-------
                                                              Table 5
                                     Detection of Contaminants in Water from Susquehanna River
                          (Concentrations of Hazardous Materials in mg/1 showing a measureable response)
QJ Oi 4-1 OJ
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-------
SURVEY OF MARYLAND WATERS

    Natural waters from north central Maryland were sampled to determine
range of properties and concentrations of natural constituents.

    Twenty-two water sarr.pes were taken from a loop which reached from
approximately 10 miles north of Baltimore, northwest to Emmitsburg, south
toward Frederick, south-easterly towards Laurel, around Baltimore and back
to five miles south of the starting point.  The names of the waters where
known were noted; others were identified by their location.  The selected
detection methods were used to characterize, the waters and to anticipate
any problems which might arise in use of the kit.  ^o difficulties were
experienced in analysis.  Generally speaking the waters were of high quality
and changes in them due to contamination should be easy to detect.  Only
when samples were taken near the city of Baltimore, in the harbor area, did
some of the background readings (e.g. conductivity, sulfate and chloride)
get so high as to present a significant background.

    Data are summarized in  Table 6.
-------
                                                  -"able 6

                           Background of Natural Waters of North Central Maryland
Water Source
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1. Loch Raven Reservoir
2. Liberty Reservoir
3. Stream West of Taneytown
4. Stream West of Taneytown
5. Stream West of Taneytown
6. Monacacy River, Rt 97
7. Stream East of Enmitsburg
8. Stream South of £minitsburg
9. Stream North of Frederick
10. Stream North of Frederick
11. Monacacy River, Rt 80
12. Hawlings Run
13. Pautuxent River, Rt 97
14. Cattail Creek
15. Pautuxent River, Rt 108
16. Stream Near Brinklow
17. Middle Pautuxent River
18. Little Pautuxent River
19. Patapsco River, Rt 144
20. Patapsco River, Baltimore
21. Patapsco River, Baltimore
22. Falls Run
10
10
10
10
10
10
10
10
10
10
10
26
10
10
10
10
10
10
10
10
10
10
-
-
-
-
-
-
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-
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-
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+
-
+
+
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-
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-
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-
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-
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-
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-
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-
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-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
-
6.9
6.9
7.1
7.1
7.2
7.1
7.4
7.1
6.8
7.1
7.0
6.8
6.9
6.8
6.9
6.8
7.3
7.2
7.3
6.6
7.3
7.5
139
136
165
135
249
185
165
104
60
160
200
78
106
110
95
84
130
142
113
162
600
165
4.8
6.2
7.5
5.7
4.8
3.8
2.2
1.8
0.0
7.0
7.5
5.3
4.8
6.2
4.0
3.7
4.8
4.0
4.8
3.8
3.7
4.0
20
40
30
30
40
50
40
10
10
10
30
20
20
10
0
10
0
0
0
0
30
0
3
4
7
8
18
16
12
4
1
11
15
1
1
1
3
3
6
8
7
12
35
5
<0.1
<0.1
<0.1
<0.1
0.3
0.2
<0.1
< 0.1
<0.1
<0.1
0.2
< 0.1
<0.1
<0.1
<0.1
<0.1
<0.1
<0.1
<0.1
< 0.1
0.4
<0.1
<0.1
0.7
<0.1
0.4
0.8
0.6
<0.1
<0.1
<0.1
<0.1
0.3
<0.1
<0.1
<0.1
<0.1
<0.1
<0.1
<0.1
0.3
1.6
0.5
<0.1
10.4
15.9
9.1
8.2
25.4
10.4
5.0
4.0
1.3
5.5
8.8
6.0
6.4
9.1
7.8
7.8
13.4
17.7
12.5
16.5
110.0
15.0
0.1
0.1
0.1
0.2
0.2
0.3
0.2
0.2
0.1
0.2
0.2
0.1
0.1
0.1
0.2
0.1
0.1
0.2
0.2
0.1
0.2
0.2
*Stains were less than l-2mm, tests considered negative.
NOTE:  All samples represent different sources of water, or significantly different points of the same body of

       water.
-------
                                SECTION 5
                    FORMULATION OF DETECTION CONCEPT
SELECTED TESTS
    Many of the reasons for selection or rejection of individual tests have
been discussed (Experimental Studies) .  Unfortunately, selection is often
based not necessarily on capability required, but on what is available.
All-in-all every effort was made to assemble the best combination of tests
from what is available, with emphasis placed on reaching previously set
goals of the detector kit.  Generally, procedures which are simple, reliable,
stable and commercially available (when possible) and lend themselves to the
detection concept were selected.  To maintain compactness, duplication of
detection capability was avoided.  For example, numerous metal tests were
eliminated by adopting dithizone as a general heavy metals test.

    A summary of characteristics of the 15 procedures selected for the kit
are given in  Table  7 .

PROJECTED DETECTION  CAPABILITY

    A "paper analysis" was made to project the probability of detection of
the 370 compounds listed in the Federal register.  Each compound was screened
by comparison with the detection tests (except turbidity) listed in  Table  7 ;
that is, each compound was compared with a) data derived from laboratory test-
ing with contaminants from the model list, and b) data derived from handbooks.
A compound was considered detectable by a particular test if it was judged that
a saturated solution or 1000 mg/1 of the compound (whichever was less)  has a
significantly greater than 5<"7 chance of responding.  Where information was
considered inadequate to make a satisfactory judgment, individual additional
testing was considered.  (For example,  in this manner it was determined that
                                     28
-------
to
CD
TABLE 7
Summary of Methods Selected for Detector Kit
Detection
Parameter
Cholinesterase
Inhibitors
Benzene
Heavy Metals
Phenol
Cyanide
pH
Conductivity
Nitrate
Nitrogen
Color
Sulfate
Phosphate
Ammonia
Chloride
Fluoride
Turbidity
Type*
Qualitative
Qualitative
Qualitative
Qualitative
Qualitative
Quantitative
Quantitative
Quantitative
Quantitative
Quantitative
Quantitative
Quantitative
Quantitative
Quantitative
Quantitative
Process
Enzyme
Ticket
Detector
Tube
Extraction/
Test Tube
Extraction/
Cent. Tube
Detector
Tube
Meter
Meter
Spectro-
photometer
Spectro-
photometer
Spectro-
photometer
Spectro-
photometer
Spectro-
photometer
Spectre-
photometer
Spectro-
photometer
Spectro-
photometer
Reagents**
M30A1, Chemical
Agent Detector
Kit
Bendix/Gastec
Hach/Laboratory
Hach
Kitagawa
—
—
Hach
—
Hach
Hach
Hach
Laboratory
Hach
—
Tine,
Min.
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<2
< 1
< 1
<1
<1
<1
<6
< 1
-------
 nitrites would respond  to  the  nitrate  test  and  sulfites  were  detected  by
 the  sulfate  test,  whereas,  thiosulfates  were  not.   Also,  certain  arsenates,
 arsenites and  bromates  respond to  the  phosphate test,  but chromate  does
 not).   Extensive  testing was conducted with heavy  metals  and  ammonia con-
 taining compounds.   These  data have  already been reported under appropriate
 sections in  Experimental Studies.

     Highlights of  the "paper analysis" are  given in Table 8      Data  from
 this study indicate  that 857, of the  contaminants would respond to at least
 one  parameter;  587,  30% and 10% would  respond  to two,  three,  and  four  or
 more parameters respectively.   (See  complete  data  in Appendix A.)

     Because  certain  compounds  don't  show responses  for the detection
 parameters doesn't necessarily mean  non-detection.  Rather, many  of these
 structures are very  complex and their  reactivity cannot  be predicted.
 Judging by some of the  unexpected  responses obtained with many of the
 detection methods  it is to  be  expected that some of these materials are
 detectable by  present methods.

                                 Table 8

             Probability of Detection  of Water  Contaminants

                   (Based on nominally 370  compounds)

             Detection Parameter             Probable Responses

          Cholinesterase Inhibitors                  16
          Benzene                                    20
          Heavy Metals                              102
          Phenol                                     12
          Cyanide                                    11
          pH                                         66
          Conductivity                              2C1
          Nitrate Nitrogen                           18
          Color                                      50
          Sulfate                                    23
          Phosphate                                  18
          Ammonia Nitrogen                           58
          Chloride                                   72
          Fluoride                                   24

USE CONCEPT

     Our  goal was to develop a  field kit  using a standardized,  system so that
 results  are easily obtained and interpreted by a senior technician.  This
 goal, generally, has been met;   tests are  easy to perform,  short and designed
 for  ease of operation in the field.  However,  detecting almost any contami-
nant in  any water background is a formidable task which requires ingenuity
and  the  interpretive skills of a dedicated investigator.
                                     30
-------
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
PH
Conductivity
Turbidity
Nitrate Nitrogen
Color
Sulfate
Phosphate
Ammonia Nitrogen
Chloride
Fluoride
    The detection concept relies basically on three evaluations as shown:

                            DETECTION CONCEPT

General Assessment                           Relative Measurements

1.  Appearance

2.  Color of Filtered Water

3.  Color of Suspended Matter



Spot Tests

4.  Cholinesterase Inhibitors

5.  Benzene

6.  Heavy Metals

7.  Phenol

8.  Cyanide

    General Assessment procedures allow the operator to make a general
evaluation of the water to be tested.  That is, are there slicks  present?  —
is the water colored? — is there a lot of suspended material?—  is  the
suspended material colored?  Spot Tests are used to indicate if a parti-
cular type of contaminant is present.  A positive  response  to any of  these
tests should be considered contamination since  it  would indicate  compounds
not normally found or desired in water.  The  final group of tests,
Relative Measurements, is based on constituents of natural  water.  Contami-
nation is indicated by a significant  increase in one of these parameters
compared to uncontaminated water.

