Attachment G

Quality Assurance  

Project Plan

   
Quality Assurance Project Plan

for Periodic Analytical Evaluation

of Delisted Waste

Project/Task Description

The requirements of this QAPP will be implemented to support periodic sampling and analysis of

delisted waste at the ConocoPhillips Refinery in Billings, Montana.  Sludge contained in two storm water

tanks will be processed (de‐oiled/dewatered using a filter press and/or a portable centrifuge).  The filter

pressed material will then be stored in roll‐off containers.   Once the sludge processing is completed,

samples of the waste material representing  each roll‐off bin will be composited as described below  The

composite waste samples will be submitted for laboratory analysis according to the requirements of this

QAPP.  During each clean out event, four composite samples and one field duplicate will be submitted

for analysis.

Reported concentrations must be less than the values presented in Table QA‐1.  If none of the detected

concentrations are greater than the values in Table QA‐1, then the waste material in all roll‐off

containers meets the listing criteria and may be disposed in a Subtitle D landfill.  If any concentration is

greater than the value in Table QA‐1, then a second round of sample collection (consisting of one

sample and one field duplicate) will be performed for the associated roll‐off boxe(s) and the samples

analyzed only for the constituent(s) exceeding the maximum value in the initial analysis.  If the results

from the second round of sampling are less than the value presented in Table QA‐1, then the initial

concentration is not confirmed and the material may be disposed in a Subtitle D landfill.  If the results

from the second round of sampling are greater than the value presented in Table QA‐1, then the original

result is confirmed and the material does not meet the delisting criteria.

Quality Objectives and Criteria

The following general requirements will ensure the quality of the analytical data:

• All quality control (QC) procedures specified in utilized analytical methods must be performed.

• Laboratory‐derived control limits must be reviewed at least annually and updated as

appropriate.

• The laboratory must spike, as appropriate, all target analytes.

The primary objective is to accurately determine the representative concentration of constituents in

samples of the delisted waste.  Samples will be collected and analyzed to support these objectives.  The

overall quality objective is to develop and implement procedures for sampling, chain‐of‐custody,

analysis, and reporting that will provide scientifically valid results that are sufficient to meet data quality

objectives (DQOs).  In order to ensure that the analytical methodologies are capable of achieving the

DQOs, measurement performance criteria have been set for the analytical measurements in terms of

accuracy, precision, representativeness, completeness, sensitivity, and comparability.  All measurement
performance criteria have been established for each parameter in order to ensure that the data are

sound, highly defensible, and with sufficiently low quantitation limits to meet objectives.

Accuracy – Accuracy (bias) is the closeness of agreement between an observed value and an accepted

reference value. The difference between the observed value and the reference value includes

components of both systematic error and random error.  Accuracy will be assessed through the analysis

of method blanks.

Method blank results will indicate any adverse effects of sample contamination from an outside source

(i.e., sample preparation or sample analysis) that could result in a positive bias.

Precision – Precision is the agreement among a set of replicate measurements without consideration of

the “true” or accurate value (i.e., variability between measurements of the same material for the same

analyte).   Precision will be assessed through the collection and measurement of field duplicates (one

extra sample collected as close in space and time as the original field sample).   

One field duplicate will be collected and submitted for analysis during each storm water tank clean out

event.  Precision will be measured through the calculation of relative percent difference (RPD).   Field

duplicate RPDs must be <30% for site samples.  These criteria apply only if the sample and/or duplicate

results are greater than five times the reporting limit; if both results are less than five times the

reporting limit, the criterion will be doubled.

Representativeness – Representativeness is a qualitative parameter which expresses the degree to

which the data and sampling design accurately and precisely represent a characteristic of a population,

parameter variations at a sampling point, a process condition, or an environmental condition within a

defined spatial and/or temporal boundary.  Representativeness is dependent upon the proper design of

the sampling program and the laboratory QC program.

