United States
Environmental
Protection
Agency
                Office of Water     Office of Solid Waste EPA
                Regulations and    and Emergency    530-SW-8 7-005 C
                Standards (WH-552)  R.«8P?n««  „ _

                      ' D'C'    20 4609  '
   TECHNICAL REPORT: APPENDIX  G


EXPLORATION, DEVELOPMENT, AND PRODUCTION
                        •*»£:'
                       |^™P v %i

          CRUDE OIL AND NATURAL GAS
                          U.S. Environmental Protection Agency
                          Region 5, library (Pt-12J)
                          77 West Jackson Boulevard, 12th Floor
                          Chicago, tl  60604-3590

-------
                           OSW/OW - ITD
       OIL AND GAS EXPLORATION,  DEVELOPMENT, AND PRODUCTION
                        SAMPLING PLAN AND
         SAMPLING QUALITY ASSURANCE/QUALITY CONTROL  PLAN
                           PREPARED FOR
              U. S. ENVIRONMENTAL  PROTECTION AGENCY
                        401 M STREET,  S.W.
                      WASHINGTON,  DC   20460
                           PREPARED BY
                        CENTEC CORPORATION
                     11260 ROGER BACON DRIVE
                     RESTON, VIRGINIA  22090
APPROVAL SIGNATURES:
Susan L. de Nagy
EPA Project Manager
EPA
          y Assurance Officer
Andrew Procko
CENTEC Quality Assurance Officer
Kerri C. Kennedy
CENTEC Project Manager
                         JANUARY 31,  1987

-------
                        TABLE OF CONTENTS
                                                          Page

DISCLAIMER	iii
LIST OF ABBREVIATIONS	   iv

1.0   PROJECT DESCRIPTION 	    1
2.0   PROJECT ORGANIZATION AND RESPONSIBILITY 	    3
3.0   DATA QUALITY REQUIREMENTS AND ASSESSMENTS 	    6
4.0   QUALITY ASSURANCE OBJECTIVES FOR MEASUREMENT
      DATA IN TERMS OF PRECISION, ACCURACY, COMPLETENESS,
      REPRESENTATIVENESS, AND COMPARABILITY 	    7
5.0   SAMPLING PROCEDURES AND PROTOCOLS 	   10
6.0   SAMPLE CUSTODY	   33
7.0   CALIBRATION PROCEDURES AND FREQUENCY  	   38
8.0   ANALYTICAL PROCEDURES 	   39
9.0   DATA REDUCTION, VALIDATION, AND REPORTING 	   40
10.0  INTERNAL QUALITY CONTROL CHECKS 	   41
11.0  SYSTEM AUDITS	   42
12.0  PREVENTIVE MAINTENANCE  	   43
13.0  SPECIFIC ROUTINE PROCEDURES USED TO ASSESS
      DATA PRECISION, ACCURACY, AND COMPLETENESS  ....   44
14.0  CORRECTIVE ACTION 	   45
15.0  REPORTS TO MANAGEMENT	   47

REFERENCES	   48
                                11

-------
                           DISCLAIMER








Mention of trade names or commercial products does not constitute




EPA endorsement or recommendation for use.
                               iii

-------
                      LIST OF ABBREVIATIONS
AA
COD
cm
DOT
EPA
ft
GC
GC/MS
ICP
ICR
in
ITD
ml
mm
NH3
NO 2
NO 3
OSW
OWRS
Pt
POC
QA
QC
RCRA
TCLP
TOG
VOA
Atomic absorption
Chemical oxygen demand
Centimeter
Department of Transportation
Environmental Protection Agency
Foot
Gas Chromatography
Gas Chromatography/Mass Spectrometry
Inductively Coupled Plasma
Ignitability, corrosivity, reactivity
Inch
Industrial Technology Division
Milliliter
Millimeter
Ammonia
Nitrite
Nitrate
Office of Solid Waste
Office of Water Regulations and Standards
Pint
Purgeable Organic Compounds
Quality Assurance
Quality Control
Resource Conservation and Recovery Act
Toxicity Characteristic Leaching Procedure
Total Organic Carbon
Volatile Organics Analysis

-------
                                           Section No. 	1	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                               Page   1   of   48

       OIL AND  GAS  EXPLORATION,  DEVELOPMENT,  AND PRODUCTION
SAMPLING PLAN AND SAMPLING QUALITY ASSURANCE/QUALITY CONTROL PLAN
1.0   PROJECT DESCRIPTION

This document presents the sampling plan and the quality

assurance/quality control (QA/QC) plan for the Office of Solid

Waste/Office of Water Regulations and Standards Exploration,

Development, and Production of Crude Oil and Natural Gas Field

Sampling and Analytical Results Project.!/2  The sampling project

began in early June 1986.  The sampling project was completed in

September 1986.  This final revision to the project sampling plan

and QA/QC plan reflects comments received and includes

clarifications to the original text.



The objective of this sampling project was to collect preliminary

information regarding the constituents of wastes from oil and gas

exploration, development, and production activities.  A secondary

objective was to develop technical information regarding the

sources, volumes, and characteristics of wastes generated from

oil and gas activities.  The results were included in a technical

report providing information about the wastes from this industry

and their waste management practices (EPA 530-SW-87-005).

Samples were collected from exploration,  development, and

production sites.  After collection and preservation, samples

were shipped to laboratories for analysis.  Laboratory tests were

performed for organic compounds, metals,  classical wet chemistry

parameters, and for certain other analytes.

-------
                                           Section No.    1	
                                           Revision No.    6	
                                           Date:  January 31, 1987
                                               Page   2   of   48
This document describes the sampling and quality assurance/

quality control (QA/QC) requirements for the field sampling

portion of the OSW/OWRS Exploration, Development,  and Production

of Crude Oil and Natural Gas Project only (see EPA

530-SW-87-005).  This document describes practices and procedures

for sample collection, preservation, and shipment, and for

quality assurance of these activities.   This document does not

include any portion of the analytical QA/QC or data validation

procedures.

