of RTR1; PRO-1608-VECRTR-371, RTR Visual Examination Confirmation,
Building 3712; and 4-H80-776-ASRF-007, Visual Examination for
Confirmation of RTR.3  Together these documents identify the selection,
training, and qualification requirements for the VE personnel and the
VEE.  Visual examination personnel are requalified once every two years.
 The RFETS training program contains the following required elements:

B1-3b(4)	Formal Training

Project Requirements

State and Federal Regulations

Application Techniques

Site-Specific Instruction

B1-3b(5)	On-the-Job Training

Identification of Packaging Configurations

Identification of Waste Material Parameters

Weight and Volume Estimation

Identification of Prohibited Items

The TWCP Site PM designates the VEE based on qualifications, training,
and RFETS process and acceptable knowledge.  The VEE is responsible for
the overall direction and implementation of the VE examination.  VE
qualification through completion of a formal qualification document
incorporates both the formal and on-the-job training elements as listed
above (refer to the TWCP TIP, Appendix 1, TWCP Training Matrix).
Overall, the VE training and qualification program is used to assess
operator performance before actual waste characterization by VE.  With
the exception of items or conditions that could pose a hazard to VE
personnel, the audio/videotape results of the RTR evaluation of the
container shall not be available until after VE is completed.

For newly generated waste and when repackaging retrievably stored waste,
the formal and OJT training requirements for the visual verification
personnel are incorporated into a formal qualification process that is
specific for the waste generation and packaging activity.  The
qualification documents identify completed formal training on general
and site-specific training requirements for visual verification, and
also credits classroom training on the visual verification process in
activity-specific operating procedures (refer to the TWCP TIP, Appendix
1, TWCP Project Training Matrix, and Appendix 2, Residues Program).  The
qualification documents also provide documentation for OJT and
performance demonstration activities that meet the OJT requirements.

A description of the waste container contents is recorded on a Visual
Examination Drum Log.  The description clearly identifies the Waste
Matrix Code listed in the Waste Isolation Pilot Plant Transuranic Waste
Baseline Inventory Report (DOE 1995b) and DOE Waste Treatability Group
Guidance (DOE 1995a).  In cases where bags are not opened, a brief
written description of the contents of the bags must contain an estimate
of the amount of each constituent in the bags.  The written records of
VE, when using VE for confirmation of RTR or when using VE in lieu of
RTR, must be supplemented with the audio/videotape recording.

B1-4	Custody of Samples

Chain-of-Custody on field samples (including field QC samples) is
initiated immediately after sample collection or preparation (refer to
L-4006, Chain-of-Custody and Sample Administration for Headspace Gas
Sample Canisters; and PRO-543-ASD-002, Initiation, Preparation, and
Implementation of Chain-of-Custody Forms for solid samples).  Sample
custody is maintained by ensuring that samples are custody sealed during
transfer to the laboratory.  After samples are accepted by the
laboratory, custody is maintained by ensuring the samples are:

in the possession of an authorized individual; or

in that individual's view; or

in sealed or locked container controlled by that individual; or

in a secure controlled access location.

Sample custody is maintained until the sample is released by the TWCP
Site PM or until the sample is expended.

Custody of RFETS wastes samples collected and/or analyzed at INEEL is
described in the Attachment to the SOW for the INEEL TWCP (DOE 2003a).
Samples from RFETS waste are retained until INEEL is notitifed by the
RFETS TWCP Site PM, or the sample is expended.

Sampling personnel record all information pertinent to the collection of
samples on appropriate documentation.  This documentation includes
sample logbooks, data sheets, etc.  All information is legible and
contains only facts and observations (including modifications to planned
sampling activities). Records are dated and signed by the individual who
made the entry.  The key to producing legally admissible and defensible
data is effective COC procedures and the absolute requirement that no
movement of an analytical sample is permitted without custody control.

Section B1-4a, below, presents details on the documentation associated
with the collection of gas samples and the Gas Canister COC.  Prior to
October 22, 2002 headspace gas samples were collected using both SUMMA(
or equivalent canisters and on-line integrated sampling/analysis
systems.  Following this date, all headspace gas sampling and analysis
is conducted at RFETS utilizing on-line integrated systems.  Samples are
not transported to another location when using on-line integrated
sampling/analysis systems; therefore, the sample custody requirements of
this Section do not apply.  COC information relative to headspace
sampling with SUMMA( canisters is included for historical traceability.

Section B1-4b presents details on the documentation associated with the
collection of solid and soil/gravel samples and the associated COC.
Section B1-4c presents details on the field documentation that is
recorded at the time of sampling.

B1-4a	Gas Samples

Gas samples are collected in accordance with Section B1-1 of this
document.

Laboratory procedure L-4146, Headspace Gas Sampling of Waste Containers,
describes how sampling conditions and sample canister conditions are
documented.  L-4006, Chain-of-Custody and Sample Administration for
Headspace Gas Sample Canisters1, describes how COC for sample canisters
is maintained and documented.

B1-4a(1)	Sequence of Activities for Gas Canisters, COC form, and Other
Sample Documents

B1-4a(1)(i)	COC  -  Immediately after sample canister cleaning

Immediately after sample canister cleaning (i.e., prior to next sampling
event), the following activities occur:

A Headspace Sample Canister COC (refer to Figure B1-1) accompanies the
“certified clean” sample canister.

The Headspace Sample Canister COC includes provisions for each of the
following:

	Signature of individual initiating custody control, along with the date
and time.

	Documentation of sample numbers for each sample under custody.  The
sample number is referenced to a specific sampling event description
that identifies the sampler(s) through signature, the date and time of
sample collection, type/number of containers for each sample, sample
matrix, preservatives (if applicable), requested method of analysis,
place/address of sample collection and the waste container number.  The
Laboratory Sample Identification Number is a unique 7-digit number as
described in Section B1-4a(6)).

	Signatures of custodians relinquishing and receiving custody, along
with date and time of the transfer.

	Description of the final sample canister disposition, along with
signature of individual removing sample canister from custody.

	Comment section.

	Documentation of discrepancies, breakage, or tampering.

B1-4a(1)(i)	COC  -  Immediately after sample canister cleaning
(continued)

The Sample Canister Information Document (refer to Figure B1-2 for an
example) is initiated and accompanies the “certified clean” sample
canister.  The “certified clean” canister pressure is recorded, and
the final pressure is recorded for the manifold gauge and the canister
gauge.

The Sample Canister Information Document (SCID) includes provisions for
each of the following:

	Canister Identification Number (the Canister Identification Number is a
four-digit number as described in Section B1-4a(5).

	Sampler name and signature.

	Ambient temperature and pressure.

	Sample description.

	Requested analysis.

Date and time of collection.

A Sample Canister Tag (refer to Figure B1-3 for an example) with a
unique Laboratory Sample Identification Number is attached to the
“certified clean” sample canister.  The Sample Canister Tag is
removable.

The Sample Canister Tag contains the following information:

Each Sample Canister Tag has a unique seven-digit Laboratory Sample
Identification Number as described in Section B1-4a(6).  The Sample
Canister Tag Number and the Laboratory Sample Identification Number are
the same numbers.  The Laboratory Sample Identification Number is
located on one side of the tag.

Canister Identification Number (the Canister Identification Number is a
four-digit number as described in Section B1-4a(5).  The Canister
Identification Number, and the remaining information listed below, is
listed on the other side of the tag.

Sampler initials and organization.

Ambient temperature and pressure.

Sample description.

Requested analysis.

Date and time of collection.

QC designation (if applicable).

Name and signature of the individual applying the custody seal.

B1-4a(1)(ii)	COC  -  At the time of sampling

At the time of sampling, the following activities occur (laboratory
personnel collect the headspace gas samples; and therefore the headspace
gas samples are in the receipt of the laboratories at the time of sample
collection):

A custody seal is applied to the sample canister in accordance with
L-4006, Chain-of-Custody and Sample Administration for Headspace Gas
Sample Canisters.

A Headspace Sample Canister COC form is appropriately completed for each
sample. The Headspace Sample Canister COC form demonstrates sample
control from the time of sampling through sample disposal and also
documents sample integrity.

It is verified that a Sample Canister Tag (with Laboratory Sample
Identification Number) is attached to each sample canister (including QC
sample).

The following information is recorded in a bound sampling logbook:

	Sampling date

Sampling time

Container number

WIPP tag number

Canister number

Sample type

Volume removed

Batch number

RF number of pressure gauge, vacuum gauge, temperature sensor

PID span reading

	Comments (as necessary)

B1-4a(1)(iii)	COC  -  Immediately after sampling

Immediately after sampling, the following activities occur:

Sample canisters are externally smeared by Radiation Control Technicians
(RCTs);

In-line filters on sampling manifolds are utilized to survey the gross
alpha internal contents of the sample canisters; and

The COC and the Sample Canister Tag accompany the sample canister during
movement from the sampling area to the laboratory for analysis.

B1-4a(2)	COC Practices

Sample COC practices are carried out in accordance with the requirements
of the WIPP-WAP, and sample custody is maintained as described in
Section B1-4 (refer to L-4006, Chain-of-Custody and Sample
Administration for Headspace Gas Sample Canisters).

A Headspace Gas Sample Canister COC (refer to Figure B1-1 for an
example) is used to track the sample canister throughout the entire
process from cleaning through sampling, analysis, temporary storage, and
release to cleaning.  Whenever a transfer of custody takes place, the
receiving party (i.e., the party that is accepting sample custody)
inspects the COC, the SCID, the Sample Canister Tag, and all
accompanying documentation to ensure that the information is accurate
and complete.  The receiving party also inspects the samples for signs
of damage or tampering.  Any discrepancies in information or signs of
sample damage or tampering are documented by the receiving party in the
Comment Section of the COC.  When sample custody transfer takes place,
both the relinquishing and receiving parties sign and date the COC
document, and at that time the receiving party becomes the sample
custodian.

The Project Sample Coordinator ensures that all samples received by
sample receiving personnel are submitted with properly completed COCs.
The Analytical Laboratories management ensures that proper COC for each
sample is maintained at the laboratory, and that all laboratory
personnel responsible for COC are trained and understand their
responsibilities for COC (refer to L-4006, Chain-of-Custody and Sample
Administration for Headspace Gas Sample Canisters).

Completed samples are relinquished to sample receiving personnel for
temporary storage.  After sample analysis is complete, the original COC,
reduced and raw data, and other accompanying sample documentation are
submitted to records in accordance with L-4026, Records Handling,
Storage, and Retrieval for the WIPP Project File.  Project level support
personnel utilize this reduced and raw data for preliminary and final
report data packages.

After Batch Data Report verification and approval by the TWCP Site PQAO
and the TWCP Site PM are completed, corresponding sample canisters are
submitted to the canister cleaning laboratory.  Prior to canister
cleaning, Canister Sample Tags are removed from completed samples by the
Project Sample Coordinator for submittal to records in accordance with
L-4026, Records Handling, Storage, and Retrieval for the WIPP Project
File3.

B1-4a(3)	Headspace Sample Size, and Sample Canister Holding Temperatures
and Storage Conditions

The holding temperature of canisters containing samples is 0° to 40°C.
 All storage areas that have temperature requirements are monitored by a
calibrated temperature monitoring and recording device.

Minimum volumes for headspace gas samples are presented in Table B1-1.

B1-4a(4)	WIPP Sample Identification Number

Each sample is assigned a unique 14-digit WIPP Sample Identification
Number with the following format:

ZZ	MMDDYY	RX A ZZZ

(Sample Site ID)	(Date)	(Canister ID)

ZZ is the two-digit alpha character designating the sample site (RF for
Rocky Flats), and MMDDYY are the numeric characters indicating the
sampling data (month-day-year).  The characters “RX” designate the
analysis area within the laboratory performing sample analysis, and the
character “A” designates the canister volume.  The characters
“ZZZ” characters are the last three numerical digits of the canister
identification.

B1-4a(5)	Canister Identification Number

L-4006, Chain-of-Custody and Sample Administration for Headspace Gas
Sample Canisters1, documents canister identification requirements.  Each
canister is inscribed with the site identification “Rocky Flats Plant
Mass Spectrometry Lab” and a four-digit canister identification number
consisting of one alpha and three numeric characters, in the form LZZZ.
The alpha character represents the volume of the canister, as shown
below, and the three numeric numbers establish the serial number.

The Canister Identification Number is in the following format:

L	ZZZ

(Volume)	(Sequential Number:

	001 through 099)

A	=	100 ml

B	=	250 ml

C	=	500 ml

D	=	2.8 liter

E	=	6.0 liter

B1-4a(6)	Laboratory Sample Identification Number

Each sample is assigned a unique seven-digit Laboratory Sample
Identification Number with the following format:

YY	A	1XXX

(Year)	(Project Designation)	(Sequential

		Number)

YY is the two-digit numeric character designating the sample
identification number assignment year.  “A” is the alpha character
designating the project code (W for WIPP).  1XXX is numeric characters
that represent a unique sequential sample number.  The Sample Canister
Tag Number (i.e., the number on one side of the Sample Canister Tag) and
the Laboratory Sample Identification Number are the same number.

Section B1-4a(7), Field QC Record Form – Headspace Gas Sample, has
been deleted.

B1-4b	Homogeneous Solids and Soil/Gravel Sample Container

Samples of homogeneous solids and soil/gravel are collected by trained
personnel, who follow standard operating procedures.  All activities
related to the sampling and analysis events are recorded on documents
such as sampling request forms, sample labels, and COC forms.  The
Analytical Laboratories procedure L-4028, Sample Administration for the
Radiological Laboratories, describes the administrative tasks for
control of laboratory samples collected and analyzed at RFETS.

B1-4b(1)	Chain-of-Custody

Procedure PRO-543-ASD-002, Initiation and Preparation of
Chain-of-Custody Forms, provides information used to initiate
chain-of-custody for samples of homogeneous solids and soil/gravel.
Figure B1-4 provides an example of this COC form.

