7 CFR 94.103 - Analytical methods.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for egg...

7 CFR 94.103 - Analytical methods.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 3 2011-01-01 2011-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for egg...

7 CFR 94.103 - Analytical methods.

Code of Federal Regulations, 2013 CFR

2013-01-01

... 7 Agriculture 3 2013-01-01 2013-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for egg...

7 CFR 94.103 - Analytical methods.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 3 2012-01-01 2012-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for egg...

7 CFR 94.4 - Analytical methods.

Code of Federal Regulations, 2014 CFR

2014-01-01

... 7 Agriculture 3 2014-01-01 2014-01-01 false Analytical methods. 94.4 Section 94.4 Agriculture... POULTRY AND EGG PRODUCTS Mandatory Analyses of Egg Products § 94.4 Analytical methods. The majority of analytical methods used by the USDA laboratories to perform mandatory analyses for egg products are listed as...

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS § 136.6 Method... person or laboratory using a test procedure (analytical method) in this part. (2) Chemistry of the method means the reagents and reactions used in a test procedure that allow determination of the analyte(s) of...

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2011 CFR

2011-07-01

... PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS § 136.6 Method... person or laboratory using a test procedure (analytical method) in this Part. (2) Chemistry of the method means the reagents and reactions used in a test procedure that allow determination of the analyte(s) of...

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2012 CFR

2012-07-01

... PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS § 136.6 Method... person or laboratory using a test procedure (analytical method) in this part. (2) Chemistry of the method means the reagents and reactions used in a test procedure that allow determination of the analyte(s) of...

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2014 CFR

2014-07-01

... PROGRAMS (CONTINUED) GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS OF POLLUTANTS § 136.6 Method... person or laboratory using a test procedure (analytical method) in this part. (2) Chemistry of the method means the reagents and reactions used in a test procedure that allow determination of the analyte(s) of...

DOE Office of Scientific and Technical Information (OSTI.GOV)

Green, D.W.; Heinrich, R.R.; Jensen, K.J.

The Analytical Chemistry Laboratory is a full-cost-recovery service center, with the primary mission of providing a broad range of technical support services to the scientific and engineering programs at ANL. In addition, ACL conducts a research program in analytical chemistry, works on instrumental and methods development, and provides analytical services for governmental, educational, and industrial organizations. The ACL handles a wide range of analytical problems, from routine standard analyses to unique problems that require significant development of methods and techniques. The purpose of this report is to summarize the technical and administrative activities of the Analytical Chemistry Laboratory (ACL) atmore » Argonne National Laboratory (ANL) for Fiscal Year 1985 (October 1984 through September 1985). This is the second annual report for the ACL. 4 figs., 1 tab.« less

MODULAR ANALYTICS: A New Approach to Automation in the Clinical Laboratory.

PubMed

Horowitz, Gary L; Zaman, Zahur; Blanckaert, Norbert J C; Chan, Daniel W; Dubois, Jeffrey A; Golaz, Olivier; Mensi, Noury; Keller, Franz; Stolz, Herbert; Klingler, Karl; Marocchi, Alessandro; Prencipe, Lorenzo; McLawhon, Ronald W; Nilsen, Olaug L; Oellerich, Michael; Luthe, Hilmar; Orsonneau, Jean-Luc; Richeux, Gérard; Recio, Fernando; Roldan, Esther; Rymo, Lars; Wicktorsson, Anne-Charlotte; Welch, Shirley L; Wieland, Heinrich; Grawitz, Andrea Busse; Mitsumaki, Hiroshi; McGovern, Margaret; Ng, Katherine; Stockmann, Wolfgang

2005-01-01

MODULAR ANALYTICS (Roche Diagnostics) (MODULAR ANALYTICS, Elecsys and Cobas Integra are trademarks of a member of the Roche Group) represents a new approach to automation for the clinical chemistry laboratory. It consists of a control unit, a core unit with a bidirectional multitrack rack transportation system, and three distinct kinds of analytical modules: an ISE module, a P800 module (44 photometric tests, throughput of up to 800 tests/h), and a D2400 module (16 photometric tests, throughput up to 2400 tests/h). MODULAR ANALYTICS allows customised configurations for various laboratory workloads. The performance and practicability of MODULAR ANALYTICS were evaluated in an international multicentre study at 16 sites. Studies included precision, accuracy, analytical range, carry-over, and workflow assessment. More than 700 000 results were obtained during the course of the study. Median between-day CVs were typically less than 3% for clinical chemistries and less than 6% for homogeneous immunoassays. Median recoveries for nearly all standardised reference materials were within 5% of assigned values. Method comparisons versus current existing routine instrumentation were clinically acceptable in all cases. During the workflow studies, the work from three to four single workstations was transferred to MODULAR ANALYTICS, which offered over 100 possible methods, with reduction in sample splitting, handling errors, and turnaround time. Typical sample processing time on MODULAR ANALYTICS was less than 30 minutes, an improvement from the current laboratory systems. By combining multiple analytic units in flexible ways, MODULAR ANALYTICS met diverse laboratory needs and offered improvement in workflow over current laboratory situations. It increased overall efficiency while maintaining (or improving) quality.

MODULAR ANALYTICS: A New Approach to Automation in the Clinical Laboratory

PubMed Central

Zaman, Zahur; Blanckaert, Norbert J. C.; Chan, Daniel W.; Dubois, Jeffrey A.; Golaz, Olivier; Mensi, Noury; Keller, Franz; Stolz, Herbert; Klingler, Karl; Marocchi, Alessandro; Prencipe, Lorenzo; McLawhon, Ronald W.; Nilsen, Olaug L.; Oellerich, Michael; Luthe, Hilmar; Orsonneau, Jean-Luc; Richeux, Gérard; Recio, Fernando; Roldan, Esther; Rymo, Lars; Wicktorsson, Anne-Charlotte; Welch, Shirley L.; Wieland, Heinrich; Grawitz, Andrea Busse; Mitsumaki, Hiroshi; McGovern, Margaret; Ng, Katherine; Stockmann, Wolfgang

2005-01-01

MODULAR ANALYTICS (Roche Diagnostics) (MODULAR ANALYTICS, Elecsys and Cobas Integra are trademarks of a member of the Roche Group) represents a new approach to automation for the clinical chemistry laboratory. It consists of a control unit, a core unit with a bidirectional multitrack rack transportation system, and three distinct kinds of analytical modules: an ISE module, a P800 module (44 photometric tests, throughput of up to 800 tests/h), and a D2400 module (16 photometric tests, throughput up to 2400 tests/h). MODULAR ANALYTICS allows customised configurations for various laboratory workloads. The performance and practicability of MODULAR ANALYTICS were evaluated in an international multicentre study at 16 sites. Studies included precision, accuracy, analytical range, carry-over, and workflow assessment. More than 700 000 results were obtained during the course of the study. Median between-day CVs were typically less than 3% for clinical chemistries and less than 6% for homogeneous immunoassays. Median recoveries for nearly all standardised reference materials were within 5% of assigned values. Method comparisons versus current existing routine instrumentation were clinically acceptable in all cases. During the workflow studies, the work from three to four single workstations was transferred to MODULAR ANALYTICS, which offered over 100 possible methods, with reduction in sample splitting, handling errors, and turnaround time. Typical sample processing time on MODULAR ANALYTICS was less than 30 minutes, an improvement from the current laboratory systems. By combining multiple analytic units in flexible ways, MODULAR ANALYTICS met diverse laboratory needs and offered improvement in workflow over current laboratory situations. It increased overall efficiency while maintaining (or improving) quality. PMID:18924721

International Council for Standardization in Haematology (ICSH) Recommendations for Laboratory Measurement of Direct Oral Anticoagulants.

PubMed

Gosselin, Robert C; Adcock, Dorothy M; Bates, Shannon M; Douxfils, Jonathan; Favaloro, Emmanuel J; Gouin-Thibault, Isabelle; Guillermo, Cecilia; Kawai, Yohko; Lindhoff-Last, Edelgard; Kitchen, Steve

2018-03-01

This guidance document was prepared on behalf of the International Council for Standardization in Haematology (ICSH) for providing haemostasis-related guidance documents for clinical laboratories. This inaugural coagulation ICSH document was developed by an ad hoc committee, comprised of international clinical and laboratory direct acting oral anticoagulant (DOAC) experts. The committee developed consensus recommendations for laboratory measurement of DOACs (dabigatran, rivaroxaban, apixaban and edoxaban), which would be germane for laboratories assessing DOAC anticoagulation. This guidance document addresses all phases of laboratory DOAC measurements, including pre-analytical (e.g. preferred time sample collection, preferred sample type, sample stability), analytical (gold standard method, screening and quantifying methods) and post analytical (e.g. reporting units, quality assurance). The committee addressed the use and limitations of screening tests such as prothrombin time, activated partial thromboplastin time as well as viscoelastic measurements of clotting blood and point of care methods. Additionally, the committee provided recommendations for the proper validation or verification of performance of laboratory assays prior to implementation for clinical use, and external quality assurance to provide continuous assessment of testing and reporting method. Schattauer GmbH Stuttgart.

Analysis of Ethanolamines: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS888

DOE Office of Scientific and Technical Information (OSTI.GOV)

Owens, J; Vu, A; Koester, C

The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method titled 'Analysis of Diethanolamine, Triethanolamine, n-Methyldiethanolamine, and n-Ethyldiethanolamine in Water by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS): EPA Method MS888'. This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to validate and verify the analytical procedures described in 'EPA Method MS888' for analysis of themore » listed ethanolamines in aqueous samples. The gathered data from this validation study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of 'EPA Method MS888' can be determined.« less

40 CFR 136.6 - Method modifications and analytical requirements.

Code of Federal Regulations, 2010 CFR

2010-07-01

... person or laboratory using a test procedure (analytical method) in this Part. (2) Chemistry of the method... (analytical method) provided that the chemistry of the method or the determinative technique is not changed... prevent efficient recovery of organic pollutants and prevent the method from meeting QC requirements, the...

DOE Office of Scientific and Technical Information (OSTI.GOV)

Campbell, J.A.; Clauss, S.A.; Grant, K.E.

The objectives of this task are to develop and document extraction and analysis methods for organics in waste tanks, and to extend these methods to the analysis of actual core samples to support the Waste Tank organic Safety Program. This report documents progress at Pacific Northwest Laboratory (a) during FY 1994 on methods development, the analysis of waste from Tank 241-C-103 (Tank C-103) and T-111, and the transfer of documented, developed analytical methods to personnel in the Analytical Chemistry Laboratory (ACL) and 222-S laboratory. This report is intended as an annual report, not a completed work.

Analysis of Carbamate Pesticides: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS666

DOE Office of Scientific and Technical Information (OSTI.GOV)

Owens, J; Koester, C

The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method for analysis of aldicarb, bromadiolone, carbofuran, oxamyl, and methomyl in water by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), titled Method EPA MS666. This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to validate and verify the analytical procedures described in MS666 for analysis of carbamatemore » pesticides in aqueous samples. The gathered data from this validation study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of Method EPA MS666 can be determined.« less

Analysis of Thiodiglycol: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS777

DOE Office of Scientific and Technical Information (OSTI.GOV)

Owens, J; Koester, C

The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method for the analysis of thiodiglycol, the breakdown product of the sulfur mustard HD, in water by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), titled Method EPA MS777 (hereafter referred to as EPA CRL SOP MS777). This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to verifymore » the analytical procedures described in MS777 for analysis of thiodiglycol in aqueous samples. The gathered data from this study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of Method EPA MS777 can be determined.« less

Integrating a Smartphone and Molecular Modeling for Determining the Binding Constant and Stoichiometry Ratio of the Iron(II)-Phenanthroline Complex: An Activity for Analytical and Physical Chemistry Laboratories

ERIC Educational Resources Information Center

de Morais, Camilo de L. M.; Silva, Se´rgio R. B.; Vieira, Davi S.; Lima, Ka´ssio M. G.

