3546-1 Revision 0
February 2007
METHOD 3546
MICROWAVE EXTRACTION
SW-846 is not intended to be an analytical training manual. Therefore, method
procedures are written based on the assumption that they will be performed by analysts who are
formally trained in at least the basic principles of chemical analysis and in the use of the subject
technology.
In addition, SW-846 methods, with the exception of required method use for the analysis
of method-defined parameters, are intended to be guidance methods which contain general
information on how to perform an analytical procedure or technique which a laboratory can use
as a basic starting point for generating its own detailed Standard Operating Procedure (SOP),
either for its own general use or for a specific project application. The performance data
included in this method are for guidance purposes only, and are not intended to be and must
not be used as absolute QC acceptance criteria for purposes of laboratory accreditation.
1.0 SCOPE AND APPLICATION
1.1 This method is a procedure for extracting water insoluble or slightly water soluble
organic compounds from soils, clays, sediments, sludges, and solid wastes. This method was
developed and validated on commercially-available solvent extraction systems. Its procedure
uses microwave energy to produce elevated temperature and pressure conditions (i.e., 100 -
115 EC and 50 - 175 psi) in a closed vessel containing the sample and organic solvent(s) to
achieve analyte recoveries equivalent to those from Soxhlet extraction (Method 3540), using
less solvent and taking significantly less time than the Soxhlet procedure. Other systems and
other types of vessels may be used, provided that the analyst demonstrates appropriate
performance for the specific application.
1.2 This method is applicable to the extraction of semivolatile organic compounds,
organophosphorus pesticides, organochlorine pesticides, chlorinated herbicides, phenoxyacid
herbicides, substituted phenols, PCBs, and PCDDs/PCDFs, which may then be analyzed by a
variety of chromatographic procedures. This method may also be applicable for the extraction
of additional target analytes, provided that the analyst demonstrates adequate performance for
the intended application (see Method 3500 and Chapter Two).
1.3 This method has been validated for solid matrices containing from 50 to 10,000
µg/kg of semivolatile organic compounds, 250 to 2,500 µg/kg of organophosphorus pesticides,
10 to 5,000 µg/kg of organochlorine pesticides and chlorinated herbicides, 50 to 2,500 µg/kg of
substituted phenols, 100 to 5,000 µg/kg of phenoxyacid herbicides, 1 to 5,000 µg/kg of PCBs,
and 10 to 6000 ng/kg of PCDDs/PCDFs.
This method may be applicable to samples containing these analytes at higher
concentrations and may be employed after adequate performance is demonstrated for the
concentrations of interest (see Method 3500). It may also be applicable to classes of analytes,
to fuel types, and to ...
Following are the list of attributes to be followed;
1.0 Objective:
The purpose of the study is to develop analytical method for determination of Assay & Related substances in new formulation product by HPLC using UV-Visible detector.
2.0 Introduction:
This document will help analyst to develop robust Analytical method for routine testing.
3.0 Scope:
This guideline will provide information about analytical method development to be carried out as per ICH Guidelines.
4.0 Physico-Chemical details of API:
Following items to be checked viz;
IUPAC name, Molecular formula, Chemical structure, Molecular weight, Solubility, Appearance, Melting Point, pH solubility, pKa, LogP, BCS Classification, Polymorphism, Isomerism, Density, Hygroscopicity, Impurities listed as per process either in DMF or official monograph
Thuốc thử là hóa chất không thể thiếu của bất kỳ phòng thí nghiệm nào và do đó đóng vai trò quan trọng trong việc đảm bảo kết quả phân tích. Thuốc thử phải phù hợp với mục đích sử dụng.
Trong phòng thí nghiệm, hai loại thuốc thử chính thường được phân biệt: loại thương mại và loại được điều chế trong phòng thí nghiệm. Hai loại thuốc thử này chủ yếu được đề cập riêng trong tài liệu này.
Các khuyến nghị về thời hạn sử dụng của dung dịch thuốc thử được chuẩn bị và sử dụng trong phòng thí nghiệm và được trình bày trong tài liệu này được thiết lập dựa trên dữ liệu khoa học (bao gồm dữ liệu xác nhận thu được từ biểu đồ kiểm soát chất lượng, hướng dẫn, tiêu chuẩn, dược điển, ấn phẩm, v.v.) và trên phân tích. kinh nghiệm và kiến thức về OMCL. Thời gian chuẩn bị, chi phí, chính sách quản lý chất thải bền vững và các mối quan tâm về bảo vệ môi trường cũng được xem xét trong quá trình chuẩn bị các khuyến nghị này.
Các khuyến nghị về thời hạn sử dụng của các dung dịch thuốc thử được cung cấp ở đây sẽ cho phép các phòng thí nghiệm đánh giá liệu một dung dịch nhất định có thể được sử dụng một cách an toàn và đáng tin cậy hay không (với điều kiện là các điều kiện bảo quản tuân thủ các yêu cầu) khi chúng tính đến các yếu tố khác nhau góp phần làm giảm chất lượng của một số thuốc thử (nhiệt độ, tiếp xúc với không khí, độ ẩm).
Following are the list of attributes to be followed;
1.0 Objective:
The purpose of the study is to develop analytical method for determination of Assay & Related substances in new formulation product by HPLC using UV-Visible detector.
2.0 Introduction:
This document will help analyst to develop robust Analytical method for routine testing.
3.0 Scope:
This guideline will provide information about analytical method development to be carried out as per ICH Guidelines.
4.0 Physico-Chemical details of API:
Following items to be checked viz;
IUPAC name, Molecular formula, Chemical structure, Molecular weight, Solubility, Appearance, Melting Point, pH solubility, pKa, LogP, BCS Classification, Polymorphism, Isomerism, Density, Hygroscopicity, Impurities listed as per process either in DMF or official monograph
Thuốc thử là hóa chất không thể thiếu của bất kỳ phòng thí nghiệm nào và do đó đóng vai trò quan trọng trong việc đảm bảo kết quả phân tích. Thuốc thử phải phù hợp với mục đích sử dụng.
Trong phòng thí nghiệm, hai loại thuốc thử chính thường được phân biệt: loại thương mại và loại được điều chế trong phòng thí nghiệm. Hai loại thuốc thử này chủ yếu được đề cập riêng trong tài liệu này.
Các khuyến nghị về thời hạn sử dụng của dung dịch thuốc thử được chuẩn bị và sử dụng trong phòng thí nghiệm và được trình bày trong tài liệu này được thiết lập dựa trên dữ liệu khoa học (bao gồm dữ liệu xác nhận thu được từ biểu đồ kiểm soát chất lượng, hướng dẫn, tiêu chuẩn, dược điển, ấn phẩm, v.v.) và trên phân tích. kinh nghiệm và kiến thức về OMCL. Thời gian chuẩn bị, chi phí, chính sách quản lý chất thải bền vững và các mối quan tâm về bảo vệ môi trường cũng được xem xét trong quá trình chuẩn bị các khuyến nghị này.
Các khuyến nghị về thời hạn sử dụng của các dung dịch thuốc thử được cung cấp ở đây sẽ cho phép các phòng thí nghiệm đánh giá liệu một dung dịch nhất định có thể được sử dụng một cách an toàn và đáng tin cậy hay không (với điều kiện là các điều kiện bảo quản tuân thủ các yêu cầu) khi chúng tính đến các yếu tố khác nhau góp phần làm giảm chất lượng của một số thuốc thử (nhiệt độ, tiếp xúc với không khí, độ ẩm).
Preparation of Samples for Compositional AnalysisBiorefineryEPC™
Preparation of Samples for Compositional Analysis
Disclaimer-
YOU AGREE TO INDEMNIFY BioRefineryEPC™ , AND ITS AFFILIATES, OFFICERS, AGENTS, AND EMPLOYEES AGAINST ANY CLAIM OR DEMAND, INCLUDING REASONABLE ATTORNEYS' FEES, RELATED TO YOUR USE, RELIANCE, OR ADOPTION OF THE DATA FOR ANY PURPOSE WHATSOEVER. THE DATA ARE PROVIDED BY BioRefineryEPC™ "AS IS" AND ANY EXPRESS OR IMPLIED WARRANTIES, INCLUDING BUT NOT LIMITED TO THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY DISCLAIMED. IN NO EVENT SHALL BioRefineryEPC™ BE LIABLE FOR ANY SPECIAL, INDIRECT OR CONSEQUENTIAL DAMAGES OR ANY DAMAGES WHATSOEVER, INCLUDING BUT NOT LIMITED TO CLAIMS ASSOCIATED WITH THE LOSS OF DATA OR PROFITS, WHICH MAY RESULT FROM ANY ACTION IN CONTRACT, NEGLIGENCE OR OTHER TORTIOUS CLAIM THAT ARISES OUT OF OR IN CONNECTION WITH THE USE OR PERFORMANCE OF THE DATA.
Determination of Extractives in Biomass
DISCLAIMER:
YOU AGREE TO INDEMNIFY BioRefineryEPC™ , AND ITS AFFILIATES, OFFICERS, AGENTS, AND EMPLOYEES AGAINST ANY CLAIM OR DEMAND, INCLUDING REASONABLE ATTORNEYS' FEES, RELATED TO YOUR USE, RELIANCE, OR ADOPTION OF THE DATA FOR ANY PURPOSE WHATSOEVER. THE DATA ARE PROVIDED BY BioRefineryEPC™ "AS IS" AND ANY EXPRESS OR IMPLIED WARRANTIES, INCLUDING BUT NOT LIMITED TO THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY DISCLAIMED. IN NO EVENT SHALL BioRefineryEPC™ BE LIABLE FOR ANY SPECIAL, INDIRECT OR CONSEQUENTIAL DAMAGES OR ANY DAMAGES WHATSOEVER, INCLUDING BUT NOT LIMITED TO CLAIMS ASSOCIATED WITH THE LOSS OF DATA OR PROFITS, WHICH MAY RESULT FROM ANY ACTION IN CONTRACT, NEGLIGENCE OR OTHER TORTIOUS CLAIM THAT ARISES OUT OF OR IN CONNECTION WITH THE USE OR PERFORMANCE OF THE DATA.
pilot plant is a small system which is operated to find out about the behavior of a process before using it on a large industrial scale. so, this presentation tries to illustrate its objective and significance to understand the methodologies of various pharmaceutical dosage forms.