A signed and dated custody seal is affixed to each sample container and
installed across the container lid and body to provide visual evidence
of tampering.  An example custody seal is provided in Figure B1-5.
Tamper-indicating devices (TIDs) may be used on sample containers
instead of applying a signed and dated custody seal across the container
lid (i.e., TIDs and custody seals both provide visual indication of
sample custody).  The signature and date documenting sample custody is
recorded on the COC.  SOPs outline the flow of information between
parties responsible for sample acquisition, sample transfer, sample
analysis, data validation, data storage, data evaluation, and data use.

Participating laboratories have a documented sample custody program that
includes procedures for sample receiving and log-in, sample storage and
numbering, sample tracking in the laboratory, and storage of laboratory
data.  Refer to Section B1-2 and/or the project specific sampling and
analysis plans for detailed descriptions and procedures.

A COC accompanies each homogeneous solids and soil/gravel sample (refer
to Figure B1-4 for the COC).  The COCs used for RFETS sampling
activities are referenced in applicable project procedures and plans.
Sample custody is initiated at the time of sampling, and is maintained
until the sample is released by the TWCP Site PM or until the sample is
expended.

When sample custody transfer takes place, both the relinquishing and
receiving parties sign and date the COC document.  The party accepting
sample custody inspects the COC documents, sample tags, sample canister
information documents, and any other accompanying documentation to
ensure that the information is accurate and complete.  Discrepancies in
information or signs of damage “and tampering” to sample containers
shall be documented by the receiving custodian in the Comment section of
the COC document.  Original COC and sample information documents are
maintained in the RFETS project files after sample analysis is
completed.

B1-4b(2)	Handling

Handling requirements for samples of homogeneous solids and soil/gravel
conform to the requirements specified in Table B1-4 for sample quantity,
container, preservation, and holding time.  The sample quantities
provided are the suggested minimum amounts that must be collected for
each parameter per sample.  Additional sample quantities are collected
for QC samples.  The sample preservation requirement, “cool to 4°C”
means that the samples are placed in an insulated container and packed
with frozen chemical ice.  Sufficient ice is used to ensure the samples
remain cool until analyzed or stored in a refrigerated unit.
Temperature records of the sample are not required.

B1-4b(3)	Homogeneous Solids and Soil/Gravel Sample Containers

A twelve-digit sample identification number is assigned to each sample
of homogeneous solids and soil/gravel collected.  The sample
identification number has the following format:  12 alpha-numeric
characters; two alpha characters to designate the sampling site (RF),
and the remaining ten characters are unique to each homogeneous solids
and soil/gravel sample collection.  A sample label is affixed to each
individual sample of homogeneous solids and soil/gravel collected (refer
to Section B-4a(3) for a summarization of sample control).  The
following information is recorded in permanent ink on each COC:

Signature of individual initiating custody control, along with date and
time

Sample identification number.  Sample numbers are referenced to a
specific sampling event description that identify the sampler(s) through
signature, the date and time of sample collection, the type/number of
sample containers for each sample, the sample matrix, sample
preservatives (if applicable), requested methods of analysis,
place/address of sample collection, and the waste container number.

Signatures of custodians relinquishing and receiving custody, along with
the date and time of the transfer.

Description of sample disposition, along with the signature of the
individual removing the sample container from custody.

Comment section.

Documentation of discrepancies, breakage, or tampering.

Sample quantities and container volumes included in Table B1-4 are
suggested only, and are not required.  Sample quantities and containers
that meet analytical sample and QC requirements are stated in applicable
project procedures and plans.

All samples and reusable sampling equipment are identified with unique
identification numbers.  Sampling tools and equipment are identified
with unique equipment numbers to ensure all sampling equipment are
traceable to equipment cleaning batches.

Samples are uniquely identified to ensure the integrity of the sample.
The sample tag can be used to identify the generator site and the date
of collection.  Sample tags are affixed to all samples and identify at a
minimum:

Sample ID number

Sampler initials and organization

Sample description

Requested analyses

Date and time of collection

QC designation (if applicable)

B1-5	Sample Packing and Shipping

On-Site sample-transfer activities conducted at RFETS are performed in
accordance with PRO-908-ASD-004, On-Site Transfer and Off-Site Shipment
of Samples and/or MAN-T91-STSM-001, Site Transportation Safety Manual
(STSM).  Sample containers are packaged and shipped in accordance with
the requirements of PRO-908-ASD-004, On-Site Transfer and Off-Site
Shipment of Samples and the STSM to meet DOT regulations.  Sample
packages contain cushioning compatible to the package to prevent
shifting of and damage to sample containers during transport.  Off-site
shipping packages contain trip blank samples to detect any VOC cross
contamination.  Sufficient Blue Ice packs, or equivalent, are added to
the shipping container to maintain preservation temperature through
laboratory receipt.

Sample custody documentation, with the signature of the current
custodian showing sample custody release, shall be placed inside the
transfer container.  A seal shall then be placed on the outside of the
transfer container, or the transfer container shall be locked, so that
the integrity of the custody of the sample inside the transfer container
is evident.  Transfer of sample custody is complete when the receiving
custodian opens the transfer container and signs the sample custody
documentation.

RFETS waste analyzed at INEEL may or may not be sampled at INEEL.
Individual waste containers to be sampled are selected according to
Section B2-2.  Sample packaging and shipping is performed in accordance
with PRO-908-ASD-004, On-Site Transfer and Off-Site Shipment of Samples.
 Sample reciept at INEEL is conducted as described in the Attachment to
the SOW for the INEEL TWCP (DOE 2003a).

Table B1-1, Headspace Gas: SUMMA® Canisters, Canister Volumes and
Holding Temperatures

PARAMETER	HEADSPACE SAMPLE MINIMUM VOLUME (ML)

HOLDING TEMPERATURE

Hydrogen and Methane	100	0-40 o C

VOCs	250a,b	0-40 o C

a	Alternatively, if available headspace is limited, 100 mL samples may
be collected for determination of volatiles.

b	Alternatively, canisters, other than SUMMA® canisters, that meet QAOs
may be used.

Table B1-2, Headspace Gas: Summary of Field Quality Control Sample
Frequencies

QC SAMPLES	MANIFOLD	DIRECT CANISTER	ON-LINE SYSTEMS

Field Blanksa	1 per sampling batchd	1 per sampling batchd	1 per on-line
batchf

Sampling Equipment Blanksb

Or

On-Line Equipment Blanksb	1 per sampling batchd	Oncee	1 per on-line
batchf

Field Reference Standards

Or

Field Duplicates

Or

On-Line Duplicates	1 per sampling batchd	1 per sampling batchd	1 per
on-line batchf

a	Analysis of field blanks and equipment blanks for VOCs (Table B3-2),
only, is required.

b	One equipment blank or on-line equipment blank must be collected,
analyzed for VOCs (Table B3-2), and demonstrated  as clean prior to
first use of the headspace sampling equipment with each of the sampling
heads, then at the specified frequency, for VOCs, only thereafter.
Daily, prior to work, the sampling manifold, if in use, must be verified
as clean using an OVA.  Analysis of an on-line equipment blank is
required only if the field blank fails to meet the QAOs specified in
Table B1-3.

c	One field reference standard or on-line control sample must be
collected, analyzed, and demonstrated to meet the QAOs specified in
Table B3-2 prior to first use, then at the specified frequency
thereafter.

d	A sampling batch is a suite of samples collected consecutively using
the same sampling equipment within a specific time period.  A sampling
batch can be up to 20 samples (excluding field QC samples), all of which
must be collected within 14 days of the first sample in the batch.

e	One equipment blank and field reference standard must be collected
after equipment purchase, cleaning, and assembly.

f	An on-line batch is the number of samples collected within a 12-hour
period using the same on-line integrated sampling/analysis system.  The
analytical batch requirements are specified by the analytical method
being used in the on-line system.

Table B1-3, Headspace Gas: Summary of Field Quality Control Sample
Acceptance Criteria

QC SAMPLES	ACCEPTANCE CRITERIA	CORRECTIVE ACTION a

Field Blanks	VOC amounts ( 3 x MDLs in

Table B3-2 for GC/MS or GC/FID;

( PRQLs in Table B3-2 for FTIRS	Nonconformance if any VOC amount  > 3 x
MDLs in Table B3-2 for GC/MS or GC/FID; > PRQLs in Table B3-2 for FTIRS

Sampling Equipment Blanks	VOC amounts ( 3 x MDLs in

Table B3-2 for GC/MS or GC/FID;

( PRQLs in Table B3-2 for FTIRS	Nonconformance if any analyte amount > 3
x MDLs in Table B3-2 for GC/MS or GC/FID; > PRQLs in Table B3-2 for
FTIRS

Field Reference Standards

Or

On-Line Control Samples	70 - 130 %R	Nonconformance if %R <70 or > 130

Field Duplicates

Or

On-Line Duplicates	RPD < 25 %	Nonconformance if RPD > 25 %

a	Corrective action is only required if the final reported QC sample
results do not meet the acceptance criteria.

MDL	=	Method detection limit

%R	=	Percent recover

RPD	=	Relative percent difference

Table B1-4, Sample Handling Requirements for Homogeneous Solids and
Soil/Gravel

PARAMETER

SUGGESTED QUANTITYa

REQUIRED PRESERVATIVEb

SUGGESTED

CONTAINER

MAXIMUM HOLDING TIMEc

VOCs	15 grams	Cool to 4 o C	Glass Viald	14 Days Prep/

40 Days Analyzee

SVOCs	50 grams	Cool to 4 o C	Glass Jarf	14 Days Prep/

40 Days Analyzee

Metals	10 grams	Cool to 4 o C	Plastic Jarg	180 Daysh

a	Quantity may be increased or decreased according to the requirements
of the analytical laboratory, as long as the QAOs are met.

b	“Cool to 4 o C” means that the samples are placed in an insulated
cooler and packed with frozen chemical ice.

c	Holding time begins at sample collection (holding times are consistent
with SW-846 requirements).

d	40-mL VOA vial or other appropriate containers shall have an airtight
cap (e.g., septum cap).

e	40-day holding time allowable only for methanol extract - 14-day
holding time for non-extracted VOCs.

f	Appropriate containers (e.g., opaque glass container) should be used
and should have Teflon® lined caps.

g	Polyethylene or polypropylene is preferred, glass jar is allowable.

h	Holding time for mercury analysis is 28 days.

Note:  Preservation requirements in the most recent version of SW-846
may be used if appropriate.

TABLE B1-5, HEADSPACE GAS DRUM AGE CRITERIA SAMPLING SCENARIOS

Scenario	Description

1	A.	Unvented drums without rigid poly liners are sampled through the
drum lid at the time of venting

B1.	Unvented drums with unvented rigid poly liners are sampled through
the rigid poly liner at the time of venting or prior to venting.

B2.	Vented drums with unvented rigid poly liners are sampled through the
rigid poly liner at the time of venting or prior to venting.

C.	Unvented drums with vented rigid poly liners are sampled through the
drum lid at the time of venting.

2		Drums that have met the criteria for Scenario 1 and then are vented,
but not sampled at the time of venting.a

3		Containers (i.e., drums, SWBs, and pipe components) that are
initially packaged in a vented condition and sampled in the container
headspace and containers that are not sampled under Scenario 1 or 2..

a 	Containers that have not met the Scenario 1 DAC at the time of
venting must be categorized under Scenario 3.  This requires the
additional information required of each container in Scenario 3 (i.e.,
determination of packaging configuration), and such containers can only
be sampled after meeting the appropriate Scenario 3 DAC.

TABLE B1-6, SCENARIO 1 DRUM AGE CRITERIA (in days) MATRIX

Summary Category Group	DAC (days)

S3000/S4000	127

S5000	53

Note:	Containers that are sampled using the Scenario 1 DAC do not
require information on the packaging configuration because the Scenario
1 DAC are based on a bounding packaging configuration.  In addition,
information on the rigid liner vent hole presence and diameter do not
apply to containers that are sampled using the Scenario 1 DAC because
they are unvented prior to sampling.

TABLE B1-7, SCENARIO 2 DRUM AGE CRITERIA (in days) MATRIX

	Summary Category Group S3000/S4000	Summary Category Group S5000

Filter H2 Diffusivity a	Rigid Liner Vent Hole Diameter (in) b	Rigid
Liner Vent Hole Diameter (in) b

(mol/s/mod fraction)	0.30	0.375	0.75 	1.0	0.30	0.375	0.75 	1.0

1.9 x 10-6	36	30	23	22	29	22	13	12

3.7 x 10-6	30	25	19	18	25	20	12	11

3.7 x 10-5	13	11	11	11	7	6	6	4

a	The documented filter H2 diffusivity must be greater than or equal to
the listed value to use the DAC for the listed filter H2 diffusivity
(e.g., a container with a filter H2 diffusivity of 4.2 x 10-6 must use a
DAC for a filter with a 3.7 x 10-6 filter H2 diffusivity).  If a filter
H2 diffusivity for a container is undocumented or unknown or is less
than 1.9x10-6 filter H2 diffusivity, a filter of known H2 diffusivity
that is greater than or equal to 1.9x10-6 filter H2 diffusivity must be
installed prior to initiation of the relevant DAC period.

b	The documented rigid liner vent hole diameter must be greater than or
equal to the listed value to use the DAC for the listed rigid liner vent
hole diameter (e.g., a container with a rigid liner vent hole of 0.5
inches must use a DAC for a rigid liner vent hole of 0.375 inch).  If
the rigid liner vent hole diameter for a container is undocumented
during packaging (Section B-3d(1)), repackaging (Section B-3d(1)),
and/or venting (Section B1-1a[6][ii]), that container must use a DAC for
a rigid liner vent hole diameter of 0.30 inch.

Note:  Containers that are sampled using the Scenario 2 DAC do not
require information on the packaging configuration because the Scenario
2 DAC are based on a bounding packaging configuration.

