s>EPA
United States
Environmental Protection
Agency
Region 5
Central Regional Lab
536 South Clark Street
Chicago. Illinois
January 1984
905R84112
State Agency Access
To The National
Contractor Laboratory
Program
QUALITY ASSURANCE
-. ' • . AMI*
DATA REVIEW
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STATE AGENCY ACCESS TO THE NATIONAL CONTRACTOR LABORATORY PROGRAM
Narrative Audio/Slide Presentation
(SLIDE 1)
Hello and welcome to the Region V training program whlcn 1s Intended
to familiarize State Agency personnel with the requirements of the EPA
Contractor Laboratory Program herein referred to as the CLP or NCLP. "N"
stands for National.
I am Chuck Elly, Sample Analysis Coordinator for the EPA Region V,
Central Regional Laboratory (CRL), Chicago.
I have prepared slides which, if followed, samplers would have all of
the information necessary to successfully sample, maintain custody, complete
forms and send samples to National Contractor Laboratories.
Additional slides were prepared by Ms. Marcia Kuehl, Region V, CRL
Quality Control Coordinator and will acquaint you with the elements
necessary to successfully review data generated by the National Contractor
Laboratories.
(SLIDE 2, 3)
These slides are intended to Illustrate the mass of paperwork generated
by the program, that doesn't mean that 1t 1s bad however. That's a picture
of me in my office.
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(SLIDE 4)
ELIGIBILITY REQUIREMENTS: 1) Samples collected must be from a Superfund
Site or potential Superfund site; 2) States must have a cooperative
agreement with EPA, Remedial Response Branch or permission from a Remedial
Response official. (This is also known as the 3012 Program.)
(SLIDE 5)
REQUESTING PROTOCOL
1. The first step is to submit a study plan to the U.S. EPA, On-Scene
Coordinator (OSC) the Remedial Response Branch.
2. Case set-up is with the EPA, Sample Management Office (called the SMO)
which I am responsible for. State personnel will eventually be delegated
this task.
3. Shipping requirements are the responsibilities of State personnel, and
are explained in later slides.
4. Quality assurance and data review are the responsibility of State
samplers and reviewers, and will be explained in detail by Marcia Kuehl.
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(SLIDE 6)
STUDY PLAN REQUIREMENTS
1. The Information shown here are the items which absolutely must be
Included in the plan submitted to the EPA, OSC.
A. Number of samples (add to this blanks and duplicates).
8. Parameters (such as Priority Pollutant organics, Task 1&2 Metals,
etc.). I will explain the term Task 1 and 2 Metals on later slides.
C. Matrix types (water, soil/sediment, oil, fish, tissue).
0. Concentration level (low, medium, high - these are contractor
terms and I will explain these later also).
E. Survey type (Routine or SAS - routine means standard priority
pollutant organics, Task 1, 2, or 3 inorganics with a turnaround time
of 30 days). SAS stands for Special Analytical Services - and will be
explained on later slides.
F. Shipment date (this must be firm, since National Contractor Labs
are reserved by date).
6. Order for bottles - cleaned bottles are available through the CLP.
It takes 3 to 5 weeks after I send the order in for routine requests.
Emergency orders can be telephoned in and speeds up the time
substantially.
H. SAS Request, if applicable (I have prepared 3 slides which will
show you the required information) if necessary. SAS's should be very
infrequent. They help to use up the routine lab capacity.
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(SLIDE 7)
1. OSC sends study plan to Chuck Elly.
2. Elly reviews study plan.
3. If Elly has comments, OSC negotiates differences with State contact
person.
4. If no comments, Elly sends copy of approved study plan to OSC.
5. Elly sets up case with SMO.
6. Elly telephones information to designated State contact and approves
SAS request (if any).
7. Elly sends SMO forms and returns copy of bottle order form to designated
State contact. Note that only one State person should be the designated
contact with Elly.
(SLIDE 8) .
When are SAS's required?
1. For atypical matrices such as oils and tissues.
2. Faster turnaround times than 30 days.
3. Parameters other than the 114 Priority Pollutant Organics or the Task
1, 2, or 3 Inorganics are requested.
4. Lower detection limits or more extensive quality control than in the
regular IF3s are requested. (IFBs stand for Invitation to Bid.)
5. Dioxins/Furans are requested.
6. EP Toxicity, Flashpoint, or other RCRA solid waste parameters are
requested.
7. Items not mentioned above are requested.
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(SLIDE 9)
Sample Descriptions;
These are terms, defined in the contract which must, repeat must, be
placed on the traffic forms, since National Contractor Labs have contracts
based on concentration levels. Definitions will be given on later slides.
1. Low
2. Medium
3. High
(SLIDE 10)
Orgam'cs Analysis Data Sheet II
This is the top sheet of the three page analysis from which contains
the priority pollutant acids, base neutral and volatile compounds. (Consult
Appendix C of the SMO Users Guide to the EPA Contractor Laboratroy Program.)
The upper right hand corner will contain the laboratory traffic number.
Results are generally reported in micrograms per liter (ppb) for waters and
micrograms per gram (ppm) for soil/sediment.
(SLIDE 11)
Organics Analysis Data Sheet 12
This sheet includes- the chlorinated pesticides, PCBs, and non-priority
pollutant compounds. A third sheet is almost always included which contains
the tentatively Identified compounds; which Marcia Kuehl explains later.
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(SLIDE 12)
Inorganic Analysis Data Sheet
This is a one-page form which Includes all of the Task 1 and 2 Metals
and Task 3 parameters. Task 1 parameters are generally analyzed by
Inductively coupled argon plasma (ICAP) or atomic absorption (AA for short).
Task 2 Metals are those generally analyzed by flame!ess AA. Ammonia and
sulfide are SAS parameters. They used to be Task 3 parameters.
(SLIDE 13)
Definitions - Low Concentration Samples
A. 0-10 ppm of a single contaminant
B. Environmental soils and water samples, groundwaters, surface waters,
most off-site wastes, soils, wells, leachate springs, ditches, rivers
C. Any diluted samples
D. Low-hazard samples
(SLIDE 14)
Medium Concentration Samples
A. 10 ppm to 15% of a single contaminant
B. On-site water-soil samples, samples lying beside drums, lagoons, on-
site impoundments, leachate collection pools, on-site ditches
C. Areas of direct, but diluted concentrations
0. Medium-hazard samples
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(SLIDE 15)
High Concentration Samples
A. 15% to 100% of a single contaminant
8. Samples collected from drums, surface Impoundments, storage tanks,
spills or direct discharges from Impoundments l
C. Little or no evidence of dilution
D. High, unknown hazard
(SLIDE 16)
Sample Size and Preservation; Orgam'cs - Low Level:
A. Waters:
For Extractables: You must send two one-half gallon amber narrow neck
glass bottles with teflon-inserted cap and iced to
For Volatiles: Two 40-ml Borosilicate glass vials, each sample, iced
to 4°C.
B. Soils:
You must send one 8-ounce wide-mouth glass jar, with a teflon insert,
iced to 4°C for each sample.
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(SLIDE 17)
Sample Size and Preservation; Organics - Medium Level
A. Waters (Extractables and VOAs)
You may send four 32-ounce or eight 16-ounce wide-mouth glass bottles
with teflon-inserted caps for each sample. You will see later that the
bottles must be sent in one-half gallon paint cans.
8. Soils
You may send one 8-ounce wide-mouth glass bottle with teflon-inserted
cap for each sample. No preservative.
Medium soil samples also have to be sent in one-half gallon paint cans.
(SLIDE 18)
Orgam'cs and Inorganics - High Level
These include concentrated waters, liquids, soils, sludges, solids out
of drums.
You must send one 8-ounce wide-mouth glass bottle with teflon-inserted
cap for each sample. No preservative.
If EP Toxicity or Flashpoint is requested, you should send two 8-ounce
glass bottles.
Each sample must be sent in a one-half gallon paint can.
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(SLIDE 19)
Sample Size and Preservation; Task 1 and 2 Metals - Low level
A. Waters
You must send one, one-liter high density polyethylene bpttle
preserved with 3 ml of 1:1 HN03 or the sample must be preserved to a pH
of 2.
B. Cyanide
You may send one, one-liter or one 500 ml high density polyethylene
bottle for each sample preserved with 5 ml of six normal sodium hydroxide.
The sample must be iced to 4°C.
C. Soils
You may send one 8-ounce plastic or glass wide-mouth bottle for each
sample. The sample must be iced to 4°C.
(SLIDE 20)
Sample Size and Preservation; Inorganic - Medium Level
A. Water and Soils
1. Task 1 and 2 Metals
2. Cyanide
3. Ammonia
4. Sulfide
B. You must send one 8-ounce plastic or glass wide-mouth bottle for each
sample.
No preservative.
Each sample must be sent in a one-half gallon paint can.
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(SLIDE 21)
1. Routine
A. Low and medium soil and water samples; 30 days.
8. High concentration samples; 51 days (this Includes 21 days at the
EPA, National Enforcement Investigations Center Laboratory - Fred C. Hart
Associates Contractor, and 30 days at the National Contractor Laboratory).
2. Special Analytical Services (SAS)
A. Low and medium soil and water samples; 2 days to 30 days (a frequent
request is for 14 to 21 days.
3. High concentration samples; 5 days to 30 days.
(SLIDE 22)
Field Quality Control; Low and Medium Samples
You should send for each group of samples:
1. A Field Reagent blank containing distilled-dionized water for
inorganics (carbon-free water for organics). The reagent blank should
also contain a preservative. Example for low metals, you should send
one-liter of distilled-dionized water plus 3 ml of 1:1 HN03.
2. A duplicate of one of the samples in a batch.
High Hazard Samples
1. A reagent blank is not necessary.
2. But you should send a duplicate of one of the samples.
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(SLIDE 23)
For the Contract Laboratory Program, you must do the following.
1. Use U.S. EPA Chain-of-Custody forms and sample tags. Seals should
be used on the picnic coolers.
2. Every member of the sampling team must be listed on the Chain-of-
Custody form. •
3. Information on the sample tag and the cha1n-of-custody forms must
match.
4. Cha1n-of-Custody forms must be completed properly (as you will see
on the next slide).
5. The method of shipment should be listed in the lower right-hand
corner of the Chain-of-Custody form under "Remarks".
6. A separate chain-of-custody of custody form must be sent for each
site and for samples sent to each lab. (Generally one custody for
will be sent to the Organic Lab and one to the Inorganic Lab.
(SLIDE 24)
This 1s a picture of a Chain-of-Custody form.
The project number should contain either the partial or entire
laboratory sample number. An example of an EPA laboratory number is
"83-CY05S01". The Federal Fiscal Year 1984, started October 1, 1983, so
the 83 number becomes "84-CY05S01". Note the requirements for date, time,
and station location. Time may be either conventional or military. The
number of containers and the parameters requested per sample must be listed
clearly.
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(SLIDE 26)
This is a picture of a sample tag. One tag must be attached to each
bottle and should contain the laboratory number, date, time, names of
samplers, station location, parameters, and preservative (if any).
Note also that it is a good idea to 11st the traffic numbers from the
SMO traffic form. In this case it was organics as noted by the number E5123.
(SLIDE 27)
Sample Custody Tag (Address Side)
This is the reverse side of the tag. Note that the U.S. EPA Region V
Regional Office is the official address. The EPA, Region V Laboratory is
actually located at 536 South Clark Street, Chicago.
(SLIDE 28)
Official Seal
This is an illustration of the Region V Offical Seal which should be
secured. Transparent red or clear tape should be used over the seal. A
broken seal indicates that the cooler has been tampered with. If it was by
anyone other than the designated laboratory custodian, custody is broken.
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(SLIDE 29)
Forms required for shipment of samples to NCL's. (Note that Region V
will supply all forms.)
Low and Medium Samples
1. The SMO Organic Traffic report and the Inorganics Traffic report are
required for all routine sample requests. Illustrations of these forms are
shown on the next two slides.
2. Packing List form for SAS's, when the packing list is used on organic
and inorganic traffic forms is not required, unless the SAS also contains a
routine case request (seldom), I will indicate if a traffic form is required.
3. EPA Chain-of-Custody Form
4. EPA Sample Custody Tag.
5. EPA Custody Seal
6. Stick-on label from the Organics Traffic Form. Each traffic form
contains a stick-on label containing a laboratory number (such as E5000 for
organics and ME5104 for inorganics).
This label should be removed from the traffic form and placed on the
sample bottle. In some cases there are enough labels to put one on the
bottle and one on the sample custody tag.
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(SLIDE 30)
ORGANICS TRAFFIC REPORT
This form must accompany all samples for routine organics analysis.
Two very important items are: the case number and the concentration type.
If you make a mistake and check medium concentration when you meant low
concentration, the NCL will expect you to send four 32-ounce bottles
instead of two one-half gallon bottles. They will also note that you did
not send the samples in cans and possibly exposed them to hazards.
It is also a good idea to put your laboratory sample number somewhere
on the form. EPA samplers put it under the case number.
Other items, such as the National Contractor Laboratory address,
matrix type, number of sample bottles, sample description, and method of
shipment, must be completed.
The Special Handling Instructions column at the bottom of the form
should be used to note any hazards or other information related to the
sample.
(SLIDE 31)
INORGANICS TRAFFIC REPORT
This form must accompany all routine low and medium samples. It
contains the same information as the organics form except for the parameter.
At the bottom left-hand corner there is a statement which says "Matches
Organic Traffic Report No.XXXX.
It's a good idea to complete this column, because it helps to resolve
sample bottle mix-ups. And mix-ups do occur—believe me.
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(SLIDE 32)
FORMS REQUIRED FOR HIGH HAZARD SAMPLES
Don't forget these are samples generally out of drums and go to the
NEIC first for extraction and dilution then to National Contractor Labs for
analysis.