2016-01-01

The binding constant and stoichiometry ratio for the formation of iron(II)-(1,10-phenanthroline) or iron(II)-o-phenanthroline complexes has been determined by a combination of a low-cost analytical method using a smartphone and a molecular modeling method as a laboratory experiment designed for analytical and physical chemistry courses. Intensity…

Teaching Analytical Method Transfer through Developing and Validating Then Transferring Dissolution Testing Methods for Pharmaceuticals

ERIC Educational Resources Information Center

Kimaru, Irene; Koether, Marina; Chichester, Kimberly; Eaton, Lafayette

2017-01-01

Analytical method transfer (AMT) and dissolution testing are important topics required in industry that should be taught in analytical chemistry courses. Undergraduate students in senior level analytical chemistry laboratory courses at Kennesaw State University (KSU) and St. John Fisher College (SJFC) participated in development, validation, and…

Organic Analytical Service within the Superfund Contract Laboratory Program

EPA Pesticide Factsheets

This page contains information about the SOM02.4 statement of work for the analysis of organic compounds at hazardous waste sites. The SOW contains the analytical method and contractual requirements for laboratories.

Inorganic Analytical Service within the Superfund Contract Laboratory Program

EPA Pesticide Factsheets

This page contains information about the ISM02.4 statement of work for the analysis of metals and cyanide at hazardous waste sites. The SOW contains the analytical method and contractual requirements for laboratories.

[Quality Management and Quality Specifications of Laboratory Tests in Clinical Studies--Challenges in Pre-Analytical Processes in Clinical Laboratories].

PubMed

Ishibashi, Midori

2015-01-01

The cost, speed, and quality are the three important factors recently indicated by the Ministry of Health, Labour and Welfare (MHLW) for the purpose of accelerating clinical studies. Based on this background, the importance of laboratory tests is increasing, especially in the evaluation of clinical study participants' entry and safety, and drug efficacy. To assure the quality of laboratory tests, providing high-quality laboratory tests is mandatory. For providing adequate quality assurance in laboratory tests, quality control in the three fields of pre-analytical, analytical, and post-analytical processes is extremely important. There are, however, no detailed written requirements concerning specimen collection, handling, preparation, storage, and shipping. Most laboratory tests for clinical studies are performed onsite in a local laboratory; however, a part of laboratory tests is done in offsite central laboratories after specimen shipping. As factors affecting laboratory tests, individual and inter-individual variations are well-known. Besides these factors, standardizing the factors of specimen collection, handling, preparation, storage, and shipping, may improve and maintain the high quality of clinical studies in general. Furthermore, the analytical method, units, and reference interval are also important factors. It is concluded that, to overcome the problems derived from pre-analytical processes, it is necessary to standardize specimen handling in a broad sense.

Introduction to Validation of Analytical Methods: Potentiometric Determination of CO[subscript 2

ERIC Educational Resources Information Center

Hipólito-Nájera, A. Ricardo; Moya-Hernandez, M. Rosario; Gomez-Balderas, Rodolfo; Rojas-Hernandez, Alberto; Romero-Romo, Mario

2017-01-01

Validation of analytical methods is a fundamental subject for chemical analysts working in chemical industries. These methods are also relevant for pharmaceutical enterprises, biotechnology firms, analytical service laboratories, government departments, and regulatory agencies. Therefore, for undergraduate students enrolled in majors in the field…

Molecular detection of Borrelia burgdorferi sensu lato – An analytical comparison of real-time PCR protocols from five different Scandinavian laboratories

PubMed Central

Faller, Maximilian; Wilhelmsson, Peter; Kjelland, Vivian; Andreassen, Åshild; Dargis, Rimtas; Quarsten, Hanne; Dessau, Ram; Fingerle, Volker; Margos, Gabriele; Noraas, Sølvi; Ornstein, Katharina; Petersson, Ann-Cathrine; Matussek, Andreas; Lindgren, Per-Eric; Henningsson, Anna J.

2017-01-01

Introduction Lyme borreliosis (LB) is the most common tick transmitted disease in Europe. The diagnosis of LB today is based on the patient´s medical history, clinical presentation and laboratory findings. The laboratory diagnostics are mainly based on antibody detection, but in certain conditions molecular detection by polymerase chain reaction (PCR) may serve as a complement. Aim The purpose of this study was to evaluate the analytical sensitivity, analytical specificity and concordance of eight different real-time PCR methods at five laboratories in Sweden, Norway and Denmark. Method Each participating laboratory was asked to analyse three different sets of samples (reference panels; all blinded) i) cDNA extracted and transcribed from water spiked with cultured Borrelia strains, ii) cerebrospinal fluid spiked with cultured Borrelia strains, and iii) DNA dilution series extracted from cultured Borrelia and relapsing fever strains. The results and the method descriptions of each laboratory were systematically evaluated. Results and conclusions The analytical sensitivities and the concordance between the eight protocols were in general high. The concordance was especially high between the protocols using 16S rRNA as the target gene, however, this concordance was mainly related to cDNA as the type of template. When comparing cDNA and DNA as the type of template the analytical sensitivity was in general higher for the protocols using DNA as template regardless of the use of target gene. The analytical specificity for all eight protocols was high. However, some protocols were not able to detect Borrelia spielmanii, Borrelia lusitaniae or Borrelia japonica. PMID:28937997

Analysis of Phosphonic Acids: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS999

DOE Office of Scientific and Technical Information (OSTI.GOV)

Owens, J; Vu, A; Koester, C

The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method titled Analysis of Diisopropyl Methylphosphonate, Ethyl Hydrogen Dimethylamidophosphate, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid, and Pinacolyl Methylphosphonic Acid in Water by Multiple Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry: EPA Version MS999. This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to validate and verify the analytical procedures describedmore » in EPA Method MS999 for analysis of the listed phosphonic acids and surrogates in aqueous samples. The gathered data from this validation study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of EPA Method MS999 can be determined.« less

Basic Information for EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM)

EPA Pesticide Factsheets

Contains basic information on the role and origins of the Selected Analytical Methods including the formation of the Homeland Security Laboratory Capacity Work Group and the Environmental Evaluation Analytical Process Roadmap for Homeland Security Events

External Standards or Standard Addition? Selecting and Validating a Method of Standardization

NASA Astrophysics Data System (ADS)

Harvey, David T.

2002-05-01

A common feature of many problem-based laboratories in analytical chemistry is a lengthy independent project involving the analysis of "real-world" samples. Students research the literature, adapting and developing a method suitable for their analyte, sample matrix, and problem scenario. Because these projects encompass the complete analytical process, students must consider issues such as obtaining a representative sample, selecting a method of analysis, developing a suitable standardization, validating results, and implementing appropriate quality assessment/quality control practices. Most textbooks and monographs suitable for an undergraduate course in analytical chemistry, however, provide only limited coverage of these important topics. The need for short laboratory experiments emphasizing important facets of method development, such as selecting a method of standardization, is evident. The experiment reported here, which is suitable for an introductory course in analytical chemistry, illustrates the importance of matrix effects when selecting a method of standardization. Students also learn how a spike recovery is used to validate an analytical method, and obtain a practical experience in the difference between performing an external standardization and a standard addition.

Methods for geochemical analysis

USGS Publications Warehouse

Baedecker, Philip A.

1987-01-01

The laboratories for analytical chemistry within the Geologic Division of the U.S. Geological Survey are administered by the Office of Mineral Resources. The laboratory analysts provide analytical support to those programs of the Geologic Division that require chemical information and conduct basic research in analytical and geochemical areas vital to the furtherance of Division program goals. Laboratories for research and geochemical analysis are maintained at the three major centers in Reston, Virginia, Denver, Colorado, and Menlo Park, California. The Division has an expertise in a broad spectrum of analytical techniques, and the analytical research is designed to advance the state of the art of existing techniques and to develop new methods of analysis in response to special problems in geochemical analysis. The geochemical research and analytical results are applied to the solution of fundamental geochemical problems relating to the origin of mineral deposits and fossil fuels, as well as to studies relating to the distribution of elements in varied geologic systems, the mechanisms by which they are transported, and their impact on the environment.

Laboratory Analytical Procedures | Bioenergy | NREL

Science.gov Websites

analytical procedures (LAPs) to provide validated methods for biofuels and pyrolysis bio-oils research . Biomass Compositional Analysis These lab procedures provide tested and accepted methods for performing

Development of a reference material for routine performance monitoring of methods measuring polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans and dioxin-like polychlorinated biphenyls.

PubMed

Selliah, S S; Cussion, S; MacPherson, K A; Reiner, E J; Toner, D

2001-06-01

Matrix-matched environmental certified reference materials (CRMs) are one of the most useful tools to validate analytical methods, assess analytical laboratory performance and to assist in the resolution of data conflicts between laboratories. This paper describes the development of a lake sediment as a CRM for polychorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and dioxin-like polychlorinated biphenyls (DLPCBs). The presence of DLPCBs in the environment is of increased concern and analytical methods are being developed internationally for monitoring DLPCBs in the environment. This paper also reports the results of an international interlaboratory study involving thirty-five laboratories from seventeen countries, conducted to characterize and validate levels of a sediment reference material for PCDDs, PCDFs and DLPCBs.

Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts.

PubMed

Hollands, Wendy J; Voorspoels, Stefan; Jacobs, Griet; Aaby, Kjersti; Meisland, Ane; Garcia-Villalba, Rocio; Tomas-Barberan, Francisco; Piskula, Mariusz K; Mawson, Deborah; Vovk, Irena; Needs, Paul W; Kroon, Paul A

2017-04-28

There is a lack of data for individual oligomeric procyanidins in apples and apple extracts. Our aim was to develop, validate and evaluate an analytical method for the separation, identification and quantification of monomeric and oligomeric flavanols in apple extracts. To achieve this, we prepared two types of flavanol extracts from freeze-dried apples; one was an epicatechin-rich extract containing ∼30% (w/w) monomeric (-)-epicatechin which also contained oligomeric procyanidins (Extract A), the second was an oligomeric procyanidin-rich extract depleted of epicatechin (Extract B). The parameters considered for method optimisation were HPLC columns and conditions, sample heating, mass of extract and dilution volumes. The performance characteristics considered for method validation included standard linearity, method sensitivity, precision and trueness. Eight laboratories participated in the method evaluation. Chromatographic separation of the analytes was best achieved utilizing a Hilic column with a binary mobile phase consisting of acidic acetonitrile and acidic aqueous methanol. The final method showed linearity for epicatechin in the range 5-100μg/mL with a correlation co-efficient >0.999. Intra-day and inter-day precision of the analytes ranged from 2 to 6% and 2 to 13% respectively. Up to dp3, trueness of the method was >95% but decreased with increasing dp. Within laboratory precision showed RSD values <5 and 10% for monomers and oligomers, respectively. Between laboratory precision was 4 and 15% (Extract A) and 7 and 30% (Extract B) for monomers and oligomers, respectively. An analytical method for the separation, identification and quantification of procyanidins in an apple extract was developed, validated and assessed. The results of the inter-laboratory evaluation indicate that the method is reliable and reproducible. Copyright © 2017. Published by Elsevier B.V.

SRC-I demonstration plant analytical laboratory methods manual. Final technical report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Klusaritz, M.L.; Tewari, K.C.; Tiedge, W.F.

1983-03-01

This manual is a compilation of analytical procedures required for operation of a Solvent-Refined Coal (SRC-I) demonstration or commercial plant. Each method reproduced in full includes a detailed procedure, a list of equipment and reagents, safety precautions, and, where possible, a precision statement. Procedures for the laboratory's environmental and industrial hygiene modules are not included. Required American Society for Testing and Materials (ASTM) methods are cited, and ICRC's suggested modifications to these methods for handling coal-derived products are provided.

EPA Contract Laboratory Program Statement of Work for Inorganic Superfund Methods Multi-Media, Multi-Concentration ISM02.3

EPA Pesticide Factsheets

This document contains analytical methods for the analysis of metals and cyanide in environmental samples. It also contains contractual requirements for laboratories participating in Superfund's Contract Laboratory Program.

EPA Contract Laboratory Program Statement of Work for Inorganic Superfund Methods Multi-Media, Multi-Concentration ISM02.4

EPA Pesticide Factsheets

This document contains analytical methods for the analysis of metals and cyanide in environmental samples. It also contains contractual requirements for laboratories participating in Superfund's Contract Laboratory Program.