TABLE B1-8, SCENARIO 3 PACKAGING CONFIGURATION GROUPS

Packaging Configuration Group	Covered S3000/S4000 Packaging
Configuration Groups	Covered S5000 Packaging ConfigurationGroups

Packaging Configuration Group 1, 55-gallon drums a	No layers of
confinement, filtered inner lid b

No inner bags, no liner bags (bounding case)	No layers of confinement,
filtered inner lid b

No inner bags, no liner bags (bounding case)

Packaging Configuration Group 2, 55-gallon drums a	1 inner bag

1 filtered inner bag

1 liner bag (bounding case)

1 filtered liner bag	1 inner bag

1 filtered inner bag

1 liner bag

1 filtered liner bag

1 inner bag, 1 liner bag

1 filtered inner bag, 1 filtered liner bag

2 inner bags

2 filtered inner bags

2 inner bags, 1 liner bag

2 filtered inner bags, 1 filtered liner bag

3 inner bags

3 filtered inner bags

3 filtered inner bags, 1 filtered liner bag

3 inner bags, 1 liner bag (bounding case)

TABLE B1-8, SCENARIO 3 PACKAGING CONFIGURATION GROUPS (continued)

Packaging Configuration Group	Covered S3000/S4000 Packaging
Configuration Groups	Covered S5000 Packaging ConfigurationGroups

Packaging Configuration Group 3, 55-gallon drums a	1 inner bag, 1 liner
bag

1 filtered inner bag, 1 filtered liner bag

2 inner bags

2 filtered inner bags

2 liner bags (bounding case)

2 filtered liner bags	2 liner bags

2 filtered liner bags

1 inner bag, 2 liner bags

1 filtered inner bag, 2 filtered liner bags

2 inner bags, 2 liner bags

2 filtered inner bags, 2 filtered liner bags

3 filtered inner bags, 2 filtered liner bags

4 inner bags

3 inner bags, 2 liner bags

4 inner bags, 2 liner bags (bounding case)

Packaging Configuration Group 4, pipe components	No layers of
confinement inside a pipe component

1 filtered inner bag, 1 filtered metal can inside a pipe component

2 inner bags inside a pipe component

2 filtered inner bags inside a pipe component

2 filtered inner bags, 1 filtered metal can inside a pipe component

2 inner bags, 1 filtered metal can inside a pipe component (bounding
case)	No layers of confinement inside a pipe component

1 filtered inner bag, 1 filtered metal can inside a pipe component

2 inner bags inside a pipe component

2 filtered inner bags inside a pipe component

2 filtered inner bags, 1 filtered metal can inside a pipe component

2 inner bags, 1 filtered metal can inside a pipe component (bounding
case)

TABLE B1-8, SCENARIO 3 PACKAGING CONFIGURATION GROUPS (continued)

Packaging Configuration Group	Covered S3000/S4000 Packaging
Configuration Groups	Covered S5000 Packaging ConfigurationGroups

Packaging Configuration Group 5, Standard Waste Box a	No layers of
confinement

1 SWB liner bag (bounding case)	No layers of confinement

1 SWB liner bag (bounding case)

Packaging Configuration Group 6, Standard Waste Box a	any combination of
inner and/or liner bags that is less than or equal to 6

5 inner bags, 1 SWB liner bag (bounding case)	any combination of inner
and/or liner bags that is less than or equal to 6

5 inner bags, 1 SWB liner bag (bounding case)

a	If a specific Packaging Configuration Group cannot be determined based
on the data collected during packaging (Section B-3d(1)) and/or
repackaging (Section B-3d(1)), a conservative default Packaging
Configuration Group of 3 for 55-gallon drums and 6 for SWBs must be
assigned provided the 55-gallon drums do not contain pipe component
packaging. If pipe components are present as packaging in the 55-gallon
drums, the pipe components must be sampled following the requirements
for Packaging Configuration Group 4.

b	A “filtered inner lid” is the inner lid on a double lid drum that
contains a filter.

Definitions:

	Liner Bags:  One or more optional plastic bags that are used to control
radiological contamination.  Liner bags for drums have a thickness of
approximately 11-mils.  SWB liner bags have a thickness of approximately
14-mils.  Liner bags are typically similar in size to the container.

	Inner Bags:  One or more optional plastic bags that are used to control
radiological contamination.  Inner bags have a thickness of
approximately 5-mils and are typically smaller than liner bags.

TABLE B1-9, SCENARIO 3 DRUM AGE CRITERIA (in days) MATRIX FOR S5000
WASTE BY PACKAGING CONFIGURATION GROUP

Packaging Configuration Group 1

	Rigid Liner Vent Hole Diameter b

Filter H2 Diffusivity a (mol/s/mol fraction)	0.3-inch Diameter Hole
0.375-inch Diameter Hole	0.75-inch Diameter Hole	1-inch Diameter Hole	No
Liner Lid	No Liner

1.9x10-6	131	95	37	24	4	4

3.7x10-6	111	85	36	24	4	4

3.7x10-5	28	28	23	19	4	4

Packaging Configuration Group 2

	Rigid Liner Vent Hole Diameter b

Filter H2 Diffusivity a (mol/s/mol fraction)	0.3-inch Diameter Hole
0.375-inch Diameter Hole	0.75-inch Diameter Hole	1-inch Diameter Hole	No
Liner Lid	No Liner

1.9x10-6	175	138	75	60	30	11

3.7x10-6	152	126	73	59	30	11

3.7x10-5	58	57	52	47	28	8

Packaging Configuration Group 3

	Rigid Liner Vent Hole Diameter b

Filter H2 Diffusivity a (mol/s/mol fraction)	0.3-inch Diameter Hole
0.375-inch Diameter Hole	0.75-inch Diameter Hole	1-inch Diameter Hole	No
Liner Lid	No Liner

1.9x10-6	199	161	96	80	46	16

3.7x10-6	175	148	93	79	46	16

3.7x10-5	72	72	67	62	42	10

TABLE B1-9, SCENARIO 3 DRUM AGE CRITERIA (in days) MATRIX FOR S5000
WASTE BY PACKAGING CONFIGURATION GROUP (continued)

Packaging Configuration Group 4

Filter H2 Diffusivity a (mol/s/mol fraction)	Headspace Sample Taken
Inside Pipe component

> 1.9x10-6	152

Packaging Configuration Group 5

Filter H2 Diffusivity a, c (mol/s/mol fraction)	Headspace Sample Taken
Inside SWB

> 7.4x10-6	15

Packaging Configuration Group 6

Filter H2 Diffusivity a, c (mol/s/mol fraction)	Headspace Sample Taken
Inside SWB

> 7.4x10-6	56

a	The documented filter H2 diffusivity must be greater than or equal to
the listed value to use the DAC for the listed filter H2 diffusivity
(e.g., a container with a filter H2 diffusivity of 4.2 x 10-6 must use a
DAC for a filter with a 3.7 x 10-6 filter H2 diffusivity).  If a filter
H2 diffusivity for a container is undocumented or unknown or is less
than 1.9x10-6 filter H2 diffusivity, a filter of known H2 diffusivity
that is greater than or equal to 1.9x10-6 filter H2 diffusivity must be
installed prior to initiation of the relevant DAC period.

b	The documented rigid liner vent hole diameter must be greater than or
equal to the listed value to use the DAC for the listed rigid liner vent
hole diameter (e.g., a container with a rigid liner vent hole of 0.5
inches must use a DAC for a rigid liner vent hole of 0.375 inch).  If
the rigid liner vent hole diameter for a container is undocumented
during packaging (Section B-3d(1)), repackaging (Section B-3d(1)),
and/or venting (Section B1-1a[6[[ii]), that container must use a DAC for
a rigid liner vent hole diameter of 0.30 inch.

c	The filter H2 diffusivity for SWBs is the sum of the diffusivities for
all of the filters on the container because SWBs have more than one
filter.

TABLE B1-10, SCENARIO 3 DRUM AGE CRITERIA (in days) MATRIX FOR S3000 AND
S4000 WASTE BY PACKAGING CONFIGURATION GROUP

Packaging Configuration Group 1

	Rigid Liner Vent Hole Diameter b

Filter H2 Diffusivity a (mol/s/mol fraction)	0.3-inch Diameter Hole
0.375-inch Diameter Hole	0.75-inch Diameter Hole	1-inch Diameter Hole	No
Liner Lid	No Liner

1.9x10-6	131	95	37	24	4	4

3.7x10-6	111	85	36	24	4	4

3.7x10-5	28	28	23	19	4	4

Packaging Configuration Group 2

	Rigid Liner Vent Hole Diameter b

Filter H2 Diffusivity a (mol/s/mol fraction)	0.3-inch Diameter Hole
0.375-inch Diameter Hole	0.75-inch Diameter Hole	1-inch Diameter Hole	No
Liner Lid	No Liner

1.9x10-6	213	175	108	92	56	18

3.7x10-6	188	161	105	90	56	17

3.7x10-5	80	80	75	71	49	10

Packaging Configuration Group 3

	Rigid Liner Vent Hole Diameter b

Filter H2 Diffusivity a (mol/s/mol fraction)	0.3-inch Diameter Hole
0.375-inch Diameter Hole	0.75-inch Diameter Hole	1-inch Diameter Hole	No
Liner Lid	No Liner

1.9x10-6	283	243	171	154	107	34

3.7x10-6	253	225	166	151	106	31

3.7x10-5	121	121	115	110	84	13

TABLE B1-10, SCENARIO 3 DRUM AGE CRITERIA (in days) MATRIX FOR S3000 AND
S4000 WASTE BY PACKAGING CONFIGURATION GROUP (continued)

Packaging Configuration Group 4

Filter H2 Diffusivity a (mol/s/mol fraction)	Headspace Sample Taken
Inside Pipe component

> 1.9x10-6	152

Packaging Configuration Group 5

Filter H2 Diffusivity a, c (mol/s/mol fraction)	Headspace Sample Taken
Inside SWB

> 7.4x10-6	15

Packaging Configuration Group 6

Filter H2 Diffusivity a, c (mol/s/mol fraction)	Headspace Sample Taken
Inside SWB

> 7.4x10-6	56

a	The documented filter H2 diffusivity must be greater than or equal to
the listed value to use the DAC for the listed filter H2 diffusivity
(e.g., a container with a filter H2 diffusivity of 4.2 x 10-6 must use a
DAC for a filter with a 3.7 x 10-6 filter H2 diffusivity).  If a filter
H2 diffusivity for a container is undocumented or unknown or is less
than 1.9x10-6 filter H2 diffusivity, a filter of known H2 diffusivity
that is greater than or equal to 1.9x10-6 filter H2 diffusivity must be
installed prior to initiation of the relevant DAC period.

b	The documented rigid liner vent hole diameter must be greater than or
equal to the listed value to use the DAC for the listed rigid liner vent
hole diameter (e.g., a container with a rigid liner vent hole of 0.5
inches must use a DAC for a rigid liner vent hole of 0.375 inch).  If
the rigid liner vent hole diameter for a container is undocumented
during packaging (Section B-3d(1)), repackaging (Section B-3d(1)),
and/or venting (Section B1-1a[6[[ii]), that container must use a DAC for
a rigid liner vent hole diameter of 0.30 inch.

c	The filter H2 diffusivity for SWBs is the sum of the diffusivities for
all of the filters on the container because SWBs have more than one
filter.

Figure B1-1, Example of the Chain-of-Custody for Headspace Gas Sample
Canisters

        (The COC, the SCID, and the Sample Canister Tag accompany the
sample canister)

(For the most current Sample Canister Tag, refer to

L-4006, Chain-of-Custody and Sample Administration for Headspace Sample
Canisters)

Figure B1-2, Example of the Sample Canister Information Document

       (The SCID, the COC, and the Sample Canister Tag accompany the
sample canister)

(For the most current Sample Canister Tag, refer to

L-4006, Chain-of-Custody and Sample Administration for Headspace Sample
Canisters)

Figure B1-3, Example of the Sample Canister Tag

              (The COC, the SCID, and the Sample Canister Tag accompany
the sample canister)

(For the most current Sample Canister Tag, refer to

L-4006, Chain-of-Custody and Sample Administration for Headspace Sample
Canisters)

Figure B1-4, Example of the Chain-of-Custody/Sample Analysis Request
(WIPP)

(COC used for homogeneous solids and soil/gravel samples)

(For the most current COC, refer to PRO-543-ASD-002, Initiation,
Preparation, and

Implementation of Chain-of-Custody Forms)

CUSTODY SEAL

DATE:

SIGNATURE:

Figure B1-5, Example Custody Seal

                      (Custody Seal used for homogeneous solids and
soil/gravel samples)

Figure B1-6, Overall Programmatic Approach to Visual Examination of the
Waste for Confirmation of RTR

Figure B1-7, Headspace Gas Drum Age Criteria Sampling Scenario Selection
Process

B2.	statistical methods used in sampling and analysis

B2-1	Approach for Statistically Selecting Waste Containers for Visual
Examination (to Confirm RTR)

As a Quality Control check on the radiographic examination of waste
containers, a statistically selected portion of the certified waste
containers is opened and visually examined.  The data from VE are used
to verify the waste matrix code, waste material parameter weights, and
absence of prohibited items as determined by RTR.

The data obtained from the visual examination are also used to
determine, with acceptable confidence, the percentage of miscertified
waste containers from the radiographic examination.  Miscertified
containers are those that RTR indicates meet the Waste Acceptance
Criteria for the Waste Isolation Pilot Plant (WIPP-DOE-69) and the
Safety Analysis Report for the TRUPACT-II Shipping Package, NRC Docket
Number 71-9218, Appendix 1.3.7 - TRUPACT-II Authorized Methods for
Payload Control, but that VE indicates do not meet these criteria.

Initially, RFETS uses an eleven-percent (11%) miscertification rate to
calculate the number of waste containers to undergo VE until an
RFETS-specific miscertification rate is established.  An initial
site-specific miscertification rate is established by characterizing a
lot of no less than fifty containers in a single Summary Category Group
at the initial 11% miscertification rate.  The results of this initial
characterization then serve as the site-specific miscertification rate
until reassessed annually as described below.

