440189024
      ivEPA
United States Environmental Protection Agency
Office of Water Regulations and Standards
Industrial Technology Division
Office of Water
August 1989
         Sampling Procedures
         and Protocols for the
         National Sewage Sludge Survey

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SAMPLING PROCEDURES AND PROTOCOLS FOR
    THE NATIONAL SEWAGE SLUDGE SURVEY
         Prepared for:

           William A. Telliard, Chief
           Analysis and Analytical Support Branch
           USEPA Office of Water Regulations and Standards
           401 M Street, SW
           Washington, DC 20460
Under EPA Contract No. 68-03-3410



Publication Date: August 1989





   U.S. Environmental Protection Agency
   Region 5 .Library (PL-12 i)
   77 West Jackson Boulevard 19H, rr
   Chicago, IL  60604-3590   2Bl Fl°°f
                                                      Printed on Recycled Paper

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                        TABLE OF CONTENTS

                                                             Page

1.0  PROJECT DESCRIPTION  	   1


2.0  SAMPLE METHOD SELECTION 	   2

3.0  SAMPLE COLLECTION 	   4

     3.1  Sample Point Identification   	   5

          3.1.1  Sample Type Classification  	   5
          3.1.2  Sample Collection Point Selection  	   9

     3.2  Sample Collection Procedures  	  11

          3.2.1  Solid Sludge Sample Collection  	  15
          3.2.2  Solid Sludge Handling  	  18
          3.2.3  Liquid Sludge Sample Collection 	  19
          3.2.4  Liquid Sludge Handling  	  20


4.0  SAMPLE HANDLING AND CUSTODY   	  21

     4.1  Sample Handling	21
     4.2  Sample Preservation  	  21
     4.3  Sample Shipment	22
     4.4  Field Custody Procedures 	  23

5.0  SAMPLING EQUIPMENT   	  23


Appendix A - Commonly Used Sewage Sludge Sampling Points


Appendix B - Sample Control Center: Sample Scheduling
             and Shipment Instructions
                                11

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                  NATIONAL SEWAGE SLUDGE SURVEY
                SAMPLING PROCEDURES AND PROTOCOLS
1.0   PROJECT DESCRIPTION

This document presents the sampling procedures and protocols for

the National Sewage Sludge Survey.



The objective of this sampling project is to visit and collect

samples of sewage sludge from a variety of Publicly Owned

Treatment Works (POTWs) in an effort to identify the presence and

level of toxic pollutants contained in municipal sewage sludge

(hereinafter referred to as sludge).  After collection and icing,

samples will be shipped to laboratories for preservation and

analysis.  Laboratory tests will be performed for:  1) those

analytes listed in The 1987 Industrial and Technology Division

List Of Analvtes.  and 2)  the following non-conventional

pollutants:

     Fluoride
     TKN
     Nitrate
     Nitrite
     Phosphorous
     Percent solids
     Cyanide



2.0   SAMPLE METHOD SELECTION

Representative sampling may be performed using either grab

samples or long-term composite samples.

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Grab sampling consists of collecting a single sample for each
different and segregated sludge product produced during a POTW's
normal daily operations.  A grab sample is a sample collected
over a short period (usually less than 15 minutes) during the
daily operation of a POTW.  This is the quickest and least
expensive way of collecting reliable sludge samples.

Composite sampling consists of consecutively collecting samples
(weekly, monthly, etc.) over a period of time and requires
considerably more man-hours to accomplish.  Long-term sampling
incorporates the effects of seasonal climatic changes, POTW
operating procedures,  long-term industrial production cycles, and
the number and type of POTW collection system connections
(domestic/industrial)  on the sludge pollutant concentrations.  A
long-term sampling program is of more benefit in describing the
changes associated with POTW sludge production over extended
periods.

The quickest and most cost effective, yet representative, sample
collection method for the purpose of this study is short-term
sampling.  Grab samples are adequate to characterize the quality
of sludges prior to final disposal, because the long sludge
detention times found at POTWs reduces the variability of the
sludge characteristics.  Processes which produce sludge and/or
add to a POTW's sludge detention time include:

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     A.   Primary Clarification:  Located at the head of the
          treatment plant, easily settleable and floatable
          materials are removed from the wastewater.  Sludge
          mixing is minimal until the primary sludge is pumped to
          digesters and thickeners for mixing with other process
          sludges.

     B.   Activated Sludge/Secondary Clarification:  The constant
          recycling of biomass within the process generates
          sludges with process ages (sludge detention times) of 5
          to 30 days.  Sludge detention times vary dependent upon
          process modifications.

     C.   Other Biological Treatment Processes:  Trickling
          filters, rotating biological contactors and other fixed
          media systems have intermittent sloughing off of
          biomass which cause sludge to vary in quality and
          quantity.

     D.   Chemical Precipitation/Coagulation: After secondary
          treatment (where 80% to 90% of the pollutants have been
          removed), chemicals such as aluminum hydroxide, ferric
          chloride, lime and polymers are added to further treat
          the wastewater.  Some sludge is recycled and detention
          times reach 1 to 2 days.  These sludges are frequently
          difficult to dewater and are normally mixed with
          digested or undigested biological sludges prior to
          further processing.

     E.   Sludge Holding/Gravity Thickeners/Elutriation Tanks:
          Due to process constraints such as septicity, sludge
          detention time is normally no more than 1 to 2 days.

     F.   Aerobic/Anaerobic Digesters:  Detention times of 20 to
          30 days normally are found in these sludge
          stabilization processes.