1. The SMO High Hazard Traffic Form (a packing list is sometimes required
when additional tests, such as HP Toxicity or Inorganics are requested).
2. Hazardous Waste Sample Preparation Request Form (a picture os this form
will be shown on the slide after the high hazard traffic form).
3. EPA Chain-of-Custody Form and Tag
4. The EPA, Region V Custody Seal
5. The stick-on label from the High Hazard Form
6. A Hazardous Shipping Certificate (a picture of the certificate is shown
in later slides.
(SLIDE 33)
HIGH HAZARD TRAFFIC REPORT
This form 1s very similar to the other reports, except that it is a
combined Organics/Inorganics form. It 1s very important to fill out the
known or suspected hazards column.
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(SLIDE 34)
THE HAZARDOUS SAMPLE PREPARATION REQUEST FORM
This sheet is very similar to the chain-of-custody form but must
accompany the Cha1n-of-Custody form and High Hazard sheet for each group of
samples. You may check any or all of the preparation fractions under the
column "Check Preparations Requested". The parameters you will get are:
Total Metals (similar to Tasks 1 and 2 Metals)
Total Mercury
Strong Acid Anions ($04 , Cl , N03 , F )
Volatile Organics
Base Neutrals, Acids, TCDD (Dioxins)
Pesticides, PC8s
Other
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(SLIDE 35)
PACKING LIST
This 1s a picture of the Packing List Form which must accompany all
samples analyzed under an SAS request. My name will always appear as»the
Regional Contact.
Note the SAS number in the top right-hand corner of the sheet.
In the left-hand corner you will see the sample number. The SMO
Coordinator prefers that you use sample numbers starting with 355E-1, E-2,
and continuing to the last sample such as 355E-4 in this case. You can put
up to 20 samples on each packing list. It is better to put your laboratroy
sample number under the additional "sample description" column and any
other pertinent information that you can fit on the sheet. Somewhere
towards the bottom of the sheet, you should Indicate your parameter request.
In this case the request was for PCBs only. (This means not the Pesticides/
PCB fraction, but only the PCS fraction.
At the bottom of the four-page form are instructions as to what copies
go where. (Two get shipped with the samples, one goes to SMO, one is kept
by the sampler, and the sampler sends one copy to me.)
(SLIDE 36)
REGIONAL REQUEST - SAS FORM
This three page form should be completed for all SAS's. This particular
SAS Involved the analysis of fish samples at Chem Dyne for Priority Pollutant
organics (no volatiles - volatiles can't be done in fish). The request
also was for the analysis of C-56 (which 1s hexachlorocyclopentadiene).
Note that % Lipids is a requirement for all fish. Item 2 requires
specification of the number of samples and matrix type or level concentration
for each sample. Items 3, 4, 5 require program specification and dates of
collection and shipment.
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(SLIDE 37)
Page 2 slides
Item 6 of the sheet requires the number of days to complete the sample
analyses. While Items 7, 8, 9 deal with the analytical protocols, special
technical Instructions and analytical results requirements (deliverables.
Item 7 for example stated to use the attached CRL Method for the
analysis of non-volatile extractable organic compounds, sections of the
method are referred to for % lipids, grinding and clean-up.
Item 8 of the form is for special instructions, i.e., for spiking with
various compounds, detection limits specification, etc.).
Item 9 we usually specify to report all raw QA/QC information inclusive
of re-constructed ion chromatograms, library searches, and computer
calculations. Instrument and method blanks must be specified and sent with
the data.
Item 10. "Other" column is used to state that detection limit
verification should be done by spiking at levels below the listed detection
limit of the method.
(SLIDE 38)
Page 3 of the form is a supplement to instructions on page 2. Data
requirements include the parameters, detection limit, and precision
requirements. While QC requirements Include the audits, frequency, and
limit requirements.
Item III is an invitation for the requestor to specify the quality of
data he can live with. In some cases, 1f audits are out-of-control a rerun
may not be necessary.
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(SLIDE 39)
DEPARTMENT OF TRANSPORTATION (DOT) SHIPPING REGULATIONS
These apply mainly to medium and high hazard samples. The bottles and
preservatives amounts for low samples are generally exempt from DOT
regulations.
1. Each sample bottle must be placed in a one-half or a one-gallon can
(generally paint cans are used).
2. Each sample bottle must be placed inside a plastic bag which can be
sealed.
3. Vermiculite or other absorbent material must be placed inside the can.
4. The paint can top must be sealed with five (5) clips or can be taped.
5. The NCL address and the hazard label must be put on each can.
6. A Hazardous Shipping certificate (also known as Shippers Certification
for restricted articles) must be completed for each group of samples sent.
7. The cans must be packed in a metallic or rigid plastic picnic cooler
which is able to withstand a 4-foot drop without breakage of samples.
The picnic cooler must be labeled with the following information.
1. EPA label
2. "THIS SIDE UP" labels (2)
3. "UP" arrow (4)
4. "DANGER" label
5. "FLAMMABLE SOLID" (or LIQUID)
6. "FLAMMABLE SOLID, N.O.S. (or LIQUID N.O.S.)
7. Laboratory address label
8. Number of samples in shipment
9. Number of cans in ice-chest.
(SLIDE 40)
Here's an illustration of a cooler that is ready to go, with all of the
labels.
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(SLIDE 41)
SHIPPERS CERTIFICATION FOR RESTRICTED ARTICLES
This is a picture of the Federal Express Form.
If you were shipping hazardous wastes for example, you would put the
following information on the form.
Flammable liquid, Flam Liq, NOS
Corrosive solid
Corrosive liquid, etc.
(SLIDE 42)
SMO SHIPPING REQUIREMENTS
This information is required by the Sample Management Office within 24
hours after samples are shipped. It is a good idea to do it the same day
of shipment.
You should telephone me at (312) 353-8370 with the following.
1. Carrier and Air Bill Number
2. The Case Number
3. The Laboratory the samples were shipped to
4. The date of shipment
5. The number of samples
6. The number of picnic coolers
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(SLIDE 43)
INTERNAL RECORDKEEPING
1. It is a good Idea to keep a log with the SMO Case Numbers after a case
has been set up. A picture of my log is shown on the next slide.
2. The Central Regional Laboratory data coordinator also maintains an
internal tracking sheet which tracks sample collection through data review.
I'll show you a picture of our sheet on a subsequent slide.
3. Raw data returned:
A. Unfortunately, I was unsuccessful in my request to have the data
send directly to the State requestor. It would mean a change in the
contract and SMO will not do it.
B. State Agency data will be sent to me and I will forward it
(unreviewed) to the State Agency Contact.
The additional information listed below is not in the slide-audio but
should be followed.
C. The State reviews its own data.
0. State Contact sends copies of all Data Review summaries to the
Regional NCL Coordinator.
E. State Contact refers all un-resolvable. non-routine QC problems to
the new Regional Deputy Project Officer (DPO). State Contact resolves
all routine QC problems.
F. NCL Coordinator refers the QC problem to the Regional DPO for the
laboratory which has the QC problem.
4. Return of picnic coolers.
This same procedure will be followed for the return of picnic coolers.
However, you can solve this problem by putting your return address and
stick-on labels on the coolers and they will be returned directly to you.
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(SLIDE 44)
VIAR CASE PLANNING LOG
This is a picture of the form which I use for pending and future cases.
After the data are received, I file this sheet. It includes the case
number, site name, originator, parameters, projected number of samples,
actual number of samples, projected shipmnet date, NCL, etc.
(SLIDE 45)
INTERNAL TRACKING SHEET
This is the most valuable document we have to track the whereabouts of
samples.
The sheet includes the following.
1. EPA Data Set (which is how we log samples in)
2. Decision Units/Activity Number (Superfund Projects are
Decision Units Y905 and Y306)
3. Case Number and/or SAS Number
4. Number of samples and parameters
5. National Contractor Laboratory
6. Date samples were shipped by the collector
7. Date the analysis results are done (31 days after shipment)
8. 1st arrival date of data results at the Central Regional Lab
9. Last arrival date (for which all data are in)
ID. Contractor turnaround time for analysis
11. Date of Data Analysis Review by the Central Regional Lab
chenri st
12. Date the data were sent to the Data User
13. Time (in hours) it took the chemist to review the data
14. The turnaround time it took from the time the data arrived at the
Central Regional Lab to the time it was sent to the Data User
This concludes my presentation. If there are any questions, please
refer to the Region V Sample Handling Protocol for Hazardous Waste and the
SMO Users Guide to the EPA Contractor Laboratory Program, both of which
were sent to your Agency.
Additional ...now Marcia Kuehl will present slides which will acquaint
you with other areas of the Contractor Laboratory Program.
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STATE AGENCY ACCESS
TO THE
EPA
CONTRACTOR LABORATORY PROGRAM
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Eligibility Requirements
1. Samples must be from a Superfund site (EPA,
Hazardous Waste-National Priorities List) or a
Potential Superfund Site.
2. States must have co-operative agreements with EPA,
Remedial Response Branch or Permission of EPA,
Remedial Response Branch to use National
Contractor Laboratories.
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REQUESTING PROTOCOL
1. Submittal of Study Plan
2. Case Set-Up
3. Shipping Requirements
4. Quality Assurance and Data Review
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STUDY PLAN REQUIREMENTS
1. Submit To EPA OSC
2. Include:
A. Number Of Samples
B. Parameters
C. Matrix Type
D. Concentration Level
E. Survey Type
F. Shipment Date
G. Order For Bottles
H. SAS Request If Applicable
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CASE SET-UP
1. OSC Sends Study Plan To Chuck Elly
2. Elly Reviews Study Plan
3. If Comments, OSC Negotiates Differences
With State Contact.
4. If No Comments, Elly Sends Copy Of The Approved
Study Plan To OSC
5. Elly Sets Up Case With SMO
6. Elly Telephones Information To Designated State
Contact And Approves SAS Request (If Any)
7. Elly Sends Forms & Returns Copy Of Bottle Order
Form To Designated State Contact.
9
NOTE: Only One State Person Should Be A Designated
Contact With Elly
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WHEN TO REQUEST SAS
1. For Organic And/Or Inorganic Analysis Of Oils Or
Other Atypical Matrices Such As Fish, Mammal
Tissues, Air.
2. For Parameters Other Than The 114 PP Orgs Or
Task 1,2,3 Inorganics
3. For Lower Detection Limits Than In The Regular
IFB's. For Quality Control Which Is More
Extensive Than In The Regular IFB's.
4. For Quicker Turnaround Times Than The Normal
30 Days Of The Regular IFB's.
5. Foe EP Toxicity, Flashpoint And Other RCRA
Solid Waste Parameters.
6. Dioxins/Furans Are Requested.
7. Other Requests Not Covered Above.
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SAMPLE DESCRIPTIONS
1. Low Concentrations
2. Medium Concentration
3. High Concentration
4. Analysis Parameters
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US. ENVIRONMENTAL PROTECTION AGENCY - CLP Sample Management Offic*
P.O. Box SIS, Alexandria, Virginia 22313 - 703/557-2490
ORGANICS ANALYSIS DATA SHEET
Laboratory Name: • Cue Not
Lab Samole ID. No:
Pff
(21A)
(22A)
(24A)
(31 A)
(34 A)
(37 A)
(3SA)
(39 A)
(60 A)
(64 A)
(63 A)
(IB)
(38)
(SB)
(9B)
(12B)
(18B)
(20B)
(23 B)
(26 B)
(27 B)
(28 B)
(33B)
• (36B)
(37 B)
(39B)
(40B)
(4 IB)
(428)
<43B>
* -~ (52B)
(33B)
(54B)
(33B)
(568)
(628)
(638)
(668)
(67B)
(6SB)
(6*6)
(70S)
(718)
(72B)
CAS*
$8-06-2
39-50-7
95-57 -S
120-83-2
105-67-9
SS-75-5
100-02-7
51-2S-5
534-52-1
87-86-5
108-93-2
Sample Nunbe-
ESV3-3
OC Report Not
Multiply Detection Limits by 1 Q or 10 Q (Check Box for Appropriate Factor)
ACID COMPOUNDS BASE/NEUTRAL COMPOUNDS
«R/> «Vt
oru»/V» oruR/kg
(circle on*) PP« CAS* (circlTone)
2,4,6- trichlorophenol (738) 50-32-8 benzo(a)pyrene «
p-cft loro-m^reso 1
2- ctilorophenol
2,4-dichlorophenol
2, 4-dimethy (phenol
2- nitrophenol
4-flitrophenol
2,4-dinitrophenol
4,6-dinitro-2-fhethylphenol
pentachlorophenol
phenol
BASE/NEUTRAL COMPOUNDS
83-32-9 acenaphthene
92-87-5
120-82-1
1 18-74- 1
67-72-1
111 -44-4
91-3S-7
95-50-1
541-73-1
106-46-7
91-94-1
121-14-2
606-20-2
122-66-7
206-44-0
7005-72-3
101-55-3
39638-32-9
111-91-1
87-68-3
77-47-4
78-59-1
91-20-3
9S-95-3
86-30-6
621-64-7
117-81-7
85-68-7
84.74-2
117-84-0
84-66-2
131-U-J
56-55-3
benzidine
1,2,4-trichlorobenzene
hexachlorobenzene
hexachloroethane
bis(2-ch loroethy Dether
2-chloronaphthalene
1,2-dicnlorobenzene
1,3-didilorobenzene
1,4-dichlorobenzene
3,3'-dichlorobenzidine
2,4-d in itr oto luene
2,6-dinitrotoluene
1 ,2-diphenv Ihydrazine
Uuoranthene
4-chlorophenyl phenyl ether
4-bromophenyl phenyl ether
bU (2-chloroisopropyl) ether
bis (2-chloroethoxy) methane
hexachlorobutadiene
hexachlorocyclooentadiene
isophorone
naphthalene
nitrobenzene
N-n i trosod ipheny lamine
N-oitrosodipropylamine
bis (2-ethylhexyl) phthalate
benzyl butyl phthalate
di-n-butyl phthalate
di-n-octyl phthalate
diethyl phthalate
dimethyl phthalate
benzo(a)anthracene
(74B).
