NEIC
        NEIC PESTICIDE SAMPLING GUIDE
        August 1985
       National Enforcement Investigations Center, Denver
U.S. Environmental Protection Agency
                                   Office of Enforcement

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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT AND COMPLIANCE MONITORING
NEIC PESTICIDE SAMPLING GUIDE
August 1985
Robert F. Schneider
 NATIONAL  ENFORCEMENT  INVESTIGATIONS  CENTER

 Denver, Colorado

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                            ABSTRACT
     This  guidance  manual  describes equipment  and  methods  for
sampling  pesticides.    Included  are procedures  for  collecting
representative  samples  of  pesticide  products  for  formulation
evaluation as  well  as methods  for  collecting  environmental  sam-
ples  to  be  analyzed  for  suspected  pesticide residues.   Also
included are brief  discussions  on container preparation, packag-
ing,  storage,  labeling,  recordkeeping and  safety.   The Appendix
contains  a summary  of sampling and  packing  methods  for specific
agricultural  commodities  to be analyzed for food or feed pesti-
cide tolerances.

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                         ACKNOWLEDGMENT
     This  manual  represents  the  third  edition  of a  pesticide
sampling guide  published by the  National  Enforcement  Investiga-
tions Center  (NEIC).   Sincere appreciation  is  expressed  to Dean
F.  Hill,  Chief,  Pesticides  and  Toxic Substances  Branch  at NEIC
for his  review, suggestions  and  criticisms in the preparation of
this document.  Gratitude  is expres-sed to Marcia Colvin and Ilia
Schipporeit of the  Information  Services  Branch at NEIC for their
assistance with photographic work  and the  final  preparation of
the manual.

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                           DISCLAIMER
     Mention of  trade names  or  commercial products  and sources
does not constitute  endorsement  or recommendation for use by the
U.S. Environmental Protection Agency.

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                                 CONTENTS

INTRODUCTION .............................      l

  CONTAINER PREPARATION  .......................      \
  PACKAGING AND STORAGE  .......................      *
  LABELING ..............................      ;
  RECOROKEEPING  ...........................      J
  SAFETY ...............................      3

FORMULATION AND USE DILUTION .....................      7

  PESTICIDE LABEL  .........................      J
  FORMULATION (BULK SAMPLES. DRY MATERIAL) ..............      /
  FORMULATION (BULK SAMPLES. LIQUID MATERIAL)  ............      9
  FORMULATION (RETAIL-SIZED UNITS. DRY OR LIQUID)  ..........     11
  USE DILUTION ..........................     11

RESIDUE  ...............................     14

  SURFACES ..............................     }*
  WATER (STREAMS AND OTHER SURFACE WATER)  ..............     17
  WATER (SURFACE SLICKS) ......................     «
  WATER (TAP OR WELL)    ......................     "
  SOIL ............................     "
  SEDIMENT .............................     **
  PLANTS ...............................     tn
  ANIMALS  ............................     *
  AIR (PESTicioE DROPLET DRIFT)   ...................    34
  AIR (PESTICIDE VAPOR DRIFT)     ..................    3/


APPENDIX

SAMPLING AGRICULTURAL COMMODITIES  TO DETERMINE PESTICIDE TOLERANCE
  COMPLIANCE
 FIGURES

  1   Grain  Sampler and  Disposable  Plastic  Tube  	     8
  2   Vacuum Pump Syphon Device	      •    •      	     "?
  3   Swab of Template Area 	     "
  4   Hand-dipped Sampling Jar  	     |'
  5   Weighted Water Bottle Sampler       .  -              	     |»
  6   Sampling With a Saturation Pad  	     "
  7   C-18 Extraction Column  	     "
  8   Vacuum Pump Syphon Device    	      	     "
  9   Soil Sampling With a Spatula       	     £7
 10   Phelger Corer           	      	     ?g
 11   Eknan  Grab  . .      .       	     2«
 12   Vegetation Sampling Gear  	     "
 13   Animal Sampling Gear    	     "
 14   Sling  Psychrometer                •        	     "
 15   Wind Meter  .               	     "
 16   Droplet Indicator Paper         ...     •  •        	     ^
 17   Puf Column  .                     	     ,£
 18   Constant-flow Vacuum Pump With Puf Column   .      	      •»»

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                               INTRODUCTION

     This is the  third  edition of the National  Enforcement Investigations
Center  (NEIC)  Pesticide Sampling Guide.   Procedures in this  edition  are
presented in the  format established in earlier  editions published by  NEIC
in 1975  and  1981.   Sampling techniques are arranged in  sections  titled:
Formulation and Use Dilution and Residue.   The Residue  section is  subdivided
into topics  on  surfaces,  water,  soil, sediment, plants, animals and air.
Each section describes appropriate sampling methods, lists  needed  apparatus
and  then presents a  step-by-step procedure  for  sampling.   Procedures
described are  based  on current  sampling practices  by  Federal  and State
inspectors involved in agricultural  or structural  pesticide investigations.

     The methods  represent  state-of-the-art  techniques;  however,  sampling
technology and pesticide use patterns are revised  constantly so the user of
this guide is  encouraged  to suggest and forward changes or additions to:

     Robert F.  Schneider, Senior Scientist
     EPA - National Enforcement Investigations Center
     Denver Federal Center,  Box 25227
     Denver,  Colorado  80225
     (303) 236-5120
     FTS 776-5120

     Before  sampling,  there are  certain  responsibilities  the pesticide
inspector must consider.  Foremost,  is determining if sampling is  necessary
to document  a  suspected situation such as  a violation  of Federal  or State
laws, environmental  harm  or health  risks.   Laboratory  analyses are  time
consuming and costly.   If analyses  are not needed  to  document an issue,
samples  should  not be collected.  In  regulatory work, negative results may
undermine an otherwise  solid  case,  especially in  the event of a long  time
lapse between  an incident and sampling.   If  sampling  is necessary, the
inspector must decide whether to collect samples from the pesticide product,
the environment or both.

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     Typically, samples fall  into two categories:   those related to  product
quality and those associated with use investigations.   Product quality sam-
ples include those  from  businesses  that manufacture,  formulate or process
pesticides (producers) and those  from businesses  that wholesale or  retail
pesticides (dealers).   In product-quality studies, formulation  or  high-
residue samples of  the pesticide product are the type collected typically.
Use-investigation samples  include  those from  environmental  monitoring,
experimental  use permits, use or misuse investigations and accident  or inci-
dent reports.   In use  studies,  trace or low-residue environmental samples
(soil,  vegetation,  water,  etc.) are the type  collected  but  occasionally
formulation samples  are needed also  for complete documentation.

     Authority, employee  conduct,  custody and  related  administrative or
legal  issues are  also  the responsibilities of  inspectors; however,  these
are beyond the  scope of  this  document.  Once the decision has been made to
collect a pesticide or its suspected  residue,  the  inspector must  determine
how to collect a representative sample, how many samples to collect, how to
prepare the sample properly and how to package and preserve it for shipment
to the laboratory.  Although these issues are discussed in each of the pro-
cedures presented in this manual, general considerations of container prep-
aration,  packaging  and storage, labeling  and  recordkeeping  are repeated
here for emphasis.

CONTAINER PREPARATION

     Residue or formulation subsamples should not be in contact with rubber
or non-teflon  plastic.   Organic material can leach from rubber or plastic
into samples causing contamination,  or pesticides can absorb into or adsorb
onto rubber and plastics.  In both cases, analytical results may be  invali-
dated.   To avoid preparation problems, samples must be collected with clean
tools  (preferably of glass or stainless  steel)  and placed  into  clean  glass
jars or  acetone-washed  aluminum foil.  Never  place samples directly  into
plastic bags or plastic  bottles.   Bottle  caps  or  jar lids must be lined
with foil or teflon.

