the six day cycle specified as minimum in 40 CFR 51
4. J.S. Drury, et al,  Review of the Environmental Effects of Asbestos (Draft),
Oak Ridge National Laboratory, April 1977, Contract No. W-7405-eng-26.

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                                     JO
                                                                                RESERVE MINING
                                                                                    COMPANY
             
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                          - 6 -
(3)  Analytical Technique
     The analysis for particulate was in accordance with the
     reference method and completed by MPCA.  All membrane
     samples were analyzed by the Lake Superior Basin Studies
     Center under contract with the Duluth Laboratory using

     X-ray diffraction techniques developed at the laboratory.
     A random selection of the membrane samples (5 per station
     per quarter) was analyzed for fibers using electron micro-
     scopic techniques.  The randomized fiber sample schedule
     is described in Table 1 below:


                        TABLE 1


                RANDOMIZED FIBER SAMPLES
                                              CALENDER SCHEDULE
                                              June 17, June 26
                                              July 14
                                              Aug. 19, Aug. 29
SAMPLE
1,
5
1 ,
9,
1,
9
1
3,
1,
9
6,
9,
3
NOS.
4

10
4
9


10
5

9
5

                                              Sept,
25
      10, Sept.
Oct. 1, Oct. 25
November 28
December 1
Jan. 9, Jan. 30
Feb. 2, Feb. 14
March 25
April 18, April 25
May 15, May 27
June 8
(4)  Quality Assurance
    Quality control  of the fiber data was under the general
    supervision of the Duluth Laboratory.  However, additional
    procedures  were  also agreed upon and utilized throughout the
    study.


    (a)   Calibration - the high volume samplers were calibrated
         initially by the Central District Office, S&AD,  prior to
         shipment  to the site (one of the samplers was  calibrated
         by the Western District Office). Three spare motors were
         also calibrated for immediate use in the field in the
         event  of  breakdown. Subsequent calibrations are  reported
         in the Discussion section of the report. No standard tech-
         nique  was available for calibrating the membrane samplers.
         It was agreed that a technique using a hot wire  anemometer
         employed  by MPCA would be used for this calibration.  The
         membrane  samplers were calibrated by MPCA prior  to shipment
         to the site.  Subsequent calibrations required at selected
         stations  because of equipment failures were completed
         by MPCA.

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             (b)   Filter  processing  -  glass  fiber  filters  for  sampling
                  particulate were processed  in  accordance with  existing
                  MPCA  procedures as described in  Appendix A.  In  addi-
                  tion  to analysis,  MPCA is  responsible  for  storage  of
                  the  filters.   Filters  were  maintained  on site  in envelopes
                  for  periodic  shipment  to MPCA.   Membrane filters were
                  secured in plastic petri dishes  for  shipment to  the
                  Duluth  Laboratory.   A  numbering  procedure  was  established
                  and  chain of  custody was exercised.


             (c)   Operation of  the network -  checklists  pertaining to  the
                  operation and daily  service of the  stations  were developed
                  by S&AD. Copies of  these  procedures are in  Appendix  B.


        (5)   Data Analysis


             Data analysis was  to be completed by  S&AD for comparison  with
             the  appropriate air quality standard.  To relate  the  X-ray
             diffraction  analysis of the fiber samples with  the  electron
             microsopic analysis, correlation coefficients were  to be  developed
             for  each  station  as well  as the  overall  data  set.


5.   DISCUSSION


     a.  Ambient  Monitoring


         The operation and maintenance of the network was  completed  by the
     Air Surveillance  Branch,  S&AD during the initial phase  of the study,
     June 17 - August  19, 1977.  Subsequent  to this,  the service of  the net-
     work was contracted  with  the Lake Superior  Basin Studies  Center,
     University of Minnesota,  Duluth.   The responsiblity for maintenance  of
     the network remained with S&AD.  Training for the student operators
     was provided by S&AD personnel.


         (1)  Sampling Network


              The final design of the  ambient network resulted from  site
              evaluations completed  with the assistance  of personnel from
              MPCA and the Western  District  Office, S&AD.   The sites in
              Silver Bay were  selected because they meet siting  guidelines, 5
              are representative of  the  populated  area and,  historically,
              are locations  used in  previous monitoring  completed in Silver
     5. Guidance for Air Quality Monitoring Network Design and Instrument
     Siting, OAQPS 1.2-012, Office of Air Quality Planning and Standards,  RTP,
     September 1975.

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Bay.  The site in Beaver Bay was chosen as meeting siting
guidelines and being representative of the limited population
in the area.  The outlying sites were selected primarily because
of the availability of power and proximity to the land disposal
sites at Milepost 7.  The sampling locations are described
below and on Figure 1.

(a)  Station 1 - Campton Elementary School, Silver Bay.
                 Station equipment - High Volume sampler
                                     Membrane sampler
                 Station height - roof height of 24 feet
                 Obstructions - none

(b)  Station 2 - William Kelly High School, Silver Bay.
                 Station equipment - High Volume sampler
                                     Membrane sampler
                 Station height - roof height of 36 feet
                 Obstructions - none

(c)  Station 3 - Holiday Gas Station, Beaver Bay.
                 Station Equipment - High Volume sampler
                                     Membrane sampler
                 Station height - roof height of 14.5 feet
                 Obstructions - trees in rear of building 50 feet
                 away, possible re-entrained road dust, construction
                 at adjacent building during Fall 1977.

(d)  Station 4 - Highway 3, location of Reserve Mining Company's
     High Volume sampler (Site #11).
                 Station equipment - High Volume sampler
                                     Membrane sampler
                 Station height - platform 4.5 feet above ground,
                 total height of filter - 8 feet.
                 Obstructions - none

(e)  Station 5 - Dr. Rodney Nelson's property off of Highway 5.
                 Station equipment - High Volume sampler
                                     Membrane sampler
                                     Wind set mounted on a 40 foot towe
                 Station height - platform 4.5 feet above ground, total
                 height of filter - 8 feet
                 Obstructions - possible interference from trees, excep
                 no obstructions for wind measurements.

(f)  Station 6 - Mr. W.J. Nosek, Jr.'s property off of Highway 4,
     location of Reserve Mining Company's High Volume sampler (Site #8)
                 Station equipment - High Volume sampler
                                     Membrane sampler
                 Station height - platform 4.5 feet above ground, total
                 height of filter - 8 feet.
                 Obstructions - interference from nearby trees

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                                - 9 -


          A wind set was also installed at the Reserve Mining Company
          office complex.  The transmitter was mounted on a 40 foot
          tower.  A weather shelter was also installed to house the
          following equipment:


                           Hygrothermograph
                           Minimum/maximum thermometers


      (2)  Quality Assurance


           Numerous audits were performed during the study to ensure
           proper operation of the network and equipment.  Periodic
           calibration of the high volume samplers were completed co-
           incident with the change of motor brushes.  These calibrations
           were completed as part of the maintenance responsibility by
           the S&AD.  A significant role was that carried out by MPCA.
           In addition to calibrating the membrane samplers, periodic
           audits were performed on the network operation and sampler
           flow rates (both membrane and Hi-Vol samplers).  Audits of the
           network operation were also carried out by personnel of the
           Air Surveillance Branch, S&AD.  During the performance of routine
           maintenance on the Hi-Vols, calibration following motor brush
           changes, audits of the operation were also completed by S&AD,
           District Office personnel.  The audits and calibrations completed
           during the background study are described in Table 2 below:


                               TABLE 2
TYPE OF AUDIT


Hi-Vols, membrane
samplers , network
operation.
Hi-Vol calibration,
network operation


Network operation
Hi-Vo1s,  membrane
samplers, network
Hi-Vol calibration,
network operation
                        PERFORMANCE AUDITS
RESPONSIBLE
  AGENCY


   MPCA
                    PROBLEMS
              MAJOR*        MINOR
              None
   S&AD
   S&AD
   MPCA
   S&AD
8/29-30/77    None
10/5-6/77
10/7/77
11/8/77
None
None
None
              Loose wing
              nuts on filter
              holder.
              Transducer hose
              splitting.


              None
None
Loose wing
nuts. Transducer
hose cracking.


None

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                                - 10 -


                            TABLE 2 (cont.)


                         PERFORMANCE AUDITS


                       RESPONSIBLE                  PROBLEMS

TYPE OF AUDIT            AGENCY        DATE     MAJOR*       MINOR


Hi-Vols, membrane         MPCA       12/12/77   Tearing      None
samplers, network                               filters

operation.


Wind set, Dr.             S&AD       12/2/77    Malfunctioning  None

Nelson's property                               recorder


 * Major problems are those which could result in invalid data.


          The most serious problem which resulted in the loss of data
          involved the wind recorder at Site #5, Dr. Nelson's property.
          The recorder malfunctioned in August and was only discovered
          in early December during an analysis of the wind charts for
          that period.  The malfunction resulted in a loss of a portion
          of the trace and was not readily discernable.  As a result,
          the data were lost for the period August 30 through
          December 21, 1977.  Another significant problem which could
          have affected the fiber data was tearing filters.  This
          problem occurred in early winter and was resolved through
          proper handling techniques.


     b.   Laboratory Analysis


          The laboratory analysis for amphibole fibers was completed by
     the Lake Superior Basin Studies Center under contract with and the
     general supervision of ERL. All samples were analyzed using X-ray
     diffraction techniques while a random sample of the membrane filters
     were analyzed using electron microscopy. Brief descriptions of the
     methods follows:
      (1)  X-Ray Diffraction


          Methods  for the semi-quantification of mass concentration of
          of amphibole  fibers have  previously been reported.   Following
          collection on a micrometer Millipore membrane  filter,  a  section
          of the  filter is mounted  on  a glass slide which  is  placed in a
          Phillips APD  3500  automated  powder diffractometer  for  analysis.
          An amphibole  (110) diffraction  peak and a (310)  peak unique to
   6.  Cook,  P.M. et  al,  Semi-Quantitative  Determination  of  Asbestiform
   Amphibole Mineral  Concentrations  in Western  Lake  Superior  Water  Samples,
   Advances  in  X-Ray  Analysis,  Ed.,  18:557-567,  1975.

