ENVIRONMENTAL SERVICES DIVISION
STANDARD OPERATING PROCEDURES
FOR FIELD SAMPLERS
EPA - REGION VIII
DENVER, COLORADO
MARCH 1986
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ENVIRONMENTAL SERVICES DIVISION
STANDARD OPERATING PROCEDURES
FOR FIELD SAMPLERS
EPA - REGION VIII
DENVER, COLORADO
MARCH 1986
-------
Standard Operating Procedures
For Field Samplers
Revision No. 2 Date: 3/15/86
Page: i
TABLE OF CONTENTS
Page
No.
I. General Information 1
II. Sampling Survey Design Plan 1-4
III. Sampling Procedures 5-14
A. Collection, Handling, Preservation 5-10
1. Collection 5-6
2. Quality Assurance 6-8
3. Preservation 8-10
B. Sample Identification 10-11
C. Chain-of-Custody Procedures 11-14
1. Sample Custody 12
2. Field Custody Procedures 12
3. Transfer of Custody and Shipment 12-13
D. Field Forms 13-14
IV. Flow Measurements 14
V. Personnel Training 15
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Standard Operating Procedures
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TABLE OF CONTENTS (Continued)
Exhibit
No.
Laboratory Services Request A
Required Containers, Preservation Techniques and Holding Times B-1, B-2
Sample Tag C
Hi-Vol Data Record D
Cha1n-of-Custody Record E
NPDES Compliance Inspection Report F
Field Sample Record 3
Official Custody Seal, EPA 7500-2 (R7-75) H
Quality Assurance Project Plan for NPDES Compliance
Inspection Program Appendix A
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Standard Operating Procedures
For Field Samplers
Revision No. 2 Date: 3/15/86
Page: 1
I. GENERAL INFORMATION
Although there are many references available on the proper methodology for
performing laboratory procedures, few such "guides" are available for planning
and conducting field investigations to obtain environmental or hazardous waste
samples. The same amount of care must be exercised in the design and
Implementation of field sampling as 1s exercised 1n the analysis of the
samples. No analytical result is better than the sample from which it was
obtained.
The following guide has been prepared to assist all Region 8 and Region 8
contract people who conduct field sampling. This guidance will make the
sampler aware of the factors affecting sampling so he or she can plan, correct
or adjust a program to assure an accurate representation of existing
conditions.
This guide has been developed to cover samples collected and returned to a
laboratory for analysis. It does not cover automatic in-situ monitoring (such
as continuous gaseous air quality monitors) or inspection procedures (such as
auditing continuous emission monitoring activities, SPCC Inspections, visible
emission observations, etc.).
II. SAMPLING SURVEY DESIGN PLAN
Every field investigation must have a survey design (sampling plan). Each
investigation must be evaluated on an Individual basis. With this approach in
mind, a consideration of several areas common to all field investigations
should assure that the best approach to a particular study is followed and
that the samples obtained are a true representation of the existing conditions.
These items apply equally well to stream and lake studies, municipal and
Industrial effluent sampling, hazardous waste samples and air samples.
Items which are common to most studies:
1. Designate a Project Officer for the study. This person will be
responsible for seeing that the project plan is written and approved
and all subsequent items are carried out. In routine NPDES
compliance work a team leader will be appointed as project officer.
A sampling team leader will be appointed from Environmental Services
Division for sampling requested by other Divisions.
2. Determine why samples are being taken. The basic survey design is
dictated by the objective for sampling. Several objectives for
sampling are:
a. Compliance with discharge permit conditions (routine compliance
monitoring or case preparation studies).
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Standard Operating Procedures
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Revision No. 2 Date: 3/15/86
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b. Air compliance.
c. Baseline information studies.
d. Hazardous waste disposal site studies.
e. Intensive cause and effect studies.
f. Emergency spill and response needs.
3. Review existing information. This would include such information
sources as:
a. Existing Investigation files (permit files, SIP files).
b. Reports of previous studies (Federal, state, universities, etc.).
c. Correspondence files.
d. Personal communications.
Care must be exercised to assure that investigative files and
one-of-a-kind reports are not misplaced nor inadvertently destroyed.
Removal from the office should be discouraged. If the material is to
be taken into the field, copies should be made.
4. Obtain adequate maps and/or diagrams to define the study area.
5. Conduct a reconnaissance of the proposed study area If possible. A
reconnaissance can save much time and energy by eliminating
unsatisfactory study areas. Some analytical work may be useful
during the reconnaissance to assist the laboratory in its analysis by
establishing ranges of values or by surfacing unknown interferences.
This allows the laboratory to adjust procedures if necessary.
Sometimes a reconnaissance may not be possible due to lack of time,
money, people, etc.
6. Make a 11st of proposed sampling locations, sampling frequency, and
sample analyses. In some instances these items will be predetermined
such as for NPDES or RCRA permit compliance monitoring or case
preparation studies. Stream and lake studies, on the other hand,
must be designed with flexibility in mind. In both cases, however,
unpredictability is the rule rather than the exception. Sampling
sites should be proposed with the purpose of the study in mind.
Developing criteria for acceptable sampling sites based upon the
objectives of the study will aid in selecting the stations.
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Standard Operating Procedures
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Control samples from uncontaminated areas adjacent to the primary
study site will be taken when appropriate to provide background data
and to better define the affected area.
In preparing this list, close coordination must be maintained with
the Chemistry and Biology Sections. This is to assure that the
laboratory will be prepared to handle the samples or make other
arrangements for analyses. Laboratory Services Request (LSR) forms
(Form R8 EPA-012, Exhibit A) must be filled out indicating source of
sample and parameters of interest. A copy of the LSR must be
submitted to the laboratory to indicate the anticipated sample load.
The sampler must retain the original LSR and complete filling it out
when the sample 1s collected, making any changes or remarks that will
assist the laboratory in Its work. The original LSR then accompanies
the samples to the laboratory.
7. The field quality assurance (QA) samples to be taken must be
specified (see QA section). The quality assurance project plan
(QAPP) must be referenced (see example Appendix A). If a QAPP does
not exist, it must be written into the sampling plan.
8. Safety must be considered and Included 1n the survey design plan,
listing appropriate safety precautions. Determine need for special
safety gear; for example, protective clothing, breathing apparatus,
first aid equipment, nearest hospital or clinic, emergency
transportation, etc.
9. Make a list of all necessary equipment and supplies. This list
should be prepared in cooperation with all personnel involved in the
study. Items should be checked and rechecked against the list prior
to departure so nothing will be forgotten. The list should include:
a. portable analytical equipment
b. sample preservatives
c. analytical reagents
d. glassware
e. appropriate sampling gear (e.g., Kemmerer samplers, DO samplers,
buckets, air samplers, etc.)
f. sample containers
g. shipping and sample storage containers (ice chests)
h. photographic equipment
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1. Travel Status Accident Report Forms
j. notebooks, sample tags, field data sheets
This list is by no means complete! Special requirements such as
motor boats and/or mobile laboratories require a separate equipment
list.
10. Check the mechanical and/or analytical operation of all equipment
prior to departure. This includes replacing or recharging batteries
as necessary.
11. Obtain all necessary approvals. Develop a schedule for the shipment
of samples back to the Region VIII laboratory if necessary to assure
arrival, pick-up and set-up of the sample within prescribed holding
times and custody requirements. Make other appropriate arrangements
if samples are shipped to contract laboratories.
References:
1. USDI, FWPCA; CWR-5; 1969:
A Practical Guide to Water Quality Studies of Streams.
2. Environmental Protection Agency Manual:
Biological Field and Laboratory Methods for Measuring the Quality of
Surface Waters and Effluents, EPA-670/4-73-001 .
3. Environmental Protection Agency Manual:
Handbook for Sampling and Sample Preservation of Hater and Wastewater,
EPA-600/4-76-049.
4. Environmental Protection Agency:
Methodologies and Flow Measurement Techniques,
_---_
EPA-907/9-74-005.
5. Samples and Sampling Procedures for Hazardous Waste Streams,
EPA-600/2-30-018, January, 1980.
6. Quality Assurance Handbook for Air Pollution Measurement Systems,
vol. II, Ambient Air Specific Methods, EPA-600/4-77-OZ7a.
7. Quality Assurance Project Plan for the TSCA and FIFRA Investigation
Programs. EPA Region VIII. Air and Toxics Division, April 15. 1985.
8. The Quality Assurance Project Plan for the NPDES Compliance Inspection
Program, EPA Region VIII. Environmental Services Division. February 5,
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Standard Operating Procedures
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III. SAMPLING PROCEDURES
A. Collection, Quality Assurance. Preservation
1. Collection
Collection of the sample can be divided Into basically three
types or methods. These are:
a. the grab or discrete sample (water, soil, leachate, etc.)
b. the composite sample (water, soil, leachate, etc.)
c. the continuous sample (usually automatic collection
devices, air samplers, etc.).
