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5.0
SAMPLE CUSTODY AND DOCUMENTATION
The following discussions outline the
minimum record keeping requirements as they relate to sample collection, sample
handling and sample analysis activities. The
protocols and requirements outlined in this section emphasize the use of
unequivocal, accurate and methodical records to document all activities
affecting
sample data.
Additional requirements may be imposed
by specific DER programs (e.g. Drinking Water) or other agencies (e.g. HRS, EPA,
etc.). If applicable, the
organization shall meet the DER QA requirements and the additional or more
stringent requirements of the other programs or agencies.
There are two levels of custody: 1) Sample custody or tracking and 2) Legal or evidentiary
chain of custody.
1. Sample custody or
tracking is required by DER. It
includes all records and documentation necessary to trace a sample from point of
origin through final report and sample disposal.
Sample custody requires that each event or procedure to which the sample
is subjected be documented. These
include, but are not limited to: sample
collection, field preservation, sample receipt and log in, sample preparation,
sample analysis and sample disposal. In
addition, those tasks or activities that relate to each of the above-mentioned
events (e.g. reagent preparation, calibration, preventative maintenance, quality
control measures, etc.) must be documented.
The history of the sample must be readily understood through the
documentation. The required
documentation that is associated with sample custody is outlined in Sections 5.1
through 5.5.
2. Legal or Evidentiary
Chain of Custody (COC) is a special type of sample custody which requires that
the physical possession, transport and storage of a sample be documented in
writing. The records must account
for all periods of time from sample container acquisition through sample
disposal. COC protocols are not
required by the Department, but are recommended.
If implemented, the minimum documentation requirements outlined in
Section 5.6 must be followed.
5.1
GENERAL REQUIREMENTS FOR CUSTODY AND DOCUMENTATION
5.1.1
Record Keeping System Design - General Requirements
Each organization shall design and
maintain a record keeping system that is succinct and efficient:
1. All records shall be
maintained in a manner which facilitates documentation tracking and allows
historical reconstruction of all analytical events and ancillary procedures that
produced the resultant sample analytical data.
2. The system shall
unequivocally link all documentation associated with a sampling event from
sample collection through the final analytical result and sample disposal. This may be accomplished through either direct or
cross-references to specific documentation.
3. The system shall be
straightforward and shall facilitate the retrieval of all working files and
archived records for inspection and verification purposes.
4. Final reports, data
summaries, or other condensed versions of data that have been prepared by
external parties shall be linked to internal records by an unequivocal
cross-referencing mechanism (usually field and/or laboratory ID numbers).
1. The history of a
sample must be clearly evident from the retained records and documentation. Copies or originals of all documentation which are associated
with the analysis or sample collection event must be kept.
This includes the documentation
that
is sent to or received from all sampling and analysis organizations.
2. All applicable
documentation specified in this section shall be available for inspection during
any sampling-site, facility (laboratory or offices) or data audit conducted by
authorized representatives of DER.
3. The records must
contain enough information so that excessive clarifications, interpretations or
explanations of the data are not required from the originator.
4. All documentation and
record entries shall clearly indicate the nature and intent of each entry.
a.
All documentation entries shall be signed or initialed by responsible
staff. The reason for the signature or initials shall be clearly indicated in
the records (e.g. sampled by; prepared by; reviewed by, etc.).
b.
Often, documentation requirements can be met by making brief references
to procedures written in internal SOPs or approved methodology promulgated by
external sources. If these standard procedures are routinely repeated in your
operations (e.g., sample preparation procedures, decontamination protocols,
analytical method, etc.), then citing these references may be appropriate.
Such citations must specifically identify the document, method or SOP
(e.g. sample preparation by 3010; field decon per internal SOP for teflon
sampling equipment, etc.), and must include the revision number or revision
date. Copies of all revisions must
be retained as part of the laboratory documentation.
5.1.3
Record-keeping Protocols
1. Entries into all
records shall be made with waterproof ink.
2. Entries in records
shall not be obliterated by erasures or markings.
All corrections to record-keeping errors shall be made by one line marked
through the error. The individual
making the correction shall sign (or initial) and date the correction.
5.2
PREPARATION OF FIELD SAMPLING SUPPLIES AND EQUIPMENT
All parties providing sample
containers, preservation reagents or sampling equipment shall maintain tracking
records.
A system of records or codes shall be
designed to link cleaning records, preservation or reagent preparation records
and trip blanks (if applicable) to the associated equipment, containers,
prepreserved containers, analyte-free water and preservatives which may be
shipped in sampling kits.