    To use the detection concept the  investigator  must assess  two major
factors:  a) The nature of the water  source —  is  it stationary,  like a
lake or pond, or is it moving like a  stream or  river?  b) The nature of  the
contaminant — is it  specifically known or partially known, such  that it
may be acid or base,  organic or  inorganic, phosphate containing,  colored,
etc?

    In situations where the contaminant is unknown,  the  investigator
confronts the situation in an orderly fashion:   (1)  He  immediately conducts
the General Assessment evaluations.   (2) He considers using the  Spot Tests
since  these are simple to use and easy to  evaluate.   (3) He proceeds to  the
Relative Measurements.  If the  location of the  contaminant  is  based  on  a
relative measurement  then he must make a comparison  between the  area of
                                     31
-------
 suspected contamination and a clean source of water  (reference sample).
 Tn  the case of a stream,  the reference sample may be taken at a location
 upstrean from the contamination.  If the body of water is a lake, he must
 use his best judgment and select an area believed to he clean.  Once the
 reference sample is established, it is a matter of deciding which relative
 tests can be used in detecting significant changes.

    In cases where the specific contamination is known, the investigator
 proceeds directly to the applicable tests.  For example, an investigator
 confronted with a spill of phosphoric acid would immediately perform pH,
 conductivity and phosphate tests and determine which is most suitable
 for this situation.

    A special data sheet for recording and reporting of contamination has
been designed to correspond with the detection concept (see Appendix B,
p. 10).

DESIGN AND FABRICATION OF PROTOTYPE KITS

    A significant part of design was concerned with human factors
considerations, i.e. man/machine interfaces.  The. purpose is to select
procedures and instrumentation which, make tests easy to perform and
evaluate and which provide reliable information.  Some of these factors
have already been considered when procedures were selected.  For example,
use of test papers, color comparators and pK indicators are considered too
 subjective, particularly when measurements must be made relative to a
reference sample.  Use of a quality pH meter, conductivity meter and
colorimeter is a prerqulsite.  Spot tests, which are also subjective, are
adopted for use in the detection concept as gross tests to be used only
on a "go no-go" basis.

    Some of the instruments considered for this program (e.g. the
Chemtrix Type 40E pH meter and Chemtrix Type 70 conductivity meter) have
already been discussed.  Much of the development data was obtained with
 the instruments; both meet the level of quality and performance required
 for the kit.  Also, the Hach PR Colorimeter was used extensively and was
 found to be a highly satisfactory portable colorimeter.

    The Mini-Spec 20 Spectrophotometer (marketed by Bausch and Lomb,
Analytical Systems Division) was also considered briefly for the kit.  A
demonstration of the Mini-Spec 20, which is a full grating spectrophotometer
about the size of a pocket calculator, showed it to be a sensitive, accurate
and versatile instrument.   The feeling, however, is that it may be too delicate
and sophisticated for field use; many of the pieces used are small and do not
appear to easily lend themselves to operation under rugged conditions.

    Originally it was planned to integrate the best available instrumentation
into a suitable carrying case.   A prime concern ail-along was to restrict
kit size and x^eight to maintain the man-portable concept.   When it appeared
the final package might become too large ar.d unwieldy,  instruments combining
-------
several functions were sought.   In fact, at that tine, a 4 Function
Water Analyzer (International Ecological Systems) was on the market.   The
instrument, which measured about 5x10x11 inches provided pH, conductivity,
colorimeteric and thermal measurements.  This item was considered until
its continued availability, service and replacement parts became uncertain.

    Finally, a decision was made to adapt the DR-EL/2 portable test kit
marketed by Hach which incorporates a spectrophotometer and a conductivity
meter.  Hach agreed to provide this item without the standard equipment or
reagents.  In addition, a Hach Model 1975 battery-operated pH meter was
dismantled and reassembled into a special compartment fabricated into the
lid of the case; when the case is open the pH meter faces the operator.  The
battery for the pH meter is  next   to the power supply for the spectrophoto-
meter and conductivity meter.

    A significant human factors advantage is gained by use of the
spectrophotometer instead of a filter colorimeter since color filter
changes are not required for the different colorimetric analyses.

    It was originally planned to use a case meeting military specifications
for the detector kit.  However, the Fach case by comparison, while not as
rugged, is considerably lighter and less expensive.  Also use of the Hach
case significantly reduces special design and fabrication costs for the kit.

    A particularly important piece of equipment included in the kit is a
plastic syringe with stainless steel head fitted with a glass fiber disc
to filter the water sample.  It is used for general assessment of the water
sample and to process it for colorimetric analysis.

    Other necessary ancillary equipment or reagents were purchased from
available sources or prepared in the laboratory.  Many of the purchased
reagents and equipment were repackaged in the kit in  the interest of
economy of space.  It must be remembered that only the detector tickets
and substrate are used from the M30A1 Chemical Agent Detector Kit.  The
Tris buffer is prepared in the laboratory (Experimental Studies,  m.
Enzyme Systems) since it must be washed with dithizone for use in the
heavy metals test.

    An Operator's Manual  (Appendix B) was prepared for use with the
kit.  It describes in detail the use concept, equipment and procedures
used.  A source listing for consumable parts is  given.  Pach manuals for
the DR-EL/2 portable test kit and Yodel 1975 pH meter are also provided.
In addition, laminated outlines of procedures are included  for use in  the
field.

    Tests were  conducted with the kits  to demonstrate their fieldability.
Modifications were made to the Operator's Manual as a result of these
exercises.  The detector kits resulting from this program are shown in
Figures  1 and 2.
-------
           HAZARDOUS MATERIALS  DETECTOR  KIT
co
                               Figure 1 Hazardous Materials Detector Kit
-------
co
01
            HAZARDOUS MATERIALS DETECTOR KIT
                           Figure 2 Hazardous Materials Detector Kit, In Use

-------
                                REFERENCES

  1.   Prober,  R.,  "CRC Handbook of Environmental Control",  Vol.  Ill,  Water
      Supply and Treatment.   CRC Press,  Cleveland,  OH (1973).

  2.   Annual Book  of  ASTM Standards",  Part 23,  Water;  Atmospheric  Analysis,
      Philadelphia, PA (1973).

  3.   "Standard  Methods  for  the Examination of  Water  and Wastewater",  13th
      ed., American Public Health Association,  Washington DC  (1971).

  4.   "Methods for Chemical  Analysis of  Water and Wastes",  US  Environmental
      Protection Agency,  Analytical Quality Control Laboratory,  National
      Environmental Research Center, OH  (1971).

  5.   Wilder,  I.,  Lafornara,  J.P., Water and Sewage Works,  119,  82 (1972).

  6.   Duke,  F.R. and  Smith,  G.F.,  Industrial and  Engineering Chemistry, 12,
      201  (1940).

  7.   Feigl,  F., "Spot Tests  in Organic  Analysis",  7th ed., Elsevier
      Publishing Co., Amsterdam,  Netherlands (1966).

  8.   Elsheimer, H.N., Kocken,  R.L., Anal.  Chem.  3£,  145 (1966).

  9.   Utsumi,  S.,  J.  Chem. Soc.  Japan ^3_,  835 (1952).

 10.   Fehringer, N.V., Ogger, J.D., J. Chromatog. 23_, 95 (1966).

 11.   Kovacs, M.F., J. of the AOAC, 47_,  1097 (1964).

 12.   Abbott, D.C., Egan, H., Thomson, J.,  J. Chromatog. 16, 481 (1964).

 13.   Kenner, R.A., Aboderin, A.A., Biochemistry, 1£, 4433  (1971).

 14.   Burnhan, K., Calder, G.V.,  Fritz,  J.S., Junk, G.A., Svel, H.J.,
     Willis, W., Anal. Chem.,  44, 139 (1972).

 15.   Braun, R.A., Mosher, W.A.,  J. of the American Chemical Society,
     80, 2749 (1958).

 16.  Mellan, I.,  "Organic Reagents in Inorganic Analysis", The Blakiston
     Co., Philadelphia,  PA  (1941).

 17.  Braun, T.,  Farag, A.B., Analytica Chimica Acta, 73_. 301  (1974).

 18.  Berthelot,  M.t  Repertaire de Chemil Applique, 1^, 284  (1859).

19.  Searcy, R.L., Gaugh, G.S., Karotger, J.J., Berquist,  L.M., Am. J.
     Med. Tech., 27_,  255 (1962).

20.  Chancy, A.L., Marbach,  C.P., Clin.  Chem.,  £, 130 (1962).


                                   36
-------
                   LIST OF MANUFACTURERS AND SUPPLIERS


 1.  Anderson Laboratories Corporation, Fort Worth, TX

 2.  Bausch and Lomb,  Analytical Systems Division, Rochester, NY

 3.  Bendix/Gastec (Products available from National Environmental
     Instruments, Inc., Warwick, RI)

 4.  Boehringer Mannheim GMBH, Biochemcial Department (Products available
     from Fisher Scientific Co.)

 5.  Chemtrix, Inc., Hlllsboro, OR

 6.  Corning Class Co. (Electrodes are available from VWR Scientific
     Division of Univar)

 7.  Hach Chemical Co., Ames IA

 8.  International Ecological Svstems Corporation, Mt. Laurel, NJ

 9.  Kitagava (Products are available from Matheson Gas Products,
     East Rutherford,  NJ)

10.  Micro-Essential Laboratory, Brooklyn, *TY

11.  Rohm and Haas, Philadelphia, PA

12.  Worthington Biochemical Corporation, Freehold, NJ
                                    37
-------
                                                            APPENDIX A