(75B)
(76B)
(77B)
(78B)
(798)
(SOB)
(SIB)
(S2B)
(S3B)
(SUB)
(2V)
(3V)
(4V)
(6V)
(7V)
UOV)
(11V)
(13V)
(14V)
(15V)
(16V)
(19V)
(23V)
(29V)
(30V)
(32V)
(33V)
(3SV)
(44V)
(45V)
(46V)
(47V)
(48 V)
(49V)
(30V)
(31 V)
(S3V)
(86 V)
(S7V)
(SSV)
203-99-2
207-08-9
218-01-9
208-96-8
120-12-7
191-24-2
86-73-7
83-01-8
33-70-3
193-39-5
129-00-0
107-02-8
107-13-1
71-43-2
56-23-5
10S-90-7
107-06-2
71-55-6
75-34-3
79-00-3
79-34-3
73-00-3
110-73-8
67-66-3
73-33-4
136-60-5
78-87-5
10061-02-6
10061-01-05
100-41-4
75-09-2
74-87-3
74-83-9
75-23-2
75-27-4
75-69-4
75-71-8
(24-48-1
127-18-4
LOS-SS-3
79-01-6
75-01-*
oenzo
-------
bora wry
Name:
b Sample I.D. No:
PP*
(S9P)
(90P)
(9 IP)
(92P)
(93P)
(94p)
(95P)
(%P)
(97P)
(9SP)
(99P)
(100P)
(101P)
(102P)
•
...... . .^* j^^-^-g—-
Case No:
, QC Report Not
Multiply Detection Limits by I Q or '° D (Check Box for Appropriate Factor)
PESTICIDES PESTICIDES
"8/1 . v«/l
orug/kg orus/Vg
CAS* • (circle one) PP*- CAS* , (circTone)
309-00-2 aldrin (103P) 319-83-7 y^-BHC
60-57-1 dieldrin
57-74-9 ehlordane
30-29-3 4,4'-DDT
72-J5-9 4,4'-DDE
72-54-8 4,4'-ODD
UJ-29-7 cC-endosulfan
1 1 3-29-7 A -endosulf an
1031-07-2 endosulfan sullate
72-20-8 endrin
7421-93-4 endrin aldehyde
76-44.3 heptachlor
1024-57-3 heptachlor epoxide
319-84-6 CC-BHC
ACID COMPOUNDS
^i.
w««/lq{
CAS » (circle one)
63-85-0 ben zoic acid
95-4S-7 2-methylphenol
108-39-a 4-methy!phenot
95-95-4 2,4,5-trichlorophenol
BASE/NEUTRAL COMPOUNDS
62-53.3 aniline
100-31-6 benzyl alcohol
106-47.* 4-chloroaniline.
132-64-9 dibenzofuran
91-57-6 2-methylnaphthalene
gJ-74-4 2-nitroaniline
99-09-2 3-oitroaniline
100-01-6 4-nitroaniiine
(104P) 319-J6-8 «P-BHC
(105P) 58-49-9 y.BHC (lindane)
(106P) 53469-21-9 PCB-1242
(107P) 11097-69-1 PCB-1234
(10SP) 11104-28-2 PCB-1221
(109P) 11141-16-5 PCB-1232
(HOP) 12672-29-6 PCB-1248
(HIP) 11096-82-5 PCB-1260
(112P) 12674-11-2 PCB.1016
(113P) 8001-35-2 toxaphene
DKDXINS
(129B) 1746-01-6 2,3,7,8-tetrachlorodibenzo-p-djoxin
VOLATDLES
"^L
orug/kg
CAS * (circle one)
67-64-1 acetone
78-93-3 2-butanone
73-15-0 carbondisulfide
519-78-6 2-hexanone
108-10-1 4-methyl-2-o«ntanone
100-42-5 styrene
108-03-4 vinyl acetate
93-47-6 o-xylene
4/S
-------
US ENVIRONMENTAL PROTECTION AGENCY
HWI Sample Management Office
P.O. Box SIS - Alexandria, Virginia 22313
703/557-2*90 FTS S-557-2*90
Sample No.
INORGANICS ANALYSIS DATA SHEET
LAB NAME
LAB SAMPLE ID. NO.
CASE NO.
QC REPORT NO.
1. Aluminum
2. Chromium
3. Barium
Beryllium
5. Cobalt
6.
Copper
7. Iron
8. Nickel
9. Manganese
TASK I (Elements to be Identified and Measured)
ug/1 or mg/kg
(circle one)
10. Zinc
ug/1 or mg/kg
(circle one)
11. Boron
12. Vanadium
13. Silver
1. Arsenic
2. Antimony
3. Selenium
Thallium
TASK 2 (Elements to be Identified and Measured)
ug/1 or mg/kg
(circle one)
5. Mercury
ug/1 or mg/kg
(circle one)
6. Tin
7. Cadmium
8. Lead
TASK 3 (Elements to be Identified and Measured)
ug/1 or mg/kg
(circle one)
1. Ammonia
2. Cyanide
3. Sulfide
COMMENTS:
-------
LOW CONCENTRATION SAMPLES
A. 0-10 PPM of Single Contaminant
B. Environmental Soils & Water Samples,
Groundwaters, Surface Waters, Most Off-Site
Waters, Soils, Wells, Leachate Springs, Ditches,
Rivers
C. Any Diluted Samples
D. Low Hazard
-------
MEDIUM CONCENTRATION SAMPLES
A. 10 PPM to 15% of Single Contaminant
B. On Site Water-Soil Samples, Samples Lying Besides
Drums, Lagoons, On-Site Impoundments, Leachate
Collection Pools, On-Site Ditches.
C. Areas of Direct, But Diluted Concentrations.
D. Medium Hazard
-------
HIGH CONCENTRATION SAMPLES
A. 15% to 100% of Single Contaminant
B. Drums, Surface Impoundments, Storage Tanks, Spills or
Direct Discharges From Impoundments
C. Little or No Evidence of Dilution
D. High, Unknown Hazard -
-------
Sample Size & Preservation
Organics - Low Level
A. Waters
EXTRACTABLES (Acids, B/N's, Pests/PCB )
Send 2-1 /2 Gal. Amber, Narrow Neck Glass
Bottles With Teflon - Inserted Cap, Iced to 4 C.
VOLATILES
Send 2 - 4O ml Borosilicate Glass Vials With
Teflon Septums, Iced To 4°C.
B. Soils
1 - 8 oz. Wide Mouth Glass Bottles With A Teflon
Insert, Iced To 4°C.
-------
Sample Size & Preservation
Organics - Medium Level
A. Waters (Extractables & VOA's)
4-32 oz. or 8-16 oz. Wide Mouth Bottles With
Teflon - Inserted Cap. Ship In Paint Cans.
NO PRESERVATIVE
B. Soils
1 -8 oz. Wide Mouth Glass Bottle With
Teflon-Inserted Cap. Ship In 1 72 Gal. Paint Cans.
NO PRESERVATIVE
-------
SAMPLE SIZE & PRESERVATION
Organics-High Level Inorganics
Waters, Liquids, Soils, Sludges, Solids
1 -8 oz. Wide Mouth Glass Jar, Teflon
NO PRESERVATIVE
-------
SAMPLE SIZE & PRESERVATION
Task 1&2 Metals - Low Level
Waters
1-1 Liter HD Plastic
3 ml 1:1 HNO3
or to pH 2.
Cyanide
1-1 Liter HD Plastic
5 ml 6N NaOH
Iced to 4 C.
Soils
1-8 oz. Plastic or Glass Bottle
Iced to 4 C.
-------
SAMPLE SIZE & PRESERVATION
Inorganic * Medium Level
A. Water & Soils
1. Task 1&2 Metals
2. Cyanide
3. NH3
4. Sulfide
B. 1 -8 oz. Plastic or Glass, Wide Mouth Jar
NO PRESERVATIVE
-------
TURN AROUND TIMES
1. Routine
A. Low and Medium Soil and Water Samples
30 DAYS
B. High Concentration Samples
51 DAYS
2. SAS
A. Low and Medium Soils and Water Samples
2 to 30 DAYS
B. High Concentration Samples
5 to 30 DAYS
-------
FIELD QUALITY CONTROL
Low & Medium Samples
1. Field Reagent Blank
2. Duplicate of Sample
High Hazard Sample
1. Duplicate of Sample
-------
CHAIN OF CUSTODY
Requirements
1. USEPA Forms & Tags, Seals (Optional)
2. Sampling Team Listed
3. Info on Tags & Forms Match
4. Custody Forms Completed Properly
5. Method of Shipment Listed
6. SEPARATE FORM FOR EACH SITE & LAB,
-------
CUSTODY
A Sample Is In Your Custody If The Following Criteria Are Met:
1. It is in your possession, or
2. It is in your view, after being in your possession, or
3. It was in your possession and then locked up
to prevent tampering, or
4. It was in your possession and then transferred
to a designated secure area.
-------
TRANSFER OF CUSTODY & SHIPMENT
1. Relinquishing & Receiving Samplers Sign, Date, Time
2. Ship To Laboratory
3. Separate Custody Record For Split Samples And To Each Lab
4. Retain Bill Of Lading From Carrier
5. Lab. Custodian Signs Upon Receipt
6. Original Stays With Samples
-------
u §
-------
-------
EPA S/tnfLE TA
-------
si ii?e~ a?
s i D &
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION 5
230 South Dearborn Street
Chicago, Illinois 60604
&EPA
-------
;v/;;r-*'>::>cV-'- '••-'.'-'.'-" -••"•'. yr'^"-*-'.'*- Xr^-^fe^/'-^^'j^^''--^'::"
m
I
o 1
"14
1
-------
FORMS REQUIRED
Low & Medium Samples
1. SMO Org. Traffic Report
SMO Inorg. Traffic Report
2. (Packing List For Sas's)
3. EPA Custody Form
4. EPA Custody Tag
5. EPA or State Custody Seal
6. Stick-On Label Traffic Report
-------
Case Number:
Sample Site Name/Code
Fo*
(2) SAMPLE CONCENTRATION
(Check One)
*
Low Concentration
Medium Concentration
SAMPLE MATRIX
J^heckOne)
S Water
Soil/Sediment
Ship To:
Transfer
Ship To:
© Regional Office:
Sampling Personnel:
(D For each sample collected specify numbe
of containers used and mark volume level
on each bottle.
Number of
Containers
(Phone)
Sampling Date:
Water
(Extractable)
(Begin)
(End)
Water
(VOA)
(?) Shipping Information
SoiVSediment
Name of Carrier
Water
(Ext/VOA)
Other
Date Shipped:
Airbill Number:
(§) Sample Description
Surface Water
J*L_ Ground Water
Leachate
Mixed Media
Solids
Other (specify).
Approxima1
Total Volun
Sample
E 3451
E 3451
Y3451
E~3451
E 3451
E 3451
E 3451
E 3451
E 3451
E 3451
Water
(Extractable)
Water
(Extractable)
Water
(Extractable)
Water
(Extractable)
• Water
(VOA)
Water
(VOA)
- Soil/Sediment
(Ext & VOA)
- Soil/Sediment
(Ext & VOA)
• Water
(Ext & VOA)
-Water
(Ext & VOA)
QO) Special Handling Instructions:
(e.g., safety precautions, hazardous nature)
SMOCOPY
-------
Sample Site Name/Code
r
) Sampling Office: _
Sampling Personnel:
(Name)'.
(Phone)
Sampling Date;
(Begin)
g Date:
iA
Sample Description:
(Check One)
Surface Water
Ground Water
Leachate
Mixed Media
Solids
Other
(specify)
MATCHES ORGANIC SAMPLE NO.
SAMPLE CONCENTRATION
(Check One)
Low Concentration
— Medium Concentration
0 SAMPLE MATRIX
.X (Check One)
!—- Water
Soil/Sediment
Transfer
Ship To:
0 Shipping Information:
Name Of Carrier
Date Shipped:
Airbill Number:
(m\ Mark Volume Level
On Sample Bottle
JKieck Analysis required
^L Task 1 & 2
__ Task 3 Ammonia
Sultide
Cyanide
SMOCOPY
^ME0176
-T«ikl&2
ME 017 6 -Tasltl&2
ME 017 6 -TaakS
ME 6 176 -T«k3
ME 0176 -Ta»k3
ME 0176 -TaskS
• ME 0176 -TaskS
-------
FORMS REQUIRED HIGH HAZARD SAMPLE
1. SMO High Hazard Traffic Form (Packing List For SAS's)
2. Hazardous Waste Samp. Prep Request
3. EPA Custody Form & Tag
4. EPA or State Custody Seal
5. Label From Traffic Report
6. Hazardous Shipping Certificate
-------
c c c c c c
o o o o o o
o
FIELD SAMPLE RECORD
3) Case N
Sample Site Name/Code:
1 ~ • » -*—
Field Sample Description:
Aqueous Liquid
_2udge
_Sobd
Z Other
,3) SUpTb:
Attn:
Jf^
Sampling Personnel:
(ptone)
Sampling Date:
(begin)
(end)
Shipping Information:
(airbi number)
Known or Suspected Hazards:
ftt
Preparations Requested:
(check below)
Sample Volume: O #">
i^Organics
Organics
Total Metals
.j^jjptal Mercury
strong Aod Anicns
Sample Location:
E 5102
E 5102
B 5102
• 5102
E 5102
Special Handling Instructions:
SMOCopy
-------
o
^•^
LU
I/I
01
e-o
re a>
oo >
•*-
0}
x
LU
-------
US. ENVIRONMENTAL PROTECTION AGENCY
HWI Sample Management Office
P.O. Box SIX . Alexandria, Virginia 22313
Phone 703/557-2*90 - FTS/557-2490
PACKING LIST
SAS Number
3S5 £
Regional Office:
Regional Contact:
E//
(name)
(phone)
Sampling Date(s):
Date Shipped:
//* 3
Ship To:
For Lab Use Only
5*330
Date Samples Rec'd:
S/,
' $000*
. rw/r
Received By:
Sample
Numbers
Additional Sample
Description
Sample Condition
On Receipt
5.
cyp5"S^ - Me4.