HSRP and HSRP Partner Analytical Methods and Protocols

EPA Pesticide Factsheets

HSRP has worked with various partners to develop and test analytical methods and protocols for use by laboratories charged with analyzing environmental and/or buildling material samples following contamination incident.

Analytical Chemistry Laboratory Progress Report for FY 1994

DOE Office of Scientific and Technical Information (OSTI.GOV)

Green, D.W.; Boparai, A.S.; Bowers, D.L.

The purpose of this report is to summarize the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for Fiscal Year (FY) 1994 (October 1993 through September 1994). This annual report is the eleventh for the ACL and describes continuing effort on projects, work on new projects, and contributions of the ACL staff to various programs at ANL. The Analytical Chemistry Laboratory is a full-cost-recovery service center, with the primary mission of providing a broad range of analytical chemistry support services to the scientific and engineering programs at ANL. The ACL also has a research program inmore » analytical chemistry, conducts instrumental and methods development, and provides analytical services for governmental, educational, and industrial organizations. The ACL handles a wide range of analytical problems. Some routine or standard analyses are done, but it is common for the Argonne programs to generate unique problems that require significant development of methods and adaption of techniques to obtain useful analytical data. The ACL has four technical groups -- Chemical Analysis, Instrumental Analysis, Organic Analysis, and Environmental Analysis -- which together include about 45 technical staff members. Talents and interests of staff members cross the group lines, as do many projects within the ACL. The Chemical Analysis Group uses wet- chemical and instrumental methods for elemental, compositional, and isotopic determinations in solid, liquid, and gaseous samples and provides specialized analytical services. Major instruments in this group include an ion chromatograph (IC), an inductively coupled plasma/atomic emission spectrometer (ICP/AES), spectrophotometers, mass spectrometers (including gas-analysis and thermal-ionization mass spectrometers), emission spectrographs, autotitrators, sulfur and carbon determinators, and a kinetic phosphorescence uranium analyzer.« less

Analytical difficulties facing today's regulatory laboratories: issues in method validation.

PubMed

MacNeil, James D

2012-08-01

The challenges facing analytical laboratories today are not unlike those faced in the past, although both the degree of complexity and the rate of change have increased. Challenges such as development and maintenance of expertise, maintenance and up-dating of equipment, and the introduction of new test methods have always been familiar themes for analytical laboratories, but international guidelines for laboratories involved in the import and export testing of food require management of such changes in a context which includes quality assurance, accreditation, and method validation considerations. Decisions as to when a change in a method requires re-validation of the method or on the design of a validation scheme for a complex multi-residue method require a well-considered strategy, based on a current knowledge of international guidance documents and regulatory requirements, as well the laboratory's quality system requirements. Validation demonstrates that a method is 'fit for purpose', so the requirement for validation should be assessed in terms of the intended use of a method and, in the case of change or modification of a method, whether that change or modification may affect a previously validated performance characteristic. In general, method validation involves method scope, calibration-related parameters, method precision, and recovery. Any method change which may affect method scope or any performance parameters will require re-validation. Some typical situations involving change in methods are discussed and a decision process proposed for selection of appropriate validation measures. © 2012 John Wiley & Sons, Ltd.

[The subject matters concerned with use of simplified analytical systems from the perspective of the Japanese Association of Medical Technologists].

PubMed

Morishita, Y

2001-05-01

The subject matters concerned with use of so-called simplified analytical systems for the purpose of useful utilizing are mentioned from the perspective of a laboratory technician. 1. The data from simplified analytical systems should to be agreed with those of particular reference methods not to occur the discrepancy of the data from different laboratories. 2. Accuracy of the measured results using simplified analytical systems is hard to be scrutinized thoroughly and correctly with the quality control surveillance procedure on the stored pooled serum or partly-processed blood. 3. It is necessary to present the guide line to follow about the contents of evaluation to guarantee on quality of simplified analytical systems. 4. Maintenance and manual performance of simplified analytical systems have to be standardized by a laboratory technician and a selling agent technician. 5. It calls attention, further that the cost of simplified analytical systems is much expensive compared to that of routine method with liquid reagents. 6. Various substances in human serum, like cytokine, hormone, tumor marker, and vitamin, etc. are also hoped to be measured by simplified analytical systems.

Clean Water Act Analytical Methods

EPA Pesticide Factsheets

EPA publishes laboratory analytical methods (test procedures) that are used by industries and municipalities to analyze the chemical, physical and biological components of wastewater and other environmental samples required by the Clean Water Act.

Evaluation of analytical performance based on partial order methodology.

PubMed

Carlsen, Lars; Bruggemann, Rainer; Kenessova, Olga; Erzhigitov, Erkin

2015-01-01

Classical measurements of performances are typically based on linear scales. However, in analytical chemistry a simple scale may be not sufficient to analyze the analytical performance appropriately. Here partial order methodology can be helpful. Within the context described here, partial order analysis can be seen as an ordinal analysis of data matrices, especially to simplify the relative comparisons of objects due to their data profile (the ordered set of values an object have). Hence, partial order methodology offers a unique possibility to evaluate analytical performance. In the present data as, e.g., provided by the laboratories through interlaboratory comparisons or proficiency testings is used as an illustrative example. However, the presented scheme is likewise applicable for comparison of analytical methods or simply as a tool for optimization of an analytical method. The methodology can be applied without presumptions or pretreatment of the analytical data provided in order to evaluate the analytical performance taking into account all indicators simultaneously and thus elucidating a "distance" from the true value. In the present illustrative example it is assumed that the laboratories analyze a given sample several times and subsequently report the mean value, the standard deviation and the skewness, which simultaneously are used for the evaluation of the analytical performance. The analyses lead to information concerning (1) a partial ordering of the laboratories, subsequently, (2) a "distance" to the Reference laboratory and (3) a classification due to the concept of "peculiar points". Copyright © 2014 Elsevier B.V. All rights reserved.

RCRA Facility investigation report for Waste Area Grouping 6 at Oak Ridge National Laboratory, Oak Ridge, Tennessee. Volume 5, Technical Memorandums 06-09A, 06-10A, and 06-12A

DOE Office of Scientific and Technical Information (OSTI.GOV)

None

This report provides a detailed summary of the activities carried out to sample groundwater at Waste Area Grouping (WAG) 6. The analytical results for samples collected during Phase 1, Activity 2 of the WAG 6 Resource Conservation and Recovery Act Facility Investigation (RFI) are also presented. In addition, analytical results for Phase 1, activity sampling events for which data were not previously reported are included in this TM. A summary of the groundwater sampling activities of WAG 6, to date, are given in the Introduction. The Methodology section describes the sampling procedures and analytical parameters. Six attachments are included. Attachmentsmore » 1 and 2 provide analytical results for selected RFI groundwater samples and ORNL sampling event. Attachment 3 provides a summary of the contaminants detected in each well sampled for all sampling events conducted at WAG 6. Bechtel National Inc. (BNI)/IT Corporation Contract Laboratory (IT) RFI analytical methods and detection limits are given in Attachment 4. Attachment 5 provides the Oak Ridge National Laboratory (ORNL)/Analytical Chemistry Division (ACD) analytical methods and detection limits and Resource Conservation and Recovery Act (RCRA) quarterly compliance monitoring (1988--1989). Attachment 6 provides ORNL/ACD groundwater analytical methods and detection limits (for the 1990 RCRA semi-annual compliance monitoring).« less

An intercomparison study of analytical methods used for quantification of levoglucosan in ambient aerosol filter samples

NASA Astrophysics Data System (ADS)

Yttri, K. E.; Schnelle-Kreiss, J.; Maenhaut, W.; Alves, C.; Bossi, R.; Bjerke, A.; Claeys, M.; Dye, C.; Evtyugina, M.; García-Gacio, D.; Gülcin, A.; Hillamo, R.; Hoffer, A.; Hyder, M.; Iinuma, Y.; Jaffrezo, J.-L.; Kasper-Giebl, A.; Kiss, G.; López-Mahia, P. L.; Pio, C.; Piot, C.; Ramirez-Santa-Cruz, C.; Sciare, J.; Teinilä, K.; Vermeylen, R.; Vicente, A.; Zimmermann, R.

2014-07-01

The monosaccharide anhydrides (MAs) levoglucosan, galactosan and mannosan are products of incomplete combustion and pyrolysis of cellulose and hemicelluloses, and are found to be major constituents of biomass burning aerosol particles. Hence, ambient aerosol particle concentrations of levoglucosan are commonly used to study the influence of residential wood burning, agricultural waste burning and wild fire emissions on ambient air quality. A European-wide intercomparison on the analysis of the three monosaccharide anhydrides was conducted based on ambient aerosol quartz fiber filter samples collected at a Norwegian urban background site during winter. Thus, the samples' content of MAs is representative for biomass burning particles originating from residential wood burning. The purpose of the intercomparison was to examine the comparability of the great diversity of analytical methods used for analysis of levoglucosan, mannosan and galactosan in ambient aerosol filter samples. Thirteen laboratories participated, of which three applied High-Performance Anion-Exchange Chromatography (HPAEC), four used High-Performance Liquid Chromatography (HPLC) or Ultra-Performance Liquid Chromatography (UPLC), and six resorted to Gas Chromatography (GC). The analytical methods used were of such diversity that they should be considered as thirteen different analytical methods. All of the thirteen laboratories reported levels of levoglucosan, whereas nine reported data for mannosan and/or galactosan. Eight of the thirteen laboratories reported levels for all three isomers. The accuracy for levoglucosan, presented as the mean percentage error (PE) for each participating laboratory, varied from -63 to 23%; however, for 62% of the laboratories the mean PE was within ±10%, and for 85% the mean PE was within ±20%. For mannosan, the corresponding range was -60 to 69%, but as for levoglucosan, the range was substantially smaller for a subselection of the laboratories; i.e., for 33% of the laboratories the mean PE was within ±10%. For galactosan, the mean PE for the participating laboratories ranged from -84 to 593%, and as for mannosan 33% of the laboratories reported a mean PE within ±10%. The variability of the various analytical methods, as defined by their minimum and maximum PE value, was typically better for levoglucosan than for mannosan and galactosan, ranging from 3.2 to 41% for levoglucosan, from 10 to 67% for mannosan, and from 6 to 364% for galactosan. For the levoglucosan to mannosan ratio, which may be used to assess the relative importance of softwood vs. hardwood burning, the variability only ranged from 3.5 to 24%. To our knowledge, this is the first major intercomparison on analytical methods used to quantify monosaccharide anhydrides in ambient aerosol filter samples conducted and reported in the scientific literature. The results show that for levoglucosan the accuracy is only slightly lower than that reported for analysis of SO42- on filter samples, a constituent that has been analyzed by numerous laboratories for several decades, typically by ion chromatography, and which is considered a fairly easy constituent to measure. Hence, the results obtained for levoglucosan with respect to accuracy are encouraging and suggest that levels of levoglucosan, and to a lesser extent mannosan and galactosan, obtained by most of the analytical methods currently used to quantify monosaccharide anhydrides in ambient aerosol filter samples, are comparable. Finally, the various analytical methods used in the current study should be tested for other aerosol matrices and concentrations as well, the most obvious being summertime aerosol samples affected by wild fires and/or agricultural fires.

An intercomparison study of analytical methods used for quantification of levoglucosan in ambient aerosol filter samples

NASA Astrophysics Data System (ADS)

Yttri, K. E.; Schnelle-Kreis, J.; Maenhaut, W.; Abbaszade, G.; Alves, C.; Bjerke, A.; Bonnier, N.; Bossi, R.; Claeys, M.; Dye, C.; Evtyugina, M.; García-Gacio, D.; Hillamo, R.; Hoffer, A.; Hyder, M.; Iinuma, Y.; Jaffrezo, J.-L.; Kasper-Giebl, A.; Kiss, G.; López-Mahia, P. L.; Pio, C.; Piot, C.; Ramirez-Santa-Cruz, C.; Sciare, J.; Teinilä, K.; Vermeylen, R.; Vicente, A.; Zimmermann, R.