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                              -li-

        the  amphibole  mineral  cummingtonite-grunerite (c-g)
        are  observed  in  samples  containing  amphibole  fibers
        as  shown in Figure  2.   The  amphibole  (110)  and c-g
        (310)  peak intensities are  determined by step scanning
        with copper K^ radiation in 0.02° increments  over the
        26  ranges 9.9  -  11.1  and 28.8  -  29.6  degrees, respectively.
        The  integrated peak count is calculated  by  summing the net
        counts above  background  for each increment.

    (a)  Sample Preparation

        Samples were  prepared  for X-ray  diffraction analysis  by
        mounting the  membrane  filter on  a 17  x 26 millimeter
        (mm) piece of glass cut  from a microscope slide.   A
        light  coating of clear lacquer sprayed on the glass  provided
        a smooth, effective adhesive for the  filter piece which was
        then trimmed  with a razor blade  to  the edge of the glass.
        A light coating  of  lacquer  was sprayed on the filter  sample
        surface prior to mounting on the glass piece  to prevent any
        of  the particles from  being rubbed  off.   The  layer of lacquer
        causes a small loss of X-ray intensity due  to scattering of
        the  X-rays.  Once placed in the  diffractometer sample changer,
        the  filter sample was  held  flush with the top surface of the
        sample holder  by sealing the reverse  side of  the  sample into
        the  holder with  a few drops of wax.

    (b)  External Standard

        The  mass of amphibole  in a  sample is  calculated from  an
        external standard curve  (Figure  2 insert) which is deter-
        mined  by X-ray diffraction  of  prepared samples of taconite
        tailings.  The fine tailings contain  approximately 80%
        amphibole, mostly c-g  with  some  actinolite.   The  remaining
        20%  is quartz with  traces of other  minerals.   The amphibole
        fibers in the  standard are  essentially the  same as those
        present in air samples from Silver  Bay but  tend to have a
        smaller diameter distribution.  Standard samples  were
        prepared by filtration of known amounts  of  amphibole  mixture
        on  960 mm2 areas of millipore  filters.  Each  filter  was
        coated with lacquer and  mounted  for X-ray diffraction
        analysis in the  same  way as the  air sample  filters.

(2)  Electron Microscope

    Fiber counts are  made by  identifying individual fibers among
    the  many particles present in the  sample.  Since  the  number of
    fibers  which are  actually  counted  is a  small fraction of  the
    calculated fiber  concentration, the  sample must be prepared
    for  electron microscope examination  in  a  way that preserves
    the  original particulate  concentration  and distribution.
    The  direct transfer  of  filtered particles from  the surface of
    the  filter to a carbon  film replica  on  an electron microscope
    grid, without the  rearrangement of the  particles, allows  the
    viewing of microcosms which are representative  of the total
    sample .

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- 12 -

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                               - 13  -

   (a)   Sample  Preparation

        The  relatively large  mass  loadings  and  the  millipore filters
        required for sample  collection and  X-ray diffraction analysis
        (72-hour sample period)  do not lend to  electron microscope
        analysis.  The heavy particulate loading on the filters
        required a sample  dilution step prior to electron microscope
        grid preparation.  Also, efficient  direct transfer of particles
        to  electron microscope  grids requires that  the  sample be
        placed  on the flat surface of  a Nuclepore membrane filter.   In
        this event, procedures  required low temperature ashing of a
        piece of the original membrane filter,  resuspension of the  ash
        in  0.1  urn filtered distilled water  with five minutes of low
        energy  sonification  and filtration  on a 47  mm,  0.1 urn Nuclepore
        filter.  The preparation of  electron microscope grids was per-
        formed  in a filtered air environment as follows (see Figure 3).
        Nuclepore filters  or filter  sections were carbon coated to
        create  an approximately 500A thick  carbon film  with particles
        inbedded in it.  Small  sections of  the  filter were cut and
        placed  carbon side down on Formvar  film coated  electron micro-
        scope grids.  The  grids were placed on  a piece  of coarse  metal
        screen  on top of several layers of  filter paper in a petri
        dish.   A small drop of chloroform  was  placed on each filter
        section and the layers  of filter paper  were saturated with
        chloroform.  The petri  dish  was covered and chloroform vapors
        allowed to slowly dissolve away all of the  filter and Formvar
        film.  This step takes  from  4  to 24-hours.   The grid which
        results is covered with a carbon film in which  the sample
        particles are imbedded.  The technique  minimizes the loss
        of  particles during  the  transfer of the sample from filter
        to  grid and leaves a replica of the filter  (0.1 urn holes)
        which can be used  to check on  folds or  breaks in the carbon
        film.  Blank samples were prepared  from unused  Millipore
        filters in the same  manner as  air samples.

    (b) Sample  Analysis

        Randomly chosen grid openings  were  systematically scanned at
        a magnification of 10,000 X  or greater on a JEOL 100C or
        Phillips 201 transmission electron  microscope.   Grid openings
        with broken carbon films or  other disruptions of the sample
        are rejected.  Each  particle which  has  a length to width  ratio
        j> 3 is  studied by selected area electron diffraction (SAED) to
        determine its mineralogical  identity.  Amphibole and chrysotile
        filbers produce characteristic SAED patterns when oriented
        properly in the electron beam.7  Fiber size, orientation  or
        interferring particles  cause many SAED patterns which are
        ambiguous.  All fibers  which cannot be determined to be chrysotile,
        amphibole or non-amphibole by  SAED  are classified as ambiguous.
7. Cook, P.M., et al,  X-Ray Diffraction and Electron Beam Analysis of
Asbestiform Minerals in Lake Superior Waters, The Institute of Electrical
and Electronics Engineers, Inc., Annals No. 75CH1004-1, 1976.

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                       - 14 -
        TRANSFER  OF AIR SAMPLES  TO
        ELECTRON  MICROSCOPE GRIDS
  Air Sample
                      Low Temperature
                         Ashing
 Ash +
 0.1 jum Filtered
 Distilled H20
                     filter piece
         7
O.Sjum or 1.2jum

Millipore Filter
    .carbon
       .filter
Sonification (bath)
                                                  Filter
                              _ Carbon
                                 Coat
                 formvar
                                            O.l/jm or 0.2,/jm
                                            Nuclepore Filter
               carbon
                           ELECTRON MICROSCOPE
         Figure 3: Preparation of Electron Microscope Grids

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                               - 15 -

         This  includes  fibers  which are clumped with other particles.
         The result of  this procedure is to underestimate the actual
         fiber concentrations  present in the sample.  At least 10
         grid  squares for each sample were examined.  This resulted in
         a range of 0 - 127 amphibole fibers observed for shutdown
         period air samples.  The amphibole fiber concentration is cal-
         culated from the formula:
                                                                        2
  # amphibole  fibers/m^ (cubic meter) = # amph. fibers X filter area (urn )

                                                  2                          3
                                 area examined (um ) X air volume sampled (m >
 c.  Data Analysis

     (1)  Statistical Methods

         (a)  Statistical Analysis  System (SAS)

              The Statistical  Analysis System (SAS), Version 76, was
              used to analyze  the data for certain of the statistics
              reported.   SAS  is an integrated system for data
              management and  statistical analysis which is operational
              on the USEPA Computing Center, Washington, D.C.  Access
              is available from the Region V office  through terminals.
              The functions utilized in the data analysis are listed in
              in Table  3 below:

                                  TABLE 3

                   STATISTICAL ANALYSIS SYSTEM FUNCTIONS

   DATA                                  FUNCTION

   Particulate                           1. Creation of data set
                                            a. DATA (p. 10)*
                                            b. INPUT (p. 11)
                                            c. LOG (p. 283)
                                            d. CARDS (p. 18)
                                         2. Selection of data from data set
                                            a. IF-THEN (p. 35)
                                            b. DELETE (p. 45)
                                         3. Data listing
                                            a. PRINT (p. 204)
                                            b. SORT (p. 233)
                                         4. Descriptive Statistics
                                            a. MEANS (p. 180)
                                            b. Regression, correlation,
                                               analysis of variance and
                                               covariance - ANOVA (p.  57)
                                         5. T Test (p. 275)
   Amphibole fibers                         1. All of the above
                                            2. CORR. (p. 92)


* refers to page number of manual referred to in footnote 8, below
 8. Barr, A.J., Goodnight, J.H., A Users Guide to SAS 76, SAS Institute,
 Inc, Raleigh, N.C.,  1976.

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                                - 16 -
         Prior to the computer analysis,  the data were keypunched to
         cards from data sheets.  The data were subsequently listed
         and verified for any keypunching or transcription errors.
         Statistical formulae used by SAS are referenced specifically
         in the Users Manual.  Examples of the techniques used are
         described below.  The symbols used in the various formulae
         are described in Table 4.


                             TABLE 4


                       STATISTICAL SYMBOLS


     SYMBOL                                   DESCRIPTION
       n                                Total samples collected
       N                                Total possible samples
       Xi                               Concentration of each sample
       In                               Natural logrithm function
                                         (log to base e)
       EXP                              Exponential function (inverse
                                         of the In function)
       Zi                               Total summation of the
                                        appropriate values
       X                                Arithmetic mean*
       Xg                               Geometric mean
       S                                Arithmetic standard deviation
       Sg                               Geometric standard deviation


* Arithmetic mean is always equal to or greater than the geometric mean.

         Although  not  used  in the  data  analysis,  formulae  for  the  arithmetic
         mean  and  standard  deviation  are  displayed  for  comparison  purposes.


          _!_  Arithmetic Mean


             x.I  I  X1


          2  Geometric Mean

             _           n
             Xg= EXP {I  E  In Xi}
                      ^  i

          3  Arithmetic Standard Deviation
             S =
                     1
Xi2 - i  ( E  Xi )
                   r, - TT  ' i        r\  * i

          4  Geometric Standard Deviation
             Sg - EXP        ( n  (ln xi)2 .i(J


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                         - 17  -
      _5  Correlation


         Let n = number of values
         Xi, Yi = pairs of values
         r = sample correlation coefficient

         then r =  n I Xi Yi - (Z  Xi)  (I Yi)	

                  [(n I Xi2 - (z Xi)2) (n i Yi2 - (I
 (b)  Additional Analyses


      Other statistical routines are used to estimate annual
      statistics and levels of confidence.