The site-specific miscertification rate is applied initially to each
Summary Category Group to determine the number of containers in that
Summary Category Group requiring visual examination, as specified in
Table B2-1.  However, a Summary Category Group-specific miscertification
rate is determined when either six months have passed since radiographic
characterization commenced on a given Summary Category Group, or at
least 50% of a given Summary Category Group has undergone radiographic
characterization, whichever occurs first.  The Summary Category Group is
then subject to the VE requirements of this reevaluated Summary Category
Group-specific miscertification rate to ensure that the entire Summary
Category Group is appropriately characterized.  Table B2-1 provides the
number of waste containers per Summary Category Group that undergo VE
for various miscertification rates and waste container population sizes
using a hypergeometric sampling approach.  A miscertification rate of 1%
is used for any Summary Category Group-specific miscertification rate
calculated to be less than 1%.

The site-specific miscertification rate is reassessed annually by
calculating a container-weighted average of all historic Summary
Category Group-specific miscertification rates.  Each Summary Category
Group-specific miscertification rate is rounded off to the nearest
integer value before being used to calculate the new site-specific
miscertification rate.  A miscertification rate of 1% is used for any
site-specific miscertification rate calculated to be less than 1%.

The number of waste containers requiring VE (as identified in Table
B2-1) utilizes a hypergeometric approach is based on a 90 percent
confidence that the actual miscertification rate (for the population) is
less than the 90 percent upper confidence level (UCL), and also an 80
percent confidence that the UCL will be less than 14 percent if the
actual miscertification rate is the same as the targeted percent of
miscertified waste containers (column heading of Table B2-1).  Thus,
there is only a 10 percent probability that the UCL will be below 14
percent in the case where the actual miscertification rate is 14 percent
or greater.  Also, there is only a 20 percent probability that the UCL
will be above 14 percent in the case where the actual miscertification
rate is the same as the targeted percent.

B2-1	Approach for Statistically Selecting Waste Containers for Visual
Examination (to Confirm RTR)  (continued)

The hypergeometric approach to determining the number of containers to
undergo VE is dependant upon the defined estimate of the allowable
proportion of containers that were miscertified and information on
previous percentages of containers that were miscertified.  The
rationale and details of this methodology are discussed further below.
Compliance with the requirements for statistical selection of waste
containers for VE is achieved through the execution of site-specific
procedure PRO-945-WIPP-009, RCRA Characterization of TRU Waste to be
Disposed of at WIPP.

 ) of the true population proportion ptrue is:

 					(B2-1)

This value is only an estimate, and as a result has some uncertainty
associated with it.  This uncertainty is quantified by calculating the
upper one-sided (1 - () percent confidence limit for p, call it pUCL.
This confidence limit gives the largest value the true proportion could
take on and still have a "reasonable" chance (e.g., an ( = .10
probability) of producing x miscertified containers in a sample of n out
of N.  This upper confidence limit is calculated as:

 						(B2-2)

where MUCL is the largest value of M such that the probability of
observing x or fewer miscertified containers in a sample of size n is
less than or equal to (.  That is, it is the largest value of M such
that the following inequality is true:

 						(B2-3)

where each term in parentheses has the usual combinatorial
interpretation.  For example:

  						(B2-4)

Each term in the sum in Equation (B2-3) is the hypergeometric
probability of observing k miscertified containers in a sample size n
from a population of size N in which there are M miscertified containers
(and hence the population proportion of miscertified containers is p =
M/N).  The value MUCL is obtained by substituting different values for M
into Equation (B2-3) until the largest value satisfying the inequality
is found.

Note that in Equation (B2-3), the upper confidence limit is dependent on
x, the number of miscertifications observed in the sample, as well as on
n, the sample size.  To obtain the required sample size, the values of x
that are likely to be seen also need to be considered.  Sample size that
are visually examined are determined by setting a desired upper
confidence limit value and then manipulating x and n in Equation (B2-3).

B2-2	Approach for Selecting Waste Containers for Statistical Sampling

B2-2a	Statistical Selection of Containers for Total (or TCLP) Analysis

The statistical approach for characterizing retrievably stored
homogeneous solids and soil/gravel waste and repackaged or treated S3000
waste that RFETS demonstrates is not suitable for control charting using
sampling and analysis relies on using acceptable knowledge to segregate
waste containers into relatively homogeneous waste streams.  Using
acceptable knowledge, the entire waste stream is classified as hazardous
or nonhazardous rather than individual waste containers.  Individual
waste containers serve as convenient units for characterizing the
combined mass of waste from the waste stream of interest.

Once segregated by waste stream, random selection and sampling of the
waste containers followed by analysis of the waste samples is performed
to ensure that the resulting mean contaminant concentration provides an
unbiased representation of the true mean contaminant concentration for
each waste stream.  The TWCP Site PM verifies that the samples collected
from within a waste stream were selected randomly in accordance with
PRO-945-WIPP-009, RCRA Characterization of TRU Waste to be Disposed of
at WIPP.

An end use of analytical results for retrievably stored homogeneous
solids and soil/gravel is for assigning the Environmental Protection
Agency hazardous waste D-codes that apply to each mixed waste stream and
to confirm acceptable knowledge.  The D-codes are indicators that the
waste exhibits the toxicity characteristic for specific contaminants
under RCRA.  The RCRA-toxicity determination is made on the basis of
sampling and analysis of waste streams and on whether or not the waste
stream includes F-code wastes.  If a waste stream includes one or more
RCRA F-codes identified via acceptable knowledge, toxicity
characteristic contaminants associated with the F-code waste(s) are not
included in the RCRA-toxicity characteristic determination.  That is,
the F-codes take precedence over RCRA-toxicity D-code, and the waste
stream is assumed hazardous regardless of the concentration.  Therefore,
toxicity characteristics contaminants associated with F-codes(s) for a
waste stream are omitted from all calculations for determining the
number of containers to sample because these wastes streams are assumed
to be hazardous.  In addition, each toxicity characteristic contaminant
associated with the F-code(s) is excluded from evaluation of analytical
results to determine D-codes.  Contaminants of interest for the
sampling, analysis, and RCRA-toxicity determination of a waste stream,
then, excludes contaminants associated with F-codes that have been
assigned to the waste stream.

The sampling and analysis strategy is illustrated in Figure B2-1.
Preliminary estimates of the mean concentration and variance of each
RCRA regulated contaminant in the waste is used to determine the number
of waste containers to select for sampling and analysis.  The
preliminary estimates are made by obtaining a preliminary number of
samples from the waste stream or from previous sampling from the waste
stream.  Preliminary estimates are based on samples from a minimum of 5
waste containers.  Samples collected to establish preliminary estimates
that are selected, sampled, and analyzed in accordance with applicable
provisions of the WAP may be used as part of the required number of
samples to be collected.  The applicability of the preliminary estimates
to the waste stream to be sampled is justified and documented.  The
preliminary estimates for the mean, variance and the appropriate number
of samples (n) to be collected for each contaminant is calculated in
accordance with the following equations:

											(B2-5)

											B(2-6)

B2-2a	Statistical Selection of Containers for Total (or TCLP) Analysis
(continued)

where x is the calculated mean and s2 is the calculated concentration
variance, n is the number of samples analyzed, xi is the concentration
determined in the ith sample, and i is an index from 1 to n.

Based upon the preliminary estimates of x and s2 for each chemical
contaminant of concern, the appropriate number of samples (n) to be
collected for each contaminant is estimated using the following
formulas:

											(B2-7)

Where:

	n0 = the initial number of samples used to calculate the preliminary
sample estimate.

	n = the calculated number of samples in the preliminary estimate.

	t2 = the 90th percentile for a t distribution with n0-1degrees of
freedom.

	RT = Regulatory Threshold of the contaminant (TC limit for toxicity
characteristic wastes, PRQL for listed wastes).

The number of samples collected is based upon the largest n calculated
for each of the contaminants of concern.  The actual number of samples
collected is adjusted as necessary to ensure that an adequate number of
samples are collected to allow for acceptable levels of completeness.

All calculations are rounded up to the nearest integer.  A minimum of
five containers are sampled and analyzed in each waste stream.  If there
are fewer than the minimum of the required number of containers in a
waste stream, one or more containers is sampled more than once to obtain
the samples of the waste.  Otherwise any one container may be selected
for sampling only once.

The calculated total number of required waste containers is then
randomly sampled and analyzed.  Waste container samples from the
preliminary mean and variance estimates may be counted as part of the
total number of calculated required samples if and only if:

There is documented evidence that the waste containers for the
preliminary estimate samples were selected in the same random manner as
is chosen for the required samples.

There is documented evidence that the method of sample collection in the
preliminary estimate samples were identical to the methodology to be
employed for the required samples.

There is documented evidence that the method of sample analysis in the
preliminary estimate samples were identical to the analytical
methodology employed for the required samples.

There is documented evidence that the validation of the sample analyses
in the preliminary estimate samples were comparable to the validation
employed for the required samples.  In addition, the validated sample
results shall indicate that all sample results were valid according to
the analytical methodology.

For waste streams with calculated upper confidence limits below the
regulatory threshold, the required number of samples is collected to
establish that the constituent is below the regulatory threshold.  Upon
collection and analysis of the preliminary samples, or at any time after
the preliminary samples have been analyzed, RFETS may assign hazardous
waste codes to a waste stream.

B2-2a	Statistical Selection of Containers for Total (or TCLP) Analysis
(continued)

Compliance with the requirements for statistically selecting retrievably
stored waste containers for total/TCLP analysis is achieved through the
execution of procedure PRO-945-WIPP-009, RCRA Characterization of TRU
Waste to be Disposed of at WIPP.  Document RMRS-WIPP-98-100, Acceptable
Knowledge TRU/TRM Waste Stream Summaries identifies the various
transuranic waste streams based on acceptable knowledge.

B2-2b	Statistical Selection of Containers for Headspace Gas Analysis

If a waste stream meets the conditions for representative headspace gas
sampling in Section B-3a(1), headspace gas sampling of that waste stream
may be done on a randomly selected portion of containers in the waste
stream.  The minimum number of containers (n) that must be sampled is
determined by taking an initial VOC sample from 10 randomly selected
containers.  These samples are analyzed for all the target analytes.
The standard deviation (s) is calculated for each of the nine VOCs in
Module IV, Table IV.D.1. of the WIPP-WAP.  The value of n is determined
in accordance with the equation presented in Section B2-2b of the
WIPP-WAP.

											B(2-8)

Where:

nvoci is the number of samples needed to representatively sample the
waste stream for the VOCi from Table IV.D.1.

sevoci is the estimated standard deviation, based on the initial
10-samples, for VOCi from Table IV.D.1.

Evoci is the allowable error determined as 1 percent of the limiting
concentration for VOCi from Table IV.D.1.

Waste container samples from the preliminary mean and variance estimates
may be counted as part of the total number of calculated required
samples if and only if:

There is documented evidence that the waste containers for the
preliminary estimate samples were selected in the same random manner as
is chosen for the required samples.

There is documented evidence that the method of sample collection in the
preliminary estimate samples were identical to the methodology to be
employed for the required samples.

There is documented evidence that the method of sample analysis in the
preliminary estimate samples were identical to the analytical
methodology employed for the required samples.

There is documented evidence that the validation of the sample analyses
in the preliminary estimate samples were comparable to the validation
employed for the required samples.  In addition, the validated sample
results shall indicate that all sample results were valid according to
the analytical methodology.

The mean and standard deviation calculated after sampling n containers
can be used to calculate a UCL90 for each of the headspace gas VOCs
using the methodology presented in Section B2-3b.

B2-3	Upper Confidence Limit for Statistical Sampling

B2-3a	Upper Confidence Limit for Statistical Solid Sampling

Upon completion of the required sampling, final mean and variance
estimates and the UCL90 for the mean concentration for each contaminant
is determined.  The observed sample n* is checked against the
preliminary estimate for the number of samples (n) to be collected
before proceeding using the equation presented in Section B2-3a of the
WIPP-WAP.

If the observed sample n* estimate results in greater than 20 percent
more required samples than were originally calculated, then the
additional samples required to fulfill the revised sample estimate are
collected and analyzed.  The determination of n* is an iterative process
that continues until the difference between n* and the previous sample
determination is less than 20 percent.

Once sufficient sampling and analysis has occurred, the waste
characterization will proceed.  The assessment is made with 90 percent
confidence.  The UCL90 for the mean concentration of each contaminant
will be calculated in accordance with the equation presented in Section
B2-3a of the WIPP-WAP.

When composite sample headspace gas sample results are used, the mean,
standard deviation, and t-statistic are based on the number of composite
samples analyzed, rather than the number of containers sampled.  If the
UCL90 for the mean concentration is less than the regulatory threshold
limit, the waste stream is not assigned the hazardous waste code for
this contaminant.  If the UCL90 is greater than or equal to the
regulatory threshold limit, the waste stream is assigned the hazardous
waste code for this contaminant.

Compliance with the requirements for calculation and comparison of the
UCL90 to regulatory thresholds is achieved through the execution of
procedure PRO-945-WIPP-009, RCRA Characterization of TRU Waste to be
Disposed of at WIPP.

B2-3b	Upper Confidence Limit for Statistical Headspace Gas Sampling

If a waste stream meets the conditions for representative headspace gas
sampling in Section B-3a(1), a UCL90 concentration for each of the
headspace gas VOCs is calculated from the sample data collected. The
observed sample n* is checked against the estimate for the number of
samples (n) to be collected before proceeding using the equation
presented in Section B2-3b of the WIPP-WAP.

If the observed sample n* estimate results in greater than 20 percent
more required samples than were originally calculated, then the
additional samples required to fulfill the revised sample estimate are
collected and analyzed.  The determination of n* is an iterative process
that continues until the difference between n* and the previous sample
determination is less than 20 percent.

Then, the UCL90 is calculated using the UCL90 equation presented in
Section B2-3a of the WIPP-WAP.  In this case, the UCL90 is the 90
percent upper confidence VOC concentration, x is the calculated mean VOC
concentration and s is the standard deviation.  The value of t(a, n-1)
is taken from Table 9-2 of Chapter 9 of SW-846.