Introduction to Hazard Studies
CONTENTS
1 INTRODUCTION
2 HAZARD EVALUATION TECHNIQUES
2.1 Hazard Identification and Control
2.2 Selection of Technique
2.3 GBHE Hazard Study Procedure
2.3.1 Study One – Concept stage hazard review
2.3.2 Study two - Front-end engineering design
and project definition
2.3.3 Study three – detailed design hazard study
2.3.4 Study four – construction/ design verification
2.3.5 Study five – pre-commissioning safety review
2.3.6 Study six – project close-out/ post start-up review
2.4 Application of Hazard Study Procedure
2.5 Outcomes from the Process
2.6 the Hazard Study Toolkit
2.7 Change Management/Modifications
3 HAZARD STUDY LEADER CAPABILITY AND APPOINTMENT
REFERENCES
APPENDICES
A THE PROJECT PROCESS
B GBHE HAZARD STUDY TOOLKIT
(No Plagiarism) Explain the statement Although many leading organi.docxtamicawaysmith
(No Plagiarism) Explain the statement: "Although many leading organizations have invested significant resources in developing the culture and routines for this innovation processes, most organizations continue to rely on the efforts of a handful of people and chance. An innovative organization is one that can perfect these routines in addition to creating an innovation culture in the organization that engages people. Five key routines can facilitate its management of the innovation process” (Dooley & O'Sullivan, 2003).
.
What made you choose this career path What advice do you hav.docxtamicawaysmith
What made you choose this career path?
What advice do you have for those hoping to enter this career path?
What were some obstacles you faced upon graduating from college?
Does your career require graduate school? What programs would be acceptable?
Is there anything you wish you would have done differently?
Is it difficult to find a job in this area?
What is a typical work week like?
Etcetera, depending on the field and what you’re interested in.
.
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Preparation of Samples for Compositional Analysis
Disclaimer-
YOU AGREE TO INDEMNIFY BioRefineryEPC™ , AND ITS AFFILIATES, OFFICERS, AGENTS, AND EMPLOYEES AGAINST ANY CLAIM OR DEMAND, INCLUDING REASONABLE ATTORNEYS' FEES, RELATED TO YOUR USE, RELIANCE, OR ADOPTION OF THE DATA FOR ANY PURPOSE WHATSOEVER. THE DATA ARE PROVIDED BY BioRefineryEPC™ "AS IS" AND ANY EXPRESS OR IMPLIED WARRANTIES, INCLUDING BUT NOT LIMITED TO THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY DISCLAIMED. IN NO EVENT SHALL BioRefineryEPC™ BE LIABLE FOR ANY SPECIAL, INDIRECT OR CONSEQUENTIAL DAMAGES OR ANY DAMAGES WHATSOEVER, INCLUDING BUT NOT LIMITED TO CLAIMS ASSOCIATED WITH THE LOSS OF DATA OR PROFITS, WHICH MAY RESULT FROM ANY ACTION IN CONTRACT, NEGLIGENCE OR OTHER TORTIOUS CLAIM THAT ARISES OUT OF OR IN CONNECTION WITH THE USE OR PERFORMANCE OF THE DATA.
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DISCLAIMER:
YOU AGREE TO INDEMNIFY BioRefineryEPC™ , AND ITS AFFILIATES, OFFICERS, AGENTS, AND EMPLOYEES AGAINST ANY CLAIM OR DEMAND, INCLUDING REASONABLE ATTORNEYS' FEES, RELATED TO YOUR USE, RELIANCE, OR ADOPTION OF THE DATA FOR ANY PURPOSE WHATSOEVER. THE DATA ARE PROVIDED BY BioRefineryEPC™ "AS IS" AND ANY EXPRESS OR IMPLIED WARRANTIES, INCLUDING BUT NOT LIMITED TO THE IMPLIED WARRANTIES OF MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY DISCLAIMED. IN NO EVENT SHALL BioRefineryEPC™ BE LIABLE FOR ANY SPECIAL, INDIRECT OR CONSEQUENTIAL DAMAGES OR ANY DAMAGES WHATSOEVER, INCLUDING BUT NOT LIMITED TO CLAIMS ASSOCIATED WITH THE LOSS OF DATA OR PROFITS, WHICH MAY RESULT FROM ANY ACTION IN CONTRACT, NEGLIGENCE OR OTHER TORTIOUS CLAIM THAT ARISES OUT OF OR IN CONNECTION WITH THE USE OR PERFORMANCE OF THE DATA.
pilot plant is a small system which is operated to find out about the behavior of a process before using it on a large industrial scale. so, this presentation tries to illustrate its objective and significance to understand the methodologies of various pharmaceutical dosage forms.
Introduction to Hazard Studies
CONTENTS
1 INTRODUCTION
2 HAZARD EVALUATION TECHNIQUES
2.1 Hazard Identification and Control
2.2 Selection of Technique
2.3 GBHE Hazard Study Procedure
2.3.1 Study One – Concept stage hazard review
2.3.2 Study two - Front-end engineering design
and project definition
2.3.3 Study three – detailed design hazard study
2.3.4 Study four – construction/ design verification
2.3.5 Study five – pre-commissioning safety review
2.3.6 Study six – project close-out/ post start-up review
2.4 Application of Hazard Study Procedure
2.5 Outcomes from the Process
2.6 the Hazard Study Toolkit
2.7 Change Management/Modifications
3 HAZARD STUDY LEADER CAPABILITY AND APPOINTMENT
REFERENCES
APPENDICES
A THE PROJECT PROCESS
B GBHE HAZARD STUDY TOOLKIT
(No Plagiarism) Explain the statement Although many leading organi.docxtamicawaysmith
(No Plagiarism) Explain the statement: "Although many leading organizations have invested significant resources in developing the culture and routines for this innovation processes, most organizations continue to rely on the efforts of a handful of people and chance. An innovative organization is one that can perfect these routines in addition to creating an innovation culture in the organization that engages people. Five key routines can facilitate its management of the innovation process” (Dooley & O'Sullivan, 2003).
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What made you choose this career path What advice do you hav.docxtamicawaysmith
What made you choose this career path?
What advice do you have for those hoping to enter this career path?
What were some obstacles you faced upon graduating from college?
Does your career require graduate school? What programs would be acceptable?
Is there anything you wish you would have done differently?
Is it difficult to find a job in this area?
What is a typical work week like?
Etcetera, depending on the field and what you’re interested in.
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Jean-Bapiste Belley
Harriet Elizabeth Brown
Monte Irvin
Shirley Graham Dubois
Vernon Dahmer
Hale Woodruff
Jo Ann Robinson
Eugene "Pineapple" Jackson
Dr. Francis Cress Welsing
Dr. Kenneth Clark
Amy Jacques Garvey
Ophelia DeVore
Augusta Fells Savage
Eugene Jacques Bullard
Bobby Timmons
Clyde Kennard
Madison Washington
Joseph Winters
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Joseph Rainey
Bessie Stringfield
DJ Kool Herc
Lonnie Clayton
Mrs. Mamie Lang Kirkland
Lucius Septimius Bassianus
Carolyn Gudger
Jasmine Twitty
Daisy Bates
Ella Jenkins
Lewis Henry Douglass
Cynthia Robinson
Sylvester Magee
Mabel Fairbanks
Cathay Williams
Clara Belle Williams
John Baxter Taylor Jr.
Anna J. Cooper
The Black Seminoles
Dr. Daniel Hale Williams
Matthew Williams
Phillipa Schuyler
Yarrow Mamout
Mamie "Peanut" Johnson
Frank E. Petersen
"Miss Maggie" Walker
Paul Robeson
Olivia J. Hooker
Dr. Henry T Sampson
Lovie Yancy
Willie James Howard
Toni Stone (Marcenia Lyle Alberga)
Lucien Victor Alexis
Mevinia Sheilds
Dr. Lonnie Smith
Rosewood
Miss Jane Pittman
Lucy Terry
Abraham Galloway
Thomas Jennings
Irene Morgan
Paul Lawrence Dunbar
Jean Toomer
Doris Payne
Ann Petry
Madam C.J. Walker
Dr. May Edward Chinn
Greenwood, Tulsa, OK
Karen Bass
Dr. Dorothy Height
Dr. Geneva Smitherman
Michaëlle Jean
Robin Kelly
Mary Macleod Bethune
Jane Bolin
Donna Edwards
Dame Eugenia Charles
Dr. Thomas Elkins
Wilma Rudolph
Annie Malone
Ann Lowe
Black Wall Street
Cathy Hughes
Kamala Harris
Fannie Lou Hamer
Sarah Rector
Ruth Simmons
Claudette Colvin
MC Lyte
Benajin Banneker
Benjamin O. Davis, Jr.
Thurgood Marshall
Doris "Dorie" Miller
Cecil Noble
WC Handy
Dorothy Counts
Bayard Rustin
Dr. Eliza Ann Grier
Matthew Henson
Jesse Owens
Nina Simone
Wendell Scott
Adam Clayton Powell
Percy Julian
Dr. Charles Drew
Thomas "Fats" Waller
Satchel Paige
Bass Reeves
Marian Anderson
Josephine Baker
Joe Louis
Walter White
William Hastie
Elijah McCoy
Jan Matzelger
Lewis Latimer
Granville T. Woods
Fred Jones
Nella Larsen
Lloyd Hall
A. Philip Randolph
Althea Gibson
Barbara C. Jordon
Marcus Garvey
Malcolm X
James Meridith
Guy Buford
Hazel Scott
Stokely Carmichal
Denmark Vessey
Alex Haley
Virginia Hamilton
Ishmael Reed
Nalo Hopkinson
George Schuyler
Patricia Roberts Harris
John Lewis
Les McCann
Martin Delany
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▪ What are your current goals
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Physical fitness benchmark assessments
Fitness assessment data sheet
Exercise charts
Personal physical fitness progress chart
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⦁One to two paragraph brief summary of the book. ⦁Who is the.docxtamicawaysmith
⦁One to two paragraph brief summary of the book.
⦁Who is the author and his/her background?
⦁Does the author have any particular ideological viewpoint that he or she is trying to advance or do you consider the author to have been neutral and presented both sides of controversial issues? (You will find asking this same question will help you in other courses and your future career.)
⦁When was this book written? Does the author reflect the views (biases) of the time when the book was written? Why or why not?
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⦁What additional topics should the author have included in the book? Why?
⦁How had people before the age of the telegraph attempted to communicate faster over distances?
⦁How did the telegraph reflect scientific and technological developments, both in the United States and other countries?
⦁Why did the telegraph represent such a revolutionary development and not just an incremental improvement in communication?
⦁How did the telegraph impact politics, journalism, business, military strategy and society in general?