The grab or discrete sample is an instantaneous collection of a
single amount of sample.
There are two types of composite samples:
a. the simple composite, and
b. the proportioned composite.
The simple composite is a fixed amount of sample collected at a
fixed time interval and combined to make a single sample for
analysis. This procedure is valid only if flow properties are
relatively constant.
The proportioned composite can be further divided into two basic
types where:
(1) the amount of sample collected is varied with flow, and
(2) frequency of collection is varied with flow.
Proportioned composite samples can be obtained either
manually or by using automated devices.
The choice of collection method is usually dictated by
the circumstances surrounding the sample site such as:
(a) The site must yield samples representative of the
parameters being considered.
(b) The site must have good mixing horizontally,
vertically and longitudinally.
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Standard Operating Procedures
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(c) The site must be accessible and safe. The site
and procedures used to collect the sample must
conform to regulations set forth in the Health
and Safety Manual for Field and Laboratory
Activities, EPA Region VIII.
2. Quality Assurance
Sample quality assurance of the sample starts when the sample is
initially collected. This requires some basic handling
procedures. These are:
a. If several locations are to be sampled during one sample
run which include both clean and polluted sites, use
separate collection equipment (buckets, automatic sampler,
shovels, bailers, coring tools, etc.) at each location.
Where this is not possible or practical, sampling should
progress from the clean areas to the polluted areas. This
lessens the chance of the unintentional contamination of
cleaner samples through the use of contaminated sampling
equipment.
b. Sampling equipment (buckets, funnels, graduated cylinders,
etc.) should be rinsed with the stream, lake or effluent
water to be sampled. PCB's, oil and grease, phenols and
hazardous waste samples should be taken directly into the
sample container. If collection equipment is needed for
PCB's or hazardous waste, one-time-use equipment should be
used, if possible, to eliminate contamination/decontamina-
tion problems. Automated equipment should be properly
cleaned and new intake hose used if appropriate.
c. The sample container must be appropriate to the sampled
parameter. Use special cleaning procedures If necessary.
If cleaned in the field, rinsate field blanks should be
collected.
d. Air samples collected and returned to a laboratory are
usually hi-vol (particulate) or bubbler (24-hour gaseous)
samples. These sampling procedures are defined in EPA
manuals. Refer to Quality Assurance Handbook for Air
Pollution Measurement Systems, Vol II, Ambient ATr Spedfie
Methods EPA-600/4-77-027a.
e. A regular schedule of calibration of field instrumentation
can be found in the Quality Assurance Project Plan for the
NPDES Compliance Inspection Program.
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Standard Operating Procedures
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All Instrumentation used in field activities must be
calibrated prior to field use and periodically thereafter,
according to the manufacturers' instructions. Where
required, field Instrumentation must be calibrated at the
beginning and end of each sampling day.
Continuous sampling devices must be calibrated according to
manufacturer's specifications at the time of field set-up
and checked as often as necessary. Sample lines for
continuous devices must be clean or provided new prior to
each installation.
In those Instances where field equipment cannot be
calibrated, the Project Officer/Team Leader will attempt a
field repair of the affected equipment. The equipment
manager, appointed by an appropriate section chief, is
responsible for seeing that spare parts and other
appropriate items for field equipment are available for
field repairs and to minimize equipment down times. To the
extent possible/practical, backup field equipment should be
available.
A logbook is assigned to each instrument requiring
calibration prior to and during use. these logbooks should
accompany the instruments at all times. Log all
calibration information. Information must include the date
and time of calibration, method of calibration, person or
persons performing the calibration and any comments. Also
include any recommendations regarding needed equipment
maintenance and repair. All instrumentation and logbooks
returned from the field will be examined for maintenance/
repair recommendations and checked for proper operation by
the team leader. Any necessary maintenance will be
performed immediately to assure instrumentation is 1n
operating condition prior to the next use. All maintenance
and repairs performed will be logged with the name of the
individual(s) doing the work. The calibration process is
necessary to insure that the instrument(s) are working
properly and within the range of acceptability as
determined by the manufacturer's specifications and the
equipment manager. The recording of the calibration data
is to maintain a record of documentation of this fact for
later challenges and proof of acceptability.
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Standard Operating Procedures
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f. For major investigations, field blanks for each set of
samples should be prepared in the laboratory, taken to the
field, subjected to the same conditions as the samples and
returned to the laboratory for analyses. These samples
will be a check on contamination which may be Introduced in
the field
g. Field-originated QA samples will be submitted to the
laboratory as appropriate and as often as practical during
the fieldwork season. When QA check samples are submitted
to the laboratory, they will consist of:
(1) One or more "blind" duplicate samples as appropriate
to the study.
(2) "Spiked" samples prepared with known amounts of
constituents added to an ambient water sample.
The field personnel, working 1n coordination with the
Chief, Chemistry Section, will select the sampling
source(s), parameters to be audited, the appropriate spike
and method of field preparation of the "spiked" sample, and
assure the proper sample container and method of preserva-
tion is used. (A suggested procedure for the field
preparation of the "Spiked" samples appears in the Handbook
for Analytical Quality Control In Water and Wastewater
Laboratories. EPA 600/4-79-019) page 6-10. 6-11.)
The "blind" duplicate and "spiked" samples, after initial
field preparation, will be handled in the same manner as
all other samples of the same parameter. Identification
will be fictitious, but consistent with the identification
of actual study samples. Records of the QA check samples
and results of analyses are to be maintained by the Project
Officer. A summary of the results and any problems will be
brought to the attention of the Chief, Chemistry Section.
3. Preservation
Since few analyses will take place at the sampling site, except
on-site bloassay, samples may have to be preserved and returned
to the laboratory (mobile or Denver laboratory) for analyses.
The proper preservative, appropriate container and holding times
are given 1n Table II (Exhibit 3), as taken from Federal
Register, October 26, 1984, Volume 49, No. 209, pp. 28 and 29.
This table was published for use in the Clean Water Act; however,
its contents can be used with the Safe Drinking Water Act also.
Preservation of samples for other acts (CERCLA, RCRA, FIFRA,
TSCA) will generally be refrigeration or not preserved at all.
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Standard Operating Procedures
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When grab sampling, preservation must be performed immediately.
When composite sampling, sample preservative must be available
at the time the initial portion of sample is obtained and
available for all subsequent proportional parts. No
preservatives are to be used on hazardous waste samples.
When working with preservatives in the field, be careful not to
contaminate other samples with preservatives intended for a
specific sample.
Note: Nitric acid in any concentration may not be transported
on common carriers. Therefore, the sampler may have to obtain
nitric acid in the field or make arrangements with the
analytical laboratory to preserve the sample when received.
When fish are collected for toxic analysis, the following
information and handling requirements are to be used:
a. The following information should be provided for each fish:
(1) Genus, species and common name
(2) Station location
(3) Fork length (mm)
(4) Weight (gms)
(5) Date collected
(6) Condition
b. Fish selected should be older and/or larger fish that have
been exposed to water conditions for as long as possible.
(Do not include fish less than 150 mm unless they are pan
fish which may be a minimum of 100 mm). If fish are larger
than one and one-half Ibs. (675 g), three of each species
will be sufficient. If less than one and one-half Ibs.,
four to six fish are required of each specie, depending on
their size. Include a sports fish or predator and a bottom
feeder.
c. Wash fish off in water from the stream, lake, etc., where
caught before packaging. Do not include mud or debris with
the fish.
d. Each fish must be wrapped in clean aluminum foil and tagged
separately. Place the tag on the outside of each
foil-wrapped fish. (NOTE: Do not allow fish to come in
contact with plastic bags, ice chest interior, or
styrofoam.)
e. Place all Individually wrapped and tagged fish from one
station in one large bag (when possible).
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Standard Operating Procedures
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f. Freeze specimens as soon as possible. Otherwise, place on
ice immediately and freeze as soon as practical. Before
shipping, freeze fish solid and pack with dry ice or block
ice. (Ice cubes are not cold enough to hold the samples
during shipment.)
When benthlc organisms are collected for analysis, collection
and preservation will be along the guidelines established in
"Biological Field and Laboratory Methods for Measuring the
Quality of Surface Waters and Effluents" (EPA-670/4-73-001).
B. Sample Identification
A sample* Is physical evidence collected from a facility or from the
environment. An essential part of all enforcement investigations is
that evidence gathered be controlled. To accomplish this, the
following sample identification and Chain-of-Custody procedures have
been established.
The method of identification of a sample depends on the type of
measurement or analyses performed. When in-situ measurements are
made, the data are recorded directly in logbooks or Field Sample
Records (FSRs), with Identifying Information (project code, station
numbers, station location, date, time, samplers, field observations
and remarks). Examples of in-situ measurements are pH, temperature,
conductivity, flow measurement, continuous air monitoring, and stack
gas analysis.