                     PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                                              REGISTER,  VOL. 40, NO. 250,  DEC. 75
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Acetaldehyde
Acetic acid
Acetic anhydride
Acetone cyanohydrin
Acetyl bromide
Acetyl chloride
Acrolein
Acrylonitrile
Adiponitrile
Aldrin
Allyl alcohol
Allyl chloride
Aluminum sulfate
Ammonia
Ammonium Compounds :
Ammonium acetate
Ammonium benzoate
Ammonium bicarbonate
Ammonium bisulfite
Ammonium bromide
Ammonium carbamate
Ammonium carbonate
Ammonium chloride
Ammonium citrate, dibasic
Ammonium ferrocyanide
Ammonium fluoborate
Ammonium formate
Ammonium gluconate
Ammonium hydroxide
Ammonium hypophosphite























































































































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-------
                                     APPENDIX A

PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                  REGISTER,  VOL.  40,  NO. 250, DEC.  75 (continued)
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Ammonium iodide
Ammonium molybdate
Ammonium nitrate
Ammonium oxalate
Ammonium pentaborate
Ammonium silicofluoride
Ammonium sulfamate
Ammonium sulfate
Ammonium sulfide
Ammonium sulfite
Ammonium tartrate
Ammonium thiocyanate
Ammonium thisulfate
Amyl acetate
Aniline
Antimony Compounds :
Antimony pentachloride
Antimony pentafluoride
Antimony potassium tartrate
Antimony tribromide
Antimony trichloride
Antimony trifluoride
Antimony triiodide
Antimony trioxide
Arsenic Compounds :
Arsenic acid
Arsenic disulfide
Arsenic pentaoxide

























































































































































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-------
                                      APPENDIX A

PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                   REGISTER, VOL. 40,  NO. 250, DEC.  75 (continued)
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Arsenic tribromide
Arsenic trichloride
Arsenic trifluoride
Arsenic triiodide
Arsenic trioxide
Arsenic trisulfide
Cacodylic acid
Calcium arsenate
Calcium arsenite
Potassium arsenate
Potassium arsenite
Sodium arsenate
Sodium arsenite
Sodium cacodylate
Benzene
Benzole acid
Benzonitrile
Benzoyl chloride
Benzyl chloride
Beryllium Compound a :
Beryllium chloride
Beryllium fluoride
Beryllium hydroxide
Beryllium nitrate
Beryllium phosphate
Beryllium sulfate
Boric acid
Brucine
Butyl acetate










































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-------
                                   APPENDIX A

PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                 REGISTER. VOL. 40,  NO. 250, DEC. 75 (continued)
                               03
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Butylamine
Butyric acid
Cadmium Compounds :
Cadmium acetate
Cadmium bromide
Cadmium chloride
Cadmium fluoborate
Cadmium nitrate
Cadmium sulfate
Calcium carbide
Calcium hydroxide
Calcium hypochlorite
Calcium oxide
Captan
Carbaryl
Carbon disulflde
Catechol
Chlordane
Chlorine
Chlorobenzene
Chloroform
Chlorosulfonic acid
Chromium Compounds :
Ammonium bichromate
Ammonium chromate
Calcium chromate
Chromic acid
Chromic sulfate
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-------
                                  APPENDIX A
PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL
                 REGISTER. VOL. 40.  NO. 250, DEC. 75 (continued)
t-t 
-------
                                                              APPENDIX A

                       PROBABLE  RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                                          REGISTER,  VOL. 40,  NO. 250,  DEC. 75 (continued)
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-------
                                   APPENDIX A
PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL
                 REGISTER, VOL. 40, NO. 250, DEC.  75 (continued)
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Diazinon
Dicamba
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Dichlorvos
Dieldrin
Diethy lamine
D ime thy lamine
Dinitrobenzene
Dinitrophenol
Diquat
Disulfoton
Diuron
Dodecyl benzenesulfonic acid
Dodecyl benzenesulfonic acid, calcium
salt
Dodecyl benzenesulfonic acid
isopropanol amine salt
Dodecyl benzenesulfonic acid, sodium
salt
Dodecyl benzenesulfonic acid,
triethanolamine salt
Dursban
Endosulfan
Endrin
Ethion
Ethylbenzene
Ethy lened lamine
Ethylenediamine-tetraacetic acid

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-------
                                                           APPENDIX A

                     PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                                        REGISTER, VOL.  40,  NO. 250, DEC. 75 (continued)
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-------
                                      APPENDIX A
PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL
                  REGISTER,  VOL.  40,  NO. 250.  DEC. 75 (continued)
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Ferrous chloride
Ferrous oxalate
Ferrous sulfate
Isoprene
Kelthane
Lead Compel ^i,, •
Lead acetate
Lead arsenate
Lead bromide
Lead chloride
Lead tluoborate
Lead t!Uoride
Lead iodide
Lead nitrate
Lead 8tearate
Lead SUlfate
Lead SUlfide
Lead tetraacetate
Lead thiocyanate
Lead Chiosulfate
Lead tungstate
Lindane
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-------
                                      APPENDIX A

PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                   REGISTER, VOL. 40, NO. 250,  DEC. 75 (continued)
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Mercuric acetate
Mercuric ammonium chloride
Mercuric bromide
Mercuric chloride
Mercuric cyanide
Mercuric Iodide
Mercuric nitrate
Mercuric oxide
Mercuric sulfate
Mercuric thlocyanate
Mercurous chloride
Mercurous Iodide
Mercurous nitrate
Methoxychlor
Methyl mercaptan
Methyl methacrylate
Methyl parathlon
Mevlnphos
Molybdlc trloxlde
Monoethylamlne
Naled
Naphthalene
Naphthalenic acid
Nickel Compounds :
Nickel acetate
Nickel ammonium sultate
Nickel bromide
















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-------
                                                    APPENDIX A

                  PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                                   REGISTER, VOL.  40, NO. 250, DEC.  75 (continued)
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Nickel fluoride
Nickel formate
Nickel hydroxide
Nickel iodide
Nickel nitrate
Nickel perchlorate
Nickel aulfate
Nitric acid
Nitrobenzene
Nitrogen dioxide
Nitrophenol
Paraformaldehyde
Parathion
Pentachlorophenol
Phenol
Phosgene
Phosphoric acid
Phosphorus
Phosphorus oxychloride
Phosphorus pentasulflde
Phosphorus trichloride
Polychlorinated blphenyls
Potassium hydroxide
Potassium permanganate
Proplonlc acid
Propionlc anhydride
Propyl alcohol
Pyrethrins
Pyrogallic acid
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-------
                                       APPENDIX A

PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                   REGISTER,  VOL. 40,  NO. 250, DEC. 75 (continued)
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-------
                                     APPENDIX A

PROBABLE RESPONSES OF DETECTOR KIT TO MATERIALS LISTED IN FEDERAL

                  REGISTER, VOL.  40,  NO. 250, DEC. 75 (continued)
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Phosphati
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Chloride
Fluoride
Toxaphene
Trichlorfon
Trichlorophenol
Trlethvlamine
Tr ime thy lamine
Uranium Compounds:
Uranium peroxide
Uranvl acetate
Uranyl nitrate
Uranyl sulfate
Vanadium Compounds:
Vanadium oxytrichloride
Vanadium pentoxide
Vanadvl sulfate
Vinyl acetate
Xvlenol
Xylene
Zectran
Zinc Compounds:
Zinc acetate
Zinc ammonium chloride
Zinc ammonium sulfate
Zinc borate

Zinc carbonate
Zinc chloride
Zinc fluoride 	 _^___

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-------
                                     APPENDIX A
PROBABLE RESPONSES OF DETECTOR KIT TO  MATERIALS LISTED IN FEDERAL
                  REGISTER, VOL. 40,  NO. 250, DEC. 75 (continued)
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-------
                               APPENDIX B


    OPERATOR'S MANL'AL FOR HAZARDOUS MATERIALS DETECTOR KIT


                                SECTION I

                              INTRODUCTION
     The Hazardous Materials Detector Kit is a portable self-sufficient
laboratory capable of providing the investigator in the field with a
variety of valuable information to assist him in detecting  (not neces-
sarily identifying) and tracing contamination in inland waters.  While
similar to other water test kits, the eouioment and orocedures contained
are designed to be used as a part of a total concept.  Before attempting
to use the kit in an investigation, the operator should thoroughly famil-
arize himself with the concept of use and obtain an understanding of the
significant data that can be derived.  Snecial apparatus, tests taken
from commercial and military kits, and procedures designed  specifically
for this item form the makeup of the kit.