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     For  proper  pre-cleaning of sample containers,  consult  the chemist.
Generally, the cleaning method consists of flushing  inner surfaces of con-
tainers (bottles  or  foil)  including lined lids with appropriate solvents.
An ounce  of  solvent  (acetone or equivalent) per  pint-sized  container  is
usually sufficient.  Allow  the  container  and lid to dry thoroughly before
use.   Solvent rinse  should  be properly discarded with other wastes; do not
reuse it.

PACKAGING AND STORAGE

     Separate containers should be used for each sample  or subsample unless
composite-type sampling is  preplanned by  the inspector and chemist.  After
samples are placed into clean bottles,  jars or foil, they can be tagged and
sealed in plastic bags to comply with identification and custody procedures.

     Many samples  require chilling  or  freezing to prevent degradation en
route to the analytical laboratory.   Inspectors should discuss with chemists
the specific preservation requirements  for samples.   Generally, an ice or
picnic-type chest with crushed ice is satisfactory to maintain samples  below
40° F.  A similiar-type chest with  heavy  paper-wrapped dry ice  is suitable
to hold temperatures  below  10°  F.,  if  necessary.   For safety, never place
dry ice in glass  or air-tight containers.

     Sample shipping time should be minimized.   Quick delivery to the labor-
atory is  necessary to meet  prearranged analytical  schedules  and holding
time (storage) requirements.

LABELING

     Identification tags,  labels or seals  attached to samples vary in format
but all  must have at least the following information:  sample number, date,
contents and collector's name or initials.  This minimal  information should
be supplemented by detailed  logbook information about the sample.

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RECORDKEEPING

     Bound logbooks are used to record detailed information about samples.
The format of recordkeeping varies for formulation,  use-dilution and residue
samples but,  at minimum,  the following is required:

          Sample Site Identification

               general  location
               specific location

          Date and Time Period  of  Sampling

          Sample Description

               container  contents  (specific material  collected)
               name of  pesticide or residue suspected for which  analysis is
               needed
               reason for collection
               quantity (volume, number,  weight)
               identity of related samples (formulation  and related  residue
               samples)

          Sampling Method

               composite  or grab
               instruments, devices and tools  used
               area, depth and  related facts
               purge time and volume (well water)
               precleaning tools and cleaning  between uses

          Storage and Shipping

               container  type and  precleaning
               packaging  routine
               preservation
               transport  method (date and time)

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          Other Documentation

               maps
               field record sheets
               custody and document control  records
               books and records
               photographs
               statements or affidavits
               technical and professional  remarks
SAFETY
     Safety is an  aspect  of pesticide sampling too often ignored.  It is
the responsibility of  inspectors  to protect themselves and others during
pesticide handling and sampling activities associated with an investigation.
Each sampling procedure described  in this manual  poses a degree of health
and safety risk.   To  minimize this risk, protective  clothing  and safety
equipment must be used by inspectors.   The protective gear must be adequate
to prevent accidental  exposure to  pesticides through  eyes, nose, mouth and
skin.   For specifics,  inspectors should  refer to the  precautions described
on the labels of pesticides being  handled and sampled  in addition to being
fully acquainted  with safety  protocols  issued by their Agency.   For  a
detailed discussion on safety,  inspectors are encouraged to refer to the
EPA Pesticide Inspectors Manual.*

     Procedures described in the following pages can be impacted by analyti-
cal requirements, quality control considerations and other technical  factors;
therefore, the inspector and chemist should discuss proposed sampling before
field work begins.   A good synopsis of the value of proper sampling is  pre-
sented in the  1979 EPA Sample Collection Manual published by the Benefits
and Field Studies  Division,  Office of Pesticide Programs,  Washington,  DC.
     Dellavecchia, Anthony J.,  et al.,  1975,  "Pesticide Inspection Manual",
     U.S. Environmental Protection Agency:  Section 21, SAFETY,  8pp.

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     "No chemical analysis can be better than the sample on which
it is based.  The task of procuring a representative sample pre-
sents a challenge,  first  to the sampler in  the  field,  then to
every person involved with that sample until  the final  analytical
results are known."

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                       FORMULATION AND USE DILUTION

     This section  describes  the  apparatus and procedures for subsampling
bulk containers of formulation pesticides from the producer, marketplace or
user, as well  as diluted pesticides from  the user.  Some of the procedures
described are  from the  EPA Pesticide  Inspectors  Manual*  while others are
based on  current  practices  of  State  and Federal  pesticide inspectors.

     Every ounce of formulated or diluted pesticide cannot be collected and
analyzed; therefore, sampling must be  designed so all  portions of the pesti-
cide have an equal  chance  of being examined.  Procedures discussed in this
section take into account this scientific approach of random sampling which
maximizes the  possibility  of  obtaining  representative samples.   Equipment
and miscellaneous supplies needed for  formulation and use-dilution sampling
range in cost from $10 to $125.

PESTICIDE LABEL

     A duplicate label must accompany  each formulation or use dilution sample.
To avoid misbranding, never  remove labels from  bulk  containers.   Bin or
file copy label  is satisfactory  if a word for word comparison is made to
ensure it is identical with the  label on  the container sampled.   If  labels
are unavailable, a legible photograph  of the container label should be sub-
mitted with the sample.

FORMULATION (BULK SAMPLES. DRY MATERIAL)

     Subsampling of bulk  containers  is  usually  recommended because:   (1)
the cost of larger amounts is frequently prohibitive,  (2) larger size units
are difficult  to handle and costly to ship and (3) the increased  amount of
material left  over after  testing may create disposal  problems.  Therefore,
dry products in containers in excess of 40 pounds are usually subsampled at
the inspection site.  Use discretion if you feel  there is reason to deviate
from these guidelines.
     De2Iavacchia, Anthony J., et al., 1975, "Pesticide Inspection Manual",
     U.S.  Environmental Protection Agency:   22 Sections  and Appendix.

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           FIGURE 1.   GRAIN SAMPLER AND DISPOSABLE PLASTIC TUBE
Apparatus
     1.    Acetone-washed grain sampler or previously unused, disposable-type
          plastic tube (Fisher Grain Sampler, Stock No.  14-208, Fisher Sci-
          entific,  711  Forbes  Avenue,  Pittsburg,  Pennsylvania   15219)

     2.    Widemouth glass pint or quart jars with teflon-lined lids

     3.    Data sheets and identification tags

     4.    Labeled shipping container
Procedure
     1.   Lay the bag of pesticide on its side.

     2.   Insert closed metal grain sampler or plastic tube diagonally into
          the bag through the seam at the top corner.

     3.   Push  the  closed  sampler or  tube  to  the  opposite  bottom corner  of
          the bag.  By opening and closing the sampler or  filling the tube,

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          collect a  representative  sample  of the material from different
          sections of the bag.

     4.   Carefully withdraw the sampler or tube containing sampled material.

     5.   Transfer dry material into glass  jar;  label  and prepare  for ship-
          ment to the  laboratory.   Collect about a pound (a pint) for low
          concentration fertilizer-pesticide combination products.   Collect
          at  least  4 ounces for wettable  powders  or  other concentrates.

     6.   Samples from the same batch or lot code may  be composited.   Samples
          from different codes must be packaged  separately.

Comments

     Avoid cross-contaminating  samples  by  cleaning or replacing sampling
tools between each  sampling use.   If  a  plastic  tube is used to collect the
sample, it should be destroyed by cutting and disposed of in a satisfactory
manner.  Because the grain sampler is a reusable tool, it should be acetone-
washed and rinsed with water before continuing its use for additional samples.

     If the dealer,  producer  or agent  requests  a  duplicate sample,  it is
collected, identified  and  sealed  in the same manner  as  described above.

     For detailed information  on  resealing (restoring) the bulk container,
obtaining bin label  copies,  and preparing  appropriate paperwork,  see EPA
Pesticide Inspection Manual, Section 12, pp. 6-8.