Representativeness may also be assessed by the use of field duplicate samples.    By definition, field

duplicate samples are collected so that they are equally representative of a given point in space and

time.  In this way, they provide both precision and representativeness information.  As stated previously,

field duplicate samples will be collected at a frequency of one per event.  Following approved Standard

Operating Procedures (SOPs), appropriate site selection, sampling all pertinent media, proper sample

homogenization procedures, proper sample preservation procedures, using experienced/trained

sampling crews, and conducting field audits, if required will maximize representativeness in the field.

Using the proper analytical procedures, appropriate methods, and meeting sample holding times ensure

representativeness in the laboratory.

Completeness – Completeness is a measure of the amount of valid data obtained from a measurement

system compared to the amount that are planned.   

Field completeness is a measure of the amount of valid measurements obtained from all of the

measurements taken in the project and valid samples collected.    The field completeness objective is
greater than 90 percent.    This allows for the potential loss of samples due to sampling problems or

bottle breakage during transport.

Laboratory completeness is a measure of the number of valid measurements obtained from all valid

samples submitted to the laboratory.  The laboratory completeness objective is greater than 95 percent.

This allows for the potential loss of samples impossible to analyze due to unforeseen interferences and

rejected data following data validation.

Reporting Limits – Sensitivity is the ability of the method or the instrument to detect the contaminants

of concern at the level of interest (i.e., having adequate reporting limits).  The project‐required reporting

limits for each contaminant of concern are summarized in Table QA‐2.  Laboratory reporting limits must

be at or below the required reporting limit for each parameter.

Comparability – Comparability is a qualitative parameter that expresses the confidence with which one

data set can be compared to another.

Comparability depends on the proper design of the sampling program and will be satisfied by ensuring

that QAPP requirements are followed as well as those in approved, accepted SOPs.  Other measures to

ensure comparability in the field are the use of proper sampling and preservation techniques.

Comparability depends on the use of recognized USEPA or equivalent analytical methods, the reporting

of data in standardized units, using accepted rules for rounding values, and by reporting data in a

standard format.   

Sample Collection Locations and Procedure

Once processed, material is gathered in a dump box which is then transferred to a nearby roll‐off bin.  

Approximately two dump box loads of processed material are generated per filter‐press run.  Roughly

six to eight dump box loads are required to fill a 20 yd3 roll‐of bin.

Individual grab samples of the processed material (the waste) will be collected from alternating dump

box loads prior to placement in roll‐off containers.  Samples will be placed into glass jars with Teflon‐

lined closures and will be stored under refrigeration (< 6°C) for future compositing after all the sludge

has been processed.  Sample containers will be filled completely with no headspace.  Containers will be

labeled with the date collected, sampler’s identification, and receiving roll‐off bin identifier.  When the

clean‐out    campaign is complete, the individual grab samples from the jars will be allocated and

composited to make four samples and one duplicate for laboratory analysis.  The composite samples will

be prepared to represent the contents of one or more roll‐off boxes, depending on the number of

resulting boxes.  Each campaign will be represented by four composite samples and one field duplicate.   

Sample Shipment

A completed COC form will accompany samples during each step of custody transfer and shipment.  

When physical possession of samples is transferred, both the individual relinquishing the samples and

the individual receiving them will sign, date, and record the time on the COC form.  In the case of sample
shipment by an overnight courier, a properly prepared air bill (waybill) will serve as an extension of the

COC form while the samples are in transit.

The following steps must be followed when packing environmental samples for shipment by air:

1. Select a sturdy cooler in good condition.  Secure and tape the drain plug with duct tape.

2. Ensure the caps on all bottles are tight (will not leak); check to see that labels and chain‐of‐

custody records are completed properly.

3. Place all bottles in separate and appropriately sized plastic zip‐top bags and close the bags.  

Bottles may be wrapped in bubble wrap.  It is preferable to place glass sample bottles and

jars into the cooler vertically.  Due to the strength properties of a glass container, there is

much less chance for breakage when the container is packed vertically rather than

horizontally.

4. Place two to four inches of packing peanuts, vermiculite, or other cushioning material into

the bag in the cooler and then place the bottles and cans in the bag with sufficient space to

allow for the addition of more packing peanuts or vermiculite between the bottles and cans.