     G.   Miscellaneous Stabilization Processes:  Additional
          sludge stabilization processes, such as lime
          stabilization, chlorine oxidation, heat treatment, and
          wet air oxidation, can drastically change a sludge's
          characteristics but have a very small effect on its
          detention time.
A POTW may use one or more of the above processes to treat

wastewater and to condition sludge before dewatering, composting,

and final use/disposal.  The combined detention times:  1)

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disperse and dilute any slugs or otherwise non-representative
concentrations of pollutants, and 2) produce a consistently
homogenous mixture of sludge.  For this reason, a grab sample
could adequately represent a 20- or 30-day composite sample.

A short-term effect on sludge quality may be felt during
dewatering.  Equipment used in the process (belt presses,
centrifuges, vacuum filters) does not generate a product of
constant dryness.  The percent solids (or percent moisture) may
vary, depending on chemical feed rates, septicity of incoming
liquid sludge, and differences among machines.  As the percent
solids of the final product varies so will the amount of water
soluble pollutants.  This can be avoided to some degree by
sampling only during normal operating hours (i.e., never during a
dewatering facilities start-up mode).

Under these controlled sampling circumstances, short-term
sampling will provide representative samples of sewage sludges.

3.0   SAMPLE COLLECTION
This section provides the rationale for selecting sampling
locations and describes the protocols to be used for sample
collection and handling.

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 3.1   Sample Point  Identification
 3.1.1  Sample Type  Classification
 All samples to be collected will be grab  samples of the  final
 sludge product or products produced by the POTW.  The  final
 sludge product will be defined as sewage  sludge after  all
 conditioning, dewatering, etc., but before disposal (i.e., before
 land application, incineration, landfill, distribution and
marketing, permanent lagooning or ocean disposal).  In cases
where a sewage treatment plant's sludge is transported to another
 facility for further processing, the sample will be collected, at
the facility of origin, before transfer.

Individual samples will be collected for each distinct type of
sludge segregated and disposed of by the POTW.  Individual sludge
types may be classified in two categories:  liquid and solid.
Liquid sludge is defined as any sludge which has the capacity to
flow and is conveyed via pump.  Solid sludge is defined as any
sludge which does not meet the liquid sludge definition.

Liquid and solid subcategories may evolve when sludges produced
during various plant processes are segregated, treated, and
disposed of individually, as opposed to being blended before
treatment and disposal.  Each of these final sludge products will
be considered as a different and individual sample.  Therefore, a
POTW may have a variety of final sludge products, liquid and/or
solid, combined or individual.  Each type will require an

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individual grab sample.  However, grab samples will be collected
and combined when similar dewatering devices are used for the
same type of sludge.

The following is a description of an imaginary POTW to
demonstrate the classification of various final sludge types.

                             EXAMPLE
     POTW "X" (refer to "Generic" POTW flow diagram, Figure 1)
     consists of primary clarification, activated sludge and
     secondary clarification, chemical treatment/precipitation,
     aerobic digestion, sludge thickening and dewatering through
     the use of one centrifuge, two belt presses and a drying
     bed.

     Primary clarifier sludge and secondary clarifier sludge
     (i.e., waste activated sludge) are sent to the aerobic
     digester for stabilization.  Sludge from the aerobic
     digester is then dewatered using a centrifuge, belt press
     #1, and the drying bed.  The solid sludge is landfilled.

     Sludge produced in the chemical treatment/precipitation unit
     is mixed with additional aerobically digested sludge in the
     thickener.  Half of this mixture is dewatered using belt
     press 12 and landfilled.  The other half is hauled away as a
     liquid and applied to  farmland.

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The individual sludge samples that should be collected at



this imaginary POTW are as follows:







     Sample fl - Aerobically digested sludge from the



centrifuge and belt press #1:  Both the centrifuge and belt



press #1 are dewatering the same type of sludge.  A grab



sample would be collected from each machine and combined to



form a single representative sample.







     Sample *2 - Aerobically digested sludge from the drying



bed:  This is a separate sample.  Aerobically digested



sludge in Sample #2 is being dewatered in a radically



different way than in Sample #1.  Drying beds reduce the



moisture content of a sludge much more than centrifuges and



belt presses.  Also chemical and physical changes in the



sludge occur due to the long holding time and exposure to



elements while on a drying bed.  Grab samples of different



areas of the drying bed (as described in Section 3.2.1.C)



would be collected and combined to form a representative



sample.







     Sample #3 - The chemical and aerobically digested



sludge mixture dewatered on belt press #2:  This is a



different sludge type from Samples #1 and #2.  A separate



grab sample would be collected.

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          Sample f4 - The chemical and aerobically digested

     sludge mixture hauled away as a liquid:  This is the same

     sludge as in Sample #3, except in liquid form.  The liquid

     is treated as a different sludge type, and  a grab sample is

     collected.



Sampling points for the above samples are shown in Figure 1.



3.1.2   Sample Collection Point Selection

The following procedures should be followed to select the

appropriate collection point necessary for representative grab

samples once each individual sludge type has been identified.

Appendix A, taken from the U.S. EPA POTW Sludge Sampling and

Analysis Guidance Document, contains additional information on

commonly used sludge sampling points.



     Solid Sludge Collection Point

Samples of solid sludge should be collected directly from the

final sludge treatment processes.  These processes include, but

are not limited to, belt filter press (continuous), plate and

frame sludge press (batch), centrifuge, vacuum filter, compost

pile and drying beds (sand beds, cement pads, drying lagoons,

vacuum assisted drying beds).

     A.   Belt Filter Press/Centrifuge/Vacuum Filter:  Each
          process dewaters sludge continuously.  The sample
          should be collected from the sludge discharge chute.

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     B.   Sludge Press (plate and frame):  This is a batch
          process and discharges sludge cake intermittently.
          Sludge is dewatered in the press until plates are full.
          The unit is then opened and sludge cake is dropped into
          a bin.  Samples should be collected directly from the
          storage bin.