Samples, other than in-situ measurements, are identified by a sample
tag (Exhibit C and Exhibit D) or other appropriate identification
(hereinafter referred to as a sample tag).
These samples are removed from the sample location and transported to
a laboratory or other location for analysis. Before removal,
however, a sample is often separated into portions depending upon the
analyses to be performed. Each portion is preserved in accordance
with applicable procedures and the sample container is Identified by
a sample tag. Sample tags shall be completed for each sample, using
waterproof ink unless prohibited by weather conditions. For example,
a logbook notation would explain that a pencil was used to fill out
the sample tag because a ballpoint pen would not function in freezing
weather. The information recorded on the sample tag includes:
*For purposes of this manual, the term 'sample' includes remote sensing
Imagery.
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Standard Operating Procedures
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Project code
Station Number
Date
Time
Station Location
Samplers
Tag Number
Remarks
- A number assigned by ES Division.
- A number assigned by the Project Officer/Team
Leader and listed in the project plan or the
NPDES permit number if used for NPDES
inspections.
- A six-digit number indicating the year, month,
and day of collection.
- A four-digit number indicating the military
time of collection - for example: 0954
- The sampling station description as specified
in the project plan.
- Name of person(s) collecting the sample.
- A unique serial number is stamped on each tag
that identifies Region with consecutive
number, I.e., 8-1239.
- The samplers record pertinent observations.
The tag used for water samples (also soil, sediment and biotic
samples) contains an appropriate place for designating the sample as
a grab or a composite, and identifying the type of sample collected
for analyses and preservative if any. The tag used for air samples
requires the sampler to designate the sequence number and identify
the sample type. The sample tags are attached to or folded around
each sample.
After collection, separation, identification, and preservation, the
sample is maintained under Chaln-of-Custody procedures discussed
below. If the composite or grab sample is to be split, it is
allquoted into similar sample containers. Sample tags are completed
and attached to each split and marked " Split". The tag
identifies the split sample for the appropriate government agency,
facility, laboratory, or company. In a similar fashion, all tags on
blank samples will be marked "Blank." Duplicate and spike samples
will remain blind.
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Standard Operating Procedures
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C. Chain-of-Custody Procedures
Due to the evidentiary nature of samples collected during enforcement
investigations, possession must be traceable from the time the
samples are collected until they are introduced as evidence in legal
proceedings. To maintain and document sample possession,
chain-of-custody procedures are followed.
1. Sample Custody
A sample is under custody if:
a. It is in your possession, or
b. It is in your view, after being in your possession, or
c. It was in your possession and then you locked it up or
placed it in a sealed container to prevent tampering, or
d. It is in a designated secure area.
2. Field Custody Procedures
a. In collecting samples for evidence, collect only that
number which provides a good representation of the media
being sampled. To the extent possible, the quantity and
types of samples and sample locations are determined prior
to the actual field work. As few people as possible should
handle samples.
b. The team leader is personally responsible for the care and
custody of the samples collected until they are transferred
or dispatched properly.
c. The Project Officer/team leader determines whether proper
custody procedures were followed during the field work and
decides if additional samples are required.
3. Transfer of Custody and Shipment
a. Samples are accompanied by a Chain-of-Custody Record (see
Exhibit E). When transferring the possession of samples,
the individuals relinquishing and receiving will sign,
date, and note the time on the record. This record
documents sample custody transfer from the sampler, often
through another person, to the analyst in a mobile
laboratory, or at the laboratory.
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b. Samples will be packaged properly for shipment and
dispatched to the appropriate laboratory for analysis, with
a separate custody record accompanying each shipment (e.g.,
one for each field laboratory, one for samples driven to
laboratory). Shipping containers will be padlocked or
sealed for shipment to the laboratory. Seals are made of
paper and perforated so they will tear easily to Indicate
possible tampering. The seals have an adhesive back and
must be partially covered with tape so they are not
accidentally torn. (See Exhibit H). The method of
shipment, courier name(s) and other pertinent Information
are entered in the "Remarks" box.
c. Whenever samples are split with a source or government
agency, it is noted in the remarks section. The note
indicates with whom the samples are being split and signed
by both the sampler and recipient. If the split is refused
this will be noted and signed by both parties. The person
relinquishing the samples to the facility or agency should
request the signature of a representative of the
appropriate party, acknowledging receipt of the samples.
If a representative is unavailable or refuses to sign, this
is noted in the "Remarks" space. When appropriate, as in
the case where the representative is unavailable, the
custody record should contain a statement that the samples
were delivered to the designated location at the designated
time.
d. All shipments will be accompanied by the Chain-of-Custody
Record identifying its contents. The original record will
accompany the shipment, and a copy will be retained by the
Project Officer/team leader.
e. If sent by mail, the package will be registered with return
receipt requested. If sent by common carrier, a Government
Bill of Lading will be used. A1r freight shipments are
sent collect. Freight bills, Post Office receipts and
Bills of Lading will be retained as part of the permanent
documentation.
f. A record custodian or clerk should receive and date all
samples as they arrive and determine whether they should be
placed in a locked and secure area.
D. Field Forms
Appropriate field sheets must be completed at the time of sample
collection. These would include NPDES Compliance Inspection Report
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forms (EPA Form 3560-3, Exhibit F) and Region VIII Field Sample
Record forms (Exhibit G).
In addition to sample tags and field sheets, a bound field notebook
must be maintained by the project officer or team leader to provide a
daily record of significant events. All entries must be signed and
dated. Keep the notebook as a permanent record. In a legal
proceeding, notes, if referred to, are subject to cross-examination
and admissible as evidence.
IV. FLOW MEASUREMENTS
In the determination of loadings, effluent limitation quantities, and in
flow-proportional sampling, flow measurements of some type are needed. The
details of flow measurement will not be discussed here, as good discussions of
the methods and procedures involved appear in the following publications:
1. USDI, Bureau of Reclamation - Mater Measurement Manual
2. OWDC, USDI - Recommended Methods for Water Data Acquisition
3. ASTM - Annual Book of ASTM Standards, Water
4. Environmental Protection Agency Manual - Handbook for Sampling and
Sample Preservation of Water and Wastewater
Flow is generally not a direct measurement. Usually other things are
measured first, such as velocity, depth, width, and area. Permanently-
installed devices for flow measurement usually Integrate these separate
measurements and record the result as flow. These devices can be checked by
making the Individual measurements, calculating the flow and comparing the
result to that reported by the permanently-installed recorder. Flow
(velocity) measuring devices used by field personnel in performing flow
checking activities shall be calibrated according to manufacturer's
specifications prior to use in the field and checked periodically, as
necessary, to assure accurate performance. Calibration checks, comments on
instrument operation, and any recommendations regarding maintenance and/or
repair shall be entered into the log book provided for each field flow
measuring device. Other information to be entered Into the log book shall
include the date and time of calibration and indivldual(s) performing the
calibration. The instrument and log book will be examined upon returning from
the field and any necessary maintenance and/or repairs performed immediately
to assure instrument is In operating condition prior to the next use. All
maintenance and/or repairs shall be entered into the log book along with the
name of the individual(s) effecting the maintenance/repair.
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V. PERSONNEL TRAINING
The successful Implementation of the field sampling plan ultimately
depends on the competence of the monitoring personnel.
New employees at the professional and technician level are given formal
and on-the-job training by experienced staff professionals 1n all facets of
field investigations. This instruction includes, but 1s not limited, to:
1. Sample collection techniques.
2. Calibration, maintenance and use of field instruments.
3. Maintenance and use of other field equipment (boats and trailers,
mobile labs, biological collection gear, etc.).
4. First aid and CPR training.
5. Safety instruction (as required by EPA Orders 1440.2 - Health and
Safety Requirements for Employees Engaged in Field Activities, and
1440.3 - Respiratory Protection.
6. Data tabulation and use of calculators.
7. Report preparation and graphic displays.
This training is supplemented by specialty courses given at EPA National
Training Centers and local colleges and universities, where appropriate.
While on OJT status, new employees are accompanied on field investigations by
experienced professionals where classroom instruction is put to use under
actual field conditions. A periodic assessment of training need is done
annually. Recommendations are made for both technician and professional level
employees to receive refresher and advance level training at EPA National
Training Centers and local colleges and universities, where appropriate, and
as funding permits. Participation in professional society activities is
encouraged with an occasional opportunity to attend professional seminars, as
funds permit.
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EXHIBITS
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ENVIRONMENTAL PROTECTION AGENCY
REGION VIII. DENVER, COLORADO
LABORATORY SERVICES REQUEST
PROJECT NAME
PROJECT CODE
SAMPLES COLL BY.
DATE.
SAMPLES RECEIVED AT LABORATORY BY
DATE.
DATA REVIEWED BY.
1
1
\
1
1
TAG COLOR SYMBOL |
STATION CODE
SAMPLE COLL. TIME
STATION DESCRIPTION
AND REMARKS
CODE
PARAMETER
"
"OX
O> (D
^
O
m 3
X
3* 2
-i. a
o- «
n- (\
c
ri
ID
U
^.