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⦁Do you think the author makes the material interesting, understandable and relevant to the general public? Why or why not?
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100.0 Criteria10.0 Part 1 PLAAFP The PLAAFP thoroughly an.docxtamicawaysmith
100.0 %Criteria
10.0 %Part 1: PLAAFP
The PLAAFP thoroughly and adeptly incorporates student's academic strengths, evaluations, performance in classes, and any other relevant issues.
10.0 %Part 2: Present Levels for Transition COE 3.8 [CEC 5.1, ICSI.5.S8, ICSI.5.S15, IGC.5.K1, IGC.5.S7, IGC.5.S23, IGC.5.S24; InTASC 1(b), 2(d), 5(f), 6(v), 8(s), 9(h); MC2, MC3, MC4, MC5]
Preferential learning environment, strengths and interests relating to the transition, and areas in need of improvement for transition are substantially described.
15.0 %Part 2: Transition Plan COE: 3.10 [CEC 5.5, ICSI.5.S8, ICSI.5.S8, ICSI.5.S15, ICSI.5.S17, ICSI.5.S19, IGC.5.K1, IGC.5.K3, IGC.5.K8, IGC.5.S1, IGC.5.S2, IGC.5.S11 IGC.5.S23, IGC.5.S24; InTASC 7(b), 7(e); MC1, MC2, MC4, MC5]
The transition plan demonstrates best practices in identifying proficient, measureable transition plan goals that are aligned with student's interests and present levels. Also includes quality aligned activities/services, persons/agency involved and realistic expected dates of achievement.
10.0 %Part 3: Rationale - Justification COE: 5.1 [ACEI 5.0; CEC 6.1, ICSI.6.K2, ICSI.6.K4 ICSI.6.S1, ICSI.6.S2, ICSI.6.S3, ICSI.6.S4, ICSI.6.S5, ICSI.6.S7, IGC.6.K4, IGC.6.K6, IGC.6.S2; InTASC 9(l), 9(o); MC2, MC3, MC4]
Rationale skillfully justifies content and decisions displayed in PLAAFP, annual goals, and transition plan, convincingly demonstrating how they meet the needs of the student. Claims are fully grounded in CEC Code of Ethics.
15.0 %Part 4: Rationale - Confidentiality COE: 5.8 [CEC 6.1, ICSI.6.S1, ICSI.6.S2, ICSI.6.S4, ICSI.7.S1, IGC.6.K1, IGC.6.K6; InTASC 5(k); MC1, MC2, MC4, MC5]
The rationale thoroughly defends the legal, ethical, and quality requirements related to the management of confidential student information.
10.0 %Reflection COE: 5.4 [CEC 6.2, ICSI.6.S1, ICSI.6.S2, ICSI.6.S4, IGC.6.K1, IGC.6.K2, IGC.6.K3; InTASC 10(h); MC1, MC2, MC4; COE 5.4]
Reflection convincingly relates how foundational knowledge developed relating to providing professional, ethical and legal educational services will be used in future professional practice.
5.0 %Research
Research strongly supports the information presented. Sources are timely, distinctive and clearly address all of the criteria stated in the assignment.
10.0 %Organization
The content is well-organized and logical. There is a sequential progression of ideas that relate to each other. The content is presented as a cohesive unit and provides the audience with a clear sense of the main idea.
10.0 %Mechanics of Writing (includes spelling, punctuation, grammar, language use)
Submission is virtually free of mechanical errors. Word choice reflects well-developed use of practice and content-related language. Sentence structures are varied and engaging.
5.0 %Documentation of Sources (citations, footnotes, references, bibliography, etc., as appropriate to assignment and style)
Sources are documented completely and correctly, as appropria.
102120151De-Myth-tifying Grading in Sp.docxtamicawaysmith
10/21/2015
1
De-Myth-tifying Grading
in Special Education
1980 2015
10/21/2015
2
Primary Purpose
• “the primary purpose of…grades…
(is) to communicate student
achievement to students, parents,
school administrators,
post-secondary institutions and
employers.” and
• To provide teachers with information
for instructional planning.
Taken from “Reporting Achievement at the Secondary School Level: What and How?”, in Communicating Student
Learning: ASCD Yearbook 1996, p. 120.
What makes grading so
hard?
• Teacher preparation programs seldom include course work or
even discussions of recommended practices for grading
students in general, much less for students who may be
struggling learners. As a result, teachers at all grade levels
grapple with issues of fairness in grading.
• Despite the magnitude of this problem, few recommendations
for grading struggling learners can be found in the research
literature or in education policy.
• Urban Grading Legends
10/21/2015
3
Urban Legends:
Bigfoot/Sasquatch
Urban Legends
• I can’t fail a special education
student.
• I give all my Life Skills students an
85.
• The report card grade does not really
mean anything.
10/21/2015
4
Urban Legends
• The grade on the report card can’t be less
than the IEP mastery level (default 70%)
• I teach a lot in my classroom, but I can
only grade the things that are on the IEP.
• I don’t do the grades for my special
education students in my classroom, the
special education teacher does that for
me.
What’s the
problem??
• Some students are not getting REAL
grades.
• Multiple court cases regarding failing
students who are not receiving
appropriate specially designed instruction
or students only get “A’s” and it doesn’t
truly reflect how he/she really performs in
relation to the curriculum
10/21/2015
5
What does the law really
say?
• Neither the Individuals with Disabilities Education Act
(IDEA) nor any other federal education laws contain
requirements for grading. Therefore, each state has
discretion on the issue.
• The TEC is the set of state laws our state legislators have
passed that relate to education. ARD committees do not
have the authority to override state laws. The Texas
Administrative Code (TAC) is the set of rules that the State
Legislature has authorized Texas Education Agency (TEA)
or the State Board to write. ARD committees must also
follow these rules.
• The state statutes apply to all public school students in
Texas regardless of special education eligibility.
Local Grading Policies
TEC §28.0216
(1) “must require a classroom teacher to assign a grade that
reflects the students’ relative mastery of an assignment;
[and]
(2) may not require a classroom teacher to assign a
minimum grade for an assignment without regard to the
student’s quality of work.”
(3) may allow a student a reasonable opportunity to make up
or redo a class .
100.0 %Criteria
30.0 %Flowchart Content
The flowchart skillfully depicts the two possible discipline paths following the manifestation determination. In addition, there are two comprehensively aligned IEP goals for each determination.
40.0 %Legal Issues Analysis
A compelling analysis is included regarding any legal issues raised by the change in Carrie's transportation, proficiently incorporating relevant statutes, regulations, and case decisions.
5.0 %Research
Research strongly supports the information presented. Sources are timely, distinctive and clearly address all of the criteria stated in the assignment.
5.0 %Rationale Organization
The content is well organized and logical. There is a sequential progression of ideas related to each other. The content is presented as a cohesive unit and the audience is provided with a clear sense of the main idea.
5.0 %Overall Flowchart Presentation
The work is well presented. The overall appearance is neat and professional. Work would be highly desirable for public dissemination.
10.0 %Mechanics of Writing (includes spelling, punctuation, grammar, language use)
Submission is virtually free of mechanical errors. Word choice reflects well-developed use of practice and content-related language. Sentence structures are varied and engaging.
5.0 %Documentation of Sources (citations, footnotes, references, bibliography, etc., as appropriate to assignment and style)
Sources are documented completely and correctly, as appropriate to assignment and style, and format is free of error.
100 %Total Weightage
.
100 words agree or disagree to eac questions Q 1.As her .docxtamicawaysmith
100 words agree or disagree to eac questions
Q 1.
As her defense attorney, I will argue that the officer did not only not read Sally's Miranda rights; he also did not respect her right to consul. After Sally made her allegedly verbal utterance, the Officer should have known to read Sally her rights. I will bring up that during New Jersey v. James P. Kucinski, Oct 26, 2016, the defendant was arrested for the bludgeoning death of his brother. The defendant was taken to police headquarters for questioning after the defendant was advised of his Miranda rights; he requested an attorney. The law enforcement officers terminated the interrogation, spoked with their supervisor, and approximately eight minutes later, the officers returned into the room and advised the defendant that he was being charged with murder. The scare tactic worked, and the defendant asked to speak with the officers. The defendant reluctantly answered a series of questions. Before trial, the defendant moved for suppression motion because the officers did not honor his request for counsel. The court denied the motion, during further questioning the defendant claimed to have acted in self-defense, the defense counsel moved for a mistrial. The trial court denied the motion for mistrial but instructed the jury that the defendant's right to remain silent should be limited to assessing his credibility. The defendant was charged with first-degree murder and third-degree possession of a weapon for unlawful purposes The Appellate Division reversed the defendant's conviction and motion for a new trial due to the prosecutor's question doing cross-examination was improper. The panel concluded that the defendant invoked his right to remain silent by telling law enforcement officers that he did not want to talk or answer questions. The Appellate Division found that the trial court instructions to the jury were flaws, and the supreme court agreed and affirmed. The officers should have stopped all questioning and contacted the defendant's attorney.
New Jersey v. Kucinski (2017). https://law.justia.com/cases/new-jersey/supreme-court/2017/a-58-15.html
Q 2.
My last name begins with a K. so I am answering in the role of prosecutor. Sally was originally pulled over because she had shown probable cause of drunk driving. Upon her traffic stop, Sally was then searched after being arrested and the handgun and drugs were found on her body. The police asked about the two items but did not “interrogate” her. Sally voluntarily answered the arresting officers’ questions and in doing so piled new charges onto her initial arrest charge. I believe that the judge will deny the request to suppress the admission of Sally’s statements. Sally does have rights under the Fifth Amendment, but her statements to the police officers were not coerced out of her. The Cornell Law School website states that the Fifth Amendment, under the self-incrimination clause, if an individual makes a spo.
101118, 4(36 PMCollection – MSA 603 Strategic Planning for t.docxtamicawaysmith
10/11/18, 4(36 PMCollection – MSA 603 Strategic Planning for the Admin ...
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Thread: dis 4
Post: dis 4
Author:
Posted Date: October 9, 2018 8:50 PM
Status: Published
Overall Rating:
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(Post is Read)
Brian Mcleod
I would say that for them to move the work and still be ethical defensible are work conditions,
respect for labor laws of the parent company, and job opportunities for the long-term
employees.
To expand on this would be the work conditions. The conditions that the workers have to work
under should be the same conditions that workers in the US have to work under. This involves
safety and environmental protection for the workers.
Labor laws of the host country and “most” of the internally recognized laws must be observed.
Overtime and child labor are a couple of items.