These records shall be maintained by
the party responsible for providing any or all of the above-mentioned equipment,
containers and/or reagents.
5.2.1
Content Requirements For Sampling Kit Documentation
The contents of each prepared sampling
kit (see Appendix A for definition) shall be documented.
A packing list or similar record shall be transmitted to the receiving
party with the sampling kit and a copy or other record shall be retained by the
preparing party.
5.2.1.1
The following information shall be transmitted to the receiving party:
a.
Quantity, description and material composition of all containers,
container closures or closure liners (if method specified) and all sampling
equipment;
b.
Intended application for each container type indicated by approved
analytical method or method group;
c.
Type and concentration of preservative added to clean sample containers
and/or shipped as additional preservative;
d.
Intended use of any additional preservatives or reagents;
e.
Description of any analyte-free water (i.e. deionized, organic-free,
etc.);
f.
Types and number of any quality control blanks (e.g., trip blanks);
g.
Date of kit preparation; and
h.
Description and material composition of all reagent transfer implements,
e.g., pipets, shipped in the kit.
This information may be in the form of
a packing slip (e.g., 6-125 ml plastic containers for metals, 12 VOC vials for
601/602, etc.).
5.2.1.2 In
addition to maintaining records of the above information, the preparing party
shall maintain records or cross reference links of the following information:
a.
Lot numbers of any commercially obtained sources of analyte-free water
(if provided);
b.
Material composition of all reagent and analyte-free water containers (if
provided);
c.
A code or reference (i.e., lot numbers) to dates in container and/or
equipment cleaning logs;
d.
A code or reference that links preservatives to preparation logs for
preservatives or vendor lots;
e.
Name of receiver of kit;
f.
Project name for kit use, if known;
g.
Name of individual(s) preparing the kit; and
h.
Date the kit was shipped or provided.
5.2.1.3 If
the sampling kits are prepared for internal use (i.e. they will not be shipped
to any external party, including branch offices of the same organization) and
the sampling kits are used for collecting routine (i.e. daily, weekly or monthly
monitoring) samples, the records in 5.2.1.1 and 5.2.1.2 may be reduced to the
following:
a.
The cleaning records for sampling equipment and/or sample containers (see
5.2.3 below) shall indicate who received the cleaned containers or equipment and
the date of receipt.
b.
The preservation and/or reagent preparation records shall indicate that
the preservative or reagent was prepared for use in the field.
5.2.2
Documentation for Preservatives
Sample preservatives and other reagent
preparations shall be traceable to preparation dates and vendor sources and/or
lot numbers.
Records shall be maintained for all
container or equipment cleaning. This
requirement shall apply to all containers and equipment cleaned or prepared for
use in field sampling activities. Field-meter
probes or other devices contacting the sample or sample source are also included
in this category:
1. The
material composition, size and any other description of all sample, preservative
or analyte-free water containers, container closures and closure liners or
sampling equipment cleaned or prepared;
2. A
detailed, step-by-step description of the cleaning protocols including cleaning
agents, water types or other reagents used in the procedure.
Reference to internal SOPs may be used (see 5.1.2.4.b);
3. Date
of cleaning;
4.
Individual(s) responsible for cleaning;
5. Storage
conditions (i.e. wrapped in foil, boxed, etc.) shall be described (internal SOPs
may be referenced);
6. Storage
location for cleaned containers and equipment;
7. Unique
ID numbers or codes assigned to individual containers or pieces of equipment;
8. The
number of cleaned containers or equipment if prepared or cleaned in groups or
lots (i.e., cleaned or prepared in the same session, using the same lots of
cleaning materials). A group or lot number may be assigned. This code must be linked to any individual IDs (if used), the
cleaning date (see 5.2.3.3 above) and any sampling kit IDs and records.
9. Any
quality control information concerning the cleanliness of the containers and/or
equipment must be retained and must be linked to the set (see 5.2.3.8).
10. The
intended end use of the equipment and/or containers shall be indicated (e.g.
Teflon bailers cleaned for organics; 30 plastic containers cleaned for metals,
etc.).
5.3
CUSTODY
AND DOCUMENTATION REQUIREMENTS FOR FIELD OPERATIONS
The following documentation requirements shall be followed for all
field-sampling operations.
1. Copies of all COC
forms (if applicable) or sample transmittal forms shall be maintained with
project records. If the sampling
and analysis activities are performed by the same organization at the same
physical location (e.g. wastewater
sampling
and analysis) and if all records are maintained in a central location, a single
copy of the COC form (if used) or the laboratory transmittal form may be
retained.