5. Put ice in large plastic zip‐top bags and properly seal.  Place these ice bags on top of and

between the samples.  Fill all remaining space between the bottles or cans with packing

peanuts, bubble wrap, or vermiculite.

6. Place the completed Chain‐of‐Custody Record into a plastic zip‐top bag, tape the bag to the

inner side of the cooler’s lid, and then close the cooler.

7. Wrap strapping tape around each end of the cooler two times, and completed custody seals

affixed to the top on adjacent sides of the cooler.  Place the custody seals so that the cooler

cannot be opened without breaking the seal.  Place clear shipping tape over the custody

seals.

8. A label containing the name and address of the shipper shall be placed on the outside of the

container, preferably using a handle‐tag or secured with extra tape across the top of the

cooler.

Toxicity Characteristic Leaching Procedure (TCLP)

Samples will be analyzed for both total and TCLP volatiles, semivolatiles, and metals. Regarding TCLP

analyses, all samples will be extracted using the appropriate extraction fluid as determined using TCLP

method (SW846 Method 1311) criteria and procedures. Additionally, all samples for metals analyses will

be extracted using extraction fluids with pH values of 7.0 and 10.1 (as noted in delisting guidance

documents). The laboratory must be contacted well in advance of receiving samples to discuss the

generation and use of these non‐standard extraction fluids.
The extraction fluid with a neutral pH is described in Method 1311, Section 5.2 as reagent water and has

a pH of 7.0 ± 0.5 standard units.

The extraction fluid with an alkaline pH is described in Standard Methods for the Examination of Water

and Wastewater.  It is prepared by mixing 2.092 grams of 0.025 molar sodium bicarbonate (NaHCO3)

and 2.640 grams of 0.025 molar sodium carbonate in 1000 mL aqueous solution at 25°C.  This solution

must have a pH of 10.01 ± 0.05 standard units.
Table QA-1. Maximum Concentrations for Future Analytical Results 

Analyte 

Maximum Total 

Concentration (mg/kg) 

Maximum TCLP 

Concentration (mg/L) 

Cyanide -- 110 

Antimony -- 3.83 

Arsenic 54,100 0.301 

Barium -- 1,280 

Cadmium 204,000 3.25 

Chromium 197,000 63.8 

Cobalt 262,000 7.34 

Lead -- 18.7 

Mercury 72.6 2.42 

Nickel -- 480 

Selenium -- 31 

Silver -- 242 

Vanadium -- 117 

Zinc -- 7,230 

2-Methylphenol -- 103 

3&4-Methylphenol -- 1,030 

Phenol -- 6,190 

Acenaphthene -- 379 

Anthracene -- 924 

Benzo(a)anthracene 2,970 2.5 

Benzo(a)pyrene 220 939 

Benzo(b)fluoranthene 1,730 7,990 

Benzo(k)fluoranthene 20,500 -- 

Chrysene 291,000 250 

Dibenz(a,h)anthracene 232 -- 

Fluoranthene 745,000 87.8 

Fluorene -- 175 

Indeno(1,2,3-cd)pyrene 5,470 -- 

Naphthalene -- 1.17 

Pyrene -- 159 

2-Butanone -- 12,400 

Benzene -- 2.75 

Carbon disulfide -- 2,010 

Ethylbenzene -- 387 

Tetrachloroethene 75,800 0.729 

Toluene -- 539 

Trichloroethene -- 2.76 

Xylenes, total -- 341 

-- DRAS Maximum Allowable Concentration is greater than one million parts per 

million. 