     C.   Drying Beds (drying lagoons, cement pads, sand beds,
          vacuum assisted drying beds):  Drying beds are also a
          batch process.   Each bed should be divided into
          quarters.  One grab sample should be collected from the
          center of each quarter and all grabs combined from all
          beds to form a complete sample.  Sludge should not be
          sampled until ready for removal from beds.  The
          criteria for removal vary from facility to facility.
          Sludge should be collected from beds which are ready
          for clearing, as deemed by the facility's manager.
          Drying beds are normally encountered at smaller POTWs,
          where sludge production is variable.  Therefore, sample
          scheduling must be coordinated to take place when
          sludge is available and ready for removal.

     D.   Compost Piles:   This is an additional conditioning
          process in which the dewatered sludge (from one of the
          previous processes) is mixed with a bulking agent such
          as wood chips,  aerated in large piles, and allowed to
          stabilize.  This process takes a few weeks.  The sample
          should be collected from piles which have completed
          composting and are ready for disposal.  A
          representative sample scheme should be determined
          through discussions with the compost facility manager.
     Liquid Sludge Collection Point

Liquid sludge normally is transported off the POTW site in tanker

trucks.  The sampling point should be as close to the truck

loading point as possible.  The ideal liquid sludge sample point

would be at the end of the hose or pipe that is used to fill the

tanker truck.  If this is inaccessible, optional sampling points

such as taps on sludge process piping should be used.  When

locating a sampling point within the process piping, the
                                10

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following procedures should be followed to ensure that

representative samples are obtained.

     A.   In sludge treatment process trains the most represent-
          ative sample typically is obtained from a tap on the
          discharge side of sludge pumps.  Flow at this point in
          the system is turbulent and the sludge is well mixed.

     B.   If a sample is drawn from a tap on a pipe containing
          sludge that is distant from the sludge pump, the
          average flow velocity of the sludge in the pipe should
          be determined.  Average velocities of less than 2 feet
          per second are likely to result in solids separation
          and settling, with an attendant effect on sample solids
          content, depending on the location of the tap (top,
          side or bottom of the pipe).  Given a choice, a tap on
          the side of the pipe is preferable.
3.2   Sample Collection Procedures

The following general steps are to be taken by the sampling team

for proper sample collection:

     A.   The sampling team leader, through consultation with the
          POTW Manager, should establish the number of sludge
          types leaving the plant for final disposal and the
          sample points for each sludge type as designated in
          Section 3.1.  The percent solids of each type also must
          be established.  Sludges with solid contents more than
          2 percent should use the sample volumes shown in Table
          1; sludges with solid contents less than 2 percent
          should use the sample volumes listed in Table 2.  This
          information, along with contacts, phone numbers,
          facility address, directions to facility, and necessary
          safety equipment required (hard hat, safety shoes,
          etc.), should be written up in a pre-sampling report.
          One copy each should go to the project manager, sample
          team, and file.

          If unexpected difficulties are encountered on site when
          locating sludge sample points, or if sampling is
          impossible, the project manager should be notified
          immediately and sampling plan modifications made.

     B.   To remove any sample contamination potential, all
          sampling equipment is to be made of polyethylene or
          polypropylene, used only once, and discarded.


                                11

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                             TABLE  1
                   SAMPLE  CONTAINER DESCRIPTIONS

               Sludge Samples Containing >2% Solids
SAMPLE TYPE
GC/MS  for:
Semi-volatile  Org
Volatile Organics

GC/MS  for:
Dioxin/Furan

GC  for:
Pesticides/PCBs
Herbicides

ICP &  AA for:
27  IFB metals

Non-conventionals:
     Fluoride
     TKN
     Nitrate
     Nitrite
     Phosphorous
     % Solids
     Cyanide
 G  -  glass
 P  -  polyethylene
VOLUME REQUIRED
   2  each  500ml
   2  each  4oz
     500ml
  2  each  500ml
     500ml
     500ml

  4  each  500ml
 TYPE OF
CONTAINER
    G
    G
    G
    G
                                 12

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                             TABLE  2
                   SAMPLE  CONTAINER  DESCRIPTIONS

               Sludge Samples Containing <2% Solids

                                                    TYPE OF
SAMPLE TYPE                 VOLUME REQUIRED        CONTAINER

GC/MS  for:
Semi-volatile Org             4 each 500ml             G
Volatile Organics             4 each 4oz               G

GC/MS  for:
Dioxin/Furan                     500ml                  G

GC for:
Pesticides/PCBs              4 each 500ml              G
Herbicides                   2 each 500ml              G

ICP & AA for:
27 IFB metals                    500ml                  P

Non-conventionals:           4 each 500ml              P
     Fluoride
     TKN
     Nitrate
     Nitrite
     Phosphorous
     % Solids
     Cyanide
G - glass
P - polyethylene
                                13

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     Polyethylene gloves also must be worn to prevent sample
     contamination and to provide for worker safety.

C.   Prior to sample collection, each sample container
     should be labeled with a sample number.  A set of
     sample numbers (all identical) should be used for one
     sample point and discarded.  Each sample number label
     should have the sample type written on it (i.e.,
     metals, classicals, dioxin/furan, extractables, VOA
     unpreserved, VOA unpreserved duplicate, VOA trip blank,
     VOA trip blank duplicate, pesticides/PCB's or
     herbicides).  Some labels are preprinted; others will
     require the sample type to be written in.  After the
     sample number is applied to the container, a piece of
     wide clear type should be applied to protect the label
     from dirt and liquids.  If a label is mis-marked, it
     should be replaced; do not write over a mistake.
     Dioxin/furan samples should be labeled on both the
     inside glass sample container and outside plastic
     secondary container.  Only one metals sample is
     collected and the label used may say ICP or AA.