U
^
O
o
Standard Operating Procedures
For Field Samplers
Kltflll In mg/| vnUli olh.rwli. indicaUd. pHin vnill. luibldily In JTU, ip.cflic condudanc* In^mhoi/cm. i>» p«i STOREf. * Gpo' I979-6IO-S70
-------
28 Federal Register / Vol. 49. No. 209 / Friday. October 26. 1984 / Rules and Regulations
prescribed in Table II. Any person may
apply for a variance from the prescribed
preservation techniques, container
materials, and maximum holding times
applicable to samples taken from a
specific discharge. Applications for
variances may be made by letters to the
Regional Administrator in the Region in
which the discharge will occur.
Sufficient data should be provided to
assure such variance does not adversely
affect the integrity of the sample. Such
data will be forwarded by the Regional
Administrator to the Director of the
Environmental Monitoring and Support
Laboratory in Cincinnati, Ohio for
technical review and recommendations
for action on the variance application.
Upon receipt of the recommendations
from the Director of the Environmental
Monitoring and Support Laboratory, the
Regional Administrator may grant a
variance applicable to the specific
discharge to the applicant. A decision to
approve or deny a variance will be
made within 90 days of receipt of the
application by the Regional
Administrator.
TABLE II.REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, AND HOLDING TIMES
Paramalar Na/nama
TaMa lA-Bactertal Taata:
1-4 Golform laeal and total -,-,--, ,,, ,,--, -
3 Faoal ftnptotfmc' , u . --,,,, ,- ,-,--,- -
Tabto IB Inoroanto TaapK
1 AdrJIly -n ... . . -. * ... . ........ . .
2 Alkalinity . _ ..........
4. Ammonia.
9, Btocnantica) oxygan damand ... -. -
11 Bromlda ..._- . ~. _. ... .-........
14 Btocnamlcal onyfltn damand, cartmnaeaom.. ,.,,.,., t,
IS GHamleal mr/flan fltmand .,..,. ,
1ft. Chloride ~ .... ... ....... ~«_ .
17 CMoitnt total reiMual ... ..... ..........
21 Color - . ._..._..... .....
23-24. CyanUe. total and amenable to cntorinaUon
25 Fhiorlde
27 Hardnoea «« . -.... - . -
28. Hydrogen Ion (pH) .__ «... _...._. ......... ._._....__.
31, 43. KJeldahl and organic ntiiooan.. .......... - ~
Metala:'
IB. Chromium VI __.. ___ _. _.
35 Mercury. ...,. i .., , ,, .,.,.., ,, ,..,, ,..,--, ,,, --.-
3. 8-8. 10. 12. 13. 19, 20. 22, 28, 28. 30. 32-34, 38. 37, 45. 47. 51. 52. 58-
80, 82. 83, 70-72. 74, 71 MelaJa. axoipt chromium VI and mercury.
38 Nftrata .- .. . .- . . ... ..
38. NltratfrrtMM. - -
JO Nnrttt ... ,.,, . ,-,-,.,- ,.,,. , ,.,,
41 OHandgnaaa ......... ,,.i ul ,,,........,.
*2. Qrjarto carbon.., , ..,,,,,.,,, ,..,-,-, . ,,.,........., , ,,
44. Cftnopnoaphate _...«._. ..... .....................................w.,.,..^.
48. Oxygen, OtaaoNad Proba
47, Wflnklar,. .,,,., ,-,-,_,.. .. ,--,--,. .-... . -.,,,,.1,,,1i
*8. POenOta -....,...... ,.,.. .,.. u , ,.,. .. !
48. Phoaphorua (alamanlaD .
53. RaaMue, total ..- . - . ...... . .... -
M Rtakjw Filterable . ,
58. Raaldue, NonNtarable (TSS) _.__....._ .
58. ReaMue. SattlaaWa ..
57. Realdue, volatHa - -. ._._..........._ .. _.
81. SWtaa.............. ...... _..._...._ ..... _._........_....._.._...
85. SuKata.... . . ....... ._ .. ... . _
94. Sulflda
87 Sulflta
88. Surfactant*............ . ~ ._...__. ._._...............
88. Tarnparatufa..... m...........».w.w.. .....«............_..............«
73. TurMtty mil..!.!."" j jrzir !Z.~iri"! ...!zirr~iir
Tibia 1C OnjarUe Taata.*
13. 18-20, 22. 24-28. 34-37. 38-43, 45-47, 58. 88, 88. 88, 82-85. 87.
4, 97, M. PurgtaMa aramaM nydrmartiona. .,., .......,..,..,,,,...,,,., ,,
23, 30, 44, 48. S3, 87, 70, 71. 83, 85, 88. Phanota "....... ....-....-............_._...._..
7 38. BatilMnaa" ... . -
14, 17. 48, 50-52. Phttialata a*tar*"« -... _....._.-..... ....__.
72-74. Nltro»amln«ilv "...., ................_.........__. ..._..._ ......_....
78-82. PCBa" aefytonrtrOa ....... .._._......_........ _.._. ...._... .
54, 55. 85. 89. Nltrotromitxa and iaophoiana11
1. 2. 6, 8-12. 32. 33, 58. 58, 84. 88. 84, 81 Porynudaar aramaUc
hydrocarbon*".
15, 18, 21, 31, 75. Haloattwn" ~. .
28. 35-37, 80-83. 91. Chlorlflatad hydrocarbona ' '
87. TCOO"
Ttbla I0-Paa«eldta TattK
t-70. Paatddaa " .. . ... .-
Ttbla IE Radlotogloal Ttttu
1-5. Alpha, bata and radkirn _
Contalnar1
p, Q _. .
p. Q_
P, Q ... .
P Q .. . .
p, ° - -- ,
p, a_. _ . _
p. a.
p, q,...,, ,.,, .....
p, Q
P Q
P Q
P, Q.. _ .... .
P, Q
p Q, .
p, Q
p, Q _
P. Q
P, Q_
p, Q
P, Q.
p. a ..
p, a
Q __
P. Q
p, Q.
QBalttaandtop-
Oonly
Q
. (3. ._._.-.._.____.,...__...
', Q". .~ZZT~ "I
Q
, a
,Q _
, a
a "" "~~~ ~~
Q
,a. ...
, Q_
.0... ....._.._.....__.. _....
. 'oZZHZZI !!!!!_!".
Q
Q, TaMon-tnad aaptmn..
49, ., .,
. .do
Q, TaHon4nad cap
do .
__.do.. _..._._
......do _
......do
do ...«..«.. «.
.do...I
......do.......... ............_............,
......do - . ..
do
do
p, Q
Praaarvatton '
Cool. 4*C 0 008% Ma»Si(% '
do
COOL 4*c.
... .da
Cool, 4'C, H,SO. to pH<2
CooL4*C.. .
Nona raqulrad.-
Cod. 4'C
CooL 4'C, HHSO. to pH<2
do
CoOi 4"C
Coot, 4'C NaOH to pH> 12. 0.8g tscortnc add
HNO> to pH<2. HiSO, lo pH<2
Nona raqurad ..
CocH. 4'C, HiSO> to pM<2
Cod. 4'C .
HNCs to pH<2
do
CooL 4'C. __
Cool. 4'C H.SO. to pH<2
Cool 4'C _
CooL 4*C HtSO. to pH<2
CooL 4'C HO or HtSO, to pH<2
Filtar irnmadtataly CooL 4'C
Nona raoufcad........ - «... ^......^^....M^^.^.
R» on ttta and nora In dark _.. . . .....
CooL 4*C HsSO* to pH<2
CooL 4"C
COOL 4'c Htsb, to pH"8.
Nona raqurad
CooL 4'C
Nona raQuvao........ .....»«... .lu...
Cool, 4'C
Cool, 4'C 0.008% NaiSiOi.1
Cool, 4*C 0008% NaiSiOi* HC1 to pH2*
CooL 4'C 0.008% NaiSiOi1' Adkttt pH to 4-5 to
COOL 4'c o.66e% Natsiol1 ..-...'...~r....._"!.....!!!3
do
CooL 4'C
Cod 4'C More in dark. 0.008% Na.S.0,'.
CooL 4*C ~
CooL 4'C aboeWNaAft 'a^'ln"o*ii.".'33Zl~
. do .
Cool. 4'C 0.008% NaiSiOi1 ~
COOL 4*c
CooL 4*C 0.008S NatStOt*
Cool, 4'C pH 5-9 ».
HNOi to pH<2
Maximum holding Uma<
8 hom.
Do.
14 daya.
Oo.
28 daya.
48 houra.
48 houra.
28 daya.
Oo.
Udiyc.4
29 dcyt.
Analyze lmm*KJi*ttty
28 days.
48 hour*.
29 day*.
Analyxa unmadiataly.
8 hours.
28 day*.
?day$.
28 days.