The long-term employees should be given the opportunity to move to another US based plant if
possible or to the new country.
Sometimes because of the state of the industry companies do have to make these decisions or
face possible bankruptcy. This alternative may not be the perfect solution but better than
bankrupting a company that still has operation in the US.
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10/11/18, 4(38 PMCollection – MSA 603 Strategic Planning for the Admin ...
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Thread: DB4
Post: DB4
Author:
Posted Date: October 10, 2018 8:51 PM
Status: Published
Overall Rating:
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(Post is Read)
Christina Lacroix
It is ethically defensible to outsource production when the outcome of not outsourcing
would negatively impact stakeholders. Organizations define their most important
stakeholders, often the shareholders, as they invested capital. While some risk is
assumed by shareholders as a fiduciary managers have an obligation to the
shareholders to protect their interest when possible. A company risks shareholder
investment (access to capital) and jeopardizes all other stakeholders such as
employees, suppliers, and creditors. An organization cannot risk itself and the other
stakeholders depending upon in order to save employees.
The organization should do its due diligence in securing its outso.
100 words per question, no references needed or quotations. Only a g.docxtamicawaysmith
100 words per question, no references needed or quotations. Only a general idea or opinion.
A.
· Compare and contrast two works from the Italian Baroque period with two works from the Renaissance. Be sure to note the appearance in the works of the defining characteristics from each period.
· Discuss why artistic expression shifted from the restrained stoicism of the Renaissance to that of the heightened emotion in the religious and other works of the Baroque.
B. From video
Goya -
The Third of May
- If you cannot see this video, click here -
https://youtu.be/e7piV4ocukg
Respond in writing to the following questions after reading Chapter 12, watching the video, and exploring the sites above.
1. Heroism, nationalism, and passion are themes associated with Romanticism. Which
three
landmarks of the nineteenth century are most representative of these themes? You can discuss art, philosophy, or literature.
2. Compare Neoclassicism and Romanticism as styles and sensibilities. What do their differences reflect about patronage, popular taste, and historical change? Provide specific examples from the chapters.
C.
1. From the arts of West Africa, what are some characteristics of African cultural heritage?
2. How did their religious beliefs influence their art and music.
D.
Watch video below
Manet -
Déjeuner
sur
l’herbe -
If you cannot see this video, click
https://youtu.be/3xBGF8H3bQ4
1. Viewers of Manet’s
Déjeuner sur l’herbe
initially responded to its public display by attacking the canvas with their umbrellas. Why?
2. What kind of art has evoked a comparable response in our own time? Do some research online. Find a recent work of art that caused controversy. Summarize the reasons for the controversy and your reaction to it. Try not post the same article as someone else. (This board is not POST FIRST, so you will be able to see what others have posted right away.) If you can, attach a picture of the image you are describing to your posting.
E.
Watch the video below. If you cannot see the video, click here:
https://youtu.be/XyLNPumMMTs
George Braque, Violin and Pitcher, (1909)
•
Pablo Picasso, Guernica, (1937)
•
Marcel Duchamp, Nude Descending a Staircase, (1912)
Respond in writing to the following question after reading Chapter 14 in your text, watching the video above, viewing the Web Assignments, and the sites above.
1. Describe how they three have departed from styles such as symbolism and impressionism of the late nineteenth century.
F.
Take some time to reflect on all we have covered in this course. Then, respond in writing to the following question.
1. After your experience in this course, describe why you feel the humanities are important.
.
100A 2
2 4 4
5
1A 1034 5
1B 1000 10
1C 1100 1
1D 1123 20
1E 1210 5
20 10 10
7
1A 2180 20
1B 1283 20
1C 3629 5
1D 3649 3
1E 4051 15
1F 4211 1
1G 5318 5
100B 1
2 4 1
3
1A 2180 10
1B 1283 10
1C 3629 5
100C 2
0 0 0
3
1A 6774 5
1B 6869 5
1C 6879 2
0 0 0
4
1A 6774 2
1B 6869 5
1C 6879 1
1D 7555 10
100D 1
10 5 3
3
1A 2180 5
1B 3649 2
1C 4211 3
Self-care and Residency Reflection Paper Scoring Rubric -
Content
80 Points
Points Earned
Additional Comments:
All key elements of the assignment are covered in a substantive way.
Write a 700- to 1,050-word paper to reflect on your residency experience and outline your plan for self-care. Please use the self-care and residency reflection paper template posted in Student Materials for this assignment.
Consider the following questions when writing your reflection:
a) What have you learned about yourself during residency?
b) What have you learned about yourself as a counselor-in-training during residency?
c) What are aspects of residency that you enjoyed? Why did you enjoy these aspects?
d) What aspects of residency did you not enjoy? Why did you not enjoy these aspects?
e) What is counselor self-care? Why is it important? Include two separate in-text and end of work references.
f) What strategies for maintaining self-care did you try throughout this program? How can you implement these strategies?
g) How will you know when you are experiencing burnout? What can you do to prevent this?
The content is comprehensive, accurate, and /or persuasive.
The paper links theory to relevant examples of current experience and industry practice and uses the vocabulary of the theory correctly. This refers to the use of literary references. Generally you will need one separate literary reference for each main point (objective) of your paper.
Major points are stated clearly and are supported by specific details, examples, or analysis.
Organization / Development
35 Points
Points Earned
Additional Comments:
The paper has a structure that is clear, logical, and easy to follow.
The paper develops a central theme or idea, directed toward the appropriate audience.
The introduction provides sufficient background on the topic and previews major points.
The conclusion is logical, flows from the body of the paper, and reviews the major points.
Transitions between sentences/ paragraphs/sections aid in maintaining the flow of thought.
The tone is appropriate to the content and assignment.
Mechanics
35 Points
Points Earned
Additional Comments:
The paper, including the title page, reference page, tables, and appendices follow APA guidelines for format.
Citations of original works within the body of the paper follow APA guidelines.
The paper is laid out with effective use of headings, font styles, and white space.
Rules of grammar, usage, and punctuation are followed.
Sentences are complete, clear, concise, and varied.
Spelling is correct.
.
10122018Week 5 Required Reading and Supplementary Materials - .docxtamicawaysmith
10/12/2018
Week 5 Required Reading and Supplementary Materials - MGMT 670 9042 Strategic Management Capstone (2188)
https://learn.umuc.edu/d2l/le/content/333174/viewContent/13406413/View
/2
Required Readings:
From the UMUC library: (Note: You must search for these articles in the UMUC library. In the case of video links in the UMUC library, exact directions are given on how to find the video.)
Porter's Five-Forces model. (2009). In Encyclopedia of management (6th Ed., pp. 714-717).
From Other websites:
Evaluating the industry. (2012). In Mastering strategic management. Washington, DC: Saylor Academy. Retrieved from https://saylordotorg.github.io/text_mastering-strategic-management/s07-03-evaluating-the-industry.html
The impact of external and internal factors on strategy. (2016, 31 May). In Boundless Management. Retrieved from https://courses.lumenlearning.com/boundless-management/chapter/strategic-management/
Mapping strategic groups. (2012). In Mastering strategic management. Washington, DC: Saylor Academy. Retrieved from https://saylordotorg.github.io/text_mastering-strategic-management/s07-04-mapping-strategic-groups.html
The PESTEL and SCP frameworks. (2016, 26 May). In Boundless management. Retrieved from https://courses.lumenlearning.com/boundless-management/chapter/external-inputs-to-strategy/
The relationship between an organization and its environment. (2012). In Mastering strategic management. Washington, DC: Saylor Academy. Retrieved from https://saylordotorg.github.io/text_mastering-strategic-management/s07-01-the-relationship-between-an- or.html
Strategic group mapping. (2010, October 5). MBA lectures. Retrieved from http://mba-lectures.com/management/strategic- management/1000/strategic-group-mapping.html
Supplementary Materials:
From the UMUC library: (Note: You must search for these articles in the UMUC library. In the case of video links in the UMUC library, exact directions are given on how to find the video.)
Anand, B. N. (2006). Crafting business strategy and environmental scanning [Video]. Harvard Business School Faculty Seminar Series.
Follow these steps to find this video:
Go to http://sites.umuc.edu/library/index.cfm
Type in the entire name of the article: "Crafting business strategy and environmental scanning," into the search box and click on "search."
Click on "multimedia" in the upper left hand corner of the webpage (under "Ask a Librarian.)
Type in the entire name of the article: "Crafting business strategy and environmental scanning," in the box at the top of the page to the left of the word, "Search."
Make sure only "Business Videos" and "Find all my search term" are the only boxes that are checked. Uncheck both "Image Collection" and "Apply equivalent
subjects"
Click on "Search" at the bottom right hand corner of the webpage. It is a small word in a box. The next page shows the article. Click on the article.
Dahab, S. (2008). Five forces. In S. R. Clegg & J. R. Bailey (Eds.), International en.
101416 526 PMAfter September 11 Our State of Exception by .docxtamicawaysmith
10/14/16 5:26 PMAfter September 11: Our State of Exception by Mark Danner | The New York Review of Books
Page 1 of 11http://www.nybooks.com/articles/2011/10/13/after-september-11-our-state-exception/?printpage=true
After September 11: Our State of Exception
Mark Danner OCTOBER 13, 2011 ISSUE
We are in a fight for our principles, and our first responsibility is to live by them.
—George W. Bush, September 20, 2001
1.
We are living in the State of Exception. We don’t know when it will end, as we don’t know when the War on Terror will
end. But we all know when it began. We can no longer quite “remember” that moment, for the images have long since
been refitted into a present-day fable of innocence and apocalypse: the perfect blue of that late summer sky stained by acrid
black smoke. The jetliner appearing, tilting, then disappearing into the skin of the second tower, to emerge on the other
side as a great eruption of red and yellow flame. The showers of debris, the falling bodies, and then that great blossoming
flower of white dust, roiling and churning upward, enveloping and consuming the mighty skyscraper as it collapses into the
whirlwind.
To Americans, those terrible moments stand as a brightly lit portal through which we were all compelled to step, together,
into a different world. Since that day ten years ago we have lived in a subtly different country, and though we have grown
accustomed to these changes and think little of them now, certain words still appear often enough in the news—
Guantánamo, indefinite detention, torture—to remind us that ours remains a strange America. The contours of this
strangeness are not unknown in our history—the country has lived through broadly similar periods, at least half a dozen or
so, depending on how you count; but we have no proper name for them. State of siege? Martial law? State of emergency?
None of these expressions, familiar as they may be to other peoples, falls naturally from American lips.
