[Federal Register Volume 83, Number 49 (Tuesday, March 13, 2018)]
[Notices]
[Pages 10945-10946]
[FR Doc No: 2018-05005]

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DEPARTMENT OF TRANSPORTATION

Federal Motor Carrier Safety Administration

[Docket No. FMCSA-2017-0267]

Agency Information Collection Activities; Renewal of an Approved
Information Collection: Motor Carrier Records Change Form

AGENCY: Federal Motor Carrier Safety Administration (FMCSA), DOT.

ACTION: Notice and request for comments.

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SUMMARY: In accordance with the Paperwork Reduction Act of 1995, FMCSA
announces its plan to submit the Information Collection Request (ICR)
described below to the Office of Management and Budget (OMB) for review
and approval. The purpose of this ICR titled ``Motor Carrier Records
Change Form,'' is to more efficiently collect information the Office of
Registration and Safety Information (MC-RS) requires to process name
and address changes and reinstatements of operating authority.

DATES: Please send your comments by April 12, 2018. OMB must receive
your comments by this date in order to act quickly on the ICR.

ADDRESSES: All comments should reference Federal Docket Management
System (FDMS) Docket Number FMCSA-2017-0267. Interested persons are
invited to submit written comments on the proposed information
collection to the Office of Information and Regulatory Affairs, Office
of Management and Budget. Comments should be addressed to the attention
of the Desk Officer, Department of

Transportation/Federal Motor Carrier Safety Administration, and sent
via electronic mail to [email protected], or faxed to (202)
395-6974, or mailed to the Office of Information and Regulatory
Affairs, Office of Management and Budget, Docket Library, Room 10102,
725 17th Street NW, Washington, DC 20503.

FOR FURTHER INFORMATION CONTACT: Jeff Secrist, Division Chief, East-
South Division, FMCSA Office of Registration and Safety Information,
Department of Transportation, Federal Motor Carrier Safety
Administration, 6th Floor, West Building, 1200 New Jersey Avenue SE,
Washington, DC 20590-0001. Telephone:<PHONE_NUMBER> Email Address:
[email protected]. Office hours are from 9 a.m. to 5 p.m., Monday
through Friday, except Federal Holidays.

SUPPLEMENTARY INFORMATION:
    Title: Motor Carrier Records Change Form.
    OMB Control Number: 2126-0060.
    Type of Request: Renewal information collection.
    Respondents: For-hire motor carriers, brokers and freight
forwarders.
    Estimated Number of Respondents: 44,900.
    Estimated Time per Response: 15 minutes per response.
    Expiration Date: July 31, 2018.
    Frequency of Response: On occasion.
    Estimated Total Annual Burden: 11,225 hours [44,900 annual
responses x 0.25 hours].

Background

    FMCSA registers for-hire motor carriers under 49 U.S.C. 13902,
surface freight forwarders under 49 U.S.C. 13903, and property brokers
under 49 U.S.C. 13904. Each registration is effective from the date
specified under 49 U.S.C. 13905(c). 49 CFR part 365.413 states for-hire
motor carriers, brokers and freight forwarders are required to notify
the Office of Registration and Safety Information when they change the
name or form of business. Currently, the name change request can be
filed online through the Licensing and Insurance (L&I) website, or
companies can fax or mail a letter requesting either name or address
changes. Carriers can also request reinstatement of a revoked operating
authority either via fax or online via the L&I website. About 39% of
name change, address change, and reinstatement requests are received by
mail; 38% are filed online; and 23% are filed by faxing a request
letter to MC-RS. The information collected is then entered in the L&I
database by FMCSA staff. This enables FMCSA to maintain up-to-date
records so that the agency can recognize the entity in question in case
of enforcement actions or other procedures required to ensure that the
carrier is fit, willing and able to provide for-hire transportation
services, and so that entities whose authority has been revoked can
resume operation if they are not otherwise blocked from doing so. This
multi-purpose form simplifies the process of gathering the information
needed to process the entities' requests in a timely manner, with the
least amount of effort for all parties involved. This multi-purpose
form is filed by registrants on an as-needed basis. This multi-purpose
form is on the FMCSA website so entities could access and print/fax/
email the form to MC-RS.
    The form prompts users to report the following data points
(whichever are relevant to their records change request): (1) What are
the legal/doing business as (dba) names of the entity/representative?
(2) What is the contact information of entity/representatives (phone
number, address, fax number, email address)? (3) What are the requested
changes to name or address of entity? (4) What is the docket MC/MX/FX
number of the entity? (5) What is the US DOT number of the entity? (6)
Is there any change in ownership, management or control of the entity?
(7) What kind of changes is the entity making to the company? (8) Which
authority does the entity/representative wish to reinstate, motor
carrier or broker? (9) Does the entity/representative authorize the fee
for the name change or reinstatement? (10) Does the entity/
representative authorize the reinstatement of operating authority or
name/address change? (11) What is the credit card information (name,
number, expiration date, address, date) for the card used to pay the
fee?
    The Agency received three comments on the 60-day notice (82 FR
50481). The comments were not directly related to the information
collection. Therefore, FMCSA did not make any changes to the
information collection.
    Public Comments Invited: You are asked to comment on any aspect of
this information collection, including: (1) Whether the proposed
collection is necessary for the FMCSA to perform its functions; (2) the
accuracy of the estimated burden; (3) ways for the FMCSA to enhance the
quality, usefulness, and clarity of the collected information; and (4)
ways that the burden could be minimized without reducing the quality of
the collected information.

    Issued under the authority delegated in 49 CFR 1.87 on: March 5,
2018.
G. Kelly Regal,
Associate Administrator for Office of Research and Information
Technology.
[FR Doc. 2018-05005 Filed 3-12-18; 8:45 am]
 BILLING CODE 4910-EX-P


[Federal Register Volume 77, Number 13 (Friday, January 20, 2012)]
[Notices]
[Page 2974]
[FR Doc No: 2012-1075]

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DEPARTMENT OF ENERGY

Federal Energy Regulatory Commission

[Project No. 14341-000]

Longview Energy Exchange, LLC; Notice of Preliminary Permit
Application Accepted for Filing and Soliciting Comments, Motions To
Intervene, and Competing Applications

    On January 3, 2012, Longview Energy Exchange, LLC, filed an
application for a preliminary permit, pursuant to section 4(f) of the
Federal Power Act (FPA), proposing to study the feasibility of the
Longview Pumped Storage Project (project) to be located Ash Fork City,
Yavapai County, Arizona. The sole purpose of a preliminary permit, if
issued, is to grant the permit holder priority to file a license
application during the permit term. A preliminary permit does not
authorize the permit holder to perform any land-disturbing activities
or otherwise enter upon lands or waters owned by others without the
owners' express permission.
    The proposed project would consist of the following: (1) Two upper
reservoirs constructed of rock fill each with a dam drainage system;
(2) a single lower reservoir dam constructed of earth fill materials
with an internal dam drainage system; (3) concrete inlet-outlet
structures at both upper reservoirs equipped with trash racks; (4)
water conductors constructed of concrete-lined pressure tunnels; (5)
three 12.5-foot-diameter penstocks serving the pump-turbine units
associated with both upper reservoirs; (6) surge control facilities;
(7) a 500-foot-long by 100-foot-wide and 150-foot-high reinforced
concrete powerhouse containing 6 units; (8) a switchyard to be located
near the powerhouse; (9) a 38-mile-long, 500-kilovolt (kV) transmission
line extending from the project to an interconnection with the existing
Arizona Public Service owned and operated Eldorado-Moenkopi 500-kV
line; (10) a 27-mile-long, 500-kilovolt (kV) transmission line
extending from the project to an interconnection with an existing
Western Area Power Administration owned and operated 230-kV (to be
upgraded to 500-kV); and (11) appurtenant facilities. The estimated
annual generation of the Longview Pumped Storage Project would be
35,040 gigawatt-hours.
    Applicant Contact: Mr. Mitchell M. Wexler, Manager, Longview Energy
Exchange, 13397 Lakefront Drive, Saint Louis, Missouri 63045; phone:
(314) 739-5555.
    FERC Contact: Mary Greene; phone:<PHONE_NUMBER>.
    Deadline for filing comments, motions to intervene, competing
applications (without notices of intent), or notices of intent to file
competing applications: 60 days from the issuance of this notice.
Competing applications and notices of intent must meet the requirements
of 18 CFR 4.36. Comments, motions to intervene, notices of intent, and
competing applications may be filed electronically via the Internet.
See 18 CFR 385.2001(a)(1)(iii) and the instructions on the Commission's
Web site http://www.ferc.gov/docs-filing/efiling.asp. Commenters can
submit brief comments up to 6,000 characters, without prior
registration, using the eComment system at http://www.ferc.gov/docs-filing/ecomment.asp. You must include your name and contact information
at the end of your comments. For assistance, please contact FERC Online
Support at<EMAIL_ADDRESS>or toll free at 1-(866) 208-3676,
or for TTY,<PHONE_NUMBER>. Although the Commission strongly encourages
electronic filing, documents may also be paper-filed. To paper-file,
mail an original and seven copies to: Kimberly D. Bose, Secretary,
Federal Energy Regulatory Commission, 888 First Street NE., Washington,
DC 20426.
    More information about this project, including a copy of the
application, can be viewed or printed on the ``eLibrary'' link of
Commission's Web site at http://www.ferc.gov/docs-filing/elibrary.asp.
Enter the docket number (P-14341) in the docket number field to access
the document. For assistance, contact FERC Online Support.