     The kit contains delicate instrumentation and should be treated
accordingly.  Care and maintenance suggested in the manuals should serve
to prolong its usefulness.  Instrumentation consists of a battery or
line-operated spectrophotometer and a conductivity meter contained in a
Hach Chemical Co. DR-EL/2 Laboratory enclosure.  In addition, the Hach
Model  1975 battery-operated pH meter has been modified and  incorporated
in the enclosure.  Hach manuals for the nR-EL/2 Laboratory  and Model
1975 pH Meter are provided with the kit and should be referred to
frequently for operation, service and maintenance,  in addition to this
manual and the Hach manuals, abbreviated, laminated instruction cards
(sufficient to provide the operator in the field with auidance) are
included.   Data sheets are provided for reporting and recording data.

     To assist the operator in quickly gaining familiarity  with use of
the kit, this manual is divided into sections:  (a) Concept of Use, (b)
Equipment and Methodology, (c) Analytical Procedures and (d) Consumable
Materials.
-------
                               SECTION  II
CONCEPT
                                        USE
     Orininally, it was intended to develop a field kit usinq a
standardized system, in which results are easily obtained and inter-
preted by a senior technician.  These cioals, in part, have been net;
the tests are easy to perform, short, and desioned for the nreatest
ease of operation in the field.  However, the task of detecting almost
any contaminant in any water backaround is
the ingenuity and interpretive skills of a
kit combines instrumental and wet chemical
chemist with experience in water chenisty,
sary to detect and follow contamination in
kit relies basically on three types of evaluations as shown in the table
below.  Details of these procedures are m'ven in the section on Analytical
Procedures.
              a formidable one and reauires
              dedicated investiqater.  The
              methods; in the hands of a
              it can provide the data neces-
              inland waterways.  Use of the
      Detection Procedures of the Hazardous "aterials Vtector Kit
     General Assessment

     a.  Appearance

     b.  Color of Filtered Hater

     c.  Color of Suspended Matter

     Spot Tests

     d.  Cholinesterase  Inhibitors

     e.  Benzene

     f.  Heavy Metals

     q.  Phenol

     h.  Cyanide
                 Relative Mpasurements
                 k.  Turbidity

                 1 .  Nitrate  "Mtroqen

                 n.  rrlor

                 n.  Sijlfate

                 o.  p^osohate

                 D.  A^r>onia  Nitroqen

                 q.  Chloride
                                               r.   Fluoride
      The tests as a whole are larnelv nonsoecific and are capable of
 detectinn a much wider range of contaminants than is indicated.  General
-------
 Assessment procedures (a to c) allow the ooerator to nake a general
 evaluation of the water to he tested.  Snot Tests orocedures (r1 to h)
 indicate that a particular type of contaminant is or is not present.
 However, any positive resoonse by the Soot T«sts should he considered
 as contamination since this indicates a oronerty not normally found or
 desired in water.   The final  nroup of tests (i to r),  ^lative  M»asure-
 nents,  is based on a natural  oronerty of water.   rontamination  is  indi-
 cated when a significant increase in  one of these parameters is observed
 over uncontaminated water.

      Hhile use  of the kit  cannot  be  standardized  for all  situations, a
 systematic approach can  make  qatherinq  of data more  direct and  meaning-
 ful.   First the investigator  assesses the oresence  of  contamination by
 evaluating two  major factors:   (a) The  nature  of  the water source  -- is
 it stationary,  like a lake  or a oond, or is it movinq  like a stream or
 river;  and (b)  The nature  of  the  contaminant  --  is  it  specifically known,
 totally unknown or partially  known,  such that  it  may be  acid or base,
 orqanic or inorganic, phosphate containing, colored, etc.

      Second the investigator  confronts  the  situation in  an orderly
 fashion:   (a) He immediatly conducts  a  "Gpneral  Assessment"  (tests a  to
 c);  (b)  He considers  using  Soot Tests (•"- to 8)  since these are  simple  and
 easy  to evaluate.   If he knows, or suspects strongly,  that the  contami-
 nant  will  resoond  to  one of these  tests,  this  may he the  only tool  he
 needs  to  conduct his  investigation; and  (c) M° noes  to  Relative Measure-
 ments  (tests  9  to  18).   If  location of  the  contaminant  is  based on a
 relative  measurement  then he  must nake  a  comparison  between  the area of
 suspected  contamination  and a  clean source  of  water  (reference  sample).
 In the  case of  a stream, the  reference  sample  may be taken at a location
 upstream  from the  contamination.   If  the  bodv  of  water  is  a  lake,  he must
 use his  best  iudament and select an area  believed to be clean.   Once the
 reference  water  is  established, it is a  matter of determining which  rela-
 tive  tests  will  be  most useful in detecting significant differences.

     Hhen  the pollutant  is  totally unknown, the investiaator may have  to
 run the entire  series  of tests, looking  for those revealing  the most
 significant  differences.  T^ese differences nay then he taken as indicators
 of suspected contamination.  THereafter,  only  tests  showing  the significant
 differences need he run on  suspect samples.

      In those cases where some information  is  L'.nown about  the contaminant,
 it may  be sufficient  to run only tests which are  relevant.   For example,
 if the  investigator knows the contaminant to he an inorganic acid, he may
 proceed immediately to DM and conductivity  measurements and  run  tests  for
 inornanic ions.   For  example, the investiaator knows that  the contaminant
 is chlorosulfonic acid.  H° has ootions to  make nu, conductivity,  chloride
 and/or sulfate determinations.  H^ would  probably select several parameters
which have  the lowest background readinq  with resoect to the reference
water.
                                    .54
-------
     If the investigator knows the contaminant to be detected but not if it
responds to any of the tests, he may wish to nake some quick soot tests in
the laboratory before taking the kit into the field.

     After the investigator has selected indicators for contamination he
will want to record his data carefully and systematically.  T^e gradual
change in the data will eventually orovide clues to the location and level
of contamination.   Data sheets designed soecifically for this purpose are
included in the kit.

     As indicated  earlier, use of the kit cannot ^e fully standardized;
the investigator must be ready at each occasion to nake judgments relative
to the surroundings and the circumstances of the contamination.  In the
procedures section all possible anticipated reactions to the tests have been
noted.  If, however, in the performance of a test, a precipitate or unusual
color not indicated occurs in the test sanole but not the reference sample,
then it is very possible that contamination of some sort is present.

     In making determinations with the soectroohotometer, it may often
suffice simply to  mark the test positive when a sinnificant color indicative
of contamination starts to develoo.  It may be adeouate for the investinator
to know the sample is still heavilv contaminated without actually determining
a specific value.

     Perhaps the most difficult judgment to make is to determine how qreat a
difference between the test sample and reference water samnle  is significant
in the Relative Measurements tests.  It will take familiarization with  the
kit and experience in its application to make reliable assessments  in  a given
situation.  As a "rule-of-thumb", based on the studies conducted to date,  the
following are considered significant instrumental chanaes:

      (a)  Change in pH of 0.5 units.

      (b)  20 percent gain in conductivity.

      (c)  10 percent nain in the  full scale deflection  (not concentration)  in
spectrophotometric procedures.

      Experience may show that these  values  are conservative and  smaller
differences will be found significant.

      As a final note,  a fluorescent  dye marker  is  included  in  the  kit.  This
may be of use  in marking the  location of a  contaminant.
-------
                               SECTION III

                        EQUIPMENT AND METHODOLOGY
                                                          r
     General.   With the exception of a container to collect water samples,
the Hazardous Materials Detector Kit contains the necessary instrumentation,
equipment and reagents to perform all the methods described in Analytical
Procedures.  This manual provides the user with an overview sufficient for
operation of the instruments.  Instruments are from the Hach Chemical Company
and Hach manuals are provided as part of the detector kit package.  Hach
manuals should be consulted for operation, maintenance, and servicing of
their instruments.

     Power.  The instruments are powered by batteries for field use.  In
addition, the spectrophotometer and conductivity meter may be modified for
120 or 240 VAC operation using an adapter and cable provided with the kit.
The procedure for the conversion is described in the Hach manual.  The pH
meter will operate only from the battery supply.
     Batteries reouired for the kit are 1 each, 6.75 V, Mallory TR-235P. (or
equivalent), 8 each, .1.5 V size D, and 4 each 1.5 V size AA.  It is recom-
mended that expendable alkaline manganese batteries be used, when available,
for economy and widest environmental range of operation.  The investigator
should minimize the on-time of all instrumentation in order to conserve
battery life in the field.

     Batteries may be checked by the following procedure:

     (a)  Set the POWER switch on the pH meter to the BATT CHECK position.
If the needle deflects beyond BAT OK, the battery is alright.  Otherwise
replace the 6.75 V battery.

     (b)  Set the conductivity meter range switch to the BATT CHECK position.
Hold the BATT CHECK switch on the spectrophotometer face in the DR position to
check only the D size batteries.  The needle should deflect beyond 83 percent.
Hold the same BATT CHECK switch in the COND position to check both the D and
AA size batteries.  Again the needle should deflect 83 percent.