FORMULATION (BULK SAMPLES. LIQUID MATERIAL)

     Subsampling  is  recommended  for  liquids  in containers in excess of
1 gallon.  Smaller  volumes can either  be  taken  as a  unit or thoroughly
shaken and poured  into an appropriate sample container.   Various types of
siphon devices or chemically-cleaned glass  tubes (glass thief) are typically
used to collect bulk-stored liquids.

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                                                                         10
                   FIGURE 2.   VACUUM PUMP SYPHON DEVICE
Apparatus
     1.    Acetone-washed glass  tubing  or  a siphon device with disposable
          hose (Hand-operated vacuum pump, Stock No.  TR-6513-00,  Cole-Parmer
          Instrument Company.  7425 N.   Oak Park Ave.,  Chicago,  Illinois
          60648)

     2.    Glass pint or quart bottle with teflon-lined lid

     3.    Data sheets and identification tags

     4.    Labeled shipping container with appropriate packing, as stipulated
          by DOT regulations
Procedure
     1.   Thoroughly  agitate  liquid  material  by rolling and  shaking  can,
          barrel or drum before sampling.

     2.   Insert siphon hose or glass tubing (thief) through open pour hole
          in bulk container.

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                                                                         11
     3.    Collect a composite sample from three depths;  near bottom,  middle
          and at top of liquid level.   If sediment,  layering or  phase sepa-
          ration is observed, collect a duplicate sample.

     4.    Collect at least 4 ounces from concentrated products and 8  ounces
          from diluted products where active ingredients are less  than 10%.

     5.    Transfer liquid sample  into  glass sample  container,  then seal,
          tag and pack for shipment.

     6.    Properly dispose of  hose.   Reclean  sampling tools with acetone
          and rinse with clean water before collecting additional  samples.

FORMULATION (RETAIL-SIZED UNITS. DRY OR LIQUID)

     Container  sizes  in this category are  usually  1-gallon or  less  for
liquids  and 40 pounds or less for dry-granular material.   Often, the entire
container randomly selected  from  a  lot can  be  purchased from the  producer,
dealer or user.   Details for payment and related paperwork are  presented in
the EPA Pesticide Inspection Manual, Section 13, pp.  7-8.   If it is necessary
to subsample a retail-sized unit, follow the procedure described previously
for either dry or liquid bulk sampling.

     Collect enough retail units to equal 8 ounces for concentrated products
with more than 10% active ingredients.   Collect 16 ounces for products with
single active ingredients  of 10% or less.  At least four pressurized con-
tainers should  be  obtained to  provide  an  adequate sample  size for chemical
analyses of the product.

USE DILUTION

     Most of  this  type material  is  in  liquid  form  (water or occasionally
oil).  Analytical results of use-dilution samples will identify the product,
cross-contamination of  products  and  relative  strength of  diluted  material.
Sampling and  analysis  of material from a service container or application

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                                                                         12
tank will seldom  document  that materials were mixed and diluted properly.
Documentation of  proper  mixing should be obtained  through  interview  and
observation techniques;  sampling  is  seldom  required if this  is  the  sole
purpose.

Apparatus

     1.    Siphon  device  with  disposable  tubing  (Stock No.  TR-6513-00,
          Cole-Parmer Instrument Company, 7425 N.  Oak Park Ave., Chicago,
          Illinois  60648)

     2.    Glass pint or quart bottle with teflon-lined lid

     3.    Data sheets and identification tags

     4.    Labeled shipping container  with appropriate  packing to meet DOT
          regulations.

Procedure

     1.    Thoroughly agitate liquid in service container or tank (as  appro-
          priate, operate mechanical  agitator  to  assure adequate mixing).

     2.    For aerial  application  sampling,   collect use-dilution samples
          from spray boom  nozzles.   Following  actual application, loosen
          boom nozzle and drain the pesticide mix into a glass sample con-
          tainer.    (Previous  aircraft movement usually assures  complete
          pesticide mixing.)

     3.    For service  containers  or tanks,   insert  siphon  tubing through
          fill opening or collect  a well-mixed sample from the drain  system.
          In some cases,  a  sample  from a service  container can be collected
          by directing nozzle spray into a collection bottle.

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                                                                         13
     4.   To assure randomness, collect a composite sample from three depths;
          near bottom, middle  and  at top of the liquid level or from dif-
          ferent drain points on the rig.  Collect at least a pint of pesti-
          cide mix.

     5.   Transfer liquid  sample  into  glass sample container, then seal,
          tag and pack for shipment.

     6.   Properly dispose of  used  tubing and reclean other  sampling tools
          with acetone and rinse  with  clean water before collecting addi-
          tional samples.

Comment

     If proper agitation of the use-dilution sample is in question, collect
the  sample  by  the siphon technique.  A  drain  sample of poorly agitated
liquid in a  tank usually  is  not representative of the tank  contents.   If
severe undermixing (settling or separation)  is suspected, collect  a sample
of dilutent  and  a  sample of the parent formulation.  With these additional
samples,  the chemist can perform a stability test on the mixture and provide
quantitative results on the  formulation  product.   If the sample container
has a rubber or paper gasket,  a piece of acetone-washed aluminum foil should
be placed between  the cap  and  bottle to  avoid contact of the liquid sample
with the rubber or paper.   Consult the  chemist for advice on preserving the
sample during transport to the laboratory.

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                                                                         14
                                  RESIDUE

     This  and  following sections  describe  the  apparatus  and  procedures  for
pesticide  residue  sampling.   Because the enforcement goal of residue sam-
pling  is  to document human  health and  environmental  problems or  risks,  the
procedures  presented emphasize  collecting  the fewest samples from highly
suspect areas of potential pesticide contamination.

SURFACES

     To determine  the extent of application coverage or contamination  of
surfaces, a technique known as wipe or swab sampling is often used.

     Measured  non-porous  areas, such as finished  wood,  tiles,  linoleum,
metal  and  glass, are swabbed  with an absorbant paper wetted with an appro-
priate solvent  to  remove  the compounds of interest from the surface.   The
absorbant paper  is  packaged and transferred to the  laboratory,  extracted
with solvent and analyzed by  gas  and/or  liquid chromatography.   Concentra-
tions  are  normally  reported  either as weight (usually micrograms) per unit
area or weight per swab.

     Porous areas,  such as  carpet or drapes,  can be sampled with the same
technique to provide qualitative identification of pesticide application or
contamination.

     Inspectors should  wear  impervious  disposable gloves, either nitrile,
vinyl  or  latex.  Iso-octane and isopropanol are relatively non-toxic; how-
ever, care should be taken to minimize respiratory and skin exposure.   Both
solvents are flammable; thus, care should be taken when using these  solvents
around pilot lights,  lit  burners,  contact switches, cigarettes and other
sources of  ignition.   Absorbant pads (swabs)  should not  be  handled  with
bare hands, but with clean gloves  or decontaminated forceps.   Chlordane and
heptachlor  are  suspected  carcinogens and should  be  handled  accordingly.

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                                                                         15
     The technique described  here  and additional information on storage,
extraction and related analytical methods can be found in the NEIC publica-
tion Sampling and Analysis of Surfaces for Pesticides and PCBs.*
                     FIGURE 3.  SWAB OF TEMPLATE AREA
Apparatus
     1.   Absorbant pad, 10 cm x 10 cm [Stock No. 7588 - Alltech Associates,
          Waukegan Dr.,  Deerfield,  Illinois  60015 (available in boxes of
          100)].