2. Entries into all
field records shall be made with waterproof ink.
3. Errors in all
documents shall be deleted with one line (see Section 5.1.3.2).
4. All
documentation/logs shall be signed/initialed by the appropriate personnel.
5. It is recommended
that all time be recorded using 24 hour notation (e.g., 2:00 PM is 1400 hours).
5.3.2
Sample Identification Requirements
1.
All sample containers must be labeled (tagged).
a.
At a minimum, the label or tag shall identify the sample with the field
ID number.
b.
Additional information (i.e. preservation, sampler's name, etc.) may be
included as a part of the tag or label.
c.
The label or tag shall be attached so that it does not contact any
portion of the sample that is removed or poured from the container.
2. The Field ID number
shall be a unique number or code that is assigned to EACH sample container. The assigned code must unequivocally link the collected
sample to the time or date of sampling, and may include information concerning
the location of the sampling point. Samples
that are routinely collected from the same location (e.g. monitoring wells,
outfalls, etc.) must be identified by more than the designated location code.
For example:
a.
MW-1V does not adequately identify a VOC sample collected at monitor well
1;
b.
MW-1-392V would identify the sample as being collected from monitor well
1 in March 1992 for VOCs.
3. At a minimum, the ID
numbers must be recorded on all sample tags (or labels), in the field records,
and on all transmittal records or COC forms.
4. Ancillary
records (photographs, videotapes, maps, etc.) must be easily traced to specific
sampling events and are subject to the same custody requirements as other
records discussed in this Section.
All activities related to sampling
events shall be documented in the field records.
At a minimum, the types of records that must be maintained include, but
are not limited to the following:
1.
Sample labels/tags (with identifying ID#s).
2.
Sample seals (if required)
3.
Sample transmittal forms (or COC forms).
4.
Field sheets, logs, notebooks or other records
5.3.4.1
Sample Transmittal Records
All samples that are submitted to a
laboratory must be accompanied by a sample transmittal or Chain of Custody
record (see Section 5.6). This
record may be designed as individual forms for each sample or a summary form for
a set of samples. AT A MINIMUM, the
information transmitted to the laboratory shall include:
a.
Site name and address (Client Code may be acceptable if samples are
considered sensitive information and if the field records clearly trace the code
to a specified site and address)
b.
Date and time (military time preferred) of sample collection
c.
Name of sampler responsible for sample transmittal
d.
Field ID#(s) (see 5.3.2 above)
e.
Number of samples
f.
Intended analyses - The analytical method number shall be listed if the
sample results are related to a QAPP or other document (e.g. DER Rule or permit)
which specifies the method to be used.
g.
Preservation (may be indicated on sample label/field sheets)
h.
Comments section (about sample or sample conditions)
I.
Appropriate place for identification of common carrier (if used)
5.3.4.2
Field Records
The following information must be
documented in the records maintained by the sampling organization.
This information may be recorded in bound notebooks or on field sheets
that have been designed for a specific purpose. All loose records (i.e. field sheets, photographs, etc.)
shall be unequivocally linked to the sampling event by code, facility name
and/or client name and address.
a.
General Information - the following information shall be recorded for all
sampling events:
1.
Names of all personnel and visitors on site during sampling
2.
Date and time (military time preferred) of sample collection
3.
Ambient field conditions, to include, but not limited to information such
as weather, tides, etc.
4.
Specific description of sample location including site name and address.
The specific sampling point must be further identified (Well ID #,
outfall number, lat/longs, station number, etc.).
5.
Field ID# (see 5.3.2 above) for each sample container and parameters to
be analyzed
6.
Field measurement data (e.g., pH, specific conductance, etc.)
a.
Records shall indicate when measurements were taken; and
b.
Calibration information to include:
time of all calibrations or calibration checks, concentration(s) of
standards and calibration acceptance (information may be kept in a separate
calibration log)
7.
Sample sequence - identify the order in which each sample is taken (time
of sample collection is acceptable).
NOTE: if
the collection time is used, the time that each sample aliquot is collected
(i.e. VOC, metals, nutrients, etc.) MUST BE NOTED.
8.
Preservative used -
information must include, but is not limited to:
a.
Preservative name;
b.
pH verification (if applicable)
c.
Amount/quantity of preservative that is added (if adding preservatives in
the field); and
d.
Amount/quantity of additional preservative that is added (if using sample
containers with premeasured preservatives)
9.