                                          9
      i  Arithmetic Mean to Geometric Mean


         Xg -    X	  „
               EXP (0.5 (In Sgr)


      _2  Maximum and Second High Predicted 24 Hour Concentrations


         For a geometric mean Xg, and geometric standard deviation,
         Sg, based on a log normal distribution of concentrations
         throughout the year, the maximum and second high concentra-
         tion predicted for the year are estimated as follows.9


         C                —     2 94*
          max (Maximum) - Xg Sg

                                        ±L

          2nd (second high) = Xg Sg


         Example: Xg = 70 ug/m

                  Sg = 1.50

         C             3        2 94           3
          max * 70 ug/m  (1.50)  '   = 231 ug/m


         C2nd = 70 ug/m3 (1.50) 2>63 = 203 ug/m3
9. Larsen, R, A Mathematical Model for Relating Air Quality
Measurements to Air Quality Standards, Office of Air Programs,
USEPA, November, 1971.


^Statistic for 24 hour samples, for 3 day samples use 2,58 and
 2.22 respectively.

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                        -  18  -
          Precision of Noncontinuous Sampling

          The following formulas  are from Hunt (1972)  and
          provide the difference  between the geometric mean
          and the upper and lower 95% confidence limits as
          a fraction of the geometric mean.10

          Lower limit fraction (m,)
                                  In Ss
I                                             ,          in  s§  /    £ \ 2 \
                                m,  -  1  -  EXP   I-  t.025    \     \1  - N /  /
                                  i             *          n
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          Upper limit fraction = n^       ^
                            In Sg      n. 2 .
          m2 = EXP  (t.025  uh    [l - N|   /  - 1
          where t.025 = "t" statistic for (n - 1) degrees of
                         freedom at the 95% confidence level

          then: lower confidence limit (LCL) = Xg - m^ Xg

                upper confidence limit (UCL) = Xg + n^ Xg

          Example: Xg = 14
                   Sg = 2.11
                   n  = 45
                   N  = 365
                t.025 = 2.016

          mi = 1 - EXPF 2.016  .747     II -  45 \  2 ~|  = 0.190
           J.           1         — Mil  III -II III!	- I     — ..II-I.M |    I
                       L        .   .k
          m2 = EXP P 2.016 .747     /I -  45 \ ^ ~~J  - 1 = 0.234
                   "-        ,,^*f    »     365'   -1
          then  LCL - 11
                UCL = 17

      Therefore, because sampling occurred only once every three
      days, the true annual mean is between 11 ug/m3 and 17 ug/m3
      at the 95% confidence level.
10. Hunt, W.F., Jr., The Precision Associated with the Sampling
Frequency of Lognormally Distributed Air Pollution Measurements,
Journal of Air Pollution Control Association, 22, 687-691, 1972.

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                                  - 19 -
    (2)   Wind Data


         Wind direction and speed were recorded at two locations, near

         the Reserve Mining Company Office and at Station 5.  Subsequent
         data reduction was completed by Air Surveillance Branch personnel.
         Hourly average values of wind direction and speed were determined
         from the trace recordings for subsequent averaging to 24 hour
         values.  A wind rose based on the one hour values was developed

         from the data collected at the Reserve office.


6.   FINDINGS


     Although not of concern to this interim report on background levels of
     pollution, the production rates for the beneficiation plant are described
     in Appendix C.  Of interest to this report are the specific days when
     the plant was shut down.  In the final report, the relationship of
     particulate and fiber levels during production and non-production
     periods will be fully explored.


     a.  Ambient Monitoring


         (1)  Suspended Particulate


              Total suspended particulate (TSP) were monitored every third
              day at each of the six sites, using the Federal reference method.
              TSP data were analyzed for each site for the period June 26, 1977
              to December 5, 1977, when the beneficiation plant was shut down.
              The detailed list of all TSP data may be found in Appendix D.
              Table 5 below is a summary of the number of observations, geomet-
              ric means, minimum, maximum and second maximum 24-hour averages
              and standard geometric deviations for these sites and time periods


                                    TABLE 5


                    SUSPENDED PARTICULATE SUMMARY STATISTICS, ug/m3
                           JUNE 26, 1977 - DECEMBER 6, 1977
                                 NON-PRODUCTION DAYS
                                                                STANDARD
                     GEOMETRIC                       SECOND     GEOMETRIC
LOCATION     #OBS.     MEAN      MINIMUM   MAXIMUM   MAXIMUM    DEVIATION
1
2
3
4
5
6
45
50
51
48
49
50
14
18
20
10
9
10
2
1
1
2
1
1
57
43
70
33
47
35
41
37
49
30
38
31
2.11
1.84
1.95
1.90
2.29
2.18

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LOCATION

   1
   2
   3
   4
   5
   6
                              - 20 -

              The second maximum values are useful for comparison to
              the 24-hour standard of 260 ug/m3 (primary) and 150 ug/m3
              (secondary) not to be exceeded more than once per year.
              However, the comparison should be made from data collected
              over a full year.  As discussed earlier, annual statistics
              can be estimated from shorter term data.  These maximum
              and second maximum values are described in Table 6 below
              (see Footnote 9, page 17).

                                    TABLE 6

                       PROJECTED ANNUAL STATISTICS, ug/m3

GEOMETRIC
MEAN
14
18
20
10
9
10
STANDARD
GEOMETRIC
DEVIATION
2.11
1.84
1.95
1.90
2.29
2.18
MAXIMUM

  124
  107
  144
   66
  108
   93
SECOND
MAXIMUM

   98
   89
  117
   54
   83
   76
              Other statistics are useful to establish the precision of
              the mean value when the data are not collected daily (see
              Footnote 10, page 18).  Upper and lower control limits about
              the mean at the 95% confidence level are described in
              Table 7.

                                    TABLE 7

                     PRECISION OF NONCONTINUOUS SAMPLING
                                                  CONCENTRATION ug/m3
                                                       GEOMETRIC
                                                 LCL      MEAN     UCL


LOCATION
1
2
3
4
5
6


#OBS .
45
50
51
48
49
50
STANDARD
GEOMETRIC
DEVIATION
2.11
1.84
1.95
1.90
2.29
2.18


t.025
2.016
2.011
2.009
2.013
2.012
2.011
                                                  11
                                                  15
                                                  16
           14
           18
           20
           10
            9
           10
     17
     21
     24
     12
     12
     12

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                        - 21 -
     Prior to the start of the survey,  construction of the
     tailings basin at Milepost 7 had started.  Initial
     construction includes two dams to  be located in the
     southern portion of the disposal site (see Figure 1,
     page 5).  Once completed the two dams will form a basin
     two by three miles in size.  The work involves consider-
     able clearing of vegetation and earth moving.  A review
     of the average particulate sampled at Sites 4, 5 and  6
     indicates that the construction has had minimal impact
     during this phase of the study.


(2)   Amphibole Fibers


     Amphibole fibers were monitored at each of six sites.
     Continuously, a composite sample was collected over a
     period of three days.  Two analyses were completed, all
     samples  were analyzed using X-ray diffraction techniques
     and a selected number of samples (five per site per quarter)
     were analyzed using electron microscopy.  To preclude any
     bias affecting the levels of mineral fibers sampled and
     selected for analysis on the electron microscope, a random
     schedule was developed using the random number generator
     available on SAS.  The X-ray diffraction mass data are described
     in Appendix E.  The amphibole fiber count data for those samples
     analyzed using electron microscopy are described in Appendix
     F.  During the survey, problems were noted, some of which could
     affect the samples collected.  These problems were generally
     associated with potential interferences or with the service
     of the network and are described in Appendix G.  If the
     problem associated with the sample was of sufficient  magnitude
     to invalidate the sample, no data are reported in Appendices
     E and F.


     Summary statistics of the X-ray diffraction data are  described
     in Table 8 below.  During this period, the levels of the
     amphibole mass data were relatively low, particularly at the
     more rural sampling stations, sites 4, 5 and 6. The bulk of
     the data from these sites are below the detection limit of the
     X-ray diffraction analytical method.  In this event,  the data
     are assigned the value of the detection limit.

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TOTAL
LOCATION
TOTAL
                             - 22 -


                             TABLE 8


               AMPHIBOLE MASS SUMMARY STATISTICS, ug/m3


LOCATION
1
2
3
4
5
6


#OBS.
56
54
54
59
59
58
#OBS.
BELOW
DETECTION
LIMIT
18
15
9
55
53
54

GEOMETRIC
MEAN
0.667
0.674
0.880
0.299
0.309
0.299
STANDARD
GEOMETRIC
DEVIATION
2.20
1.95
2.00
1.22
1.28
1.08


MINIMUM
< 0.26
< 0.26
< 0.24
< 0.24
< 0.15
< 0.24


MAXIMUM
3.44
2.39
2.45
0.84
0.94
0.39
340
204
0.463
1.98
< 0.15
3.44
              It is of interest to note the low number of observations
              at Site 3 (Beaver Bay) that were below the detection limit
              of the X-ray diffraction analysis.  This might well suggest
              the presence of an amphibole source near the sampling station.
              Note that the average and maximum values compare favorably
              with Sites 1 and 2.  During the course of the survey, several
              parties to the study expressed the opinion that the Beaver
              Bay location was subject to fugitive dust from the construction
              nearby and from tailings used in previous years for snow and
              ice control on the nearby road surfaces (see site description
              on page 7).  The X-ray diffraction data tends to confirm that
              a bias may exist.  Comparable statistics for the amphibole
              fiber count data are described in Table 9.


                                TABLE 9


            AMPHIBOLE FIBER SUMMARY STATISTICS, fibers/m3
           #OBS.