2015-01-01

The monosaccharide anhydrides (MAs) levoglucosan, galactosan and mannosan are products of incomplete combustion and pyrolysis of cellulose and hemicelluloses, and are found to be major constituents of biomass burning (BB) aerosol particles. Hence, ambient aerosol particle concentrations of levoglucosan are commonly used to study the influence of residential wood burning, agricultural waste burning and wildfire emissions on ambient air quality. A European-wide intercomparison on the analysis of the three monosaccharide anhydrides was conducted based on ambient aerosol quartz fiber filter samples collected at a Norwegian urban background site during winter. Thus, the samples' content of MAs is representative for BB particles originating from residential wood burning. The purpose of the intercomparison was to examine the comparability of the great diversity of analytical methods used for analysis of levoglucosan, mannosan and galactosan in ambient aerosol filter samples. Thirteen laboratories participated, of which three applied high-performance anion-exchange chromatography (HPAEC), four used high-performance liquid chromatography (HPLC) or ultra-performance liquid chromatography (UPLC) and six resorted to gas chromatography (GC). The analytical methods used were of such diversity that they should be considered as thirteen different analytical methods. All of the thirteen laboratories reported levels of levoglucosan, whereas nine reported data for mannosan and/or galactosan. Eight of the thirteen laboratories reported levels for all three isomers. The accuracy for levoglucosan, presented as the mean percentage error (PE) for each participating laboratory, varied from -63 to 20%; however, for 62% of the laboratories the mean PE was within ±10%, and for 85% the mean PE was within ±20%. For mannosan, the corresponding range was -60 to 69%, but as for levoglucosan, the range was substantially smaller for a subselection of the laboratories; i.e. for 33% of the laboratories the mean PE was within ±10%. For galactosan, the mean PE for the participating laboratories ranged from -84 to 593%, and as for mannosan 33% of the laboratories reported a mean PE within ±10%. The variability of the various analytical methods, as defined by their minimum and maximum PE value, was typically better for levoglucosan than for mannosan and galactosan, ranging from 3.2 to 41% for levoglucosan, from 10 to 67% for mannosan and from 6 to 364% for galactosan. For the levoglucosan to mannosan ratio, which may be used to assess the relative importance of softwood versus hardwood burning, the variability only ranged from 3.5 to 24 . To our knowledge, this is the first major intercomparison on analytical methods used to quantify monosaccharide anhydrides in ambient aerosol filter samples conducted and reported in the scientific literature. The results show that for levoglucosan the accuracy is only slightly lower than that reported for analysis of SO42- (sulfate) on filter samples, a constituent that has been analysed by numerous laboratories for several decades, typically by ion chromatography and which is considered a fairly easy constituent to measure. Hence, the results obtained for levoglucosan with respect to accuracy are encouraging and suggest that levels of levoglucosan, and to a lesser extent mannosan and galactosan, obtained by most of the analytical methods currently used to quantify monosaccharide anhydrides in ambient aerosol filter samples, are comparable. Finally, the various analytical methods used in the current study should be tested for other aerosol matrices and concentrations as well, the most obvious being summertime aerosol samples affected by wildfires and/or agricultural fires.

Plasma creatinine in dogs: intra- and inter-laboratory variation in 10 European veterinary laboratories

PubMed Central

2011-01-01

Background There is substantial variation in reported reference intervals for canine plasma creatinine among veterinary laboratories, thereby influencing the clinical assessment of analytical results. The aims of the study was to determine the inter- and intra-laboratory variation in plasma creatinine among 10 veterinary laboratories, and to compare results from each laboratory with the upper limit of its reference interval. Methods Samples were collected from 10 healthy dogs, 10 dogs with expected intermediate plasma creatinine concentrations, and 10 dogs with azotemia. Overlap was observed for the first two groups. The 30 samples were divided into 3 batches and shipped in random order by postal delivery for plasma creatinine determination. Statistical testing was performed in accordance with ISO standard methodology. Results Inter- and intra-laboratory variation was clinically acceptable as plasma creatinine values for most samples were usually of the same magnitude. A few extreme outliers caused three laboratories to fail statistical testing for consistency. Laboratory sample means above or below the overall sample mean, did not unequivocally reflect high or low reference intervals in that laboratory. Conclusions In spite of close analytical results, further standardization among laboratories is warranted. The discrepant reference intervals seem to largely reflect different populations used in establishing the reference intervals, rather than analytical variation due to different laboratory methods. PMID:21477356

Missed detection of significant positive and negative shifts in gentamicin assay: implications for routine laboratory quality practices.

PubMed

Koerbin, Gus; Liu, Jiakai; Eigenstetter, Alex; Tan, Chin Hon; Badrick, Tony; Loh, Tze Ping

2018-02-15

A product recall was issued for the Roche/Hitachi Cobas Gentamicin II assays on 25 th May 2016 in Australia, after a 15 - 20% positive analytical shift was discovered. Laboratories were advised to employ the Thermo Fisher Gentamicin assay as an alternative. Following the reintroduction of the revised assay on 12 th September 2016, a second reagent recall was made on 20 th March 2017 after the discovery of a 20% negative analytical shift due to erroneous instrument adjustment factor. The practices of an index laboratory were examined to determine how the analytical shifts evaded detection by routine internal quality control (IQC) and external quality assurance (EQA) systems. The ability of the patient result-based approaches, including moving average (MovAvg) and moving sum of outliers (MovSO) approaches in detecting these shifts were examined. Internal quality control data of the index laboratory were acceptable prior to the product recall. The practice of adjusting IQC target following a change in assay method resulted in the missed negative shift when the revised Roche assay was reintroduced. While the EQA data of the Roche subgroup showed clear negative bias relative to other laboratory methods, the results were considered as possible 'matrix effect'. The MovAvg method detected the positive shift before the product recall. The MovSO did not detect the negative shift in the index laboratory but did so in another laboratory 5 days before the second product recall. There are gaps in current laboratory quality practices that leave room for analytical errors to evade detection.

High Throughput Determination of Tetramine in Drinking ...

EPA Pesticide Factsheets

Report The sampling and analytical procedure (SAP) presented herein, describes a method for the high throughput determination of tetramethylene disulfotetramine in drinking water by solid phase extraction and isotope dilution gas chromatography/mass spectrometry. This method, which will be included in the SAM, is expected to provide the Water Laboratory Alliance, as part of EPA’s Environmental Response Laboratory Network, with a more reliable and faster means of analyte collection and measurement.

Analytical Chemistry Laboratory. Progress report for FY 1996

DOE Office of Scientific and Technical Information (OSTI.GOV)

Green, D.W.; Boparai, A.S.; Bowers, D.L.

The purpose of this report is to summarize the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for Fiscal Year (FY) 1996. This annual report is the thirteenth for the ACL. It describes effort on continuing and new projects and contributions of the ACL staff to various programs at ANL. The ACL operates in the ANL system as a full-cost-recovery service center, but has a mission that includes a complementary research and development component: The Analytical Chemistry Laboratory will provide high-quality, cost-effective chemical analysis and related technical support to solve research problems of our clients --more » Argonne National Laboratory, the Department of Energy, and others -- and will conduct world-class research and development in analytical chemistry and its applications. Because of the diversity of research and development work at ANL, the ACL handles a wide range of analytical chemistry problems. Some routine or standard analyses are done, but the ACL usually works with commercial laboratories if our clients require high-volume, production-type analyses. It is common for ANL programs to generate unique problems that require significant development of methods and adaption of techniques to obtain useful analytical data. Thus, much of the support work done by the ACL is very similar to our applied analytical chemistry research.« less

Errors in clinical laboratories or errors in laboratory medicine?

PubMed

Plebani, Mario

2006-01-01

Laboratory testing is a highly complex process and, although laboratory services are relatively safe, they are not as safe as they could or should be. Clinical laboratories have long focused their attention on quality control methods and quality assessment programs dealing with analytical aspects of testing. However, a growing body of evidence accumulated in recent decades demonstrates that quality in clinical laboratories cannot be assured by merely focusing on purely analytical aspects. The more recent surveys on errors in laboratory medicine conclude that in the delivery of laboratory testing, mistakes occur more frequently before (pre-analytical) and after (post-analytical) the test has been performed. Most errors are due to pre-analytical factors (46-68.2% of total errors), while a high error rate (18.5-47% of total errors) has also been found in the post-analytical phase. Errors due to analytical problems have been significantly reduced over time, but there is evidence that, particularly for immunoassays, interference may have a serious impact on patients. A description of the most frequent and risky pre-, intra- and post-analytical errors and advice on practical steps for measuring and reducing the risk of errors is therefore given in the present paper. Many mistakes in the Total Testing Process are called "laboratory errors", although these may be due to poor communication, action taken by others involved in the testing process (e.g., physicians, nurses and phlebotomists), or poorly designed processes, all of which are beyond the laboratory's control. Likewise, there is evidence that laboratory information is only partially utilized. A recent document from the International Organization for Standardization (ISO) recommends a new, broader definition of the term "laboratory error" and a classification of errors according to different criteria. In a modern approach to total quality, centered on patients' needs and satisfaction, the risk of errors and mistakes in pre- and post-examination steps must be minimized to guarantee the total quality of laboratory services.

Amino acid racemization dating of fossil bones, I. inter-laboratory comparison of racemization measurements

USGS Publications Warehouse

Bada, J.L.; Hoopes, E.; Darling, D.; Dungworth, G.; Kessels, H.J.; Kvenvolden, K.A.; Blunt, D.J.

1979-01-01

Enantiomeric measurements for aspartic acid, glutamic acid, and alanine in twenty-one different fossil bone samples have been carried out by three different laboratories using different analytical methods. These inter-laboratory comparisons demonstrate that D/L aspartic acid measurements are highly reproducible, whereas the enantiomeric measurements for the other amino acids show a wide variation between the three laboratories. At present, aspartic acid measurements are the most suitable for racemization dating of bone because of their superior analytical precision. ?? 1979.

Quality-assurance results for routine water analyses in U.S. Geological Survey laboratories, water year 1998

USGS Publications Warehouse

Ludtke, Amy S.; Woodworth, Mark T.; Marsh, Philip S.

2000-01-01

The U.S. Geological Survey operates a quality-assurance program based on the analyses of reference samples for two laboratories: the National Water Quality Laboratory and the Quality of Water Service Unit. Reference samples that contain selected inorganic, nutrient, and low-level constituents are prepared and submitted to the laboratory as disguised routine samples. The program goal is to estimate precision and bias for as many analytical methods offered by the participating laboratories as possible. Blind reference samples typically are submitted at a rate of 2 to 5 percent of the annual environmental-sample load for each constituent. The samples are distributed to the laboratories throughout the year. The reference samples are subject to the identical laboratory handling, processing, and analytical procedures as those applied to environmental samples and, therefore, have been used as an independent source to verify bias and precision of laboratory analytical methods and ambient water-quality measurements. The results are stored permanently in the National Water Information System and the Blind Sample Project's data base. During water year 1998, 95 analytical procedures were evaluated at the National Water Quality Laboratory and 63 analytical procedures were evaluated at the Quality of Water Service Unit. An overall evaluation of the inorganic and low-level constituent data for water year 1998 indicated 77 of 78 analytical procedures at the National Water Quality Laboratory met the criteria for precision. Silver (dissolved, inductively coupled plasma-mass spectrometry) was determined to be imprecise. Five of 78 analytical procedures showed bias throughout the range of reference samples: chromium (dissolved, inductively coupled plasma-atomic emission spectrometry), dissolved solids (dissolved, gravimetric), lithium (dissolved, inductively coupled plasma-atomic emission spectrometry), silver (dissolved, inductively coupled plasma-mass spectrometry), and zinc (dissolved, inductively coupled plasma-mass spectrometry). At the National Water Quality Laboratory during water year 1998, lack of precision was indicated for 2 of 17 nutrient procedures: ammonia as nitrogen (dissolved, colorimetric) and orthophosphate as phosphorus (dissolved, colorimetric). Bias was indicated throughout the reference sample range for ammonia as nitrogen (dissolved, colorimetric, low level) and nitrate plus nitrite as nitrogen (dissolved, colorimetric, low level). All analytical procedures tested at the Quality of Water Service Unit during water year 1998 met the criteria for precision. One of the 63 analytical procedures indicated a bias throughout the range of reference samples: aluminum (whole-water recoverable, inductively coupled plasma-atomic emission spectrometry, trace).