The calculated UCL90 concentration for each headspace gas VOC is then
assigned to those containers in the waste stream not selected for
headspace gas sampling.  If the calculated UCL90 concentration is less
than the applicable MDL, the MDL for the VOC is assigned to each
unsampled container instead of the UCL90 concentration.

B2-4	Control Charting for Newly Generated Waste Stream Sampling

For newly generated waste streams that RFETS characterizes using control
charts, significant process changes and process fluctuations associated
with newly generated waste is determined using statistical process
control (SPC) charting techniques; these techniques require historical
data for determining limits for indicator species, and subsequent
periodic sampling to assess process behavior relative to historical
limits.  SPC is performed on waste prior to solidification or packaging
for ease of sampling.  If the limits are exceeded for any toxicity
characteristic parameter, the waste stream is recharacterized, and the
characterization is performed according to procedures required in the
WAP.

A Shewhart control chart (Gilbert 1987) is a control chart for means
that can be used for checking whether current data are consistent with
past data and whether shifts or trends in means have occurred.  The
control chart for means is constructed of a center line and upper and
lower control limits that are based on the mean and standard deviation
of historical data for the process.  If a current sample mean from the
process lies within the limits, the process is said to be “in
control”, or consistent with historical data.  If the current mean
exceeds the limits, the process has likely changed from historical
periods.

Logical sets of historical data are used for the construction of limits
in this application.  The sets originate from initial characterization
of the waste stream (if available), from characterization of a different
lot of the same waste stream, or from a similar retrievably stored waste
stream.  At a minimum, a logical set includes ten representative sample
values collected and analyzed from the newly generated waste stream.
The data used for construction of the limits is justified.  The
underlying assumptions for control charts are that the data are
independent and normally distributed with constant mean ( and constant
variance (2.  The statistical tests for normality are conducted and data
transformation to normality performed, if necessary.  Transformations
take place prior to any calculations that use the data.

Each limit is constructed such that there is a 90 percent confidence
that the true mean does not exceed a limit.  One-sided control limits
are used because once a waste stream has been determined to be
RCRA-hazardous, the limit exceedance of interest is on the lower side;
that is when the process may become nonhazardous.  Likewise, once a
waste stream has been determined not to be RCRA-hazardous, the limit
exceedance of interest is on the upper side; that is when the process
may become RCRA-hazardous.  Whether or not exceeding the limit would
result in a change in the RCRA-hazardous nature of the waste stream
depends on how close the observed control limits are to RCRA limits.

Current process data is collected and averaged for comparison to the
control limit for the mean.  The collection period and number of samples
included in the average are dependent on the waste stream
characteristics.  A small number of samples will reflect more of the
process variability and there will potentially be more limit exceedance.
 If two or three samples are collected for the mean in the required
annual (or batch) sampling of a relatively homogeneous waste stream,
limit exceedances may not occur.  If the waste stream is less
homogeneous, it is necessary to collect more samples to meet the
required confidence limit.

Periodically it is necessary to update the control limit for a process.
An update is performed that includes all historical data if there is no
evidence of a trend in the process or a shift in the mean for the
process.  If there has been a shift in the mean, only more recent data
that reflects the shift is used.  Control limits are based on at least
ten data points that are representative of the process and do not
exhibit outliers or a trend with time.

B2-4	Control Charting for Newly Generated Waste Stream Sampling
(continued)

Unless a waste generating process is designed to control RCRA
parameters, it is not possible to demonstrate that the waste stream has
a constant mean and constant variance, and as a result, it is not
feasible to develop meaningful control charts.  Baseline sampling and
acceptable knowledge may be used to demonstrate this lack of feasibility
(refer to WIPP Clarification Number CAO-00-029).

Control charting is not acceptable for uncontrolled processes, and
therefore wastes from such processes must be sampled using the
requirements in Section B2-2, Approach for Statistically Selecting
Retrievably Stored Waste Containers for Total (or TCLP) Analysis.
Because control charting is not useful in controlling hazardous waste
constituents in such cases, the Site characterizes these homogeneous
wastes in accordance with Section B2-2, and documents that the control
charting was unuseable (refer to WIPP Clarification Number CAO-00-029).

Table B2-1, Number of Waste Containers Requiring Visual Examination

ANNUAL NUMBER OF WASTE CONTAINERS  PER SUMMARY CATEGORY GROUP UNDERGOING
CHARACTERIZATION	NUMBER OF WASTE CONTAINERS REQUIRING VISUAL EXAMINATION

BASED ON PERCENT OF WASTE CONTAINERS MISCERTIFIED TO WIPP-WAC

 BY RADIOGRAPHY IN PREVIOUS YEAR(S)

	1%

or less	2%	3%	4%	5%	6%	7%	8%	9%	10%	11%	12%	13%	14%

or greater

50 or less	22a	22	22a	22	29a	29	41a	41	46a	46	50a	50	50a	50

100	15	24	24	33	33	41	48	62	69	81	87	96	100	100

200	15	26	26	35	44	52	68	83	105	126	152	176	196	200

300	15	26	26	35	44	53	70	94	116	153	202	247	287	300

400	15	26	26	36	45	62	79	103	134	178	235	316	377	400

500	16	26	26	36	45	63	80	104	143	196	268	364	465	500

1000	16	27	27	36	46	64	81	114	162	239	359	568	848	1000

1500	16	27	27	37	46	64	81	123	171	257	416	701	1176	1500

2000	16	27	27	37	46	64	90	123	172	266	441	795	1453	2000

a	Number of containers for the higher even-number percent of
miscertified containers is used because an odd percent implies a
noninteger number of containers are likely to be miscertified.

Figure B2-1, Statistical Approach to Sampling and Analysis of Waste
Streams of Retrievably Stored Homogeneous Solids and Soil/Gravel

B3.	Quality assurance objectives and data validation techniques for
Waste characterization sampling and analytical methods

B3-1	Validation Methods

Qualitative as well as quantitative validation of all data are performed
so that data used for WIPP compliance activities are of known and
acceptable quality.  Validation includes a quantitative determination of
precision, accuracy, completeness, and method detection limit (as
appropriate) for headspace gas, VOC, SVOC, and metals analysis.  These
quantitative data validations are performed by TWCP staff and compared
to the QAOs specified in Sections B3-2 through B3-9.  A qualitative
determination of comparability and representativeness is also performed.

Data generation level validation for RFETS waste solid sampled and
analyzed at INEEL is conducted by the INEEL TWCP as described in the
Attachment to the SOW for the INEEL TWCP (DOE 2003a).

Validation methods for RTR QAOs are presented in Section B3-10 of this
document.  VE, which occurs on a subpopulation of containers which have
already undergone RTR, is used to verify waste matrix codes and waste
material parameter weights as described in Section B1-3 and Section
B3-4.  During VE, the waste matrix code is determined and the waste
material parameter codes are estimated to verify that the container is
properly included in the appropriate waste stream.

The TWCP Site PM documents that the selected waste containers from
within a waste stream are randomly selected according to 95-WP/SAP-001,
Transuranic (TRU/TRM) Waste Sampling Plan.  Sampling personnel follow
current procedures (as described in Section B1 of this document) to
ensure that samples are representative of the waste contained in a
particular waste container or a waste stream.

Data validation will be used to assess the quality of waste
characterization data collected based upon project precision, accuracy,
completeness, comparability, and representativeness objectives.  These
objectives are described below:

B3-1a	Precision

Precision is a measure of the mutual agreement among multiple
measurements of a single analyte, either by the same method or by
different methods.  Precision is either expressed as the relative
percent difference (RPD) for duplicate measurements or as the percent
relative standard deviation (%RSD) for three or more replicate
measurements.  For duplicate measurements, the precision expressed as
the RPD is calculated as follows:

Where C1 and C2 are the two values obtained by analyzing the duplicate
samples.

For three or more replicate measurements, the precision expressed as the
%RSD is calculated as follows:

Where s is the standard deviation and y is the mean of the replicate
sample analyses.

B3-1a	Precision  (continued)

The standard deviation, s, is calculated as follows:

Where yi is the measured value of the ith replicate sample analysis
measurement, and n equals the number of replicate analyses.

Another aspect of precision is associated with analytical equipment
calibration.  In these instances, the percent difference (%D) between
multiple measurements of an equipment calibration standard are
calculated as follows:

Where C1 is the initial measurement and C2 is the second or other
additional measurement.

B3-1b	Accuracy

Accuracy is the degree of agreement between a measured analyte
concentration (or the average of replicate measurements of a single
analyte concentration) and the true or known concentration.  Accuracy is
determined as the percent recovery (%R).

For situations where a standard reference material is used, the %R is
calculated as follows:

Where Cm is the measured concentration value obtained by analyzing the
sample and Csrm is the “true” or certified concentration of the
analyte in the sample.

For measurements where matrix spikes are used, the %R is calculated as
follows:

Where S is the measured concentration in the spiked aliquot, U is the
measured concentration in the unspiked aliquot, and Csa is the actual
concentration of the spike added.

B3-1c	Method Detection Limit

The method detection limit (MDL) is the minimum concentration of an
analyte that can be measured and reported with 99 percent confidence
that the analyte concentration is greater than zero.  The MDL for all
quantitative measurements is defined as follows:

Where                            is the t-distribution value appropriate
to a 99-percent confidence level and a standard deviation estimate with
n-1 degrees of freedom, n is the number of observations, and s is the
standard deviation of replicate measurements.

B3-1d	Completeness

Completeness is a measure of the amount of valid data (i.e., data that
meets all QA/QC requirements) obtained from the overall measurement
system compared to the amount of data collected and submitted for
analysis.  Completeness must be expressed as the number of samples
analyzed with valid results as a percent of the total number of samples
submitted for analysis.  Completeness, expressed as the percent complete
(%C), is calculated as follows:

Where V is the number of valid analytical results obtained and n is the
number of samples submitted for analysis.

B3-1e	Comparability

Comparability is the degree to which one data set can be compared to
another.  Comparability of data generated at different sites is assured
through the use of standardized, approved testing, sampling,
preservation, and analytical techniques and by meeting the QAOs
specified in Sections B3-2 through B3-9.  The criteria for data
usability are provided in EPA 540/R-99/008, USEPA Contract Laboratory
Program National Functional Guidelines for Organic Data Review (EPA
1999); and EPA 540-R-01-008, USEPA Contract Laboratory Program National
Functional Guidelines for Inorganic Data Review (EPA 2002).

The criteria shall address, as appropriate, the following:

Definition or reference of criteria used to define and assign data
qualifier flags based on Quality Assurance Objective results,

Criteria for assessing the usability of data impacted by matrix
interferences,

Criteria for assessing the usability of data based upon positive and
negative bias as indicated by quality control data, of data qualifiers,
and qualifier flags,

Criteria for assessing the usability of data due to:

	Severe matrix effects,

	Misidentification of compounds,

	Gross exceedance of holding times,

	Failure to meet calibration or tune criteria

Criteria for assessing the usability of data that does not meet minimum
detection limit requirements.

B3-1f	Representativeness

Representativeness is the degree to which sample data represent a
characteristic of a population, parameter variations at a sampling
point, or an environmental condition.  Representativeness is a
qualitative parameter that concerns the proper design of the sampling
program.

The representativeness of waste containers from waste streams subjected
to visual examination, reduced headspace gas sampling per Section
B-3a(1)(i) or B-3a(1)(ii), and homogeneous solids and soil/gravel
sampling and analysis is validated, through documentation, and this
confirms that a true random sample with an adequate population was
collected.  Since representativeness is a quality characteristic that
expresses the degree to which a sample or group of samples represents
the population being studied, the random selection of waste containers
ensures representativeness on a Program level.  The TWCP Site PM
documents that the selected waste containers from within a waste stream
were randomly selected.  Sampling personnel verify current procedures
are followed to ensure that samples are representative of the waste
contained in a particular waste container or a waste stream.

B3-1g	Nonconformance to DQOs

The analytical procedures contain specific QC requirements to ensure
that the data generated meets the DQOs.  Sections B3-5 through B3-8
provide more details on how the data from the analytical procedures is
assessed for compliance with the DQOs.  If data is generated which
doesn’t meet the DQOs, it is treated as a nonconformance.  Section
B3-13 describes the nonconformance procedure.  Failure to meet a DQO
which is first discovered at the TWCP Site PM signature release level
will be identified and reported as a nonconformance as described in
Section B3-13.  For analytical data, if a DQO is not met due to matrix
effects, the data is not considered a nonconformance.  Such data is
flagged appropriately and discussed in the case narrative of the
associated Batch Data Report.

B3-1h	Identification of Tentatively Identified Compounds

In accordance with SW-846 convention, identification of compounds
detected by gas chromatography/mass spectrometry methods that are not on
the list of target analytes shall be reported.  Both composited and
individual container headspace gas, volatile analysis (Totals), and
semi-volatile (Totals) shall be subject to tentatively identified
compound (TIC) reporting.  These TICs for GC/MS Methods are identified
in accordance with the following SW-846 criteria:

Relative intensities of major ions in the reference spectrum (ions
greater than 10% of the most abundant ion) should be present in the
sample spectrum.

The relative intensities of the major ions should agree within + 20
percent.

Molecular ions present in the reference spectrum should be present in
the sample spectrum.

Ions present in the sample spectrum but not in the reference spectrum
should be reviewed for possible background contamination or presence of
coeluting compounds.

Ions present in the reference spectrum but not in the sample spectrum
should be reviewed for possible subtraction from the sample spectrum
because of background contamination or coeluting peaks.

The reference spectra used for identifying TICs shall include, at a
minimum, all of the available spectra for compounds that appear in the
<IP_ADDRESS> NMAC (incorporating 40 CFR Part 261) Appendix VIII list.  The
reference spectra may be limited to VOCs when analyzing headspace gas
samples.