Purging and sampling equipment used (ID# if applicable)
10.
Field decontamination performed. All field-sampling equipment
decontamination, whether performed in the field, on site or in a headquarters
facility or laboratory, must be documented per 5.2.3 above.
11.
Types of QC samples collected. Include
when and where collected, preservative (if applicable) and type (e.g., trip
blank, equipment blank, duplicate, etc.). QC
samples must be documented in the same manner as all other samples.
12.
Use and location of fuel powered units (if applicable)
13.
Composite samples (if collected) shall indicate number of samples in the
composite and approximate amount/quantity of each subsample
14.
Signature of sampler(s).
b.
Additional documentation for monitoring wells shall include:
1.
Well casing composition and diameter of well casing
2.
Water table depth and well depth
3.
Calculations used to determine purge volume
4.
Total amount of water purged
5.
Date well was purged
6.
Beginning and ending purge times (military preferred)
7.
Measurement data to monitor stabilization, if applicable (see 5.3.4.2.a.6
above)
8.
Drilling/boring method (if known), including type/name of drilling mud
used (if known) - These may be by reference to associated well logs or well
installation records.
c.
Additional documentation for in-place plumbing and/or drinking water
sources shall include:
1.
Plumbing and tap material construction (if known)
2.
Flow rate at which well was purged
3.
Time well was allowed to purge
4.
Flow rate when sample collected
5.
Public water system ID # (if applicable)
6.
Name and address of water supply system as well as an emergency phone
number for notification of sample results (if applicable)
d.
Additional documentation for surface water shall include:
Depth samples were taken.
e.
Additional documentation for wastewater effluent shall include:
1.
Beginning and ending times (24 hr) for timed composite sampling
2.
Type of composite (e.g. flow proportioned, continuous, etc.)
f.
Additional documentation for sediments and soils shall include:
1.
Depth from the surface that samples were taken
2.
Drilling/boring method (if known), including type/name of drilling mud
used (if known). See 5.3.4.2.b.8 above.
g.
Additional documentation for drum sampling shall include:
1.
Type of drum, description of contents and markings
2.
If stratified, what layer(s) were sampled
1. All sample
transmittal forms shall be placed in waterproof bags and sealed in the transport
containers with the samples.
2. If
shipped by common carrier, transport containers should be securely sealed with
strapping tape or other means to prevent lids from accidentally opening.
COC Seals (if used) shall be applied after containers have been secured.
3. All
shipping bills from common carriers shall be kept with the COC or transmittal
forms.
5.4
SAMPLE
CUSTODY TRACKING AND DATA DOCUMENTATION FOR
LABORATORY OPERATIONS
5.4.1
Initial Check of Samples and Documentation
When
samples are received by the laboratory the following checks shall be made upon
receipt:
1.
Verify the integrity and condition of all sample containers.
a.
Check for leakage, cracked or broken closures or containers, evidence of
grossly contaminated container exteriors or shipping cooler interiors, and
obvious odors, etc.
b.
Check for air headspace or bubbles in VOC containers.
2.
Verify receipt of complete documentation for each container.
a.
The minimum information FOR EACH SAMPLE CONTAINER must include the items
listed in 5.3.4.1.
b.
Verify that sample identification numbers on sample transmittal forms
correspond to sample identification numbers on the sample containers.
5.4.2
Verification of Sample Preservation
1. Verify proper field
preservation of each sample by examination of documentation received from the
field-sampling party. There must be clear documentation of any chemical
preservation of the sample. This documentation must demonstrate proper
preservation per approved preservation protocols listed in 4.4.2.
2. For samples which
require thermal preservation (i.e. wet ice), verify proper storage temperature
by determining that sample containers are in adequate contact with wet ice in
the shipping chest. The following
alternate techniques may be used to verify the actual sample temperature:
a.
The temperature may be verified by determining the temperature of a
surrogate water sample which has been shipped with the samples or placed in the
transport containers with the samples after arrival in the laboratory.
In the latter case, the surrogate sample must be allowed to equilibrate
to the temperature of the samples in the cooler.
b.
The temperature of incoming samples may also be verified by a
non-invasive temperature probe.
c.
The temperature of the melted ice water in the cooler may also be used as
an indicator of proper temperature.
UNDER NO CONDITIONS SHALL A THERMOMETER
OR OTHER TEMPERATURE MEASURING DEVICE BE PLACED INTO THE COLLECTED SAMPLE
CONTAINER.