Analytical methods manual for the Mineral Resource Surveys Program, U.S. Geological Survey

USGS Publications Warehouse

Arbogast, Belinda F.

1996-01-01

The analytical methods validated by the Mineral Resource Surveys Program, Geologic Division, is the subject of this manual. This edition replaces the methods portion of Open-File Report 90-668 published in 1990. Newer methods may be used which have been approved by the quality assurance (QA) project and are on file with the QA coordinator.This manual is intended primarily for use by laboratory scientists; this manual can also assist laboratory users to evaluate the data they receive. The analytical methods are written in a step by step approach so that they may be used as a training tool and provide detailed documentation of the procedures for quality assurance. A "Catalog of Services" is available for customer (submitter) use with brief listings of:the element(s)/species determined,method of determination,reference to cite,contact person,summary of the technique,and analyte concentration range.For a copy please contact the Branch office at (303) 236-1800 or fax (303) 236-3200.

METHOD 544. DETERMINATION OF MICROCYSTINS AND ...

EPA Pesticide Factsheets

Method 544 is an accurate and precise analytical method to determine six microcystins (including MC-LR) and nodularin in drinking water using solid phase extraction and liquid chromatography tandem mass spectrometry (SPE-LC/MS/MS). The advantage of this SPE-LC/MS/MS is its sensitivity and ability to speciate the microcystins. This method development task establishes sample preservation techniques, sample concentration and analytical procedures, aqueous and extract holding time criteria and quality control procedures. Draft Method 544 undergone a multi-laboratory verification to ensure other laboratories can implement the method and achieve the quality control measures specified in the method. It is anticipated that Method 544 may be used in UCMR 4 to collect nationwide occurrence data for selected microcystins in drinking water. The purpose of this research project is to develop an accurate and precise analytical method to concentrate and determine selected MCs and nodularin in drinking water.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wiedenman, B. J.; White, T. L.; Mahannah, R. N.

Ion Chromatography (IC) is the principal analytical method used to support studies of Sludge Reciept and Adjustment Tank (SRAT) chemistry at DWPF. A series of prior analytical ''Round Robin'' (RR) studies included both supernate and sludge samples from SRAT simulant, previously reported as memos, are tabulated in this report.2,3 From these studies it was determined to standardize IC column size to 4 mm diameter, eliminating the capillary column from use. As a follow on test, the DWPF laboratory, the PSAL laboratory, and the AD laboratory participated in the current analytical RR to determine a suite of anions in SRAT simulantmore » by IC, results also are tabulated in this report. The particular goal was to confirm the laboratories ability to measure and quantitate glycolate ion. The target was + or - 20% inter-lab agreement of the analyte averages for the RR. Each of the three laboratories analyzed a batch of 12 samples. For each laboratory, the percent relative standard deviation (%RSD) of the averages on nitrate, glycolate, and oxalate, was 10% or less. The three laboratories all met the goal of 20% relative agreement for nitrate and glycolate. For oxalate, the PSAL laboratory reported an average value that was 20% higher than the average values reported by the DWPF laboratory and the AD laboratory. Because of this wider window of agreement, it was concluded to continue the practice of an additional acid digestion for total oxalate measurement. It should also be noted that large amounts of glycolate in the SRAT samples will have an impact on detection limits of near eluting peaks, namely Fluoride and Formate. A suite of scoping experiments are presented in the report to identify and isolate other potential interlaboratory disceprancies. Specific ion chromatography inter-laboratory method conditions and differences are tabulated. Most differences were minor but there are some temperature control equipment differences that are significant leading to a recommendation of a heated jacket for analytical columns that are remoted for use in radiohoods. A suggested method improvement would be to implement column temperture control at a temperature slightly above ambient to avoid peak shifting due to temperature fluctuations. Temperature control in this manner would improve short and longer term peak retention time stability. An unknown peak was observed during the analysis of glycolic acid and SRAT simulant. The unknown peak was determined to best match diglycolic acid. The development of a method for acetate is summaraized, and no significant amount of acetate was observed in the SRAT products tested. In addition, an alternative Gas Chromatograph (GC) method for glycolate is summarized.« less

Reduction of multi-dimensional laboratory data to a two-dimensional plot: a novel technique for the identification of laboratory error.

PubMed

Kazmierczak, Steven C; Leen, Todd K; Erdogmus, Deniz; Carreira-Perpinan, Miguel A

2007-01-01

The clinical laboratory generates large amounts of patient-specific data. Detection of errors that arise during pre-analytical, analytical, and post-analytical processes is difficult. We performed a pilot study, utilizing a multidimensional data reduction technique, to assess the utility of this method for identifying errors in laboratory data. We evaluated 13,670 individual patient records collected over a 2-month period from hospital inpatients and outpatients. We utilized those patient records that contained a complete set of 14 different biochemical analytes. We used two-dimensional generative topographic mapping to project the 14-dimensional record to a two-dimensional space. The use of a two-dimensional generative topographic mapping technique to plot multi-analyte patient data as a two-dimensional graph allows for the rapid identification of potentially anomalous data. Although we performed a retrospective analysis, this technique has the benefit of being able to assess laboratory-generated data in real time, allowing for the rapid identification and correction of anomalous data before they are released to the physician. In addition, serial laboratory multi-analyte data for an individual patient can also be plotted as a two-dimensional plot. This tool might also be useful for assessing patient wellbeing and prognosis.

Analytical Methods for Trace Metals. Training Manual.

ERIC Educational Resources Information Center

Office of Water Program Operations (EPA), Cincinnati, OH. National Training and Operational Technology Center.

This training manual presents material on the theoretical concepts involved in the methods listed in the Federal Register as approved for determination of trace metals. Emphasis is on laboratory operations. This course is intended for chemists and technicians with little or no experience in analytical methods for trace metals. Students should have…

Determination of Mercury in Milk by Cold Vapor Atomic Fluorescence: A Green Analytical Chemistry Laboratory Experiment

ERIC Educational Resources Information Center

Armenta, Sergio; de la Guardia, Miguel

2011-01-01

Green analytical chemistry principles were introduced to undergraduate students in a laboratory experiment focused on determining the mercury concentration in cow and goat milk. In addition to traditional goals, such as accuracy, precision, sensitivity, and limits of detection in method selection and development, attention was paid to the…

Evaluation of Analytical Errors in a Clinical Chemistry Laboratory: A 3 Year Experience

PubMed Central

Sakyi, AS; Laing, EF; Ephraim, RK; Asibey, OF; Sadique, OK

2015-01-01

Background: Proficient laboratory service is the cornerstone of modern healthcare systems and has an impact on over 70% of medical decisions on admission, discharge, and medications. In recent years, there is an increasing awareness of the importance of errors in laboratory practice and their possible negative impact on patient outcomes. Aim: We retrospectively analyzed data spanning a period of 3 years on analytical errors observed in our laboratory. The data covered errors over the whole testing cycle including pre-, intra-, and post-analytical phases and discussed strategies pertinent to our settings to minimize their occurrence. Materials and Methods: We described the occurrence of pre-analytical, analytical and post-analytical errors observed at the Komfo Anokye Teaching Hospital clinical biochemistry laboratory during a 3-year period from January, 2010 to December, 2012. Data were analyzed with Graph Pad Prism 5(GraphPad Software Inc. CA USA). Results: A total of 589,510 tests was performed on 188,503 outpatients and hospitalized patients. The overall error rate for the 3 years was 4.7% (27,520/58,950). Pre-analytical, analytical and post-analytical errors contributed 3.7% (2210/58,950), 0.1% (108/58,950), and 0.9% (512/58,950), respectively. The number of tests reduced significantly over the 3-year period, but this did not correspond with a reduction in the overall error rate (P = 0.90) along with the years. Conclusion: Analytical errors are embedded within our total process setup especially pre-analytical and post-analytical phases. Strategic measures including quality assessment programs for staff involved in pre-analytical processes should be intensified. PMID:25745569

Lack of grading agreement among international hemostasis external quality assessment programs

PubMed Central

Olson, John D.; Jennings, Ian; Meijer, Piet; Bon, Chantal; Bonar, Roslyn; Favaloro, Emmanuel J.; Higgins, Russell A.; Keeney, Michael; Mammen, Joy; Marlar, Richard A.; Meley, Roland; Nair, Sukesh C.; Nichols, William L.; Raby, Anne; Reverter, Joan C.; Srivastava, Alok; Walker, Isobel

2018-01-01

Laboratory quality programs rely on internal quality control and external quality assessment (EQA). EQA programs provide unknown specimens for the laboratory to test. The laboratory's result is compared with other (peer) laboratories performing the same test. EQA programs assign target values using a variety of methods statistical tools and performance assessment of ‘pass’ or ‘fail’ is made. EQA provider members of the international organization, external quality assurance in thrombosis and hemostasis, took part in a study to compare outcome of performance analysis using the same data set of laboratory results. Eleven EQA organizations using eight different analytical approaches participated. Data for a normal and prolonged activated partial thromboplastin time (aPTT) and a normal and reduced factor VIII (FVIII) from 218 laboratories were sent to the EQA providers who analyzed the data set using their method of evaluation for aPTT and FVIII, determining the performance for each laboratory record in the data set. Providers also summarized their statistical approach to assignment of target values and laboratory performance. Each laboratory record in the data set was graded pass/fail by all EQA providers for each of the four analytes. There was a lack of agreement of pass/fail grading among EQA programs. Discordance in the grading was 17.9 and 11% of normal and prolonged aPTT results, respectively, and 20.2 and 17.4% of normal and reduced FVIII results, respectively. All EQA programs in this study employed statistical methods compliant with the International Standardization Organization (ISO), ISO 13528, yet the evaluation of laboratory results for all four analytes showed remarkable grading discordance. PMID:29232255

PRN 96-1: Tolerance Enforcement Methods - Independent Laboratory Validation by Petitioner

EPA Pesticide Factsheets

This notice is intended to clarify the requirements for submission of an Independent Laboratory Validation to accompany new pesticide analytical methods and does not contain additional data requirements.This notice supersedes PR Notice 88-5.

Biological Matrix Effects in Quantitative Tandem Mass Spectrometry-Based Analytical Methods: Advancing Biomonitoring

PubMed Central

Panuwet, Parinya; Hunter, Ronald E.; D’Souza, Priya E.; Chen, Xianyu; Radford, Samantha A.; Cohen, Jordan R.; Marder, M. Elizabeth; Kartavenka, Kostya; Ryan, P. Barry; Barr, Dana Boyd

2015-01-01

The ability to quantify levels of target analytes in biological samples accurately and precisely, in biomonitoring, involves the use of highly sensitive and selective instrumentation such as tandem mass spectrometers and a thorough understanding of highly variable matrix effects. Typically, matrix effects are caused by co-eluting matrix components that alter the ionization of target analytes as well as the chromatographic response of target analytes, leading to reduced or increased sensitivity of the analysis. Thus, before the desired accuracy and precision standards of laboratory data are achieved, these effects must be characterized and controlled. Here we present our review and observations of matrix effects encountered during the validation and implementation of tandem mass spectrometry-based analytical methods. We also provide systematic, comprehensive laboratory strategies needed to control challenges posed by matrix effects in order to ensure delivery of the most accurate data for biomonitoring studies assessing exposure to environmental toxicants. PMID:25562585

Quality-assurance results for routine water analysis in US Geological Survey laboratories, water year 1991

USGS Publications Warehouse

Maloney, T.J.; Ludtke, A.S.; Krizman, T.L.