6.
7.
S.
9.
10.
11.
12.
13.
PCfe* flivlv
1*.
15.
16.
17.
IS.
19.
20J
For Lab Use Only
White - SMO Copy, Yellow - Region Copy, Pink - Lab Copy for return to SMO, Gold - Lab Copy
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
rltfl Sample Management Office
P.O. Sox 813 - Alexandria, Virginia 22313
Phone: 703/557-2*90 - FTS/557-2*90
SPECIAL ANALYTICAL SERVICES
Regional Request
Regional Transmittal . . _ Telephone Request
\ _ |
A. EPA Region:
B. Regional Representative: £,/•> t/C fa Ell
y
C. Telephone Number: 3/^* 35*3*^37 O
D. Date of Request: $ 4J?T*H b* A, Ij
Please provide below a description of your request for Special Analytical Services
under the Uncontrolled Hazardous Waste Dumpsite Program. In order to most
efficiently obtain laboratory capability for your request, please address the
following considerations, if applicable. Incomplete or erroneous information may
result in a delay in the processing of your request. Please continue response on
additional sheets, or attach supplementary information as needed.
X^**1.
' Definition and number of workrunits involved (specify whether whole samples
or fractions; whether organics or inorganics; whether aqueous or soil and
sediments: and whetherlow. medium or his
*A ** <••>• I _i «te ft r
of analytical service requested:
3. Purpose of^nalysis (specify.whether enforcement, RCRA, NPDES, etc.):
'
Estimated date(s)of collection:
5. Estimated date(s) and method of shipment:
-------
6. Approximate number of days results required after lab receipt of samples:
40-tiC. No /**<*. +h*u NOV. /?,/<./»>/>< Tg *OA5Ttf ^r?. /OX c,hAiH*T* 9
10. Other (use additional sheets or attach supplementary information, as needed):
Vti^ti** J * -*£ '*- -*--•• -•--*<*•- Jr.. -
PcTfVf A-Tfr /tVt/4 ~
fy^Yf-7ft p «»H! jw 7^?
11. Name of samplins/shippmg contact: JoAv P/€/S5K< ^
«a V
P/€
JL4
Please return this request to the Sample Management Office as soon as possible to
expedite processing of your request for special analytical services. Should you
have any questions or need any assistance, please call us at the Sample Manage-
ment Office.
-------
-3-
I.
Data Requirements
Parameter:
ff
II. QC Requirements
Audits Required
/•(
Oetection Limit
.ycQM
't- &
III. *Action Required if Limits are Exceeded :
IP
Precision Desired
(±% or Cone.)
¥0
Frequency of Audits Limits* (% or Cone.)
4J*4~to* 4/
-------
DOT SHIPPING REGs
Medium & High Hazards
1. In 1/2 or 1 Gal. Cans
2. Inside Plastic Bag
3. Vermiculite (Zono-Lite)
4. Clips or Tape on Cans
5. Address & Hazard
6. Haz. Shipping Cert.
7. Metallic or Plastic Picnic Cooler Required
-------
SHIPPER'S CERTIFICATION FOR RESTR|CTED ARTICLES
(excluding radioactive materials)
Two completed and signed copies of this certification shall be handed to the carrier. (Use block letters)
WARNING: Failure to comply in all respects with the applicable regulations of the Department of
Transportation, 49-CFR, CAB 82 and, for international shipments, the IATA Restricted Articles Regulations may
be a breach of the applicable law, subject to legal penalties. This certification shall in no circumstance be signed
by an IATA Cargo Agent or a consolidator for international shipments.
'This shipment is within the limitations prescribed for: (mark one)
C£ passenger aircraft D cargo-only aircraft v
i Number
1 of
I Packages
PfcS #1
Article
Number
(Int'l only
See Section
IV IATA RAR)
Proper Shipping Name of Articles as
shown in Title 49 CFR. CAB 82 Tariff 6-D,
and (for int'l shipments) the IATA
Restricted Articles Regulations. Specify
each article separately. Technical name
must follow in parenthesis the proper
shipping name for N.O.S. items.
Poison B, Solids, NOS:
Polycyclic Aromatic Hydro-
carbons
Poison Babel
Class
Poisor
B
IATA
Packing
Note No.
Applied
(int'l
only)
L 364
a)(l)
Net
Quantity
of Each
Package
100 tag
m
Flash Point T
(closed cup) 1 A
For Flammable u£
Liquids Kg
•c.
•F. |r
V
S
r
Special Handling Information:
I hereby certify that the contents of this consignment are fully and accurately described above by Proper
Shipping Name and are classified, packed, marked, labelled and in proper condition for carriage by air
according to applicable national governmental regulations, and for International Shipments, the current IATA
Restricted Articles Regulations.
Name and full address of Shipper
Analabs
Name and title of person signing Certification
80 Republic Drive
North Haven, Conn. 06473
Eleanor Rome, Export Clerk
Date
?Q.1Q30
Air Waybill No.*
Sigrja*ure of the Shipper (see WARNING above)
O<
OOX i
dl for,
,ion
Airport of Departure*
,g can-
Airport of Destination*
JBMt
J626 3'
-------
5 5"
-»• 13
ro> CD §
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2.0
z= S1 3"
~w w - o 5 c
o*0 • f * o
S 3 o P r x
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-------
Internal Record Keeping
and
Data Handling , Review
1. VIAR Case Planning Log for future and pending cases.
2. Internal Tracking Sheet
3. Raw Data Return
a) NCL Data to EPA, CRL.
b) CRL forwards it to State
c) State reviews own data
d) State sends copy of review comments to CRL
e) States resolve Q..C. probs.
f) Unresolved Q.C. probs. referred to Regional DPO
For lab which has the Q.C. problem.
4. Picnic Cooler Return
-------
VlAZ
NO.
I
-------
-------
CLP SCRIPT
QUALITY ASSURANCE AND DATA REVIEW
SEPTEMBER 1983
-------
QA 0
Hello I am Marcla Kuehl. I am the Quality Control Coordinator for the
Region V Central Regional Laboratory. My duties Include auditing not
only the data generated by our In-house laboratory but data generated by
the National Contract Laboratory Program. I am one of a five person team
responsible for CLP data review. Two people review organic data, two
review inorganic data, and I do both on an as needed basis. I have been
with the lab for three years, in the capacity of Chemist, GC/MS Operator
and now paper pusher. I have retained both my eyesight and my sense of
humor since I began reviewing CLP data in January of 1980.
-------
INTRODUCTION
Now that you have collected, packed, and shipped your samples you will
be buried in a sea of data. It is essential that this data he reviewed
by competent technical level personnel before it is released for use.
It would be very naive to think that this slide show alone will enable
everyone to quickly review Contractory laboratory program data. Persons
responsible for review should already have working and preferably hands-on
knowledge of AA, ICAP, GC/EC, GC/MS and basic extraction chemistry.
QA 1
This presentation will deal with the technical review and quality level
assessment of the data. The contract specifies the general quality
assurance program to be followed and details the specific quality
control audits to be used. It is your job as the reviewer to determine
the level of quality of the data based on these audit results and
recommend if the data quality is sufficient to meet its intended use.
I will discuss both organic and inorganic data review by examining the
specific pieces of paper we at the Region V Central Regional Laboratory
key in on. Examples presented are from various Contract laboratories
and several cases. The names have been deleted to protect the innocent
or the guilty as the case may be. Actual forms and data printouts in your
data packages may vary from Contractor to Contractor based on instrument
differences. Guidelines for the preparation of Special Analytical Services
requests relating to QC requirements will also be presented.
QA 2
All data review requires the Elementary School three R's- reading, writing
and arithmetic. Keep this in mind and you will not be side-tracked or
put unnecessary time into paper shuffling.
QA 3
Before you even look at any data, read the Statement of Work, the analytical
methods and the QA/QC sections of the contract. Imagine that you are a
sample and trace your progress through the laboratory and note what kinds
of paper are generated along the way. You may find deficiencies in the
methods, or lapses in the documentation. The Contractor is only responsible
for what is written in the contract. There is no such thing as a free lunch-
Contractors generally will not provide extras. Recommendations for additions,
deletions, or changes to existing contracts should be made in writing to SMO.
-------
- 2 -
Write down the data or sampling objective for the case to be reviewed. This
is determined by consultation with the Samplers, Engineers and Project Leader.
I usually classify the overall level of the study into one of three categories:
Category 1 - Screening Surveys: These are intended to serve as quick looksees.
Quantisation, precision and accuracy is not as vital. Correct
qualitative identification is needed.
Category 2 - Remedial or Monitoring Surveys: These surveys require more
quantitative results in order to determine whether the clean-up
level is sufficient or to detect trends in ambient levels.
Category 3 - Criminal or Known Enforcement Investigations:
These necessitate that the custody paper trail be reviewed
carefully as well as flagging all out of control situations.
Precision and accuracy of both quantitative and qualitative
data is crucial.
When the end action or purpose of the study is not known, aim for the
criminal category as it is much better to be safe than sorry.
The calculations involved in the basic statistical expressions of mean
and standard deviation should be reviewed. In order to cross-check Contractor
values, you should known how to calculate percent recovery, relative percent
difference (RPD), response factor (RF), relative response factor (RRF),
relative retention time (RRT), and mean percent change. Definitions of
these can be found in the text of the contract. Arithmetic errors do occur,
and may often directly involve the sample values reported.
QA 4
Since organic data generally constitutes a bigger and more awesome pile, I
will tackle its review first. Listed here are eight target areas that are
examined during the data review process. They are not listed in order
of importance, but in an order that personally like to use. Once you
are familiar with the layout of the data packages you may wish to revise
the order. On the following slides each of the eight items will be
presented along with key forms to look at.
QA 5
Do decafluorotriphenylphosphine and bromofluorobenzene mass spectra meet
the contract required abundance criteria? The required abundance criteria
were taken directly from the December 3, 1979 Federal Register. These
criteria were meant to help laboratories determine if their GC/MS system
is in tune and stable enough to generate reproducible data. The key piece
of paper to look at is the mass spec abundance list, either computer
generated or a form similar to the ones seen in the next slides.
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QA 6
This form is for OFTPP, injected on January 26, 1983 relating to all samples
in run OH830136C15. This information is at the top of the form and should
be used to correlate real samples to the appropriate DFTPP injection. You
should_be able to find at least one injection per 8-hour shift. The two
masses most often out of specs for DFTPP are 51 and 443. There are two
schools of thought on what effect flags like these have on sample data.
One school recommends scrapping the associated sample data as invalid,
since adherence to these criteria are required by law. The other school
relies on whether the specific masses out of spec affect the identification
of any priority pollutants or tentatively identified compound search matches.
Your professional judgement should be used to choose what criteria you will
follow- but be consistent.
Note that that chromatography and sensitivity checks are also listed on this
form below the DFTPP specs. When these do not meet the contract limits, a
notation of poor chromatography conditions or sensitivity should be made
and affected samples in the run flagged. Contract limits for these audits
are:
- pentachlorophenol response factor should be greater than 0.05
relative to dig-anthracene.
- 50ng of benzidine should be detectable, double check the actual
RIC for its presence.
- Area counts for 20ng d]Q anthracene should be between 20,000-
50,000 to avoid detector saturation at the higher standard
concentration levels.
The column description should be checked to see that the contract specified
column has been used in the instrument.
QA 7
Recently, the Regional data reviewers have requested that the contract lab
summarize their tuning results on an easy-to-find one page form such as
this one. I will then randomly check actual abundance lists in a case to
verify the presence or absence of listed deviations.
QA 8
Are the instrument and method blanks contaminated? The key item to look at
is the actual RIC of the blank and the reagent blank summary. Contamination
of lab or instrument blanks negates any quantitative sample results for those
compounds detected in the blank. This is especially vital where sample
results are of the same order of magnitude as the blank. Blank subtraction,
when done, will be noted by the contract lab. If you are not sure, contact
the contract lab before you release data.
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QA 9
Here are some examples of contractor generated QC notices to alert you to
blank problems and calm your fears that the lab is totally out-of-control.
The top notice refers to the presence of siloxane in the volatile blank
fraction due to the anti-foaming agent added to the purge and trap vessel.
The bottom notice attempts to determine the source of 4-hydroxy-4-methyl,
2-pentanone which is a common artifact seen in ABN fraction blanks and
field blanks. This compound is formed from residual acetone reacting
with NaOH during the pH'^ adjustment. Check to make sure that these
compounds are not listed as positive hits in the samples for this case.
QA 10
Highlighted in this reagent blank summary is the presence of acetone and
methylene chloride in the volatile fraction above the contract detection
limit and trace amounts of three phthalates in the semi-volatile fraction.
The K code under "concentration found" stands for a trace value present,
which is below the contract detection limit but not quantifiable. The
presence of these lab blank contaminants is not an unusual occurence, but
is an annoying one. What do you do for samples in this case that have
similar levels of these compounds reported? You flag them as being
indistinguishable from lab induced contamination and therefore not a reliable
indication of the actual sample level. You may circle the results directly
on the result sheet, or list them on a review form. At any rate, do not
let these contamination notes be separated from the associated data.