3. For acid- or
base-preserved samples, verify the pH of the samples at time of receipt in the
laboratory or upon preparation of subsamples and other aliquots for analysis
(see 5.4.8.3 below).
5.4.3
Rejection of Received Samples
1.
Rejection Criteria - Samples shall be rejected according to the following
criteria.
a.
The integrity of sample containers is compromised as described in 5.4.1
b.
The identification of a container cannot be verified
c.
The proper preservation of the container cannot be established
d.
VOC vials contain bubbles of sizes greater than 1% of the vial volume
(usually a bubble size of 5 mm in diameter).
Note: the presence of any
bubbles in VOC vials must be documented and reported with the final results.
2. The laboratory shall
obtain concurrence or further instruction from the sample submitter regarding
any proposed rejection. All
correspondence and/or conversations concerning the final disposition of the
samples shall be documented.
3. Any decision to
proceed with the analysis of compromised samples shall be fully documented.
a.
The condition of these samples shall be noted in all documentation
associated with the sample.
b.
The analysis data shall be appropriately qualified as estimated on all
internal documentation and on the final report (see Data Qualifiers, Table
10.2).
4. Rejected
samples shall be logged in the laboratory sequential log per Section 5.4.4 below
with appropriate comments.
1. The laboratory shall
employ a logical system for assigning a unique identification code to EACH
SAMPLE CONTAINER received in the laboratory.
Multiple aliquots of a sample that have been received for different
analytical tests (e.g., nutrients, metals, VOCs, etc.) shall be assigned a
different ID code.
a.
This laboratory code shall maintain an unequivocal link with the unique
field ID assigned each container.
b.
The identification of containers by container shape or size is not
adequate.
c.
Sample containers will be labeled with the unique code upon assignment of
the code.
2. A chronological log
shall be employed to document receipt of all sample containers.
The following information will be recorded in the laboratory sequential
log:
a.
date of laboratory receipt of sample
b.
sample collection date
c.
unique laboratory ID code
d.
field ID code supplied by sample submitter
e.
required analyses, including approved method number
f.
signature or initials of logger
g.
comments resulting from sample integrity inspection (Section 5.4.1) or
sample rejection (Section 5.4.3).
h.
sampling kit code (if applicable)
3. Smaller laboratories
whose function is to analyze on-site samples that have been collected by the
laboratory staff (e.g. in-house domestic wastewater treatment laboratories) may
use the sample transmittal forms as the sample log provided:
a.
The information in 5.4.4.2 above is included on the forms; and
b.
The sheets are maintained in chronological order as a permanent
laboratory record.
In these cases, the laboratory ID number may be
the same as the field ID number, subject to the requirements listed in Sections
5.4.4.1 and 5.4.4.2 above.
4. Retain all
documentation that is transmitted to the laboratory by the sample transmitter.
1. Parent samples,
sample replicates and subsamples received in the laboratory shall be stored
under approved conditions as described in Tables 4.2, 4.3, 4.4 and 4.5.
2. Sample fractions,
extracts, eluates, leachates, digestates, etc. shall be stored according to
requirements of 5.4.5.1 above or according to guidance found in the approved
preparation or analytical method used to prepare or analyze the subsample, as
applicable. In cases of conflicting
guidance, the storage/preservation requirements specified in 5.4.5.1 above shall
supersede method guidance. No
specific requirements apply to other cases not comprised by the above.
3. Samples
and all subsamples, sample fractions, extracts, eluates, leachates and
digestates shall be stored separately from all standards, reagents, cleaning
supplies, fuels, food, etc.
4. VOC samples shall be
stored separately from all other samples.
5. The manner in which
samples and subsamples are stored shall be documented.
This may be recorded in the sample receipt log (5.4.4) or other linked
documentation.
At a minimum, record the date of sample
and/or subsample disposal and either the name (or initials) of the individual
authorizing the disposal or the person who is responsible for the disposal.
5.4.7
Intralaboratory Distribution of Samples for Analysis
1. The laboratory shall
utilize a proactive procedure to ensure that all samples and subsamples are
analyzed within allowed maximum holding times (specified in 5.4.5.1 above).
2. All distribution of
samples and subsamples for preparation and analysis shall be documented as to
task assignment and analysis date deadline.
5.4.8
Laboratory Preparation of Samples for Analysis
Record all sample preparation procedures that may impact the analytical
results.
5.4.8.1
Preparation Records
a.