1994-01-01

The US. Geological Survey operates a quality- assurance program based on the analyses of reference samples for the National Water Quality Laboratory in Arvada, Colorado, and the Quality of Water Service Unit in Ocala, Florida. Reference samples containing selected inorganic, nutrient, and low ionic-strength constituents are prepared and disguised as routine samples. The program goal is to determine precision and bias for as many analytical methods offered by the participating laboratories as possible. The samples typically are submitted at a rate of approximately 5 percent of the annual environmental sample load for each constituent. The samples are distributed to the laboratories throughout the year. Analytical data for these reference samples reflect the quality of environmental sample data produced by the laboratories because the samples are processed in the same manner for all steps from sample login through data release. The results are stored permanently in the National Water Data Storage and Retrieval System. During water year 1991, 86 analytical procedures were evaluated at the National Water Quality Laboratory and 37 analytical procedures were evaluated at the Quality of Water Service Unit. An overall evaluation of the inorganic (major ion and trace metal) constituent data for water year 1991 indicated analytical imprecision in the National Water Quality Laboratory for 5 of 67 analytical procedures: aluminum (whole-water recoverable, atomic emission spectrometric, direct-current plasma); calcium (atomic emission spectrometric, direct); fluoride (ion-exchange chromatographic); iron (whole-water recoverable, atomic absorption spectrometric, direct); and sulfate (ion-exchange chromatographic). The results for 11 of 67 analytical procedures had positive or negative bias during water year 1991. Analytical imprecision was indicated in the determination of two of the five National Water Quality Laboratory nutrient constituents: orthophosphate as phosphorus and phosphorus. A negative or positive bias condition was indicated in three of five nutrient constituents. There was acceptable precision and no indication of bias for the 14 low ionic-strength analytical procedures tested in the National Water Quality Laboratory program and for the 32 inorganic and 5 nutrient analytical procedures tested in the Quality of Water Service Unit during water year 1991.

Assuring the Quality of Test Results in the Field of Nuclear Techniques and Ionizing Radiation. The Practical Implementation of Section 5.9 of the EN ISO/IEC 17025 Standard

NASA Astrophysics Data System (ADS)

Cucu, Daniela; Woods, Mike

2008-08-01

The paper aims to present a practical approach for testing laboratories to ensure the quality of their test results. It is based on the experience gained in assessing a large number of testing laboratories, discussing with management and staff, reviewing results obtained in national and international PTs and ILCs and exchanging information in the EA laboratory committee. According to EN ISO/IEC 17025, an accredited laboratory has to implement a programme to ensure the quality of its test results for each measurand. Pre-analytical, analytical and post-analytical measures shall be applied in a systematic manner. They shall include both quality control and quality assurance measures. When designing the quality assurance programme a laboratory should consider pre-analytical activities (like personnel training, selection and validation of test methods, qualifying equipment), analytical activities ranging from sampling, sample preparation, instrumental analysis and post-analytical activities (like decoding, calculation, use of statistical tests or packages, management of results). Designed on different levels (analyst, quality manager and technical manager), including a variety of measures, the programme shall ensure the validity and accuracy of test results, the adequacy of the management system, prove the laboratory's competence in performing tests under accreditation and last but not least show the comparability of test results. Laboratory management should establish performance targets and review periodically QC/QA results against them, implementing appropriate measures in case of non-compliance.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Green, D.W.; Boparai, A.S.; Bowers, D.L.

This report summarizes the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for Fiscal Year (FY) 2000 (October 1999 through September 2000). This annual progress report, which is the seventeenth in this series for the ACL, describes effort on continuing projects, work on new projects, and contributions of the ACL staff to various programs at ANL. The ACL operates within the ANL system as a full-cost-recovery service center, but it has a mission that includes a complementary research and development component: The Analytical Chemistry Laboratory will provide high-quality, cost-effective chemical analysis and related technical support tomore » solve research problems of our clients--Argonne National Laboratory, the Department of Energy, and others--and will conduct world-class research and development in analytical chemistry and its applications. The ACL handles a wide range of analytical problems that reflects the diversity of research and development (R&D) work at ANL. Some routine or standard analyses are done, but the ACL operates more typically in a problem-solving mode in which development of methods is required or adaptation of techniques is needed to obtain useful analytical data. The ACL works with clients and commercial laboratories if a large number of routine analyses are required. Much of the support work done by the ACL is very similar to applied analytical chemistry research work.« less

Developing and Implementing Inquiry-Based, Water Quality Laboratory Experiments for High School Students to Explore Real Environmental Issues Using Analytical Chemistry

ERIC Educational Resources Information Center

Mandler, Daphna; Blonder, Ron; Yayon, Malka; Mamlok-Naaman, Rachel; Hofstein, Avi

2014-01-01

This paper describes the rationale and the implementation of five laboratory experiments; four of them, intended for high-school students, are inquiry-based activities that explore the quality of water. The context of water provides students with an opportunity to study the importance of analytical methods and how they influence our everyday…

Recommendations for accreditation of laboratories in molecular biology of hematologic malignancies.

PubMed

Flandrin-Gresta, Pascale; Cornillet, Pascale; Hayette, Sandrine; Gachard, Nathalie; Tondeur, Sylvie; Mauté, Carole; Cayuela, Jean-Michel

2015-01-01

Over recent years, the development of molecular biology techniques has improved the hematological diseases diagnostic and follow-up. Consequently, these techniques are largely used in the biological screening of these diseases; therefore the Hemato-oncology molecular diagnostics laboratories must be actively involved in the accreditation process according the ISO 15189 standard. The French group of molecular biologists (GBMHM) provides requirements for the implementation of quality assurance for the medical molecular laboratories. This guideline states the recommendations for the pre-analytical, analytical (methods validation procedures, quality controls, reagents), and post-analytical conditions. In addition, herein we state a strategy for the internal quality control management. These recommendations will be regularly updated.

Quantitative Comparison of Three Standardization Methods Using a One-Way ANOVA for Multiple Mean Comparisons

ERIC Educational Resources Information Center

Barrows, Russell D.

2007-01-01

A one-way ANOVA experiment is performed to determine whether or not the three standardization methods are statistically different in determining the concentration of the three paraffin analytes. The laboratory exercise asks students to combine the three methods in a single analytical procedure of their own design to determine the concentration of…

Evaluation of nutrient quality-assurance data for Alexanders and Mount Rock Spring basins, Cumberland County, Pennsylvania

USGS Publications Warehouse

Witt, E. C.; Hippe, D.J.; Giovannitti, R.M.

1992-01-01

A total of 304 nutrient samples were collected from May 1990 through September 1991 to determine concentrations and loads of nutrients in water discharged from two spring basins in Cumberland County, Pa. Fifty-four percent of these nutrient samples were for the evaluation of (1) laboratory consistency, (2) container and preservative cleanliness, (3) maintenance of analyte representativeness as affected by three different preservation methods, and (4) comparison of analyte results with the "Most Probable Value" for Standard Reference Water Samples. Results of 37 duplicate analyses indicate that the Pennsylvania Department of Environmental Resources, Bureau of Laboratories (principal laboratory) remained within its ±10 percent goal for all but one analyte. Results of the blank analysis show that the sampling containers did not compromise the water quality. However, mercuric-chloride-preservation blanks apparently contained measurable ammonium in four of five samples and ammonium plus organic nitrogen in two of five samples. Interlaboratory results indicate substantial differences in the determination of nitrate and ammonium plus organic nitrogen between the principal laboratory and the U.S. Geological Survey National Water-Quality Laboratory. In comparison with the U.S. Environmental Protection Agency Quality-Control Samples, the principal laboratory was sufficiently accurate in its determination of nutrient anafytes. Analysis of replicate samples indicated that sulfuric-acid preservative best maintained the representativeness of the anafytes nitrate and ammonium plus organic nitrogen, whereas, mercuric chloride best maintained the representativeness of orthophosphate. Comparison of nutrient analyte determinations with the Most Probable Value for each preservation method shows that two of five analytes with no chemical preservative compare well, three of five with mercuric-chloride preservative compare well, and three of five with sulfuricacid preservative compare well.

How to conduct External Quality Assessment Schemes for the pre-analytical phase?

PubMed

Kristensen, Gunn B B; Aakre, Kristin Moberg; Kristoffersen, Ann Helen; Sandberg, Sverre

2014-01-01

In laboratory medicine, several studies have described the most frequent errors in the different phases of the total testing process, and a large proportion of these errors occur in the pre-analytical phase. Schemes for registration of errors and subsequent feedback to the participants have been conducted for decades concerning the analytical phase by External Quality Assessment (EQA) organizations operating in most countries. The aim of the paper is to present an overview of different types of EQA schemes for the pre-analytical phase, and give examples of some existing schemes. So far, very few EQA organizations have focused on the pre-analytical phase, and most EQA organizations do not offer pre-analytical EQA schemes (EQAS). It is more difficult to perform and standardize pre-analytical EQAS and also, accreditation bodies do not ask the laboratories for results from such schemes. However, some ongoing EQA programs for the pre-analytical phase do exist, and some examples are given in this paper. The methods used can be divided into three different types; collecting information about pre-analytical laboratory procedures, circulating real samples to collect information about interferences that might affect the measurement procedure, or register actual laboratory errors and relate these to quality indicators. These three types have different focus and different challenges regarding implementation, and a combination of the three is probably necessary to be able to detect and monitor the wide range of errors occurring in the pre-analytical phase.

A short history, principles, and types of ELISA, and our laboratory experience with peptide/protein analyses using ELISA.

PubMed

Aydin, Suleyman

2015-10-01

Playing a critical role in the metabolic homeostasis of living systems, the circulating concentrations of peptides/proteins are influenced by a variety of patho-physiological events. These peptide/protein concentrations in biological fluids are measured using various methods, the most common of which is enzymatic immunoassay EIA/ELISA and which guide the clinicians in diagnosing and monitoring diseases that inflict biological systems. All the techniques where enzymes are employed to show antigen-antibody reactions are generally referred to as enzymatic immunoassay EIA/ELISA method. Since the basic principles of EIA and ELISA are the same. The main objective of this review is to present an overview of the historical journey that had led to the invention of EIA/ELISA, an indispensible method for medical and research laboratories, types of ELISA developed after its invention [direct (the first ELISA method invented), indirect, sandwich and competitive methods], problems encountered during peptide/protein analyses (pre-analytical, analytical and post-analytical), rules to be followed to prevent these problems, and our laboratory experience of more than 15 years. Copyright © 2015 Elsevier Inc. All rights reserved.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of inorganic and organic constituents in water and fluvial sediments

USGS Publications Warehouse

Fishman, M. J.

1993-01-01

Methods to be used to analyze samples of water, suspended sediment and bottom material for their content of inorganic and organic constituents are presented. Technology continually changes, and so this laboratory manual includes new and revised methods for determining the concentration of dissolved constituents in water, whole water recoverable constituents in water-suspended sediment samples, and recoverable concentration of constit- uents in bottom material. For each method, the general topics covered are the application, the principle of the method, interferences, the apparatus and reagents required, a detailed description of the analytical procedure, reporting results, units and significant figures, and analytical precision data. Included in this manual are 30 methods.

Laboratory analytical methods for the determination of the hydrocarbon status of soils (a review)

NASA Astrophysics Data System (ADS)

Pikovskii, Yu. I.; Korotkov, L. A.; Smirnova, M. A.; Kovach, R. G.

2017-10-01

Laboratory analytical methods suitable for the determination of the hydrocarbon status of soils (a specific soil characteristic involving information on the total content and qualitative features of soluble (bitumoid) carbonaceous substances and individual hydrocarbons (polycyclic aromatic hydrocarbons, alkanes, etc.) in bitumoid, as well as the composition and content of hydrocarbon gases) have been considered. Among different physicochemical methods of study, attention is focused on the methods suitable for the wide use. Luminescence-bituminological analysis, low-temperature spectrofluorimetry (Shpolskii spectroscopy), infrared (IR) spectroscopy, gas chromatography, chromatography-mass spectrometry, and some other methods have been characterized, as well as sample preparation features. Advantages and limitations of each of these methods are described; their efficiency, instrumental complexity, analysis duration, and accuracy are assessed.

40 CFR 141.33 - Record maintenance.

Code of Federal Regulations, 2010 CFR

2010-07-01

... laboratory reports may be kept, or data may be transferred to tabular summaries, provided that the following...) Laboratory and person responsible for performing analysis; (5) The analytical technique/method used; and (6...