     Batteries may be reached for servicing by unloosening the two knurled
screws and removing the spectrophotometer.  Arrangement of the batteries is
shown in Figure 1.

     Loading Diagram.  Location of the kit components is shown in Figure 2.
The tray is easily removed by lifting the top out by one of the finger holes
and then grasping the inner partitions of the tray and lifting straight up.

     Setting UP the Kit in the Field.  The investigator should attempt to
find several sauare feet of flat area.  A raised surface like a mound or
large rock would give greater operating comfort.  The investigator may use
a layout according to his own requirements, but that shown in Figure 3 is
convenient for reaching all necessary pieces.  Note that the tray top doubles
as a small work surface.  The arrangement of the pH measuring components is
shown in Figure 4.

                                      56
-------
                                                                    1.5V, AA SIZE CELL
en
                                 MALLORY TR-235R.6.75V
                                    OR EQUIVALENT
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                                       Figure 1.  BATTERY  ARRANGEMENT
-------
                                            TOP
                          pH ELECTRODE
                                                 INSTRUCTIONS
   pH METER
                                               .
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                                                        n

                                                                             ENZYME TICKETS
                                                                             30 & 50 ml BEAKERS
                                                                              -GRADUATE
                                                                               SUBSTRATE
  PLASTIC TUBES
CYANIDE TUBES
              Alka-Seltzer
                               NitraVer V
                                  BOTTOM
                                   CALIBRATION SCALES
                            DIST. WATER SRADNS
BENZENE TUBES
                                                                              JRIS BUFFER
                                                                              -BUFFER, pH 7.0
                                                                              BUFFER SOLUTION,
                                                                                 HARDNESS 1
                                                                             —PHENOL REAGENT
        PHENOL 2    Suifav8r IV
                      t
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                                                                        'CHLOROFORM
                          FILTERS        \ CELLS '       \ CENj TUBE\   FERRIC ION SOLUTION
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DISPENSER CAP
pH CAP
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                                   FILTER HOLDER
                                   DROPPING  PIPETTE
                                                                         O

                                                                              -TRAY TOP
                            Figure  2.  LOADING DIAGRAM
                                              58
-------
                                 KIT
                                       TRAY TOP
        TRAY
    Figure 3.  TYPICAL  FIELD SETUP
                                  ELECTRODE CLIP





                                  STAND
  30 ml BEAKER
Figure 4.  pH  MEASURING COMPONENTS
                      59
-------
     pH dieter.  Hang the 30 ml beaker on the edge of the case using the
beaker clip as shown in Figure 4.  Stand the support rod, with the electrode
spring clip in place, in the vertical hole located inside, the left front
corner of the case.  Remove the wetting cap from the electrode and replace
with the plastic bulb protector.  Install the electrode in the spring clip
and set at a suitable height to reach into the beaker.  Fill  the beaker with
distilled water to start the electrode soaking immediately.  The liquid
junction must always be below the water level.  After about 10 minutes, fill
the beaker with 25 ml of pH 7.0 buffer and immerse the electrode again.  Set
the TEMP dial to the approximate solution temperature and turn the POWER
switch to the ON position.  Adjust the STANDARDIZE switch to  read exactly
7.0 and turn the power off.  Discard the buffer, rinse the electrode and soak
in distilled water.  The instrument is ready for use.
     The above procedure performed dailv is adequate for field use.  For more
exacting standardization on a less frequent basis refer to the Hach manual.
     Conductivity Meter.  The conductivity probe requires no  conditioning and
is readied for use by plugging into the PROBE INPUT socket and inserting the
Conductivity Meter Scale into the meter.  The probe is submersed in water
sample sufficient to cover the vent holes.  The RANGE switch  is placed in the
"5" position and is worked down until an on-scale reading is  obtained.  If
the reading is in the lower 10 percent of the scale, the next lower RANGE
position should be used.
     Spectrophotometer.  The Hach Spectrophotometer is designed to be used
with insertable meter scales which are provided.  (If the operator wishes to
devise his own analytical procedures, he may prepare calibration scales fol-
lowing instructions in the Hach manual and using blank meter  scales available
for this purpose.)
     The Spectrophotometer should be adjusted to zero before  each use, but
need not be done so before each test.  Using a- right-to-left  reading meter
scale, hold the light switch in the ZERO CHECK position and use the ZERO
ADJUST knob to set the meter needle to the extreme left mark  of the scale.

     Each time the Spectrophotometer is used the proper meter scale is
inserted and the wavelength is set.  A sample cell containing a blank pre-
pared as described in the procedures is inserted and, after turning the
instrument on, the LIGHT CONTROL switch is ad.iusted to zero on the meter
scale.  Once the instrument is zeroed, a cell containing the  true sample is
placed in the Spectrophotometer.  The instrument is turned on and the meter
reading is noted.  All readings with the instrument should be sufficiently
long to obtain a stable reading, still the on-time should be  kept to a
minimum to prolong battery life.
     In those instances where the concentration of a component is so high as
to run off scale, a dilution should be made.  The 1 ml dropping pipet and
the 25 ml graduate may be used for this purpose.  The scale reading will then
be multiplied by the dilution factor.

     Filter Assembly.  In making spectrophotometric determinations with the
exception of turbidity measurement, filtered water samples are used.  Because
gravity filtration is too slov.1, the assembly shown in Figure  5, for which
glass fiber filters are provided, is used to quickly obtain clear samples.
Filter changes are easily made using the flat ended tweezers.

                                      60
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       It may  be desirable  in some  instances to save the filter discs in order
  to  use the color accummulated on  them as a means to monitor contamination
  in  this use, of course, each disc would be used only once and with a specified
  volume of water.

       It is important that samples be filtered only when indicated   Many
  contaminants may be in the form of slicks, solids or emulsions and their
  removal prior to analysis in procedures such as the spot test may grossly
  affect the result of the test.

      Effervescent Jar.  The Effervescent Jar assembly (Figure 6) is used to
  detect contaminants in water which may be expelled by an effervescent material.
 Alka-SeltzerP. tablets are used for effervescence and Bendfx-Gastec benzene
 analyzer tubes, which are sensitive to a variety of contaminants are used as
 tne detector.

      The jar is filled to the  level  mark with the water sample (about 80 ml)
 The triangular file is used to score and remove  the tips  of an analvzer tube.
 Ilr   Sn ni'u  clMnSent?dJn  tf?e cap asserTlbly with  arrow pointing away from the
 jar.  An Alka-SeltzerR tablet  is dropped into the jar and  the  cap ouickly and
 snugly screwed on.   The test  is  allowed  to  continue until  effervescence ceases.

      Caution should be taken not to  drive water  droplets  into  the analyzer
 tube since  this would  inhibit  the reaction.

      Chromatographic Tube  Test.   Kitagawa detector  tubes included in  the  kit
 are  miniature Chromatographic  columns  impregnated with  reagents  to  detect
 Til VJ  Wat|['   The tr1an9ular  f11e ^ used to score and  remove  the"  tips
 of the tube.   The tube  is  stood   with the red  ball  pointed  up)  in a depth  of
 1-2  cm of water sample  (Figure 7).  As the water  is drawn up the  tube  by
 capillary action, a  blue stain will form on the  silica gel  if  cyanide  is
 present.                                                •
                     The enzyme ticket (Figure 8) contains glass fiber spots
 impregnated with horse serum cholinesterase.  When wetted with pH 8 0 Tris
 buffer, or neutral water not containing a cholinesterase inhibitor, 'the
 enzyme becomes active and will change the color of the orange color substrate
 to blue.  If the enzyme is exposed to a cholinesterase inhibitor such as
 certain insecticides, rodenticides or some other toxic materials  it is
 inactivated and unable to change the color of the substrate.   One end of 'the
 ticket is immersed in the water sample and the other is used as a control.

     Data Sheets.  Forms shown in Figure 9 are provided with the kit and may
 be used for recording and reporting data.

     General  Maintenance.   For specific maintenance and servicing problems
regarding instrumentation  refer to the Hach manuals.   As a  matter of general
upkeep, some common sense  approaches to the equipment will  be helpful' "
Obviously, delicate instrumentation requires gentle handling; drons  arid
severe jarring should be avoided.   It may  be desirable to pass a  wire loop
around the battery clips to prevent the cells from "popping"  out.
                                      61
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FILTER HOLDER
     TYGON TUBE
    Figure  5.  FILTER ASSEMBLY
SYRINGE
                              DETECTOR TUBE





                              CONNECTOR
                        -*	4 OZ. JAR
Figure 6.  EFFERVESCENT  JAR ASSEMBLY
                 (12
-------
         50 ml BEAKER
                                                CYANIDE DETECTOR TUBE
            Figure  7.  CHROMATOGRAPHIC  TUBE TEST
                                       2)  SOAK IN WATER SAMPLE
           DROPPER
U  ADD THIS BUFFER
                        ENZYME TICKET
                                                            50 ml BEAKER
                                                    SUBSTRATE
                           ADD SUBSTRATE



         Figure 8.  CHOLINESTERASE INHIBITOR TEST
-------
                   FIGURE 9
DATA SHEET FOR HAZARDOUS MATERIALS DETECTOR KIT
   GENERAL ASSESSMENT                     SPOT TESTS
Choi.
Sample Time Location Appearance Col. Water Col. Matter Inhib. Benzene H'vy Metals Phenol Cyanide
1
2
3
4
5
6
7
8
9
10




































































































          RELATIVE MEASUREMENT TESTS
Conduct. Turbidity Nitrate, N? Color Sulfate Phosphate Ammonia, N? Chloride
Sample pH umhos/cm. FTU mg/1 APHA Units mq/1 mq/1 mq/1 mg/1
1
2
3
4
5
6
7
8
9
10


























































































Fluoride
mg/1










-------
     The investigator should avoid gettino excessive amounts of water
into the kit.   The electronics would he damaaed; the filter wheel of
the spectrophotometer is sensitive to extended periods of high humidity.
Certainly, in  returning equipment to the kit care should be taken to
shake or wine  off excess water.  °n returnino to the laboratory after a
day in the field, allow the kit to stand open to dry out.