-------
                                           Section No.     2	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                               Page   3   of   48

2.0   PROJECT ORGANIZATION AND RESPONSIBILITY



The sampling project was administered through EPA's Industrial

Technology Division (ITD).  It was organized as shown in Figure

1.  Ms. Susan de Nagy was the EPA Project Manager.  Ms. Kerri C.

Kennedy was the Sampling Project Manager.  Day-to-day sampling

activities were conducted by EPA contract sampling teams in

direct contact with the EPA Project Manager and the Sampling

Project Manager.



On-site activities were managed by a Sampling Engineer.  The

Sampling Engineer was responsible for all onsite decisions

pertaining to safety, equipment, sample collection, and sampling

personnel.



William A. Telliard was the EPA Project Quality Assurance

Officer.  Reporting to Mr. Telliard was Mr. Andrew Procko, the

Sampling Project QA Officer.  Mr. Telliard was responsible for

the quality of the entire sampling project.  Mr. Procko was

responsible for quality assurance of sampling activities.  The

Project QA Officer and the Sampling QA Officer had full authority

to visit sites, audit sampling activities, and audit reports and

data to assure that all sampling activities resulted in data

which met Agency requirements.

-------
      EPA
Project Manager
 Susan de Nagy
       EPA
Project QA Officer
 William Telliard
    Sampling
Project Manager
 Kerri Kennedy
    (CENTEC)
     Sampling
    QA Officer
   Andrew Procko
     (CENTEC)
                          Sampling Teams
                          Bruce Hoskins
                          Jamie Mclntyre
                              (CENTEC)
             Figure 1.  Sampling Project Organization
                                                                            o
                                                                            H>
                                                                            CD
                             O JO CO
                             P (0 (0
                             ft « O
                             fl> H- ft
                             .. W P-
                              H-O
                             Q O 3
                             (u 3
                             3  ZS
                             c z o
                              0 •
                             3*
                                                                              co
                                NJ

-------
                                           Section No.     2	
                                           Revision No.    6	
                                           Date: January 31,  1987
                                               Page   5   of   48
The Sampling Engineer conducted onsite evaluations,  and

supervised sampling, sample preservation, and sample shipment.

The Sampling Engineer was in daily or near daily telephone

communication with the Sampling Project Manager and the EPA

Project Manager for resolution of technical and logistical

problems.  She or he kept detailed records of these activities in

the form of Sampling Reports (Appendix C of the EPA Technical

Report [EPA 530-SW-87-005]) that became a permanent record of

these activities.  These Reports were forwarded to the Sampling

Project Manager and Sampling QA Officer after each site visit.

The Sampling QA Officer audited the Sampling Reports to assure

that proper sampling procedures were followed and documented.

-------
                                           Section No. 	3	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                               Page   6   of   48
3.0   DATA QUALITY REQUIREMENTS AND ASSESSMENTS



3.1   Field Site Investigations

During the site visit, data regarding the physical

characteristics of the site were documented.  This data included

information regarding operating, control, or disposal practices,

and physical characteristics of specific features of the site

(for example, the size of a pit).  These technical data and any

modification of the sampling procedures were documented in the

Sampling Report (Appendix C of the EPA Technical Report [EPA

530-SW-87-005]) for each site.



3.2  Documentation of Sampling, Preservation, and Shipping

The sample site locations were documented in the Sampling Reports

in sufficient detail to permit the Agency and the operator to

unambiguously reference the location from which a given sample

was taken.  The sampling records showed the date, time, and

location sampled.   The individual bottles used for each

fraction of each sample collected were documented on the

EPA-ITD Sample Control Center "Traffic Report" for that sample.

A copy of the Traffic Report became a permanent part of the

Sampling Report.  Shipping records, in the forms of copies of

bills of lading or airbills became a permanent part of the

sampling records,  so that sample holding times could be audited.

-------
                                           Section No.     4	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                               Page   7   of   48

4.0   QUALITY ASSURANCE OBJECTIVES FOR MEASUREMENT DATA IN TERMS
      OF PRECISION, ACCURACY, COMPLETENESS, REPRESENTATIVENESS,
      AND COMPARABILITY
4.1   Precision and Accuracy

Measurements of concern to this sampling project included length,

width, height, and volume.  Linear measurements (length, width,

and height) were essential to identify and obtain the sampling

location within a site (for example, the center of a quadrant in

a pit).  These measurements were taken using a standard tape

measure, accurate to 0.32 cm (1/8 in).



Volume measurement was needed to assure that an adequate size

sample was taken.  Sampling kits were designed which carried the

essential type, number, and size of sample containers.  If these

containers were more than 80 percent full, an adequate sample was

obtained.  (VOA vials were completely filled without any air

space.)  Table 1 lists the contents of one complete sample kit.



4.2   Completeness

Completeness was assured through onsite audits of the sample kit

and containers.  The completeness objective was greater than 98

percent for the sampling portion of this project.

-------
                                                      Section No.
                                                      Revision No.
              TABLE  1.
SAMPLE CONTAINER SIZE
                            Date: January  31,  1987
                                 Page    8    of    48
SAMPLE CONTAINERS REQUIRED  FOR SAMPLE  KITS
     1 gallon (glass)
     1 gallon (glass)
(6) 40 ml VGA vials (glass)
(4) 40 ml VOA vials (glass)
     1 gallon (glass)
     1 gallon (glass)
     1 gallon (glass)
     1 gallon (glass)
(2) 40 ml TOA vials (glass)
     1 quart (glass)
(2) 40 ml VGA vials (glass)
     1 quart (plastic)
     1 quart (plastic)
     1 quart (glass)
     1 quart (glass)
     100 ml  (plastic)
     1 quart (plastic)
     1/2 gallon (glass)

 (2) 40 ml VOA vials (glass)
     1 gallon (glass)
     1 gallon (glass)
      REQUIRED ANALYSIS
    GC/MS for semivolatile  organics
    GC/MS for semivolatile  organics
    GC/MS for volatile organics
    GC/MS for volatile organics
    GC/MS for dioxins/furans
    GC/MS for dioxins/furans
    GC for pesticides/herbicides
    GC for pesticides/herbicides
    TCLP volatile fraction
    TCLP semivolatile fraction
    Purgeable organics
    ICP and AA for metals
    Cyanide
    Oil and grease
    TOC, COD, NH3, NQ2 and  N03
    Sulfide
    Conventionals, RCRA ICR
    Metals, cyanide, conventionals,
      RCRA ICR, TCLP metals
    Purgeable organics
    Refrigerate and retain
    Refrigerate and retain
SAMPLE PHASE