Oo.
48 hours.
Anaryz*.
14 daya.
7 days untM trtracdon,
40days«Ttsr
H If action.
7 daya unM amracDon:
40dayaan*r
axiracUon.
Oo.
Oo.
Oo.
Oo.
Do.
DA.
rvv
Tabla II Notaa
' Polyathylana (P) or GUM (Q).
Standard Operating Procedures
For Field Samplers
Revision No. 2 Date: 3/15/86
Page: Exhibit B-1
PVTITPTT P 1
-------
Federal Register / Vol. 49, No. 209 / Friday. October 26. 1984 / Rules and Regulations 29
Sample preservation should be performed immedwlely upon umple collection Fa composite chemical temples each aliquot should be preserved e! the time ol collection When uee ol
an tulomiled sampler makei it impossible to pretense each aliquot, then chemical camples may Be preserved by maintaining at 4'C until compovung ana umple (putting » completed
'Wnen any sample it to be ahippad by common earner or cent through the limed Stales Mail*, it mutt comply with me Department of Transportation Hazardous Materials Regulations (46
CFR Pan 172j The person ottering much material lor transportation is responsible for ensunng auch compliance. For the preservation requirements ot Table II, the Office of Hazardous
Materials. Materials Transportation Bureau. Department ol Transportation has determined mat the Hazardous Materials Regulations da not apply to tne following materials Hydrochloric text
(HO) in water solutions at concentrations of 0.04% by weight or less (pH about 1 96 or greater): Nitnc aod (HMO,) m water solutions at concentrations of 0 15% by weight or leas (pH about
1 62 or greater). Sultunc acid (H,SO.) m water solutions at concentrations of 0.35N try weight or less (pH about 1 15 v greater), and Sodium hydroxide (NaOH) m water solutions at
; .ncenlrat.on; of OCflOV b\ weight or lest fpH about 1230 or less)
'Samples should be analyzed as soon as possible after collection The times rated are the maximum times that samples may be held before analysis and mil be considered valid SanuMes
may be held for longer periods only if the permittee, or monrtonng laboratory has data on file to show thai tne specific types ol samples under stuoy are stable for the longer time, and has
received a vanance from the Regional Administrator under {136 3ie) Some samples may not be stable for tne maximum time period grver, m the table A permmee. or monitoring laboratory, is
obligated to hold the sample lor a shorter time rf knowledge enisis to snow that this is necessary to maintain sample stability See 5 136 3(e) tor details
Should only be used in the pretence o' residual chlonne
Maximum holding time is 24 hours when sulfide is present Optionally al1 samples may be tested with lead acetate paper before pH annulments m order to determine if surhde is present
II aultide is present, it can be removed by the addition of cadmium nitrate powder until a negative spot test a obtained The sample is tnteieC and then NaOH it added to pH 12
' Samples should be filtered immediately orvsne before adding preservative tor dissolved metals.
Guidance applies to samples to be analyzed by GC LC. or GC/MS for specific compounds
Sample receiving no pH adjustment must be analyzed within seven days of sampling.
"The pH adiustment is not required rl acroMin will not be measured Samples for aciolein receiving no pH adfuatment must be analyzed within 3 days of sampling
11 When the extractable analytes of concern fall within a tingle chemical category, the specified preservative and maximum holding times should be observed tor optimum safeguard o<
sample integrity. When the analytes of concern fall within two or more chemical categories, the sample may be presarveo by cooling to 4'C. reducing residua! chlorine with 0.008% sodium
thiosuDate. storing in the dark, and adjusting the pH to 6-8 samples preserved in this manner may be held for seven days before extraction and for forty days after extraction Exceptions to
this optional preservation and holding time procedure are noted m footnote S (re the requirement for ttuosurtate reduction of residual chlorine), and footnotes 12. 13 (re the analysis of
benzidine).
"It 1.2-drphenylhydrazine is HKejv to be present adjust the pH of the sample to 4.Or0.2 to prevent rearrangement to benzidine
" Extracts may be stored up to 7 days before analysis If storage is conducted under an inert (oxxSant-free) atmosphere
"For the analysis of diphenytnftrosamme. add 0.008% Na,S,O» and adiust pH to 7-10 wrth NaOH withm 24 hours of sampling
"The pH adiustment may be performed upon receipt at the laboratory and may be omitted rf the samples are extracted within 72 hours of collection. For tne analysa of aldm add 0 008%
NaAO,
8. Appendices A. B, and C are added to
Part 136 to read as follows:
APPENDIX A TO PART 136METHODS
FOR ORGANIC CHEMICAL ANALYSIS OF
MUNICIPAL AND INDUSTRIAL
WASTEWATER.
Method 601Purgeable Halocarbonc
1. Scope and Application
l.l This method covers the determination
of 29 purgeable halocarbons.
The following parameters may be
determined by this method:
Parameter
Bromodichloromethane
Bromoform
Carbon tatrachlonde .. .... .
Oioromocnioromethane
1 ,3-Dichlorobenzene
1.4-Dichlorobenzene
Dtchlorodrfluoromethane ... ..
1,1-DichloroBthane
1 .2-Dichloroethane _
l,1*Dich!oroetriane
trana- 1 .2-Duhloroethene
1 ,2-Dichloropropane ......................
ca-1,3-Dier)loropropane
trans- 1 .3-Dicnloropropane
Memytene chloride
1 .1 .2.2-Tetrachloroethana
Telrachforootnene _. .....
1.1,1-Triehloroelhan*
1 ,1 ,2-TricMoroethane
Tetrachioroethene
Terichtorofluorofnethane
Vinyl chloride _
STORET
No.
32101
32104
34413
32102
34301
34311
34576
32106
34418
32105
34536
34586
34571
34668
34496
34531
34501
34546
34541
34704
34699
34423
34516
34475
34606
34511
39180
34488
39715
CAS No.
75-27-4
75-25-2
74-83-9
56-23-5
108-90-7
75-00-3
100-75-8
67-46-3
74-87-3
124-48-1
95-50-1
541-73-1
106-46-7
75-71-8
75-34-3
107-06-2
75-35-4
156-60-5
78-87-5
10061-01-5
10061-02-6
75-09-2
79-34-5
127-18-4
71-55-6
79-00-5
79-01-6
75-69-4
75-01-4
1.2 This is a purge and trap gas
chromatographic (GC) method applicable to
the determination of the compounds listed
above in municipal and industrial discharges
as provided under 40 CFR 136.1. When this
method is used to analyze unfamiliar samples
for any or all of the compounds above.
compound identifications should be
supported by at least one additional
qualitative technique. This method describes
analytical conditions for a second gas
chromatographic column that can be used to
confirm measurements made with the
primary column. Method 624 provides gas
chromatograph/mass spectrometer (GC/MS]
conditions appropriate for the qualitative and
quantitative confirmation of results for most
of the parameters listed above.
1.3 The method detection limit (MDL.
defined in Section 12.1] ' for each parameter
is listed in Table 1. The MDL for a specific
wastewater may differ from those listed,
depending upon the nature of interferences in
the sample matrix.
1.4 Any modification of this method.
beyond those expressly permitted, shall be
considered as a major modification subject to
application and approval of alternate test
procedures under 40 CFR 136.4 and 136.5.
1.5 This method is restricted to use by or
under the supervision of analysts
experienced in the operation of a purge and
trap system and a gas chromatograph and in
the interpretation of gas chromatograms.
Each analyst must demonstrate the ability to
generate acceptable results with this method
using the procedure described in Section 8.2.
2. Summary of Method
2.1 An inert gas is bubbled through a 5-
mJL water sample contained in a specially-
designed purging chamber at ambient
temperature. The halocarbons are efficiently
transferred from the aqueous phase to the
vapor phase. The vapor is swept through a
sorbent trap where the halocarbons are
trapped. After purging is completed, the trap
is heated and backflushed with the inert gas
to desorb the halocarbons onto a gas
chromatographic column. The gas
chromatograph is temperature programmed to
separate the halocarbons which are then
detected with a halide-specific detector.13
2.2 The method provides an optional gas
chromatographic column that may be helpful
in resolving the compounds of interest from
interferences that may occur.
3. Interferences
3.1 Impurities in the purge gas and
organic compounds outgassing from the
plumbing ahead of the trap account for the
majority of contamination problems. The
analytical system must be demonstrated to
be free from contamination under the
conditions of the analysis by running
laboratory reagent blanks as described in
Section 8.1.3. The use of non-Teflon plastic
tubing. non-Teflon thread sealants, or flow
controllers with rubber components in the
purge and trap system should be avoided.
3.2 Samples can be contaminated by
diffusion of volatile organics (particularly
fluorocarbons and methylene chloride]
through the septum seal into the sample
during shipment and storage. A field reagent
blank prepared from reagent water and
carried through the sampling and handling
protocol can serve as a check on such
contamination.