Note: Di-n-octyl phthalate, phenanthrene, and bis(2-ethylhexyl) phthalate were 

detected in the analyses included in this petition; however, maximum concentrations are 

listed as “Not Applicable” for phenanthrene while both maximum concentrations are 

greater than one million parts per million for di-n-octyl phthalate and bis(2-ethylhexyl) 

phthalate in the DRAS output. 
Table QA-2. Measurement Performance Specifications 

Analyte Method

Total Target

Reporting Limit

(mg/kg)1

Total

LCS/LSCD MS/MSD

%R RPD %R RPD

Antimony

6010;

6020

0.5 75‐125 25 70‐130 30

Arsenic 0.5 75‐125 25 70‐130 30

Barium 0.5 75‐125 25 70‐130 30

Cadmium 0.5 75‐125 25 70‐130 30

Chromium 0.5 75‐125 25 70‐130 30

Cobalt 0.5 75‐125 25 70‐130 30

Lead 0.5 75‐125 25 70‐130 30

Nickel 0.5 75‐125 25 70‐130 30

Selenium 0.5 75‐125 25 70‐130 30

Silver 0.5 75‐125 25 70‐130 30

Vanadium 0.5 75‐125 25 70‐130 30

Zinc 0.5 75‐125 25 70‐130 30

Mercury 7471 0.005 75‐125 25 70‐130 30

Benzene

8260

0.005 75‐125 25 70‐130 30

Carbon disulfide 0.010 75‐125 25 70‐130 30

Ethylbenzene 0.005 75‐125 25 70‐130 30

Methyl ethyl ketone 0.010 75‐125 25 70‐130 30

Tetrachloroethylene 0.005 75‐125 25 70‐130 30

Toluene 0.005 75‐125 25 70‐130 30

Trichloroethylene 0.005 75‐125 25 70‐130 30

Xylenes (total) 0.005 75‐125 25 70‐130 30

Acenaphthene

8270

0.167 60‐120 25 50‐130 30

Anthracene 0.167 60‐120 25 50‐130 30

Benzo(a)anthracene 0.167 60‐120 25 50‐130 30

Benzo(a)pyrene 0.167 60‐120 25 50‐130 30

Benzo(b)fluoranthene 0.167 60‐120 25 50‐130 30

Benzo(k)fluoranthene 0.167 60‐120 25 50‐130 30

Chrysene 0.167 60‐120 25 50‐130 30

o, m, p‐Cresol 0.167 60‐120 25 50‐130 30

Dibenz(a,h)anthracene 0.167 60‐120 25 50‐130 30

Fluoranthene 0.167 60‐120 25 50‐130 30

Fluorene 0.167 60‐120 25 50‐130 30

Indeno(1,2,3‐cd)

pyrene

0.167 60‐120 25 50‐130 30

Naphthalene 0.167 60‐120 25 50‐130 30

Phenol 0.167 60‐120 25 50‐130 30

Pyrene 0.167 60‐120 25 50‐130 30 1

Reporting limits presented here represent ideal conditions. Actual limits will differ based on sample‐

specific factors (e.g., percent moisture, dilution factor, etc.).

2

Analysis can be performed using Method 8260 or Method 8270.
Table QA-3. Sample Handling Requirements 

Analyte Method

Typical

Containers1 Preservative Holding Time

Total and Amenable

Cyanide 9014; 9213 4 ounceGlass Cool to 4°C 14 days

Hexane‐Extractable

Material (Oil & Grease) 9071 4 ounceGlass Cool to 4°C 14 days

Metals 6010; 6020 4 ounce

Glass Cool to 4°C 180 days

Mercury 7471 4 ounce

Glass Cool to 4°C 28 days

Moisture Content ASTM D2216 4 ounce

Glass Cool to 4°C 28 days

pH 9045   4 ounce

Glass Cool to 4°C 7 days

Semivolatile Organics 8270 4 ounce

Glass Cool to 4°C

14 days to

extraction; 40

days from

extraction to

analysis

Volatile Organics 8260 4 or 8 ounce

Glass Cool to 4°C 14 days

Sulfide 9034; 9215 4 ounce

Glass

Cool to 4°C;

Zn Acetate

until surface

moistened

7 days

Reactive Sulfide SW‐846 Chapter

7

4 ounce

Glass Cool to 4°C 14 days

Reactive Cyanide SW‐846 Chapter

7

4 ounce

Glass Cool to 4°C 14 days

TCLP 1311a See Determinative Method

1 Containers presented here assume one sample for one method is being submitted for analysis. The

laboratory may use larger containers and/or use the material from one container for multiple methods.

Contact the laboratory for specific advice regarding containers.