Information Management Systems in the Undergraduate Instrumental Analysis Laboratory.

ERIC Educational Resources Information Center

Merrer, Robert J.

1985-01-01

Discusses two applications of Laboratory Information Management Systems (LIMS) in the undergraduate laboratory. They are the coulometric titration of thiosulfate with electrogenerated triiodide ion and the atomic absorption determination of calcium using both analytical calibration curve and standard addition methods. (JN)

Methods for determination of inorganic substances in water and fluvial sediments

USGS Publications Warehouse

Fishman, Marvin J.; Friedman, Linda C.

1989-01-01

Chapter Al of the laboratory manual contains methods used by the U.S. Geological Survey to analyze samples of water, suspended sediments, and bottom material for their content of inorganic constituents. Included are methods for determining the concentration of dissolved constituents in water, the total recoverable and total of constituents in water-suspended sediment samples, and the recoverable and total concentrations of constituents in samples of bottom material. The introduction to the manual includes essential definitions and a brief discussion of the use of significant figures in calculating and reporting analytical results. Quality control in the water-analysis laboratory is discussed, including the accuracy and precision of analyses, the use of standard-reference water samples, and the operation of an effective quality-assurance program. Methods for sample preparation and pretreatment are given also. A brief discussion of the principles of the analytical techniques involved and their particular application to water and sediment analysis is presented. The analytical methods of these techniques are arranged alphabetically by constituent. For each method, the general topics covered are the application, the principle of the method, the interferences, the apparatus and reagents required, a detailed description of the analytical procedure, reporting results, units and significant figures, and analytical precision data, when available. More than 126 methods are given for the determination of 70 inorganic constituents and physical properties of water, suspended sediment, and bottom material.

Methods for determination of inorganic substances in water and fluvial sediments

USGS Publications Warehouse

Fishman, Marvin J.; Friedman, Linda C.

1985-01-01

Chapter Al of the laboratory manual contains methods used by the Geological Survey to analyze samples of water, suspended sediments, and bottom material for their content of inorganic constituents. Included are methods for determining the concentration of dissolved constituents in water, total recoverable and total of constituents in water-suspended sediment samples, and recoverable and total concentrations of constituents in samples of bottom material. Essential definitions are included in the introduction to the manual, along with a brief discussion of the use of significant figures in calculating and reporting analytical results. Quality control in the water-analysis laboratory is discussed, including accuracy and precision of analyses, the use of standard reference water samples, and the operation of an effective quality assurance program. Methods for sample preparation and pretreatment are given also.A brief discussion of the principles of the analytical techniques involved and their particular application to water and sediment analysis is presented. The analytical methods involving these techniques are arranged alphabetically according to constituent. For each method given, the general topics covered are application, principle of the method, interferences, apparatus and reagents required, a detailed description of the analytical procedure, reporting results, units and significant figures, and analytical precision data, when available. More than 125 methods are given for the determination of 70 different inorganic constituents and physical properties of water, suspended sediment, and bottom material.

Analytical performances of food microbiology laboratories - critical analysis of 7 years of proficiency testing results.

PubMed

Abdel Massih, M; Planchon, V; Polet, M; Dierick, K; Mahillon, J

2016-02-01

Based on the results of 19 food microbiology proficiency testing (PT) schemes, this study aimed to assess the laboratory performances, to highlight the main sources of unsatisfactory analytical results and to suggest areas of improvement. The 2009-2015 results of REQUASUD and IPH PT, involving a total of 48 laboratories, were analysed. On average, the laboratories failed to detect or enumerate foodborne pathogens in 3·0% of the tests. Thanks to a close collaboration with the PT participants, the causes of outliers could be identified in 74% of the cases. The main causes of erroneous PT results were either pre-analytical (handling of the samples, timing of analysis), analytical (unsuitable methods, confusion of samples, errors in colony counting or confirmation) or postanalytical mistakes (calculation and encoding of results). PT schemes are a privileged observation post to highlight analytical problems, which would otherwise remain unnoticed. In this perspective, this comprehensive study of PT results provides insight into the sources of systematic errors encountered during the analyses. This study draws the attention of the laboratories to the main causes of analytical errors and suggests practical solutions to avoid them, in an educational purpose. The observations support the hypothesis that regular participation to PT, when followed by feed-back and appropriate corrective actions, can play a key role in quality improvement and provide more confidence in the laboratory testing results. © 2015 The Society for Applied Microbiology.

Comparison of multianalyte proficiency test results by sum of ranking differences, principal component analysis, and hierarchical cluster analysis.

PubMed

Škrbić, Biljana; Héberger, Károly; Durišić-Mladenović, Nataša

2013-10-01

Sum of ranking differences (SRD) was applied for comparing multianalyte results obtained by several analytical methods used in one or in different laboratories, i.e., for ranking the overall performances of the methods (or laboratories) in simultaneous determination of the same set of analytes. The data sets for testing of the SRD applicability contained the results reported during one of the proficiency tests (PTs) organized by EU Reference Laboratory for Polycyclic Aromatic Hydrocarbons (EU-RL-PAH). In this way, the SRD was also tested as a discriminant method alternative to existing average performance scores used to compare mutlianalyte PT results. SRD should be used along with the z scores--the most commonly used PT performance statistics. SRD was further developed to handle the same rankings (ties) among laboratories. Two benchmark concentration series were selected as reference: (a) the assigned PAH concentrations (determined precisely beforehand by the EU-RL-PAH) and (b) the averages of all individual PAH concentrations determined by each laboratory. Ranking relative to the assigned values and also to the average (or median) values pointed to the laboratories with the most extreme results, as well as revealed groups of laboratories with similar overall performances. SRD reveals differences between methods or laboratories even if classical test(s) cannot. The ranking was validated using comparison of ranks by random numbers (a randomization test) and using seven folds cross-validation, which highlighted the similarities among the (methods used in) laboratories. Principal component analysis and hierarchical cluster analysis justified the findings based on SRD ranking/grouping. If the PAH-concentrations are row-scaled, (i.e., z scores are analyzed as input for ranking) SRD can still be used for checking the normality of errors. Moreover, cross-validation of SRD on z scores groups the laboratories similarly. The SRD technique is general in nature, i.e., it can be applied to any experimental problem in which multianalyte results obtained either by several analytical procedures, analysts, instruments, or laboratories need to be compared.

Standardization in laboratory medicine: Adoption of common reference intervals to the Croatian population.

PubMed

Flegar-Meštrić, Zlata; Perkov, Sonja; Radeljak, Andrea

2016-03-26

Considering the fact that the results of laboratory tests provide useful information about the state of health of patients, determination of reference value is considered an intrinsic part in the development of laboratory medicine. There are still huge differences in the analytical methods used as well as in the associated reference intervals which could consequently significantly affect the proper assessment of patient health. In a constant effort to increase the quality of patients' care, there are numerous international initiatives for standardization and/or harmonization of laboratory diagnostics in order to achieve maximum comparability of laboratory test results and improve patient safety. Through the standardization and harmonization processes of analytical methods the ability to create unique reference intervals is achieved. Such reference intervals could be applied globally in all laboratories using methods traceable to the same reference measuring system and analysing the biological samples from the populations with similar socio-demographic and ethnic characteristics. In this review we outlined the results of the harmonization processes in Croatia in the field of population based reference intervals for clinically relevant blood and serum constituents which are in accordance with ongoing activity for worldwide standardization and harmonization based on traceability in laboratory medicine.

Standardization in laboratory medicine: Adoption of common reference intervals to the Croatian population

PubMed Central

Flegar-Meštrić, Zlata; Perkov, Sonja; Radeljak, Andrea

2016-01-01

Considering the fact that the results of laboratory tests provide useful information about the state of health of patients, determination of reference value is considered an intrinsic part in the development of laboratory medicine. There are still huge differences in the analytical methods used as well as in the associated reference intervals which could consequently significantly affect the proper assessment of patient health. In a constant effort to increase the quality of patients’ care, there are numerous international initiatives for standardization and/or harmonization of laboratory diagnostics in order to achieve maximum comparability of laboratory test results and improve patient safety. Through the standardization and harmonization processes of analytical methods the ability to create unique reference intervals is achieved. Such reference intervals could be applied globally in all laboratories using methods traceable to the same reference measuring system and analysing the biological samples from the populations with similar socio-demographic and ethnic characteristics. In this review we outlined the results of the harmonization processes in Croatia in the field of population based reference intervals for clinically relevant blood and serum constituents which are in accordance with ongoing activity for worldwide standardization and harmonization based on traceability in laboratory medicine. PMID:27019800

Methods for Analysis and Simulation of Ballistic Impact

DTIC Science & Technology

2017-04-01

ARL-RP-0597 ● Apr 2017 US Army Research Laboratory Methods for Analysis and Simulation of Ballistic Impact by John D Clayton...Laboratory Methods for Analysis and Simulation of Ballistic Impact by John D Clayton Weapons and Materials Research Directorate, ARL...analytical, and numerical methods of ballistics research . Similar lengthy references dealing with pertinent aspects include [8, 9]. In contrast, the

Accuracy verification and identification of matrix effects. The College of American Pathologists' Protocol.

PubMed

Eckfeldt, J H; Copeland, K R

1993-04-01

Proficiency testing using stabilized control materials has been used for decades as a means of monitoring and improving performance in the clinical laboratory. Often, the commonly used proficiency testing materials exhibit "matrix effects" that cause them to behave differently from fresh human specimens in certain clinical analytic systems. Because proficiency testing is the primary method in which regulatory agencies have chosen to evaluate clinical laboratory performance, the College of American Pathologists (CAP) has proposed guidelines for investigating the influence of matrix effects on their Survey results. The purpose of this investigation was to determine the feasibility, usefulness, and potential problems associated with this CAP Matrix Effect Analytical Protocol, in which fresh patient specimens and CAP proficiency specimens are analyzed simultaneously by a field method and a definitive, reference, or other comparative method. The optimal outcome would be that both the fresh human and CAP Survey specimens agree closely with the comparative method result. However, this was not always the case. Using several different analytic configurations, we were able to demonstrate matrix and calibration biases for several of the analytes investigated.

Environmental Contaminants, Metabolites, Cells, Organ Tissues, and Water: All in a Day’s Work at the EPA Analytical Chemistry Research Core

EPA Science Inventory

The talk will highlight key aspects and results of analytical methods the EPA National Health and Environmental Effects Research Laboratory (NHEERL) Analytical Chemistry Research Core (ACRC) develops and uses to provide data on disposition, metabolism, and effects of environmenta...

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

The purpose of this report is to summarize the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for Fiscal Year (FY) 1993 (October 1992 through September 1993). This annual report is the tenth for the ACL and describes continuing effort on projects, work on new projects, and contributions of the ACL staff to various programs at ANL. The Analytical Chemistry Laboratory is a full-cost-recovery service center, with the primary mission of providing a broad range of analytical chemistry support services to the scientific and engineering programs at ANL. The ACL also has research programs in analyticalmore » chemistry, conducts instrumental and methods development, and provides analytical services for governmental, educational, and industrial organizations. The ACL handles a wide range of analytical problems. Some routine or standard analyses are done, but it is common for the Argonne programs to generate unique problems that require development or modification of methods and adaption of techniques to obtain useful analytical data. The ACL is administratively within the Chemical Technology Division (CMT), its principal ANL client, but provides technical support for many of the technical divisions and programs at ANL. The ACL has four technical groups--Chemical Analysis, Instrumental Analysis, Organic Analysis, and Environmental Analysis--which together include about 45 technical staff members. Talents and interests of staff members cross the group lines, as do many projects within the ACL.« less

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Moderate-Use Pesticides and Selected Degradates in Water by C-18 Solid-Phase Extraction and Gas Chromatography/Mass Spectrometry

USGS Publications Warehouse

Sandstrom, Mark W.; Stroppel, Max E.; Foreman, William T.; Schroeder, Michael P.