     2.   Isopropanol  (pesticide  or  reagent grade).  Consult chemist  for
          other suitable solvents.

     3.   Screwcap 40  ml Volatile  Organic Analysis  (VGA)**  vials with
          teflon®-lined  septum

     4.   Disposable gloves  of  latex (Markson 17118),  nitrile  (Fisher 11
          394 23A) or  vinyl (Bard-Parker H8294-002510)
 *   Hill, Dean,  1984,  "Sampling and Analysis  of  Surfaces for Pesticides
     and  PCBs",  National  Enforcement Investigations Center, U.S. Environ-
     mental Protection Agency, Denver, Colorado, 7 pp.
**   Vials 28mm 6y 98mm, No. 22483; caps, open-top screw type,  size 24-400,
     No.  240518;  cap  liners,  Telfon®-faced silicone,  24  mm No.  240588;
     wheaton Scientific, Nillville, NJ   08332
®    Telfon is a registered trademark; hereinafter shown with ®.

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                                                                         16
     5.   Eye-dropper bottle  filled with appropriate  solvent  (isopropanol,
          iso-octane, etc.)

     6.   Disposable template with 10 x 10 cm  square  (4"  x 4") opening cut
          from cardboard

     7.   Plastic bag for used gloves and other onsite disposables

     8.   Data sheets,  tags and shipping containers

Procedure

     1.   Fold a 10-cm-square absorbant pad into a 2.5 cm-square.

     2.   Grasp the two inner pockets formed in folding with freshly gloved
          fingers.

     3.   Wet both external surfaces of pad with isopropanol  or other appro-
          priate solvent  (do  not  use solvent when  surface to  be sampled  is
          visibly wet;  simply blot liquid within measured area).

     4.   Place template on surface to delineate area to be sampled.

     5.   Blot 10 cm square area horizontally with one side of the wet swab
          and then vertically with the other.   Blot uniformly at least five
          times in each direction.

     6.   Carefully roll  the  sample swab into  a cylinder with exposed, wet
          areas inside.

     7.   Insert rolled swab  into VOA  vial and cap with teflon-lined lid.

     8.   Seal, tag and prepare for transport to laboratory.

     9.   Place used  template and gloves  in plastic  bag and dispose of
          properly.


Comments


     It is possible  that  dirt or finishes, such as wax, paint, lacquer or

other debris, could give rise to analytical interferences.  Blotting versus
wiping  or  rubbing  is recommended  to  minimize  inadvertent collection of

debris  and to  maximize  uptake of the pesticide.   For quality control, at
least one side-by-side  duplicate  should be taken  for each  surface type.

Also,  it is  desirable  to  obtain a background  sample  from an  untreated or

"clean" area of the same surface composition as  the area  of interest.

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                                                                         17
WATER (STREAMS AND OTHER SURFACE WATER)

     A common method  for collecting water  from ponds, lakes and streams is
by dipping  the  sample bottle to obtain water at or near the surface.  This
technique is effective because many pesticides,  especially oil-based,  remain
on the water  surface.   If physical conditions, such as inaccessible shore-
line, preclude  the  dip  method  or, if subsurface water samples are needed,
alternate methods are available  using a sampling jar attached to a tele-
scoping pole, hand pumps, or weighted water samplers.   Consequently, equip-
ment costs  vary from  less  than $1 for a sample  jar to $250 for commercial
water-sampling devices.
                    FIGURE 4.  HAND-DIPPED SAMPLING JAR

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                                                                         18
                 FIGURE 5.   WEIGHTED WATER BOTTLE SAMPLER
Apparatus
     1.    Widemouth glass  jar  with teflon-lined lid for use  as  sampling
          device and/or sample container

     2.    Hand  pump or weighted water sampler  (Van  Dorn,  Kemmerer,  APHA
          sampler) for subsurface sampling or situations where bottle cannot
          be dipped

     3.    Ice for chilling samples

     4.    Data sheets, identification tags and shipping container

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                                                                         19
Procedure

     1.    Dip, pump or  otherwise  collect a minimum of a quart (950 m£) of
          water into a clean glass jar (never use plastic bottles).  Collect
          a duplicate sample for quality control analysis.

     2.    Avoid collection of bottom sediment; guard against roiling sediment
          when collecting a subsurface water sample.

     3.    Each sample  container should  represent a single  sample  location.
          Submit an unused  sample jar and  lid to the chemist as a  blank for
          quality control analysis.

     4.   Seal,  tag and  pack  glass  jars to comply with  shipping needs.
          Typically, water  samples should  be  kept  on  ice and protected from
          direct  sunlight.   Consult chemist for  special  preservation  and
          holding  time  precautions.

 WATER  (SURFACE SLICKS)

      If shallowness precludes  dipping  a bottle to collect a slick on the
 surface of  the water,  the preferred  method is the saturation pad  technique.
                   FIGURE 6.   SAMPLING  WITH  A SATURATION  PAD

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                                                                         20
Apparatus

     1.    Saturation (absorbant) pad, 10 cm square [Stock No.  7588 - Alltech
          Associates, Waukegan  Dr.,  Deerfield,  Illinois  60015 (available
          in boxes of  100)].   Extract with methanol  at least 10 cycles on
          Soxhlet apparatus when using for organophosphate sampling.

     2.    Precleaned forceps or disposable gloves of latex, nitrile or vinyl

     3.    Screwcap 40 mSL VOA vials* with teflon-lined septum

     4.    Data sheets, tags and shipping container

Procedure

     1.    Grasp the  saturation  pad firmly with freshly gloved  fingers or
          clean forceps and gently swab over the slick on the water surface.
          Collect a  duplicate  sample from the same  site  and  submit it to
          the chemist for quality control analysis.

     2.    Roll the pad into a cylinder with swab surface inside.

     3.    Insert rolled pad into a VOA vial and cap.   Insert a second unused
          pad in another clean VOA vial and submit to the chemist as a blank
          for quality control analysis.

     4.    Seal, tag and pack vial containing swab pad for shipment.

     5.    Reclean forceps with acetone and rinse with clean water.  Replace
          disposable  gloves before  collecting  additional  surface-slick
          samples.
     Ibid

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                                                                         21
Comment

     Analytical results are  reported on a weight per pad basis.  It may be
appropriate to  composite  several  swab  pads for a  single  sample.   Do not
re-dip a saturation pad or use both sides to collect a surface slick.   Such
procedure often results in flushing collected material from the pad.

WATER  (TAP OR WELL)

     Tap  or  well-water samples are often collected directly  into a sample
bottle   If  numerous  samples of water  are needed,  volume, weight and  glass-
ware may become  of  concern  to  the collector.  An alternate method  is
 described below for conserving space and weight when  large  volumes of
water  (low  amounts of particulates)  are required for an investigation.
    FIGURE  7.   C-18  EXTRACTION  COLUMN      FIGURE 8.  VACUUM PUMP SYPHON DEVICE

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                                                                         22
Apparatus

     1.    Disposable C-18 extraction column (Bond Elut  columns, Analytichem
          International, 24210 Frampton Ave.,  Harbor City, California  90710)

     2.    Flexible tubing

     3.    Hand-operated vacuum  pump (Stock No.  TR-6513-00,  Cole-Parmer
          Instrument Company,  7425 N.   Oak Park Ave., Chicago, Illinois
          60648)

     4.    500 mS. beaker or jar

     5.    500 m£ vacuum flask with stopper

     6.    Acetone-washed aluminum foil

     7.    Plastic bag

     8.    Data sheets,  tags and shipping container

Procedure

     1.    Insert luer  fitting of the C-18  extraction  column into the flex-
          ible tubing  and  connect  the  other end to  the  vacuum flask and
          pump assembly.

     2.    Submerge the  tip  of  extraction column in  a clean beaker or jar
          filled with tap or well  water to be  sampled.

     3.    Filter 500 mi of  the  water sample through  the  C-18  extraction
          column; discard the filtrate.   Collect a duplicate  sample from at
          least one  site  and  submit it to the chemist for quality control
          analysis.
     Registered trademark; appears hereafter without ®.

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                                                                         23
     4.    Wrap the  used  extraction column in aluminum  foil,  place in a
          properly labeled plastic bag and pack  for shipment to laboratory.
          Also submit an  unused column to the chemist as a blank sample for
          quality control  analysis.