           BELOW

         DETECTION

 #OBS.     LIMIT
1
2
3
4
5
6
10
9
9
10
10
9
0
0
0
0
1
0

GEOMETRIC
MEAN
4332
5457
10100
2059
1572
1055
STANDARD
GEOMETRIC
DEVIATION
4.21
2.11
1.45
3.53
2.54
2.32


MINIMUM
200
2000
5000
200
<200
200


MAXIMUM
21000
14500
14000
14000
4000
3000
  57
                3017
                 3.42
                 200
                 21000

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                       - 23 -


        Again it is noted that the highest mean value of fibers
        is at Site 3.  It is also of interest that the standard
        deviation is relatively low indicating lesser variability
        in the data.  This would tend to confirm the presence of
        a local amphibole source.  The average background levels
        of amphibole fibers for Silver Bay, considering Sites 1 and
        2, are approximately 5000 fibers/m3.   Considering the inher-
        ent analytical error in electron microscopy of about 50%,
        the background level for Silver Bay is 7500 fibers/m3.
        The annual statistics estimated from these sets of data,
        maximum and second maximum values are described in Table 10.
        The data for certain of the stations are grouped together to
        estimate maximum and second maximum 72 hour average fiber
        levels.  For Silver Bay, the data for Sites 1 and 2 are summa-
        rized in total to estimate the second maximum 72 hour back-
        ground level not to be exceeded more than once per year.  The
        data at Site 3 in Beaver Bay are treated individually.  To
        estimate the second maximum 72 hour background level adjacent
        to the disposal site which should not be exceeded more than
        once per year, the data for Stations 4, 5 and 6 are summarized
        together.
                              TABLE 10


             PROJECTED ANNUAL STATISTICS, AMPHIBOLE FIBERS


                                           AMPHIBOLE FIBERS/m3
LOCATION


   1


   2


   3


   4
   5
   6


TOTAL
AMPHIBOLE MASS (ug/m3)

             SECOND
 MAXIMUM     MAXIMUM
  4.38
  5.26
  .495
  2.70
3.37
4.10
.463
2.11
             MAXIMUM
91010
26,300
 21917
72,000
          SECOND
          MAXIMUM
60422
23,000
 15110
46,300
        Correlation coefficients were calculated for each site and

        in total relating the X-ray diffraction mass analysis and
        the fiber count for each of the randomly selected samples.
        It is important to emphasize that the levels of fibers are
        relatively low during the background period.  As a result,
        most of the mass data, particularly at Sites 4, 5 and 6 are
        near or below the detectable limit.  The relationship between
        the data sets are depicted in Table 11.

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                                  - 24 -


                                    TABLE 11


               CORRELATION BETWEEN THE AMPHIBOLE MASS AND FIBER DATA


      LOCATION     #OBS.     #OBS.  
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                                 - 25 -



                              TABLE 12 (CONT'D)


                              SUMMARY OF ANOVA


DATA TYPE          STATIONS                  RESULTS OF TEST


 Fiber              1>2,3 vs.      Reject Ho, station sets are significantly
                    4,5,6          different.


        In the analysis of variance, the means of the data for each station
        are evaluated for differences as compared to other stations or sets
        of stations.  The test is made against the hypothesis that the means
        are equal.  In this evaluation, one can be 95% confident of the test
        results.


    c.  Wind Data.


        In this interim report, no attempt was made to relate levels of
        pollution with emission sources because no specific source of
        amphibole fibers or particulate was in operation during this period.
        The average one hour values of wind direction and speed collected
        at the Reserve office were summarized and are described in Figure 3
        as a wind rose. The frequency distribution is also tabulated in
        Appendix H. During this period prevailing wind directions were from
        the northwest.


7.  CONCLUSIONS


    a.  Suspended Particulate


        (1)  Background levels of suspended particulate are very low in
             comparison to the air quality standards.


        (2)  As measured at Sites 1 and 2, the background level of particu-
             late in Silver Bay is 16 ug/m^.  Near the tailings basin,
             Milepost 7, the background level is 10 ug/m^.


        (3)  Construction at Milepost 7 had minimal impact on the levels
             of particulate during the period of the background study.


    b.  Amphibole Fibers.


        (1)  Background levels of amphibole fibers are low, at or near
             the detection limit of the X-ray diffraction analytical
             technique .


        (2)  As measured at Sites 1 and 2 and considering the error of + 50%
             inherent in electron microscopy, the background level of amphibole
             fibers in Silver Bay is 7,500 fibers/m^.  Near the tailings basin,
             Milepost 7, the background level is estimated at 3,000 fibers/m-*.
             Second maximum 72 hour average background levels of fibers are
             estimated as 60,000 fibers/m^ in Silver Bay and 15,000 fibers/m3
             near the tailings basin.

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                                            - 26 -

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                        - 27 -
(3)   Present techniques  in X-ray diffraction analysis  are not
     sufficiently sensitive to be used as a surrogate  for
     electron microscope analyis of amphibole fibers when the
     Reserve Mining Company beneficiation plant  is  not operating
     However, the presence of low mass concentrations  as  measured
     by X-ray diffraction does indicate that the levels of fibers
     are correspondingly low.

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                 APPENDIX A





     MINNESOTA POLLUTION CONTROL AGENCY


SUSPENDED PARTICULATE DATA ANALYSIS PROCEDURE

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                                   -  28  -


                   High Volume Data Analysis Procedure





1.    General


     The high volume data analysis procedure details the steps involved in
data handling from ordering the filters to final editing of data.  Particulate
concentration determinations are described in the Attachment.


2.    Equipment


     Clean filters


     Laboratory Data Sheet for clean, weighed filters


     Stamped envelope


     Form DA#5, Filter Distribution Log


     Form DA#1, Hi-Vol Filter Log Sheet


     Form DA#6, High Volume Motor Calibration Curve


     Form DA#7, High Volume Sample Coding Sheet


     Form DA#3, Coding Log Sheet


     Form DA#4, Laboratory Sample and Accounting Record


3.    Procedure
 »                a.   Filters  are  ordered by Air Monitoring Unit.


                  b.   Clean, boxed filters  are  taken  to  the lab  by  Data  Analysis  Unit


 I                    (usually semi-annually).


                  c.   Each month,  the  lab processes clean  filters required  for  the  next


 |                    month's  operation  as  follows:


 •                    (1)  The clean filters are removed from  the box  and the identifying


                           number,  which is stamped on both sides of the filter,  is typed


 •                         using a teletype into the  computer.


                      (2)  The filter  is weighed on the  electronic  balance  to get the


 I                         tare weight.
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(3)   The filter number and the corresponding tare weight along with


     temperature and relative humidity are stored by the computer.


     Standard weights are used to check the balance before weighing
•

                           and 10% of the filters are reweighed for quality control.

•                    (4)   When the entire box of filters has been weighed, all filters

                           and two copies of the data sheet containing each filter's

|                         identifying number, tare,  weight and the lab humidity,  temperature

•                         and quality control data are placed in the box.   The laboratory

                           also retains a copy of the filter tare weight data.

•               d.    The  Data Analysis Unit retrieves the clean, weighed filters  from the

                      laboratory and provides the Quality Assurance Unit with one  copy of

•                    the  data sheet.

•               e.    Data Analysis prepares sample envelopes (without clasps)  by  stamping

                      a 9" x 12" manila envelope with a rubber stamp.  The  stamp has  spaces

•                    for  recording tare weight, loaded weight, filter number,  date and

                      site of run, start and end time of run and start and  end  flow.

•               f.    Data Analysis removes each individual filter from the box, package

•                    it in a sample envelope, and records the filter number and tare

                      weight in the spaces provided on the sample envelope.

•               g.    Clean filters are provided to the operators as follows:

                      (1)   Metropolitan sampling - site operators secure filters from

•i                         Data Analysis Section as they are needed.

•                    (2)   Outstate sampling - enough clean filters to sustain  the next

                           month's sampling are mailed or dispatched with MPCA  air monitoring

•                         personnel monthly.




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                      (3)  Local agencies - currently purchase and use their own  filters.
I                    (4)  Form DA#5 is completed as the filters are dispatched.  As  the
•                         log sheet is completed it is sequentially assigned a page  number
                           in the upper right corner and the  sheet is filed in the  log book.
•                         Form DA#5 identifies where the filters are dispatched.
                 h.   High volume sample is run, starting and ending flow, sampling site
•                    and data, and starting and ending time  are recorded on the  sample
•                    envelope; the folded filter and transducer chart if used are  placed
                      in the sample envelope.
•               i.   Samples are returned to the MPCA as follows:
                      a)   Outstate monitors - samples are mailed back to the Data Analysis
•                         Unit on a sample-by-sample basis.
•                    b)   Metropolitan area samples are returned to the Data Analysis Unit
                           as they are run.
•               j.   As samples are returned from  the field, date of run, site of  run,
                      and filter number are recorded on the Hi-Vol Filter Log Sheet (Form
•                    DA#1, 1-15-76).  Sample exposure time (minutes) is calculated from
•                    the starting and ending times on the sample envelope.  Filters  are
                      visually inspected for holes, flows out of range or other conditions
•                    which invalidate the sample.  Filters are also checked to be  sure
_                    that the ID number of the filter matches that recorded on the sample
"                    envelope.  Form DA#1 is reviewed to be  sure that a sample from  the
•                    site and date has not previously been received.  Inconsistencies
                      from these checks are recorded on Form  DA#1; 1-15-76.  If the filter
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                                               - 31 -



                      validity is questioned and if the  filter  is not  invalidated  for
                      physical reasons an attempt  is made  to correct data believed  to


                      be in error  (e.g., to determine on what date a filter actually


                      ran in the case of a duplicate site  and date).


•                    If the filter was physically damaged an error code is assigned to


                      the sample and recorded on the log sheet  (Form DA#1; 1-15-76).   If


I                    physical damage appears to be consistent  from a particulate site,


                      the site and nature of the problem are reported to the Air Monitoring


                      Unit.


•                    The error codes include:


                      - 1 — no analysis


I                    - 2 — PGA


•                    - 3 — laboratory

                      - 4 — operator

•                    - 5 — vandalism


                      - 6 — natural (rain, wind)


•                    - 7 — equipment failure

•                    - 8 — generated by computer, quality assurance

                      The laboratory may assign codes - 2  or -  3; operators may assign any

•                    code except  -3 or -8; -8  is a quality  assurance code and can only

                      be assigned  by the computer.

^                    If the sample appears to be valid but is  excessively loaded,  the


•                    Engineering  and Enforcement  Sections are  notified.





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                              .            .
                       Along with  logging  in the  filters,  site number,  date of run,  tare
                       weight  and  calculated exposure  time in minutes  are  recorded on
                       Hi-Vol  DATA Form DA#7 ;  3-16-76.   True  flow rate  is  determined by
 _

                       averaging  the  starting  flow and  ending  flow logged  on the  sample

 •                     envelope.   This  average number is  then  located  on the appropriate

                       high  volume motor  calibration curve  (DA#6;  1-16-76).


                       Each  page  of data  form  DA#7 is sequentially assigned  a sheet number

 I                     (starting  value  is taken from the  last  coding sheet log form DA#3 ;

                       1-15-76).   This  sheet number is  also logged on  the  high volume filter

 |                     log sheet  (DA#1; 1-15-76).