D.   At each sampling point, the required amount of sample
     should be collected, following procedures as described
     in this document.

E.   Fifteen percent of the samples are to have duplicates
     collected.   Duplicate samples are to be identified with
     a new sample number.  There should be no written
     reference to the duplication of samples on traffic
     reports.

F.   Organic volatile trip blanks should be used to
     determine the extent of contamination, if any, arising
     from sample container handling and field conditions
     encountered during the POTW visits.  Trip blanks are
     organic-free samples of reagent grade water prepared by
     a designated laboratory before the sampling trip.
     These blanks are to be handled and shipped with the
     collected sludge samples to the laboratory for
     analysis.  These blanks should not be opened until
     arrival at the laboratory.   One set of two trip blanks
     will be used at 15 percent of the sites.

G.   All sample containers (including trip blanks) should be
     sealed by applying a piece of clear wide tape around
     the top,  thus preventing the lid from popping off or
     unscrewing.  Each glass sample container should be
     wrapped with a piece of bubble wrap.  The bubble wrap
     should be secured with a piece of shipping tape.
                           14

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     H.   After all containers have been taped and wrapped, they
          should be packed into their respective coolers.  All
          material (except one layer of bubble wrap on the bottom
          of the cooler) should be removed from the cooler and
          the cooler lined with a large trash bag.  Each sample
          container then should be packed into the cooler, and
          ice should be applied to the samples.  All ice should
          be packed in zip-lock bags to help prevent any leaking
          during shipment.  With sample containers and ice inside
          the cooler, the trash bag should be tied closed (also
          to help prevent leaks).  More bubble wrap should be
          added to fill the remaining space in the cooler, the
          pink and gold copies of trip report enclosed on top,
          and the cooler closed and wrapped with shipping tape.

     I.   Refer to Appendix B for instructions on completing
          traffic reports and other pertinent information about
          the Sample Control Center.

     J.   Each cooler should be shipped via overnight delivery
          service.  The Sample Control Center should be called
          to provide them with sample collection information.

     K.   The sampling team also will record site information.
          These data will be recorded on a preprinted log sheet
          and will include at least:  date, POTW name and
          address, name of POTW contact, sample identification
          number and sample point description, basic descriptions
          of POTW sludge treatment processes and final sludge
          disposal method(s).
3.2.1  Solid Sludge Sample Collection

At the sample point(s), a sample of solid sludge will be

collected using a polyethylene pail and polypropylene scoop.

     A.   Belt Press/Centrifuge/Vacuum Filter:  These sludge
          dewatering processes are continuous.  When one or a
          combination of these dewaterinq devices are encountered
          and used to dewater the same sludge type, then only one
          sample is collected.

          1.   If just one dewatering unit is present, a
               sufficient amount of solid sludge is collected
               (refer to sample amounts in Table 1) in the
               polyethylene pail directly from the sludge
               discharge chute.  The sample is thoroughly mixed
               with the polypropylene scoop and/or coring device
               (Figure 2).  The sludge should be transferred to

                                15

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          FICUftE 2.  Coring
*These devices do very well at roixinq and reducing
 particle size of samples, as well as the actual sample
 collection.

                        16

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          the required sample containers by means of the
          polypropylene scoop as described in Section 3.2.2.

     2.   If two or more dewatering units (any combination)
          machines are present (dewatering the same sludge
          type), equal amounts of solid sludge are to be
          collected from each discharge point and combined
          in the polyethylene pail, the sample thoroughly
          mixed with the polypropylene scoop and/or coring
          device, and the sludge transferred to the required
          sample containers by means of the polypropylene
          scoop as described in Section 3.2.2.

B.   Sludge Press (plate and frame):  To collect a
     representative sample, at least four points within the
     sludge bin must be selected.  An equal amount of sample
     is collected (refer to Table 1) from each point and
     combined in the polyethylene pail.  The sample is
     thoroughly mixed with the polypropylene scoop and/or
     coring device,  and the sludge is transferred to the
     required sample containers by means of the
     polypropylene scoop as described in Section 3.2.2.

C.   Drying Beds:  The sludge must be sufficiently dry
     before sampling may take place.  The sludge dryness
     will vary based on the particular POTW's circumstances.
     The sampling visit should be scheduled to coincide with
     a POTW's decision that a drying bed is ready for
     cleaning.   Sludge should be collected from only those
     beds deemed ready for cleaning.  The POTW Manager's
     assistance should be used for scheduling.

     1.   To collect the sample,  the bed is divided into
          quarters and equal amounts of sample are grabbed
          from the center of each quarter using a coring
          device.  Enough sample should be collected to fill
          the sample containers (refer to Table 1).  The
          sample should include the entire depth of sludge
          on the bed.  Care must be taken not to include
          large amounts of the drying bed sand when the
          sample is collected.  A small amount of sand is
          allowable though, as this would be representative
          of the fact that during normal sludge removal,
          small amounts of sand are usually taken.  The four
          grabs should be combined in the polyethylene pail,
          the sample thoroughly mixed with the polypropylene
          scoop and/or coring device,  and the sludge
          transferred to the required sample containers by
          means of the polypropylene scoop as described in
          Section 3.2.2.
                           17

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          2.   If more than one drying bed is used to dewater the
               same sludge type, the above sampling technique
               should be used on each bed.  All the samples
               should be combined in the polyethylene pail, the
               sample thoroughly mixed with the polypropylene
               scoop and/or coring device, and the sludge
               transferred to the required sample containers by
               means of the polypropylene scoop as described in
               Section 3.2.2.