Sample preparation records shall include, but are not limited to:
1.
digestions
2.
filtrations
3.
distillations
4.
extractions
5.
leachings
6.
sample extract cleanup procedures
b.
The specific sample processing protocol shall be identified.
Where the procedure is routinely performed according to approved
methodology or internal SOPs, preparation records may refer to the specific
method or SOP (see 5.1.2.4.b)
5.4.8.2
Required information
a.
All numerical parameters associated with the preparation technique shall
be recorded. These data shall include, but are not limited to:
1.
Sample or subsample ID number
2.
Duration times for processes (e.g., extraction cycles, digestions,
distillations, sonications, etc.) if the method specifies a time limitation
3.
Volumes or weights of subsamples, reagents or dilution water
4.
Dilution factors
5.
Meter and other instrument readings
6.
Chromatography column elution profile retention times
7.
Adsorption column efficiency or breakthrough determinations
8.
pH checks
b.
Where specific materials or supplies are explicitly required by the
approved method, record description and the material composition of such
equipment, labware or supplies. This
information may be by reference to internal standard operating procedures (see
5.1.2.4.b).
c.
Record all calculations associated with the preparation procedure.
d.
Retain all elution profile chromatograms, pH meter recorder charts or
other products of automatic instrument data recordings associated with the
procedure.
e.
Link all reagents that are used in the procedure to the applicable
reagent preparation records.
5.4.8.3
pH Checks of Samples and Subsamples
a.
Verify the pH of all pH-preserved samples before any sample preparation
or sample analysis procedure. Additional
pH checks and adjustments, where required by the approved method, shall be
documented.
b.
Record the results of pH checks on samples and subsamples.
c.
The proper pH value as stipulated by approved preservation protocols or
approved sample preparation methods shall follow the method prescribed
procedures. If none are specified,
the pH shall be determined as follows:
1.
Use narrow-range pH paper.
2.
Do not contaminate the sample or subsample by contact with pH paper or pH
electrode.
3.
Use non-contaminating transfer implements, if necessary, to obtain a
sample portion for use in the pH check procedure.
4.
Check pH of VOC samples after taking aliquot for analysis, or check pH on
duplicate sample that can be destroyed for this purpose
5.
Pour a portion of the sample on the pH paper, unless the sample is an
analytical portion that cannot suffer significant quantitative loss. In this
case, transfer a test specimen with disposable pipet or other implement to the
pH paper (see 5.4.8.3.c.3 above)
5.4.9
Tracking for Interlaboratory Transfer of Samples/Subsamples
If samples or sample
extracts/digestates are sent to another laboratory, the information transmitted
to the receiving laboratory must include, at a minimum:
1.
Field ID number (optional)
2.
Date and time of sample collection
3.
Intended analyses by approved method designation
4.
Method of preservation
5.
Comments about sample or sample container (if applicable)
6.
Date of sample preparation (if applicable)
7.
Laboratory ID number (if applicable)
5.4.10
Sample Analyses Documentation Requirements
All sample analyses shall be completely
documented by retaining all associated records.
These records shall include, but are not limited to the following:
5.4.10.1
Information concerning all sample data:
a.
all sample identifications
b.
dates of analyses
c.
instrumentation ID and instrumentation parameters affecting the
analytical run
d.
approved method numbers for the analyses performed
e.
all raw and reduced analytical data
f.
all calculations
g.
analyst's initials or signature
5.4.10.2
GC/MS analyses:
a.
Retain all electronically generated records (including the tune file and
calibration date) on a write-protected diskette or tape in an orderly, logical
manner; OR
b.
Retain the hard copy records of all data in the analytical run (blanks,
QC samples, standards, samples, etc.) which must include:
1.
A copy of the total ion chromatogram, normalized to the highest
non-solvent base peak;
2.
Complete quantitation report;
3.
Confirmation of all hits (mass spectra from the sample and library); and
4.
Mass spectra from all unidentified compounds that exceed 5% of the
highest base peak (excluding solvent fronts).
This includes retention time, tabulation of mass abundances, and mass
spectra of the 5 most probable library hits.
5.4.10.3
Assure that all analysis data is linked with records for ancillary data
and procedures (e.g. sample preparation).
5.4.11
Documentation Requirements for Other Laboratory Operations
The following activities, which are not
specifically discussed in this Section, shall be documented according to the
requirements found in the cited sections.
1.
Preparation of Reagents and Analyte-Free Water - Section 6.2
2.
Preparation of Analytical Calibration Standards - Section 7.2
3.
Analytical Calibrations and Standardizations - Section 7.5 and 7.8
4.