QA 11
Are positively identified or positive "hit" priority pollutants actually
present? In order to minimize the cost and panic over false positives,
each positive "hit" should be verified by you. Look at the dual display
Mass Spectrum of the sample peak and associated standard peak. The sample
and standard retention times should agree to within j* 8 seconds. The
contract also requires that all ions present in the standard at a relative
intensity of greater than 10% must also be present in the sample spectrum
and that the relative intensities must agree to within _+20%. Extraneous
ions greater than 10% intensity in the sample and not in" the standard
must also be accounted for.
QA 12
Here is a dual display of sample 023890 peak (shown above) which was
identified as priority pollutant 445 which is pyrene. The pyrene
standard mass spectrum is shown below. This is an obvious good match.
Also check the retention time of the scan (1922) against the retention
time of pyrene for the initial or continuing calibration standards found
on other forms in the packet. Remember that a +_ 8 second or scan window
is allowed. "~
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"Hits" not meeting these criteria should he considered false positives
and be labelled accordingly on the data sheets.
QA 13
This 1s the associated GC/MS computer generated quantitation report foV
sample~023890. This is an example from a Finnegan OWA system. Hewlett
Packard and other GC/MS system printouts vary in format, but the basic
information is still similar. The first column on the left labelled No refers
to compound number- usually the contractor lab will list these in order
of f>C column elution. Compound number 62 represents pyrene. The next
column labelled m/e is the mass of the base peak of compound 62, mass 202.
The scan column contains the scan number the compound pyrene eluted at,
here 1922, at a retention time of 24 minutes, 1 second. Remember that this
retention time should be within that 8 seconds of the pure pyrene standard
run that day. Pyrene relative response time (RRT) is calculated relative
to compound 48 (nearest internal standard, D-jgchrysene). A base-to-base
peak integration was done resulting in an area of 41541, representing
an injection concentration of 22.604ng, or 2.42% of the total RIC peak
area.
The circled amounts with a "Y" scribbled near them means that these
priority pollutants were verified by the contractor GC/MS supervisor
or expert to be present at a quantifiable level. You should also
examine their dual display spectra and RIC and confirm their presence.
QA 14
This sheet reflects the contractors worksheet for calculation of positive
final results. The compound number 445 or pyrene quant report value from
the previous slide was rounded up to 23. The correction factor includes
dilution, original sample weight and dry weight calculations. When multiplied
by the quant report value, the result of 920 ug/Kg should be found on the
data report form. Double check multiplication on all positive "hits" as
time permits. The column labelled detection limit is the low level solid
determined value in ug/Kg and gives you a comparison of how high above the
matrix detection levels the compound actually is.
QA 15
Are the tentatively identified compounds matches reasonable? Once the
positive priority pollutants are confirmed by your review, the tentatively
identified compound searches should be visually examined by keying in on
the RIC to determine the approximate size of the unknown peak, and the
mass spectra of the unknown and the top three ranked computer library
searches. Not only is a visual inspection needed, but a mental one is'
needed also. Is the compound match too exotic to survive the extraction
or GC/MS conditions? Is the compound one not expected in the sample or
site? For example, long chain sugars are not usually found in environ-
mental water or sediment samples.
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QA 16
This is the simultaneous display of the sample unknown peak I486, of sample
023890, of a base peak of 97 and the top three ranked library search matches:
1,1,2-trichloroethane, 2,2-dichloropropanoyl-chloride and 1,1-dichloro-l-
nitroethane. The unknown was identified by the contract lab as 1,1,2-tri-
chloroethane, purity 892. This area of data review is where GC/MS spectral
interpretation experience will be needed. Although several light masses
appear in the sample and not in the match, all trichloroethane masses are
accounted for in the sample. Note that the sample base peak is 97 whereas
the best match base peak is 83. Generally speaking, purity or fit figures
of less than 800 or 80% are often questionable matches. Contractors are also
required to estimate the concentration of these unknowns (up to 20 A8N, up to
10 VOAs) will be estimated this way on the basis of internal standard response.
You may check the reasonableness of the magnitude of tentative ID concentrations
by checking the Quant report or RIC for relative area response. Since quantitation
of these compounds is only an estimate, I rarely try to recalculate the reported
figure. Unreasonable matches in your opinion should be deleted and marked with
your initials and date. Identification of unknown peaks spectra using hard bound
library spectra is a colossal task and should not be attempted unless you are
requested to do so by the Project Leader and are well versed in MS interpretation.
QA 17
Were the sample extraction and analysis holding times met? The contract requires
that volatiles be extracted within 7 days and ABN's be extracted within 5 days
of sample receipt by the contract lab. To monitor this, the laboratory analysis
chronicle copy could be checked. Recently, this can additionally be monitored
by internal lab GC screen bench records.
The holding time requirements delineated in the contract must be met or data
should be flagged. Remember the end use of the data when you do flag holding
times. Samples sitting in drums for years should not change if held in a lab
over 14 or 30 days. The lab analysis chronicle is a key item to check as it
lists all of the sample extraction and analysis times.
QA 18
This is a contract lab GC screen extraction record for Case 1850. The sample
extraction procedure is clearly spelled out in the narrative below. These
samples were extracted on 6/29/83. Check your sampling and chain-of-custody
record to calculate the days elapsed since collection, shipment and lab receipt.
Note that the contract lab is not responsible for your shipping delays. Their
holding and data turnaround time clock starts when they actually receive the
samples. Now that these liquid samples have been extracted for pesticides,
they are screened by GC/EC.
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QA 19
The sample extracts of 6/29/83 were screened on 7/4/83 by GC/EC according
to the procedure narrated in the top three items on this Screen Evaluation
Form. Note that all of these extracts were judged to be low based on
Point #3: No peaks appeared in the screen chromatogram at a response
greater than 25% of p,p'-methoxychlor. Also note that the contractor was
working on the fourth of July.
QA 20
Sample E3434's GC/EC pesticide screen chromatogram is shown here. Note
that no peaks of a response near 25% of p,p'-methoxychlor are seen. You
should particularly check screen chromatograms of samples designated as
medium level to ensure that the higher detection limits were justified
based on screen peak response. Also verify that 5ng methoxychlor does
produce at least a 50% full scale deflection response.
•
OA 21
Are the results reported of acceptable precision? Matrix spiked duplicates
should be included in each case or one per 20 samples, whichever is more
frequent. This duplicate should be an environmental sample, split by the
laboratory, not^ a method blank. The key form to look at is the presentation
of duplicate relative percent difference (RPO). A matrix spike duplicate is
a random environmental sample that is split into three separate aliquots. One
is extracted and analyzed as is, the other two are spiked with a variety of
priority pollutants at the same level, then extracted and analyzed. This
concept was used to give some meaningful precision and recovery data in actual
sample matrices, as samples chosen at random, and analyzed without a matrix
spike were more often than not, clean samples. Not detected compared to not
detected is great, but not useful precision.
QA 22
This is a summary of the QC sample and original sample results for a matrix
spike duplicate pair pertaining to Case 1439. The sample chosen for the
matrix spike duplicate is in the upper left hand corner under EPA Number. Other
samples in the case containing this duplicate pair are listed under associated
sample numbers. The first seven compounds listed are the surrogate spike
compounds. Note that four out of six show poor precision. The next 11 compounds
are those used in the matrix spike solution. 1,2,4-trichlorobenzene, hexachloro-
benzene, and 1,4-dichloronenzene are outside the contract precision allowances.
Contract precision allowances expressed as RPO are: +, 15% for volatiles, ^ 40%
for acids, +_ 50% for base neutrals, ^40% for pesticides and TCOO. Similar
sheets in the data packet should list" the other fractions' precision results.
What should you do for a case where the matrix spike
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duplicate floes not meet precision limits? First flag the actual sample
chosen as yielding erratic results, therefore quantitative sample results
for the affected sample fractions may only be considered as precise as
the matrix spike fraction precision. This statement may or may not be
extended to the other samples in the case, depending on their degree of
similarity to the matrix chosen.
QA 23
Are the results reported of acceptable accuracy? Surrogate spike compounds
are added to every real sample, QC sample, and blank, the recovery of these
compounds are your key to the extraction efficiency and therefore accuracy
of each sample fraction. The contract lab will summarize the entire case
surrogate recovery on a form to enable you to quickly scan for out-of-control
results.
QA 24
This is a percent recovery summary for a case of low level water samples.
The three volatile surrogates used are Ds-toluene, bromofluorobenzene (8FB),
and 04-!,2-dichloroethane. Advisory limits only have been set for 8FB and
04-1,2,-dichloroethane due to lack of enough interlab data points. No
samples were outside of the QC or advisory limits. The next seven surrogate
compounds are used to evaluate semi-volatile fraction accuracy. Ds-nitrobenzene,
2-fluorobiphenyl, Ds-phenol, 2-fluorophenol and 2,4,6-tr'ibromophenol are the
required surrogates. Pentafluorophenol and decafluorobiphenyl are two additional
chosen by the contract lab as an option. Since no QC or advisory limits have
been set for these two optional surrogates, no flags can be assigned. This
data is evaluated by the contract lab to judge the suitability of these optional
surrogates. 2,4,6-tribromophenol recovery was out-of-control low for the
entire case. This surrogate is one of four compounds used to assess acid
fraction accuracy- the others are pentafluorophenol, 05-phenol, and 2-fluorophenol
Look in the data package for an explanation of consistent low recoveries such as
these. None of the three base-neutral surrogates have any flags assigned- look
at the actual Ds-nitrobenzene, 2-fluorobiphenyl and Decafluorobiphenyl recoveries.
Although generally biased low, none are outside the lower limit. Decafluoro-
biphenyl has no limits assigned to it due to inadequate data base. The current
sole pesticide surrogate 1s dibutylchlorendate. No recoveries are outside
the 67-114% limit. The surrogate used for 2,3,7,8-TCDD analysis is 1,2,3,4-TCDD,
chosen because of its lower toxicity and rare occurence in environmental samples.
Two recoveries of 332 and 334% were flagged by the contract lab. An explanation
as to the possible spiking error or evidence of native 1,2,3,4-TCOO in these
samples should be included with the data package. A 0% recovery was also found
for sample E3431. If any positive 2,3,7,8-TCDO is reported for this sample,
its quantitatlon may be biased low due to the poor surrogate recovery.
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Sample E3432 1,2,3,4-TCOD recovery was 17.1%, below the QC limit of 26-104%,
but was not asterisked or flagged by the contractor. In the comments section,
there should be explanations of out-of-control situations or notation of reruns,
but alas there is nothing there in this example. The contract requires that
any out-of-control surrogate recovery occuring in a blank necessitates reinjection
or repurging. If the recovery is still outside limits, no data is to be generated
or reported until corrective action is taken, such as recalibration. When the
recovery of any one surroga'te falls outside the limits for a sample, the contractor
must verify and document that the deviation is due to the sample matrix itself
and not his laboratory. This may be done by checking calculations, instrument
conditions and time, and surrogate/internal standard solutions. If an error
in any of these systems cannot be established, the affected sample fraction
should be re-extracted and reanalyzed if sufficient native sample remains.
If this repeat indicates the same type of surrogate flag, the situation may
then genuinely be termed a matrix problem. You should be able to find both
sets of data(the original and repeat) and you should qualify the affected
sample fraction data as biased due to an intractable matrix or matrix interference
problem. The contractor gets paid for this additional rerun only if it turns
out that poor recovery was not his problem.
Since no clear correlation of extraction behavior of each surrogate to specific
priority pollutants has been made yet, a whole fraction such as acid, base-
neutral, pesticide, must be flagged as biased high or low when out-of-control
surrogate recoveries occur. Do this directly on the final sample data sheet or
on your review form. You might also note an estimate of the magnitude of the
bias, for example for sample E3430, 2,3,7,8-TCOn results (if positive) may have
been biased 200% high. An additional means of verifying the accuracy of reported
positive "hit" sample values is by examining the initial and subsequent checks
of the GC/MS calibration.
QA 25
This is the response factor and retention time information of the initial
injections of 3 concentrations of volatile priority pollutants. At the top of
the form is the instrument identifier- which becomes extremely important if the
contract lab has more than one GC/MS and therefore must calibrate each one used
to run your samples. You should be able to trace the instrument to the samples
run to check that the appropriate standard response factors and retention
times are used to calculate final results. Note the calibration date of
August 3-4, 1983 in the upper right hand corner. Make sure your samples and
calibration checks were run after or on this date. Highlighted is the statement
minimum mean RF (response factor) for SPCC is 0.30. This means that for all
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compounds designated as a system performance check (labelled with an asterisk
in the SPCC column) the minimum response factor of the instrument should be
0.30. Note that all SPCC compounds meet this criteria. Response factors are
obtained at the three concentration levels of 20, 100 and 200ng. You may want
to eyeball the values contributing to the mean to check for any wild deviations.
The effect of are inadequate response factor for a SPCC may be minimal, but
several- indicates poor response and the system should have been recalibrated.
t
The mean RRT column should be used to check against the positive "hits"
identified in the sample case mentioned previously. At least once every 8 hour
shift subsequent to the initial calibration, a calibration check standard
solution should be injected.
QA 26
These are the results for such a check. The OWA instrument which was initially
calibrated on August 3-4, 1983 was checked on 8/12/83 at 17:47 hours by an
injection of VOAICS812C. Note the highlighted statements "maximum % 0 for CCC
is 20" and "minimum RF for SPCC is 0.300". CCC refers to calibration check
compounds which are different than the SPCC's indicated earlier. These compounds
are used to verify that the original calibration curve is stable to within
4^20% measured as daily response factor deviation from the initial calibration
"response factor mean. All of the % D or % deviations (alias mean percent change)
are in control, as are the SPCC responses. This gives you confidence that the
GC/MS instrument quantitation of positive sample results are accurate to within
+ 20%. Compounds showing much greater deviations (for example methylene chloride
T-40.6%), acrolein (36.4%) and 4-methyl-2-pentanone indicate that quantitative
sample results for these compounds may he less accurate.