     5.    Acetone-rinse the beaker or jar before collecting additional tap
          or well water samples.

Comment

     For technical  assistance  or  ordering Bond  Elut columns, phone (800)
421-2825.  Cost is about  70
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                                                                        24
                  FIGURE 9.   SOIL SAMPLING WITH A SPATULA
Apparatus
     1.   Stainless steel spatula, spoon or scoop
     2.   Acetone (pesticide grade)
     3.   Acetone-washed aluminum  foil  or glass jar with teflon-lined lid
     4.   Shallow, steel pan or pail
     5.   Plastic bag
     6.   Data sheets, tags and shipping container with crushed ice
Procedure
      1.    Scrape  and  scoop with the  spatula  approximately  a pint of top
           soil  (to  a  depth of  less  than  1  inch)  from  the  sample  site.  Mini
           mize  collection  of rocks,  sticks,  leaves  and  debris.

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                                                                         25
     2.   Directly place  soil  into  labeled glass jar or onto aluminum foil
          lining a shallow pan (pan supports foil  to prevent tearing during
          soil collection).

     3.   Seal jar or  wrap  each sample in foil and place it in a plastic
          bag.

     4.   Label samples with  appropriate  identification  and place them in
          the shipping container.

     5.   Reclean sampling  tools with  acetone  and rinse with clean water
          before collecting additional  soil  samples.

Comment

     Inspector judgment is essential to minimize the number of soil  samples
collected and  to  ensure  that samples are taken only  in  situations  where
environmental or human health risk is probable.   In agricultural  situations,
soil samples  from fence lines  and turnrows often produce highest pesticide
concentrations but may be of no importance in an investigation.   Similarly,
in structural  pesticide work,  properly treated soil around  foundations may
not be of use for identifying contamination inside the building.

     Soil acidity or  alkalinity will  deteriorate  aluminum  foil over long
storage  periods;  therefore, when sample  storage  exceeds  96 hours,  soil
should be placed in glass containers fitted with teflon-lined lids and kept
refrigerated.

SEDIMENT

     Pesticide residues often  accumulate  in  the bottom sediment of lakes
and streams.  Under certain physical and chemical  conditions, these  residues
can be  rapidly re-released  into the water causing  fish kills or other con-
tamination problems.   To document the pesticide source, it may be necessary
to conduct sediment sampling

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                                                                         26
     Commercially available  devices  for sediment sampling  include  Emery
bacteriological  sampler ($300),  Phleger  corer ($350),  mud snapper ($150),
Petersen Grab ($300)  and  Ekman Grab ($175).  These devices often require
extensive cleaning between sampling to alleviate cross-contamination, so a
simple and  inexpensive  ($3)  technique  is recommended  in  this section:   a
disposable core tube.
      FIGURE 10.  PHLEGER CORER
FIGURE 11.   EKMAN GRAB
 Apparatus
      1.   Disposable type core tube or commercial device
      2.   Wash pan  (prec'eaned with acetone)

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                                                                         27
     3.    Widemouth glass jar with teflon-lined lid

     4.    Data sheets, tags and shipping container with crushed ice

Procedure

     1.    Carefully  lower  disposable core tube or other  sampling  device
          through water  into sediment  (minimize  roiling the sediment).

     2.    Retrieve approximately 1 pint of sediment.

     3.    Directly transfer  sediment  into a  clean glass sample jar  or  a
          clean pan.

     4.    Remove rocks, leaves and other debris from  sediment before trans-
          ferring to the widemouth glass jar.   Collect a duplicate  sediment
          sample from  at  least  one site and submit it to the chemist for
          quality control analysis.

     5.    Label  samples  and store  them in the shipping  container with
          crushed ice for transport to laboratory.

     6.    Properly dispose  of core  tube.  Rinse pan with acetone and flush
          it with clean water before collecting additional  sediment samples.

Comment

     Directly scooping sediment into a glass  jar avoids the cost and use of
sampling devices so this procedure is recommended for shallow sampling situ-
ations.   Where water  depths exceed a few inches,  sediment contents can be
flushed or diluted  as  the jar is  lowered or retrieved through  the water.
Thus, the core tube  technique described  is satisfactory for  unconsolidated
sediment and  use of  a  commercial  sediment-collecting device  is  recommended
for firm bottom deposits.

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                                                                          28
 PLANTS
      Pesticide  drift,  overspray  or  other  misapplication  incidents  are  often
 documented  by collecting and analyzing plants  for  residues.   The  sampling
 technique described  below  is  applicable for  most  agricultural  crops  as well
 as  non-crop vegetation where drift  or overspray  is  to be  documented.  For
 documenting acceptable pesticide tolerance  levels  in feed and foodstuffs,
 refer to the sampling  method described  in the Appendix of this  manual.
 Cost  of  supplies  for plant  sampling  usually  is  less  than $25.
                   FIGURE 12.  VEGETATION SAMPLING GEAR
Apparatus
     1.    Shovel and clippers
     2.    Acetone-washed aluminum foil
     3.    Disposable gloves of latex, vinyl or nitrile
     4.    Plastic or paper  bags,  glass  jars or new  quart-size  ice cream
          cartons

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                                                                         29
     5.    Data sheets, tags  and  shipping  container with freezer paks,  dry
          ice or crushed ice
Procedure

     1.    Collect approximately 1 pound  (1 quart) of affected vegetation.
          For small  plants where systemic pesticide absorption is suspected,
          uproot entire plant; otherwise remove plant parts such as leaves.
          If possible, collect  an unaffected  plant and submit  it  to  the
          chemist for use as a quality control  specimen.

     2.    Cover work surfaces with clean aluminum foil and, wearing dispos-
          able gloves, prepare  samples  by removing soil and cutting into
          suitable length size for wrapping.

     3.    Wrap sample  in  foil;  usually  one type of vegetation or crop per
          sample.

     4.    Place foil-wrapped sample  in bag or box and label.

     5.    Place samples in shipping  container and chill or freeze.

     6.    Properly dispose of gloves and then acetone-rinse shovel  or clip-
          pers and  flush  them with  clean  water  before  continuing to sample
          other vegetation.

Comment

     Plants are  often  very perishable and must  be  chilled or preferably
frozen as  soon  as possible for transport  to  the laboratory.   It may be
necessary  to  air-dry damp vegetation  before wrapping  or to freeze wet sam-
ples to prevent rotting during shipment.   If dry ice is shipped with samples,
it  should  be  wrapped  securely in heavy  paper  (for  safety, never pack dry
ice in glass, metal or air-tight containers).

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                                                                         30
     The  Appendix  to  this manual  contains  procedures  for  collecting
representative plant  parts normally  consumed  by humans  and livestock.
These sampling and packing instructions  for agricultural commodities are
modified  from  Guidelines  for  Collecting  Field  Samples.  U.S.  Environmental
Protection Agency,  Office of Pesticide Programs,  Washington,  DC,  March 1979.
If the  purpose of plant sampling  is other than for identifying residues to
determine pesticide tolerance  compliance in  food,  the investigator should
consult the chemist for  information on plant parts to be sampled, amount
                                          *
and proper preservation.

ANIMALS

     Misapplication,  drift, overspray, spillage  and  other incidents with
pesticides often result  in harm or death to animals.   Pesticide residue
sampling of tissue,  blood, urine or related material  from livestock or wild-
life is to be done by a veterinarian or authorized agent.  Such sampling is
beyond  the scope of  this manual  so it will not be addressed; however, if
the  source  of animal  illness or death  is  suspected  to be  pesticide-
contaminated feed, the  inspector  should  collect a sample.   Refer  to the
sampling and packing instructions in the  Appendix of  this report.