Preventative Maintenance - Section 8.0
5.
Quality Control - Section 9.4
6.
Corrective Actions - Section 11.6
5.5
ELECTRONIC
DATA DOCUMENTATION
These requirements apply to all
laboratory and field records which are generated or stored electronically.
5.5.1
Retention of Automatic Data Recording Products
1. All products or
outputs of automatic data recording devices, such as chart strip recorders,
integrators and computers, shall be retained either in electronic, magnetic or
paper form.
2. All such records
shall be properly identified as to purpose, analysis date, and field and/or lab
ID number. The information in
Section 5.4.10.1 shall be recorded for all laboratory and all applicable field
analyses.
5.5.2
Electronic Data Security
1. Controlled
or secured access to levels of data-editing capability are recommended.
Software should provide prompts to the user for double-checking entries
before executing deletions or changes to data.
User-interaction or data-alteration tracking software is recommended, if
available.
2. Raw
data that is electronically collected from instrumentation shall not be altered
in any fashion. Software that
allows an analyst to correct raw data (e.g. change baseline) is acceptable.
5.5.3
Electronic Data Storage and Documentation
1. Electronically
or magnetically stored data shall be easily retrievable for printing to paper.
2. All
electronic/magnetic data files shall be coded, indexed, cross-referenced, etc.,
to allow linkage to sample data, analytical events and other laboratory
procedural records. These file designations shall allow easy retrieval of the
record.
3. All
software algorithms employed to perform calculations required by the approved
methodology or procedures shall be verified for accuracy and conformance with
the methodology protocols, formulas, etc. This
verification shall be documented.
a.
This requirement applies to all automatic calculations and automatic data
collection affecting calibrations, analyses, QC determinations, spread sheets,
etc.
b.
The vendor literature for software products may fulfill this requirement,
if sufficiently detailed.
4. All
software problems and their resolution shall be documented in detail, where
these problems affect the correctness of laboratory data documented per this
Custody SOP or where problems affect the cross-indexing of records.
Record the calendar date, time, responsible personnel and relevant
technical details of all affected data and software files.
Indicate which files have been affected. All software changes, updates, installations, etc. shall be
similarly documented per the above concerns.
File and link all associated service records supplied by vendors or other
service personnel.
5.6
LEGAL OR EVIDENTIARY CUSTODY PROCEDURES
The use of Legal Chain-of-Custody (COC) protocols are not required by
DER. The following procedures are
designed to document and track all time periods and the PHYSICAL POSSESSION
AND/OR STORAGE of sample containers and samples from point of origin through the
final analytical result and sample disposal.
This type of documentation is useful in
establishing the evidentiary integrity of samples and/or sample containers.
It can be used to demonstrate that the samples and/or sample containers
were handled and transferred in such a manner to eliminate possible tampering.
As such, these protocols are advantageous if data is to be used in legal
cases such as law suits, criminal actions, enforcement actions, etc.
In addition to the records listed in
Sections 5.1 through 5.5, the following protocols shall be incorporated IF legal
COC is implemented by the organization:
1. The Chain of Custody
records shall establish an intact, contiguous record of the physical possession,
storage and disposal of sample containers; collected samples; sample aliquots;
and sample extracts or digestates. For
ease of discussion, the above-mentioned items shall be referred to as
"samples":
a.
The COC records shall account for all time periods associated with the
samples.
b.
The COC records shall include signatures of all individuals who were
actively involved with physically handling the samples.
1.
The signature of any individual on any record that is designated as part
of the Chain of Custody is their assertion that they personally handled or
processed the samples identified on the record.
2.
Each signature shall be accompanied by a short statement which describes
the activity of the signatory (i.e. received by, relinquished by, etc.).
c.
In order to simplify record-keeping, the number of people who physically
handle the sample should be minimized.
d.
The COC records are not limited to a single form or document.
However, organizations should attempt to limit the number of documents
that would be required to establish COC.
1.
DER recommends grouping activities on documents (e.g., a sample
transmittal form to document field activities and laboratory receipt; a sample
storage and disposal form to document storage; etc.).
2.
A COC Form shall document all sample transmittals from one party to
another (see 5.6.3).
3.
The laboratory records such as initial sample log records, sample
preparation logs, analyst's run logs, etc. shall also be considered as part of
the chain of custody unless the organization has established other records or
protocols to document these laboratory functions.
2.
Legal chain of custody shall begin when the precleaned sample containers
are dispatched to the field.
a.