What are we to call this subtly altered America? Clinton Rossiter, the great American scholar of “crisis government,”
writing in the shadow of World War II, called such times “constitutional dictatorship.” Others, more recently, have spoken
of a “9/11 Constitution” or an “Emergency Constitution.” Vivid terms all; and yet perhaps too narrowly drawn, placing as
they do the definitional weight entirely on law when this state of ours seems to have as much, or more, to do with politics
—with how we live now and who we are as a polity. This is in part why I prefer “the state of exception,” an umbrella term
that gathers beneath it those emergency categories while emphasizing that this state has as its defining characteristic that it
transcends the borders of the strictly legal—that it occupies, in the words of the philosopher Giorgio Agamben, “a position
at the limit between politics and law…an ambiguous, uncertain, borderline fringe, at the intersection of the legal and the
political.”
Call it, then, the s.
100 words per question, no references needed or quotations. Only.docxtamicawaysmith
100 words per question, no references needed or quotations. Only a general idea or opinion.
A.
· Compare and contrast two works from the Italian Baroque period with two works from the Renaissance. Be sure to note the appearance in the works of the defining characteristics from each period.
· Discuss why artistic expression shifted from the restrained stoicism of the Renaissance to that of the heightened emotion in the religious and other works of the Baroque.
B. From video
Goya -
The Third of May
- If you cannot see this video, click here -
https://youtu.be/e7piV4ocukg
Respond in writing to the following questions after reading Chapter 12, watching the video, and exploring the sites above.
1. Heroism, nationalism, and passion are themes associated with Romanticism. Which
three
landmarks of the nineteenth century are most representative of these themes? You can discuss art, philosophy, or literature.
2. Compare Neoclassicism and Romanticism as styles and sensibilities. What do their differences reflect about patronage, popular taste, and historical change? Provide specific examples from the chapters.
C.
1. From the arts of West Africa, what are some characteristics of African cultural heritage?
2. How did their religious beliefs influence their art and music.
D.
Watch video below
Manet -
Déjeuner
sur
l’herbe -
If you cannot see this video, click
https://youtu.be/3xBGF8H3bQ4
1. Viewers of Manet’s
Déjeuner sur l’herbe
initially responded to its public display by attacking the canvas with their umbrellas. Why?
2. What kind of art has evoked a comparable response in our own time? Do some research online. Find a recent work of art that caused controversy. Summarize the reasons for the controversy and your reaction to it. Try not post the same article as someone else. (This board is not POST FIRST, so you will be able to see what others have posted right away.) If you can, attach a picture of the image you are describing to your posting.
E.
Watch the video below. If you cannot see the video, click here:
https://youtu.be/XyLNPumMMTs
George Braque, Violin and Pitcher, (1909)
•
Pablo Picasso, Guernica, (1937)
•
Marcel Duchamp, Nude Descending a Staircase, (1912)
Respond in writing to the following question after reading Chapter 14 in your text, watching the video above, viewing the Web Assignments, and the sites above.
1. Describe how they three have departed from styles such as symbolism and impressionism of the late nineteenth century.
F.
Take some time to reflect on all we have covered in this course. Then, respond in writing to the following question.
1. After your experience in this course, describe why you feel the humanities are important.
Edit question's body
.
Embracing GenAI - A Strategic ImperativePeter Windle
Artificial Intelligence (AI) technologies such as Generative AI, Image Generators and Large Language Models have had a dramatic impact on teaching, learning and assessment over the past 18 months. The most immediate threat AI posed was to Academic Integrity with Higher Education Institutes (HEIs) focusing their efforts on combating the use of GenAI in assessment. Guidelines were developed for staff and students, policies put in place too. Innovative educators have forged paths in the use of Generative AI for teaching, learning and assessments leading to pockets of transformation springing up across HEIs, often with little or no top-down guidance, support or direction.
This Gasta posits a strategic approach to integrating AI into HEIs to prepare staff, students and the curriculum for an evolving world and workplace. We will highlight the advantages of working with these technologies beyond the realm of teaching, learning and assessment by considering prompt engineering skills, industry impact, curriculum changes, and the need for staff upskilling. In contrast, not engaging strategically with Generative AI poses risks, including falling behind peers, missed opportunities and failing to ensure our graduates remain employable. The rapid evolution of AI technologies necessitates a proactive and strategic approach if we are to remain relevant.
A Strategic Approach: GenAI in EducationPeter Windle
Artificial Intelligence (AI) technologies such as Generative AI, Image Generators and Large Language Models have had a dramatic impact on teaching, learning and assessment over the past 18 months. The most immediate threat AI posed was to Academic Integrity with Higher Education Institutes (HEIs) focusing their efforts on combating the use of GenAI in assessment. Guidelines were developed for staff and students, policies put in place too. Innovative educators have forged paths in the use of Generative AI for teaching, learning and assessments leading to pockets of transformation springing up across HEIs, often with little or no top-down guidance, support or direction.
This Gasta posits a strategic approach to integrating AI into HEIs to prepare staff, students and the curriculum for an evolving world and workplace. We will highlight the advantages of working with these technologies beyond the realm of teaching, learning and assessment by considering prompt engineering skills, industry impact, curriculum changes, and the need for staff upskilling. In contrast, not engaging strategically with Generative AI poses risks, including falling behind peers, missed opportunities and failing to ensure our graduates remain employable. The rapid evolution of AI technologies necessitates a proactive and strategic approach if we are to remain relevant.
How to Make a Field invisible in Odoo 17Celine George
It is possible to hide or invisible some fields in odoo. Commonly using “invisible” attribute in the field definition to invisible the fields. This slide will show how to make a field invisible in odoo 17.
The French Revolution, which began in 1789, was a period of radical social and political upheaval in France. It marked the decline of absolute monarchies, the rise of secular and democratic republics, and the eventual rise of Napoleon Bonaparte. This revolutionary period is crucial in understanding the transition from feudalism to modernity in Europe.
For more information, visit-www.vavaclasses.com
Biological screening of herbal drugs: Introduction and Need for
Phyto-Pharmacological Screening, New Strategies for evaluating
Natural Products, In vitro evaluation techniques for Antioxidants, Antimicrobial and Anticancer drugs. In vivo evaluation techniques
for Anti-inflammatory, Antiulcer, Anticancer, Wound healing, Antidiabetic, Hepatoprotective, Cardio protective, Diuretics and
Antifertility, Toxicity studies as per OECD guidelines
Model Attribute Check Company Auto PropertyCeline George
In Odoo, the multi-company feature allows you to manage multiple companies within a single Odoo database instance. Each company can have its own configurations while still sharing common resources such as products, customers, and suppliers.
2024.06.01 Introducing a competency framework for languag learning materials ...Sandy Millin
http://sandymillin.wordpress.com/iateflwebinar2024
Published classroom materials form the basis of syllabuses, drive teacher professional development, and have a potentially huge influence on learners, teachers and education systems. All teachers also create their own materials, whether a few sentences on a blackboard, a highly-structured fully-realised online course, or anything in between. Despite this, the knowledge and skills needed to create effective language learning materials are rarely part of teacher training, and are mostly learnt by trial and error.
Knowledge and skills frameworks, generally called competency frameworks, for ELT teachers, trainers and managers have existed for a few years now. However, until I created one for my MA dissertation, there wasn’t one drawing together what we need to know and do to be able to effectively produce language learning materials.
This webinar will introduce you to my framework, highlighting the key competencies I identified from my research. It will also show how anybody involved in language teaching (any language, not just English!), teacher training, managing schools or developing language learning materials can benefit from using the framework.
Acetabularia Information For Class 9 .docxvaibhavrinwa19
Acetabularia acetabulum is a single-celled green alga that in its vegetative state is morphologically differentiated into a basal rhizoid and an axially elongated stalk, which bears whorls of branching hairs. The single diploid nucleus resides in the rhizoid.
Normal Labour/ Stages of Labour/ Mechanism of LabourWasim Ak
Normal labor is also termed spontaneous labor, defined as the natural physiological process through which the fetus, placenta, and membranes are expelled from the uterus through the birth canal at term (37 to 42 weeks
Operation “Blue Star” is the only event in the history of Independent India where the state went into war with its own people. Even after about 40 years it is not clear if it was culmination of states anger over people of the region, a political game of power or start of dictatorial chapter in the democratic setup.
The people of Punjab felt alienated from main stream due to denial of their just demands during a long democratic struggle since independence. As it happen all over the word, it led to militant struggle with great loss of lives of military, police and civilian personnel. Killing of Indira Gandhi and massacre of innocent Sikhs in Delhi and other India cities was also associated with this movement.
1. 3546-1 Revision 0
February 2007
METHOD 3546
MICROWAVE EXTRACTION
SW-846 is not intended to be an analytical training manual.
Therefore, method
procedures are written based on the assumption that they will be
performed by analysts who are
formally trained in at least the basic principles of chemical
analysis and in the use of the subject
technology.
In addition, SW-846 methods, with the exception of required
method use for the analysis
of method-defined parameters, are intended to be guidance
methods which contain general
information on how to perform an analytical procedure or
technique which a laboratory can use
as a basic starting point for generating its own detailed Standard
Operating Procedure (SOP),
either for its own general use or for a specific project
application. The performance data
included in this method are for guidance purposes only, and are
not intended to be and must
not be used as absolute QC acceptance criteria for purposes of
laboratory accreditation.
1.0 SCOPE AND APPLICATION
2. 1.1 This method is a procedure for extracting water insoluble or
slightly water soluble
organic compounds from soils, clays, sediments, sludges, and
solid wastes. This method was
developed and validated on commercially-available solvent
extraction systems. Its procedure
uses microwave energy to produce elevated temperature and
pressure conditions (i.e., 100 -
115 EC and 50 - 175 psi) in a closed vessel containing the
sample and organic solvent(s) to
achieve analyte recoveries equivalent to those from Soxhlet
extraction (Method 3540), using
less solvent and taking significantly less time than the Soxhlet
procedure. Other systems and
other types of vessels may be used, provided that the analyst
demonstrates appropriate
performance for the specific application.
1.2 This method is applicable to the extraction of semivolatile
organic compounds,
organophosphorus pesticides, organochlorine pesticides,
chlorinated herbicides, phenoxyacid
herbicides, substituted phenols, PCBs, and PCDDs/PCDFs,
which may then be analyzed by a
variety of chromatographic procedures. This method may also
be applicable for the extraction
of additional target analytes, provided that the analyst
demonstrates adequate performance for
the intended application (see Method 3500 and Chapter Two).