B3-1h	Identification of Tentatively Identified Compounds  (continued)

TICs shall be reported as part of the analytical batch data reports for
GC/MS methods in accordance with the following minimum criteria:

A TIC in an individual container headspace gas or solids sample shall be
reported in the analytical batch data report if the TIC meets the SW-846
identification criteria listed above and is present with a minimum of
10% of the area of the nearest internal standard.

A TIC in a composited headspace gas sample that contains 2 to 5
individual container samples shall be reported in the analytical batch
report if the TIC meets the SW-846 identification criteria listed above
and is present with a minimum of 2% of the area of the nearest internal
standard.

A TIC in a composited headspace gas sample that contains 6 to 10
individual container samples shall be reported in the analytical batch
report if the TIC meets the SW-846 identification criteria listed above
and is present with a minimum of 1% of the area of the nearest internal
standard.

A TIC in a composited headspace gas sample that contains 11 to 20
individual container samples shall be reported in the analytical batch
report if the TIC meets the SW-846 identification criteria listed above
and is present with a minimum of 0.5% of the area of the nearest
internal standard.

TICs that meet the SW-846 identification criteria, are reported in 25
percent of all waste containers sampled from a given waste stream, and
that appear in the <IP_ADDRESS> NMAC (incorporating 40 CFR §261) Appendix
VIII list, will be compared to acceptable knowledge data to determine if
the TIC is a listed waste in the waste stream.  TICs identified through
headspace gas analyses that meet the Appendix VIII list criteria and the
25 percent reporting criteria for a waste stream will be added to the
headspace gas waste stream target list regardless of the hazardous waste
listing associated with the waste stream.  TICs reported from the Totals
VOC or SVOC analyses may be excluded from the target analyte list for a
waste stream if the TIC is a constituent in an F-listed waste whose
presence is attributable to waste packaging materials or radiolytic
degredation from acceptable knowledge documentation.  If a listed waste
constituent TIC cannot be attributed to waste packaging materials,
radiolysis, or other origins, the constituent will be added to the
target analyte list and new hazardous waste codes will be assigned, if
appropriate.  TICs subject to inclusion on the target analyte list that
are toxicity characteristic parameters shall be added to the target
analyte list regardless of origin because the hazardous waste
designation for these codes is not based on source.  However, for
toxicity characteristic and non-toxic F003 constituents, RFETS may take
concentration into account when assessing whether to add a hazardous
waste code.  If a target analyte list for a waste stream is expanded due
to the presence of TICs, all subsequent samples collected from that
waste stream will be analyzed for constituents on the expanded list.

Method 8260B and Method 8270C state the following:  “only after visual
comparison of sample spectra with the nearest library searches may the
analyst assign a tentative identification.  Use the following guidelines
for making tentative identification…”  A visual comparison of sample
spectra allows the analyst to override potential spurious matches,
occasionally made by otherwise reliable criteria and/or algorithms.

B3-1h	Identification of Tentatively Identified Compounds  (continued)

The TIC identification procedure is outlined below:

An initial TIC report, generated by the instrument software, provides
background subtracted spectra for all compounds with peak areas greater
than 10% of the nearest internal standard.  The report lists the top
five library matches for each TIC found by the searching algorithm.
Generally, it is only necessary to evaluate the top hit, but it is
acceptable to evaluate as many of the compounds in the library search as
deemed necessary by the chemist to fully characterize the spectrum.

For WIPP evaluations, the TICs may be limited to the available spectra
for compounds that appear in the <IP_ADDRESS> NMAC (incorporating 40 CFR
Part 261) Appendix VIII list.

The chemist evaluates the compounds that provide the best library match
for each of the TIC’s found using the following criteria.

All ions that have a relative abundance of 10% or greater in the
reference spectrum (major ions) must be present in the sample spectrum.
The relative abundance scale of the spectrum may be used to evaluate
this criterion.  It is not necessary to print out the tabulated spectrum
to find the major ions.

The relative abundance of the major ions in the sample spectrum should
be within ( 20% of the relative abundance of the corresponding ions in
the reference spectrum.  The chemist will use judgment and visual
inspection of the spectra to determine if the relative abundance of the
ions from the sample and reference spectra are in agreement.

If a molecular ion is present in the reference spectrum it must be
present in the sample spectrum.

Any major ions that are present in the sample spectrum but not present
in the reference spectrum should be carefully evaluated for the presence
of a co-eluting compound or general chemical noise.  Special attention
should be given to ions at higher masses as these are more important for
compound identification than low mass ions.  High mass ions that are not
due to co-eluting compounds or chemical background should be considered
even if they are present with a relative abundance of less than 10%.

Any major ions that are present in the reference spectrum but not in the
sample spectrum should be carefully evaluated to assure that the ion was
not removed from the spectrum by the background subtraction algorithm.

If, after careful inspection by the chemist, the criteria from 2.1
through 2.5 have been satisfied then the compound is reported as a TIC.

If, after careful inspection by the chemist, one or more of the criteria
specified in sections 2.1 through 2.5 have not been satisfied, but the
sample spectrum is similar to the reference spectrum then the compound
is NOT reported as a TIC.

If, after careful inspection by the chemist, the criteria from 2.1
through 2.5 have not been satisfied then the compound is NOT reported as
a TIC.

IF a positive match cannot be established based on the above criteria,
the component in the sample spectrum is reported as an unknown.

B3-2	Headspace Gas Sampling

B3-2a	Quality Assurance Objectives

Headspace gas sampling will occur from the headspace within each
container of TRU mixed waste or randomly selected containers from waste
streams that meet the conditions for reduced headspace gas sampling
listed in Section B-3a(1).  Headspace gas samples are collected
following procedures PRO-1676-HGAS-S&A, Headspace Gas Sampling and
Analysis Using an On-Line Integrated System; L-4231, Headspace Gas
Sampling and Analysis Using an Automated Manifold; and L-4146, Headspace
Gas Sampling of Waste Containers.

Precision and accuracy of container headspace gas sampling operations
are assessed by analyzing field QC headspace samples, which consist of
field blanks, field duplicates, equipment blanks, and field reference
standards (refer to PRO-1669-HGAS-V&V, Headspace Gas V&V (Data Generator
Level); L-4053, Headspace Gas V & V (Data Generator Level); and L-5017,
HVOC Data Review and Validation (Data Generator Level)2).  If the QAOs
described in this section are not met, a nonconformance report is
prepared, submitted and resolved.  Table B1-2 summarizes the field QC
sample collection requirements and Table B1-3 summarizes the QC sample
acceptance criteria.

B3-2b	Precision

The precision of headspace gas sampling and analysis is assessed by
simultaneous collection of field duplicates for manifold sampling
operations.  The RPD is calculated for each field sample/duplicate pair
and compared to the criterion of 25%.  If the RPD exceeds the criterion
and the analyte concentration exceeds its PRQL, remedial actions must be
taken.  If the problem cannot be resolved, a nonconformance must be
written for any affected samples.  If there are no target analytes above
the PRQL detected in the duplicate samples then a second field reference
standard will be used as the duplicate.  The two field reference
standards must meet the same duplicate drum sample criteria.

B3-2c	Accuracy

Field reference standards are collected using the headspace sampling
equipment to assess the accuracy of the headspace sampling operations at
a frequency of one field reference standard per sampling batch.  The %R
for each analyte in the field reference sample will be calculated and
compared to the acceptance criteria of 70 – 130%, inclusive.  If a %R
is outside of the criteria, remedial actions must be taken.  If the
problem cannot be resolved, a nonconformance must be written for any
affected samples.

Field and equipment blanks are collected using the headspace sampling
equipment to assess the accuracy of the headspace sampling operations
with respect to contamination.  For the equipment blank, a clean gas
canister is selected from a batch of canisters that were cleaned at the
same time, the canister is filled with blank gas and then analyzed for
cleanliness.  For both field blanks and equipment blanks, the
concentration of each target analyte must be less than or equal to three
times the MDL.  If the concentration of any target compound is outside
of the criteria, remedial actions must be taken.  If the problem cannot
be resolved, a nonconformance must be written for any affected samples.

B3-2d	Completeness

Sampling completeness is expressed as the number of valid samples
collected as a percent of the total number of samples collected for each
waste stream.  The completeness can also be expressed as the number of
valid samples collected as a percent of the total number of containers
for each waste stream.  A valid sample is defined as a sample collected
in accordance with approved sampling methods and the container was
properly prepared for sampling (refer to Section B3-10 for data review,
validation, and verification).  The amount and type of data that may be
lost during the headspace gas sampling operation cannot be predicted in
advance. The TWCP Site PQAO evaluates the importance of any lost or
contaminated headspace gas samples and takes corrective action as
appropriate.  The project level office calculates the QAO for
completeness on a waste stream basis (i.e., the waste stream basis
calculation is not performed at the data generation level).

B3-2e	Comparability

Consistent use and application of uniform procedures and equipment as
specified in Section B1 of this document, and application of data
usability criteria [refer to EPA 540/R-099/008, USEPA Contract
Laboratory Program National Functional Guidelines for Organic Data
Review (EPA 1999); and EPA 540-R-01-008, USEPA Contract Laboratory
Program National Functional Guidelines for Inorganic Data Review (EPA
2002)] should ensure that headspace gas sampling operations are
comparable when sampling headspace at the different sampling facilities.
 RFETS takes corrective actions if uniform procedures, equipment, or
operations are not followed without approved and justified deviations.
In addition, laboratories analyzing samples successfully participate in
the Performance Demonstration Program (PDP).

B3-2f	Representativeness

Specific headspace gas sampling steps to ensure samples are
representative include:

Selection of the correct DAC Scenario and waste packaging configuration
and meeting DAC equilibrium times.

A sample canister cleaning and leak check after assembly.

Sampling equipment cleaning or disposal after use.

Sampling equipment leak check after sample collection.

Use of sample canisters with passivated internal surfaces.

Use of low-internal-volume sampling equipment.

Collection of samples with a low-sample volume to available headspace
volume ratio (less than 10 percent of the headspace when the headspace
can be determined).

Careful and documented pressure regulation of all activities specified
in Section B1-1 of this document.

Performance audits.

Collection of equipment blanks, field reference standard, field blanks,
and field duplicates at the specified frequencies.

Manifold pressure sensors and temperature sensors calibrated before
initial use and annually using NIST, or equivalent standards.

OVA calibrated daily, prior to first use, or as necessary according to
manufacturer’s specifications.

Failure to perform the checks at the prescribed frequencies will result
in corrective actions.  Procedures include specific steps and
requirements to ensure the representativeness of sampling.

B3-3	Sampling of Homogeneous Solids and Soils/Gravel

B3-3a	Quality Assurance Objectives

This section presents quality assurance objectives to ensure sampling is
conducted in a representative manner on a waste stream basis for
containers containing homogeneous solids and soil/gravel.  Samples are
randomly collected in both the horizontal and vertical planes of each
waste container.  For waste containers that contain homogeneous waste in
smaller containers within the waste container, one randomly chosen
smaller container must be sampled from each drum.

Quality assurance objectives for RFETS waste sampled at INEEL are
described in the Attachment to the SOW for the INEEL TWCP (DOE 2003a).

B3-3b	Precision

Sampling precision is determined by collecting and sampling duplicates,
once per sampling batch or once per week during the sampling operations,
whichever is more frequent.  A sampling batch is a suite of homogeneous
solids and soil/gravel samples collected consecutively using the same
sampling equipment within a specific time period.  A sampling batch can
be up to 20 samples (excluding field QA samples), which are collected
within 14 days of the first sample in the batch.  The Relative Percent
Difference (RPD) between co-located core samples will be calculated and
reported at the generation level and verified by the TWCP Site PQAO.

For RFETS waste sampled at INEEL the RPD of co-located core samples is
calculated and reported by the RFETS TWCP Site PQAO.

The recommended method for establishing acceptance criteria for
co-located cores and co-located samples is the F-Test method because the
F-Test:  1) does not require potentially arbitrary groupings into
batches, 2) is based on exact distributions, and 3) is more likely to
detect a change in the process.  When a sufficient number of samples are
collected (25 to 30 pairs of co-located cores or samples), control
charts of the RPD are developed for each constituent and for each waste
matrix or waste type (e.g., pyrochemical salts or organic sludges).  The
limits for the control chart are three standard deviations above or
below the average RPD.  Once constructed, RPDs for additional co-located
pairs will be compared with the control chart to determine whether or
not the co-located cores are acceptable.  Periodically, the control
charts are updated using all available data.  The RPD and F-Test
calculations are performed in accordance with PRO-604-RC-001, Field
Sample QC Data Calculation, Review, and Validation Batch Reports.

The statistical test involves calculating the variance for co-located
cores and samples by pooling the variances computed for each pair of
duplicate results.  The variance for the waste stream is computed
excluding any data from drums with co-located cores, because the test
requires the variance estimates to be independent.  All data must be
transformed to normality prior to computing variances and performing the
test.  The test is evaluated using the F distribution and the method for
testing the differences in variances.

B3-3c	Accuracy

Sampling accuracy using standard reference materials will not be
measured.  Because containers containing homogeneous solids and
soil/gravel with known quantities of analytes are not available,
sampling accuracy cannot be determined.  However, sampling methods and
requirements described are designed to minimize sample degradation and
hence maximize sampling accuracy.

Sampling accuracy as a function of sampling cross-contamination is
measured.  Equipment blanks are collected at a frequency of once per
equipment cleaning batch.  Corrective actions are taken if the blank
exceeds three times the MDLs (PRDLs for metals) listed for any of the
compounds or analytes listed in Tables B3-4, B3-6, and B3-8.  Equipment
blanks are collected from the following equipment types:

Fully assembled coring tools.

Liners cleaned separately from coring tools.

Miscellaneous sampling equipment that is reused (e.g., bowls, spoons,
chisels).

B3-3d	Completeness

Sampling completeness is expressed as the number of valid samples
collected as a percent of the total samples collected for each waste
stream.  A valid sample is any sample that is collected from a randomly
selected drum using randomly selected horizontal and vertical planes in
accordance with approved sampling methods.  RFETS must achieve a minimum
of 90% completeness.