    Dated: January 12, 2012.
 Kimberly D. Bose,
 Secretary.
[FR Doc. 2012-1075 Filed 1-19-12; 8:45 am]
BILLING CODE 6717-01-P


[Federal Register Volume 84, Number 26 (Thursday, February 7, 2019)]
[Notices]
[Pages 2527-2528]
[FR Doc No: 2019-01517]

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DEPARTMENT OF HEALTH AND HUMAN SERVICES

Food and Drug Administration

[Docket No. FDA-2018-D-1334]

Opioid Use Disorder: Developing Depot Buprenorphine Products for
Treatment; Guidance for Industry; Availability

AGENCY: Food and Drug Administration, HHS.

ACTION: Notice of availability.

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SUMMARY: The Food and Drug Administration (FDA or Agency) is announcing
the availability of a final guidance for industry entitled ``Opioid Use
Disorder: Developing Depot Buprenorphine Products for Treatment.'' This
guidance reflects the Agency's current thinking regarding drug product
development and trial design issues relevant to the study of depot
buprenorphine products (i.e., modified-release products for injection
or implantation) for the treatment of opioid use disorder. Passive-
compliance formulations such as sustained-release injectable depots and
implants can provide effective treatment of opioid use disorder in a
treatment paradigm that may be less subject to misuse, abuse, or
accidental exposure compared to self-administered formulations such as
transmucosal tablets and films. This guidance finalizes the draft
guidance entitled ``Opioid Dependence: Developing Depot Buprenorphine
Products for Treatment'' issued in April 2018.

DATES: The announcement of the guidance is published in the Federal
Register on February 7, 2019.

ADDRESSES: You may submit either electronic or written comments on
Agency guidances at any time as follows:

Electronic Submissions

    Submit electronic comments in the following way:
     Federal eRulemaking Portal: https://www.regulations.gov.
Follow the instructions for submitting comments. Comments submitted
electronically, including attachments, to https://www.regulations.gov
will be posted to the docket unchanged. Because your comment will be
made public, you are solely responsible for ensuring that your comment
does not include any confidential information that you or a third party
may not wish to be posted, such as medical information, your or anyone
else's Social Security number, or confidential business information,
such as a manufacturing process. Please note that if you include your
name, contact information, or other information that identifies you in
the body of your comments, that information will be posted on https://www.regulations.gov.
     If you want to submit a comment with confidential
information that you do not wish to be made available to the public,
submit the comment as a written/paper submission and in the manner
detailed (see ``Written/Paper Submissions'' and ``Instructions'').

Written/Paper Submissions

    Submit written/paper submissions as follows:

     Mail/Hand Delivery/Courier (for written/paper
submissions): Dockets Management Staff (HFA-305), Food and Drug
Administration, 5630 Fishers Lane, Rm. 1061, Rockville, MD 20852.
     For written/paper comments submitted to the Dockets
Management Staff, FDA will post your comment, as well as any
attachments, except for information submitted, marked and identified,
as confidential, if submitted as detailed in ``Instructions.''
    Instructions: All submissions received must include the Docket No.
FDA-2018-D-1334 for ``Opioid Use Disorder: Developing Depot
Buprenorphine Products for Treatment.'' Received comments will be
placed in the docket and, except for those submitted as ``Confidential
Submissions,'' publicly viewable at https://www.regulations.gov or at
the Dockets Management Staff between 9 a.m. and 4 p.m., Monday through
Friday.
     Confidential Submissions--To submit a comment with
confidential information that you do not wish to be made publicly
available, submit your comments only as a written/paper submission. You
should submit two copies total. One copy will include the information
you claim to be confidential with a heading or cover note that states
``THIS DOCUMENT CONTAINS CONFIDENTIAL INFORMATION.'' The Agency will
review this copy, including the claimed confidential information, in
its consideration of comments. The second copy, which will have the
claimed confidential information redacted/blacked out, will be
available for public viewing and posted on https://www.regulations.gov.
Submit both copies to the Dockets Management Staff. If you do not wish
your name and contact information to be made publicly available, you
can provide this information on the cover sheet and not in the body of
your comments and you must identify this information as
``confidential.'' Any information marked as ``confidential'' will not
be disclosed except in accordance with 21 CFR 10.20 and other
applicable disclosure law. For more information about FDA's posting of
comments to public dockets, see 80 FR 56469, September 18, 2015, or
access the information at: https://www.gpo.gov/fdsys/pkg/FR-2015-09-18/pdf/2015-23389.pdf.
    Docket: For access to the docket to read background documents or
the electronic and written/paper comments received, go to https://www.regulations.gov and insert the docket number, found in brackets in
the heading of this document, into the ``Search'' box and follow the
prompts and/or go to the Dockets Management Staff, 5630 Fishers Lane,
Rm. 1061, Rockville, MD 20852.
    You may submit comments on any guidance at any time (see 21 CFR
10.115(g)(5)).
    Submit written requests for single copies of this guidance to the
Division of Drug Information, Center for Drug Evaluation and Research,
Food and Drug Administration, 10001 New Hampshire Ave., Hillandale
Building, 4th Floor, Silver Spring, MD 20993-0002. Send one self-
addressed adhesive label to assist that office in processing your
requests. See the SUPPLEMENTARY INFORMATION section for electronic
access to the guidance document.

FOR FURTHER INFORMATION CONTACT: Silvana Borges, Center for Drug
Evaluation and Research, Food and Drug Administration, 10903 New
Hampshire Ave., Bldg. 22, Rm. 3200, Silver Spring, MD 20993-0002, 301-
796-0963.

SUPPLEMENTARY INFORMATION:

I. Background

    FDA is announcing the availability of a guidance for industry
entitled ``Opioid Use Disorder: Developing Depot Buprenorphine Products
for Treatment.'' This guidance reflects the Agency's current thinking
regarding drug product development and trial design issues relevant to
the study of depot buprenorphine products (i.e., modified-release
products for injection or implantation) for the treatment of opioid use
disorder. Passive-compliance formulations such as sustained-release
injectable depots and implants can provide effective treatment of
opioid use disorder in a treatment paradigm that may be less subject to
misuse, abuse, or accidental exposure compared to self-administered
formulations such as transmucosal tablets and films. This finalizes the
draft guidance entitled ``Opioid Dependence: Developing Depot
Buprenorphine Products for Treatment'' issued on April 23, 2018 (83 FR
17666). In addition to editorial changes made primarily for
clarification, changes from the draft to the final guidance include
replacement of opioid dependence with opioid use disorder, the addition
of language noting that patients with moderate-severe opioid use
disorder should be enrolled in clinical trials, and clarification of
the cumulative responder curve efficacy analysis.
    This guidance is being issued consistent with FDA's good guidance
practices regulation (21 CFR 10.115). The guidance represents the
current thinking of FDA on ``Opioid Use Disorder: Developing Depot
Buprenorphine Products for Treatment.'' It does not establish any
rights for any person and is not binding on FDA or the public. You can
use an alternative approach if it satisfies the requirements of the
applicable statutes and regulations. This guidance is not subject to
Executive Order 12866.

II. Paperwork Reduction Act of 1995

    This guidance refers to previously approved collections of
information that are subject to review by the Office of Management and
Budget (OMB) under the Paperwork Reduction Act of 1995 (44 U.S.C. 3501-
3520). The collections of information in 21 CFR parts 312 and 314 have
been approved under OMB control numbers 0910-0014 and 0910-0001,
respectively. The collection of information in 21 CFR parts 50 and 56
have been approved under OMB control numbers 0910-0755 and 0910-0130.

III. Electronic Access

    Persons with access to the internet may obtain the guidance at
either https://www.fda.gov/Drugs/GuidanceComplianceRegulatoryInformation/Guidances/default.htm or
https://www.regulations.gov.

    Dated: January 24, 2019.
Leslie Kux,
Associate Commissioner for Policy.
[FR Doc. 2019-01517 Filed 2-6-19; 8:45 am]
 BILLING CODE 4164-01-P


    Fw: Boiler MACT PreambleRule    RobertJ Wayland    to:  Mary Johnson                                                12/19/2012 05:32 PM                                                             12/19/2012 05:32 PM

 From: RobertJ Wayland/RTP/USEPA/US

 To: Mary Johnson/RTP/USEPA/US@EPA

----- Forwarded by RobertJ Wayland/RTP/USEPA/US on 12/19/2012 05:32 PM -----

From:	"Higgins, Cortney"<EMAIL_ADDRESS>To:	Jim Eddinger/RTP/USEPA/US@EPA Cc:	RobertJ Wayland/RTP/USEPA/US@EPA Date:	12/19/2012 05:29 PM Subject:	RE: Boiler MACT PreambleRule

Hi Jim, Below are a couple of interagency comments that have come in today on this afternoon's drafts:   Major Source Rule. Page 198. For consistency with equation 10, we believe the symbols X1 and Y1 in equation 11 should be small x prime (small x with a bar over the top) and small y prime (small y with a bar over the top).  (Rephrased version of comment that was submitted by the SSC on 18 December 2012.)  As an aside, in equation 10, perhaps X1 and Y1 should be Xi and Yi since it is a summation equation from i to n.   Area Source Rule.  Consider revising the definitions of 10-day rolling average and 30-day rolling average in the area source rule to be consistent with the major source rule to incorporate the 240 hour and 720 hour of valid operating data criteria, respectively. Both rules should probably exclude hours during startup and shutdown as well as unit down time, from the rolling average calculations.    Regards, Cortney   From<EMAIL_ADDRESS><EMAIL_ADDRESS>Sent: Wednesday, December 19, 2012 3:50 PM To: Higgins, Cortney Cc<EMAIL_ADDRESS>Subject: RE: Boiler MACT PreambleRule   Cortney,

Please replace the redline version I sent you earlier this afternoon with this version. A few edits were made to the fourth year language on pages 26 -28.