    Liquid
    Solid
    Liquid
    Solid
    Liquid
    Solid
    Liquid
    Solid
    Solid
    Solid
    Liquid
    Liquid
    Liquid
    Liquid
    Liquid
    Liquid
    Liquid

    Solid
    Solid
  '  Liquid
    Solid

-------
                                           Section No. 	4	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                               Page   9   of   48
4.3   Representativeness

Verification was established that each type of facility to be

sampled (e.g., waste pit, produced water) had sufficient number

of samples for data analysis.  For pit sampling,

representativeness of liquid samples was assured by compositing

grab samples taken from horizontal and vertical intervals as

described in detail in Section 5.2.  Produced water samples were

similarly composited (see Section 5.3).  Representativeness of

sludge samples was assured by directing sampling and compositing

of sludge, as described in Section 5.2.  The sampling and

compositing procedures described herein were a balance of

representativeness, consideration of sampling practicality, and

logistics.



4.4   Comparability

The following measures were taken to ensure comparability of

field work performed by different sampling teams:

     o    Uniform written sampling procedures and equipment
          were provided to each sample team.

     o    Standardized field sampling data forms (SCC Traffic
          Reports) were used.

     o    Uniform handling and shipping procedures were
          implemented for all collected samples.

     o   ' Uniform sampling containers were prepared by one
          contractor for use by each sample team.

-------
                                            Section No.     5	
                                            Revision  No.    6	
                                            Date: January  31,  1987
                                               Page    10    of   48
 5.0   SAMPLING  PROCEDURES AND  PROTOCOLS
 This  section  discusses  in  detail  the  sampling  methods  and

 procedures  that were  implemented  by each  sample  team at  each

 designated  sample  site.  Protocols were established on the

 sampling equipment to be utilized, sampling  performance  for pits,

 produced waters, centralized  treatment facilities, and tank

 bottoms,  and  safety measures  to be observed.



 5.1   Sampling Equipment

 This  section  discusses  the equipment  used by the sample  team  in

.the  field to  collect  the required samples.



 5.1.1  List of Sampling Supplies  and  Equipment

 The  following supplies  and equipment  were used in this sampling

 project:

      Cleaning supplies  and equipment

      -   Cleaning brush
         Clean cloth
      -   Tap water
         Pressure sprayer for  water

      Sampling equipment

      -   Sample kit (See Table 1.  Proper  containers were
          supplied by an EPA  contract laboratory.  Sample kit
          preparation is discussed below.)
      -   Five  gallon glass  carboy
         Coring devices  and accessories (Wildlife Supply  Co.,
          Catalog  No. 2440-A10)
         Coring tube liners (glass and Teflon)
         Ponar dredge  (6 inch  x 6  inch) (Wildlife Supply  Co.,
          Cole Farmer Catalog No. J-5471-10)
         Liquid thief, Bacon Bomb  Type (1  pint) (Fisher
          Scientific, Catalog No. 14-209)

-------
                                           Section No. 	5	
                                           Revision No.    6    ~
                                           Date: January 31, 1987
                                              Page   11   of   48

     -  Gauging tape (Sentry Tank Associates, Inc., Item No.
          4464)
     -  Hammer (1 pound)
     -  Wood stakes
     -  Neoprene gloves
     -  Surgical gloves
     -  Measuring tape  (100 feet)
     -  Compass
        Range-finder
        Camera and film (35 mm)
        Stainless steel spoon
        Teflon sheets (used as funnels)
     -  pH test kit
        Free chlorine field test kit

     Miscellaneous

        Bound field logbook
        Masking tape
     -  Packing tape
     -  Writing tools
     -  Cooler boxes or ice chests (for refrigerated samples)
     -  Ice for shipping
        Shipping materials
        Shipping instructions and appropriate shipping forms
        Rope
        Rowboat (2-3 person)
     -  Plastic trash bags
     -  Draeger tubes
     -  Respirator masks
     -  Life jackets


5.1.2  Field Sample Kit Preparation

This section discusses the methods used by the laboratory to

prepare bottles included in the kits assembled for each sample

site visit.  Further discussion of the preservatives and holding

times associated with each sample bottle is presented in Section

6.2, "Sample Preservation."
     VPA Vials.  The bottles, caps, and cap liners were washed

with Alconox soap and water.  They were rinsed with three volumes

of tap water.  A final three volume rinse with deionized water

-------
                                           Section No. 	_	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                              Page   12   of   48

was performed.  The bottles and liners were dried in an oven at

105°C for one (1) hour.  Preservatives were added to the bottles

as soon as they were cool.  The bottles were then assembled and

labeled.



     Organic GC/MS, Dioxin, and Pesticide/Herbicide Bottles.  The

bottles, caps, and cap liners were washed with Alconox soap and

water.  They were rinsed with three volumes of tap water,

followed with a three volume rinse with deionized water.  The

bottles and liners were dried in an oven at 105°C.  The bottles

and liners were rinsed with one volume of methylene chloride and

allowed to air dry before assembling.



     Bottles for Metals and RCRA Analysis.  The bottles, caps,

and cap liners were washed with Alconox soap and water.  They

were rinsed with three volumes of tap water, followed by a three

volume rinse with deionized water.  They were then acid rinsed as

follows:  1:1 nitric acid followed by tap water,  and 1:1

hydrochloric acid followed by tap water.  They were given a final

three volume rinse with deionized water.  Preservatives were

added and the bottles were assembled and labeled.



     Bottles for Cyanides.  The bottles, caps, and cap liners

were washed with Alconox soap and water.  They were rinsed with

three volumes of tap water.  A final three volume rinse with

-------
                                           Section No. 	5	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                              Page   13   of   48

deionized water was performed.  Preservatives were added and the

bottles were assembled and labeled.