B3-3e	Comparability

Consistent use and application of uniform procedures, sampling
equipment, and measurement units, as specified in Section B1 of this
document, should ensure that sampling operations are comparable.  The
analysis results of duplicates as required for alternative methods are
also examined to determine comparability.  Consistent application of
data usability criteria [refer to EPA 540/R-99/008, USEPA Contract
Laboratory Program National Functional Guidelines for Organic Data
Review (EPA 1999); and EPA 540-R-01-008, USEPA Contract Laboratory
Program National Functional Guidelines for Inorganic Data Review (EPA
2002)] should also ensure comparability.  In addition, the laboratories
analyzing the samples successfully participate in the PDP.

B3-3f	Representativeness

Procedures and sampling plans provide specific steps to ensure the
representativeness of samples including:

Sampling equipment is cleaned prior to sampling.

Sample tool selection is designed to minimize alteration of the in-place
characteristics.

One randomly selected container within a drum will be chosen if the drum
contains individual waste containers.

B3-4	Radiography

B3-4a	Quality Assurance Objectives

The QAOs for Real-Time Radiography (RTR) are detailed in this section.
The objective of RTR for the TWCP is to verify the Waste Matrix Code, to
identify prohibited items for each waste container, and to estimate each
waste material parameter weight.  All activities required to achieve
these objectives are described or incorporated by reference in this
document.

Data to meet these objectives are provided by trained and qualified RTR
operators.  The RTR operators scan the waste containers and record the
results on audio/videotapes and RTR data forms.  The precision,
accuracy, completeness, and comparability objectives for RTR data are
described in the following sections.

In the event QAOs are not met, corrective action will be taken in
accordance with procedure 1-A65-ADM-15.01, Control of Nonconforming
Items.

B3-4b	Precision

The qualitative determinations made during RTR do not lend themselves to
the statistical evaluation of precision.  Comparison of data derived
from RTR and VE (to Confirm RTR) on some containers at RFETS (and INEEL)
indicate that RTR operators can provide estimated inventories and waste
material parameter weights of waste items in a waste container (EG&G
1993).  The TWCP Site PQAO calculates and reports the relative percent
difference between the estimated waste material parameter weights (by
RTR) and these same parameters as determined by VE (to Confirm RTR).

Additionally, the precision of RTR is verified prior to use by tuning
precisely enough by viewing an image test pattern to demonstrate
compliance with QAOs.

B3-4c	Accuracy

The programmatic accuracy with which the waste material parameter
weights can be determined is documented through the VE (to Confirm RTR)
of a randomly selected statistical subpopulation of containers (See
Section B2-1).  The percentage of waste containers that require a new
Waste Matrix Code or are found to contain prohibited items after VE (to
Confirm RTR) is reported as a measure of RTR accuracy.  The TWCP Site
PQAO calculates and reports the miscertification rate of waste
containers that require assignment to a different Waste Matrix Code or
are found to contain prohibited items after VE (to Confirm RTR) as a
measure of RTR accuracy.  The miscertification rate calculated by the
TWCP Site PQAO is used to determine the number of containers subject to
VE (to Confirm RTR).

B3-4d	Completeness

An audio/videotape of the RTR examination and an RTR data form,
validated according to the requirements in Section B3-10, is obtained
for 100% of the retrievably stored waste containers in the TWCP for all
waste containers subject to RTR.  All audio/videotape and RTR data forms
are subject to validation as discussed in B3-10.

B3-4e	Comparability

The use of standardized radiography procedures and operator
qualification training enhances comparability of RTR data.  Operator
training requirements are outlined in Section B1-3b.  RTR operators
comply with the training and qualification requirements of the TWCP TIP,
and 5-NDT-TC-1A, Training, Qualification and Certification of
Nondestructive Testing Personnel.  Procedures 4-W30-NDT-00664, Real-Time
Radiography Testing of Transuranic and Low-Level Waste in Building 664;
4-I19-NDT-00569, Real-Time Radiography Testing of Transuranic and
Low-Level Waste in Building 569; and PRO-1520-Mobile-RTR, Mobile
Real-Time Radiography Testing of Transuranic and Low-Level Waste, are
used in implementation of the RTR program.

B3-5	Gas Volatile Organic Compound Analysis

B3-5a	Quality Assurance Objectives

The QAOs for the TWCP are listed in Table B3-2.  The specified QAOs
represent the required quality of data necessary to draw valid
conclusions regarding the TWCP objectives.  TWCP-required limits, such
as the PRQL associated with VOC analysis, are specified to ensure that
the analytical data collected satisfy the requirements of all data
users.  Key data quality indicators for headspace measurements are
defined below for Gas VOC analysis, and the methods to quantitatively
and qualitatively assess these indicators are discussed in Section B3 of
this document.  Table B-1 contains a synopsis of the site-specific
procedures used for gas volatile sampling and analysis.

B3-5b	Precision

Precision is assessed by analyzing laboratory duplicates, replicate
analyses of laboratory control samples, and PDP blind-audit samples.
The results of QC samples are compared to the criteria listed in Tables
B3-2 and B3-3.  These QC measurements are used to demonstrate acceptable
method performance and to trigger corrective action when control limits
are exceeded.

With every sample batch, a laboratory duplicate is analyzed.  The
precision within a sample batch is assessed by calculating a relative
percent difference (%RPD) between the sample and the duplicate  results.
 For target compounds with concentrations exceeding their PRQL, the %RPD
must comply with the criteria in Table B3-2.  If the %RPD is not within
the criteria, corrective action is taken.

Headspace Analytical Services also analyzes PDP blind audit samples.  If
notified that the precision of the PDP analyses is not acceptable,
corrective action will be taken.  Further analyses cannot be performed
until acceptable precision is demonstrated through additional replicate
analyses of a laboratory control sample, or acceptable analysis of
additional PDP samples.

B3-5c	Accuracy

Accuracy as %R is assessed for the headspace operations by analyzing PDP
blind-audit samples and laboratory control samples.  The results from
these QC measurements compared to the criteria listed in listed in Table
B3-2 and Table B3-3.  These QC measurements are used to demonstrate
acceptable method performance and to trigger corrective action when
control limits are exceeded.

The accuracy within a sample batch is assessed by calculating the %R for
the Laboratory Control Sample (LCS), which is analyzed with each batch
of samples.  The %R must comply with the criteria in Table B3-2.  If the
%R is not within the criteria, corrective action is taken.  Samples
associated with the poor LCS must be re-analyzed when the problem is
corrected, if the usability of the results was impacted by the poor LCS
recovery.

Headspace Analytical Services also analyzes PDP blind audit samples.  If
notified that the accuracy of the PDP analyses is not acceptable,
corrective action will be taken.  Further analyses cannot be performed
until acceptable accuracy is demonstrated through additional replicate
analyses of a laboratory control sample, or acceptable analysis of
additional PDP samples.

B3-5d	Calibration

GC/MS Tunes, initial calibrations, and continuing calibration are
performed as specified in procedures and evaluated to the criteria
specified in Table B3-3.  These procedures follow the guidance provided
in SW-846 Method 8260 and TO-14.  They include acceptance criteria and
corrective action to demonstrate that the calibration for an analytical
run is acceptable.  These criteria will be used to demonstrate
acceptable calibration and to trigger corrective action when control
limits are exceeded

B3-5e	Method Detection Limit

MDLs are expressed in ng for gas VOCs.  The method for determining the
MDLs is specified in procedures.  It is based upon the guidance provided
in B3-1.  MDLs will be determined prior to any samples being analyzed
and semi-annually thereafter.  The measured MDLs will be compared to the
required MDLs listed in Table B3-2.  If the MDLs are not met, corrective
action will be performed and the MDLs re-determined.  Analyses will not
proceed until the MDL criteria are met.

B3-5f	Program Required Quantitation Limit

Headspace Analytical Services meets the PRQL requirement by following
the analytical procedures.  At least one of the calibration standards is
set at a concentration less than the PRQLs listed in Table B3-2.  The
concentration of target analytes in the calibration standards is listed
in procedures.

B3-5g	Completeness

Analytical completeness shall be expressed as the number of samples
analyzed with valid results as a percent of the total number of samples
submitted for analysis.  Headspace procedures include strict QC controls
to ensure that valid results are obtained for all sample analyses.  The
QC controls are described in the headspace procedures and completeness
is checked and compared to the criteria listed in Table B3-2.  A
composite sample is treated as one sample for the purpose of
completeness, because only one sample is run through the analytical
instrument.  If the observed completeness is not compliant, corrective
action is taken.  Headspace Analytical Services will attempt to resolve
the problem causing the non-compliance.  If not possible, a
nonconformance will be written.

B3-5h	Comparability

Consistent use and application of uniform procedures (e.g., standardized
methods traceable standards, etc.) as specified in Section B1 of this
document, and application of data usability criteria [refer to EPA
540/R-99/008, USEPA Contract Laboratory Program National Functional
Guidelines for Organic Data Review (EPA 1999); and EPA 540-R-01-008,
USEPA Contract Laboratory Program National Functional Guidelines for
Inorganic Data Review (EPA 2002)] should ensure that analytical data are
comparable between different analytical facilities.  Headspace
Analalytical Services achieves comparability by following standardized
methods;

The analysis is performed by following headspace procedures.  These
procedures are based primarily upon SW-846 Method 8260, and meets the QC
requirements specified in Table B3-3 of this document.

Data package verification and validation is performed by following
procedure PRO-1669-HGAS-V&V, L-4053, or L-5017 which follow the process
outlined in B3-10 of the WAP.  Completeness is checked and compared
against the QAOs listed in Table B3-2.

Using traceable standards; As part of the headspace procedures Headspace
Analytical Services uses certified, traceable standards to prepare all
QC standards and solutions.  The source of standards is documented and
the certificates of analysis maintained in the certified standards
notebook.

Successful participation in the PDP.

B3-5i	Representativeness

For VOC analyses, representativeness for VOC samples is achieved by
collecting sufficient numbers of samples using a sampling manifold.
Sample collection is described in Section B1-1 of this document.

B3-5j	Method Performance Samples (MPS)

MPS are expressed in ng for gas VOCs.  The procedure for determining the
MPS is specified in L-4231, Headspace Gas Sampling and Analysis Using an
Automated Manifold; and PR0-1676-HGAS-S&A, Headspace Gas Sampling and
Analysis Using an On-Line Integrated System.  It is based upon the
guidance provided in Section B3-1.  MPS will be determined prior to any
samples being analyzed by L-42313 and PRO-1676-HGAS-S&A, and
semi-annually thereafter.  The measured MPS will be compared to the
required MPS listed in Table B3-2.  If the MPS are not met, corrective
action will be performed and the MPS re-determined.  Analyses will not
proceed until the MPS criteria are met.

B3-6	Total Volatile Organic Compound Analysis

B3-6a	Quality Assurance Objectives

The QAOs for the TWCP are listed in Table B3-4.  The specified QAOs
represent the required quality of data necessary to draw valid
conclusions regarding TWCP objectives.  Program-required limits, such as
the PRQLs associated with VOC analysis, are specified to ensure that the
analytical data collected satisfy the requirements of all data users.
Key data quality indicators for laboratory measurements are defined
below.  The methods to quantitatively and qualitatively assess these
indicators are discussed in Section B3 of this document.  Table B-1
contains a synopsis of the site-specific procedures used for total
volatile organic compound analysis.

Procedures implemented to ensure total volatile organic compound
analysis conducted at INEEL meets quality assurance objectives are
described in the Attachment to the SOW for the INEEL TWCP (DOE 2003a).

B3-6b	Precision

Precision is assessed through the analysis of laboratory duplicates or
matrix spike duplicates, replicate analyses of laboratory control
samples, and PDP blind-audit samples.  The results of QC samples are
compared to the criteria listed in Tables B3-4 and B3-5.  These QC
measurements are used to demonstrate acceptable method performance and
to trigger corrective action when control limits are exceeded.

Initially, precision is assessed prior to using the analytical procedure
L-4165, GC/MS Determination of Volatile Organic Compounds (Solids,
Liquids, and TCLP Extracts) (referred to in this section as L-4165) for
WIPP samples by analyzing a minimum of 7 replicate method performance
samples.  The percent Relative Standard Deviation (%RSD) is calculated
for the replicate analyses and compared to the precision criteria in
Table B3-4.  The %RSD must comply with the criteria before the procedure
can be used to analyze WIPP samples.  These initial analyses fulfill the
requirement for “Method Performance Samples” listed in Table B3-5.

With every sample batch, a MS/MSD sample pair is analyzed.  The
precision within a sample batch is assessed by calculating a relative
percent difference (%RPD) between the MS and MSD results.  The %RPD must
comply with the criteria in Table B3-4.  If the %RPD is not within the
criteria, corrective action is taken.  If the poor precision is traced
to the sample matrix, sample data is flagged with a “Z”, as directed
in WAP Section B3-10 (a nonconformance report is not required when the
problem is traced to the matrix, as specified in Table B3-5).

As stated in Table B3-5, a separate laboratory duplicate analysis is not
required when a MS/MSD pair is analyzed; hence laboratory duplicates are
not used to assess precision.

Replicate low-level method performance samples are analyzed
semi-annually to update MDLs.  The %RSD for the analyses is calculated.
The %RSD must comply with the criteria in Table B3-4.  If the precision
is not acceptable, the cause of the poor precision must be determined
and corrective action performed.  Further analyses cannot be performed
until acceptable precision is demonstrated through additional replicate
analyses of method performance samples (a minimum of four analyses).
These analyses fulfill the requirement for “Method Performance
Samples” listed in Table B3-5.

The laboratory also analyzes PDP blind audit samples.  If notified that
the precision of the PDP analyses is not acceptable, corrective action
will be taken.  Further analyses cannot be performed until acceptable
precision is demonstrated through additional replicate analyses of a
laboratory control sample, or acceptable analysis of additional PDP
samples.