(See attached file: EO 12866 NESHAP for Major Sources Industrial, Commercial, and Institutional Boilers and Process Heaters 2060 121912 redline w 121312v2.docx)

Jim _______________ James A. Eddinger Energy Strategies Group Sector Policies and Programs Division 919-541-5426


[Federal Register Volume 85, Number 172 (Thursday, September 3, 2020)]
[Notices]
[Pages 55019-55020]
[FR Doc No: 2020-19495]

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DEPARTMENT OF HOMELAND SECURITY

Coast Guard

[Docket No. USCG-2020-0185; OMB Control Number 1625-0102 ]

Collection of Information Under Review by Office of Management
and Budget

AGENCY: Coast Guard, DHS.

ACTION: Thirty-day notice requesting comments.

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SUMMARY: In compliance with the Paperwork Reduction Act of 1995 the
U.S. Coast Guard is forwarding an Information Collection Request (ICR),
abstracted below, to the Office of Management and Budget (OMB), Office
of Information and Regulatory Affairs (OIRA), requesting an extension
of its approval for the following collection of information: 1625-0102,
National Response Resource Inventory; without

change. Our ICR describes the information we seek to collect from the
public. Review and comments by OIRA ensure we only impose paperwork
burdens commensurate with our performance of duties.

DATES: You may submit comments to the Coast Guard and OIRA on or before
October 5, 2020.

ADDRESSES: Comments to the Coast Guard should be submitted using the
Federal eRulemaking Portal at https://www.regulations.gov. Search for
docket number [USCG-2020-0185]. Written comments and recommendations to
OIRA for the proposed information collection should be sent within 30
days of publication of this notice to https://www.reginfo.gov/public/do/PRAMain.
    Find this particular information collection by selecting
``Currently under 30-day Review--Open for Public Comments'' or by using
the search function.
    A copy of the ICR is available through the docket on the internet
at https://www.regulations.gov. Additionally, copies are available
from: Commandant (CG-6P), Attn: Paperwork Reduction Act Manager, U.S.
Coast Guard, 2703 Martin Luther King Jr. Ave SE, Stop 7710, Washington,
DC 20593-7710.

FOR FURTHER INFORMATION CONTACT: A.L. Craig, Office of Privacy
Management, telephone<PHONE_NUMBER>, or fax<PHONE_NUMBER>, for questions
on these documents.

SUPPLEMENTARY INFORMATION:

Public Participation and Request for Comments

    This notice relies on the authority of the Paperwork Reduction Act
of 1995; 44 U.S.C. chapter 35, as amended. An ICR is an application to
OIRA seeking the approval, extension, or renewal of a Coast Guard
collection of information (Collection). The ICR contains information
describing the Collection's purpose, the Collection's likely burden on
the affected public, an explanation of the necessity of the Collection,
and other important information describing the Collection. There is one
ICR for each Collection. The Coast Guard invites comments on whether
this ICR should be granted based on the Collection being necessary for
the proper performance of Departmental functions. In particular, the
Coast Guard would appreciate comments addressing: (1) The practical
utility of the Collection; (2) the accuracy of the estimated burden of
the Collection; (3) ways to enhance the quality, utility, and clarity
of information subject to the Collection; and (4) ways to minimize the
burden of the Collection on respondents, including the use of automated
collection techniques or other forms of information technology.
Consistent with the requirements of Executive Order 13771, Reducing
Regulation and Controlling Regulatory Costs, and Executive Order 13777,
Enforcing the Regulatory Reform Agenda, the Coast Guard is also
requesting comments on the extent to which this request for information
could be modified to reduce the burden on respondents. These comments
will help OIRA determine whether to approve the ICR referred to in this
Notice.
    We encourage you to respond to this request by submitting comments
and related materials. Comments to Coast Guard or OIRA must contain the
OMB Control Number of the ICR. They must also contain the docket number
of this request, [USCG-2020-0185], and must be received by October 5,
2020.

Submitting Comments

    We encourage you to submit comments through the Federal eRulemaking
Portal at https://www.regulations.gov. If your material cannot be
submitted using https://www.regulations.gov, contact the person in the
FOR FURTHER INFORMATION CONTACT section of this document for alternate
instructions. Documents mentioned in this notice, and all public
comments, are in our online docket at https://www.regulations.gov and
can be viewed by following that website's instructions. Additionally,
if you go to the online docket and sign up for email alerts, you will
be notified when comments are posted.
    We accept anonymous comments. All comments to the Coast Guard will
be posted without change to https://www.regulations.gov and will
include any personal information you have provided. For more about
privacy and submissions to the Coast Guard in response to this
document, see DHS's eRulemaking System of Records notice (85 FR 14226,
March 11, 2020). For more about privacy and submissions to OIRA in
response to this document, see the https://www.reginfo.gov, comment-
submission web page. OIRA posts its decisions on ICRs online at https://www.reginfo.gov/public/do/PRAMain after the comment period for each
ICR. An OMB Notice of Action on each ICR will become available via a
hyperlink in the OMB Control Number: 1625-0102.

Previous Request for Comments

    This request provides a 30-day comment period required by OIRA. The
Coast Guard published the 60-day notice (85 FR 28646, May 13, 2020)
required by 44 U.S.C. 3506(c)(2). We received four submissions to the
60-day Notice. Three submissions were unrelated to the Notice, and one
submission had four ICR-related comments. The first comment noted that
the Response Resource Inventory (RRI) is a practical and useful tool
for the Coast Guard to maintain a national database for response
equipment. The second comment stated that the estimated time and cost
burden seem to be accurate. The third comment suggested that the Coast
Guard should consider enhancing the RRI by updating the database
technology and creating a public-facing portal to allow non-OSRO (Oil
Spill Removal Organizations) to access the inventory. Because the data
entered into RRI, including OSRO inventories, is categorized as For
Official Use Only (FOUO), it is not releasable to the public. The
fourth comment suggested that the Coast Guard modernize data collection
technology to reduce the burden of information collection through
automation. Due to resource constraints, the Coast Guard has not yet
developed a plan to modernizing data collection through automation. In
response to the comments, no changes were made to the Collection.

Information Collection Request

    Title: National Response Resource Inventory.
    OMB Control Number: 1625-0102.
    Summary: The information is needed to improve the effectiveness of
deploying reponse equipment in the event of an oil spill. It may also
be used in the development of contingency plans.
    Need: Section 4202 of the Oil Pollution Act of 1990 (Pub. L. 101-
380) requires the Coast Guard to compile and maintain a comprehensive
list of spill removal equipment in a response resource inventory (RRI).
This collection helps fulfill that requirement.
    Forms: None.
    Respondents: Oil spill removal organizations.
    Frequency: On occasion.
    Hour Burden Estimate: The estimated burden remains 1,378 hours a
year.

    Authority:  The Paperwork Reduction Act of 1995; 44 U.S.C.
chapter 35, as amended.

    Dated: August 28, 2020.
Kathleen Claffie,
Chief, Office of Privacy Management, U.S. Coast Guard.
[FR Doc. 2020-19495 Filed 9-2-20; 8:45 am]
BILLING CODE 9110-04-P


[Federal Register Volume 83, Number 139 (Thursday, July 19, 2018)]
[Proposed Rules]
[Pages 34072-34074]
[FR Doc No: 2018-15304]

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DEPARTMENT OF TRANSPORTATION

Federal Aviation Administration

14 CFR Part 39

[Docket No. FAA-2018-0648; Product Identifier 2017-SW-087-AD]
RIN 2120-AA64

Airworthiness Directives; Leonardo S.p.A. Helicopters

AGENCY: Federal Aviation Administration (FAA), DOT.

ACTION: Notice of proposed rulemaking (NPRM).

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SUMMARY: We propose to adopt a new airworthiness directive (AD) for
Leonardo S.p.A. (Leonardo) Model AB139 and AW139 helicopters. This
proposed AD would require replacing screws installed on the left and
right main landing gear (MLG) shock absorber assembly. This proposed AD
is prompted by a report that some screws may have been manufactured
without meeting specifications. The actions of this proposed AD are
intended to correct an unsafe condition on these helicopters.

DATES: We must receive comments on this proposed AD by September 17,
2018.

ADDRESSES: You may send comments by any of the following methods:
     Federal eRulemaking Docket: Go to http://www.regulations.gov. Follow the online instructions for sending your
comments electronically.
     Fax:<PHONE_NUMBER>.
     Mail: Send comments to the U.S. Department of
Transportation, Docket Operations, M-30, West Building Ground Floor,
Room W12-140, 1200 New Jersey Avenue SE, Washington, DC 20590-0001.
     Hand Delivery: Deliver to the ``Mail'' address between 9
a.m. and 5 p.m., Monday through Friday, except Federal holidays.

Examining the AD Docket

    You may examine the AD docket on the internet at http://www.regulations.gov by searching for and locating Docket No. FAA-2018-
0648; or in person at Docket Operations between 9 a.m. and 5 p.m.,
Monday through Friday, except Federal holidays. The AD docket contains
this proposed AD, the European Aviation Safety Agency (EASA) AD, the
economic evaluation, any comments received, and other information. The
street address for Docket Operations (telephone<PHONE_NUMBER>) is in the
ADDRESSES section. Comments will be available in the AD docket shortly
after receipt.
    For service information identified in this proposed rule, contact
Leonardo S.p.A. Helicopters, Matteo Ragazzi, Head of Airworthiness,
Viale G.Agusta 520, 21017 C.Costa di Samarate (Va) Italy; telephone
+39-0331-711756; fax +39-0331-229046; or at http://www.leonardocompany.com/-/bulletins. You may review the referenced
service information at the FAA, Office of the Regional Counsel,
Southwest Region, 10101 Hillwood Pkwy., Room 6N-321, Fort Worth, TX
76177.