3.3 Contamination by carry-over can
occur whenever high level and low level
samples are sequentially analyzed. To reduce
carry-over, the purging device and sample
syringe must be rinsed with reagent water
between sample analyses. Whenever an
unusually concentrated sample is
encountered, it should be followed by an
analysis of reagent water to check for cross
contamination. For samples containing large
amounts of water-soluble materials.
suspended solids, high boiling compounds or
high organohalide levels, it may be necessary
to wash out the purging device with a
detergent solution, rinse it with distilled
. water, and then dry it in a 105'C oven
between analyses. The trap and other parts
of the system are also subject to
contamination: therefore, frequent bakeout
and purging of the entire system may be
required.
4. Safety
4.1 The toxicity or carcinogenicity of each
reagent used in this method has not been
precisely defined: however, each chemical
compound should be treated as a potential
health hazard. From this viewpoint, exposure
to these chemicals must be reduced to the
lowest possible level by whatever means
available. The laboratory is responsible for
maintaining a current awareness file of
OSHA regulations regarding the safe
handling of the chemicals specified in this
method. A reference file of material data
handling sheets should also be made
available to all personnel involved in the
chemical analysis. Additional references to
laboratory safety are available and have
been identified *« for the information of the
analyst.
Standard Operating Procedures
For Field Samplers
Revision No. 2 Date 3/15/86
Page: Exhibit B-2
-------
Standard Operating Procedures
For Field Samplers
Revision No. 2 Date: 3/15/86
Page: 'Exhibit C
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION 8
1860 Lincoln Street
Denver, Colorado 80203
R8EPA-014A
Project Code
d
I
C
C
C
r
D
Jg*
Dz
3
i
s?
a
a.
C3
i
ca
CD
,c>
to
3.
O
5T
ca
a
i
Phenollcs
a
e
ca
Designate:
Comp.
Is
11
_
09
ANALYS
m
CO
Grab
Preserve!
YesD N
o <
X 8
D
EXHIBIT C-
-------
X
CO
HI-VOL DATA RECORD
(Continued)
PARTICULATE DATA- For Lab Use Only
Filler-Gross Wgt..
Filler-Tare Wg»
Net Particulale Wgt..
Initial CFM
Final CFM _!
Air Volume
Particulale Concentration.
Total Sampling Time
hauft
minutes
grams
grams
grams
.rnj
./ig/m3
HI-VOL DATA RECORD
EPA, REGION VIII
BLDG. 53-E5
DENVER FEDERAL CENTER
DENVER, COLORADO 60225
STATION LOCATION
CITY & STATE
OPERATOR SITF NO.
SAMPLER IDENTIFICATION NO
FILTER NUMBER
START SAMPLING
mo day yr hi
STOP SAMPLING
mo day yr hi
WIND: calm, llaKl, gusty
VISIBILITY: clear, hazy
SKY: clear, , scattered, Overcast
HUMIDITY: dry, moderate, humid,
TEMPERATURE °F: <20, 20-40, , 4).f(
>80
REMARKS:
min CFM
into CFM
TJ7O ~n t/>
n» n> o «-f
- 3
O OTO
. ., a- 01 n>
), 61- -* r>\ 3 ~S
' Ol ri- ro^ o!
rt
o a> ->
0 -J 3.
Ql U) (O
rt-
n> -o
' d 3
H n>
w g-
> 5
* 5
-------
Environmental Services Division
CHAIN OF CUSTODY RECORD
PHOJ NO PROJECT NAME
SAMPLERS: (Signature)
iTAT. NO
DATE * TIME
O
CD
<
cc
(3
STATION LOCATION
NO.
OF
CON-
TAINERS
Denver. ColutacK
REMARKS
T)
(I)
i . M Tl
H- H-
Relinquished by: (Signature)
Relinquished by: (Signature)
Relinquished by: {Sijn
Date/Time
Dale/Time
Dale/ Time
Received by: (Signature)
Received t>y:(Snjnvtuie)
Relinquished by: (Signature)
Relinquished by: (Signature)
Received lor Labuialory by:
(Signature)
Dale/Time Remarks
tiuliut' Ofitjiiidl At.t.iiiii(janie^ ijtiipdionl. I-M^I Copy loC:u^Mlinali>i I n.*UJ l-iiuu. StiLfJiitl Copy K» Htjpru^t:iilT3
" 3
OJ O
Ul C
00 (D
o\ to
bphl Samples.
f.l Accaplad LI Dacllnad
Signjluie
8- 6184
-------
United States Environmental Protection Agency uL-citlUcil U UL>bl
A PQA Washington, D.C. 20460 For field San
^CrM NPDES Compliance Inspection F Revision NO.
Transaction Code NPD
1! I 44 3| I I ||
I I
ZT
Reserved Facility Evaluation Rating
67J | | | 69 70|_|
Section A: National Data System Coding rage. C,AIIJ.UJ
'ating rroceaures
iplers
2 Date: 3/15/86
Lt F
ES yr/mo/day Inspection Type Inspector Fac Type
I I 11 d I I I I I I 17 18J I id I 2CU
Remarks
1 I
711 I 7d I 7d I 1 74 7*! I I
Section B: Facility Data
Name and Location of Facility Inspected Entry Time I | ...I I ..
l_l AM L_J PM
Name(s) of On-Site Representatives)
Name, Address of Responsible Official
(S
Permit
Records/Reports
Facility Site Review
Section D:
Name(s) and Sighature(s) of Inspectors)
Signature of Reviewer
Action Taken
Exit Time/Date
Title(s)
Title
Phone No.
Section C: Areas Evaluated During Inspection
= Satisfactory, M = Marginal, U = Unsatisfactory, N = Not Evaluated)
Flow Measurement Pretreatment
Laboratory Compliance Schedules
Effluent/Receiving Waters Self-Monitoring Program
Summary of Findings/Comments (Attach additional sheets if necessary)
Agency/Office/Telephone
Agency/Office
Regulatory Office Use Only
Date
'
66
I 1 80
Permit Effective Date
Permit Expiration Date
Phone No(s)
Contacted
D Yes D No
Operations & Maintenance
Sludge Disposal
Other:
Date
Date
Compliance Status
ENoncompliance
Comoliance
EPA Form 3660-3 (Rev. 3-86) Previous editions are obsolete.
-------
FIELD SAMPLE RECORD
I. Company/Faci11ty
Samplers
Date
Standard Operating Procedures
For Field Samplers
Revision No. 2 Date: 3/15/86
Page: Exhibit G
Custody Record STORE! Station Designation
II.
Discharge
Description
& Pipe #
FIELD MEASUREMENTS
Sample Type
& Time
Flow (cont or
intermit.) in
GPM-Est. or Act.
Temperature of
Water Air
PH
Cl?
mg/1
ml
Samp'
III.
OTHER ANALYSES & REMARKS
Analyze for
Bottle No.
Treatment Code(s) &
Preservative Added
Remarks
Custody Tag 1
UU - Unfiltered Unpreserved
FU - Filtered Unp re served^
TREATMENTCODT
UP - Unfiltered & Preserved
FP - Filtered & Preserved
C - Chilled
IV. OTHER OBSERVATIONS (Circle as appropriate)
Type Discharge: pipe, culvert, ditch, weir, and/or
Appearance of
Discharge: clean, colored, oil, floating debris, algae, bubbles, and/or_
Odor of
Discharge: none, acrid, HgS, rotten, (strong) (slight), and/or
Appearance
of Bed: clean, algae, mucKy, debris, ooze, and/or
Appearance
of Bank: clean, rubble, eroded, sludge, algae, and/or
Other Comments:
0965c
-------
Standard Operating Procedures
For Field Samplers
Revision No. 2 Date: 3/15/86
Page: Exhibit H
jf"***, UNITED STATES
2 £%k \ ENVIRONMENTAL PROTECTION AGENCY
|2527| OFFICIAL SAMPLE SEAL
SAMPLE NO.
DATE
SIGNATURE
PRINT NAME AND TITLE (Tnspoctor, Analyst or Technician)
z
w
K
O
a
w
n
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APPENDIX A
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THE QUALITY ASSURANCE PROJECT PLAN
FOR THE
NPDES COMPLIANCE INSPECTION PROGRAM
FEBRUARY, 1986
U.S. Environmental Protection Agency
Region VIII
Environmental Services Division
Field Operations Branch
Water & Hazardous Waste Operations
Section
APPROVAL:
Joanna J. Hi 11 man Date
uality Assurance Officer
Max Dodson, Director Date
Water Management
James B. Lehr, Diractor Da'te
Environnental Services Division
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1.0 QUALITY ASSURANCE PLAN
DOCUMENT TITLE: NPDES Compliance Monitoring Program
DOCUMENT CONTROL NUMBER:
ORGANIZATION TITLE: US EPA, REGION 8, Environmental Services Division
ADDRESS: US EPA Region 8
Environmental Services Division
P.O. Box 25366
Denver Federal Center
Lakewood, Colorado 80225
RESPONSIBLE SUPERVISOR: Lester D. Sprenger
QA OFFICER: Juanita J. Hi11 man
PROJECT OFFICER: Project by Project
Plan Coverage
This plan describes the Quality Assurance Project Plan for US EPA Region
VIII Compliance Monitoring Program.