1.3 This method has been validated for solid matrices
containing from 50 to 10,000
µg/kg of semivolatile organic compounds, 250 to 2,500 µg/kg
of organophosphorus pesticides,
10 to 5,000 µg/kg of organochlorine pesticides and chlorinated
herbicides, 50 to 2,500 µg/kg of
3. substituted phenols, 100 to 5,000 µg/kg of phenoxyacid
herbicides, 1 to 5,000 µg/kg of PCBs,
and 10 to 6000 ng/kg of PCDDs/PCDFs.
This method may be applicable to samples containing these
analytes at higher
concentrations and may be employed after adequate
performance is demonstrated for the
concentrations of interest (see Method 3500). It may also be
applicable to classes of analytes,
to fuel types, and to petroleum fractions other than those listed
in Sec 1.2. However, in order to
use this method for additional analytes, fuel types, petroleum
fractions, or different
concentrations, the analyst must demonstrate that the extraction
conditions are appropriate for
the analytes of interest. The analyst must also perform the
initial demonstration of proficiency
described in Sec. 9.2 and Methods 3500 and 8000. When
expanding this method to other fuel
types or petroleum hydrocarbons, the boiling point range or
carbon number range of the
material should be carefully defined and the quantitation
approach be modified to match such
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ranges. Analysts are advised to consult authoritative sources,
such as the American Petroleum
Institute (API), for appropriate definitions of other fuel types or
petroleum fractions.
NOTE: Mention of the analyses of other fuel types and
4. petroleum fractions does not imply a
regulatory requirement for such analyses, using this or any
other method.
1.4 This method is only applicable to solid samples with small
particle sizes. If
practical, soil/sediment samples may be air-dried and ground to
a fine powder prior to
extraction. Alternatively, if worker safety or the loss of
analytes during drying is a concern,
soil/sediment samples may be mixed with anhydrous sodium
sulfate or pelletized diatomaceous
earth. (Drying and grinding samples containing PCDDs/PCDFs
is not recommended, due to
safety concerns.) The total mass of material to be prepared
depends on the specifications of the
determinative method and the sensitivity needed for the
analysis, but an amount of 2 - 20 g of
material is usually necessary and can be accommodated by this
extraction procedure.
1.5 This method has been validated using a solvent mixture of
hexane and acetone
(1:1) from matrices such as soil, glass-fibers and sand. This
solvent system or other solvent
systems may be employed, provided that adequate performance
is demonstrated for the
analytes of interest (see. Sec. 7.4).
1.6 Prior to employing this method, analysts are advised to
consult the base method
for each type of procedure that may be employed in the overall
analysis (e.g., Methods 3500,
3600, 5000, and 8000) for additional information on quality
control procedures, development of
QC acceptance criteria, calculations, and general guidance.
5. Analysts also should consult the
disclaimer statement at the front of the manual and the
information in Chapter Two for guidance
on the intended flexibility in the choice of methods, apparatus,
materials, reagents, and
supplies, and on the responsibilities of the analyst for
demonstrating that the techniques
employed are appropriate for the analytes of interest, in the
matrix of interest, and at the levels
of concern.
In addition, analysts and data users are advised that, except
where explicitly specified in a
regulation, the use of SW-846 methods is not mandatory in
response to Federal testing
requirements. The information contained in this method is
provided by EPA as guidance to be
used by the analyst and the regulated community in making
judgments necessary to generate
results that meet the data quality objectives for the intended
application.
1.7 Use of this method is restricted to use by, or under
supervision of, appropriately
experienced and trained analysts. Each analyst must
demonstrate the ability to generate
acceptable results with this method.
2.0 SUMMARY OF METHOD
2.1 Samples are prepared for extraction by grinding them to a
powder and loading
them into the extraction vessel.
WARNING: The drying and grinding of samples containing
PCDDs/PCDFs is not
6. recommended, due to safety concerns. Grinding may also be a
concern for other
more volatile analytes .
2.2 The appropriate solvent system is added to the vessel and
sealed.
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2.3 The extraction vessel containing the sample and solvent
system is heated to the
extraction temperature (see Sec. 11.9) and extracted for 10 min
(or as recommended by the
instrument manufacturer).
2.4 The mixture is allowed to cool. The vessel is opened and
the contents are filtered.
The solid material is rinsed and the various solvent fractions are
combined.
2.5 The extract may be concentrated, if necessary, and, as
needed, exchanged into a
solvent compatible with the cleanup or determinative procedure
to be employed.
3.0 DEFINITIONS
Refer to Chapter One and the manufacturer’s instructions for
definitions that may be
relevant to this analytical procedure.
4.0 INTERFERENCES
7. 4.1 Solvents, reagents, glassware, and other sample processing
hardware may yield
artifacts and/or interferences to sample analysis. All of these
materials must be demonstrated
to be free from interferences under the conditions of the
analysis by analyzing method blanks.
Specific selection of reagents and purification of solvents by
distillation in all-glass systems may
be necessary. Refer to each method to be used for specific
guidance on quality control
procedures and to Chapter Four for general guidance on the
cleaning of glassware.
4.2 Refer to Method 3500 for information regarding
intereferences
4.3 If necessary, Florisil and/or sulfur cleanup procedures may
be employed. In such
cases, proceed with Method 3620 and/or Method 3660.
4.4 Samples for PCDD/PCDF analysis should be subjected to
the various cleanup
procedures described in the determinative methods (Methods
8280 and 8290).
5.0 SAFETY
5.1 This method does not address all safety issues associated
with its use. The
laboratory is responsible for maintaining a safe work
environment and a current awareness file
of OSHA regulations regarding the safe handling of the
chemicals listed in this method. A
reference file of material safety data sheets (MSDSs) should be
available to all personnel
involved in these analyses.
8. 5.2 The use of organic solvents, elevated temperatures, and high
pressures in this
method present potential safety concerns in the laboratory.
Common sense laboratory
practices can be employed to minimize these concerns. The
sections to follow describe
additional steps that should be taken.
5.3 The extraction vessels are at elevated temperatures and
pressure after the
extraction stage. Allow the vessels to cool before opening (the
use of a water bath is
recommended for this purpose) and always monitor the
temperature and pressure by re-
connecting the control vessel to the apparatus prior to opening
the vessels
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5.4 During the heating step, some solvent vapors may escape
through the vessel
liner/seal cover. Follow the manufacturer's directions regarding
the vessel assembly and
instrument setup to prevent release of solvent vapors to the
laboratory atmosphere.
5.5 The instrument may contain flammable vapor sensors and
should be operated with
all covers in place and doors closed to ensure proper operation
of the sensors. If so equipped,
follow the manufacturer's directions regarding replacement of
extraction vessel seals when
9. frequent vapor leaks are detected.
5.6 The drying or grinding of samples for PCDDs/PCDFs
generally is not
recommended due to safety concerns regarding worker exposure
to analytes.
6.0 EQUIPMENT AND SUPPLIES
The mention of trade names or commercial products in this
manual is for illustrative
purposes only, and does not constitute an EPA endorsement or
exclusive recommendation for
use. The products and instrument settings cited in SW-846
methods represent those products
and settings used during method development or subsequently
evaluated by the Agency.
Glassware, reagents, supplies, equipment, and settings other
than those listed in this manual
may be employed provided that method performance appropriate
for the intended application
has been demonstrated and documented.
This section does not list common laboratory glassware (e.g.,
beakers and flasks).
6.1 Microwave solvent extraction apparatus
6.1.1 The temperature performance specifications necessitate
that the
microwave extraction system be capable of sensing the
temperature to within ± 2.5 EC and
automatically adjusting the microwave field output power
within 2 sec of sensing.
Temperature sensors should be accurate to ± 2 EC.
Temperature feedback control
10. provides the primary performance mechanism for this method.
6.1.2 Microwave extraction vessels are needed. Vessels are
available that can
accommodate 1-g to 20-g samples. Vessels should be
transparent to microwave energy,
relatively inert to reagents and sample components, and capable
of withstanding the
temperature and pressure specifications (minimum conditions of
200 EC and 200 psi)
necessary to perform this procedure. Follow the manufacturer’s
instructions regarding
cleaning, handling, and sealing the vessels.
6.2 Apparatus for determining percent dry weight
6.2.1 Drying oven
6.2.2 Desiccator
6.2.3 Crucibles -- porcelain or disposable aluminum
6.3 Apparatus for grinding -- capable of reducing particle size
to < 1 mm.
6.4 Analytical balance -- capable to weighing to 0.01 g.
6.5 Apparatus for separating sample from solvent extract
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6.5.1 Glass funnels
11. 6.5.2 Filter paper
6.5.3 Pasteur pipettes
6.6 Vials for collection of extracts -- 40-mL or 60-mL, or other
appropriate volume, pre-
cleaned, open-top screw cap equipped with
polytetrafluoroethylene (PTFE)-lined silicone
septum..
7.0 REAGENTS AND STANDARDS
7.1 Reagent grade chemicals must be used in all tests. Unless
otherwise indicated, it
is intended that all reagents conform to the specifications of the
Committee on Analytical
Reagents of the American Chemical Society, where such
specifications are available. Other
grades may be used, provided it is first ascertained that the
reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the
determination. Reagents should be
stored in glass to prevent the leaching of contaminants from
plastic containers.
7.2 Organic-free reagent water. All references to water in this
method refer to organic-
free reagent water as defined in Chapter One.
7.3 Drying agents
7.3.1 Sodium sulfate (granular anhydrous), Na2SO4
7.3.2 Pelletized diatomaceous earth
7.3.3 The drying agents should be purified by heating at 400 EC
12. for 4 hrs in a
shallow tray, or by extraction with methylene chloride. If
extraction with methylene
chloride is employed, then a reagent blank should be prepared
to demonstrate that the
drying agent is free of interferences.
7.4 Extraction solvents
This method has been validated using a 1:1 mixture of hexane
and acetone from matrices
such as soil, glass-fibers, and sand. Other solvent systems may
have applicability in microwave
extraction, provided that at least one component absorbs
microwave energy.
Samples should be extracted using a solvent system that gives
optimum, reproducible
recovery of the analytes of interest from the sample matrix, at
the concentrations of interest.
The choice of extraction solvent will depend on the analytes of
interest and no single solvent is
universally applicable to all analyte groups. Whatever solvent
system is employed, including
those specifically listed in this method, the analyst must
demonstrate adequate performance for
the analytes of interest, at the levels of interest. At a minimum,
such a demonstration will
encompass the initial demonstration of proficiency described in
Method 3500, using a clean
reference matrix. Method 8000 describes procedures that may
be used to develop performance
criteria for such demonstrations as well as for matrix spike and
laboratory control sample
results.