     Bottles for COD, TOC, NH3, NC>2, AND NO3.  The bottles, caps,

and cap liners were washed with Alconox soap and water.  They

were rinsed with three volumes of tap water.  The bottles and

liners were then rinsed in NO-CHROMIX - Sulfuric Acid.  They were

again rinsed with three volumes of tap water, followed by three

volumes of deionized water.  Preservatives were added and the

bottles were assembled and labeled.



     Bottles for Sulfide.  The bottles, caps, and cap liners were

washed with Alconox soap and water.  They were rinsed with three

volumes of tap water, followed by a three volume rinse with

deionized water.  Preservatives 'were added and the bottles were

assembled and labeled.



     Bottles for Oil and Grease.  The bottles, caps, and cap

liners were washed with Alconox soap and water.  They were

rinsed with three volumes of tap water, followed by a three

volume rinse with deionized water.  They were rinsed with

acetone.  The bottles and liners were dried in an oven at 105°C.

Preservatives were added and the bottles were assembled and

labeled.

-------
                                           Section No. 	^	
                                           Revision No.    6	
                                           Date: January 31,  1987
                                              Page   14   of   48

     Bottles for POC and Volatile TCLP.  The bottles, caps, and

cap liners were washed with Alconox soap and water.  They were

rinsed with three volumes of tap water.  A final three volume

rinse with deionized water was performed.  The bottles and liners

were dried in an oven at 105°C for one (1) hour.  Preservatives

were added to the bottles as soon as cool.  The bottles were then

assembled and labeled.



     Bottles for Semivolatile TCLP.  The bottles, caps, and cap

liners were washed with Alconox soap and water.  They were

rinsed with three volumes of tap water, followed by a three

volume rinse with deionized water.  They were dried in an oven at

105°C.  They were then rinsed with methylene chloride and dried

in an oven at 105°C.  The bottles were then assembled and

labeled.



5.2  Pit Sampling

This section explains both the rationale for selecting sampling

locations and the proper protocols for sample collection and

handling.



5.2.1.  Sample to be Collected

All pit samples were composited grab samples.  For each pit to be

sampled, two composited samples were taken:  one of solids

(sludge) and one of liquid (supernatant).  If no discrete liquid

-------
                                           Section No.    5	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                              Page   15   of   48

phase existed in a particular pit, no liquid composited sample

was taken.



Only one pit was sampled at a given site.  When a site had

multiple pits, one pit was chosen using the following selection

process:  At a drilling site where there were working pits in

addition to a reserve pit, the reserve pit was sampled.  At a

centralized pit or treatment facility where there was more than

one pit in use, the sampled pit was chosen based on its status at

the time of sampling.  Factors involved in pit selection included

the quantities of sludge and liquid in the pit, the amount of

activity the pit was involved in, accessibility of the sample

points, and safety considerations.  For a site with multiple

centralized pits used primarily for evaporation, a recently

active pit was favored over an inactive pit as such a pit

inactive for a long period of time would probably consist of

analytes in a concentrated form.  Clearly, an inaccessible pit or

a pit  judged unsafe for sampling was not selected at a multiple

pit site.  Reasons for the selection of one pit from a choice of

more than one pit were documented in the individual Sampling

Reports  (Appendix C of the EPA Technical Report [EPA

530-SW-87-005]).



The selection of precise  sampling locations within a pit was by a

specific design.  Using this design, a standard scheme for

selecting sampling points was followed.  As shown in Figure 2,

-------
                                  Section No.     b	
                                  Revision No.    6	
                                  Date: January 31, 1987
                                     Page   16   of   48
•Sample Point
 Figure  2-   Sampling Subdivisions of a Mud Pit

-------
                                           Section No. 	5	
                                           Revision No.    6	
                                           Date:  January 31,  1987
                                              Page   17   of   48
each pit was divided into four equal area sections.   Samples were

taken from the center of each section.  The reason for this

approach was that regardless of the shape or size of the pit, the

method would introduce no subjective judgments that  would

influence the sampling.



5.2.2.  Pit Sample Collection Procedures

The following are the chronological steps taken by the sampling

team for proper sample collection.



I.    The Sampling Engineer established sample points as

      described in Section 5.2.1.



II.   To remove any contamination potential, all sampling

      equipment was rinsed by dipping at least twice in the pit

      prior to taking the sample.



III.  The sampling team attained the sampling location.



IV.   At each sampling point, the required amount of sample was

      collected by means of the relevant sampling procedures

      explained below.

-------
                                     Section No. 	j	
                                     Revision No.    6	
                                     Date: January 31,  1987
                                        Page   18   of   48

         A.  Solids sample collection

At the sample point, a sample of solids (mud or sludge) was

collected using either a coring device or a dredge (Figure

3 and Figure 4, respectively).  The preferred method was

the coring device as the cores contained stratified solids

samples that penetrated the sludge by up to 2 feet.  Dredge

samples were collected only if site specific conditions

prevented the use of the coring device.  Dredge samples

contained mostly solids from the top of the sludge level.



The coring devices were equipped with liner tubes for easy

removal of the collected sample.  The liner tubes were made

of glass or Teflon.  Plastic liners were not used in this

project as they would have contaminated the sample.



Within the same pit, core liners were reused without

cleaning.  Since the final sample was composited,

individual sample point cross-contamination was

irrelevant.



         B.  Liquid sample collection

At the sample point, liquid was collected with a stainless

steel liquid thief sampler.  The thief is pictured in

Figure 5.

-------
                              Section No.    5	
                              Revision No.    6	
                              Date: January 31, 1987
                                 Page   19   of   48
Figure 2.  Hand Coring Device and Accessories
           (From Kahl Scientific Instrument Corp.)
        Figure 4.
Ponar Grab Dredge
(From APHA, 1976)

-------
                                 Section No. 	5_
                                 Revision No.    6
                                 Date:  January 31,
                                    Page   20   of
1987
  48
Figure 5.  Liquid Thief and Tank Thief Hatch
           (From American Petroleum Institute,
           Primer of Oil and Gas Production,
           1976.)