FOR FURTHER INFORMATION CONTACT: David Hatfield, Aviation Safety
Engineer, Safety Management Section, Rotorcraft Standards Branch, FAA,
10101 Hillwood Pkwy., Fort Worth, TX 76177; telephone<PHONE_NUMBER>;
email [email protected].

SUPPLEMENTARY INFORMATION:

Comments Invited

    We invite you to participate in this rulemaking by submitting
written comments, data, or views. We also invite comments relating to
the economic, environmental, energy, or federalism impacts that might
result from adopting the proposals in this document. The most helpful
comments reference a specific portion of the proposal, explain the
reason for any recommended change, and include supporting data. To
ensure the docket does not contain duplicate comments, commenters
should send only one copy of written comments, or if comments are filed
electronically, commenters should submit only one time.
    We will file in the docket all comments that we receive, as well as
a report summarizing each substantive public contact with FAA personnel
concerning this proposed rulemaking. Before acting on this proposal, we
will consider all comments we receive on or before the closing date for
comments. We will consider comments filed after the comment period has
closed if it is possible to do so without incurring expense or delay.
We may change this proposal in light of the comments we receive.

Discussion

    EASA, which is the Technical Agent for the Member States of the
European Union, has issued EASA AD No. 2016-077, dated April 19, 2016,
to correct an unsafe condition for Finmeccanica S.p.A. (previously
Agusta) Model AB139 and AW139 helicopters if equipped with kit
``Increased Gross Weight 6800 kg'' part number (P/N) 4G0000F00111
(kit). EASA advises of a manufacturing issue with the standard screws
(P/N NAS1351-5H12P) installed on MLG shock absorber assembly P/N
1652B0000-01. According to EASA, a material analysis shows that the MLG
shock absorber screws may have a lower fatigue life than the screws
used during the certification fatigue tests. EASA states the affected
MLG units have been identified by serial number. EASA also advises that
this unsafe condition, if not detected and corrected, could result in
failure of the MLG shock absorber, collapse or retraction of the MLG,
and subsequent damage to the helicopter and injury to occupants.
    To correct this condition, the EASA AD requires replacing each
standard screw with a new screw P/N 1652A0001-01 and re-identifying the
serial number of each MLG shock absorber assembly that has the new
screw installed, and prohibits installing any affected MLG shock
absorber assembly unless the screw has been replaced.

FAA's Determination

    These helicopters have been approved by the aviation authority of
Italy and are approved for operation in the United States. Pursuant to
our bilateral agreement with Italy, EASA, its technical representative,
has notified us of the unsafe condition described in its AD. We are
proposing this AD because we evaluated all known relevant information
and determined that an unsafe condition is likely to exist or develop
on other products of the same type design.

Related Service Information

    We reviewed Finmeccanica Bollettino Tecnico No. 139-397, dated
April 7, 2016, which contains procedures for replacing the standard
screws installed on the left and right MLG assembly and for re-
identifying the MLG shock absorber assembly P/N and the MLG assembly S/
N.

Proposed AD Requirements

    This proposed AD would require replacing each standard screw P/N
NAS1351-5H12P with a screw P/N 1652A0001-01 and re-identifying the
serial number of the MLG assembly within the following compliance
times:

     For MLG assemblies with 26,800 or more landings, within
100 hours time-in-service (TIS).
     For MLG assemblies with between 22,000 and 26,799
landings, within 300 hours TIS or before the MLG assembly accumulates
27,200 landings, whichever occurs first.
     For MLG assemblies with less than 22,000 landings, within
1,200 hours TIS or before the MLG assembly accumulates 23,200 landings,
whichever occurs first.
    This proposed AD would also prohibit installing an MLG assembly on
any helicopter unless the screw has been replaced.

Costs of Compliance

    We estimate that this proposed AD would affect 111 helicopters of
U.S. Registry.
    We estimate that operators may incur the following costs in order
to comply with this proposed AD, based on an average labor rate of $85
per work-hour. Replacing the screws on the left and right MLG
assemblies would require about 16 work-hours and $200 for parts, for a
total cost of $1,560 per helicopter and $173,160 for the U.S. fleet.
    According to Finmeccanica's service information, some of the costs
of this proposed AD may be covered under warranty, thereby reducing the
cost impact on affected individuals. We do not control warranty
coverage by Finmeccanica. Accordingly, we have included all costs in
our cost estimate.

Authority for This Rulemaking

    Title 49 of the United States Code specifies the FAA's authority to
issue rules on aviation safety. Subtitle I, section 106, describes the
authority of the FAA Administrator. ``Subtitle VII: Aviation
Programs,'' describes in more detail the scope of the Agency's
authority.
    We are issuing this rulemaking under the authority described in
``Subtitle VII, Part A, Subpart III, Section 44701: General
requirements.'' Under that section, Congress charges the FAA with
promoting safe flight of civil aircraft in air commerce by prescribing
regulations for practices, methods, and procedures the Administrator
finds necessary for safety in air commerce. This regulation is within
the scope of that authority because it addresses an unsafe condition
that is likely to exist or develop on products identified in this
rulemaking action.

Regulatory Findings

    We determined that this proposed AD would not have federalism
implications under Executive Order 13132. This proposed AD would not
have a substantial direct effect on the States, on the relationship
between the national Government and the States, or on the distribution
of power and responsibilities among the various levels of government.
    For the reasons discussed, I certify this proposed regulation:
    1. Is not a ``significant regulatory action'' under Executive Order
12866;
    2. Is not a ``significant rule'' under the DOT Regulatory Policies
and Procedures (44 FR 11034, February 26, 1979);
    3. Will not affect intrastate aviation in Alaska to the extent that
it justifies making a regulatory distinction; and
    4. Will not have a significant economic impact, positive or
negative, on a substantial number of small entities under the criteria
of the Regulatory Flexibility Act.
    We prepared an economic evaluation of the estimated costs to comply
with this proposed AD and placed it in the AD docket.

List of Subjects in 14 CFR Part 39

    Air transportation, Aircraft, Aviation safety, Incorporation by
reference, Safety.

The Proposed Amendment

    Accordingly, under the authority delegated to me by the
Administrator, the FAA proposes to amend 14 CFR part 39 as follows:

PART 39--AIRWORTHINESS DIRECTIVES

0
1. The authority citation for part 39 continues to read as follows:

    Authority: 49 U.S.C. 106(g), 40113, 44701.

Sec.  39.13  [Amended]

0
2. The FAA amends Sec.  39.13 by adding the following new airworthiness
directive (AD):

Leonardo S.p.A.: Docket No. FAA-2018-0648; Product Identifier 2017-
SW-087-AD.

(a) Applicability

    This AD applies to Leonardo S.p.A. Model AB139 and AW139
helicopters, certificated in any category, with an Increased Gross
Weight 6,800 Kg kit part number (P/N) 4G0000F00111, and with a main
landing gear (MLG) assembly with a P/N and serial number (S/N)
listed in Table 1 to paragraph (a) of this AD installed.
[GRAPHIC] [TIFF OMITTED] TP19JY18.000

(b) Unsafe Condition

    This AD defines the unsafe condition as an MLG shock absorber
screw that does not meet specifications. This condition could result
in failure of the MLG shock absorber, collapse or retraction of the
MLG, and subsequent damage to the helicopter.

(c) Comments Due Date

    We must receive comments by September 17, 2018.

(d) Compliance

    You are responsible for performing each action required by this
AD within the specified compliance time unless it has already been
accomplished prior to that time.

(e) Required Actions

    (1) Within the following compliance times, replace each screw P/
N NAS1351-5H12P installed on an MLG shock absorber with a screw P/N
1652A0001-01. Re-identify the MLG assembly using black permanent ink
by marking an ``R'' at the end of the S/N of the MLG assembly and
cover with a transparent coating. For purposes of this AD, a
``landing'' is counted any time the helicopter lifts off into the
air and then lands again regardless of the duration of the landing
and regardless of whether the engine is shut down:
    (i) For MLG assemblies with 26,800 or more landings, within 100
hours time-in-service (TIS).
    (ii) For MLG assemblies with between 22,000 and 26,799 landings,
within 300 hours TIS or before the MLG assembly accumulates 27,200
landings, whichever occurs first.
    (iii) For MLG assemblies with less than 22,000 landings, within
1,200 hours TIS or before the MLG assembly accumulates 23,200
landings, whichever occurs first.
    (2) After the effective date of this AD, do not install an MLG
assembly with a P/N and S/N listed in Table 1 to paragraph (a) of
this AD on any helicopter unless the screw has been replaced and the
MLG assembly re-identified as described in paragraph (e)(1) of this
AD.

(f) Special Flight Permits

    Special flight permits are prohibited.

(g) Alternative Methods of Compliance (AMOCs)

    (1) The Manager, Safety Management Section, Rotorcraft Standards
Branch, FAA, may approve AMOCs for this AD. Send your proposal to:
David Hatfield, Aviation Safety Engineer, Safety Management Section,
Rotorcraft Standards Branch, FAA, 10101 Hillwood Pkwy., Fort Worth,
TX 76177; telephone<PHONE_NUMBER>; email [email protected].
    (2) For operations conducted under a 14 CFR part 119 operating
certificate or under 14 CFR part 91, subpart K, we suggest that you
notify your principal inspector, or lacking a principal inspector,
the manager of the local flight standards district office or
certificate holding district office before operating any aircraft
complying with this AD through an AMOC.