Since all response factors and tentatively identified compounds are quantified
on the basis of internal standard response, the contract requires tracking
internal standard response. Contract labs do this in a variety of ways, but
the principle and limits are the same.
QA 27
Here is a form entitled "Internal Standard Response Verification Control Chart".
These are plotted as relative response of one internal standard to the next
closest in elution over time (x axis). The top control chart is the response
(area) of D3~phenol to Dg-naphthalene, the middle one of Dg-naphthalene to D-jg-
phenanthrene and the bottom of D-|Q-phenanthrene to O^-chrysene. The limits
are +. one standard deviation. Notations of corrective action are made in
the Ubttom chart, and correspond to the low out-of-control points indicated
for 03-phenol/Og-naphthalene response seen in the top. I look at these
charts as an indication of the suitability of the internal standard in the
matrix and as a reflection of spiking technique. I do not flag any sample
data directly as a result of this audit. As a point of information, the
corrective action taken reads- recalculated manually- computers sometimes
do make poor judgement calls in area integration.
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QA 28
Did the method efficiently extract and quantitate the priority pollutants
present? The recovery of priority pollutants from an actual sample matrix
is the key to check. It, however, only tells you the effectiveness of the
method, for the sample chosen. Period. It cannot he extrapolated to every
sample in the case unless every sample matrix is known to be identical.
The matrix spike duplicate protocol will give you not only the accuracy
of the extraction in the matrix, but the precision.
QA 29
This is the contractor supplied matrix spike duplicate recovery summary
for Case 1927, low level water samples. SMO Sample # E3869 was chosen as
the volatile matrix sample and E3871 as the acid, base-neutral and pesticide
sample. Note that columns for both percent recovery and relative percent
difference are presented. The current QC limits for both are also listed
to make flagging or "asterisking" of out-of-limit data easier. Only two
flags were assigned. 2,4-dinitrotoluene recovery of 4.1.% was below the
limit of 43% and p,p'-DDT recovery of 60.9% was below the limit of 82%.
Since the other duplicate pair was in control and the precision was
acceptable, sample data for the base-neutral and pesticide fractions
for the E3871 or E3869 was not labelled as biased low. What number of
matrix flags constitutes invalidating the entire fraction's precision
and accuracy? This is a judgement call on your part. If a matrix spike
compound flagged appears at appreciable levels in the native sample, valid
recovery information is hard to obtain. Remember the rules of statistics when
looking at these large number of data points- most limits were calculated at a
90 or 95% confidence level- so try to avoid unnecessarily invalidating associated
sample results. Audits may be out simply due to random statistical error.
You have now finished pawing through the average 3 inches of paper for
a 5 sample case, you've waved your pen and raised your flags. Now it
is time to clearly and concisely present your review findings. The CRL
prefers a one page data cover with various options for final acceptability.
QA 30
This is a suggested format for a final review form. It contains the date
the data package was received- 9/15/83, and the date the reviewed data was
transmitted 9/22/83. At one time, we were shooting for a 5 day turnaround
per case, no matter how large or complex. This has not been reasonable as
of late. A three quarter to an hour per sample figure is a better estimate
of review time. This case, 1927, contained 5 samples- SMO Numbers E3S68 to
E3872, CRL Numbers 83MS08S47 to 83MS08R08. A field blank was sent, indicated
by the R08 sample designation. The review took 3.5 hours. The four major
findings of the review are listed.
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Point 1; Detection limits are not listed on the final reports. The reviewer
felt that the contractor should complete the data forms, including the detection
limits. Note at the bottom that copies of this review are sent to Or. Haeberer
who is in charge of technical support to the contract labs and CLP users, Ross
Robeson, who will take up these complaints on the next on-site audit by EMSL-LV
of the contract lab, and Robert Pritchard of SMO, who is responsible for obtaining
missing contract required deliverables.
Point 2: Pesticide and PCB chromatograms are of poor quality, difficult
to read and interpret. The reviewer was unable to confirm the presence of
the positive reported values because the standards did not agree with the
sample, and samples were not confirmed on GC/MS. The contract lab was called
and will send better copies,
Point 3: Several compounds were detected in the method blank, these were flagged
on the final reports with the Code "8", this indicated that the quanti-
tation and presence of these compounds may be due to lab induced contamination.
Point 4: Several of the surrogate spike recoveries did not meet the CLP
criteria although they were marginally by a (few percent) out, no major impact
on sample data was judged necessary by the reviewer. 1,2,3,4-TCDD surrogate
recovery for Sample E3871 was 223%, way outside limits, but no action was
taken to invalidate the 2,3,7,8-TCDD result as visual inspection of the
chromtogram and mass spectra indicated none was indeed present.
The final call on the data is "Data are preliminary, pending verification,
by the contractor laboratory", which in this case means receipt of better GC/EC
pesticide chromatograms.
This form gets directly attached to the data for the case and sent to the user,
in this case FIT. This ends the organic portion of data review. Are you ready
for the easy stuff? Inorganic data has mistakenly been slighted in the inches
of paper delivered, but they unfortunately are catching up.
QA 31
Inorganic data review, like organic, consists of eight major items. Again,
these are not listed in order of importance. These items are: Checking
Data Sheets for clarity, verifying that a complete package is present,
looking for positive lab blank contents, calibration check results and
frequency are sufficient, interference check samples are analyzed properly
for ICAP analyses, lab duplicates RPD are within acceptable limits, matrix
spike recovery is within acceptable limits, and positive field collected
blank and duplicate sample results are verified. Each of these items will
be explained in detail on the following slides, along with examples of actual
cases from several contractor laboratories.
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QA 32
Are the data sheets clear and properly coded? Illegible data sheets are
particularly frustrating in metals analyses. Labs often concoct additional
data qualifier codes which are not mentioned in the contract. Quality
assurance summaries, provided by the contract lab, are often hard to decipher
because of their design. Since we at the CRL send the report sheets for
both organic and inorganic data without transcription onto other forms,
clarity and readability of data sheets is an important part of data quality.
QA 33
This is a fortunately very readable Inorganics Analysis Data Sheet for
Sample E5356, a soil collected for Case 1787/701E. Note the code C flag
on aluminum and iron results. This indicates that the lab method blank
contained these metals at detectable concentrations and that the values
of 120 mg/Kg and 904 mg/Kg have been corrected for these concentrations
by subtraction of the blank value. The code ND/B indicates that zinc
and lead were found at detectable concentrations in the lab method blank
and that these concentrations were higher than the sample concentration.
For example, in this case the lab preparation blank contained 20 ug/1
lead, the detection limit for lead is 5 ug/1. Sample extract E5356 could
theoretically contain up to 25 ug/1 lead.
Note the Inorganic branch manager's signature in the lower right hand corner.
This is an indication that the contractor has reviewed this sheet for clarity
and completeness- and it shows.
QA 34
Is the data package complete enough to allow checking of positive results
reported? Just recently, raw data such as ICAP burn reports, and Atomic
absorption worksheets have been suggested as deliverables. Prior to
this point, all the reviewer had to verify data was the result sheet, a
list of detection limits and often unreadable QA Summary forms. The
deliverables should be adequate enough to allow you to recalculate the
metals values reported. If the raw data is insufficient, detail what
you need and send it to SMO for inclusion into the next contracts.
QA 35
This is an actual contractor lab logsheet for the graphite furnace analysis
of cadmium. The actual conditions are listed, as is the date of preparation
of the standard used (9/14/83). Details of the spike preparation and the
Conostan oil and NBS river sediment values are listed. The sequence of
cups is also listed. Note that the five point curve was analyzed first at
concentrations of 0 to lOppb, and the correlation coefficient was 0.9966.
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The actual absorbance was listed as well as the adjusted and unadjusted
concentrations. Check that the absorbances of the samples are within
the calibration curve range. Sample 5846 and 5849 were rerun later,
after dilution, as their absorbance exceeded the lOppb standard of 203.
The unadjusted concentration multiplied by dilution factor should equal the
adjusted and actual reported concentration. The blank in position 7 is the
prep blank, check this for contamination above the reporting detection limit,
here it is less than one. The EPA 475-S in position 6 was a check QC sample,
recovered at 99%.
QA 36
Are instrument and method blanks contaminated? As seen previously, lab
preparation blank contamination directly affects sample results. Check
the raw ICAP and AA data, if the QA summary indicates contamination.
Occasionally check raw data even if the contractor has not indicated a problem
to assure yourself that common contaminants such as Al, Zn, 8 are definitely
not present. One prep blank should be included for every 20 samples or case.
QA 37
Here is the QA summary supplied by the contractor for the Task II flameless
AA metals, Sb, As, Cd, Pb, Se, Tl, and Sn. The results reported across the
blank value row are the results of the zero standard, whereas the results
reported across the preparation blank row are the actual method blank results.
Note lead contamination at 20 ug/Kg. This was the cause of the previous
NO/8 code. As
a sidelight, the 129% recovery circled for selenium in spiked sample results is
out-of-control high, the contract limits are 75-125%.
QA 38
Was the instrument properly calibrated and verified? Initially, before samples
are sent to a lab, the lab must demonstrate that it can comply with the contract
detection limits by multiplying the standard deviation for calibration blank
solutions from 3 non-consecutive analysis days- with at least 10 consecutive
runs per day. Each day after this that samples are analyzed, the instrument
sensitivity expressed as absorbance for AA and gain for ICAP for the calibration
solution must be reported. Fresh calibration solution dilutions must be prepared
monthly and be traced to the original reference standards by a "t" test on data
from 5 alternating measurements of old and new standards. Once each 10 samples
an EPA QC Solution, a NBS solution and a contractor prepared standard must be
run. The % recovery of the measured values from the true cannot exceed those
in the contract which are generally around 80-120%. If an element recovery
is out-of-control, the instrument must be recalibrated and the proceeding
10 samples reanalyzed for the out-of-control element.
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QA 39
Here is the ICAP data system printout for a case to look at to verify ICAP
calibration frequency. Note that the first highlighted sample run AR 1s a
blank, then EPA, an EPA QC solution, then ICAP-3, EPA 10, two additional
contractor prepared QC solutions, and two ICP Interference checks. Eight
samples are run, then a duplicate and spike of sample 5850. This makes a
total of 10 real samples. Next comes the required EPA and contractor QC
solutions, 10 samples, etc... Raw burn numbers are converted and reported
as concentrations. Percent recovery calculations should be included on the
QA summary to enable you to check adherence to recovery acceptance limits.
QA 40
Were ICAP interelement corrections made properly? ICAP Interference check
samples are used to verify that interelement and background correction factors
are done properly. These samples should be run initially before the days
analysis of real samples and at the end of the day to give at least 2 runs per
8 hour shift. Results should be reported on the QA Summary and recoveries
should not be biased. There is no contractual acceptance range. It has been
discovered that several metals are known contaminants 1n these check samples:
Boron, manganese and barium have biased recoveries.
Here is a prime example of the boron contamination problem. Continuing and
initial calibration show no high bias, but the highlighted initial and final
ICP interference checks do- 172% and 146%. All other interference check agree-
ment is good. Associated data does not need to be flagged.
QA 42
Are the results reported of acceptable precision? At least one lab duplicate
per 20 samples or case should be prepared and analyzed. No contractual relative
percent difference limits have been set, we use 20% as the limit, and flag
sample elements as imprecise which exceed this limit. The QA summary reports
these RPD's.
QA 43
Here is a no miss situation of precision- less than compared to less than-
comparable to 0 vs. 0- great precision. As you recall, this was the driving
force to use matrix spike duplicates in organic analyses. But what if one
duplicate had shown a detected result and the other did not? Flag the sample
E5364 mercury result as imprecise and request a rerun if possible, or a resampling.
Note the out-of-control spike recovery of 58%. When this occurs, the sample
may have been rerun, and a notation made, but the contract does not require a
rerun, these must specifically be requested by you after you get the data, at
an additional cost.
-------
- 16 -
Did the method efficiently extract and quantitate the pollutants present?
The spiked sample recovery provides the key to the effect of the sample
matrix on the method efficiency. The spike solution, however, is added
to the extract, not prior to sample extraction. One spiked sample per
20 samples or case should be included and the results recorded on the
QA Summary sheet. The spike level should be at least twice the native
sample level if the native sample level is at least 10 times the detection
limit.
Recovery information for elements where the spike level swamped the native
level, or was much too low in comparison, is useless. The action outlined in
the contract when spike acceptance limits are not met 1s limited to reporting
the net response of the sample spike as a single point method of addition
calibration for the spiked sample.
QA 45
Here is a prime example of several out -of -control spike sample results.
Copper and maganese recoveries were out of limits- high at 121%, nickel, silver
and zinc were all low, in fact silver was not recovered at all at a spike level
of 1320 ug/1 . The 72% recovery seen for zinc may be due to the fact that the
original sample result used in the calculation was ND/B- not detected due to a
blank contamination of 1,070 ug/1. ND/B was considered as 0 in the calculation,
giving the low recovery. You might also look at the high silver recovery for
all calibration and IC^P interference checks. It would not be unwise to invalidate
the silver data for this case.
QA 46
Is the field and sampling precision and accuracy acceptable? If your field
team has collected a trip or field blank and field duplicates, these should be
sent with the samples in the case, either blind or labelled as such. Common
hefty level contaminants seen from using bakelite capliners on sample bottles
are Ca, Na, Mn, and phenol. High boron is seen when inadequate rinsing of
alconox occurs. When metals are detected in field blanks at measurable levels,
quantitative sample results should be flagged as possibly due to field contamination.