-------
                                          Section  No.      3	
                                          Revision No.     6	
                                          Date:  January  31,  1987
                                             Page    21    of    48
     The design of the  thief  sampler  allowed  a  liquid  sample  to
     be taken at any specific depth.   Several samples  were  taken
     at the same lateral  position  but at  different  depths to
     create a more representative  composited  grab sample.   In
     this projectf liquid samples  were taken  at four evenly
     spaced depths between the liquid surface and the  bottom  of
     the pit.  The reason for this approach was that regardless
     of the shape or size of  the pit  (also for  tanks), no
     subjective judgments influenced  the  sampling.   The
     amount of liquid collected at each depth approxi-
     mately equaled one-fourth of  the composited volume
     required to fill all necessary sample bottles.

     In the same pit, the thief was not cleaned between
     individual samples.   However, the exterior of  the thief  was
     wiped free of any  oil, sludge, or debris picked up by  the
     thief between samples within  the same pit.

V.   Once the individual  samples were collected, they
     were composited, mixed,  and transferred.  For  sludge
     samples, the cores or dredge  samples were  placed  in a
     stainless steel container where  they were  thoroughly
     mixed.  The mixed  sample was  then transferred  to  the
     required sample containers by means  of a stainless
     steel spoon or glass scoop.

-------
                                           Section No.  	5	
                                           Revision No.    6	
                                           Date:  January 31, 1987
                                              Page   22   of   48
      For liquid samples, the first collected grab sample was

      used to fill the VOA vials.  The remaining individual

      samples were placed in a 5-gallon glass container and

      mixed.  Mixing was accomplished by manually agitating the

      container until the contents were visually homogeneous.

      The combined grabs were then transferred to sample

      containers by means of funnel formed from a Teflon sheet.

      Sample transfers between containers were kept to a minimum

      to limit sample contact with the atmosphere.



      Before sample transfer, foreign material such as

      stones, nails, or trash was discarded.  After placing

      the sample in the proper sample containers, all

      disposable items were discarded (glass coring tube

      liners, intermediate glass sample holding containers,

      etc.) and all Teflon and reusable glass items

      cleaned.  Cleaning required washing the equipment with

      detergent and hot water followed by rinses with tap

      water.  Teflon items were shipped from the field to a

      laboratory for cleaning with methylene chloride.

      Reusable items not in direct contact with the sample

      were cleaned with water.



VI.   The sampling team collected all necessary field data

      regarding the samples and attached identifying labels

-------
                                           Section No. 	5	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                              Page   23   of   48

      to the containers.  The samples were packed,

      preserved, and shipped promptly via overnight shipping

      service.



VII.  The sampling team prepared site documentation for the

      approval of the Sampling Engineer.  This included

      recording pertinent data in the log book, drawing site

      maps, documenting Sample Control Center information^

      and photographing the site along with identifying

      landmarks.  Further information about each site was

      obtained by discussing the operation of the facility

      with a representative of each site operator.



5.3  Produced Water Sampling

This section explains both the rationale for selecting sampling

locations and the proper protocols for sample collection and

handling.



5.3.1.  Samples to be Collected

Produced water samples were either grab samples from process

lines or composited grab samples from tanks.  One sample was

collected at each designated site.  Samples were taken from

produced water tanks or process lines.



The following sampling methods were used for produced water

sampling.  Sampling from storage tanks consisted of grab samples

-------
                                           Section No.  	5	
                                           Revision No.    6	
                                           Date:  January 31, 1987
                                              Page   24   of   48

taken from four depths evenly spaced from the liquid surface to

the bottom of the tank, and then combined.  The design of the

thief hatch at the top of a tank prohibited taking samples at

different lateral positions.  When a storage tank was

inaccessible to sampling from the top,  a sample point was sought

in the form of a tap that provided direct discharge from the

tank, or a tap in a flow line exiting the tank.  Samples obtained

at taps or from process lines were taken as grab samples.



5.3.2.  Produced Water Sample Collection Procedures

The following is the chronological steps taken by the sampling

team for proper sample collection.



I.    The Sampling Engineer established sample points for

      storage tank or process line as described in Section 5.3.1.



II.   To remove any contamination potential, all sampling

      equipment was rinsed by repeated dipping in the tank or

      flow line prior to taking the sample.



III.  The sampling point location was attained by means of

      accessing the top of storage tanks, or a valve or

      other process line from the source.

-------
                                           Section No. 	5	
                                           Revision No.    6	
                                           Date: January 31,  1987
                                              Page   25   of   48

IV.   At each sampling point,  the required amount was

      collected by means of a liquid thief or similar

      device at evenly spaced intervals from the liquid

      surface to the bottom.  If an alternate sampling

      device was required, glass, Teflon,  or stainless

      steel construction was used.



V.    From each sample site location, the collected

      individual samples were placed in a container and

      mixed to create the total liquid sample.  Refer to

      Section 5.2.2.B. for mixing and transferring protocols

      for liquid samples.  Foreign material such as stones,

      nails, or trash was discarded.  After placing the

      mixed sample in the proper containers, all disposable

      items were properly discarded and all reusable items

      cleaned as previously discussed in Section 5.2.2.



VI.   The Sampling Engineer was responsible for collecting

      all necessary field data regarding the sample and for

      attachment of identifying labels to the containers.

      Samples were packed, preserved, and shipped promptly via

      overnight shipping  service.



VII.  Proper site documentation was prepared under

      direction of the Sampling Engineer.  This

      documentation included recording pertinent data  in

-------
                                           Section No.     ->	
                                           Revision No.    6	
                                           Date: January 31,  1987
                                              Page   26   of   48

      the log book,  drawing site maps,  and photographing

      the site along with identifying landmarks.  Further

      information about each site was obtained by

      discussing the operation of the facility with a

      representative of each site operator.



5.4. Centralized Treatment Facilities

This section explains both the rationale for selecting sampling

locations and the proper protocols for sample collection and

handling.



5.4.1.  Sample to be Collected

All samples were a series of composited grab samples.  Both

liquid and solid samples were collected.  For each treatment

facility, three samples were taken: liquid influent, liquid

effluent, and effluent sludge.  Specifically directed samples for

treatment facilities were taken from pits, tanks, or process

lines, using the procedures previously described.  For pit

samples, the procedures in Section 5.2.1 were used.  For tank or

process line samples, the procedures in Section 5.3.1 were used.