(h) Additional Information

    (1) Finmeccanica Bollettino Tecnico No. 139-397, dated April 7,
2016, which is not incorporated by reference, contains additional
information about the subject of this AD. For service information
identified in this AD, contact Leonardo S.p.A. Helicopters, Matteo
Ragazzi, Head of Airworthiness, Viale G.Agusta 520, 21017 C.Costa di
Samarate (Va) Italy; telephone +39-0331-711756; fax +39-0331-229046;
or at http://www.leonardocompany.com/-/bulletins. You may review the
referenced service information at the FAA, Office of the Regional
Counsel, Southwest Region, 10101 Hillwood Pkwy., Room 6N-321, Fort
Worth, TX 76177.
    (2) The subject of this AD is addressed in European Aviation
Safety Agency (EASA) AD No. 2016-0077, dated April 19, 2016. You may
view the EASA AD on the internet at http://www.regulations.gov in
the AD Docket.

 (i) Subject

    Joint Aircraft Service Component (JASC) Code: 3200 Landing Gear
System.

    Issued in Fort Worth, Texas, on July 9, 2018.
Scott A. Horn,
Deputy Director for Regulatory Operations, Compliance & Airworthiness
Division, Aircraft Certification Service.
[FR Doc. 2018-15304 Filed 7-18-18; 8:45 am]
BILLING CODE 4910-13-P


Appendix B Characterizing Measurement Variability as a Function of Analyte Concentration for a Variety of Analytical Techniques Summary EPA s Office of Science and Technology ( OST) conducted a study of measurement variability as part of an assessment of detection and quantitation limit concepts. The study utilized a large data set on measurement variability generated specifically to support this assessment and on data gathered during the course of analytical method development. The purpose of the study reported in this appendix is to determine if: ( 1) appropriate models could be found that would adequately characterize measurement variability and support the estimation of detection and quantitation limits; and ( 2) the number of models could be limited in order to minimize complications in the process of developing detection and quantitation limits. Results suggest that most measurement techniques used under the Clean Water Act ( CWA) could be described by a general two component model. The model describes measurement variability as a function of concentration in terms of two components: an additive component dominate at low concentration that represents variability to be independent of concentration and a multiplicative component dominate at higher concentrations that represents variability as proportional to the concentration of the substance measured. The model also allows for a smooth transition in the relationship in the concentration region where neither component is dominate. The study results also indicate that the two component model may not be applicable to all analytes for all methods. In some cases, measurement variability does not exhibit a pattern that would suggest a particular model. In other cases, measurement variability is observed to be effectively constant over a range that extends beyond the low concentration range. In these cases, the two component model may still be a useful tool in determining detection and quantitation levels but other approaches, e. g., that do not involve the use of a particular model or assume that variation is effectively constant, may also be suitable.

1. Introduction In 1998, EPA s Office of Science and Technology ( OST) completed several studies conducted to generate data that would characterize measurement variability as a function of concentration for a variety of analytical techniques. These studies were conducted as part of an effort to address criticism by the academic community, regulated industry, and others, of the detection and quantitation procedures used to support EPA's Clean Water Act ( CWA) programs. More recently, the Agency has agreed to a schedule for completing this work and applying the results to the evaluation and selection of detection and quantitation concepts and procedures. This document uses the data referenced above and other selected data to characterize measurement variability as a function of analyte concentration for a variety of measurement techniques 2. Data EPA has conducted an extensive review of the published literature on detection and quantitation. Unfortunately, the published literature tends to focus on concepts and methodology and contains little actual data. No data were found on the key issue ( for detection and quantitation) of the characterization and modeling of measurement variability as a function of analyte concentration. In order to fill the need for data, EPA embarked on an effort to produce data that would support the characterization of variability and the assessment of detection and quantitation. The first phase of this process was to develop data sets representative of the most commonly used analytical technologies, and the second phase was application of statistics, including model fitting, to these data.

February 2003 B 1 Assessment of Detection and Quantitation Approaches Four data sets were selected to support the analyses presented in this appendix. Three were developed by EPA for the express purpose of studying the relationship between measurement variation and analyte concentrations across a wide variety of measurement techniques and analytes. These data sets are referred to as ( 1) EPA s ICP/ MS data, ( 2) EPA s Episode 6000 data, and ( 3) EPA s Episode 6184 data. In all three data sets, replicate measurement results from each combination of analyte and measurement technique were produced by a single laboratory over a wide range and large number of spike concentrations. The fourth data set was developed by the American Automobile Manufacturer s Association ( the " AAMA Data set") for the purpose of estimating a specific quantitation value referred to as an " alternate minimum level" ( AML) ( see Gibbons, et al. 1997). For development of the AAMA data set, replicate results were measured at a limited number of spike concentrations by multiple laboratories using EPA Method 245.2 ( CVAA) for mercury and EPA Method 200.7 ( ICP/ AES) for twelve other metals. Details of these four data sets are given in the subsections that follow.

2.1 EPA s ICP/ MS Data In 1996, EPA contracted with Battelle Marine Sciences to generate data to support the assessment of measurement variability in EPA's draft Method 1638 for nine metals by inductively coupled plasma with mass spectroscopy ( ICP/ MS). The nine metals were silver, cadmium, copper, nickel, lead, antimony, selenium, thallium, and zinc. The equipment used in this study made triplicate readings of each aliquot of each sample and averaged the results. Such averaging is common for ICP/ MS design and use.

In preparation for this study, the ICP/ MS instrument was calibrated using one sample aliquot ( i. e., not triplicates) at concentrations of 100, 1,000, 5,000, 10,000, and 25,000 nanograms per liter ( ng/ L). Initially, the calibration was performed using the default instrument software to produce unweighted least squares estimates assuming a linear calibration function. Subsequently, the analytical results were adjusted using weighted least squares estimates in place of the unweighted least squares estimates. Weighted least squares estimates are used to account for the fact that measurement variability may change as concentration changes. Usually, variability increases as analyte concentration increases over the full analytical range. Because the individual readings on each triplicate were not retained; the only data available to EPA are average intensity results for the aliquot. Draft EPA Method 1638 specifies the use of an average response factor rather than least squares estimation of linear calibration curves, although it does allow for the use of such procedures.

All nine metals were spiked into water to produce solutions at concentrations of: 10, 20, 50, 100, 200, 500, 1,000, 2,000, 5,000, 10,000, and 25,000 ng/ L. Each solution was subsequently divided into 7 aliquots. The 7 replicates were measured in order of decreasing concentration. Seven replicates at 0 concentration ( what chemists term a " blank") were also measured in triplicate for all nine metals. The resulting concentrations were converted to parts per trillion ( ppt.) for ease of understanding and discussion.

Multiple instrument readings ( at multiple mass to charge ratios or m/ z s) were reported for most metals, although draft Method 1638 specifies only one acceptable m/ z for eight of the nine metals. For lead, m/ z s 206, 207, and 208 were all considered to be acceptable by draft Method 1638. The responses at the other m/ z values for a particular metal are used for analyte identification purposes. This study of measurement variation used only data associated with m/ z's that are specified by draft Method 1638.

2.2 EPA s Episode 6000 Data Episode 6000 data were collected to characterize the variability of measurement results from 0.1 times an initial estimate of the Method Detection Limit ( MDL) ( Glaser, et al., 1981) to spike concentrations 100 times the MDL. Measurement methods studied were:

B 2 February 2003 Appendix B   Total suspended solids ( TSS) by gravimetry,   Metals by graphite furnace atomic absorption spectroscopy ( GFAA),   Metals by inductively coupled plasma atomic emission spectrometry ( ICP/ AES),   Hardness by ethylene diamine tetraacetic acid ( EDTA) titration,   Phosphorus by colorimetry,   Ammonia by ion selective electrode,   Volatile organic compounds in water by purge and trap capillary column gas chromatography with photoionization detector ( GC/ PID) and electrolytic conductivity detector ( GC/ ELCD) in series,   Volatile organic compounds by gas chromatography with a mass spectrometer ( GC/ MS),   Available cyanide by flow injection/ ligand exchange/ amperometric detection, and   Metals by inductively coupled plasma spectrometry with a mass spectrometer ( ICP/ MS).

Details of the study design are described in EPA s Study Plan for Characterizing Variability as a Function of Concentration for a Variety of Analytical Techniques ( July 1998). The design is summarized below.

A method detection limit ( MDL) study was conducted for each combination of analyte and analytical technique as an initial step in the generation of the Episode 6000 data. The study plan required laboratories to calculate these initial MDLs using the procedure in Appendix A. Seven replicates were then run at 100, 50, 20, 10, 7.5, 5.0, 3.5, 2.0, 1.5, 1.0, 0.75, 0.50, 0.35, 0.20, 0.15, and 0.10 times the initial MDL.

The following iterative procedure was used for organic compounds. Methods for organics normally list many ( 15 to 100) analytes, and the response for each analyte is different. Therefore, to determine an MDL for each analyte, the concentration of the spike must be inversely proportional to the response. The process of making spiking solutions with 15 to 100 different concentrations is complicated and prone to error. A more straightforward approach, and one used in this study, was to run 7 replicates at decreasing concentrations until signal extinction or until 0.1 times the initial MDL was reached, whichever came first, then select concentrations appropriate for the MDL.

Spike concentrations were measured in order from the highest concentration to the lowest to ( 1) to minimize carry over effects and ( 2) to prevent the collection of data if when the instrument returned zeros for three or more of the replicates at a given concentration. Carry over can occur when analysis of a high concentration sample is followed by a low concentration sample. Carry over is usually less than one percent but can be a few percent in some methods. For example, if a sample at 100 times the MDL is followed by a sample at 0.1 times the MDL, the sample at 0.1 times the MDL could be compromised by carry over because a small amount of carry over from the 100 MDL sample could inflate the result for the 0.1 MDL sample. Running the samples in successive decreasing order should not affect successively lower measurements because the amount of carryover should be small relative to the measurement at the next lowest level.