     General cleaning procedures which may be applied to the conductivity
probe, electrode, cells, photocell window and filter wedqe are described
in the Hach manuals.

     f"anvpof the specially fabricated plastic parts in the kjt are made
of Lucite'  Protected with a touah vinvl oaint.  "hile Incite  is quite
strong, it may still be broken.  In this event the broken pieces should
be held in contact while a snail amount. of methvlene chloride is made to
flow into the  crack with a small syrinae.  Thp pieces will bond  immediately
and in a few hours will be as strona as new.

     Check List Before Hpino to the Field.  TH? following should be  used  as
a check list in the laboratory before takinn the kit to  the field.

     (a)  Check loadino diaqram to assure that all eauinment and reaaents
are present.  If more use of some reanents is anticipated, they  should  be
brought in an additional container.

     (b)  Perform prescribed battery checks, and replace weak batteries
where necessary.

     (c)  Check function (not  standardize1) rf the oH meter, conductivity
meter, and spectrophotometer.
-------
                                SECTION  IV

                          ANALYTICAL  PROCEDURES
     This section contains detailed  procedures  for  the  analysis  of
contaminants in water.  The arrangement  is made to  correspond  with  the
data sheet provided with the kit.  Ouestions  regarding  equipment and
its use should be referred to the previous section.

     General Assessment

     (a)  APPEARANCE

     Describe the water sample with  respect to  color, turbidity,  suspended
matter, slicks, etc.

     (b)  COLOR OF FILTERED WATER

     Apparatus:  Filter Assembly

     Procedure:  Filter 50 ml of the water sample.  Record  the visual color
of the filtered water and save a samnle  in a  clastic test tube for  reference.
Save the olass fiber filter for Procedure 3.

     (c)  COLOR OF SUSPENDED MATTER

     Record the color of the natter  collected on the glass  fiber filter  in
the previous step.  Save the filter  for  reference.

     Spot Tests

     (d)  CHPLINESTERASF INHIBITORS

     Reagents:  Enzyme Tickets
                Tris Ruffer, pH a.n
                Substrate

     Procedure:

     1.  Add about 20 ml of water samnle to the 50  nl beaker.

     2.  Remove an enzyme ticket from the plastic sleeving.  Add  several
drops of Tris Buffer to the test spot on the  round  end  of the  ticket and
1  ml  to the beaker.

     3.  Stir the buffered v/ater sample  using the sguare end of  the ticket;
then  allow the ticket to stand in the beaker  (souare end down),  being care-
ful not to wet the test spot on the  round end (blank) with  the water sample.
Allow to stand for 5 minutes.
                                     66
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     4.   Remove the ticket from solution;  shake off the excess  water.

     5.   Add several  drops of Substrate to each test spot and allow the
blue color to develop.

     6.   At the end of about 2 minutes, the round end (Mank) should he
blue.  Compare with the square end (test sample) of the ticket.  If the
square end is significantly different, i.e., no blue or only the very
siightest blue, a contaminant, probably an anticholinesterase type, may
be present.

     (e)  BENZENE

     Apparatus:  Effervescent Jar Assembly
                            p
     Reagents:  Alka-Seltzer ' Tablets
                Benzene Analyzer Tubes

     Procedure:

     1.   Fill the Effervescent Jar to the level mark with the water sample.

     2.   Score the tips of a Benzene Analyzer Tube with the  trianqular file
and remove.

     3.   Insert the tube into the tubina of the jar can assembly with  the
arrow oointed away from the cap.
                             p
     4.   Add one Alka-Seltzer' tablet to the .iar, screw the  cap on
immediately and allow the effervescence to no to comoletion.

     5.   Examine the analyzer tube for  an oranae, tan, brown,  or qreenish
discoloration of the white silica gel.  Since the tube is designed  for air
testing the concentration has no relation to water.  However,  the  length
of  the stain may be recorded as a relative  index of contamination.

      (f)   HEAVY METALS

     Apparatus:  Plastic Test Tube with On
                 Bottle Cap Disoenser

     Reagents:  Tris Buffer,  pH 8.0
                Chloroform
                MercuVer  2 Powder

     Procedure:

      1.   Add  2 ml  of Tris Buffer, oH 8.0  to a  new  olastic  test tube.   Fill
to  the  "WATER  LEVEL" mark with  the water  sample; cap  and  shake to  mix.

      2.   Add  1 ml  of  chloroform.
                               TM
      3.   Assemble  the  MercuVer   2 reagent .iar  with the bottle  cap  dispenser;
                                     67
-------
 add 1  shot to  the  test  tube.

      4.   Shake  for 30-40  seconds.

      5.   A negative test  is  indicated  by  the  blue-green  coloration  of
 the lower chloroform layer.  A  significantly  different  color such as
 Dink,  deep purple,  yellow or orange  indicates a  positive test for
 contamination.   Any questionable samoles  should  be  compared  with a
 distilled water  blank.

      (g)   PHENOL

     Apparatus:  40 ml  Glass-stopoered  Centrifuge Tube

     Reagents:   Buffer  Solution, Hardness  1
                 Phenol  Reagent  Powder  Pillows
                 Phenol  2  Powder Pillows
                 Chloroform

     Procedure:

     1.   Fill the  centrifuge tube to the  25 ml mark with the water  sample.

     2.   Add 1 ml of Buffer Solution,  Hardness 1 and mix.

     3.   Add the contents  of a  Phenol  Rpaqent  Powder Pillow;  stopper  and
 shake  to  dissolve.   Ignore any  precipitate which may form in  the aqueous
 layer.

     4.   Add the contents  of a  Phenol  2 Powder Pillow; stopper and  shake
 to  dissolve.

     5.   Add 1 ml of chloroform and shake  for  30-40 seconds.

     6.   An orangish to brown color or a  rose  to purple  color in the
 chloroform  layer indicates a positive  test.   A clear deep yellow color
 is  negative.  (If there is any  doubt a blank nay be run  using distilled
 water.)

     (h)   CYANIDE

     Reagents:  Cyanide Ion Hetector Tube

     Procedure:

     1.   Fill the 50 ml  beaker with 15-20 ml of water sample.

     2.   Score the  tips of the  Cvanide Inn Hetector Tube  with the triangular
 file and  remove the  tips.

     3.   Stand the  tube (red-nreen end down)  in the beaker;  the red dot is
 pointed upward.

     4.  Allow the water sample to chromatograph up the  tube.

     5.  A separation of a blue stain up the tube indicates  the orescence
of cyanide.  Other contaminants may cause the separation  of  a yellow, tan,
or gray stain on the column.
                                     68
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     Relative Measurement Tests

     (1)  PH
     Apparatus:  pH Meter

     Reagent:  Buffer, pH 7.0

     Procedure:

     1.  Set up the pH Meter assembly and soak the electode in distilled
water for at least 10 minutes before using.  The liquid function must
always be below the water level.

     2.  Standardize the meter using Buffer, pH 7.0.  Rinse the electrode
thoroughly with distilled water.

     3.  Fill the beaker with the water sample and immerse the electrode.

     4.  Set the TEMP control to the approximate temperature of the sample.

     5.  Turn the POWER switch to the ON nosition.  Record the pH value.

     6.  Turn the pH Meter off; rinse the electrode with distilled water
and soak again.

     (j)  CONDUCTIVITY

     Apparatus:  Conductivity Meter with the Conductivity weter Scale in
                 place

     Procedure:

     1.  Set the RANGE switch to position 5.

     2.  Plug the probe assembly into the 5 pin receptacle marked PROBE
INPUT in the Spectrophotometer panel.

     3.  Immerse the probe in the water sample in the 50 ml beaker, or
sampling container, sufficient to cover the vent holes.

     4.  Select the appropriate range beginning at the highest and working
down.  Each range on the meter scale corresponds to an equivalent range
position.  If the reading is in the lower 10 oercent of the scale, switch
to the next lower position.

     5.  Record the specific conductance in jjt mhos/cm.

     6.  Return the RANGE switch to off.

     (k)  TURBIDITY

     Apparatus:  Spectrophotometer set at 450 nm with the Turbidity Meter
                 Scale in place
                                    69
-------
     Procedure:

     1.  Using a sample cell filled with a  filtered water  sample  adjust
the Spectrophotorneter to read zero units using  the LIGHT CONTROL.