     D.   Compost Pile:  A grab sample should be collected from a
          compost pile or piles that are ready for disposal using
          the polyethylene pail, scoop and corer (refer to Table
          1 for total amount of sample needed).  The compost pile
          should be divided into equal sections.  Using the
          coring device, equal amounts of sample should be
          collected from each section to form a complete grab
          sample.  The sample should be thoroughly mixed with the
          polypropylene scoop and/or coring device and the sludge
          transferred to the required sample containers by means
          of the polypropylene scoop as described in Section
          3.2.2.
3.3.2 Solid Sludge Handling

The following describes the procedures for the handling of solid

sludge samples and filling of sample containers.  Refer to

Table 1 for sample volumes.


     A.   Organic Volatiles/Semi-volatiles:  The sludge should be
          thoroughly mixed in the sample pail, using the
          polypropylene scoop, and the labeled sample container
          filled.  The sludge should be carefully packed into the
          container so as to avoid air spaces.  Covering one's
          hand in a clean polyethylene glove and packing the
          sludge with the fingers seems to be the easiest method.
          The labeled container should be filled to overflowing,
          and the lid screwed on, wrapped, and sealed with clear
          tape.

     B.   Dioxin/Furan:  The sludge should be thoroughly mixed in
          the sample pail, Busing the polypropylene scoop, and the
          labeled sample containers filled to four-fifths full.
          This is to enable expansion of the samples when they
          are stored at <0°C.   Storing at <0°C preserves the
          samples and prevents biological activity that may
          change the chemical characteristics of the sludge.  Air

                                18

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          spaces are of no concern.  The lid should be wrapped
          and sealed with clear tape.  These samples are to be
          frozen to facilitate a longer holding time before
          analysis.

          Pesticides/PCBs/Herbicides, Metals and Non-
          Conventionals:  The sludge should be thoroughly mixed
          in the sample pail, using the polypropylene scoop, and
          each labeled sample container filled to within 1/2 inch
          of top.  This provides room for expansion should there
          be any gas production due to biological activity.  Air
          spaces within the sludge are of no concern.  The lid
          should be wrapped and sealed with clear tape.
3.2.3 Liquid Sludge Sample Collection

At the sample point, liquid sludge should be collected directly

into the 14-quart polyethylene pail.  Enough sample should be

collected to fill the sample container (refer to the appropriate

table, Table 1 or Table 2).  When drawing the liquid sludge from:

     A.   Completely Mixed Tank:

          1.   The POTW operator should start and run the pump
               for 5 minutes to clear the line of stagnant
               sludge.

          2.   Sludge must be allowed to flow for several seconds
               from the tap (or sample outlet) prior to sampling
               in order to flush out stagnant sludge and solids
               that may have accumulated in the tap.

          3.   The polyethylene pail should then be filled.



     B.   Unmixed Tank:

          1.   An unmixed tank will have a sludge layer and
               supernatant layer; the sludge pump must draw from
               the sludge layer.

          2.   The POTW operator should start and run pump for 5
               minutes to clear the line of stagnant sludge.
                                19

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               Sludge must be allowed to flow for several seconds
               from the tap (or sample outlet) prior to sampling
               in order to flush out stagnant sludge and solids
               that may have accumulated in the tap.

               The polyethylene pail should then be filled.
Before transferring liquid sludge into sample containers (see

Section 3.2.4), the liquid sludge should be manually agitated in

the pail with a polyethylene ladle until thoroughly mixed.



3.2.4 Liquid Sludge Handling

The following describes the procedures for the handling of liquid

sludge samples and filling of sample containers.  Refer to Table

1 or Table 2 for sample volumes (this will be based on the

expected percent solids of the sample).

     A.   Organic Volatiles/Semi-volatiles:  The sludge should be
          thoroughly mixed in the sample pail, using the
          polyethylene ladle, and each labeled sample container
          filled.  The sludge should be carefully side-poured
          into the container so as to avoid entrapping air within
          the sample.  The container should be filled to
          overflowing and the lid screwed down.  The sample
          should be checked for air bubbles.  To do this, the
          container is turned up-side-down and the lid tapped.
          If air bubbles rise up, the container should be opened
          and filled with additional sample.  When there are no
          further air bubbles, the container should be wrapped
          and the lid sealed with clear tape.

     B.   Dioxin/Furan:  The sludge should be thoroughly mixed in
          the polyethylene pail, using the polyethylene ladle,
          and each labeled sample container filled to four-fifths
          full; this allows for sample expansion at <0°C.
          Storing at <0°C will preserve the samples and prevent
          any biological activity.  Air spaces in the sample
          container are of no concern.  The lid should be wrapped
          and sealed with clear tape.  These samples are  to be
          frozen to facilitate a longer holding time before
          analysis.


                                20

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1

t
                 C.   Pesticides/PCBs/Herbicides, Metals and Non-
                      Conventionals:  The sludge should be thoroughly mixed
                      in the polyethylene pail, using the polyethylene ladle,
                      and each sample container filled to within 1/2 inch of
                      the top.  This will provide room for expansion should
                      there be any gas production due to biological activity.
                      Air spaces in the sample containers are of no concern.
                      The lid should be wrapped and sealed with clear tape.
            4.0   SAMPLE HANDLING AND CUSTODY

            This section describes the procedures for sample handling and

            shipment.



            4.1  Sample Handling

            Except for mixing of samples in the sample pail, no modifications

            to the structure or content (removal of plastics, paper, etc.) of

            the samples will be performed.   Sample transfer will be kept to a

            minimum.   The sludge will be placed in polyethylene or glass

            sample containers which have been analyzed for quality control by

            the supplier and which are certified to meet U.S. EPA cleanliness

            specifications.