 _                k.    On Tuesday and Friday mornings all data sheets  (DA  Form #7;  3-16-76)

                       which are  ready  to be sent  to the  laboratory are  logged (by  date)

 I                     on the coding  sheet log (DA#3; 1-15-76).   The sheet number of each

                       coding sheet used  and the date the coding sheets  and  corresponding

 |                     filters will be  taken to the laboratory are logged  in the  appropriate

 •                     columns of the coding sheet log  and  a description of  "high volume

                       samples" is entered in  the  description  column.

 •                     Data  sheet page  numbers and total  number of filters are logged on a

                       laboratory sign-in sheet (DA#4;  1-15-76).   This form  is filled out

 I
in duplicate and the laboratory must sign for the samples; the

laboratory keeps one copy and the other is returned to MPCA.

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                 1.   On Tuesday and Friday afternoons all coding sheets logged to the


                      laboratory along with corresponding filters are taken to the


                      laboratory.
•


                      The laboratory acknowledges the receipt of the filters and coding


•                    forms by signing the laboratory sign-in sheet (DA#4;  1-15-75).


                 m.    The laboratory weighs the loaded filters on the electronic balance;


•
                      standard weights and 10% audit samples are also weighed. The laboratory


•                    provides two computer printouts of the results.


                 n.   Data Analysis retreives all data sheets completed by the laboratory


I                    and logs the data returned in the "Date From Lab" column of the


                      coding sheet log (DA#3) for that coding sheet page number.  One of


•                    the two copies is sent to Quality Assurance.  In addition all data


•                    sheets which have been in the lab more than 3 weeks are reported


                      to Quality Assurance.


I               o.   Local agencies send MPCA completed coding sheets.


                 p.   Data sheets are manually edited to remove irregularities in coding


•                    and reporting of data.  Invalidated data points are checked and


B                    assigned an appropriate error code.


                 q.   All coding sheets which have been completed and edited are logged


•                    out to keypunch in the "DATE TO" column of the coding sheet log for


_                    that coding sheet page number (DA#3) and are taken to keypunch on


                      Tuesday and Friday afternoons .



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                                               - 34 -

                 r.   All data sheets  (DA#7) are keypunched on given  stripped cards.
|               s.   All keypunched cards and the corresponding data sheets  (DA#7) are
•                    retreived from keypunch, returned to the MPCA,  and  the date
                      returned is logged on the keypunch "DATE FROM"  column for  that
•                    coding sheet page number on the coding  sheet  log  (DA#3; 1-15-76).
                 t.   Form DA#1 is checked to indicated that  the filter has been returned
•                    to MPCA and Form DA#1 is then filed by  site and date.
•               u.   Keypunched cards are edited via the PDP8/E computer.  Edit checks
                      are made for illegal characters on the  card,  date within specified
•                    range, number of parameters must be equal to  7, time between 1320
                      and 1560 minutes (22 and 26 hours), flow between  32 and 72 cfm,
•                    tare weight between 3 and 5 grams, total weight between the tare weight
•                    and 5 grams, and calculated high volume results betwen 5 and 300
                      ug/m^.  The card and calculated results are printed out on the  line
I                    printer, errors  are flagged with the work "check".  Calculated
_                    results in excess of 150 ug/m3 are single starred,  and those in
™                    excess of 260 ug/nP are doubled starred.  A detailed list  of all
I                    cards in error and appropriate error messages are printed  out on
                      the console teletype.
I               v.   Keypunch errors  are corrected as found.  Coding of values  in error
_                    is verified, and if possible, corrected.  A listing of results  for
                      each local agency is dispatched to that agency  for  error checking
•                    and result verification.  An attempt is made  to correct every error,
                      if possible, or  if not possible to assign an  appropriate error  code.
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                                   -  35  -


                           Particulate Matter
1.    TARE WEIGHT


     Determine the tare weights of the clean,  numbered 8" x 10" glass fiber
 I
                  filters.   This is to be done only after the relative humidity in the

 •                laboratory has been under 50% for at least 24-hours.

             2.    GROSS WEIGHT

 •                a.    Allow a dessication period of 24-hours during which the R.H. is below

 •                     50% after the exposed filters are brought into the lab before final

                       weighing.

 •                b.    Inspect filters for holes, missing pieces of filter, loading extending

                       beyond margins and over the filter edge, and record as an invalid

 •                     sample any filter with one or more of the above defects.

 •                c.    Weigh to the nearest .1 mg and record.

             3.    QUALITY CONTROL


 I
     a.    Precision
•                     (1)  At least 10% of each box of 100 clean numbered, tare weighted


                            filters are independently reweighed.


•                     (2)  At least 5% of each batch of filters which are weighed for


                            total weight are independently reweighed.


                  b.    Accuracy


•                     (1)  Weights which have been calibrated with Class S weights are


                            used to check and adjust the balance prior to and after each


•                          batch weighing.


                       (2)  In addition, a polonium  source is  used to retard the effects of


™                          static charge on the filters.



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•                                                                          Attachment

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             APPENDIX  B
OPERATION AND SERVICE OF  THE  NETWORK

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             -  36  -
OPERATION AND SERVICE OF THE NETWORK
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             1.   MEMBRANE SAMPLERS - 72 hour samples.
•                a.   General - During each visit to a site -
•                     (1)  Check time indicator and record data.
                       (2)  Zero the magnehelic gage (right hand bottom).
•                     (3)  Push left hand button to obtain reading and record the
                            "flow" obtained.
™                b.   Changing Filters - every 72 hours
I                     (1)  Zero the magnehelic gage.
                       (2)  Push "READ" button and record the "flow".
•                     (3)  Pull monitor and time indicator plug.
_                     (4)  Read time indicator and record.
•                     (5)  Remove "Coolie Hat".
I                     (6)  Remove the three "finger-nuts".
                       (7)  Lift off the "3-point" hold down plate.
I                     (8)  Remove thick teflon washer - DO NOT LOSE  IT
_                     (9)  Using telfon coated tweezers, carefully remove  the filter
™                          and place in appropriate petri dish.   Do  not  disturb  the
I                          thin teflon washer under the filter.
                       (10) Using the tweezers/forceps, obtain a numbered filter  (the
•                          number being properly recorded in the  record  book and record
_                          sheets) and carefully place on top of  the thin  teflon washer,
™                          Now place the  thick teflon washer on top  of the filter.
I                     (11) Replace the 3-point hold down plate.

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- 37 -
                      (12)  Replace the 3-finger/thumb nuts and tighten securely.
                      (13)  Replace "Coolie Hat".


•                    (14)  Record the last time indicator data (end of previous sample)


                           as the "start" of the new sample run of 72-hours.


•                    (15)  Plug unit and timer into electric service box.


•                    (16)  After about 2-5 minutes push zero button.


                      (17)  Push read button and record observation as start of new


•                         sample run of 72-hours.


                      (18)  Ensure that the petri dish is properly identified and taped


I                         closed.


•                    (19)  Completely fill out record sheet and retain with petri dish.


            2.   HIGH VOLUME SAMPLERS - 24-hour samples.


I               a'   Use of Hi-Vol Filter Cartridge


                      (1)  Remove cover from cartridge; each cover is identified by


I                         site number, there are 12 cartridges - 2 per site.


•                    (2)  Lay cartridge flat.


                      (3)  Remove cover.


•                    (4)  Remove the 2 thumb nuts.


                      (5)  Lift off the hold-down plate or frame.


m                    (6)  Carefully remove a numbered filter from the large brown


•                         envelope.


                      (7)  Place filter on support screen - align carefully.


I                    (8)  Replace the hold-down plate or frame.


                      (9)  Secure the hold-down plate with the thumb nuts.

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(10) Replace
(11) Record
record

- 38 -

the cover.
the filter number in the log book and on the
sheet .
b. Replacing Filter Cartridges in the Field
(1) Open Hi-Vol - lift up the roof.

(2) Loosen
(3) Lift up

the 4-wing nuts that hold a cartridge in place.
the filter cartridge containing the exposed filter.
(4) Place the cover (one appropriately marked as to site number)
1
1

1

1
1

1

1
1

1
1
1
1
on the
( 5 ) Remove
filter.
(6) Put the
(7) Loosen
cartridge .
the cover from the cartridge containing an unexposed

cartridge in position and secure via the 4-wing nuts.
the 2-finger/ thumb nuts on the cartridge, then turn
the Hi-Vol on for only a few seconds to set the filter and
thus avoiding "cracking" of the filter, secure the 2 finger/


thumb nuts during the few seconds of operation.
(8) Secure
of the
the 4-wing nuts. This requires additional securing
2 finger /thumb nuts.
c. Replacing Transducer Chart
( 1 ) Remove
chart ,
has the



transducer chart - push lever to raise pen off the
carefully remove the chart and ensure that the chart
site number on the back.




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                                               - 39 -
I                     (2)  Insert new chart, use a coin or screw driver by inserting


                            it in the notch of  the center "bolt" head and rotate


|                          clockwise until the penpoint rests at midnight -  lower


_                          the pen on to  the paper keeping the lever or lift bar off


                            of or away from the chart.  Ensure that the penpoint rests


•                          on "zero" and midnight.


                  d.   Programmer Unit


|                     Check clock in the  programmer unit to ensure it is operating


_                correctly.  Then flip down the switch (day) that was just sampled.


                  Flip up the day switch  for the next sampling day which must be 3 days


•                later or  after the last  sampling day.


                  e.   Operation


I                     Close the entire unit.   It will automatically turn on  at midnight


M                (or 0000  hours) and shut off  at midnight (2400 hours) on the day on


                  which sampling is scheduled.
                   f.    Sample  Handling


                        (1)  Fill  in  completely  the "particulate record  sheet".  Do this


                            at the office  and attach  the data  sheet  to  the  folder.


•                       (2)  Carefully disassemble the  filter cartridge  and  remove the


                            filter placing it in the  appropriate  type of  folder and


•                           fold  length-wise.


•                       (3)  Insert the  folder (and filter)  in  a large white envelope.


                            Also  include the particulate record sheet and transducer


•                           chart ; but, do not  put these in the folder, just  in the


                            envelope.   Seal the envelope.
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(4)



- 40 -
Fill in the appropriate and available information on the

large brown envelope.

3. WEATHER STATION
a. Min

- Max Thermometer - At Reserve Office located in white shelter

(record daily at 12:00 a.m.).
1



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(1)


(2)



Max. - Read and record, then unlock and spin clockwise until
below temperature just recorded. Then set into locked position.