Further details are described in EPA s Study Plan for Characterizing Variability as a Function of Concentration for a Variety of Analytical Techniques ( July 1998).

2.3 EPA s Episode 6184 Data Episode 6184 data were generated to determine the concentration at which an analyte could no longer be identified as the concentration decreased. Details of the design for this study are described in EPA s Study Plan for Characterizing Error as a Function of Concentration for Determination of Semivolatiles by Gas Chromatography/ Mass Spectrometry ( December 1998). Data were generated for 82 semivolatile organic compounds by EPA Method 1625C ( semivolatile organic compounds by GC/ MS).

February 2003 B 3 Assessment of Detection and Quantitation Approaches MDLs were not determined for these compounds. Instead, solutions of the analytes were prepared at concentrations of 50.0, 20.0, 10.0, 7.50, 5.00, 3.50, 2.00, 1.50, 1.00, 0.75, 0.50, 0.35, 0.20, 0.15, 0.10, 0.075 and 0.050 ng/ µ L ( or µ g/ mL). The solution at each concentration was injected into the GC/ MS in triplicate with the mass spectrometer threshold set to 0, and again in triplicate with the mass spectrometer threshold set to a low level in the signal domain typical of that used in routine environmental analyses. As with the Episode 6000 data set, samples were analyzed in order from the highest to the lowest concentration.

2.4 AAMA Metals Data for EPA Methods 200.7 and 200.9 Data The American Automobile Manufacturer s Association ( AAMA) conducted a interlaboratory study of EPA Method 200.7 ( metals by ICP/ AES) and Method 245.2 ( mercury by CVAA). Nine laboratories participated in the study, and each reported data for the following 13 metals: aluminum, arsenic, cadmium, chromium, copper, lead, manganese, mercury, molybdenum, nickel, selenium, silver and zinc. Study samples were analyzed by EPA Method 200.7 for 12 of the metals. Mercury was determined by EPA Method 245.2.

The nine laboratories were randomized prior to the start of the study. Five matrix types ( including reagent water) were selected, including four that were representative of the automotive industry. Each matrix was spiked at five concentrations in a predetermined concentration range. Matrix A ( reagent water) was analyzed in all nine laboratories, and three laboratories analyzed each of the other four matrices. All analyses were repeated weekly over a five week period. As a result, a total of 6825 observations were obtained, which includes 2925 observations for matrix A ( 9 labs * 13 metals * 5 spike concentrations * 5 weeks) and 975 ( 3 labs * 13 metals * 5 spike concentrations * 5 weeks) for each of the other four matrices ( 6825 = 2925 + [ 975 * 4]). There were two missing values for chromium in matrix A from labs 1 and 9.

Starting from a blank or unspiked sample, all target analytes were spiked at 4 concentrations to yield a total of five concentrations per matrix. Concentrations ranged from 0.01 to 10 : g/ L for mercury and selenium, respectively, on the low end, and from 2.0 to 1000 : g/ L for mercury and selenium, respectively, on the high end. In addition, the concentrations were matrix dependent. The same concentration ranges for each metal by matrix combination were used for all five weeks of the study.

3. Statistical methodology The study data were first analyzed graphically and then numerically. Numerical analyses consisted of model parameter estimation and evaluation.

3.1 Graphical Analysis Techniques Composite plots for all combinations of analyte and analytical technique were produced. These sets include: ( 1) Measurement Results vs Spike Concentration ( Appendix B. 1), ( 2) Log10 [ Measurement Results] vs Log10 [ Spike Concentration] ( Appendix B. 2), ( 3) Observed Standard Deviation vs Spike Concentration ( Appendix B. 3), ( 4) Log10 [ Standard Deviation] vs Spike Concentration ( Appendix B. 4),( 5) Relative Standard Deviation vs Log10 [ Spike Concentration] ( Appendix B. 5), and ( 6) Standardized Residuals vs Log10 [ Spike Concentration] ( Appendix B. 6). These graphics are presented at the end of this appendix.

The purpose of these plots is to allow examination of the relationship between two numerical variables and determine if the data fall close to a curve describing an expected model.

B 4 February 2003 Appendix B ( 1) The first set of plots of measurement results versus spike concentrations can be used to evaluate the mean recovery model. If the assumed linear model were true then the relationship outlined by the plotted data would be approximately linear.

( 2) A plot of log measurement results versus log spike concentration will show an approximately linear relationship, similar to ( 1), if the relationship between measurement results and spike concentrations is well behaved. Otherwise, the log transformations used in these plots will tend to exaggerate deviations from the linear model. In particular, a positive bias in measurement results will show as an almost flat line at low concentrations before it starts to increase as concentration increases. A negative bias will show as an almost perpendicular drop at the lower concentrations. The primary advantage of the log log plot is that it allows for easier visualization of the relationship between individual measurement results spike concentration at the low concentrations. When the log log plot is combined with an indicator that identifies which data came from which calibration, the effect of changing calibration may be seen clearly.

( 3) The plot of observed standard deviations versus spike concentrations can be used to evaluate the reasonableness of the constant and/ or straight line models. If the constant model for standard deviation were true then the standard deviation would be approximately the same regardless of concentration. If the straight line model for standard deviation were true then the plots are expected to indicate an approximately linear relationship.

( 4) The log log plot is expected to display an approximately linear relationship when a logarithmic model fits the data. If the two component model were true then we would generally expect to see a relationship that looks something like the shape of a hockey stick. That is, standard deviation would be approximately constant at low concentrations and would increase in proportion to concentration at higher concentrations. However, if spike concentrations were not selected at sufficiently low concentrations, the two component model would display the approximately linear relationship of a log log model.

( 5) The plots of relative standard deviation ( RSD) versus log 10 of the spike concentration are generally expected to show high RSD for the lowest concentrations and convergence to a constant RSD at higher concentrations. This theory may be used to describe measurement variation in terms of a single number.

( 6) The plots of standardized residuals versus log 10 of the spike concentration show how well variation is estimated using the available procedures for the two component model. A residual shows how much a measurement result has deviated from the model of the relationship between measurement results and spike concentrations. Standardized residuals are generally expected to be within plus or minus 3 standard deviations of zero and are expected to average zero. Residuals at each spike concentration are standardized to the standard deviation estimated using the two component model. When residuals spread to less than three standard deviations, the model is generally overestimating variability. When residuals spread to more than three standard deviations, the model is generally underestimating variability. The exception to this rule is an apparent outlier. A secondary characteristic of this type of plot is that it accentuates any deviation from the expected linear relationship.

3.2 Model Estimation With some deviations, the two component model ( Rocke and Lorenzato, 1995) was estimated using the FORTRAN program provided ( publicly available at no cost) by Professor David Rocke ( http:// handel. cipic. ucdavis. edu/~ dmrocke/). Qualitative output and plots of deviations from this model were used to evaluate the fit of the model to the available data. The model is expressed as:

February 2003 B 5 Assessment of Detection and Quantitation Approaches + µ y =    e  +   where the parameters are defined as: y = observed instrument response e = the natural exponential function   = the intercept of a linear function   = the slope of a linear function   = independent errors with normal distribution, mean zero, and fixed variance   = independent errors with normal distribution, mean zero, and fixed variance µ = true concentration in the sample measured Two deviations from the two component model are present in this evaluation. These deviations are that results have been substituted for instrument responses and all data used in this appendix have entrained dependencies that violate the assumption of independent errors within the domain of interest ( e. g., within a single laboratory or within a group of laboratories). For analytes and analytical techniques for which results are generated by a linear response, substituting results for responses does not fundamentally change the structure of the model. With regard to independent errors, results for each combination of analyte and measurement technique were obtained in descending order of concentration. Hence, any event that happens in the measurement process during data collection has effects that systematically continue throughout the remaining portion of data collection. The most obvious event is calibration, which can be linked visually to systematic changes in results. It is not clear whether the AAMA data have the same problem. However, the AAMA data were collected in sets spaced one week apart and each set contained all of the spike concentrations used for every analyte under study. Hence, any event that affects any one result at a given spike concentration is likely to affect other results at every other spike concentration. Again, the obvious event is calibration.

Model estimates were restricted to cases for which at least 5 spike concentrations were available. Because the two component model has 4 parameters, the extra spike concentration is required to have a real indication that the model is fitting any given data set.

4. Results 4.1 Graphical Evaluations In this section, we provide some examples of diagnostic plots. Graphics referred to in the text are shown in Section 4.1.7. Complete sets are provided at the end of this appendix.

4.1.1 Results vs. Concentration In general, the observed relationship between concentration and results follows a straight line closely ( see, e. g., Figure 4 1 which shows measurement results versus concentrations for WAD Cyanide). In other cases, these plots help identify analytes with potential outlier observations ( see, e. g., Figure 4 2 which shows measurement results versus concentration for 1 chlorobutane). In still others, the linear relationship is not well demonstrated in the EPA data ( see, e. g., Figures 4 3 and 4 4). Although more difficult to visualize because of fewer spike concentrations, much of the observed AAMA data also appear to follow a straight line ( see, e. g., Figure 4 5 Cadmium data from lab 3). Because one complete set of spike concentrations were measured each week, some of the AAMA data show an effect related to the week the measurements were made. An extreme example is shown in Figure 4 6 Copper from lab 4.

B 6 February 2003 Appendix B The highest copper measurement result at each spike concentration was made during week 2 of the study. The complete set of plots for measurement results vs. spike concentrations is provided in Sections B 1 1 and B 1 2, at the end of this appendix.