     Occasionally,  the pesticide  inspector finds dead  fish,  birds, bees or
other small animals at or near a  pesticide application site.  With reason-
able suspicion that pesticides are the cause of death,  the  inspector may
have to collect an animal sample.   Sampling costs involve only miscellaneous
supplies so they are minimal (less than $5) but analysis is often expensive;
thus, inspector judgment  is essential  before collecting and shipping animal
specimens to the laboratory for pesticide residue analyses.

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                                                                         31
                               A LI-MAX
                               -OILS INC.
                     FIGURE 13.   ANIMAL SAMPLING GEAR
Apparatus
     1.    Dipnet, tongs and knife
     2.   Disposable gloves
     3.   Acetone-washed aluminum foil
     4.   Shallow, flat-bottomed pan
     5.   Plastic bag or widemouth glass jar with teflon-lined lid



     6.   Data  sheets,  tags  and  shipping  container  with  crushed  or  dry  ice
Procedure
      1.   Unless  instructed otherwise, collect only dead animals.




      2.   Preferably  collect  entire animal  but,  if  impractical,  collect at

          least a  pound  of  tissue  (approximately  1 pint).

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                                                                         32
     3.    As appropriate, place the dead animal  in an aluminum-lined pan to
          cut tissue samples before wrapping.   Avoid skin contact with dead
          and possibly  diseased animals by  wearing protective clothing
          including disposable gloves.

     4.    Place entire animal  or  tissue in clean glass jar or wrap sample
          in foil  and place  in plastic bag;  attach identification tag.

     5.    Immediately freeze  samples or place them in shipping container
          with crushed ice for transport to the  laboratory.

     6.    Wash, acetone-rinse  and  flush with  clean water all tools used in
          collecting  and  preparing animal  samples;  properly dispose of
          gloves and used aluminum foil.
Comment

     Animal deaths may  be  caused by disease, so caution must be taken to
protect the inspector and others when handling dead animals or tissue during
a pesticide investigation.   If a question about health or sample preparation
technique exists, consult a veterinarian or wildlife biologist before pro-
ceeding with collecting or dissecting dead animal  specimens.

AIR

     Sampling air for pesticide  residues is a task that requires consider-
able preplanning by the inspector, chemist and other officials of the regu-
latory agency.  The  primary  objective  that must be considered  is of what
value the air sampling and analyses will  be in documenting a health or envi-
ronmental problem.   Once the decision is  made to collect airborne pesticide
residues, the next consideration is to  select an appropriate sampling method.

     In  the  following pages,  two mechanical procedures  for collecting air-
borne pesticide residues are  described.  One method is  designed  to collect
pesticide droplets,  the  other for vapor.  Equipment and supply  costs for

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                                                                         33
the two methods range from less than $10 (droplet sampling) to nearly $1,000
(vapor sampling).

     Temperature and relative  humidity  measurements  are an essential part
of air monitoring.   These parameters provide atmospheric  information often
linked to vapor or  droplet  pesticide drift problems.   In the agricultural
or outdoor  setting,  wind direction and speed  are  important and must be
recorded also.  Inexpensive  devices  suitable for these measurements are a
pocket sling  psychrometer for  temperature 'and humidity ($35) and a pocket
wind  meter  ($10).   A manufacturing  source  is  Weather Measure, P.O. Box
41039, Sacramento, California   95841.   Respectively,  the psychrometer and
wind  meter  are model number  5220 and  2520 in the 1985  Weather Measure
Catalog.


   FIGURE  14.   SLING  PSYCHROMETER
FIGURE 15.   WIND METER

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                                                                         34
AIR (PESTICIDE DROPLET DRIFT)

     A  simple  and inexpensive  method for  detecting  pesticide deposits
(droplets) from  overspray  or  drift  is  the  use of  spray droplet paper.   Two
types of commercially available paper are recommended; one is a rigid paper
coated with a yellow surface that stains dark blue with water droplets, the
other is  also  rigid  but  coated  with  a  white  surface that stains black with
oil droplets.  Because pesticide  formulations are  usually diluted in water
or oil, these  papers are adequate for  quickly detecting spray patterns  and
droplet deposits.  To increase  monitoring  effectiveness, it  is recommended
that water and oil  sensitive paper be stapled side-by-side on posterboard
with a  third paper,  a chemically-clean,  10 mm square  saturation pad.  This
array will enable the inspector to visibly detect oil- or water-based pesti-
cide droplets  that  impinge on the papers, as well as providing a residue
sample on the saturation pad for chemical analysis.

     Oil-  water-sensitive  papers  have proven useful  in  identifying off-
target droplet patterns  of drift  or overspray from agricultural  ground or
aerial  pesticide  spraying.   Detecting misapplication at structural  pesticide
treatment sites  is another possible use of  spray  droplet  papers  and the
author of this  manual solicits suggestions.
                    FIGURE 16.   DROPLET INDICATOR PAPER

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                                                                         35
Apparatus

     1.   Water-sensitive paper, 76 mm x 52 mm [Stock No.  20301-2, Spraying
          Systems Co., North Avenue at Schmale Rd.,  Wheaton, Illinois  60187
          (available in package of 50 cards)]

     2.   Oil-sensitive paper,  76  mm x 52 mm [Stock No.  20302-1,  Spraying
          Systems Co., North Avenue at Schmale Rd.,  Wheaton, Illinois  60187
          (available in package of 50 cards)]

     3.   Saturation pad, 10 cm x 10 cm [Stock No.  7588,  Alltech Associates,
          Waukegan Dr.,  Deerfield,  Illinois   60015  (available in boxes of
          100)].  Extract with methanol at least 10  cycles on Soxhlet appa-
          ratus when using for organophosphate sampling.

     4.   Latex,  nitrile  or vinyl  gloves  (for  handling  oil- and water-
          sensitive cards)

     5.   Posterboard (at least 7-inch square)

     6.   Stapler (to attach paper to posterboard)

     7.   Nails or  tape  (to attach posterboard with papers to sample site
          support (i.e., fence, tree, building, etc.)

     8.   Acetone-washed aluminum foil

     9.   Data  sheets, tags and plastic bag's

Procedure

     1.   Assemble  array  of papers on posterboard by  stapling side-by-side
          an  oil-sensitive  paper,  water-sensitive paper and  a  saturation
          pad.  Duplicate saturation  pads may be needed for certain analyti-
          cal  purposes  such as quality control or analyzing more than one
          type  of pesticide (consult  the chemist).

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                                                                    36
2.    Nail or tape  the  poster-board array of papers (droplet indicator
     card) to a  natural  or artificial support at the sample station
     site.  The  card should  be  placed horizontally  and  above the
     groundcover canopy of  vegetation (shrubs,  grass, crops,  etc.).

3.    Handle droplet  card  with clean gloves to prevent  skin  contact
     with oil-  and water-sensitive paper or saturation pad (see comment
     below).

4.    Lay  out droplet card shortly before spraying occurs.  Identify
     each sampling  location by cross-reference to a  map  or  logbook
     entry.

5.    Following exposure to  spray  application,  retrieve droplet card
     and  examine  for stains;  record onsite results in field logbook.

6.    Wrap entire droplet card in precleaned foil  and place in a plastic
     bag.

7.    Label bag for transport to laboratory.

8.    At  the  laboratory,  remove the saturation pad  from the  droplet
     card and send  it  to the chemist for pesticide residue analysis.
     If  duplicate  pads  are needed for analytical purposes, the 10 cm
     square pad  can  be  cut in half or initially expose two pads (see
     step 1).

9.    Count and  record  the number of  droplet stains on  the sensitive
     paper.   If  stains  are  too numerous to  count,  use a template with
     a square centimeter opening and count stains in four  random areas
     on  the paper;  report as average number of  droplets  per  square
     centimeter

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                                                                        37
Comment
     limitations of water- and oil-sensitive paper include the logistics  of
placing  the  droplet cards at sailing locations  shortly  before  spraymg
     5   Also,  oil  or  perspiration  fro™ fingers can pre-stain the paper so
 at x   nitrile  or vinyl  gloves are recommended when handling the sampling
 ards'   Finally,  very  high humidity (greater than 90*) will turn the water-
 sensitive  paper light  blue making the darker b!ue stains  produced by water
 droplets difficult  to  detect.