     2.  Replace the filtered water sample  with  a second sample cell
containing the unfiltered water sample.  Record  formazan turbidity
units  (FTU).

     3.  Turn the Spectrophotometer off.

     (1)  NITRATE NITROGEN

     Apparatus:  Spectrophotmeter set at 500 nm  with the Nitrate  Nitrogen
                 Meter Scale in olace
                        n
     Reagents:  NitraVer  V Nitrate Powder  Pillows

     Procedure:

     1.  Use the graduate to add 25 ml of filtered water sample to a
sample cell.
                                         R
     2.  Add the contents of one NitraVer   V pillow to the sample cell,
stopper and shake vigorously for 1 minute,  ft nositive test is indicated
by an amber color.   Allow 4-6 minutes for maximum color development.

     3.  Using a sample cell filled with filtered but untreated water
sample adjust the LIGHT CONTROL to give a reading of zero  units on the
SoectroDhotometer.

     4.  Replace with the cell  containing the treated water sample.
Record nitrate nitrogen in mg/2.

     5.  Turn the Spectrophotometer off.

     (m)  COLOR

     Apparatus:  Spectrophotometer set at the "F" oosition with the
                 Color Meter Scale in olace

     Procedure:

     1.  Using a sample cell filled with distilled water adjust the
Spectrophotometer to read zero units using  the LIGHT CONTROL.

     2.  Replace the distilled water with a sample cell containing the
filtered water sample.   Record units of color.

     3.  Turn the Soectroohotometer off.
                                    70
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     (n)  SULFATE

     Apparatus:  Spectrophotometer set at 450 nm with the Sulfate Meter
                 Scale in place
                        p
     Reagents:  SulfaVer IV Powder Pillows

     Procedure:

     1.  Add 25 ml  of filtered water sample to a sample cell usinq the
graduate.

     2.  Add the contents of one SulfaVerR IV nil low to the cell and
swirl to mix.  A white turbidity indicates a positive test.  Allow the
turbidity to develop for 5-10 minutes.

     3.  Using a sample cell filled with distilled water adjust the
Spectrophotometer to read zero units usinq the LIGHT CONTROL.

     4.  Replace with the cell containing the water sample.  Record sulfate
in

     5.  Turn the Spectrophotoneter off.

     (o)  PHOSPHATE

     Apparatus:  Soectrophotometer set at 700 nm with the  Phosphate Meter
                 Scale in place

     Reagents:  PhosVerR III Powder Pillows

     Procedure:

     1.  Add 25 ml  of the filtered water sample to a sample cell using  the
graduate.
                                        D
     2.  Add the contents of one PhosVer  III nillow and swirl  to mix.  A
positive test  is indicated  by a blue-violet color.  Allow  1-2 minutes  for
development.

     3.  Using a sample cell filled with distilled water adjust  the
Spectrophotometer to read zero  units  usinq the LIGHT CONTROL.

     A.  Replace with the cell  containing the water sample.  Record phosphate
in mg/a.

     5.  Turn  the Spectrophotometer off.
                                      71
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     (p)  AMMONIA NITROGEN

     Apparatus:  Soectroohotometer  set  at  425  nm  with  the Armenia Nitrogen
                Meter  Scale  in  place

     Reagents:   Nesslers  Reagent

     Procedure:

     1.   Use the graduate to  add 25 ml  of distilled water to a sample cell.

     2.   Use the graduate to  add 25 ml  of filtered water samole to a
second sample cell.

     3.   Add 1 ml  of of N°sslers Reagent to each cell  and swirl to mix.
Ammonia nitrogen is indicated by a yellow color.  Allow  to stand for 5-10
minutes for maximum color development.

     4.  Using  the sample cell  containina distilled water adjust the
Spectroohotometer to read zero  units using the LIGHT CONTROL.

     5.  Replace with cell containing the water sample.   Record ammonia
nitroqen in mg/z.

     6.  Turn the Spectrophotometer off.

     Note:   Some types of contaminants may cause a  precipitate with this
 reaction.   While it  need not be measured  it  should  be  taken  as a qualitative
 indicator  of contamination.

      (q)   CHLORIDE

      Apparatus:  Spectrophotometer set at 4fi3 nm with the Chloride Meter
                  Scale in place

      Reagent:  Ferric Ion Solution
                Mercuric Thiocyanate

      Procedure:

      1.  Add 25 ml of distilled water  to a sample cell  using a graduate.

      2.  Add 25 ml of filtered water  sample  to  a second cell using a
 graduate.

      3.  Add 1 ml of  Ferric Ion Solution to  each cell  and swirl to mix.
                                       72
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      4.   Add  1  ml  of  Mercuric  Thiocyanate to each  cell  and  swirl  to mix.
A  light  orangish  to reddish-brown  color indicates  a  oositive test.   Allov/
5-10  minutes  for  maximum  development.

      5.   Using  the distilled water samnle adjust the Snectrophotometer to
read  zero units using  the  LIGHT  CONTROL.

      6.   Replace  the  distilled water  sample  with a cell  containing  the
water sample.   Record  chloride in  mg/2.

      7.   Turn the Soectrophotometer off.

      (r)   FLUORIDE

      Apparatus:   Soectrophotometer set  at 580 nm with the Fluoride  Meter
                  Scale in  place

      Reagents:  SPADNS Reagent

      Procedure:

      1.   Add 25 ml of distilled water to  a sample cell using  the  Graduate.

      2.   Add 25 ml of filtered water sample  to a second cell  using  the
graduate.

      3    Add 5 ml  of SPADNS Reagent to each  cell and swirl to mix.  At
high  concentrations a bleaching of the red color may occur indicative  of
a Dositive test   At low concentrations this will not be perceptible
visually  but can be measured with the Snectroohotometer.  Allow to  stand
one minute for maximum development.

     4   Using the distilled water sample adjust the Snectrophotometer to
read zero units using the LIGHT CONTROL.

     5.   Replace with the cell  containing the water samole.
fluoride  in mg/2.

     6.   Turn the  Soectrophotometer off.
                                    73
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                                              OUTLINE OF ANAYLTICAL PROCEDURES
                                                  Process
General Assessment
euAppearance
b.  Color of Fil-
    tered Water

c.  Color of Sus-
    pended Matter

Spot Tests
d.Cholinesterase
    Inhibitors
e.  Benzene
 f.   Heavy Metals
     Phenol
 h.  Cyanide
 Relative Measurement
 i.  PH
Describe water sample with respect to color, turbidity,
suspended matter, slicks, etc.

Filter 50 ml of water sample with the Filter Assembly.
color.

Note color of filter from previous test.
20 ml water sample+1 ml Tris Buffer, pH 8.0 in 50 ml beaker.
Wet round end of enzyme ticket with Tris Buffer.Stand square
end in beaker for 5 min. Remove add substrate to each end.

Fill effervescent jar  to level mark with water sample. Pre-
pare tube  (ends cemoved) in head  assembly, arrow pointed out
Add Alka-Seltzer  tablet to jar,  cap Immediately.

Add  2ml Tris Buffer,  pH 8.0 to plastic tube. Fill  to level
with watan  sample.  Add 1 ml chloroform. Add 1 shot
MercuVer   2. Shake  30-40 sec.

Fill centrifuge  tube  to 25 ml  mark with water sample. Add  1
ml  Buffer  Solution  Hardness 1, 1  Phenol Reagent  pillow and 1
>henol  2 pillow.  Add  1 ml  chloroform.  Shake 30-40  sec.
 Ignore  ppt in water.

 Add 15  ml  water sample to  50 ml  beaker.  Cyanide  tube (ends
 removed)  stood  up in  beaker,  red  dot up.  Allow  to  chromato-
 graph.


 Soak electrode for 10 min. in  distilled water.  Set approxi-
 mate temperature. Standardize with Buffer, pH 7.0. Measure
 and record pH of water sample. Rinse electrode,  soak in
 distilled water.
jave reference sample in plastic tube.
Save filter for next test.

Save filter for reference.
After 2 min. round end (control)
should be blue. Positive test
if square end  is white.

Allow effervescence to finish.
Positive test  if white gel turns orange,
tan, brown  or  greenish.

Positive test  (chloroform  layer) is
pink, deep  purple, yellow  or  orange.
Neqative test  is blue-green or  gray.

Positive test  (chloroform  layer) is
oranqe  to  brown  or  rose  to purple.
Neqative test  is deep yellow.
 Blue stain if cyanide is present.
 Other contaminants yellow, tan or gray.
-------
                         Tests
                          Process
Comments/Interpretation
             Relative Measurements  (Con't)
             J!Conductivity
Plug probe into PROBE INPUT. Set RANGE to position 5.
Immerse probe in water sample to cover vent holes. Switch
to lower range until a reading is obtained. Record value.

Spectrophotometric Tests
Note:Tests requiring reagents should use water volumes measured with 25 ml
       graduate. Minimize on-time of spectrophotometer. Turn off after each reading.

k. Turbidity

1. Nitrate
Nitrogen

m. Color


n. Sulfate


0. Phosphate


p. Ammonia
Nitrogen

q. Chloride


r. Fluoride


Wave
Length
450

500


F


450


700


425


463


580


blank
Cell
Filtered
Sample
Filtered
Sample

Distilled
Mater

Distilled
Water

Distilled
Water

Distilled
Water *•
Reagent
Distilled
Water +
Reagents
Distilled
Water +
Reagent
Sampl e
Cell
Unfiltered
Sample
Filtered
Sample +
Reagent
Filtered
Sample

Filtered
Sample +
Reagent
Filtered
Sample +
Reagent
Filtered
Sample +
Reagent
Filtered
Sample +
Reagents
Filtered
Sample +
Reagent
Process
Read directly, record value.