The number of low concentrations included in the EPA data made possible the examination of patterns of variation in the low concentration range. The rationale for this was the importance of variation in the low concentration range from theoretical and practical perspectives. We specifically focused on the lowest six concentrations reported in EPA studies. The selection of six was based on the judgment that six was large enough to determine a departure from the linear model and small enough to visually resolve the individual results given the range of the concentration levels. In general, the plots show patterns of variation not related to concentration. This may be considered evidence of the constant variation property in the low concentration and also may be due to the fact that the low concentration levels in the EPA studies were designed to demonstrate the performance of methods below their established detection levels. Examples of these plots are shown in Figures 4 7 and 4 8, antimony and 2,6 dinitrotoluene.

4.1.2 Log10 [ Measurement Result] vs Log10 [ Spike Concentration]

For the EPA data, these plots indicate that discontinuities in the relationship between results and spike concentrations can occur when calibration is known to change ( see, e. g., Figure 4 9, plot for 1,3 dichlorobenzene and Figure 4 10, 2 chlorotoluene). No remarkable relationships were noted among the AAMA data, though it would be difficult to discern any pattern with only five spike concentrations. The complete set of plots for Log10 [ Measurement Results] vs Log10 [ Spike Concentration] can be found in Sections B 2 1 and B 2 2 at the end of this appendix.

4.1.3 Observed standard deviation vs. spike concentration These plots generally indicate that measurement variation at low concentrations may be approximately constant ( see, e. g., Figure 4 11, sodium). However, it is unusual for measurement variation to remain constant throughout the range of spike concentrations considered in the EPA and AAMA studies. At some point, there is generally an indication that measurement variation increases with spike concentration. In certain cases, the plots provide some indication that the relationship between variability and concentration may be increasing linearly ( see, e. g., Figure 4 12, Silver [ Ag] 107). On the other hand, other graphics indicate both convex and concave curves (( Figures 4 13, 2 chorophenol and Figure 4 14, 1,4 dicholobenzene). With only five spike concentrations, the AAMA data do not appear to be informative in these plots. The complete set of plots is provided at the end of this appendix.

4.1.4 Log/ log plot ( standard deviation vs spike concentration)

The log log plots of standard deviation versus spike concentration display three general patterns. In the first, measurement variation appears random within an approximately oval shaped regions that does not suggest a relationship between log standard deviation and log concentration ( Figure 4 15 WAD Cyanide). In the second, lower concentrations exhibit roughly constant variability within an oval shaped region but higher concentrations show an increasing linear relationship between log standard deviation and log concentration ( Figure 4 16 Ammonia as Nitrogen). In the third, all concentrations exhibit log standard deviation that increases linearly with the log concentration ( Figure 4 17 Mercury). Note that the approximately linear, concave, and convex relationships shown in the figures cited in Section 4.1.3, above, all display as approximately linear in the log/ log plots ( Figure 4 18 Silver [ Ag] 107, Figure 4 19 2 chorophenol and Figure 4 20 1,4 dicholobenzene). This suggests that the apparent relationships shown in the standard deviation versus concentration plots were artifacts of a log/ log relationship that is approximately linear. The complete set of plots is provided at the end of this appendix.

February 2003 B 7 Assessment of Detection and Quantitation Approaches 4.1.5 Relative Standard Deviation versus Spike Concentration Relative standard deviation ( RSD) generally appears to decrease as concentration increases throughout the range of concentrations observed in this study although there are some exceptions ( e. g., Figure 4 21 Chlorobenzene and Figure 4 22 Dibromoethane). The more typical pattern is shown in Figure 4 23 1 chlorobutane. RSD may approach asymptotically some limiting value but it does not generally appear to become constant at any point. Note that the range on the vertical axis changes considerably between plots and that the larger ranges will tend to hide the variation that continues to exist at higher concentrations. For depicting method performance, it may be appropriate to select the lowest acceptable result, calculate the RSD, and describe the method as being capable of meeting or doing better than the selected standard. Cases where RSD increase with increasing concentration may be problematic.

4.1.6 Summary of the Graphical Analyses The primary purpose of graphing the study data was to support the selection of models for relating the variability of results to spike concentrations. However, artifacts of the way data were collected are also visible in these analyses.

The classes of models considered include: ( a) constant variability ( not related to spike concentration), ( b) variability increasing linearly with concentration, ( c) log variability increasing linearly with log concentration, and ( d) variability increasing proportionally with concentration after shifting upward some fixed amount. The data seem to indicate that model class ( d) is able to describe the relationship between results and concentrations across a wide variety of measurement techniques and analytes. One specific model in this class is the two component model described by Rocke and Lorenzato ( 1975), among others. Model classes ( a) and ( c) can be considered subsets of model class ( d) that appear when concentrations do not cover the full range of the method.

The effect of using systematic elements in the sampling design, as opposed to using completely random sampling, is present in all data sets considered here and clearly demonstrated in the Episode 6000 data and the AAMA data. In the Episode 6000 data, all results for each combination of analyte and measurement technique were measured in order from the highest to the lowest. Where significant changes in the measurement process occurred, such as instrument re calibration, visually observable effects in the relationship between results and concentration became apparent. In the AAMA data, every spike concentration in the study was measured once a week for five weeks. Where significant changes in the measurement process occurred between weeks, visually observable effects in the relationship between results and spike concentration became apparent.

B 8 February 2003 Appendix B 4.1.7 Graphics Measured Concentration 60 40 20 0 Classicals, Method 1677Classicals, 1677 WAD CYANIDE, UG/ LWAD L 0 200 400 600 800 1000 Organics, Method 524.2Organics, 524.2 1 CHLOROBUTANE, UG/ L1 L 0 50 100 150 200 0 1020304050 Spike Concentration Spike Concentration Figure 4 1 Figure 4 2 500 1000 1500 Metals, Method 1620Metals, 1620 IRON, UG/ LIRON, L Organics, Method 502.2 ELCDOrganics, ELCD DICHLORODIFLUOROMETHANE, UG/ LDICHLORODIFLUOROMETHANE, L Figure 4 3 Figure 4 4 Lab: 3Lab: 3 CADMIUM, UG/ LCADMIUM, L Lab: 4Lab: 4 COPPER, UG/ LCOPPER, L Measured Concentration 20 15 10 5 0 0 0 200 400 600 800 0246810 Spike Concentration Spike Concentration 300 80 250 200 60 150 40 100 20 50 0 0 0 20 40 60 80100 0 50 100 150 200 Spike Concentration Spike Concentration Figure 4 5 Figure 4 6 Measured Concentration Measured Concentration Measured Concentration Measured Concentration February 2003 B 9 Assessment of Detection and Quantitation Approaches Metals, Method 1620Metals, 1620 ANTIMONY, UG/ LANTIMONY, L Organics, Method 1625: T= 0Organics, 0 2,6 DINITROTOLUENE, NG/ UL2,6 UL 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.0 0.05 0.10 0.15 0.20 Spike Concentration Spike Concentration 3.0 2.5 2.0 1.5 1.0 0.5 0.0 0.4 0.3 0.2 0.1 Log 10 of Measured Concentration Measured Concentration Observed Standard Deviation Figure 4 7 Figure 4 8 10.00 Organics, Method 502.2 PIDOrganics, PID 1,3 DICHLOROBENZENE, UG/ L1,3 L Observed Standard Deviation Log 10 of Measured Concentration Measured Concentration 5.00 5.00 1.00 1.00 0.50 0.50 0.10 0.10 0.05 0.05 0.01 10.00 Organics, Method 502.2 PIDOrganics, PID 2 CHLOROTOLUENE, UG/ L2 L 0.05 0.10 0.50 1.00 5.00 10.00 0.05 0.10 0.50 1.00 5.00 10.00 Log 10 of Spike Concentration Log 10 of Spike Concentration 70 250 60 200 50 150 40 100 30 50 20 0 Figure 4 9 Figure 4 10 Metals, Method 1620Metals, 1620 SODIUM, UG/ LSODIUM, L Metals, Method ICP/ MSMetals, MS Ag 107, pptAg ppt 0 1000 2000 3000 4000 0 5000 10000 15000 20000 25000 Spike Concentration Spike Concentration Figure 4 11 Figure 4 12 B 10 February 2003 Appendix B 0.5 10 Organics, Method 1625: T= 0Organics, 0 2 CHLOROPHENOL, NG/ UL2 UL 0 20 40 60 80100 0 50 100 150 200 Organics, Method 524.2Organics, 524.2 1,4 DICHLOROBENZENE, UG/ L1,4 L Spike Concentration Spike Concentration Log 10 of Observed Standard Deviation Observed Standard Deviation 0.4 0.3 0.2 0.1 0.0 Log 10 of Observed Standard Deviation Observed Standard Deviation 8 6 4 2 0 0.40 Classicals, Method 1677Classicals, 1677 WAD CYANIDE, UG/ LWAD L 0.050 0.30 0.20 0.010 0.005 0.10 0.09 0.08 0.07 0.06 0.5 1.0 5.0 10.0 50.0 0.001 0.005 0.010 0.050 0.100 0.500 1.000 Figure 4 13 Figure 4 14 Classicals, Method 350.3Classicals, 350.3 AMMONIA AS NITROGEN, MG/ LAMMONIA L Log 10 of Spike Concentration Log 10 of Spike Concentration 0.100 50.0 0.050 Metals, Method 200.8Metals, 200.8 MERCURY, UG/ LMERCURY, L 10.0 5.0 0.010 0.005 1.0 0.5 0.005 0.010 0.050 0.100 0.500 1.000 5.000 10.000 Figure 4 15 Figure 4 16 10 100 1000 1000010000 0 100.0 Metals, Method ICP/ MSMetals, MS Ag 107, pptAg ppt Log 10 of Spike Concentration Log 10 of Spike Concentration Figure 4 17 Figure 4 18 Log 10 of Observed Standard Deviation Log 10 of Observed Standard Deviation February 2003 B 11 Assessment of Detection and Quantitation Approaches 0.500 10.000 5.000 0.100 1.000 0.500 0.050 0.100 0.050 0.010 0.005 0.010 0.005 0.01 0.10 1.00 10.00 100.00 0.1 0.5 1.0 5.0 10.0 50.0 100.0 Organics, Method 524.2Organics, 524.2 1,4 DICHLOROBENZENE, UG/ L1,4 L Log 10 of Spike Concentration Log 10 of Spike Concentration 86 5 6 4 43 2 2 1 00  1.0  0.5 0.0 0.5 1.0  1.0  0.5 0.0 0.5 1.0 Figure 4 19 Figure 4 20 Organics, Method 502.2 ELCDOrganics, ELCD DIBROMOMETHANE, UG/ LDIBROMOMETHANE, L Log 10 of Spike Concentration Log 10 of Spike Concentration Figure 4 21 Figure 4 22 2 1 0  1 100 200 300 Organics, Method 524.2Organics, 524.2 1 CHLOROBUTANE, UG/ L1 L 0  2  10 1 2 Lab: 6Lab: 6 ALUMINUM, UG/ LALUMINUM, L 110100 Log 10 of Spike Concentration Log 10 of Spike Concentration Figure 4 23 Figure 4 24 Organics, Method 1625: T= 0Organics, 0 2 CHLOROPHENOL, NG/ UL2 UL Relative Standard Deviation Log 10 of Observed Standard Deviation Relative Standard Deviation Organics, Method 502.2 ELCDOrganics, ELCD CHLOROBENZENE, UG/ LCHLOROBENZENE, L Standardized Residuals Relative Standard Deviation Log 10 of Observed Standard Deviation B 12 February 2003 Appendix B 3 2 2 1 0 Classicals, Method 160.2Classicals, 160.2 TOTAL SUSPENDED SOLIDS, MG/ LTOTAL L 0  1  2  2  3 1 10 100 0 10 100 1000 10000 Metals, Method ICP/ MSMetals, MS Ni 60, pptNi ppt Log 10 of Spike Concentration Log 10 of Spike Concentration Figure 4 25 Figure 4 26 3 2 1 0  1  2  3 0.001 0.01 0.1 1 Classicals, Method 350.3Classicals, 350.3 AMMONIA AS NITROGEN, MG/ LAMMONIA L Log 10 of Spike Concentration Figure 4 27 Standardized Residuals Standardized Residuals Standardized Residuals February 2003 B 13 Assessment of Detection and Quantitation Approaches 4.2 Two component Model fitting This section considers the results of fitting the two component Rocke Lorenzato Model to the EPA and AAMA data. The basic approach was to use maximum likelihood estimation to estimate parameters of the Rocke Lorenzato model using software developed by Professor Rocke which is available at no cost on his web site http:// www. cipic. ucdavis. edu/~ dmrocke/ software. html. The software implements a numerical optimization algorithm that solves for the maximum likelihood estimates of the parameters of the model. The results for the EPA data are summarized in Table 1 which lists the number of analytes by method and the number of times the software was run and the number of times that the software was not able to obtain a solution, i. e., failures. Failure to obtain a solution is usually the result of poor fit of the data to the data. That is, the data are so discrepant with regard to the assumed model that the algorithm fails to converge to a solution. For the EPA data, 47 of 371 cases ( about 13%) failed to obtain a solution. There were no failures for the AAMA data. The tables with results of the maximum likelihood estimation including parameter estimates along with recorded optimization failures by study, class, technique, and analyte are shown at the end of this appendix. Plots of residuals, useful for evaluating model fit are shown at the end of this appendix.