Min. - Read and record, then turn so bulb is almost vertical and
let column of mercury go past the previously recorded maximum
temperature that was read, then set in position with red bulb
slightly below the horizontal.
b. Hygrothermograph - Changing of Chart

(1)
(2)
(3)
(4)
(5)

(6)
(7)
(8)
(9)
(10)


(11)



Lift up case (cover) - release the latch on right hand site.
Use the lever to lift pens from chart.
Inside top of drum is a thumb-nut, remove it.
Lift up the drum and wind the clock mechanism.
Release the metal strip that holds the chart against the drum.

Remove the chart and place in folder.
Mark date on margin of new chart.

Place chart on drum - overlapping as required.
Insert the metal clip.
Carefully put the drum back into position. Ensure that the

day and time at point where pens rest on chart is correct.
Replace the thumb nut.



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                                -  41  -
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                   (12)   Release the pens.
•                 (13)   Put cover/case back into position.
               c.   Psychrometer - Located with wind system recorder in Reserve Office
•                 (record daily at 12:00 a.m.).
•                 (1)   Wet the sock.
                   (2)   Take unit outside and spin for 2-3 minutes or until wet bulb
•                      reading stabilizes.
                   (3)   Read wet and dry bulb temperatures and record.
™                 (4)   Subtract the "wet" reading from the "dry" reading.
•                 (5)   Using the chart find the "dry" temperature - far left column.
                   (6)   At top of table or chart find the column corresponding to the
•                      "difference" between the "wet" and "dry" bulb temperatures.
                   (7)   Read chart where the "dry" temperature and "difference"
•                      intersect.  This is the relative humidity.  Record in log.
I             d.   Barometric Pressure - obtain barometric pressure on arrival at

I
_                 (1)   Check wind sets for proper trace recording.
™                 (2)   Annotate date and time on chart.

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    Reserve Office .

e.  Wind sets - Reserve Office and Site #5.

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    APPENDIX C




PRODUCTION RATES

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- 42 -

RESERVE MINING COMPANY

= 4'*4 SILVER BAY, MINNESOTA

January 17, 1978


Mr. Gerald F. Regan, Chief
Air Surveillance Branch
United States Environmental
Protection Agency
Region V
230 South Dearborn Street
Chicago, Illinois 60604
Dear Mr. Regan:

55614












In response to Mr. Charles Miller's telephone call
and your January 10, 1978, letter, I am

the information you requested regarding
production.
^^.
Sincerely,/?^
X /S
&6&h^
(_^ ^ —
Edward Schrnid
Assistant to
ES/p
Enclosure

&ECFW

PA REGION V

attaching

our rate of
= 	 "\
0
' /
--7'^-1 — ^—&(.^^'

the President



rE
~
ANCH
i


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                                     - 43 -


                        RESERVE MINING COMPANY

                              MEMORANDUM
        Edward Schmid
        Industrial Engineering
                                           DATE  January 11, 1978
FROM.
SUBJECT.
        Production Level Comparison  (1970 vs. 1977)
        Following is the information per your request of January 10,
        1978, utilizing Reserve's full productive capacity  (as demon-
        strated in the year of 1970) as base for comparison with 1977
        production level.

                   Total Tons    No.Opera-  Avg.Tons/   Per Cent
                   Pellets(Dry)  ting Days  Op. Day     Production
Date

1970           10,434,758

1977 1/2-6/25   4,482,476
                                  362.33     28,799      lOO.OO(Base)

                                  166        27,003       93.76

            June 26 thru July 30  (scheduled plant shutdown)0.00

    July 31             9,418       1         9,418       32.70

            August 1 thru December 5  (no production or     0.00
                                      shipment due to strike)
    Dec. 6-15          73,231      10

    Dec. 16-23        174,279       8

    Dec. 24-25 (Holiday shutdown)

    Dec. 26-31        143,640       6
                                          7,323


                                         21,785




                                         23,940
25.43

75.64


 0.00

83.13

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Dec. 6,
7
8
9
10
11
12
13
lU
15

16
17
18
19
20
21
22
23
26
27
28
29
30
31
*28,799



- 44 -
SUPPLEMENTAL. INFORMATION

Total
Tons Pellets

1977
2,9^1
6,170
10,529
7,295
12 ,"162
11,836
11,395
10,903
(Power House repairs and plant start-up
12,263
.1U,108
20,998
27,263
25,359
22,87^
27,063
2U,351
(2Uth and 25th Christmas Holiday)
11,225
27,k21
26,193
22,U76
27,8UU
28,U75

tons/operating day = base 100






Per Cent
Production*

™
10.21
21. U2
36.56
25.33
te.23
Ul.10
39.57
37.86
problems)
U2.58
48.99
72.91
9^.67
88.06
79.^3
93.97
8U.56
38.98
95. 2U
90.95
78. oU
96.68
98.87




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APPENDIX D
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                          TOTAL  SUSPENDED PARTICULATE DATA SHEETS ug/m3
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                              - 45  -


                 TOTAL SUSPENDED PARTICULATES


              June 18, 1977 - December 12, 1978



Date        Campton    Kelly    Holiday   Reserve #11   Nelson    Reserve #8
June
ii
July
ii
ii
ii
ii
ii
ti
n
ti
n
Aug.
ii
n
ii
ii
n
n
ii
n
n
Sept.
n
ii
n
ii
it
ii
n
ii
ii
Oct.
ii
n
n
ii
M
n
M
II
M
II
27
30
3
6
9
12
15
18
21
24
27
30
2
5
8
11
14
17
20
23
26
29
1
4
7
10
13
16
19
22
25
28
1
4
7
10
13
16
19
22
25
28
31
27
13
26
25
10
17
23
29
20
-
41
18
20
-
-
-
-
9
8
-
20
16
-
10
9
10
-
20
2
10
-
15
6
27
-
8
36
17
25
5
28
57
27
31
15
28
21
13
21
23
36
19
35
37
15
22
-
-
20
-
11
12
-
23
21
13
9
13
14
18
29
1
9
8
23
13
28
11
16
37
31
31
16
29
43
29
32
19
39
21
15
25
28
22
21
33
49
15
27
-
-
-
22
37
8
70
18
17
28
23
10
-
28
23
1
9
6
25
9
34
11
11
37
25
30
19
42
27
27
19
10
21
16
6
14
13
18
11
25
30
8
9
12
8
-
5
8
6
7
22
-
8
7
9
-
11
17
2
6
4
9
7
20
4
5
-
13
13
4
25
22
22
19
12
21
16
8
17
15
-
15
29
38
8
12
11
2
-
-
8
6
7
24
7
-
7
8
-
11
13
1
5
5
11
3
18
5
5
15
10
5
3
22
15
22
19
14
21
19
7
12
14
18
11
22
35
12
11
-
-
15
-
8
8
7
22
24
11
11
-
9
12
17
2
7
3
8
3
18
-
4
14
10
6
3
25
13
22

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                              - 46 -

              TOTAL SUSPENDED PARTICIPATES  (Cont'd)

                June 18, 1977 - December 12,  1978


Date        Campton    Kelly     Holiday    Reserve #11    Nelson    Reserve  #8

Nov.   3       21        25        35          17            15           15
 11     6        9        11         9           7             5            6
       9       14        17        16          12            10           13
 11    12        7        12        18           -             2            3
      15       36        37        44          33            34           31
      18        3        11        23           4             -            2
      21       15-28           -            17           15
 "    24        7        24        14           -             6            7
      27        7        13        14           5            47            4
 "    30       24        23        27          20            20           21

Dec.   3        9        18        30           8            4            5
 "     6        2         8        11           4            2            1

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APPENDIX E
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                                 X-RAY DIFFRACTION ANALYSIS, AMPHIBOLE
 •                                  MASS CONCENTRATION (ug/m3)
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- 47 -
X-RAY DIFFRACTION ANALYSIS


Date
6/26/77
6/26/77
6/26/77
6/26/77
6/26/77
6/26/77
6/29/77
6/29/77
6/29/77
6/29/77
6/29/77
6/29/77
7/2/77
7/2/77
7/2/77
7/2/77
7/2/77
7/2/77
7/5/77
7/5/77
7/5/77
7/5/77
7/5/77
7/5/77
7/8/77
7/8/77
7/8/77
7/8/77
7/8/77
7/8/77
7/11/77
7/11/77
7/11/77
7/11/77
7/11/77
7/11/77
7/14/77
7/14/77
7/14/77
7/14/77
7/14/77
7/14/77



Filter
#
0118
0119
0120
0121
0122
0123
0124
0125
0126
0127
0128
0129
0130
0131
0132
0133
0134
0135
0136
0137
0138
0139
0140
0141
0143
0144
0145
0146
0147
0148
0149
0150
0151
0152
0153
0154
0155
0156
0157
0158
0159
0160



Sampling
Site #
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6



Flow
(cfm)
3.9
3.5
3.7
3.7
3.6
3.8
3.7
3.5
3.6
3.7
3.8
3.8
3.6
3.4
3.6
3.9
3.7
3.8
3.8
3.5
3.8
4.0
3.8
4.0
4.0
3.6
4.0
3.9
4.0
3.7
4.3
3.8
4.3
4.2
4.3
4.2
4.3
3.8
4.2
4.0
4.0
3.9



Time
(hours)
72.1
72.1
72.2
71.9
72.0
71.8
71.9
71.9
71.9
72.1
72.0
71.9
71.9
72.0
71.8
71.7
71.8
71.8
71.8
72.0
58.0
71.9
72.0
71.8
71.9
71.9
71.9
71.8
71.8
71.8
71.9
71.7
71.8
71.7
71.9
71.8
71.7
71.9
71.9
71.9
71.9
72.1



Amphibole Cone.
(ug/m3)
1.60
1.45
2.29
<.31
<.32
<.30
1.10
<.32
1.26
<.31
<.30
<.30
.95
<.33
.95
<.29
<.31
<.30
1.07
.65
1.29
<.28
<.30
<.28
<.28
.80
2.13
<.29
<.28
<.31
.66
.75
.66
<.27
<.26
<.27
2.38
1.34
1.49
<.28
<.28
<.29



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- 48 -
X-RAY DIFFRACTION ANALYSIS