13. Hexane is a water-immiscible solvent and acetone is a water-
miscible solvent. The
purpose of the water-miscible solvent is to facilitate the
extraction of wet solids by allowing the
mixed solvent to penetrate the layer of water on the surface of
the solid particles. The water-
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immiscible solvent extracts organic compounds with similar
polarities. The polarity of acetone
may also help extract polar analytes in mixed solvent systems.
All solvents should be pesticide quality or equivalent. Solvents
may be degassed prior to
use.
8.0 SAMPLE COLLECTION, PRESERVATION, AND
HANDLING
8.1 See the introductory material to Chapter Four, "Organic
Analytes," Method 3500,
and the specific determinative methods to be employed.
8.2 Solid samples to be extracted by this procedure should be
collected and stored as
any other solid samples containing semivolatile organics.
9.0 QUALITY CONTROL
9.1 Refer to Chapter One for additional guidance on quality
assurance (QA) and
quality control (QC) protocols. When inconsistencies exist
14. between QC guidelines, method-
specific QC criteria take precedence over both technique-
specific criteria and those criteria
given in Chapter One, and technique-specific QC criteria take
precedence over the criteria in
Chapter One. Any effort involving the collection of analytical
data should include development
of a structured and systematic planning document, such as a
Quality Assurance Project Plan
(QAPP) or a Sampling and Analysis Plan (SAP), which
translates project objectives and
specifications into directions for those that will implement the
project and assess the results.
Each laboratory should maintain a formal quality assurance
program. The laboratory should
also maintain records to document the quality of the data
generated. All data sheets and quality
control data should be maintained for reference or inspection.
9.2 Initial demonstration of proficiency
Each laboratory must demonstrate initial proficiency with each
sample preparation and
determinative method combination it utilizes by generating data
of acceptable accuracy and
precision for target analytes in a clean matrix. The laboratory
must also repeat the
demonstration of proficiency whenever new staff members are
trained or significant changes in
instrumentation are made. See Method 8000 for information on
how to accomplish a
demonstration of proficiency.
9.3 Initially, before processing any samples, the analyst should
demonstrate that all
parts of the equipment in contact with the sample and reagents
15. are interference-free. For this
method, this can be accomplished through the analysis of a solid
matrix method blank (e.g.,
clean sand). As a continuing check, each time samples are
extracted, cleaned up, and
analyzed, and when there is a change in reagents, a method
blank should be prepared and
analyzed for the compounds of interest as a safeguard against
chronic laboratory
contamination.
9.4 Any method blanks, matrix spike samples, or replicate
samples should be
subjected to the same analytical procedures (Sec. 11.0) as those
used on actual samples.
9.5 Standard quality assurance practices should be used with
this method as included
in appropriate systematic planning documents and laboratory
SOPs. All instrument operating
conditions should be recorded.
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9.6 Also refer to Method 3500 for extraction and sample
preparation QC procedures
and the determinative methods to be used for determinative QC
procedures.
9.7 When listed in the appropriate determinative method,
surrogate standards should
be added to all samples prior to extraction. For PCDDs/PCDFs,
the labeled internal standards
16. listed in the determinative methods should be added to all
samples prior to extraction. See
Methods 3500, and 8000, and the appropriate determinative
methods for more information.
9.8 As noted earlier, use of any extraction technique, including
microwave extraction,
should be supported by data that demonstrate the performance
of the specific solvent system
and operating conditions for the analytes of interest, at the
levels of interest, in the sample
matrix.
10.0 CALIBRATION AND STANDARDIZATION
There are no calibration or standardization steps directly
associated with this sample
extraction procedure, other than establishing the extraction
conditions in Sec. 11.9.
11.0 PROCEDURE
11.1 Sample preparation
The sample preparation steps vary with the type of sample to be
extracted, as described
below. Where practical, samples should be air-dried and ground
to a fine powder before
extraction. However, where such steps are not practical because
of concerns about loss of the
more volatile analytes or potential contamination of the
laboratory from high concentration
samples, samples may be mixed with a drying agent such as
sodium sulfate or pelletized
diatomaceous earth prior to extraction.
17. WARNING: The drying or grinding of samples for
PCDDs/PCDFs generally is not
recommended, due to safety concerns regarding worker
exposure to these
analytes.
11.1.1 Sediment/soil samples
Decant and discard any water layer on a sediment sample.
Discard any foreign
objects such as sticks, leaves, and rocks. Mix the sample
thoroughly, especially
composited samples. When practical, air dry the sample at
room temperature for 48 hrs in
a glass tray or on hexane-rinsed aluminum foil. Alternatively,
mix the sample with an
equal volume of anhydrous sodium sulfate or pelletized
diatomaceous earth until a free-
flowing powder is obtained.
CAUTION: Dry, finely-ground soil/sediment allows the best
extraction efficiency for
nonvolatile, nonpolar organics, e.g., 4,4'-DDT, PCBs, etc. Air-
drying may not
be appropriate for the analysis of the more volatile
organochlorine pesticides
(e.g., the BHCs) or the more volatile of the semivolatile
organics because of
losses during the drying process. Worker safety may be an
issue with the
drying of soils containing PCDDs/PCDFs as well. Oven-drying
during this
step is not recommended for any analytes.
CAUTION: Drying should always be performed in a hood, to
avoid contamination of the
18. laboratory.
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% dry weight ' g of dry sample
g of sample
x 100
11.1.2 Waste samples
Prepare multiphase waste samples by the phase separation
method in Chapter
Two before extraction. This extraction procedure is for solids
only.
11.1.3 Dry sediment/soil and dry waste samples amenable to
grinding
Grind or otherwise reduce the particle size of the waste so that
it either passes
through a 1-mm sieve or can be extruded through a 1-mm hole.
Disassemble grinder
between samples, according to manufacturer's instructions, and
decontaminate with soap
and water, followed by acetone and hexane rinses. The caution
notes regarding drying in
Sec. 11.1.1 also apply to the grinding process.
11.1.4 Gummy, fibrous, or oily materials not amenable to
grinding
Cut, shred, or otherwise reduce in size these samples to allow
19. mixing and
maximum exposure of the sample surfaces for the extraction.
The analyst may add
anhydrous sodium sulfate, pelletized diatomaceous earth, sand,
or other clean, dry
reagents to the sample to make it more amenable to grinding.
11.2 Grind a sufficient weight of the dried sample from Sec.
11.1 to yield the sample
weight needed for the determinative method (usually 10 - 30 g).
Grind the sample until it
passes through a 10-mesh sieve.
WARNING: Grinding of samples for PCDDs/PCDFs generally
is not recommended, due to
safety concerns with samples containing these analytes.
11.3 Determination of percent dry weight
When sample results are to be calculated on a dry weight basis,
a separate portion of
sample should be weighed at the same time as the portion used
for analytical determination.
CAUTION: The drying oven should be contained in a hood or
vented. Significant laboratory
contamination may result from drying a heavily contaminated
sample.
11.3.1 Immediately after weighing the sample for extraction,
weigh an additional
5-to 10-g aliquot of the sample into a tared crucible. Dry this
aliquot overnight at 105 EC.
Allow to cool in a desiccator before weighing.
11.3.2 Calculate the % dry weight as follows:
20. This oven-dried aliquot is not used for the extraction and should
be appropriately disposed
of once the dry weight is determined.
11.4 Transfer the ground sample to an extraction vessel. The
weight of a specific
sample that a vessel will contain depends on the bulk density of
the sample and the amount of
drying agent (if any) that was added to the sample in order to
make it suitable for extraction.
Analysts should ensure that the sample aliquot extracted is large
enough to provide the
necessary analytical sensitivity.
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11.5 Prepare a method blank using an aliquot of a clean solid
matrix such as quartz
sand of the approximate weight of the samples. If a drying
agent is added to the field samples
being extracted, it must also be added to the method blank, in
order to assess the possible
contribution of the drying agent to the blank results.
11.6 Add the surrogates listed in the determinative method to
each sample and method
blank. Add the surrogates and the matrix spike compounds
appropriate for the project to the
two additional aliquots of the sample selected for spiking. If a
drying agent is added to the field
samples being extracted, it must also be added to the matrix
spike aliquots, in order to assess
21. the effect of the drying agent.
11.7 Add approximately 25 mL of the appropriate solvent
system to the vessel and seal
the vessel as instructed by the manufacturer.
11.8 Place the extraction vessel into the instrument and proceed
with apparatus setup
as instructed by the instrument manufacturer. If recommended
by the manufacturer, include
additional vessels containing water or other materials to the
apparatus in order to ensure that all
samples are exposed to a consistent amount of microwave
energy across extraction batches.
11.9 Recommended extraction conditions
Temperature: 100 - 115 EC
Pressure: 50 - 150 psi
Time at Temperature: 10 - 20 min
Cooling: To room temperature
Filtering/Rinsing: With same solvent system
11.9.1 Optimize the conditions, as needed, according to the
manufacturer's
instructions. In general, the pressure is not a critical parameter,
since it is a result of the
solvent system vapor pressure at the elevated temperature.
11.9.2 Once established, the same procedure should be used for
all samples
extracted for the same type of analysis.
11.10 Begin the extraction according to the instructions
provided by the manufacturer.
22. 11.11 Allow the extracts to cool to room temperature once the
extractions are complete.
After cooling, open the vessels and proceed with filtering and
rinsing, combining all the filtrates.
11.12 The extract is now ready for concentration, cleanup, or
analysis, depending on the
extent of interferants and the determinative method to be
employed. Refer to Method 3600 for
guidance on selecting appropriate cleanup methods. Excess
water present in extracts may be
removed by filtering the extract through a bed of anhydrous
sodium sulfate. When using certain
cleanup and/or determinative methods, a solvent exchange may
be necessary prior to cleanup
and/or analysis.
12.0 DATA ANALYSIS AND CALCULATIONS
There are no calculations explicitly associated with this
extraction procedure. See the
appropriate determinative method for the calculation of final
sample results.
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13.0 METHOD PERFORMANCE
13.1 Performance data and related information are provided in
SW-846 methods only as
examples and guidance. The data do not represent required
performance criteria for users of
the methods. Instead, performance criteria should be
23. developed on a project-specific basis,
and the laboratory should establish in-house QC performance
criteria for the application of this
method. These performance data are not intended to be and
must not be used as absolute QC
acceptance criteria for purposes of laboratory accreditation.