            4.2  San>ple Preservation

            Once a sample is collected,  steps will be taken to preserve the

            chemical and physical integrity of the sample during transport

            and storage prior to analysis.   All samples will be immediately

            cooled to  a temperature of 4°C or  less using regular  (wet)  ice

            (which has been  purchased and sealed in zip-lock bags prior to

            the sampling visit)  and shipped promptly to the designated
                                           21

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laboratories.  Upon arrival at the laboratories, samples will be
preserved further or analysis begun as appropriate within 48
hours of the sample collection.

4.3  Sample Shipment
All samples will be shipped from the field on the day of
collection using an overnight commercial delivery service.  If
circumstances prohibit this, samples will be kept on ice and
shipped in the most expedient method available.

The shipment box will be of sturdy construction and insulated to
provide the proper environment for preserving the samples at <4°C
(in this case a regular, 28-quart cooler).  Each sample container
will be sealed with clear tape to prevent lid removal or leakage.
All glass sample containers will be enclosed in bubble wrap.  All
sample containers will be securely packed in the shipment box
with additional bubble wrap.  On the outside of the shipment
container the following should be placed: 1) a shipping label
with the complete address of the receiving laboratory including
the responsible laboratory person receiving the samples, 2) a
designated box number to indicate to the receiver exactly how
many sample boxes are included in the shipment, and 3) "Fragile"
and "This End-Up" labels.
                                22

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4.4  Field Custody Procedures

Each sample container will have a label attached  (Figure  3) and

covered with clear plastic tape to prevent solvent attack.

Shipment record forms will be written for each group of samples

shipped to a particular laboratory.  These forms will be  the

standard Sample Control Center Organics Traffic Report, Metals

Traffic Report, and  (generic) Sample Traffic Report shown in

Figures 4, 5 and 6.  The pink and gold copies of each form will

accompany sample shipment to the laboratory.  The yellow  copy of

each form will remain in the custody of the sample team.  The

white copy will be delivered directly to the Sample Control

Center.  Additional details are provided in Appendix B.



5.0   SAMPLING EQUIPMENT

This section lists the sampling supplies and equipment to be used

by the sampling team while in the field.  Two sets of clean

equipment will be saved for an equipment blank analysis.  The

study will consist of soaking each piece of equipment for 72

hours in laboratory water and analyzing the water for

contaminants which may have leached from the sample equipment.



5.1   Sampling Equipment

     -Sample kit (to be prepared prior to sampling visits)

          Sampling kits will be prefabricated and ready for use
          before sampling begins.  The kits will contain:

               -High impact plastic coolers with lids

               -Sample containers (see Table 1 and/or Table 2)

                                23

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EXAMPLE OF SAMPLE NUMBER LABELS
16272-c
Composite
16272-cB
Composite Blank
16272.8
Grab
16272-V1
VOA Preserved
16272-V2
VOA Preserved Dup
16272-V3
VOA Unpreserved
16272.V4
VOA Unpreserved Dup
16272.VB1
VOA Trip Blank
16272.VB2
VOA Trip Blank Oup
16272-Other
16272
16272
16272
1G272
16272
1627'2
16272
16272
16272
16272
                16272.M1
                  Metals ICP


                16272.M2
                  Metals AA

                16272-other
16272


16272


16272
        Figure  3.
                                             24

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USEPA INDUSTRIAL TECHNOLOGY DIVISION
SAMPLE CONTROL CENTER
PO. BOX 1407
ALEXANDRIA, VA 22313
703/557-5040 / FTS-8-557-5040
                                                              EPISODE NO:
                                RANGE OF SAMPLE NOS:
                              ORGANICS TRAFFIC REPORT
 INDUSTRIAL FIRM SAMPLED
 CITY .


 STATE
 INDUSTRIAL CATEGORY
 CONFIDENTIAL 	YES	NO


 SAMPLING OFFICE
 SAMPLER
                              SAMPLING DATE


                              BEGIN 	


                              END 	
SHIPPING INFORMATION


SHIP TO


ATTN




CARRIER


AIRBILL NO:


DATE SHIPPED
                      SAMPLE POINT DESCRIPTION
                                       SAMPLE TYPE
SAMPLE
NUMBER










RAW WATER
(CITY, RIVER. WELL)










IN LINE PROCESS










UNTREATED EFFLUENT
(RAW WASTE WATER)










TREATED EFFLUENT










OTHER
(SPECIFY)










ADDITIONAL SAMPLE
DESCRIPTION










PH LEVEL










SAMPLE POINT FLOW
UNITS










_ COMPOSITE
C (EXTflACTABLE OHGANICS)










CB COMPOSITE BLANK










_ GRAB I
u (£XTRACTABLE ORGANICS) |










V1 VOA PRESERVED j










uo VOA PRESERVED I
»« (DUPLICATE) |










V3 VOA UNPRESERVED










... VOA UNPRESERVED ]
" (DUPLICATE) |










VB1 VOA TRIP BLANK










UB4 VOA TRIP BLANK
VB* ((DUPLICATE)










OTHER
SPECIFY










   WHITE - SCC COPY   YELLOW — SAMPLER COPY   PINK — LAB COPY FOR RETURN TO SCC  GOLD — LAB COPY
                                  Figure  4.
                                                                                       25

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USEPA INDUSTRIAL TECHNOLOGY DIVISION
SAMPLE CONTROL CENTER
P.O. BOX 1407
ALEXANDRIA, VA 22313
703/557-5040 / FTS-8-557-5040
                                                              EPISODE NO:
                               RANGE OF SAMPLE NOS:
                                METALS TRAFFIC REPORT
 INDUSTRIAL FIRM SAMPLED
 CITY- _