Date
7/17/77
7/17/77
7/17/77
7/17/77
7/17/77
7/17/77
7/20/77
7/20/77
7/20/77
7/20/77
7/20/77
7/20/77
7/23/77
7/23/77
7/23/77
7/23/77
7/23/77
7/23/77
7/26/77
7/26/77
7/26/77
7/26/77
7/26/77
7/26/77
7/29/77
7/29/77
7/29/77
7/29/77
7/29/77
7/29/77
8/1/77
8/1/77
8/1/77
8/1/77
8/1/77
8/1/77
8/4/77
8/4/77
8/4/77
8/4/77
8/4/77
8/4/77



Filter
#
0162
0163
0164
0165
0166
0167
0168
0169
0170
0171
0172
0173
0174
0175
0176
0177
0178
0179
0180
0181
0182
0183
0184
0185
0186
0187
0188
0189
0190
0191
0192
0193
0194
0195
0196
0197
0198
0199
0200
0201
0202
0203



Sampling
Site#
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
•5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6



Flow
(cfm)
4.1
3.8
4.1
4.0
4.0
4.2
4.1
3.9
4.3
4.2
4.2
4.1
4.0
3.6
4.0
3.9
4.0
4.0
4.0
3.6
4.0
4.0
3.9
3.9
3.8
3.4
3.7
3.8
3.6
3.7
3.8
3.5
3.8
3.8
3.5
3.3
3.9
3.6
3.9
3.9
3.9
3.8



Time
(hours )
71.9
71.9
71.9
71.8
71.9
71.8
72.2
71.4
71.8
71.8
71.6
71.8
71.8
72.5
72.1
72.1
72.0
71.9
71.2
71.2
71.2
71.2
71.3
71.3
72.2
72.2
72.3
70.4
70.6
72.5
71.5
71.5
71.4
71.2
71.1
71.0
72.9
72.9
72.9
72.8
76.8
72.8



Amphibole Cone.
(ug/m3
2.62
2.39
1.25
<.28
<.28
<.27
2.07
1.46
1.32
<.27
<.27
<.27
<.28
1.27
<.29
<.28
<.28
3.44
1.43
1.88
<.29
<.29
<.29
<.30
<.33
<.30
<.30
<.32
<.30
.90
.65
1.50
<.30
<.33
<.35
1.15
1.40
1.00
<.28
<.27
<.29



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             - 49 -
X-RAY DIFFRACTION ANALYSIS
Date
8/7/77
8/7/77
8/7/77
8/7/77
8/7/77
8/7/77
8/10/77
8/10/77
8/10/77
8/10/77
8/10/77
8/10/77
8/13/77
8/13/77
8/13/77
8/13/77
8/13/77
8/13/77
8/16/77
8/16/77
8/16/77
8/16/77
8/16/77
8/16/77
8/19/77
8/19/77
8/19/77
8/19/77
8/19/77
8/19/77
8/22/77
8/22/77
8/22/77
8/22/77
8/22/77
8/22/77
8/25/77
8/25/77
8/25/77
8/25/77
8/25/77
8/25/77
Filter
#
0204
0205
0206
0207
0208
0209
0210
0211
0212
0213
0214
0215
0216
0217
0218
0219
0220
0221
0222
0223
0224
0225
0226
0227
0228
0229
0230
0231
0232
0233
0234
0235
0236
0237
0238
0239
0240
0241
0242
0243
0244
0245
Sampling
Site #
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
Flow
(cfm)
3.9
3.5
-
3.9
3.4
3.8
3.6
3.5
3.6
3.7
3.4
3.8
3.6
3.6
4.1
4.0
3.7
3.8
3.8
3.6
4.0
3.9
3.7
4.0
3.9
-
3.7
3.6
3.5
3.7
3.7
3.6
4.0
4.0
3.7
4.0
3.8
3.5
4.0
3.8
3.6
4.0
Time
(hours)
72.1
71.9
71.8
71.6
68.5
71.8
71.9
72.8
72.0
71.9
71.9
70.4
73.1
72.5
73.3
73.3
73.3
73.3
70.0
69.9
70.0
69.9
70.0
69.9
71.8
23.9
71.9
71.8
71.9
67.8
71.9
71.8
71.8
71.6
71.7
51.9
73.1
73.1
73.1
73.0
73.1
72.9
Amphibole Cone.
(ug/m3
.72
.97
-
< .29
< .35
< .30
< .31
.64
2.36
< .31
.67
< .31
1.08
1.56
.95
< .28
< .29
< .29
.77
< .32
1.16
.45
< .31
.29
.73
-
1.53
< .32
.49
< .32
.77
1.10
1.85
< .28
< .31
< .39
< .39
.80
1.67
< .29
< .31
< .28

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- 50 -
X-RAY DIFFRACTION ANALYSIS


Date
8/28/77
8/28/77
8/28/77
8/28/77
8/28/77
8/28/77
8/31/77
8/31/77
8/31/77
8/31/77
8/31/77
8/31/77
9/3/77
9/3/77
9/3/77
9/3/77
9/3/77
9/3/77
9/6/77
9/6/77
9/6/77
9/6/77
9/6/77
9/6/77
9/9/77
9/9/77
9/9/77
9/9/77
9/9/77
9/9/77
9/12/77
9/12/77
9/12/77
9/12/77
9/12/77
9/12/77
9/15/77
9/15/77
9/15/77
9/15/77
9/15/77
9/15/77



Filter
#
0246
0247
0248*
0249
0250
0251
0252
0253
0254
0255
0256
0257
0258
0259
0260
0261
0262
0263
0264
0265
0266
0267
0268
0269
0270
0271
0272
0273
0274
0275
0276
0277
0278
0279
0280
0281
0282
0283
0284
0285
0286
0287



Sampling
Site #
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6



Flow
(cfm)
3.9
3.5
4.0
3.9
3.6
3.8
3.8
3.4
4.0
3.9
3.7
3.9
3.8
3.9
3.9
3.6
3.8
3.9
4.0
3.9
4.0
3.8
4.0
3.7
4.0
3.9
3.9
3.5
4.0
3.6
3.9
3.9
3.8
3.5
3.9
3.6
3.9
3.8
3.8
3.7
3.8



Time
(hours)
71.1
71.0
71.3
71.4
71.4
71.5
72.9
72.8
72.6
72.5
72.5
72.5
70.8
71.2
71.2
71.1
71.2
71.6
71.6
71.4
71.4
71.3
71.3
71.4
71.5
65.5
65.5
65.5
71.5
72.4
72.4
72.4
72.2
72.3
72.4
71.9
72.0
72.0
72.1
72.1
72.1



Amphibole Cone.
(ug/m3)
.59
.66
.57
<.29
<.32
<.30
<.29
.82
1.54
<.29
<.30
<.29
<.30
1.47
<.29
<.32
<.30
<.29
.85
<.29
<.29
<.30
<.29
.46
<.28
1.11
<-31
<.36
<.28
1.90
1.44
.43
<.30
<.32
<.32
.47
2.18
1.19
<.30
.61
.30



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- 51 -
X-RAY DIFFRACTION ANALYSIS


Date
9/18/77
9/18/77
9/18/77
9/18/77
9/18/77
9/18/77
9/21/77
9/21/77
9/21/77
9/21/77
9/21/77
9/21/77
9/24/77
9/24/77
9/24/77
9/24/77
9/24/77
9/24/77
9/27/77
9/27/77
9/27/77
9/27/77
9/27/77
9/27/77
9/30/77
9/30/77
9/30/77
9/30/77
9/30/77
9/30/77
10/3/77
10/3/77
10/3/77
10/3/77
10/3/77
10/3/77
10/6/77
10/6/77
10/6/77
10/6/77
10/6/77
10/6/77



Filter
#
0288
0289
0290
0291
0292
0293
0294
0295
0296
0297
0298
0299
0300
0301
0302
0303
0304
0305
0306
0307
0308
0309
0310
0311
0312
0313
0314
0315
0316
0317
0318
0319
0320
0321
0322
0323
0324
0325
0326
0327
0328
0329



Sampling
Site #
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6



Flow
(cfm)
3.8
4.1
4.0
3.9
3.7
3.9
3.9
4.1
4.1
4.0
3.8
4.1
3.8
4.0
3.9
3.8
3.6
4.0
3.8
4.0
4.0
3.9
3.7
4.0
3.9
4.1
4.1
4.1
3.7
4.1
3.8
4.0
4.0
4.1
3.7
4.0
4.1
4.1
4.1
4.2
3.8
3.9



Time
(hours )
71.6
71.6
71.4
71.4
71.4
71.4
71.7
71.9
72.0
72.0
72.0
58.7
71.8
71.7
71.6
71.7
71.7
84.9
71.9
71.9
71.9
71.9
71.8
71.8
73.0
73.1
73.1
73.0
73.1
73.1
70.9
70.9
71.1
71.0
71.0
70.1
71.4
71.3
46.2
70.4
71.8
71.5



Amphibole Cone.
(ug/m3)
.75
<.28
.57
<.29
<.31
<.29
<.29
.41
<.28
<.28
<.30
<.34
<.30
.71
.58
<.30
<.32
<.24
.60
.85
1.13
<.29
<.31
<.28
1.43
.95
2.45
<.27
<.30
<.27
2.12
1.14
1.72
<.28
<.31
<.29
.28
.56
<.43
<.27
<.30
.29



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- 52 -
X-RAY DIFFRACTION ANALYSIS


Date
10/9/77
10/9/77
10/9/77
10/9/77
10/9/77
10/9/77
10/12/77
10/12/77
10/12/77
10/12/77
10/12/77
10/12/77
10/15/77
10/15/77
10/15/77
10/15/77
10/15/77
10/15/77
10/18/77
10/18/77
10/18/77
10/18/77
10/18/77
10/18/77
10/21/77
10/21/77
10/21/77
10/21/77
10/21/77
10/21/77
10/24/77
10/24/77
10/24/77
10/24/77
10/24/77
10/24/77
10/27/77
10/27/77
10/27/77
10/27/77
10/27/77
10/27/77



Filter
#
0330
0331
0332
0333
0334
0335
0336
0337
0338
0339
0340
0341
0342
0343
0344
0345
0346
0347
0348
0349
0350
0351
0352
0353
0354
0355
0356
0357
0358
0359
0360
0361
0362
0363
0364
0365
0366
0367
0368
0369
0370
0371



Sampling
Site #
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6



Flow
(cfm)
4.1
4.1
4.0
4.0
3.7
3.8
3.8
3.9
4.0
4.0
3.8
3.7
3.8
3.9
3.7
3.9
3.7
3.8
3.8
3.8
3.7
3.9
3.7
3.8
3.7
4.1
3.8
4.0
3.8
3.5
3.7
3.8
3.8
3.9
3.6
3.6
3.8
3.9
3.9
3.9
3.7
3.5