B3-6c	Accuracy

Accuracy as %R is assessed for the laboratory operations by analyzing
laboratory control samples, matrix spikes, surrogate compounds, and PDP
blind-audit samples.  The results from these measurements for matrix
spikes samples are compared to the %R criteria listed in Table B3-4.
Results for surrogates and internal standards are evaluated as specified
in SW-846 or Table B3-5.  These QC measurements are used to demonstrate
acceptable method performance and to trigger corrective action when
control limits are exceeded.

Initially, accuracy is assessed prior to using the analytical procedure
L-4165 for WIPP samples by analyzing a minimum of seven replicate method
performance samples.  The average percent recovery (%R) is calculated
for the replicate analyses and compared to the accuracy criteria in
Table B3-4.  The %R must comply with the criteria before the procedure
can be used to analyze WIPP samples.  These initial analyses fulfill the
requirement for “Method Performance Samples” listed in Table B3-5.

With every sample batch, a MS/MSD sample pair is analyzed.  Additionally
System Monitoring Compounds (SMC) are added to every sample.  The
accuracy within a sample batch is assessed by calculating the %R for the
MS and MSD results, and the accuracy within a sample is assessed by
calculating the %R for the SMC compounds.  The %R must comply with the
criteria in Table B3-4.  If a %R is not within the criteria, corrective
action is taken.  If the poor accuracy is traced to the sample matrix,
sample data is flagged with a “Z”, as directed in WAP Section B3-10
(a nonconformance report is not required when the problem is traced to
the matrix, as specified in Table B3-5).

The accuracy within a sample batch is also assessed by calculating the
%R for the LCS, which is analyzed with each batch of samples.  The %R
must comply with the criteria in Table B3-4.  If the %R is not within
the criteria, corrective action is taken.  Samples associated with the
poor LCS must be re-analyzed when the problem is corrected, if the
usability of the results was impacted by the poor LCS recovery.

Replicate low-level method performance samples are analyzed
semi-annually to update MDLs.  The average %R for the analyses is
calculated.  The %R must comply with the criteria in Table B3-4.  If the
accuracy is not acceptable, the cause of the poor accuracy must be
determined and corrective action performed.  Further analyses cannot be
performed until acceptable accuracy is demonstrated through additional
replicate analyses of method performance samples (a minimum of four
analyses).  These analyses fulfill the requirement for “Method
Performance Samples” listed in Table B3-5.

The laboratory also analyzes PDP blind audit samples.  If notified that
the accuracy of the PDP analyses is not acceptable, corrective action
will be taken.  Further analyses cannot be performed until acceptable
accuracy is demonstrated through additional replicate analyses of a
laboratory control sample, or acceptable analysis of additional PDP
samples.

Laboratory  blanks shall be assessed to determine possible laboratory
contamination and are evaluated as specified in Table B3-5.  These QC
measurements will be used to demonstrate acceptable levels of laboratory
contamination and to trigger corrective action when control limits are
exceeded.

B3-6d	Calibration

GC/MS Tunes, initial calibrations, and continuing calibration are
performed as specified in L-4165.  L-41651 follows the guidance provided
in SW-846 Method 8260.  It includes acceptance criteria and corrective
action to demonstrate that the calibration for an analytical run is
acceptable as specified in Table B3-5 and SW-846.

B3-6e	Method Detection Limit

MDLs are expressed in mg/kg for VOCs.  The procedure for determining the
MDLs is specified in L-41651, Section 5.10.  It is based upon the
guidance provided in SW-846.  MDLs will be determined prior to any
samples being analyzed by L-41651.  The measured MDLs will be compared
to the required MDLs listed in Table B3-4.  If the MDLs are not met,
corrective action will be performed and the MDLs re-determined.
Analyses will not proceed until the MDL criteria are met.

B3-6f	Program Required Quantitation Limit

The laboratory meets the PRQL requirement by following the analytical
procedure L-41651.  At least one of the calibration standards is set at
a concentration less than the PRQLs listed in Table B3-4.  The
concentration of target analytes in the calibration standards is listed
in Section 4 of L-41651.  The concentration of the continuing
calibration standard is also less than the PRQL, as specified in the
same section.

B3-6g	Completeness

Laboratory completeness shall be expressed as the number of samples
analyzed with valid results as a percent of the total number of samples
submitted for analysis.  Valid results are defined as results that meet
the data useability criteria based upon application of the Quality
Control Criteria specified in Tables B3-4 and B3-5 and meet the
calibration, detection limit, representativeness, and comparability
criteria within this section.  Laboratory procedure L-41651 includes
strict QC controls to ensure that valid results are obtained for all
sample analyses.  The QC controls are described in the laboratory
procedure.  During the validation of Batch Data Reports by procedure
L-4038, WIPP Data Review and Validation for Volatile Organic Compounds1
(referred to in this section as L-4038), completeness is checked and
compared to the criteria listed in Table B3-4.  If the observed
completeness is not compliant, corrective action is taken.  The
laboratory will attempt to resolve the problem causing the
non-compliance.  If not possible, a nonconformance will be written.

For RFETS waste analyzed at INEEL, laboratory completeness is evaluated
by the RFETS TWCP Site PQAO.  If the observed completeness is not
compliant, corrective action is taken.

B3-6h	Comparability

Consistent use and application of uniform procedures (e.g., standardized
methods traceable standards, etc.) as specified in Section B1 of this
document, and application of data usability criteria [refer to EPA
540/R-99/008, USEPA Contract Laboratory Program National Functional
Guidelines for Organic Data Review (EPA 1999); and EPA 540-R-01-008,
USEPA Contract Laboratory Program National Functional Guidelines for
Inorganic Data Review (EPA 2002)] should ensure that analytical data are
comparable between different analytical facilities.

The laboratory achieves comparability by following standardized methods:

The laboratory sample preparation and analysis is performed by following
procedures L-4165.  This procedure is based upon SW-846 Methods 5030 and
8260 and meets the QC requirements listed in Table B3-5.  The most
recent promulgated version of SW-846 may be used.  Changes to SW-846
methodology that result in the elimination of sample preparation or
analytical methods in use at RFETS are addressed as a corrective action
to address the comparability of data before and after the SW-846
modification.

Batch Data Report verification and validation is performed by following
procedure L-40381, which follows the process outlined in B3-10 of the
WAP.  Completeness is checked and compared against the QAOs listed in
Table B3-4.

Using traceable standards;  As part of the procedure L-41651 the
laboratory uses certified, traceable standards to prepare all QC
standards and solutions.  The source of standards is documented and the
certificates of analysis maintained in the certified standards notebook.

Successful participation in the PDP.

B3-6i	Representativeness

Representativeness for VOC analysis is achieved by collecting unbiased
samples in accordance with Section B1.

B3-7	Total Semivolatile Organic Compound Analysis

B3-7a	Quality Assurance Objectives

The QAOs for the TWCP are listed in Table B3-6.  The specified QAOs
represent the required quality of data necessary to draw valid
conclusions regarding TWCP objectives.  Program-required limits, such as
the PRQLs associated with SVOC analysis, are specified to ensure that
the analytical data collected satisfy the requirements of all data
users.  Key data quality indicators for laboratory measurements are
defined below.  The methods to quantitatively and qualitatively assess
these indicators are discussed in Section B3 of this document.  Table
B-1 contains a synopsis of the site-specific procedures used for total
semivolatile organic compound analysis.

Procedures implemented to ensure total semivolatile organic compound
analysis conducted at INEEL meets quality assurance objectives are
described in the Attachment to the SOW for the INEEL TWCP (DOE 2003a).

B3-7b	Precision

Precision is assessed through the analysis of laboratory duplicates or
matrix spike duplicates, replicate analyses of laboratory control
samples, and PDP blind-audit samples.  The results of QC samples are
compared to the criteria listed in Tables B3-6 and B3-7.  These QC
measurements are used to demonstrate acceptable method performance and
to trigger corrective action when control limits are exceeded.

Initially, precision is assessed prior to using the analytical procedure
L-4215, GC/MS Determination of Total SVOCs for WIPP (referred to in this
section as L-4215) for WIPP samples by analyzing a minimum of 7
replicate method performance samples.  The percent Relative Standard
Deviation (%RSD) is calculated for the replicate analyses and compared
to the precision criteria in Table B3-6.  The %RSD must comply with the
criteria before the procedure can be used to analyze WIPP samples.
These initial analyses fulfill the requirement for “Method Performance
Samples” listed in Table B3-7.

With every sample batch, a MS/MSD sample pair is analyzed.  The
precision within a sample batch is assessed by calculating a relative
percent difference (%RPD) between the MS and MSD results.  The %RPD must
comply with the criteria in Table B3-6.  If the %RPD is not within the
criteria, corrective action is taken.  If the poor precision is traced
to the sample matrix, sample data is flagged with a “Z”, as directed
in WAP Section B3-10 (a nonconformance report is not required when the
problem is traced to the matrix, as specified in Table B3-7).

As stated in Table B3-7, a separate laboratory duplicate analysis is not
required when a MS/MSD pair is analyzed; hence laboratory duplicates are
not used to assess precision.

Replicate low-level method performance samples are analyzed
semi-annually to update MDLs.  The %RSD for the analyses is calculated.
The %RSD must comply with the criteria in Table B3-6.  If the precision
is not acceptable, the cause of the poor precision must be determined
and corrective action performed.  Further analyses cannot be performed
until acceptable precision is demonstrated through additional replicate
analyses of method performance samples (a minimum of four analyses).
These analyses fulfill the requirement for “Method Performance
Samples” listed in Table B3-7.

The laboratory also analyzes PDP blind audit samples.  If notified that
the precision of the PDP analyses is not acceptable, corrective action
will be taken.  Further analyses cannot be performed until acceptable
precision is demonstrated through additional replicate analyses of a
laboratory control sample, or acceptable analysis of additional PDP
samples.

B3-7c	Accuracy

Accuracy as %R is assessed for the laboratory operations by analyzing
laboratory control samples, matrix spikes, surrogate compounds, and PDP
blind-audit samples.  The results from these measurements for matrix
spikes samples are compared to the %R criteria listed in Table B3-6.
Results for surrogates and internal standards are evaluated as specified
in SW-846 method (EPA 1996) or Table B3-7.  These QC measurements are
used to demonstrate acceptable method performance and to trigger
corrective action when control limits are exceeded.

Initially, accuracy is assessed prior to using the analytical procedure
L-4215 for WIPP samples by analyzing a minimum of seven replicate method
performance samples.  The average percent recovery (%R) is calculated
for the replicate analyses and compared to the accuracy criteria in
Table B3-6.  The %R must comply with the criteria before the procedure
can be used to analyze WIPP samples.  These initial analyses fulfill the
requirement for “Method Performance Samples” listed in Table B3-7.

With every sample batch, a MS/MSD sample pair is analyzed.  Additionally
System Monitoring Compounds (SMC) are added to every sample.  The
accuracy within a sample batch is assessed by calculating the %R for the
MS and MSD results, and the accuracy within a sample is assessed by
calculating the %R for the SMC compounds.  The %R must comply with the
criteria in Table B3-6.  If a %R is not within the criteria, corrective
action is taken.  If the poor accuracy is traced to the sample matrix,
sample data is flagged with a “Z”, as directed in WAP Section B3-10
(a nonconformance report is not required when the problem is traced to
the matrix, as specified in Table B3-7).

The accuracy within a sample batch is also assessed by calculating the
%R for the LCS, which is analyzed with each batch of samples.  The %R
must comply with the criteria in Table B3-6.  If the %R is not within
the criteria, corrective action is taken.  Samples associated with the
poor LCS must be re-analyzed when the problem is corrected, if the
usability of the results was impacted by the poor LCS recovery.

Replicate low-level method performance samples are analyzed
semi-annually to update MDLs.  The average %R for the analyses is
calculated.  The %R must comply with the criteria in Table B3-6.  If the
accuracy is not acceptable, the cause of the poor accuracy must be
determined and corrective action performed.  Further analyses cannot be
performed until acceptable accuracy is demonstrated through additional
replicate analyses of method performance samples (a minimum of four
analyses).  These analyses fulfill the requirement for “Method
Performance Samples” listed in Table B3-7.

The laboratory also analyzes PDP blind audit samples.  If notified that
the accuracy of the PDP analyses is not acceptable, corrective action
will be taken.  Further analyses cannot be performed until acceptable
accuracy is demonstrated through additional replicate analyses of a
laboratory control sample, or acceptable analysis of additional PDP
samples.

Laboratory blanks shall be assessed to determine possible laboratory
contamination and are evaluated as specified in Table B3-7.  These QC
measurements will be used to demonstrate acceptable levels of laboratory
contamination and to trigger corrective action when control limits are
exceeded.

B3-7d	Calibration

GC/MS tunes, initial calibrations, and continuing calibrations are
performed and evaluated using the procedures and criteria specified in
Table B3-6 and Table B3-7.  These criteria are used to demonstrate
acceptable calibration and to trigger corrective action when control
limits are exceeded.

GC/MS tunes, initial calibrations, and continuing calibration are
performed as specified in L-4215 (SVOCs).  L-42151 follows the guidance
provided in SW-846 Method 8270and includes acceptance criteria and
corrective actions to demonstrate that the calibration for an analytical
run is acceptable.

B3-7e	Method Detection Limit

MDLs are expressed in mg/kg for SVOCs.  MDLs are calculated based upon
the guidance provided in SW-846.  Low-level method performance samples
are prepared and analyzed as directed in L-4214, Extraction of Total
SVOCs for GC/MS Analysis for WIPP1; and L-42151.  The data is reduced
and MDLs are calculated using SQA-validated software (SVOC-01-A1).  The
MDLs are determined prior to any samples being analyzed by L-42151, and
annually thereafter.  The measured MDLs will be compared to the required
MDLs listed in Table B3-6.  If the MDLs are not met, corrective action
will be performed and the MDLs re-determined.  Analyses will not proceed
until the MDL criteria are met.

B3-7f	Program Required Quantitation Limit

The laboratory meets the PRQL requirement by following the analytical
procedure L-42151.  At least one of the calibration standards is set at
a concentration less than the PRQLs listed in Table B3-6.  The