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2.0 Table of Contents: Page
1.0 Title Page 2
2.0 Table of Contents 3
3.0 Introduction 4
4.0 Project Description 4
5.0 Project Organization 5
and Responsibility
6.0 QA Objectives for Measurement 7
Data in Terms of Precision,
Accuracy, Representativeness,
and Comparability
7.0 Sampling Procedures 7
8.0 Sample Custody 8
9.0 Calibration Procedures 9
and Frequency
10.0 Analytical Procedures 14
11.0 Data Reduction, Validation 14
and Reporting
12.0 Internal Quality Control 14
Checks
13.0 Performance and System 14
Audits
14.0 Preventative Maintenance 15
15.0 Specific Routine Procedures 15
used to Assess Data Precision,
Accuracy and Completeness
16.0 Corrective Action 15
17.0 Quality Assurance Reports 16
to Management
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3.0 Introduction:
EPA policy requires participation in a quality assurance (QA) program
by all field and laboratory personnel involved in monitoring and measurement,
activities supported by EPA contracts, grants, regulations, or other
formalized agreements.
This document describes the Quality Assurance Project Plan for the
US EPA. - Region 8 NPDES compliance monitoring program. This document
will address organizational responsibilities and objectives of compliance
inspections in Region 8.
EPA Region 8 is committed to producing a NPDES compliance inspection
program that is of a high quality level and is useful to all parties
involved, whether permittee, inspector, enforcement official or the general
public.
All personnel involved with the NPDES Compliance Inspection Program
shall be thoroughly familiar with the policies and objectives outlined in
this plan to assure proper interaction between the compliance, field,
laboratory and data management personnel.
4.0 Project Description;
The Federal Water Pollution Control Act, PL 92-500, invested the
Environmental Portection Agency (EPA) with the authority to control the
discharge of pollutants into waterways.
The resultant program, authorized under Section 402 of PL 92-500, has been
designated the National Pollutant Discharge Elimination System (NPDES) and
operated under Title 40, Part 122 of the Code of Federal Regulations,
requiring that all point source discharges to national waters be controlled by
legally binding permits. The EPA is using a variety of methods to determine
facility compliance with the conditions of issued NPDES discharge permits.
The primary inspection methods are compliance evaluation inspection (CEI),
compliance sampling inspection (CSI), performance audit inspection (PAI),
compliance biomonitoring inspection (CBI), toxic sampling inspection (XSI),
diagnostic inspections, and pretreatment inspections. The specific number of
each type of inspection (there are seven) to be performed during the Fiscal
Year (FY) will be determined based on the needs of the regional program and
through agreement between the Field Operations Branch, Environmental Services
Division and the Water Compliance Branch, Water Management Division.
The results of each inspection will be submitted via a written report
to the requesting section. The report will be utilized for determining the
status of compliance of the facility with the requirements of their MPDES
permit, Federal regulations and/or to support legal proceedings.
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Analytical data and technical reports produced by the seven types of
inspections are reviewed by the Environmental Services Division and Water
Management Division to determine facility compliance with discharge permits.
In the case of noncompliance, EPA staff may undertake one or more of the
following actions:
1. leave with or send to the facility a Deficiency Notice requesting
correction of the deficiencies and certification to EPA that
corrective actions have been taken,
2. notify the delegated State agency of the results of the inspection,
3. issue Notice of Violation, and/or
4. issue an Administrative Order or use data in referrals. Data and
reports generated by inspections are also used as evidence in
legal proceedings.
5.0 Project Organization and Responsibility:
The Compliance Branch, Water Management Division, will select the
specific facilities that are to be inspected for the fiscal year. On a
monthly basis, the Compliance Assurance Section (CAS) of the Water Compliance
Branch will review the initial list for changes of inspection type, additions
and deletions, etc., except for Pretreatment Inspections. The pretreatment
inspection list will be reviewed by Permits Section, Water Compliance Branch;
CAS will select facilities for case development and will provide specific
guidance.
The Water and Hazardous Waste Operations Section (W&HWOS), Field
Operations Branch, Environmental Services Division (ESD) will perform and lead
for EPA, Region 8, all CEIs, CSIs, PAIs, joint inspections, pretreatment
inspections, field overview, and case development inspections. W&HWOS will
prepare a schedule of all inspections expected to be performed during each
month of the fiscal year, and will distribute them to the CAS, the Analytical
Support Branch of ESD, the Quality Assurance Office of ESD and the appropriate
state agencies at the beginning of the month.
The regional laboratory (Analytical Support Branch of ESD) will perform
all analyses of samples collected by the W&HWOS personnel during NPDES
sampling inspections. All analytical data will be transmitted to W&HWOS. The
data will be included in the inspection report.
The QA of the project is the responsibility of the Project Officer.
The overall organization of the Environmental Services and Water
Management Divisions, involved in the NPDES Compliance Inspections Program is
shown in Figure 1.
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Figure 1
Region VIII
Environmental Protection Agency
Denver, Colorado
OFFICE OF THE REGIONAL ADMffllSTRATOR
REGIONAL ADMINISTRATOR
DEPUTY REGIONAL ADMINISTRATOR
WATER MANAGEMENT DrvTSTOM
ENVIRONMENTAL SERVICES
DIVISION
Field
Operations
Branch
Water & Haz.
Waste
Operations
Section
Analytical
Support
Branch
Biological
Sciences
Section
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6.0 QA Objectives for Measurement Data in Terms of Precision, Accuracy,
Completeness, Representativeness and Comparability:
A Quality Assurance Plan for water enforcement compliance activities
ensures that information collected is of known quality, technically sound,
statistically accurate, and properly documented. These elements are
essential for enforcement proceedings that arise from compliance monitoring
activities. Specific quality control procedures related to activities such
as sampling, analysis, and engineering calculations will ensure that data
are appropriate for enforcement use. Without this total Quality Assurance
Plan, efforts performed to support the Water Management Division are of
limited use and sometimes invalid.
This QA Plan addresses the quality control procedures that will be
applied to every aspect of a compliance determination work assignment.
This includes:
1. on-site inspection documentation,
2. documentation of engineering data,
3. maintenance of chain-of-evidence files,
4. sample collection and field measurements, and
5. maintenance of chain-of-custody records. Also discussed are
specific objectives for measurement data in terms of precision,
accuracy, completeness, representativeness, and comparability.
7.0 Sampling Procedures:
Wastewater sampling is an integral part of the MPDES Compliance
Inspection Program. NPDES permits contain specific and legally enforceable
effluent limitations and self-monitoring requirements for effluent
sampling/analysis and flow measurement. The sample type, the parameters
to be monitored, the parameter limitations, and the analytical methods used
in compliance inspections will generally be^determined with reference to
the permit conditions established by EPA or the authorized State regulatory
agency.
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7.1 Techniques Used to Select Sampling Sites;
Usually, the permit objectives define either the approximate or precise
locations for sampling. The selected sampling locations must be
representative. The term "representative point" is defined in 40 CFR, Part
35, Appendix A, P. 224, 1976, as:
1. "A locaton in surface waters or groundwaters at which specific
conditions or parameters may be measured in such a manner as to
characterize or approximate the quality or condition of the water
body; or
2. A location in process waters or wastewater where specific conditions
or parameters are measured that adequately reflect the actual
conditions of those waters or wastewaters."
A major consideration influencing the selection of the sampling
locations is the homogeneity of the water or wastewater. Turbulence and
good mixing enhance the homogeneity (uniform distribution of constituents)
whithin the body of water or wastewater. Other considerations for the
selection of sampling locations are: establishment of general characteristics
of a large body of water or wastewater, pronounced degradation of water
quality in specific areas, suitability for flow measurements, convenience,
and accessibility. Specific considerations relating to influent and effluent
sampling locations are described below.
Influent Samples. These should be taken at points of high turbulence
flow to ensure good mixing. In some instances, the most desirable location
may not be accessible. The preferred sampling points for raw wastewater are:
1. The upflow siphon following the comminutor (in absence of grit
chamber);
2. The upflow distribution box following pumping from the main plant
wet wel 1;
3. Aerated grit chamber;
4. Flume throat; and
5. Pump wet well (if turbulent).
Effluent Samples. These should be collected at the site specified in
the permit or, if no site is specified in the permit, at the most
representative site downstream from all entering waste streams prior to entry
into the receiving waters.
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7.2 Specific Sampling Procedures;
Samples are collected in accordance with the techniques and procedures
contained in:
"NPDES Compliance Inspection Manual," U.S. EPA, Office of Water
Enforcement and Permits, June 1984.