QA 47
In this field blank, 200 ug/1 of boron was detected, the other samples in this
case showed boron results of a similar magnitude. Boron data therefore, was
invalidated. Field duplicate precision limits have not been addressed in the
contract protocol, but we Regional reviewers generally use 20% RPO as an allowable
level .
Now that you have completed your inorganic review checklist, a summarization of
your findings should be made and attached to the data.
-------
- 17 -
QA 48
Here 1s a completed Region V review form for metals results for Case 1696,
which consisted of 18 water samples. Three major problems were cited
which were used as reasons to totally invalidate the data for Task 1 metals.
Spike recoveries were unacceptable for Be, 8, Ag and Hg. The reviewer called
the contract lab to find out if they had rerun the samples when they discovered
this. A phone memo was made to document the conversation and attached to
the review. N£ action was taken by the lab.
Duplicate precision for six metals: Cr, Co, Ni, Zn, B and Ag were erratic
and outside 20% RPD.
No ICAP interference corrections were made, which indicates that ICAP metal
data may be biased due to possible interelement interferences in the sample
matrix. Since this case was for a known enforcement action, reruns were done.
after the lab was clearly notified of these problem areas and corrected them.
QC 49
Some general data review hints are listed here to avoid discouraging you.
I realize that after looking at this slide presentation, which only represents
a small sample of the paper you must look through to assess data quality, you
must be overdosed.
FLAG. BIASED. UNACCEPTABLE. IMPRECISE. INVALID. These are not as common as you
might think. Good solid data 1s generated, it is not all questionable- but
it is your job to determine the good, the bad and the ugly.
If you have a problem with a piece of paper- For example, a chromatogram
that is unreadable, or one that's missing, call SMO. It is their responsibility
to ensure that you get a complete data package as defined in the contract.
Do you have a question on a result, a label on a chromatogram, the level of
the screen, the procedure for the calibration, or the action taken on an
out-of-control audit? Call the designated contact person at the laboratory.
Have information such as case number, affected SMO sample number, contractor
lab sample number and your exact question and document numbers written out
before hand. Document what you asked and what the answer was on a telephone
conversation record. Send a copy to the contract lab, and SMO.
Continual QC problems with a laboratory or a method should also be documented.
Notify SMO in writing of these problems and they will be covered during the
next on-s1te audit or contract preparation. You may get to feel like your
complaints are going to the Bermuda Triangle, but results are gotten by
increasing the volume and force of your concerns.
-------
- 18 -
We have looked at actual examples of review forms for CLP data. If you
develop a format similar to these to summarize your comments- do not allow
data to be released without these comments or forms attached. Cover yourself-
if your name or initials appear on CLP data, the quality of that data better
be clearly Indicated, or it will be taken carte blanche as perfect data.
I mentioned at the beginning of this presentation that you should always
keep In mind the end use of the data. Now you know why. CLP data review
is a labor and eyesight intensive process. It often requires patience in
waiting for answers from the contract lab or field team. It always involves
good technical judgement in translating study objectives to data quality
1evel.
Once you have mastered the routine menu of data packages, requests for exotic
matrices, and compounds done on unbelievably quick turnaround times need to
be addressed. Special analytical services, to quote a SMO coined phrase
"is not a candy store". You must provide not only the method but the QA for
the request. As a veteran of the school of hard QC knocks, I have taken my
lumps on inadequate methods, little to none or inappropriate QC audits and
less paper to use to assess the data. If you provide none or poor analytical
direction on SAS requests, the labs will not bid reasonable prices, they will
estimate time and resources poorly and you will pay the piper.
A 50 '
Listed here are several items to include in your SAS request. If you address
all of these, or at least realize how the data quality will be affected
without them you will be able to provide the user with known quality data.
The method you chose to have the contractor follow should be verified. If
your laboratory or another has not determined the precision and accuracy of
the method, you will need to rely on the contract lab. Any deviations that
the contract lab considers should be cleared with you after the possible
effect on the data is discussed.
If unusually low detection limits are requested, the contract lab should
verify that they can meet them. This may be accomplished by a small initial
spiking study of the blank matrix at levels equal to, twice and five times
the requested detection limit. Determination of a reasonable detection limit
should be made based on these recoveries.
If deliverables over and above those outlined in the regular contracts are
needed, list these additional paperwork requirements precisely to ensure that
you will have enough data to verify results.
Require that Instrument and method blanks be done at a prescribed frequency
and results reported with the data. Determine an action level for the lab
blank and require that no sample data be reported unless all blanks fall below
the level.
-------
- 19 -
Request additional surrogate spike compounds or different ones to monitor
the recovery of the compounds you are interested in. Choose those that
mimic the extraction behavior and are easily chromatographed. Don't forget
to define acceptable recovery limits for these surrogates and request that
action such as re-extraction be done if they are exceeded.
Matrix spikes should be requested at a suitable frequency, with the compound
or compounds of interest to determine how good the method is in the actual
matrix-. Define the concentration to be used and an acceptable recovery
range, if you know the method and matrix well. If not, you may well have
to go with the flow and take what the contractor gives you on the first
shot.
Blind QC spikes and duplicates are only as good as their disguise. I
have been known to stomp on sample tags, dip them in water, roll bottles in
vermiculite and write left handed to aid in their camouflage. I prepare these
blinds from EPA QC ampules, spikes of lab water or garden dirt. For duplicates
I rely on the field people. Reviewer know thyself in what you consider acceptable
performance on these samples before you send them out. Remember that the spike
results also are only as accurate and precise as the spikee.
A check sample alleviates some of the pressure on your spiking technique. A
check samplji is a real sample that has been analyzed over the course of several
runs and a x and sd established for the concentration level and compound(s) of
interest. The contract lab should be able to fall within your statistically
determined acceptance limits using the same method. This may be a blind, or
designated sample.
Additional field QC samples such as trip blanks, preservative blanks or equipment
rinsates should be incorporated into the SAS, with action levels determined
beforehand, so you can notify the sampling team if they are exceeded. Invalidation
of entire cases of data due to field contamination is a situation to be avoided
at all costs.
QA 51
In general, data review for SAS's is simple, as 1t follows the GIGO principle-
Garbage In, Garbage Out.
You can only expect data of the level of quality you wrote into the request
so the method supplied and the QC audits required should yield the precision
and accuracy needed to fulfill the study objectives.
Remember that there is a definite trade-off in assuring the quality of data-
QC audits mean time and time means money. There is a notion that quality is
free- unfortunately not in the contract laboratory process.
Our experience has been that contracting out for analytical services or "outhouse"
as it is coined; has become a necessity due to resource constraints. However,
with competent contract laboratories and in-house technical review, the quality
of environmental results need not suffer.
-------
- 20 -
I will now be stationed by my phone waiting to receive your questions or
comments on this presentation. My phone number is FTS or (312)353-8370.
Ask for me, Marcia Kuehl . I hope this short training/talking slide show
has been helpful in starting you on your way to data review.
-------
CLP
QUALITY ASSURANCE
AND
DATA REVIEW
-------
The Three R's
Read
'Rite
'Rithmetic
-------
BACKGROUND HOMEWORK
1. Read Statement of Work, Analytical Methods, QAIQC
Sections of Contract(s)
2. Write The Data/Sampling Objective For The Case
To Be Reviewed
3. Brush Up On Arithmetic Behind "x,SD, RPD, % Recovery
RF, RRF, RRT, % Change Calculations
-------
ORGANIC 8
1. Instrument Tune
2. Blanks
3. Positive Priority Pollutant Hits
4. Tentative ID Hits
5. Holding Times
6. Duplicates
7. Surrogates
8. Matrix Spikes
-------
ORGANIC 1
Do DFTPP and BFB
Spectra Meet Contract
Required Abundance Criteria?
Key: MS Abundance List
-------
SC/MS PERFORMANCE STANDARD - DecaHuorotriphenylphospMne
Pit* i-iu-vs tun Mo. Byiiiei'auciT Analyst
•/t
SI
«.
70
127
197
198
199
27S
365
441
442
443
Ion Abundance Criteria
30-601 of MSS 198
less than 21 of MSS (9
less than 21 of MSS 69
40-601 of MSS 198
less than 11 of MSS 198
base peak, 1001 relative abundance
5-91 of MSS 198
10-301 of MSS 198
>11 Of MSS 198
less than MSS 443
greater than 401 of MSS 198
17-231 of MSS 442
Spec «
G-^T 1
^i Q O
%
•
4^ 1 m A
K*%
^J • 0
100%
>.u%
»*%
*w
•».**
50'.
(»gV)
Spec!
dS
01
^\%
fcO%
07,
\o*'k
11*
11%
J-n
•r/.
5b7,
Spec «
31'/.
'•^
^'r/,
YIC/,
zr/.
1007.
c-f.
A3V.
17,
/of.
^7.
. 2./'/=
Coonents:
20
fentachlorophenol Response Factor » Area 166
Area 266
50
teniidfne Detectable I SOng level IT! yes PI no
Area (counts) 20ng dlO anthracene
CoTuan description
-------
INSTRUMENT TUNE AND PERFORMANCE SUMMARY
CASE NO
SAMPLE TXPS
CONTRACTOR
LEVEL
NO.'
82-AQfiQ
DFTPP and BFS Performance Results;
r^ DFTPP performance results were reviewed and found to be within specified criteria
X BFB performance results were reviewed and found to be within specified criteria
DFTPP
Mass Ion Abundance Criteria
30-60 percent of ness 198
less than 2 percent of mass 69
less than 2 percent of mass 69
40-60 percent of mass 198
less than 1 percent of mass. 198
base peak, 100 percent
5-9 percent of mass 198
10-30 percent of mass 198
greater than 1 percent of mass 198
present but less than mass 443
greater than 40 percent of mass 198
17-23 percent of mass 442
177
BFS
Ion Abundance Criteria
15-40 percent of mass 95
30-60 percent of mass 95
base peak, 100 percent
5-9 percent of mass 95
less than 2 percent of mass 174
greater than 50 percent of mass 95
5-9 percent of mass 174
greater than 95 percent but
less than 101 percent of 174
5-9 percent of mass 176
DEVIATIONS
Date/TOTe/lnst F5_Le Number Canpound
OWA
/Required
m/z . / Abundance
/
OWA /
Observed
^Abundance
nwa
CHA
CCf&ENTS
FORM VTE
-------
ORGANIC 2
Are Instruments and
Method Blanks Contaminated?
Key: Blank RIC's
-------
QUALITY CONTROL NOTICE
Tht volatile analysis of blankgBeSoT/^shows the presence of the laboratory
irtifact s1lo»at»e it «can a****- . The pre&enc* «f thi* compound Jus
resulted from the addition of an ant1foaming agent and maj- or •§/ not Actually
b« present 1n this samplt. SlUxane has not been listed as one of the non-
priority pollutant conpounds identified In this saapl*.
QUALITY ASSURANCE NOTICE
The compound 4-hydroxy-4-methyl-2-pentanone has been
detected in the semi-volatile fraction's analysis of this sample. .
This compound has been flagged in the data report as a suspected
contaminant or artifact of the analytical procedure. One
literature reference indicates that in the presence of acetone and
hyrdroxide this compound can be formed, so it 1s possible to have
been produced during extraction of the semivolatile*. The laboratory
glassware 1s rinsed prior to use with acetone, followed by methylene
chloride; if the second rinse 1s incomplete, it is possible that
residual acetone could produce, as above, this compound. Further
studies are underway to determine the source of this compound.
-------
(M
00
g
i
en
Ot
W
9
5 W
M E-
Z M
8 i
Z
o
U
63 '
GU
t
CO
o
'w
I
M •* "*•! •"
5 ij a +1
So a §
tn •* IL. iS
CO
g
H
O
M
&<
O)
U
cu
F
lo
-------
ORGANIC 3
Are Positive "Hit" Priority
Pollutants Actually Present?
Key: MS of Sample/Standard
-------
_a j •
o
-------
NO
57
58
59
*rf 9
60
A,*
Ox
62
%f ^»
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
NO
1
2
3
4
5
6
7
8
9
10
11
12
13
14
IS
16
17
18
19
20"
21
22
23
24
25
26
27
28
29
30
31
M/E SCAN TIME REF RRT HETH
NOT FOUND
&*/««r BT/M v^m
NOT rOWU
178 1658 20: 43 48 JL 002 A W
178 1666 20: 49 48 JL 007 A VB
932 .1B80 23: 3O 48 JL 137 A BB
4£ VC* ^"iS^?^^ ^M%» ' Vv^r T^rf Mto* ^»*w f ^^ vrW
202 1722" 24: 01 48 JL 162 A BB
77 1506 18: 49 48 0. 911 A W
149 1776 22: 12 48 JL 074 A BB
266 1634 20: 25 48 0. 988 A BB
240 2182 27: 16 66 JL 000 A BB
228 rgj?77 27:13 66 0.998 A BV
228 GHS9 27:22 66 1.003 A VB
NOT FOUND
149 2056 25: 42 66 0. 942 A BB
149 2209 27: 37 66 JL 012 A W
149 2437 30:28 66 1.117 A VB
NOT FOUND .