13.2 Reference 4 presents a large body of information and
specific data on a number of
analytes. It provides the basis for a major portion of the
performance work associated with this
procedure. References 3 and 5 are reports of similar, more
specific, studies. References 6 to 8
deal specifically with phenols. All of the method validation
studies described in this method
were performed using microwave apparatus operating at 2450
MHz.
13.3 Chlorinated pesticides
Single-laboratory accuracy data were obtained for chlorinated
pesticides extracted from
soil, glass-fiber, and sand matrices. Concentrations of each
target analyte ranged between 500
and 1,000 µg/kg. Four real-world split samples contaminated
with pesticides and creosotes
were also used (obtained from US EPA ERT, Edison, NJ). The
latter were extracted by an
independent laboratory using standard Soxhlet procedures and
results compared to those
obtained with this procedure. All samples were extracted using
1:1 hexane:acetone. Extracts
were analyzed by the appropriate determinative method.
Method blanks and five spiked
replicates were included. Work was also carried out to assess
the level of degradation of
24. thermally labile pesticides and it was found that no significant
degradation takes place under the
procedure described in this method. The data are reported in
detail in Reference 4. Data
summary tables are included in Method 8081, for guidance
purposes only.
13.4 Semivolatile organics
Single-laboratory accuracy data were obtained for semivolatile
organics extracted from
soil, glass-fiber, and sand samples. Concentrations of each
target analyte were about 500
µg/kg. All samples were extracted using 1:1 hexane:acetone.
Extracts were analyzed by the
appropriate determinative method. Method blanks and five
spike replicates were included. The
data are reported in detail in Reference 4. Data summary tables
are included in Method 8270,
for guidance purposes only.
13.5 PAHs
Single-laboratory accuracy data were obtained for PAHs
extracted from five reference
materials comprising marine sediments (HS-3, HS-4, and HS-5,
all from the National Research
Council of Canada), lake sediments (SRM-1491, from the
National Institute of Science and
Technology), and a soil contaminated with creosote (SRS103-
100, from Fisher Scientific,
Fairlawn, NJ). Work was also conducted with soil, glass-fiber,
and sand samples spiked
between 100 and 2,000 µg/kg. All samples were extracted using
1:1 hexane:acetone. One
real-world split sample contaminated with creosote and
25. pesticides was also used (obtained from
US EPA ERT, Edison, NJ). The latter was extracted by one
laboratory using standard Soxhlet
procedures and results compared to those obtained with this
procedure. Extracts were
analyzed by the appropriate determinative method. Method
blanks, spikes and five spiked
replicates were included. The data are reported in detail in
Reference 4. Data summary tables
are included in Method 8270, for guidance purposes only.
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13.6 PCBs
Single-laboratory accuracy data were obtained for PCBs
extracted from three reference
materials (EC-1, EC-2, EC-3 -- from Environment Canada).
Work was also conducted with soil,
glass-fiber, and sand samples spiked between 200 and 10,000
µg/kg (total PCBs). All samples
were extracted using 1:1 hexane:acetone. Extracts were
analyzed by the appropriate
determinative method. Method blanks, spikes and spike
duplicates were included for the low
concentration spikes; matrix spikes were included for all other
concentrations. The data are
reported in detail in Reference 4. Data summary tables are
included in Method 8082, for
guidance purposes only.
13.7 Chlorinated herbicides (phenoxyacid herbicides)
26. Multi-laboratory accuracy data were obtained for chlorinated
herbicides extracted from a
certified spiked material (obtained from ERA, Arvada, CO).
This soil was spiked by ERA at 100
µg/kg. All samples were extracted using 1:1 hexane:acetone.
Extracts were analyzed by
Method 8151. Method blanks and three replicates from five
laboratories were included. Data
summary tables are included in Method 8151, for guidance
purposes only.
13.8 Phenols
Single-laboratory accuracy data were obtained for phenols
extracted from a number of
spiked soils and real-world split soils. Concentrations ranged
between 200 and 10,000 µg/kg.
All samples were extracted using 1:1 hexane:acetone. Extracts
were analyzed by the
appropriate determinative method. The data are reported in
detail in References 4 to 8. Data
summary tables are included in Method 8041, for guidance
purposes only.
Multi-laboratory accuracy data were obtained for phenols
extracted from a certified spiked
material (obtained from ERA, Arvada, CO). This soil was
spiked by ERA at 250 µg/kg. All
samples were extracted using 1:1 hexane:acetone. Extracts
were analyzed by Method 8041.
Method blanks and three replicates from five laboratories were
included. Data summary tables
are included in Method 8041, for guidance purposes only.
13.9 Organophosphorus pesticides and chlorinated herbicides
27. Multi-laboratory performance data were obtained for
organophosphorus pesticides
extracted from a certified spiked material (obtained from ERA,
Arvada, CO). This soil was
spiked by ERA at 250 µg/kg. All samples were extracted using
1:1 hexane:acetone. Extracts
were analyzed by Method 8141. Method blanks and three
replicates from five laboratories were
included. Data summary tables are included in Method 8141,
for guidance purposes only.
13.10 Dioxins and furans
Single-laboratory accuracy data were obtained for dioxins and
furans extracted from two
soil reference materials (DX-1 from Environment Canada and
SRM-1944 from NIST) containing
the analytes of interest at concentrations between 10 and 6,000
ng/kg. All samples were
extracted using 1:1 hexane:acetone. Extracts were analyzed by
the appropriate determinative
method. Method blanks, spikes and spike duplicates were
included for the low concentration
spikes; matrix spikes were included for all other concentrations.
The data are reported in detail
in References 9 and 10.
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14.0 POLLUTION PREVENTION
14.1 Pollution prevention encompasses any technique that
reduces or eliminates the
28. quantity and/or toxicity of waste at the point of generation.
Numerous opportunities for pollution
prevention exist in laboratory operation. The EPA has
established a preferred hierarchy of
environmental management techniques that places pollution
prevention as the management
option of first choice. Whenever feasible, laboratory personnel
should use pollution prevention
techniques to address their waste generation. When wastes
cannot be feasibly reduced at the
source, the Agency recommends recycling as the next best
option.
14.2 For information about pollution prevention that may be
applicable to laboratories
and research institutions consult Less is Better: Laboratory
Chemical Management for Waste
Reduction available from the American Chemical Society's
Department of Government
Relations and Science Policy, 1155 16th St., NW Washington,
D.C. 20036, http://www.acs.org.
14.3 Extraction of organic compounds using microwave
extraction conforms with EPA's
pollution prevention goals. The volumes of solvent employed
are generally smaller than with
other extraction procedures.
15.0 WASTE MANAGEMENT
The Environmental Protection Agency requires that laboratory
waste management
practices be conducted consistent with all applicable rules and
regulations. The Agency urges
laboratories to protect the air, water, and land by minimizing
and controlling all releases from
29. hoods and bench operations, complying with the letter and spirit
of any sewer discharge permits
and regulations, and by complying with all solid and hazardous
waste regulations, particularly
the hazardous waste identification rules and land disposal
restrictions. For further information
on waste management, consult The Waste Management Manual
for Laboratory Personnel
available from the American Chemical Society at the address
listed in Sec. 14.2.
16.0 REFERENCES
1 K. Ganzler, A. Salgo and K. Valko, ?Microwave Extraction: A
Novel Sample Preparation
Method for Chromatography,” J. Chrom., 371, 299-306 (1986).
2. J. R. J. Paré, J. M. R. Bélanger, and S. S. Stafford,
?Microwave-Assisted Process
(MAPTM): A New Tool for the Analytical Laboratory,” Tr.
Anal. Chem. 13, 176-184 (1994).
3. V. Lopez-Avila, R. Young, and W. F. Beckert, ?Microwave-
Assisted Extraction of Organic
Compounds from Standard Reference Soils and Sediments,”
Anal. Chem. 66, 1097-1106
(1994).
4. K. Li, J. M. R. Bélanger, M. P. Llompart, R. D. Turpin, R.
Singhvi, and J. R. J. Paré,
?Evaluation of Rapid Solid Sample Extraction Using the
Microwave-assisted Process
(MAPTM) under Closed-vessel Conditions,” Spectros. Int. J. 13
(1), 1-14 (1997).
5. R. McMillin, L. C. Miner, and L. Hurst, ?Abbreviated
30. Microwave Extraction of Pesticides
and PCBs in Soil,” Spectros. Int. J. 13 (1), 41-50 (1997).
6. M. P. Llompart, R. A. Lorenzo, R. Cela, and J. R. J. Paré,
?Optimization of a Microwave-
assisted Extraction Method for Phenol and Methylphenol
Isomers in Soil Samples Using a
Central Composite Design,” Analyst, 122, 133-137 (1997).
3546-13 Revision 0
February 2007
7. M. P. Llompart, R. A. Lorenzo, R. Cela, J. R. J. Paré, J. M.
R. Bélanger, and K. Li, ?Phenol
and Methylphenol Isomers Determination in Soils by In-situ
Microwave-assisted Extraction
and Derivatisation,” J. Chromatogr. A 757, 153-164 (1997).
8. M. P. Llompart, R. A. Lorenzo, R. Cela, K. Li, J. M. R.
Bélanger, and J. R. J. Paré,
?Evaluation of Supercritical Fluid Extraction, Microwave-
assisted Extraction and Sonication
in the Determination of Some Phenolic Compounds from
Various Soil Matrices,” J.
Chromatogr. A, 774, 243-251 (1997).
9. C. Chiu, G. Poole, Y. Shu, R. Thomas, and R. Turle,
?Microwave vs. Soxhlet for the
Extraction of Dioxins and Furans from Solid Samples,”
Organohalogen Compounds 27,
333-338 (1996).
10. C. Chiu, G. Poole, M. Tardif, W. Miles, and R. Turle,
?Determination of PCDDs/PCDFs
31. Using Microwave-Assisted Solvent Extraction,” Organohalogen
Compounds 31, 175-180
(1997).
11. J. R. J. Paré, M. Sigouin, and J. Lapointe, U. S. Patent
5,002,784 (1991).
12. H. M. Kingston and S. J. Haswell, Eds., Microwave
Enhanced Chemistry: Fundamentals,
Sample Preparation and Applications, American Chemical
Society, Washington, DC,
xxviii+772 pps, 1997.
13. F. I. Onuska and T. A. Terry, ?Extraction of Pesticides from
Sediments Using a Microwave
Technique,” Chromatographia, 36, 191-194 (1993).
17.0 TABLES, DIAGRAMS, FLOW CHARTS, AND
VALIDATION DATA
There are no tables or figures associated with this method.