"Handbook for Sampling and Sample Preservation of Water and Wastewater,"
U.S. EPA, EPA-600/4-82-029, Cincinnati, Ohio, 1982.
"Standard Operating Procedures For Field Samplers, U.S. EPA, Region
VIII, Environmental Services Division, June 1982.
The type of sample (e.g., grab or composite) is specified in the permit.
7.3 Records:
Appropriate field sheets must be completed at the time of sample
collection. These would include NPDES Compliance Inspection Report forms,
Region VIII Field Sample Record forms, sample tags, Chain-of-Custody and
laboratory service.
In addition to sample tags and field sheets, a bound field notebook
must be maintained by the team leader to provide a daily record of significant
events. All entries must be signed and dated. Keep the notebook as a
permanent record. In a legal proceeding, notes, if referred to, are subject
to cross-examination and admissible as evidence.
8.0 Sample Custody:
EPA must be able to prove that any analytical data offered into evidence
accurately represent environmental conditions existing at the time of
sample collection. It must be clearly demonstrated that none of the involved
samples could have been tampered with during collection, transfer, storage, or
analysis. Therefore, an accurate chain-of-custody will be maintained to
trace the possession of each sample from the moment of its collection
through its introduction into evidence. Sample custody is in accordance
with the procedures contained in "Standard Operating Procedures For Field
Samplers." U.S. EPA, Region VIII, Environmental Services Division, June 1982.
9.0 Calibration Procedures and Frequency:
The following pages describe calibration procedures and frequencies
for the equipment most commonly used by the inspectors.
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Field Analysis Equipment
NOTE: For instruments not in routine use, the checks described below may
be done just prior to field use instead of the frequency shown.
Parameter
1. Dissolved
Oxygen
Membrane
electrode
General
Enter the make,
mode, serial
and/or ID number
for each meter
in a log book.
Winkler-
Azide
Method
Record data to
nearest 0.1 mg/1.
2.pH
Electrode
Method
Enter the make,
model, sen* al
and/or ID number
for each meter
in a log book.
1. Calibrate meter
using Winkler-Azide
method.
2. Check membrane for
air bubbles and holes.
Change membrane and
KCL if necessary.
3. Check leads, switch
contacts, etc. for cor-
rosion and shorts if
meter pointer remains
off scale.
Duplicate analysis
should be run to check
the precision of the
analyst and the method.
Duplicate values should
agree within +_ 0.2 mg/1.
1. Calibrate the system
against standard buffer
solutions of known pH
value at the start of
a sampling run.
2. Periodically check
the buffers during the
sample run and record
the data in the log
sheet or book.
3. Be on the alert for
erratic meter response
arising from weak
batteries, cracked
electrode, fouling, etc.
Quarterly
Check instrument cali-
bration and linearity
using a series of at
least three dissolved
oxygen standards.
Take all meters to the
laboratory for mainte-
nance, calibration and
quality control checks.
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Field Analysis Equipment
Parameter
General
Quarterly
3. Conductivity
Enter the make,
model, serial
and/or ID number
for each meter in
a log book.
4. Check response and
linearity following
highly acidic or alka-
line samples. Allow
additional time for
equilibration.
5. Check against the
closest reference
solution each time a
violation is found.
6. Rinse electrodes
thoroughly between
samples and after
calibration.
1. Standardize with KC1
standards having
similar specific con-
ductance values to
those anticipated in
the samples. Calculate
the cell constant using
two different standards.
Specific Cond. = Reading
multiplied by Cell
Constant.
2. Rinse cell after
each sample to prevent
carry-over.
1. Take all meters to
lab for maintenance,
calibration and
quality control
checks.
2. Check temperature
compensation.
3. Check date of last
platinizing and re-
platinize if necessary.
4. Analyze NBS or EPA
reference standard
and record actual
vs. observed readings
in the log.
5. See note on frequency
at beginning of Table.
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Field Analysis Equipment
Parameter
4. Residual
Chi on ne
DPD
General
Enter the make,
ID and/or serial
number In a log
book.
5. Temperature
Manual
Enter the make,
model , sen al
number and temp-
erature range for
each thermometer.
All stadardiz-
atlon shall be
against an MBS or
UBS calibrated
thermometer.
Readings should
agree within
Dally
Refer to kit Instruc-
tions for measurment
of Chlorine.
Check for air spaces
or bubbles in the
column, cracks, etc.
Compare with a known
source if available.
All data shall be
read to the
nearest 1°.
Report data
between QO-90C
to one significant
figure; between
1QO-990C
(500-21 OOF) to
two significant
figures.
Quarterly
Return kit to lab for
calibration against
amperometri c ti trati on
and/or EPA reference
samples before use
unless checked within
the last 3 months.
Check at two temper-
atures against an
MBS or equivalent-
thermometer. Enter
date in a log book.
Temperature readings
shall agree within
IOC or the thermom-
eter shall be replaced
or recalibrated.
Accuracy shall be
determined through-
out the expected
working range Q° to
500C (320 to 1200F).
A minimum of three
temperatures within
the range should be
used to verify
accuracy. Preferable
ranges are: 50-lQoc,
150-20QC,
350-4500.* (410-
500F, 590-770F,
950-1130F).
initially and Bi-annually.
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Samplers
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Parameter General Daily Quarterly
6. Automatic
Enter the make, Check intake velocity
model, serial vs. head (minimum of
and/or ID number three samples) and
of each sample clock time setting vs.
in the log book. actual time interval.
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10.0 Analytical Procedures:
All analytical procedures must be in compliance with Title 40, Part
136, of the Code of Federal Regulations, entitled "Guidelines Establishing
Test Procedures for the Analysis of Pollutants, Amendment of Regulations,"
Federal Register. Vol. 49, No. 209, Friday, October 26, 1984.
11.0 Data Analysis, Validation, and Reporting:
All field parameter results will be checked by the field project
officer at the end of each sampling day. Calibration records, known quality
control check sample results, etc., will be checked to ensure the validity
of the data.
Any suspicious data will result in reanalysis or resampling and
reanalysis where possible.
12.0 Internal QC Checks and Frequency;
Field-originated QA samples will be submitted to the laboratory on a
quarterly basis during the fieldwork season. When QA check samples are
submitted to the laboratory, they will consist of one or more "blind"
duplicate samples as appropriate to the study.
The "blind" duplicate samples, after initial field preparation, will be
handled in the same manner as all other samples of the same parameter.
Identification will be fictitious, but consistent with the identification of
actual study samples. Records of the QA check samples and results of analyses
are to be maintained by the Project Officer. A summary of the results and any
problems will be brought to the attention of the Chief, Analytical Support
Branch.
Field blanks for each set of case investigation samples should be
prepared in the laboratory, taken to the field, subjected to the same
conditions as the samples and returned to the laboratory for analyses.
These samples will be a check on contamination which may be introduced in
the field.
13.0 Performance and Systems Audit and Frequency:
The Region VIII EPA laboratory participates in both Water Supply and
Water Pollution performance evaluation studies on a yearly basis. These
programs ensure that the laboratory can analyze for water and wastewater
parameters.
Headquarters conducts a systems audit on the Region biannually. This
audit covers both the Water Division and uhe Environmental Services Division's
work in the NPDES area.
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14.0 Preventive Maintenance Procedures and Schedules:
All equipment (automatic samplers, thermometers, pH meters,
spectrophotometers) used in the field are maintained according to
manufacturer's recommendations.
Prior to any field sampling expedition, all equipment is checked to
ensure that it will work properly when needed.
Spare equipment is available and is taken to the field as space permits.
15.0 Routine Procedures Used to Assess Data Precision, Accuracy and
Completeness;
The EPA Regional laboratory will set up and analyze a minimum of ten
percent duplicates and matrix spikes per batch of samples collected.
The Quality Assurance type samples will be within acceptable limits;
if not, samples will be reanalyzed.
16.0 Correctie Action:
The determination of data acceptability will be the responsibility of
the Analytical Support Branch Chief and the Field Operations Branch Chief.
The Analytical Support Branch Chief will ensure that data meets the +2
standard deviation requirement and the Field Operations Branch Chief~will
ensure that samples were collected and preserved properly.
Any data which are rejected due to poor analytical or sampling technique
must result in corrective action.
Steps to be taken include:
1. reviewing all data available for transcription or math errors;
2. reviewing method with chemist/technician responsible for generating
the data;
3. finding ways to prevent problems in the future such as training,
cross-checking with two analysts, etc.;
4. training on proper sample collection/preservation; and
5. recollection and reanalysis if necessary.
All corrective action taken will be documented. If a report is sent
to the Compliance Assurance Section, Water Management Division with
questionable data, a summary of corrective action taken to prevent further
problems of the same type will be included with the report.
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17.0 Quality Assurance Reports to Management:
At the end of the inspection year, a summary of any problems encountered
during the sampling and analysis of NPDES samples will be sent to the
Regional Quality Assurance Officer.
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