Table 1:

EPA Study Measurement Method Number of Analytes Measured ( Analytes x Labs) Number of Failures Episode 6000 130.2 1 0 Episode 6000 160.2 1 0 Episode 6000 1677 1 0 Episode 6000 350.3 1 0 Episode 6000 365.2 1 0 ICP/ MS ICP/ MS 11 2 Episode 6000 1620 26 0 Episode 6000 200.8 21 9 Episode 6000 502.2 63 4 Episode 6000 524.2 80 0 Episode 6184 1625 167 32 Total 371 ( 13%) Optimization Failures for Two Component Model Estimates 47 The two component model can be judged to fit the EPA and AAMA data since the maximum likelihood algorithm was able to obtain parameter estimates for the large majority of the data sets. Evaluation of model fit should also include examination of residual plots. The two component model appears to fit the AAMA data well but the fit is inconsistent for the EPA data. For the AAMA data, the maximum likelihood algorithm had no difficulty obtaining parameter estimates for the two component model and plots generally indicate the expected random pattern of the residuals about zero ( e. g., Figure 4 24 Aluminum, Lab 6). For the EPA data, some analytes have residual plots that indicate a reasonable fit and others have residuals that indicate questionable fits. For example, the results indicate that the fit for Method 160.2 seems reasonable ( Figure 4 25 Total Suspended Solids). For other methods in the EPA studies, the model fit is inconsistent with some analytes showing reasonable residuals and others indicating problems with model fit ( e. g., Figure 4 26 Nickel 60). For many of the analytes it was B 14 February 2003 Appendix B possible to assess the effect of changes in calibration on model fit. For a number of analytes, plots of results vs. concentration were generated by calibration sequence. For example, residuals shown in Figure 4 27 Ammonia as Nitrogen indicate the presence of four different calibrations. The complete set of plots is presented at the end of this appendix. Also, in addition to performing diagnosis and analysis based on the full set of available spike concentrations for each analyte, model parameters were estimated based on calibration sequences. The tables at the end of this appendix show the estimated parameters by calibration sequence. Information was not available to allow diagnostics and the plotting of organics by calibration sequence.

5.0 On Designing Studies of Results versus Concentration Based on evaluation of the data generated, four improvements are suggested to the original EPA study design. The first suggestion is directed towards instruments that report no value or a constant value below some fixed spike concentration. In these cases, perform a preliminary assessment of instrument capabilities prior to selecting the lowest concentrations for the tests. The assessment would include a limited number of measurements at low concentrations to determine the capability of the instrument to generate low level measurements. Then, in conducting the study, restrict the selection of spike concentrations in the experiment to those concentrations high enough to generate suitable measurements.

A second suggestion would be to include replicate measurements at increasing concentrations until the upper end of the calibration range is achieved. Data at the highest possible concentrations would allow enhanced definition of the proportional error region.

The third suggestion would be to create all study samples and aliquots from the samples prior to measurement and to completely randomize the order in which aliquots are measured. The possibility of carryover would exist but it would be handled the same way it is handled by a laboratory using a measurement method in production, i. e., by re analysis of a low concentration sample that follows analysis of a high concentration sample after analysis of a blank to demonstrate that the analytical system is essentially free from carryover. This could increase the analytical cost by an order of magnitude.

The fourth suggestion would be to use multiple laboratories. This assumes that interlaboratory objectives are consistent with study goals. Of course, depending on how many and which measurement methods are selected for study, the cost of such a study using multiple laboratories could easily run into several million dollars.

6.0 Conclusions The study data suggest that measurement variation for most measurement techniques used under the Clean Water Act can be described by two models. Those models are the two component model and the constant model. Although the pure log normal model could be used to fit data that do not show a constant component, this model implies the unacceptable condition that measurement variation may become zero at some low concentration. Graphics of the variability associated with EPA s data combined with both the graphics and the two component estimates from the AAMA data makes the suggestion of these two models fairly strong for metals data. Although the two component model has an appealing physical basis ( see Rocke and Lorenzato [ 1995]), the available data do not provide strong support for or organic analytes. Graphics of variability versus concentration in many cases suggest the two component model but the actual fit of this model using the maximum likelihood algorithm sometimes fails. We assume that the cases where the two component model does not work well for the organics data in this study are due to the lack of a response at low concentrations or because of problems in the design and implementation of the procedures used to generate the data.

February 2003 B 15 Assessment of Detection and Quantitation Approaches Unfortunately, problems associated with the design of the studies considered in this assessment make it unclear whether the estimation procedures associated with the two component model can be relied on to routinely produce estimates under the necessary conditions. More than 10% of the analyte/ measurement technique combinations considered here have failed to produce maximum likelihood estimates for the two component model. More of these combinations appear to fail the graphical examination of the fit. For our purposes, the true test of the model is how well it can be used in practice to produce detection or quantitation estimates. If a simpler model produces estimates on a more reliable basis, trade offs in terms of precision and bias would have to be considered.

References ( 1) EPA ( 1995), Appendix B to Part 136  Definition and procedure for the Determination of the Method Detection Limit  Revision 1.11, 40 Code of Federal Regulations, U. S. Government Printing Office, Washington.

( 2) Glaser, J. A., Foerst, D. L., McKee, G. D., Quave, S. A., and Budde, W. L. ( 1981), Trace Analyses for Wastewaters. Environmental Science and Technology, 15, pp. 1426 1435.

( 3) Rocke, D. M., and Lorenzato, S. ( 1995), A Two Component Model for Measurement Error in Analytical Chemistry, Technometrics, 69, pp. 3069 3075.

( 4) Gibbons, R. L, Coleman, D. E. and Maddalone, R. F. ( 1997), An Alternative Minimum Level Definition for Analytical Determination, Environmental Science and Technology, 31, pp. 2071 2077.

B 16 February 2003