      Before  and after use,  the water-  and oil-sensitive  cards should be
 stored under dry conditions, preferably in an  air-tight container.

 AIR (PESTICIDE VAPOR DRIFT)

      The leading source of pesticide complaints is odor which is often asso-
 c,ated with solvent or active ingredient vapors released  during and fo   ow-
 ing  spraying.   Numerous  pesticide samplers have been developed to collect
    ticide vapors 0«ss  than 0.1  urn); these include the HISCO Model 88. the
      -  ol  high  volume  filter sampler and  others.  All have
      g  fragi  e, bulky, heavy, expensive and electric  powered.  The  sample
    vi  e described below has  but  one  of these  limitations; it ,s expensive.
 Although  the sample-collection materials  are  less than  ,10,  the por <,  1
 vacuum pump recorded costs $750 and a suitable calibrate k,t costs an
  additional  $150 to $200.

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                                                                         38
      FIGURE 17.   PUF COLUMN
FIGURE 18.   CONSTANT-FLOW VACUUM
      PUMP WITH PUF COLUMN
Apparatus
          Battery-powered, constant-flow vacuum  pump  and 110 volt, 60 Hz
          battery charger  (Dupont  P-4000,  E.I.  duPont de  Nemours  &  Co.,
          Wilmington, Delaware) flow  rate  0.02-4.0  £/minute (±5%), weight
          1.2 kg, rechargeable

          DuPont calibration  kit [Stock No. 66-242-f-l (soap bubble meter)
          or equivalent flow-rate meter,  E.I.  dupont de Nemours & Co.,  Wil-
          mington,  Delaware.

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                                                                         39
     3.    Polyurethane foam (PUF);  Gaymar Identi-Plugs foam tube plugs [Stock
          No.  L 800-13;  Gaymar Industries,  Inc.,  One Bank St.,  Orchard Park,
          New York 14127 (available in bags of 200)].   Two extractions with
          10% ether and  hexane solution;  at least 32 cycles each on Soxhlet
          apparatus and  dry overnight under  hood  to remove impurities.

     4.    Glass tubing with 15 mm ID,  5-inch length
                                          •
     5.    Rubber septum, suitable to fit tightly over ends of glass tubing
          (air-tight fitting)

     6.    Glass tubing,  3  mm ID;  4.5  cm length  (disposable  plastic  1 m£
          pipette cut into  4.5  cm  length is a satisfactory substitute for
          the glass tubing)

     7.    Flexible tubing or hose (3-foot length  is suitable for most uses)

     8.    Acetone-washed aluminum foil  and plastic  bag for sample

     9.    Data sheets, tags and shipping container

Procedure

     1.    Assemble PUF* column  centering two  foam  plugs  in glass  tubing;
          cap tube ends  with rubber septums.  Pierce one septum with 4.5-cm-
          long piece of  rigid plastic  (pipette) or  glass tubing.

     2.    Attach flexible hose to septum tubing and vacuum pump.

     3.    Remove septum  from one  end  of PUF column; calibrate vacuum pump
          for air flow of at least 2 2/minute through the PUF column.   (Cal-
          ibration can  be  done  in  the laboratory  or  office  prior to and
          after field use.)
     Lewis,  R. G. and MacLeod,  K. £.,  1982,  "Portable Sampler for Pesticides
     and Semivolatile Industrial  Organic  Chemicals in Air", Anal. Chem.,
     54: 310-315.

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                                                                         40
     4.   Wrap entire PUF  column  in clean foil for transport to sampling
          site.

     5.   At sampling site,  remove  foil  and attach PUF column and hose to
          vacuum pump.   Operate vacuum for precise preselected time to pass
          500 liters of air through the PUF column.   If possible,  collect a
          duplicate air sample to submit to the chemist for quality control
          analysis.

     6.   After sampling, disconnect PUF column and recap its open end with
          rubber septum.

     7.   Rewrap used PUF  column  in clean foil, place it in a plastic bag
          and label it for transport to the laboratory.  Also wrap a clean,
          unused PUF column in foil  and submit it as a blank to the chemist
          for quality control.

     8.   In the laboratory,  extract  pesticides with appropriate  solvents
          and report  results  as weight of pesticide/cubic  meter  of air.

Comment

     The PUF column vacuum pump described is lightweight, portable and oper-
ates quietly.  This makes it ideal for indoor sampling (structural  or agri-
cultural pesticide monitoring).  If used for termiticide indoor air sampling,
the apparatus should  be  placed at the center of  the  room  near the  normal
breathing zone (3  to  6  feet above the floor).   Agricultural monitoring is
more variable  and  site  selection must be based  on  inspector judgment.

     Actual   testing has  shown that the PUF column trapping efficiency for
numerous organochlorine,  organonitrogen,  organophosphorus  and  pyrethoid
pesticides  is greater  than 75%.  For  specifics,  refer to the Lewis  and
MacLeod publication or contact NEIC at (303) 236-5120.

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                APPENDIX

  SAMPLING AGRICULTURAL COMMODITIES TO
DETERMINE PESTICIDE TOLERANCE COMPLIANCE

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                                 APPENDIX
                   SAMPLING AGRICULTURAL COMMODITIES TO
                 DETERMINE PESTICIDE TOLERANCE COMPLIANCE
SAMPLING AND PACKING SPECIFIC CROPS
     Artichokes
Collect about  1 pound of  fruit (5  to  10
buds).   Chill,  if possible.
Packing:   Aluminum foil, paper bag, shipping
case
     Asparagus
Collect about 1 pound of stalks cut at ground
level (15 to 25 stalks).   Chill.
Packing:   Aluminum foil, paper bag, shipping
case
     Beans (for shelling,
     including peas, lima
     beans, dried beans,
     etc., not soybeans)
     Beans (snap, also
     edible, podded peas)
Cut enough plants to yield a quart of shelled
beans.   Air  dry;  shell  beans.   Discard all
plant material  except beans.
Packing:   Place  in  clean  quart jar or can;
shipping case.

Collect a  quart of  the  vegetable.   Chill.
Packing:   Aluminum  foil, paper bag, shipping
case
     Beets, red
Collect four beets.   Remove and discard tops.
Packing   Aluminum foil, paper bag, shipping
case
     Berries (all,  includ-
     ing strawberries)
Collect a  quart of ripe  berries.   Carry a
flat of  new 1-quart ice  cream  cartons  and
place berries directly into these cartons as
they are  picked.   Freeze samples.   Mark
'Perishable1
Packing:    1-quart  ice  cream cartons, ship-
ping case

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Broccoli
Collect about 1  pound  of spears (15 to 20).
Chill samples.   Mark 'Perishable1.
Packing:   Aluminum  foil, paper bag, shipping
case
Brussels Sprouts
Collect about  Ipound of sprouts  (15  to  25
sprouts).
Packing:   Aluminum foil, paper bag, shipping
case
Cabbage
Collect two heads.
Packing:   Aluminum foil, paper bag, shipping
case
Cantaloupe

Carrot
See Melons

Collect one bunch of carrots (6 to 10).   Remove
and discard tops.
Packing:  Aluminum  foil, paper bag, shipping
case
Cauliflower
Celery
Corn (field and sweet)
See Cabbage.