5.4.2.  Centralized Treatment Facility Sample Collection
        Procedures

The following are the chronological steps taken by the sampling

team for proper sample collection.

-------
                                           Section Mo. 	5	
                                           Revision No.    6    ~
                                           Date: January 31, 1987
                                              Page   27   of   48

I.    To remove any contamination potential, all sampling

      equipment was rinsed by repeated dipping in the pit or tank

      prior to taking the sample.



II.   The sampling team attained the sampling location.



III.  At each sampling point, the required amount was

      collected using equipment specified in the protocols.

       Pit sampling procedures are discussed in Section

      5.2.2.  Tank and process line sampling procedures are

      discussed in Section 5.3.2.



IV.   The individual samples from each sample site were

      placed in a container and mixed to create the total

      sample as previously described in Sections 5.2.2 and

      5.3.2.  See Sections 5.2.2 and 5.3.2 for equipment

      and protocols.  Foreign material such as stones,

      nails, or trash was discarded.  After placing the

      mixed sample in the sample containers,  all disposable

      items were properly discarded and all reusable items

      cleaned as previously discussed in Section 5.2.2.



V.    The Sampling Engineer was responsible for collection

      of all necessary field data regarding the sample and for

      attachment of identifying labels to the containers.  The

-------
                                           Section No.     5	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                              Page   28   of   48

      samples were packed, preserved, and shipped promptly

      using an overnight shipping service.



VI.   The Sampling Engineer was responsible for preparation

      of proper site documentation.  This documentation

      included recording pertinent data in the log book,

      drawing site maps, documenting Sample Control Center

      information and photographing the site along with

      identifying landmarks.  Further information about

      each site was obtained by discussing the operation of

      the facility with a representative of each site

      operator.



5.5   Field Tank Sludge

All samples were composited grab samples.  The preferred method

of sample collection at a particular tank was using the coring

device with the glass or Teflon liner.  If this was not feasible,

sampling was conducted with the Ponar dredge.  After sample

collection, the sample transfer and identification protocols

described in the above section were followed.



5.6   Safety Considerations

It was not known whether the sampled wastes were hazardous.  It

was therefore recommended that the sampling team observe EPA

Level D protection as a baseline.4  EPA Level D protection

provided a minimal level of protective equipment including:

-------
                                           Section No.  	5	
                                           Revision No.     6	
                                           Date:  January 31, 1987
                                              Page   29    of   48
         Protective gloves
         Steel toe shoes
         Cloth coveralls
         Hard hat
         Safety glasses
         Ear plugs (optional)
In addition,  life jackets were worn when sampling from the boat.

Also, when sampling required the use of chest waders to wade into

a pit, a life line was connected from the sampler to the shore.

The Sampling Engineers were fully knowledgeable in the required

levels of EPA protection for different sampling projects and

experienced in conducting field sampling of potentially hazardous

materials.



At each site, an evaluation was made by the Engineer prior to

sampling to determine if any additional levels of protection were

necessary.  This evaluation included the use of portable Draeger

tubes and hand pumps for detection of hydrogen sulfide. The

preliminary waste characterization identified hydrogen sulfide as

a constituent which might have been encountered during sampling.

If the ambient concentration of hydrogen sulfide at a site was

greater than the threshold limit value ceiling of 15 mg/m^ (10

ppm)5, sampling would have been aborted.  No sampling at any site

investigated was cancelled for this reason.
A Draeger unit consists of a calibrated glass tube filled with a

reactant (lead acetate is used in hydrogen sulfide tubes).  A

hand pump is used to draw a known volume of gas through the glass

-------
                                           Section No.     5	
                                           Revision No.    6
                                           Date: January 31, 1987
                                              Page   30   of   48

tube as shown in Figure 6.  The degree of color change in the

reactant denotes the concentration.  Several scales are usually

presented on the tube for high and low concentrations.  According

to Neil Adams**,  the quantitative measurements obtained with the

Draeger unit are accurate.  In the hands of trained personnel,

they can be used to detect a wide range of concentrations by

using various tubes and pumped volumes.  Since they are not

electronic, they are not subject to electronic malfunction

onsite.  The unit and tubes are rugged; previously opened tubes

even can be reused for hydrogen sulfide provided that in previous

uses no hydrogen sulfide was detected.°

                                        ^

The Sampling Engineer had the option to abort sampling if workers

experienced eye, skin, or bronchial irritation, or if they were

experiencing narcosis of sufficient degree to increase accident

proneness, impair self-rescue, or materially reduce work

efficiency.



Any further protective equipment required at any particular site

was at the discretion of the Sampling Engineer.  Also at the

discretion of the Sampling Engineer was whether safety conditions

(or the lack of them) warranted cancellation of sampling at a

particular site.  Such conditions included (but were not limited

to) the inability to safely reach the designated sample point,

adverse weather conditions, or incomplete sampling teams.  When

sampling required the opening of a tank thief hatch, the Sampling

-------

-------
                                           Section No.      5	
                                           Revision No.     6	
                                           Date:  January 31,  1987
                                              Page   32    of   48
Engineer wore a gas mask and used a Draeger tube for hydrogen

sulfide gas detection as soon as the hatch was opened.   If a

dangerous level of hydrogen sulfide was found coming from the

tank, sampling would have been aborted.



If sampling at a particular site was to be cancelled due to

safety concerns, this would have been immediately reported to the

EPA Project Manager and the Quality Assurance Officer along with

the reasons for the cancellation.  During the course of the

sampling project, no sampling at a site was cancelled due to

safety concerns.



Prior to sampling at each site,  the sampling team was informed of

emergency procedures, the location of the nearest hospital, the
                                                               4
location of the nearest poison center,  and the corresponding

emergency phone numbers.

-------
                                           Section No.    6	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                              Page   33   of   48

6.0  SAMPLE CUSTODY

This section describes the proper procedures for sample handling,

preservation, and shipment.



6.1  Sample Handling

As described in Section 5, after collecting the individual

samples, sample transfer was kept to a minimum.  Sample contact

with plastic was avoided unless the final sample container was

plastic.