Time
(hours )
72.0
72.0
71.8
71.8
71.8
72.1
71.5
72.0
71.7
37.4
72.2
71.8
72.1
72.1
72.1
71.6
71.7
71.7
72.9
72.7
72.8
72.7
72.6
72.7
71.3
71.3
71.3
71.2
71.2
71.2
74.2
74.3
74.4
74.3
74.4
74.3
70.5
70.4
70.5
70.5
70.5
70.5



Amphibole Cone.
(ug/m3)
.41
.41
< .28
< .28
<.31
< .30
2.40
.72
1.70
<.54
< .30
<.31
< .30
<.29
1.38
<.29
<.31
<.30
1.77
1.33
2.27
<.29
<.30
<.29
1.08
1.39
1.35
<.29
<.33
<.33
.59
1.44
.72
<.28
<.30
<.30
3.20
2.23
1.93
.59
.94
<.33



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- 53 -
X-RAY DIFFRACTION ANALYSIS

Date
10/30/77
10/30/77
10/30/77
10/30/77
10/30/77
10/30/77
11/2/77
11/2/77
11/2/77
11/2/77
11/2/77
11/2/77
11/5/77
11/5/77
11/5/77
11/5/77
11/5/77
11/5/77
11/8/77
11/8/77
11/8/77
11/8/77
11/8/77
11/8/77
11/11/77
11/11/77
11/11/77
11/11/77
11/11/77
11/11/77
11/14/77
11/14/77
11/14/77
11/14/77
11/14/77
11/14/77
11/17/77
11/17/77
11/17/77
11/17/77
11/17/77
11/17/77



Filter
#
0372
0373
0374
0375
0376
0377
0378
0379
0380
0381
0382
0383
0384
0385
0386
0387
0388
0389
0390
0391
0392
0393
0394
0395
0396
0397
0398
0399
0400
0401
0402
0403
0404
0405
0406
0407
0408
0409
0410
0411
0412
0413



Sampling
Site*
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6



Flow
(cfm)
3.7
3.9
3.9
3.9
3.6
3.6
3.8
4.0
3.9
4.0
4.8
3.8
3.8
4.1
4.0
3.9
3.9
3.7
3.8
4.0
3.9
4.0
3.7
3.7
4.1
4.2
4.3
4.3
4.0
3.8
3.9
4.1
4.0
4.0
4.0
3.5
4.1
4.2
-
4.1
4.1
3.7



Time
(hours )
71.9
72.0
72.0
72.4
72.4
72.4
72.9
72.8
72.8
72.4
72.3
73.0
64.6
70.6
70.7
70.7
70.8
70.1
78.7
72.8
72.9
72.8
72.8
72.8
71.5
71.4
71.3
71.3
71.3
71.2
72.7
72.8
72.8
71.6
71.7
66.7
72.9
72.4
70.9
70.8
128.5
70.8



Amphibole Cone.
(ug/m3)
1.53
<.29
.87
<.29
.31
<.31
1.47
1.12
.86
<.28
<.23
<.29
<.33
<.28
.43
<.29
<.29
<.31
<.27
<.28
.57
.84
<.30
<.30
<.29
<.27
<.27
<.27
<.29
<.30
.29
.27
.28
<.28
<.28
<.34
<.27
.80
—
<.28
<.15
<.31



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          - 54 -
X-RAY DIFFRACTION ANALYSIS
Date
11/20/77
11/20/77
11/20/77
11/20/77
11/20/77
11/20/77
11/23/77
11/23/77
11/23/77
11/23/77
11/23/77
11/23/77
11/26/77
11/26/77
11/26/77
11/26/77
11/26/77
11/26/77
11/29/77
11/29/77
11/29/77
11/29/77
11/29/77
11/29/77
12/2/77
12/2/77
12/2/77
12/2/77
12/2/77
12/2/77
12/5/77
12/5/77
12/5/77
12/5/77
12/5/77
12/5/77
12/8/77
12/8/77
12/8/77
12/8/77
12/8/77
12/8/77
Filter
#
0414
0415
0416
0417
0418
0419
0420
0421
0422
0423
0424
0425
0426
0427
0428
0429
0430
0431
0432
0433
0434
0435
0436
0437
0438
0439
0440
0441
0442
0443
0444
0445
0446
0447
0448
0449
0450
0451
0452
0453
0454
0455
Sampling
Site #
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
Flow
(cfm)
4.2
4.3
4.4
4.5
-
3.5
4.3
4.3
4.5
4.4
4.1
3.8
4.1
4.3
4.6
4.5
4.0
4.1
4.2
4.5
4.6
4.4
4.2
4.1
4.1
4.5
4.2
4.5
4.0
3.8
4.3
4.3
4.3
4.3
4.0
3.6
4.4
4.4
4.4
4.2
4.0
3.8
Time
(hours )
71.1
71.7
67.5
62.5
-
73.7
72.9
72.9
72.9
72.8
72.7
72.7
72.5
71.9
70.1
70.1
70.2
70.3
71.3
71.8
73.6
73.5
73.4
73,3
72.5
72.6
72.6
72.6
72.6
72.6
71.3
71.3
71.3
71.3
71.4
71.4
70.6
70.7
69.4
71.1
70.1
69.6
Amphibole Cone.
(ug/m3)
<.27
<.26
.69
< .29
-
< .32
.52
.91
.62
.25
< .27
< .30
.55
.66
.63
< .26
.27
< .28
< .27
.51
< .24
< .25
< .26
< .27
.41
.75
.80
< .25
< .28
< .29
1.2
< .27
< .27
< .27
< .29
< .32
< .26
< .26
< .27
< .27
< .29
< .31

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APPENDIX F
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•                   ELECTRON MICROSCOPE  ANALYSIS,  AMPHIBOLE  FIBERS  (fibers/m3)



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          - 55 -
Electron Microscope Analysis
Date Sample
6/267-6/29 0118
0119
0120
0121
0122
0123
/14-7/17 0155
0156
0157
0158
0159
0160
/19-8/22 0228
0229
0230
0231
0232
0233
/28-8/31 0246
0247
0248
0249
0250
0251
Location
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
1
2
3
4
5
6
Amphibole Fibers
Concentration
(fibers/m3)
11,000
4,000
14,000
4,000
3,000
2,000
15,000
10,000
14,000
3,000
4,000
2,000
21,000
	

14,000
800

2,000
2,000
6,000
800
2,000
600
Amphibole Mass
Concentration
XRD (ug/m3)
1.60
1.45
2.29
<0.31
<0.32
<0.30
2.38
1.34
1.49
<0.28
<0.28
<0.29
0.73
	
1.53
<0.32
0.49
<0.32
0.59
0.66
0.57
O.29
<0.32
<0.30

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           -  56  -
Electron Microscope Analysis
Date
9/9-9/12







9/24-9/27






9/30-10/3





10/24-10/27






11/26-11/29






Sample
270
271-1
271-2
272
273
274
275-1
275-2
300
301-1
301-2
302
303
304
305
312
313
314
315
316
317
360
361-1
361-2
362
363
364
365
426
427
428-1
428-2
429
430
431
Location
1
2
2
3
4
5
6
6
1
2
2
3
4
5
6
1
2
3
4
5
6
1
2
2
3
4
5
6
1
2
3
3
4
5
6
Concentration
(fibers/m3)
5,000
12,000
4,000
10,000
8,000
2,000
1,000
1,000
1,000
3,000
3,000
11,000
1,000
1,000
800
12,000
11,000
14,000
2,000
4,000
2,000
8,000
13,000
16,000
10,000
4,000
3,000
3,000
200
2,000
5,000
5,000
200
1,000
200
Amphibole Mass
Concentration
XRD (ug/m3)
0.46
<.28
<.28
1.11
<.31
<.36
<.28
<.28
<.30
0.71
0.71
0.58
<.30
<.32
<.24
1.43
0.95
2.45
<.27
<.30
<.27
0.59
1.44
1.44
0.72
<.28
<.30
<.30
0.55
0.66
0.63
0.63
<.26
0.27
<.28

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                               -  57  -
                      Electron Microscope Analysis
Date
Sample   Location
Concentration
 (fibers/m3)
Amphibole Mass
Concentration
 XRD (ug/m3)
11/29-12/2






432-1
432-2
433
434
435
436
437
1
1
2
3
4
5
6
4,000
3,000
7,000
12,000
800
<200
700
<.27
<.27
.51
<.24
<.25
<.26
<.27

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                                          APPENDIX G


                                         PROBLEM SAMPLES

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DATE
6/29/77
6/29/77
7/5/77
7/5/77
8/7/77
8/16/77
8/19/77
8/19/77
8/24/77
8/25/77
8/28/77
9/3/77
8/31/77
9/6/77
9/9/77
9/9/77
9/9/77
9/15/77
9/21/77
9/21/77
9/27/77
9/30/77



- 58 -

PROBLEMS SAMPLES
FILTER #
0125
0127
0136
0138
0206
0224
0229
0230
0239
0242
0248
0253
0254
0265
0272
0273
0274
0283
0295
0296
0307
0314


        PROBLEM

New sampler, calibrated 7/1/77

Earth moving nearby

Broke filter on removal, recov.
fragment from wind

Sampler unplugged, short period

No flow reading

Construction across road

No flow, sampler shut off

Construction across road

Power outage

Construction across road

Construction across road

Power out

Construction across road

Tarring roof nearby

High winds

High winds

High winds

Tarring roof nearby

Tarring roof nearby

Construction across road

Tarring roof

Construction across road

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                                    - 59 -
DATE




10/6/77




10/6/77




10/6/77




10/9/77




10/12/77




10/12/77




10/15/77




10/18/77




10/21/77




10/30/77




11/5/77




11/17/77
FILTER #




 0324




 0325




 0326




 0332




 0338




 0339




 0344




 0350




 0356




 0374




 0386




 0410
        PROBLEM




Ripped filter upon removal




Ripped filter upon removal




Construction across road




Construction across road




Construction across road




Power failure




Construction across road




Construction across road




Construction across road




Filter ripped during period




Construction across road




Snowstorm

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                                           APPENDIX  H
 I                         WIND FREQUENCY DISTRIBUTION,  RESERVE  OFFICE
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