Collect  one bunch (6  to  10 stalks).   Keep
samples chilled.  Mark 'Perishable'.
Packing:  Aluminum foil,  paper  bag, shipping
case

Collect  1 quart of kernels by  removing 8 to
10 lengthwise rows of  kernels per ear.  Collect
three  stalks; air dry; cut stalks into 6 to
10-inch  lengths;  thoroughly mix and  retain
about  1 pound as  the sample
Packing.  Corn  grain  -  clean  quart jar or
can.   Sweet corn kernels  must  be  kept frozen

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                         or chilled and should be marked 'Perishable'.
                         Corn stalks - aluminum foil, paper bag, ship-
                         ping case
Cotton
Sample three  to  five mature cotton plants.
Where average plant  height  for the site does
not exceed  3 feet,  take  the  entire  plant.
Where average height is greater than 3 feet,
             »
cut branches  from  the main  stalk, uniformly
sampling the top, middle and bottom one-third
of each plant.
Packing:   Remove all  open bolls;  wrap with
aluminum foil and  place in  a paper bag, then
in a shipping case.  Cut plants or plant  parts
into 6 to 10-inch lengths, retaining the  green
bolls.  Air  dry and  mix.  Wrap about a pound
of this composite  sample  with  aluminum foil
and place in  a paper bag, then in a shipping
case.
Cucumber
Gather two or three mature cucumbers.   Chill,
if possible.
Packing:   Aluminum  foil, paper bag, shipping
case
Eggplant
Collect one or two eggplants.
Packing:   Aluminum foil, paper bag, shipping
case.   Use packing material to prevent damage
during shipment.
Forage

Fruit (including
citrus, pomes,
stone fruit)
Sample when available.   See Hay.

For small  fruit such  as  cherries,  collect
a quart of  fruit.  For  larger fruit, collect
two or three fruit.   Keep chilled.

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                         Packing:   Pack fruit  gently  and securely in
                         suitable container to  prevent  injury during
                         shipment.   Mark shipping container with 'Per-
                         ishable1  label.
Garlic
Collect 6  to 8 bulbs.   Remove  and discard
tops.
Packing:   Aluminum foil, paper bag, shipping
case
Grains small (includ-
ing barley, buckwheat,
millet, flax, rice,
rye, wheat, wild rice,
etc.)
Grapes
Cut several  handfuls  of plants.   Cut heads
from straw.
Packing:   Heads should  be  packed separately
from  straw.   Composite  about a  pound  of
straw for sample.  Wrapping:  aluminum foil,
paper bags,  shipping cases

Collect  a  1-pound  bunch.   Keep  chilled.
Packing:   Aluminum  foil;  pack  securely  in
shipping container (not  too  tightly).   Mark
shipping container with a 'Perishable'  label.
Hay
Sample near the  end  of growing season, but
before the  last  cutting.  Cut  small handfuls
of plants.   If  vegetation  is  sparse,  take
forage within several square yards.   Air dry,
mix thoroughly and  retain  about a pound for
sample.  Packing:  Aluminum  foil, paper bag,
shipping case

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Leafy vegetables
(including chicory,
collards, endive,
escarole, field
cress, kale, leaf
lettuce, mustard
greens, parsley,
spinach, Swiss
chard, watercress,
etc.)

Lettuce, head

Melons (including
cantaloupe, honeydew,
watermelon, etc. )

Nuts and seeds
(except peanuts)
For small  plants,  gather leaves from three
plants.   For large  plants  such as collards,
gather one plant.
Packing:   Aluminum  foil, paper bag, shipping
case
See Cabbage, keep chilled.  Mark 'Perishable'.

Collect one melon.   Keep chilled.
Packing:    Aluminum  foil,  shipping  cases
Collect  1  pint of  nuts  or seeds.  Thrash
the seed.
Packing:    Clean  pint jar  or  can; shipping
case
Okra
Onion
Collect 6 to 8 okra.
Packing:   Aluminum foil,  paper bag,  box

Collect two  to  three  mature onions.   Remove
and  discard tops.   Allow  onions  to dry
slightly  before packing.   Shake  off soil
particles.
Packing:  Aluminum foil,  paper  bag,  shipping
case
Peas
See beans (for shelling).

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Peas, edible podded
(snowpeas, Chinese
peas)
See Beans, snap.
Peanuts
Collect enough  plants to yield  a pint of
shelled peanuts and  about  a pound of hulls
and vines.   Air dry.   Shell  peanuts and retain
hulls and vines.
             •
Packing:   Clean pint  jar  or metal container
for peanuts.  Aluminum  foil,  paper bag, box
for hulls and vines;  shipping case
Pepper, bell (sweet)
Collect two or three peppers.
Packing:   Aluminum foil, paper bag, box.   Use
packing material  to prevent  damage.   Keep
chilled.   Mark shipping case  with  a  'Perish-
able1  label.
Pepper, hot
Collect eight to 10 hot peppers.
Packing:   Aluminum foil, box.  Keep chilled.
Peppermint

Potatoes, sweet or
white
Sample as for hay.

Collect two or three.   Remove soil by shaking.
Packing:   Aluminum  foil, paper bag,  suitable
container.   Chill,  if possible.
Pumpkin
Radishes
Gather one pumpkin.
Packing:   Aluminum foil,  suitable container

Collect  six  to  eight radishes.  Remove  and
discard tops.
Packing:   Aluminum  foil,  paper bag,  box.
Chill, if possible.

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Rhubarb
Collect six stalks.   Chill.
Packing:   Aluminum foil, paper bag, shipping
case
Rutabaga
Collect three or four rutabaga.  Remove tops
and discard.
Packing:   Aluminum  foil,  suitable  container
Scallions (spring
onions)
Silage, corn and
sorghum
Collect eight to 10.  Shake off as much soil
as possible.   Keep chilled.   Mark 'Perishable1
Packing:   Aluminum  foil,  plastic  bag,  cloth
bag, shipping case

Collect three stalks.   Cut  stalks into 6 to
10-inch lengths.   Thoroughly mix,  air dry and
retain 1 pound as sample.
Packing:   Aluminum  foil,  paper bag,  shipping
case
Sorghum, grain
Collect  three  plants.   Remove  heads.   Air
dry.  Cut  stalks  into  6 to 10-inch lengths.
Thoroughly air dry, mix and retain 1 pound as
sample.
Packing:    Pack heads and  stalks separately.
Wrapping:  Aluminum foil,  paper bag, shipping
case
Soybeans
Cut enough plants  to yield  a pint of  shelled
beans and about  a  pound of vines.   Air dry;
shell beans.
Packing:   Vines  -  aluminum foil, paper bag
Beans -  clean  pint jar  or can,  shipping case

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Spearmint
Sample as for Hay.
Squash, summer
(yellow, white,
zucchini)
Summer squash  should be  harvested when  small
and tender.  Gather two squash.
Packing:   Keep chilled.  Aluminum foil, paper
bag, box.
Squash, winter
(acorn, butternut,
hubbard, etc.)
Sugar beets
Tobacco
Winter  squashes  should  be  harvested when
mature.  Collect two mature winter squashes.
Packing:  Aluminum  foil,  cases  suitable for
shipment

Collect two  sugar  beets.   Remove tops;  keep
chilled.
Packing:  Beets - wrap individually with alu-
minum foil  and pack in shipping case.  Tops -
aluminum foil,  paper  bag,  shipping  case

Collect two or three ripe leaves.
Packing:   Aluminum foil,  paper bag,  box
Tomatoes
Tomatoes, cherry
Collect  two  tomatoes.   Keep chilled.  Mark
shipping  case  with  a  'Perishable1  label.
Packing:  Wrap  individually  in aluminum  foil
and pack carefully  in  suitable  container.
(Use packing material  to  protect tomatoes.)

Collect  10  to  12 cherry  tomatoes.   Keep
chilled.
Packing:  New 1-pint ice cream cartons, suit-
able shipping container.   Mark  'Perishable'.
Turf
Follow instructions for Hay.

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Turnips                  Collect four to six turnips.  Remove tops and
                         freeze.
                         Packing:   Pack  tops and  roots  separately.
                         For both:   aluminum foil,  paper  bag,  box

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