6.2  Sample Preservation

Once a sample has been collected, steps were taken to preserve

the chemical and physical integrity of the sample during trans-

port and storage prior to analysis.  Depending upon the type of

analysis to be performed on the sample, preservatives such as

sodium hydroxide, sulfuric acid, or nitric acid were added to the

sample bottles (see Section 5.1.2).  All samples were shipped to

the laboratories under ice.  All required materials to preserve

samples were included in the sample kits.  Table 2 lists the

preservatives and holding times associated with each sample

container included in the sample kits.



6.3  Sample Shipment

All samples were shipped from the field on the day of collection

using an overnight commercial delivery service unless

circumstances did not permit this.  In that event, samples were

-------
        TABLE  2.
                                                    Section No.
                                                    Revision No.
                                 Date: January 31,  1987
                                    Page   34    of    48
REQUIRED PRESERVATIVES  AND MAXIMUM  HOLDING TIMES
SAMPLE CONTAINER

Metals


Cyanide


Oil and grease


Sulfide


COD, TOG,  NH3,  NO2,
Routine


FCC

VGA vial

VGA vial

VOA vial

Extractable organics
Dioxins/furans
                       REQUIRED PRESERVATIVES
                       HNO3 to pH <2
                       NaOH to pH >12
                       Cool 4°C

                       H2S04 to pH <2
                       Cool, 4'C

                       Zn(C2H302)2
                       Cool, 4°C
    H2SO4 to pH <2
    Cool, 4°C

    Cool, 4°C
    Cool, 4°C

    HC1, Cool,  4°C

    Na2S2O3,  Cool,  4°C

    Cool, 4*C

    Cool, 4°C
Pesticides/herbicides   Cool, 4°C
    Cool, 4°C
TCLP - volatiles       Cool, 4°C

TCLP - extractables    Cool, 4*C
                                  MAXIMUM HOLDING TIME

                                  6 months (except Hg, whose
                                    holding time is 28 days)

                                  14 days
28 days


 7 days



28 days


28 days (except BOD, whose
   holding time is 48 hours)

14 days

14 days

14 days

14 days

7 days until extraction;
40 days after extraction

7 days until extraction;
40 days after extraction

7 days until extraction;
40 days after extraction

14 days

7 days until extraction;
40 days after extraction

-------
                                           Section No.  	6	
                                           Revision No.    6
                                           Date:  January 31, 198f
                                              Page   35   of   48

shipped in the most expedient method available.  The outside of

the shipment container required the following information: a

shipping label with the complete address of the receiving

laboratory including the responsible laboratory person to receive

the samples, a designated box number to indicate to the receiver

exactly how many sample boxes were included in the shipment, and

any required DOT or hazardous waste labels.



Sealed sample containers were packed and sealed in shipping

containers prior to shipment.  Shipping containers were turned

over directly to the shipping agent (overnight shipper, airline,

etc.) whenever possible.  In exceptional circumstances, the

Sampling Engineer enlisted a delivery service or hotel service

staff to turn a shipment over to the shipping agent.  Care was

taken to ensure the integrity and promptness of shipment.

Documentation of the transaction was maintained.



6.4  Field Custody Procedures

Each sample had an identification tag attached to it.  Shipment

record forms were written for each group of samples shipped to a

particular laboratory.  These forms were the standard Sample

Control Center Organics Traffic Reports and Metals Traffic

Reports shown in Figure 7 and Figure 8, respectively.  At least

one copy of each form accompanied sample shipment to a

laboratory.  One copy of each form remained in the custody of the

sample team.

-------
                                                          Section  No.       6	
                                                          Revision No.§
                                                          Date:  January  31,  1987
                                                              Page     36     of     48
USEPA INDUSTRIAL TECHNOLOOY DIVISION
SAMPLE CONTROL CENTER
P.O. BOX 1407
ALEXANDRIA. VA 22313
703/557-5040 / FTS-S-557-5040
                                                        EPISODE NO:
                                             RANGE OF SAMPLE NOS:
                           ORQANIC3 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
ii
li
li
ADDITIONAL SAMPLC
OCSCMIPTION
!f
                                                                             I
    WHITE - SCC COPY  YELLOW - SAMPLER COPY   PINK — LAB COPY FOR RETURN TO SCC   GOLD - LAB COPY
                                Figure 7

-------
                                                         Section  No.        6	
                                                         Revision No.      6	
                                                         Date:  January 31,  1987
                                                              Page     37     of     48
USEPA INDUSTRIAL TECHNOLOOY DIVISION
SAMPLE CONTROL CENTER
P.O. BOX 1407
ALEXANDRIA, VA 22313
703/557-5040 / FTS-B-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) 1










8
!
i





'




L UNTREATED EFFLUENT 1
(RAW WASTE WATER) 1










I










A










ADDITIONAL SAMPLE
DESCRIPTION










i










!
|:











U4 METALS TASK 1
""' (ICPONLV)










... METALS TASK II
"«
-------
                                           Section No.     '	
                                           Revision No.    6
                                           Date: January"31,  1987
                                              Page33of
7.0  CALIBRATION PROCEDURES AND FREQUENCY



This section is not applicable to the f^eld sampling portion of

this project.

-------
                                           Section No. 	8_
                                           Revision No.    6
                                           Date: January 31, 1987
                                              Page   39   of   48
8.0  ANALYTICAL PROCEDURES



This section is not applicable to the field sampling portion of

this project.

-------
                                           Section No.     9	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                              Page   40   of   48
9.0  DATA REDUCTION, VALIDATION, AND REPORTING



During field activities, no analytical parameters were collected

with the exception of tests for pH and free chlorine.  These

tests were conducted in the field by the Sampling Engineer to

provide estimates of the pH and free chlorine content to the

receiving analytical laboratories.  These estimates were used by

the laboratories in decisions about handling and analysis of the

samples.  Since the estimates were not reported as analytical

data, they were not subject to any reduction or validation

procedures.



The remainder of the data obtained were from observations noted

in the field logbook.  These data were not analytical parameters

but site specific information such as the sizes of onsite pits or

the sequence of treatment.  Such data was confirmed by visual

observation where possible in the field.  Notes from logbooks

remained in the possession of the Sampling Engineers until the

conclusion of field sampling unless otherwise directed by the EPA

Project Manager.  Information from the logbooks was compiled and

submitted as part of the Technical Report (EPA 530-SW-87-005).