NOT FOUND
NOT FOUND
278 3600 45: 00 66 1. 650 A*BV
NOT FOUND
252 2581 32: 16 66 JL 183 A VB
NOT FOUND
RET(L) RATIO RRT2^
RATIO
1. 00
0.02
0. 16
0. 01
0. 00
O. 00
0. 01
0. 00
0. 04
0. OO
2.07
1.59
2. 28
2. 39
JL 89
2.95
1. 00
0.01
0.00
0.01
-------
IDENTIFIER SEMI-YOLATJLES
LOW LEVEL SOLID
CO^OUND QUAKT. REPORT CORRECTION DETECTION
UUJ-BER CO*OUNDS VALUE * FACTOR • RESULT LIMIT (ug,
478
460
476
479
626
401
605
607
432
417
424
604
443
414
433
>444
403 -
M31
M45
430
426
609
"405
~418
423
415
413
429
404
406
437
419
408
^•407
409
2-NITROAMILINE Vo 4000
3.N1TROANILINE \ 4000
DI BENZU" URAH ••••••••••••••••«••••
4-NlTROANILlNE •••••••••••••••••••
2.4.5-TRICHLOROPHENOL
2.4-DINITROPHENOL ; -
4-MITROr HtNOL ••••••••••••••••••••
FLUOR ENt •••••••••••••••••••••••«•
4-CHLOROPHENYL PHEMYL ETHER
DIETHYLPHTHALATE
4.6-OIN1TRO-0-CRESOL
DIPHENYLAWNE (K-NITROSO)
4-BROMOPHENYL PHEMYL ETHER
HEXACHLOROBCNZENE
PHtNANTHRtMt •••••••••••••««•••... i.^
ANTHRACENE
CJ Hftfi lUTHTUT 2.V
r LUwi\Ani ribnb •••»••«•••••••••••••• **7
PYRENE r?
1.2-DIPHENYLHYDRAZINE (AZ08ENZENE)
OI-N-BUTYLPHTHALATE
PENTACHLOROPHENOL
BEN20{ A) ANTHRACENE 2-3
CiWTStNfc ••••••••••«....•.•.•...•• •
3.3'-DICHLOROBENZIOINE
BUTYLBENZYLPHTHALATE
BIS(2-ETHYLHEXYL)PHTHAUTE
OI-M-OCTYLPHTHALATE
BbnZIUtNC •••••...••••«.•••• ••«••«
BENZO(A)PYRENE
INOENO(1.2.3-C.O)PYRENE
DIBENZO( A. H) ANTHRACENE
BENZOfG.H.nPERYLEME
400
4000
4000
400
2000
4000
400
400
400
800
400
400
400
&£ 400
400
Ho 400
?z-o 400
800
400
800
tt-» 400
/r
-------
ORGANIC 4
Are Tentatively Identified
Compound Matches Reasonable?
Key: MS of Sample/Search
-------
en
Is-
(0 P
CD
® §<5
I mca •
! in ji
in
CM
a
T
CM
CD
O
•• CO
-------
ORGANIC 5
Were Sample Extraction And
Analysis Holding Times Met?
Key: Analysis Chronicle Traffic Report
-------
EXTRACTION - GC SCREEN
NEIC II
EPA Case i
Document Control I
For: PESTICIDE
Matrix: Liquid
3-S~-/^
Dash I
EPA
Sample 1
Tare 4
sx (g)
Tare
(9)
sx Wt.
(9)
Vf
Date/
Time
Analyst
-07
/
-------
SCREEN EVALUATION FORM
NE1C »1
For: Pest1ci<1e/7££>/)
Matrix:
EPA Case I
1g/i
-------
SAMPLE NO.
PESTICIDE SCREEN
cs
24. ?
0.B
' 27.51
f ' f
RUN I 172
HEIGHT*
RT
22.38
24.99
25.78
28.82
29.23
29.48
29.69
38.77
31.21
37.76
TOTAL HGHT=
HUL FACTOR=
JUL/W/83
HEIGHT TYPE
28534 PV
41787 PB
116528 PB
46689 VB
45618 PB
24645 BB
98952 BV
1451538 SPB
52638 PB
AR/HT
8.879
8.645
8.847
8.839
8.839
8.883
8 839
6 854
8.633
24858 VB 8.112
1923788
HEIGHT*
1.483
2.168
6.857
2.427
2.371
1.281
4.72S
75.457
2.736
1.292
34.48
34.91
000253
S7
-------
ORGANIC 6
Are The Results Of Acceptable Precision?
Key: Duplicate RPD
-------
25& zwae CVK>
US MWC:
Mat
CASE
0*16. iw«»u
CWQUOS
KLATIVC KJCCWT
J-f lucre* f>Ttt*«
o-ch!oro-m-cr«soT
2.4-dlmethvlohenol
_Ifi5&)_
hsxachlorobenzene
1000
91*
1200
22 ««
t/o
0.2.
-------
ORGANIC 7
Are The Results Reported
Of Acceptable Accuracy?
Key: Surrogate Recovery
-------
FORK III
000003
-------
Initial Calibration Data - Volatile HSL Corpounds
Contractor
Case no.
Instnment Identifier
Hininun HF for SPCC IB 0.30
Contract Ho. VA 82-A069
CCM>C(JND
RKT
^
20
^
200
RF I SPCC
Chlorane thane
X.??4?
Be
thane
&gT7
Dichlarorti f luaranethane
Vinvl Chloride
Chloroe thane
Methvlene Chloride
L3JL
2S&2L.
Acrolein
Q./W
.SZfi.
Acetone
LISTS
Acrylonitrile
Carbon OisnTfirie
Trichloroflixsrome thane
1^ 1-Dichlaroethylene
1,1-Dichloroethane
trans-1 , Z-Dichloroethylene
/./<*>
2./3L5"
2.&SC*
Chlorof arm
2-Butanone
t,Z5*>
&LLL.
0.705- a.usq
1 , 2-Dichloroethane
1.1. 1-Trichlorethane
2. 636
Carbon Tetrachlaride
/,*//
/
Vinyl Acetate
EtoroiichlcDramethane
3.0X7
Carbon Tetrachlaride
1,2-Dichlc
Trlchloroethvlene
o.'fcn
Benzene
I.S3S7
1,1, 2-Trichloroethane
6S10
2-Chloroethyl vinyl ether
4-Methvl-2-pentanone
2-Hexanone
1 . 1 . 2 . 2-Ttetrachloroethane
Q3/&
TetrachloroethYlene
Toluene
Crxluii t <.**i iz
trans-1,3-DichlQropropen
M22.
Q.9/7
o"
-------
CASE SO.
INSTRUMENT IDENTIFIER
STANDARD FILE
Maximum ED for CCC is 20
CALIBRATION CHECK - VOLATILE BSL COMPOUNDS
CONTRACTOR 1SBSSB3SSSBBBSS& CONTRACT NO. VA 82-A069
QUA CALIBRATION DATE ^/3 ^
DATE %-U-*ft TIME /7
Minimum RF for SPCC is _0.300_
CCHPOJND 1
I
1
Chloromethane
BtuociiethdnB
Dichlorodi f luonromethane
Vinvl Chloride
Chloroe thane
Mfethylene Chloride
Acrolein
Acetone
Acrylonitrile
Carbon DisuLf ide
Trichlorofluorometlianc
1. 1-Dichloroethylene
1 . 1-Dichloroethane 1
trans-1 . 2*0ichloroethyljena
Qilorof onn
2-Butanone
1 . 2-Dichloroe thane
1.1, 1-Tr ichlorethane
Carbon Tetrachloride
Vonvl Acetate
Bronodichloranethane
Carbon Tetrachloride
1 f 2— Dichluji i.^>i. ufi&ns
TrichlaroethYlene
Benzene
Chlorodibraicmethane
1 . 1 . 2-TricW oroe thane
2-ChloroethYl vinyl ether
Branoform
4-MeLhvl-2-Dentanone
2-Hexanone
1.1.2. 2-Tfetrachlorcethane
Tetrachloroethvlene
Toluene
Qxlorobenzene
I trans-1, S-Duchloroytopene
Ethylbenzene
cis-1,3- Dichloropr-operie
Styrene
• o-Xylene
RF
2,051
t.SW
mi
ICLL
2.C03 1
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SEMIYGUTXL&
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ORGANIC 8
Did The Method Efficiently Extract
And Quantitate Priority Pollutants Present?
Key: Matrix Spike Recovery
-------
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION V
DATE:
SUBJECT: Review of Region V CLP Data / /
Received for Review on ?////
FROM: Curtis Ross, Director
Central Regional Laboratory
: Data User:
We have reviewed- the data for the following case(s) .
EPA Data Set No. SF J
No. of
-Samples:
SMO Case No.
D.U./Activity .
Numbers Yfaf I c
CRL No.'s
SMO Traffic No.'s
Contract Laboratory:
Hours Required
- for Review:
Following are our findings.
( ) Data are acceptable for use.
( ) Data are acceptable for use with qualifications noted above.
J^) Data are preliminary - pending verification by contractor laboratory.
( ) Data are unacceptable.
» "•
cc: Dr."Alfred Haeberer, EPA Support Services
Ross K. Robeson, EMSL-Las Vegas
Robert Pritchard. CLP-SMO
B»* FORM 12204 «EM 3-7» / .
-------
INORGANIC 8
1. Data Sheets
2. Complete Package
3. Blanks
4. Calibration Check
5. Interferences (ICP)
6. Duplicates
7. Matrix Spikes
8. Field QC
-------
INORGANIC 1
Are The Data Sheets Clear
And Properly Coded?
Key: Report Sheet, QA Summary
-------
US ENVIRONMENTAL PROTECTION ACENCY
rfTT Sample Management Office
Pa Box SIS - Alexandria. Virginia 22313
/03/357-2*90 fTS "
i-i-
SCP201C33
7S1.1V
:
INORGANICS ANALYSTS DATA-SHEET
No.
5336
LAS NAME
CASE NO.
/
LAB SAMPLE 03. NO. SS'VV £8 £94.^94 QC REPORT NO.
- 3 3
L> Aluminum
2> Chromium
3. Bartum
Bervllium
Ccbalt
6. Cfiooer
7. Iron
* NM«*
9.
TASK L (Element! to b« Identified and Measured)
10. Zinc
or
(circle ere
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HO.
12. Vanadium
Silver
VO.
16.
60.
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ug/l of ^
(circle cne
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2. Anfjr.cnv
3. Selenium
*. Thallium
TA2X 2 (Elements » be Identified and Measured}
.
3. Mefgary
4.
7. Cadmium
«. Lead
01
02
ar.aoer
-------
INORGANIC 2
Is The Data Package Complete
Enough To Allow Checking
Of Positive Results Reported?
Key: Raw Data Present
To Allow Recalculation
-------
Page
TRACE BETALS SECTION
FLAHELESS AAS ANALYSIS LOG SHEET
CLEMENT:
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Cc/
DATE
im SLIT: O, 7
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CURRENT/POWER:
BACKGROUND CORRECTION: .
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-------
INORGANIC 3
Are Instrument And Method
Blanks Contaminated?
Key: AA, ICP Printout, QA Summary
-------
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INORGANIC 4
Was The Instrument Properly
Calibrated And Verified?
Key: QA Summary
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-------
INORGANIC 5
Were ICAP Interelement
Corrections Made Properly?
Key: Standard Solution Recovery
4o
-------
! J
i
;<3:
i re O. Q «t
I ti
-------
INORGANIC 6
Are The Results Reported
Of Acceptable Precision?
Key: Duplicate RPD
-------
CASE
t A«?
INORGANICS Q,UAUTY ASSURANCE
OC HEWITT * :.
TASK 1I/COLO VAPOR
ATOMIC ABSORPTION
INITIAL CAUIAA71QM
VES1WCATHJII
STAflOAAQ
IUUIX VALUE
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mui
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Rn*
-------
INORGANIC 7
Did The Method Efficiently Extract And
Quantitate The Pollutants Present?
Key: Recovery Spiked Sample
-------
8
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-------
INORGANIC 8
Is The Field/Sampling Precision
And Accuracy Acceptable?
Key: Field Blank, Duplicate
-------
US ENVIRONMENTAL PROTECTION AGENCY
HVI Sample Management Office
P.O. Box SIS - Alexandria, Virginia 22313
703/557-2*90 FTS S-557-2*90
NEB
MAY 2 41283
535 S. Cl A<
^ $
< f 0
TASK 2 (Elements to be
^—{circle one)
«L/0
^t^>
*- Z-
«^/o
CASE NO. /^^S
QC REPORT NO. &*J
Identified and measured.)
11. Manganese
12. Zinc
13. Boron
1ft. Vanadium
15. Calcium
16. Magnesium ^*
17. Sodium ^^
identified and measured.)
3. Mercury ^»0 • 2
6. Tin
7. Silver
^ ^u(^ji/ir
Icircle one)
*- 10
1«-o
^ z^-o
«m • / 1 nr m rr ?\f rr
(circJeojic)
-^»
^ 3k,
<*/&
COMMENTS!
47
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
HEGION V
MOM. Curtis Ross. Director
'Central Regional Laboratory
TO-.Data User:
He have reviewed the data for the following case(s).
SITE
EPA DATA SET ftO.
CRL NOS.
SMO TRAFFIC MS.
CONTRACT LAB:
HOURS REQUIRED u >/
FOR REV1W: —-f-f*
Following are our findings.
, tio. D.J
Data are acceptable for use.
Data are acceptable for use with qualifications noted above.
Data are preliminary - pending verification by contractor laboratory.
Data are unacceptable.
Or. Alfred Kaeberer. EPA Support Services
Or. Gene Meier, CMSL-las Vegas
Robert Pritchart, CLP, Sample Management Office
-------
DATA REVIEW HINTS
Missing Paper? Call SMO
Questions On results? Call Lab
Document Continual QC Problems
Document Telephone Conversations
DO NOT Allow Data To Be Released
Without Review Comments Or Form Attached
Keep In Mind End Use Of Data During Review
-------
SAS QC SUGGESTIONS
Verification Of Method Adherence
Detection Limit Verification
Paperwork Requirements
Instrument And Method Blanks
Surrogate Spike(s)
Matrix Spike(s)
Blind QC Spike
Blind Duplicates
Check Sample
Field QC Samples
-------
SAS DATA REVIEW
THE GIGO PRINCIPLE
1. Can Expect Data Of Level Of Quality
YOU Wrote Into The Request So ...
2. Contract Method Supplied Or Chosen
Should Be Of Known P&A
3. Remember: QC=Time=$
------- |