 STATE:
 INDUSTRIAL CATEGORY
 CONFIDENTIAL:	YES	NO


 SAMPLING OFFICE
 SAMPLER
SAMPLING DATE


BEGIN 	


END. 	
SHIPPING INFORMATION

SHIP TO'	


ATTN:	
                              CARRIER
                              AIRBILL NO-
                              DATE SHIPPED
                      SAMPLE POINT DESCRIPTION
                                       SAMPLE TYPE
SAMPLE
NUMBER










RAW WATER
(CITY. RIVER WELL)










IN LINE PROCESS










UNTREATED EFFLUENT
(RAW WASTE WATER)










TREATED EFFLUENT










OTHER
(SPECIFY)










ADDITIONAL SAMPLE
DESCRIPTION










PH LEVEL










SAMPLE POINT FLOW
UNITS





















U1 METALS TASK I
M1 (ICP ONLY)










*
to
<
*—
CO
h
CM
s










METALS OTHER
[SPECIFY)










    WHITE - SCC COPY   YELLOW - SAMPLER COPY   PINK - LAB COPY FOR RETURN TO SCC   GOLD - LAB COPY

                                   Figure  5.
                                                                                        26

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USEPA INDUSTRIAL TECHNOLOGY DIVISION
SAMPLE CONTROL CENTER
P.O. BOX 1407
ALEXANDRIA. VA 22313
703/557-5040 / FTS-8-557-5040
                                                               | EPISODE NO:
                                 RANGE OF SAMPLE NOS:
                                      TRAFFIC REPORT
 INDUSTRIAL FIRM SAMPLED
 CITY  .


 STATE.
 INDUSTRIAL CATEGORY
 CONFIDENTIAI	YES 	NO


 SAMPLING OFFICE
 SAMPLER
                               SAMPLING DATE


                               BEGIN 	


                               END  	
SHIPPING INFORMATION


SHIP TO: 	


ATTN: 	
                               CARRIER
                               AIRBILL NO
                               DATE SHIPPED
                       SAMPLE POINT DESCRIPTION
                                        SAMPLE TYPE
SAMPLE
NUMBER










RAW WATER j
(CITY RIVER, WELL) |










IN LINE PROCESS










UNTREATED EFFLUENT
(RAW WASTE WATER)










TREATED EFFLUENT










OTHER
(SPECIFY)










ADDITIONAL SAMPLE
DESCRIPTION










UJ
>
UJ
r
a.










SAMPLE POINT FLOW
UNITS 	




















































,












    WHITE - SCC COPY   YELLOW - SAMPLER COPY   PINK - LAB COPY FOR RETURN TO SCC  GOLD - LAB COPY
                                    Figure  6.
                                                                                        27

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5.0   SAMPLING EQUIPMENT



     This section lists the sampling supplies and equipment to



used by the sampling team in the field to collect samples.
5.1  fiftTl ing Equipment



     -Sample kit (to be prepared prior to sampling visits)



     -Disposable 14 quart polyethylene pails



     -Disposable polyethylene gloves



     -Disposable polypropylene scoops



     -Disposable stainless steel corers



     -Disposable polyethylene ladles








5.2   Miscellaneous



     -Clear tape (to seal sample containers)



     -Pack ing tape



     -Writing tools



     -Clear plastic zip-lock bags



     -Shipping materials



     -Shipping instructions and appropriate shipping  forms



     -Trash bags
                                                                28

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6.0   SAMPLING KITS



     Sampling kits will be prefabricated and ready for use before



     sampling begins.   The kits will contain;



     -High impact plastic coolers with lids



     -sample containers (refer to Table I)



      all sample containers will be certified  to meet USEPA



      cleanliness specifications and will have been quality



      control analyzed  by the supplier



     -packing materials (bubble wrap,  peanuts, etc.)
                                                               29

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SAMPLE TYPE

GC/MS for:
Semi-volatile Org
Volatile Organics

GC/MS for:
Dioxin/Furan

GC for:
Pesticides/PCBs
Herbicides

ICP & AA for:
27 IFB metals

Non-conventionalsj
     Fluoride
     TKN
     Nitrate
     Nitrite
     Phosphorous
     % Solids
     Cyanide
                             TABLE  I
                  SAMPLE CONTAINER  DESCRIPTIONS
VOLUME REQUIRED
     500ml
   2  each  4oz
     500ml
  2 each  500ml
     500ml
     500ml

  4 each  500ml
 TYPE OF
CONTAINER
    G
    G
    G
    G
    P

    P
G - glass
P - polyethylene
                                                               30

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                               APPENDIX A


              COMMONLY  USED  SEWAGE SLUDGE  SAMPLING POINTb
      Sludge Type

Primary Sludge  -




Activated Sludge -



Trickling Filter Humus -
Anaerobically Digested
  Sludge -

Aerobically Digested
  Sludge -
Thickened Sludges -


•eat Treatment Sludge -
           Sampling Point

 Most frequently sampled from taps on the dis-
 charge side of positive displacement pumps.
 Difficult to sample from wells or pits  due to
 solids separation.
 Sampled from taps on lines or from open channel
 flows.   Open channel flow  can be  considered an
 acceptable sample point if the flow is  well
 mixed.