Add 1 NitraVerRV oillow.
Shake 1 min. Allow to stand 4-6 min.
Record value.
Read directly, record value.

o
Add 1 SulfaVer IV oillow. Swirl to
mix. Allow to stand 5-10 min. Record
value.
Add 1 PhosVerRIII oillow. Swirl to
mix. Allow to stand 1-2 min. Record
value.
Add 1 ml Nesslers Reagent. Swirl to
mix. Allow to stand 5-10 min. Record
value.
Add 1 ml Ferric Ion Solution. Add 1 ml
Mercuric Thiocyanate. Swirl to mix.
Allow to stand 5-10 min. Record value.
Add 5 ml SPADNS. Swirl to mix. Allow
to stand 1 m1n. Record value.

Comments/ Interpretation


Amber color indicates a
positive test.




White turbidity indicates a
positive test. Clean cell
with soap and water.
Blue-violet color indicates
positive test.

Yellow color indicates a
positive test. Ppts may
form with some contaminants.
Lt. orange to reddish brown
color indicates a positive
test.
Bleaching may occur at high
high cone, not perceptible
at low cone.
Gl
-------
                                                 SECTION V

                                         CONSUMABLE MATERIALS
Cat No
wQ w • I1W •
2387-20
151-13
2125-99
14034-99
12065-99
1836-99
424-16
444-16
872-99
2062-32
Gastec No. 121
Description
Mercu Ver™2
Nesslers Reagent
Phos VerR III Powder Pillows
Nitra VerR V Powder Pillows
Sulfa VerR IV Powder Pillows
Phenol 2 Reagent Powder Pillows
Buffer Solution, Hardness 1
SPADNS Reagent
Phenol Reagent Powder Pillows
Reference Electrode Filling Solution
Benzene Detector Tube
Unit
1 oz.
4 02.
pkg of
100
pkg of
100
pkg of
100
pkg of
100
qt
qt
pkg of
100
2 oz.
pkg of
10
Unit
Price
$5.25
2.85
8.00
6.95
6.50
6.00
4.00
6.60
15.00
2.35
7.20
Source
Hach Chemical Co.
P.O. Box 907, Ames, IA 50010
Hach Chemical Co.
Hach Chemical Co.
Hach Chemical Co.
Hach Chemical Co.
Hach Chemical Co.
Hach Chemical Co.
Hach Chemical Co.
Hach Chemical Co.
Hach Chemical Co.
National Environmental Instruments, In<
P.O. Box 590, Warwick, RI 02888
8104-204
Detector Tube,  Kitagawa Cyanide Ion
pkg of   15.00
  10
Matheson Gas Products
P.O. Box 85, East Rutherford,  NO  07073
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                                                   SECTION V
                                       CONSUMABLE MATERIALS (continued)
Cat. No.
61693
Description
Prefilters, Type A Glass Fiber, 25 mm
Unit
pkg of
500
Unit
Pri ce
$15.00
Source
Gel man Instrument Co.
600 Sourth Wagner Road
FSN 6665-00-909-
    3647
                   Shell Container, Clear cellulose acetate,
                   3/8  in. diam x 3-% in. length
Printing for above, single line 1/32 in.
wide around circumference 1-3/16 in. from
top (open end) and the words "WATER LEVEL"
in parallel slightly above the line.

Plug, natural polyethylene, for 3/8 in.
diameter shell container

Refill Kit, Chemical Agent Detector,
ABC-M30A1
1000



1000




1000


each
        Ann Arbor, MI  48106

15.72   Flex Products Corp.
        445 Industrial Road
        Carlstadt, NJ  07072

10.30   Flex Products Corp.
                                                                                   3.62   Flex Products  Corp.
20.57   Headquarters, ARMCOM
        AMSAR-MMD-L
        Rock Island, IL  61201
                   Buffer, pH 7.0

                   Chloroform

                   Dye Marker

                   Liquid Soap (Phosphorous - free)
                     Chemical  Supply House

                     Chemical  Supply House

                     Chemical  Supply House

                     Chemical  Supply House
-------
                                                    SECTION V
                                       CONSUMABLE MATERIALS (continued)
    Cat.  No.
oo
            Description
Alka-SeltzerR (Without Aspirin)

Battery, 6.75 V, Mallory TR-235R
Battery, 1.5 V, D Size, Alkaline
Battery, 1.5 V, AA Size, Alkaline
Distilled Water
Tris Buffer, pH 8.0
Ferric  Ion Solution
Mercuric Thiocyanate  Solution
                                                                   Unit
                                                         Unit
                                                         Price
pkg of
20
each
each
each
$ .60

5.85
1.00
.75
         Source
Drugstore

Electronic Supply House
Electronic Supply House
Electronic Supply House
Laboratory
Laboratory
Laboratory
Laboratory
-------
                               REFERENCES


Silvestri, A., Goodman, A., McCormack, L. M., Razulls, M. K.,  Jones, A. R.,
Jr. and Davis, M. E. P.  Development of a Kit for Detecting Hazardous
Material Spills in Waterways.  Interagency Agreement No. EPA-IAG-0546.
Chemical Systems Laboratory, ARRADCOM, Aberdeen Proving Ground, MD  21010.

Hach Direct Reading Engineer's Laboratory, Model DR-EL/2, Methods Manual.

Laboratory pH Meter, Model 1975 and 2075.
                                    79
-------
                                   TECHNICAL REPORT DATA
                            (Please read Instructions on the reverse before completing)
|1. REPORT NO.
 EPA-600/2-78-055
                                                           3. RECIPIENT'S ACCESSION-NO.
M. TITLE AND SUBTITLE
\ Development of a Kit for Detecting Hazardous  Material
\ Spills  in  Waterways
                                                           5. REPORT DATE
                                                            March  1978  issuing date
                                                           6. PERFORMING ORGANIZATION CODE
57. AUTHOR(S)
 A. Silvestri,  A.  Goodman, L.M. McCormack,  M.  Razulis,
 A.R. Jones,  Jr.,  and M.E.P. Davis
                                                           8. PERFORMING ORGANIZATION REPORT NO.
 9. PERFORMING ORGANIZATION NAME AND ADDRESS
 Chemical Detection and Alarms Branch
 Chemical Systems  Laboratory
 Aberdeen Proving  Ground, Maryland   21010
                                                           10. PROGRAM ELEMENT NO.
                                                             1BB610
                                                           11. CONTRACT/GRANT NO.
                                                                 EPA-IAG-0546
 12. SPONSORING AGENCY NAME AND ADDRESS
 industrial Environmental Research  Lab.  - Cinti, OH
 Office of Research and Development
 U.S. Environmental Protection Agency
 Cincinnati,  Ohio  45268
                                                           13. TYPE OF REPORT AND PERIOD COVERED
                                                             Final	
                                                           14. SPONSORING AGENCY CODE
                                                                EPA/600/12
 15. SUPPLEMENTARY NOTES
 16. ABSTRACT
 Chemical Systems Laboratory, under a program sponsored by the Environmental Protection
 Agency, Edison,  N.J.  has developed a kit  to  detect hazardous material  spills into
 waterways.   The  purpose of the program was to develop a man-portable field kit able to
 detect  (not  necessarily identify) as many contaminants in water in  as  low a concen-
 tration as possible.

 A list of compounds,  representative of potential contaminants, was  used  to evaluate
 commercial,  military  and specially designed  procedures which have application to water
 testing.  Following the original screening,  promising methods were  further evaluated
 against samples  of natural waters polluted in the laboratory with compounds from the
 model list.   It  was concluded that a selection of 15 multiple non-specific detection
 systems could be organized into a detection  concept which would detect a significant
 portion of potential  contaminants.  A "paper analysis" projected that  about 85% of
 potential contaminants would respond to at least one detection parameter.
 A field kit  was  designed containing a spectrophotometer,  conductivity  meter, pH meter
 and a variety of accessory equipment and  reagents.  Prototype kits  were  fabricated
 and delivered to Environmental Protection Agency along with engineering  drawings,
 parts lists  and  manuals.
 7.
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
                                              b.lDENTIFIERS/OPEN ENDED TERMS C.  COS AT I Field/Group
  Hazardous Materials,   Detection,  Kits,
  Chemical Analysis,  Water Pollution
  Water Analysis,  Spot  Tests
                                              Hazardous Materials
                                              Spill Detection
      68D
 8. DISTRIBUTION STATEMENT
 Release  to Public
                                             19. SECURITY CLASS (ThisReport)
                                              Unclassified
21. NO. OF PAGES
     88
                                              20. SECURITY CLASS (This page)
                                              Unclassified
                                                                         22. PRICE
EPA Form 2220-1 (9-73)
                                            80
                                                     U.S. GOVERNMENT PRINTING OFFICE: I 978-757-HO/6805 Region No. 5-I I
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