-------
                                           Section No.     10
                                           Revision No.    6
                                           Date: January 31, 1987
                                              Page   41   of   48
10.0  INTERNAL QUALITY CONTROL CHECKS



The required field quality control check for this project was

five percent field duplicates.  Field duplicates were collected

by the sampling team at the sites designated by the Sampling

Project Manager.  Shipment of field duplicates was concurrent

with a shipment of regular field samples.

-------
                                           Section No.      11	
                                           Revision No.     6	
                                           Date:  January 31, 1987
                                              Page   42    of   48
11.0  SYSTEM AUDITS
System audits were conducted in the field by the EPA Quality

Assurance Officer and the Sampling QA Officer.   The dates of

these audits were documented in the Sampling Reports (Appendix C

of the EPA Technical Report [EPA 530-SW-87-005]).

-------
                                           Section No.     12
                                           Revision No.     6
                                           Date:  January 31,  1987
                                              Page   43   of   48
12.0  PREVENTIVE MAINTENANCE



The Sampling Engineer visually examined all sampling equipment

upon arrival at the sample site to assure it was in proper

working order.  The Sampling Engineer re-examined the equipment

upon completion of sampling to assure that sampling equipment

remained in working order.



To prevent delays in field sample collection or shipment, the

sampling team had in its possession spare parts and tools for

field repair of critical sampling equipment.  Spares of all glass

or other breakable objects used in collection were available.

Extra shipment containers were obtained in the case of damage to

sample shipment containers.

-------
                                           Section No.     13
                                           Revision No.    6
                                           Date: January 31, 1987
                                              Page   44   of   48
13.0  SPECIFIC ROUTINE PROCEDURES USED TO ASSESS DATA PRECISION,
      ACCURACY, AND COMPLETENESS
This section is not applicable to the field sampling portion of

this project as no data generated in the field was subject to the

assessment procedures for statistical precision, accuracy, and

completeness.

-------
                                           Section No.    14
                                           Revision No.    6
                                           Date: January 31, 1987
                                              Page   45   of   48
14.0  CORRECTIVE ACTION



This section describes the conditions or situations that might

have been encountered that could have caused deviations in

standard sampling methods or cancellation of sampling at any

given site.  First, no sampling was conducted with any method

that, in the judgment of the Sampling Engineer, Sampling Project

Manager, EPA Project Manager, Sampling QA Officer, or EPA QA

Officer, endangered any member of the sampling team or would

result in an inaccurate, imprecise, or non-representative sample

being collected.  If safe or representative sampling could not be

achieved, no sampling was performed at that site.



For pit sampling, the following list of preferred and alternate

sampling methods is given.  They are listed in decreasing order

of priority:

     1.   Use of coring tube; sampling points achieved
          by use of rowboat.

     2.   Use of Ponar dredge; sampling points achieved
          by use of rowboat.

     3.   Use of coring tube; sampling points achieved
          by wading into pit or using boards to walk
          into pit.

     4.   Use of coring tube while standing at edge of
          pit.

     5.   Use of Ponar dredge while standing at edge of
          pit.

-------
                                           Section No.    14	
                                           Revision No.    6	
                                           Date: January 31, 1987
                                              Page   46   of   48

If none of the above methods could have been safely used, no

sludge sample would have been taken from the pit.



The limiting factor for pit sampling was the pit condition.   The

pit must have been reasonably accessible.  A breached pit was

sampled for solids only.  A completely evaporated pit or a pit

where the liquids were injected or land applied was sampled for

solids only.  A frozen pit was sampled using a manual auger, ice

picks, or similar appropriate equipment.



Produced water or sludge sampling from tanks were dependent upon

tank condition.  An empty tank would not be sampled.  A tank with

no thief hatch, no valves, or other reasonably accessible opening

would not be sampled.  Any tank of questionable construction

integrity would not be sampled.



Any deviations in sampling procedures were noted in the field

logbook and the individual Sampling Reports (Appendix C of the

EPA Technical Report [EPA 530-SW-87-005]).  Any major deviations

or cancellation of sampling for any reason at a site was

immediately reported to the EPA Project Manager and Quality

Assurance Officer.

-------
                                           Section No.    1->	
                                           Revision No.    6
                                           Date: January 31, 198/
                                              Page   47   of   48
15.0  REPORTS TO MANAGEMENT



15.1  Sampling Reports

A site-specific Sampling Report was generated for each location

visited or sampled.  Each Sampling Report contained the following

information:

         Sample site name and location
         Description of facility
      -  Date sampled
         Attendees' list, including sampling team members, State
           and Federal Government representatives, and other
           observers
         Photographs of site
         Specific sampling equipment used
         Description of disposal or control technology used
           onsite
         Problems encountered during sampling visit
         Deviations from sampling quality assurance plans



These Sampling Reports became part of the Technical Report (SPA

530-SW-87-005).



15.2  Quality Assurance Reports

Quality Assurance Reports were generated by the Sampling QA

Officer.  They contained the results of any and all field audits

conducted during the course of sampling along with any quality

assurance problems and recommended solutions.



At the end of the sampling project, a summary report listing the

non-conformances and corrective actions was produced by the

sampling contractor.

-------
                                           Section No.   References
                                           Revision No.     6	
                                           Date:  January 31, 1987
                                              Page   48    of   48
                           REFERENCES
1.  Environmental Protection Agency,  Contract No.  68-01-7153.

2.  Environmental Protection Agency.   Decision Document on
    Onshore Oil and Gas Regulatory Issues,  February 1986.

3.  Environmental Protection Agency.   Handbook for Sampling and
    Sample Preservation of Water and Wastewater,  September,
    1982.

4.  Environmental Protection Agency.   Dioxin Strategy,  1983.

5.  American Conference of Governmental Industrial Hygienists.
    Threshold Limit Values for Chemical Substances in Workroom
    Air, 1977"

6.  Adams, Neil,  Well Control Problems and Solutions,  Petroleum
    Publishing Company, Tulsa,Oklahoma,1980.

-------