 Sampled at taps on discharge lines from pumps or
 from wells,  pits or channels.   Care should be
 taken  to assure adequate mixing,  since  humus has
 a greater tendency for  solids separation than
 activated sludge.
 Typically sampled from  taps on the discharge side
 of positive  displacement pumps.
 Frequently sampled  from taps on discharge lines
 from pumps.   In some eases,  particularly where
 batch digestion is  used, sludge may be  sampled
directly from the digester.  Two cautions are in
order concerning this practice:
 (1)  If  aerated during  sampling, significant air
     will  be entrained  in  the  sample.  Depending
     on  parameters  to be analysed,  this may
     affect  sample  integrity.
 (2)  If  aeration is shut off,  solids separation
     will  occur rapidly in well digested sludge,
     affecting  sample representativeness.

Typically sampled from  taps  on the discharge side
of positive displacement
Generally sampled from taps on the discharge side
of positive displacement pumps after decanting.
Particular care should be taken~"wKen sampling
heat treatment sludge due to:
(1)  High tendency for solids separation, and
(2)  High temperature of sample (frequently 60'C+
Dewatared Sludges (Cake) -
               1) can cause problems with certain
     sample containers due to cooling and
     subsequent contraction of entrained gases.
Generally sampled from the conveyors on which
dewatered sludge is collected.  If sampled from
bulk containers, sample should be taken from
several locations within the sludge

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                                     APPENDIX B
                    USEPA INDUSTRIAL TECHNOLOGY DIVISION
                             SAMPLE CONTROL CENTER
               SAMPLE SCHEDULING AND SHIPMENT INSTRUCTIONS
Sample Scheduling
       To schedule a sampling site, an authorized  requestor  should call the Sample Control
Center (SCC) with the following information:
       o   Name and affiliation and the telephone number of the individual requesting the
           analysis
       o   The analyses requested
       o   Facility name and location
       o   Industrial Category
       o   Industrial Sub Category
       o   Scheduled sampling and shipping dates
       o   Sampling organization, contact, and telephone number
       o   Number and types of samples to be collected
       When an authorized requestor schedules the sampling site, the SCC assigns an Episode
number for the site (an Episode  refers to a group of  samples collected at a given plant or
location within the same calendar  week) and prepares a packet of materials to send to the
Sampler. The packet normally contains the following:
       o   Episode Number assignments
       o   Laboratory assignments
       o   Traffic Reports)
       o   Adhesive Sample Number Labels
       SCC then creates a hardcopy Episode file and enters the scheduling information in the
SAMTRAC (Sample Tracking) System.
Instructions for Completing Traffic Report
       A separate Traffic Report (TR) (see  Attachment  1), is to be  completed for  each
shipment of samples to a laboratory. For samples going to EPA Contract laboratories use the
TR provided by the SCC.
       First,  enter  the  Episode  number  on  the top  right corner of the TR form, where
indicated.  The Episode number is the identifying  number that was assigned by SCC at the
time the sampling was  scheduled. This is followed  by the Range of Sample numbers, which
are assigned by the sampler when samples are packed for shipment to the laboratory^).
       Next,  complete  header information, excluding  the grey  areas on  the  top right of the
form.

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       Along  with the TR forms, the sampler will  receive sequentially numbered sample
labels from SCC.  In order to protect  the labels from water or solvent attack,  labels on the
sample container should be covered with clear, waterproof tape.

       Enter the Sample numbers  (from  the labels) on the lower left side of the TR where
indicated.   Record all Sample numbers  for samples  included within the shipment.   Extra
numbered  labels should be  discarded and new strips  of labels should be used for the next
Episode of samples.

       For each sample, indicate sample point description by checking the appropriate box.
If additional sample  point information is required enter  it in the box  labeled "Additional
Sample Description"  located in the center of the TR. Next record the physical parameters of
the site at the time of sampling (i.e.  pH, effluent flow, etc.). In the remaining boxes indicate
what  type  of  analysis the laboratory is to perform on  a  sample.  Note: Analyses must  be
approved by EPA and requested through SCC at the  time sampling is scheduled, to ensure
that proper arrangements can be made in advance to accommodate the request

       The bottom two copies of the completed TR (pink  and gold copies) must be included
with the  sample shipment to the laboratory. The TR should be enclosed in a clear plastic bag
and securely taped to the underside of the lid of the shipping cooler.

       Following sample shipment, distribute remaining TR copies as follows:

       o   Mail the  top (white) copy to SCC at the address  shown on  the top of the TR
           form.

       o   The second (yellow) copy of TR form is retained by the sampler as  the Region's
           file copy.
Procedures for Coordinating Sample Shipment

       Immediately  following  sample shipment,  call SCC  and  provide  the  following
information:

       o   Sampler name and phone number

       o   Episode number

       o   Sampling date

       o   Sample numbers for samples included in each shipment
       o   Number  of coolers per shipment
       o   Date of shipment
       o   Courier name and airbill  number
       o   Type of  shipment (e.g., overnight,  two-day)

       o   Laboratory samples shipped to

       o   Any irregularities or anticipated problems with the samples

       o   Status  of  sampling  project  (e.g.,  final  shipment,  update   of  future shipping
           schedule)
       SCC notifies  the laboratory  that  samples are  in transit and confirms  arrival of the
samples at  the  receiving  laboratory. SCC  assists in  resolution of any problems concerning the
samples, coordinating with the appropriate sampling personnel.

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       Upon sample  receipt,  the laboratory  completes  designated  sections of  the  TR,
recording date of sample receipt and sample condition, signs the TR, and returns the copy to
SCC. SCC retains the laboratory-signed TR as written confirmation of sample receipt.

       If you have any questions or comments regarding this information please call or write
the Sample Control Center.

USEPA ITD
Sample Control Center
P.O. Box 1407
Alexandria, Virginia 22314
Phone (703) 557-5040
                  U.S. Environmental Protection Agency
                  Region 5, Library  (PL-12J)
                  77 West Jackson Boulevarjd, 12th Floor
                  Chicago, IL  60604-3590

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