A COC form must be signed by the person relinquishing the prepared sample
kits or containers and by the individual who receives the sample kits or
containers.
b.
Thereafter, all parties handling the sample are responsible for sample
custody (i.e. relinquishing and receiving) and documentation EXCEPT when the
samples or sampling kits are relinquished to a common carrier.
3.
The common carrier should not sign COC forms.
a.
The COC form shall indicate the name of a common carrier, when used.
The shipping bill or other documents must be retained
b.
All other transferor and transferee signatures associated with common
carrier transfers are required. This
shall include laboratory, field and other personnel releasing or accepting
materials from the common carrier.
c.
COC will be relinquished by the party who seals the shipping container
and accepted by the party who opens it. The
COC form shall indicate the date and time that the transport container was
sealed for shipment.
d.
Transport containers shall be sealed with strapping tape and a tamper
proof custody seal. The custody seal must have space for the signature of the
person who affixed the seal along with the date and time.
4. The COC forms shall
remain with the samples during transport or shipment.
They must be put in a waterproof closure inside the sealed cooler or
shipping chest.
5.6.2
Required Contents for Custody Records
Tracking records shall include, by direct entry or linkage to other
records:
1. Time
of day and calendar date of each transfer or handling procedure
2.
Signatures of transferors and transferees
3.
Location of samples (if stored in the field or laboratory)
4.
Handling procedures (e.g. sample preparation, sample analysis, etc.)
performed on the samples
5. Storage
conditions for the samples, including chemical and thermal preservation
6. Unique
identification for all samples
7. History
of access to samples by all personnel, with personnel names recorded
8. Final
disposition of physical sample
9.
Common carrier documents
5.6.3
Required Information to be Included on COC Forms Used for Sample
Transmittal
A Chain-of-Custody record or form shall
accompany all evidentiary samples and subsamples that are transmitted and
received by any party. The COC
record or form shall specifically contain the following information:
1.
Sampling site name and address
2. Date
and time of sample collection
3. Unique
field ID code for each sample source and container
4. Name
of personnel collecting samples
5.
Signatures of all transferors and transferees
6. Time
of day and calendar date of all custody transfers
7. Clear
indication of number of sample containers
8.
Required analyses (by approved method number where applicable, see
5.3.4.1.f.)
9.
Common carrier usage, if applicable (see 5.6.1.3)
10. Sample
container/preservation kit documentation, if applicable (see 5.4 and 5.4.1.2),
including kit ID #
At a minimum, tamper-indicating tape or
seals shall be affixed to all shipping container closures when transferring or
shipping sample container kits, or samples to another party.
1. The
seal shall be placed so that the transport container cannot be opened without
breaking the seal.
2. The
time, calendar date and signatures of responsible personnel affixing and
breaking all seals shall be recorded on the seals.
3. Seals
shall be retained as a part of the COC documentation.
[[4. While
not required, organizations may elect to apply seals to individual containers.
This establishes the history of each individual sample.
The requirements specified for transport container seals shall be
followed.]]
5.6.5
Controlled Access to Samples
1. Access to all
evidentiary samples and subsamples shall be controlled and documented.
The number of individuals who physically handle the samples should be
limited to those responsible for sample collection, initial laboratory receipt,
sample preparation and sample analysis (see 5.6.1.1.c) and sample disposal.
2.
Samples and subsamples shall be placed in locked storage (e.g., locked
vehicle, locked storeroom etc.) at all times when not in the possession or view
of authorized personnel.
a.
Some organizations maintain restricted access to their facilities and
contend that storage under these conditions should constitute secure storage.
This practice is acceptable as long as non-laboratory personnel (i.e.
janitors, security guards, etc.) are not able to gain access to the samples
after business hours.
b.
Field personnel shall not leave samples in unoccupied motel or hotel
rooms.
5.6.6
Transfer of Samples to Another Party
Transfer of samples, subsamples,
digestates or extracts to another party are subject to all of the requirements
of Section 5.6.
1. Disposal
of the physical sample shall occur only with the concurrence of the affected
legal authority, sample data user and/or submitter of the sample.
2. All
conditions of disposal and all correspondence between all parties concerning the
final disposition of the physical sample shall be recorded and retained.
3. Records
shall indicate the date of disposal, the nature of disposal (i.e. sample
depleted, sample flushed into sewer, sample returned to client, etc.), and the
name of the individual who performed the task.
Note: if samples are transferred to another party, custody transfer
shall be documented in the same manner as other transfers (see 5.6.3 above).