2001-01-01

A method for the isolation and analysis of 21 parent pesticides and 20 pesticide degradates in natural-water samples is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase-extraction columns that contain octadecyl-bonded porous silica to extract the analytes. The columns are dried by using nitrogen gas, and adsorbed analytes are eluted with ethyl acetate. Extracted analytes are determined by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 2 micrograms per liter (?g/L) for most analytes. Single-operator method detection limits in reagent-water samples range from 0.00 1 to 0.057 ?g/L. Validation data also are presented for 14 parent pesticides and 20 degradates that were determined to have greater bias or variability, or shorter holding times than the other compounds. The estimated maximum holding time for analytes in pesticide-grade water before extraction was 4 days. The estimated maximum holding time for analytes after extraction on the dry solid-phase-extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time. The method complements existing U.S. Geological Survey Method O-1126-95 (NWQL Schedules 2001 and 2010) by using identical sample preparation and comparable instrument analytical conditions so that sample extracts can be analyzed by either method to expand the range of analytes determined from one water sample.

CAP/ACMG proficiency testing for biochemical genetics laboratories: a summary of performance.

PubMed

Oglesbee, Devin; Cowan, Tina M; Pasquali, Marzia; Wood, Timothy C; Weck, Karen E; Long, Thomas; Palomaki, Glenn E

2018-01-01

PurposeTesting for inborn errors of metabolism is performed by clinical laboratories worldwide, each utilizing laboratory-developed procedures. We sought to summarize performance in the College of American Pathologists' (CAP) proficiency testing (PT) program and identify opportunities for improving laboratory quality. When evaluating PT data, we focused on a subset of laboratories that have participated in at least one survey since 2010.MethodsAn analysis of laboratory performance (2004 to 2014) on the Biochemical Genetics PT Surveys, a program administered by CAP and the American College of Medical Genetics and Genomics. Analytical and interpretive performance was evaluated for four tests: amino acids, organic acids, acylcarnitines, and mucopolysaccharides.ResultsSince 2010, 150 laboratories have participated in at least one of four PT surveys. Analytic sensitivities ranged from 88.2 to 93.4%, while clinical sensitivities ranged from 82.4 to 91.0%. Performance was higher for US participants and for more recent challenges. Performance was lower for challenges with subtle findings or complex analytical patterns.ConclusionUS clinical biochemical genetics laboratory proficiency is satisfactory, with a minority of laboratories accounting for the majority of errors. Our findings underscore the complex nature of clinical biochemical genetics testing and highlight the necessity of continuous quality management.

An interactive website for analytical method comparison and bias estimation.

PubMed

Bahar, Burak; Tuncel, Ayse F; Holmes, Earle W; Holmes, Daniel T

2017-12-01

Regulatory standards mandate laboratories to perform studies to ensure accuracy and reliability of their test results. Method comparison and bias estimation are important components of these studies. We developed an interactive website for evaluating the relative performance of two analytical methods using R programming language tools. The website can be accessed at https://bahar.shinyapps.io/method_compare/. The site has an easy-to-use interface that allows both copy-pasting and manual entry of data. It also allows selection of a regression model and creation of regression and difference plots. Available regression models include Ordinary Least Squares, Weighted-Ordinary Least Squares, Deming, Weighted-Deming, Passing-Bablok and Passing-Bablok for large datasets. The server processes the data and generates downloadable reports in PDF or HTML format. Our website provides clinical laboratories a practical way to assess the relative performance of two analytical methods. Copyright © 2017 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Post-standardization of routine creatinine assays: are they suitable for clinical applications.

PubMed

Jassam, Nuthar; Weykamp, Cas; Thomas, Annette; Secchiero, Sandra; Sciacovelli, Laura; Plebani, Mario; Thelen, Marc; Cobbaert, Christa; Perich, Carmen; Ricós, Carmen; Paula, Faria A; Barth, Julian H

2017-05-01

Introduction Reliable serum creatinine measurements are of vital importance for the correct classification of chronic kidney disease and early identification of kidney injury. The National Kidney Disease Education Programme working group and other groups have defined clinically acceptable analytical limits for creatinine methods. The aim of this study was to re-evaluate the performance of routine creatinine methods in the light of these defined limits so as to assess their suitability for clinical practice. Method In collaboration with the Dutch External Quality Assurance scheme, six frozen commutable samples, with a creatinine concentration ranging from 80 to 239  μmol/L and traceable to isotope dilution mass spectrometry, were circulated to 91 laboratories in four European countries for creatinine measurement and estimated glomerular filtration rate calculation. Two out of the six samples were spiked with glucose to give high and low final concentrations of glucose. Results Results from 89 laboratories were analysed for bias, imprecision (%CV) for each creatinine assay and total error for estimated glomerular filtration rate. The participating laboratories used analytical instruments from four manufacturers; Abbott, Beckman, Roche and Siemens. All enzymatic methods in this study complied with the National Kidney Disease Education Programme working group recommended limits of bias of 5% above a creatinine concentration of 100  μmol/L. They also did not show any evidence of interference from glucose. In addition, they also showed compliance with the clinically recommended %CV of ≤4% across the analytical range. In contrast, the Jaffe methods showed variable performance with regard to the interference of glucose and unsatisfactory bias and precision. Conclusion Jaffe-based creatinine methods still exhibit considerable analytical variability in terms of bias, imprecision and lack of specificity, and this variability brings into question their clinical utility. We believe that clinical laboratories and manufacturers should work together to phase out the use of relatively non-specific Jaffe methods and replace them with more specific methods that are enzyme based.

New reporting procedures based on long-term method detection levels and some considerations for interpretations of water-quality data provided by the U.S. Geological Survey National Water Quality Laboratory

USGS Publications Warehouse

Childress, Carolyn J. Oblinger; Foreman, William T.; Connor, Brooke F.; Maloney, Thomas J.

1999-01-01

This report describes the U.S. Geological Survey National Water Quality Laboratory?s approach for determining long-term method detection levels and establishing reporting levels, details relevant new reporting conventions, and provides preliminary guidance on interpreting data reported with the new conventions. At the long-term method detection level concentration, the risk of a false positive detection (analyte reported present at the long-term method detection level when not in sample) is no more than 1 percent. However, at the long-term method detection level, the risk of a false negative occurrence (analyte reported not present when present at the long-term method detection level concentration) is up to 50 percent. Because this false negative rate is too high for use as a default 'less than' reporting level, a more reliable laboratory reporting level is set at twice the determined long-term method detection level. For all methods, concentrations measured between the laboratory reporting level and the long-term method detection level will be reported as estimated concentrations. Non-detections will be censored to the laboratory reporting level. Adoption of the new reporting conventions requires a full understanding of how low-concentration data can be used and interpreted and places responsibility for using and presenting final data with the user rather than with the laboratory. Users must consider that (1) new laboratory reporting levels may differ from previously established minimum reporting levels, (2) long-term method detection levels and laboratory reporting levels may change over time, and (3) estimated concentrations are less certain than concentrations reported above the laboratory reporting level. The availability of uncensored but qualified low-concentration data for interpretation and statistical analysis is a substantial benefit to the user. A decision to censor data after they are reported from the laboratory may still be made by the user, if merited, on the basis of the intended use of the data.

A Spectrophotometric Study of the Permanganate-Oxalate Reaction: An Analytical Laboratory Experiment

ERIC Educational Resources Information Center

Kalbus, Gene E.; Lieu, Van T.; Kalbus, Lee H.

2004-01-01

The spectrophotometric method assists in the study of potassium permanganate-oxalate reaction. Basic analytical techniques and rules are implemented in the experiment, which can also include the examination of other compounds oxidized by permanganate.

Laboratory Methods for the Measurement of Pollutants in Water and Waste Effluents

NASA Technical Reports Server (NTRS)

Ballinger, Dwight G.

1971-01-01

The requirement for accurate, precise, and rapid analytical procedures for the examination of water and waste samples requires the use of a variety of instruments. The instrumentation in water laboratories includes atomic absorption, UV-visible. and infrared spectrophotometers, automatic colorimetric analyzers, gas chromatographs and mass spectrometers. Because of the emphasis on regulatory action, attention is being directed toward quality control of analytical results. Among the challenging problems are the differentiation of metallic species in water at nanogram concentrations, rapid measurement of free cyanide and free ammonia, more sensitive methods for arsenic and selenium and improved characterization of organic contaminants.

A Lean Six Sigma approach to the improvement of the selenium analysis method.

PubMed

Cloete, Bronwyn C; Bester, André

2012-11-02

Reliable results represent the pinnacle assessment of quality of an analytical laboratory, and therefore variability is considered to be a critical quality problem associated with the selenium analysis method executed at Western Cape Provincial Veterinary Laboratory (WCPVL). The elimination and control of variability is undoubtedly of significant importance because of the narrow margin of safety between toxic and deficient doses of the trace element for good animal health. A quality methodology known as Lean Six Sigma was believed to present the most feasible solution for overcoming the adverse effect of variation, through steps towards analytical process improvement. Lean Six Sigma represents a form of scientific method type, which is empirical, inductive and deductive, and systematic, which relies on data, and is fact-based. The Lean Six Sigma methodology comprises five macro-phases, namely Define, Measure, Analyse, Improve and Control (DMAIC). Both qualitative and quantitative laboratory data were collected in terms of these phases. Qualitative data were collected by using quality-tools, namely an Ishikawa diagram, a Pareto chart, Kaizen analysis and a Failure Mode Effect analysis tool. Quantitative laboratory data, based on the analytical chemistry test method, were collected through a controlled experiment. The controlled experiment entailed 13 replicated runs of the selenium test method, whereby 11 samples were repetitively analysed, whilst Certified Reference Material (CRM) was also included in 6 of the runs. Laboratory results obtained from the controlled experiment was analysed by using statistical methods, commonly associated with quality validation of chemistry procedures. Analysis of both sets of data yielded an improved selenium analysis method, believed to provide greater reliability of results, in addition to a greatly reduced cycle time and superior control features. Lean Six Sigma may therefore be regarded as a valuable tool in any laboratory, and represents both a management discipline, and a standardised approach to problem solving and process optimisation.

Results of the International Energy Agency Round Robin on Fast Pyrolysis Bio-oil Production

DOE Office of Scientific and Technical Information (OSTI.GOV)

Elliott, Douglas C.; Meier, Dietrich; Oasmaa, Anja

An international round robin study of the production of fast pyrolysis bio-oil was undertaken. Fifteen institutions in six countries contributed. Three biomass samples were distributed to the laboratories for processing in fast pyrolysis reactors. Samples of the bio-oil produced were transported to a central analytical laboratory for analysis. The round robin was focused on validating the pyrolysis community understanding of production of fast pyrolysis bio-oil by providing a common feedstock for bio-oil preparation. The round robin included: •distribution of 3 feedstock samples from a common source to each participating laboratory; •preparation of fast pyrolysis bio-oil in each laboratory with themore » 3 feedstocks provided; •return of the 3 bio-oil products (minimum 500 ml) with operational description to a central analytical laboratory for bio-oil property determination. The analyses of interest were: density, viscosity, dissolved water, filterable solids, CHN, S, trace element analysis, ash, total acid number, pyrolytic lignin, and accelerated aging of bio-oil. In addition, an effort was made to compare the bio-oil components to the products of analytical pyrolysis through GC/MS analysis. The results showed that clear differences can occur in fast pyrolysis bio-oil properties by applying different reactor technologies or configurations. The comparison to analytical pyrolysis method suggested that Py-GC/MS could serve as a rapid screening method for bio-oil composition when produced in fluid-bed reactors. Furthermore, hot vapor filtration generally resulted in the most favorable bio-oil product, with respect to water, solids, viscosity, and total acid number. These results can be helpful in understanding the variation in bio-oil production methods and their effects on bio-oil product composition.« less

Category 1 external quality assessment program for serum creatinine.

PubMed

González-Lao, Elisabet; Díaz-Garzón, Jorge; Corte, Zoraida; Ricós, Carmen; Perich, Carmen; Álvarez, Virtudes; Simón, Margarita; Minchinela, Joana; García-Lario, José Vicente; Boned, Beatriz; Biosca, Carmen; Cava, Fernando; Fernández-Fernández, Pilar; Fernández-Calle, Pilar

2017-03-01

The Commission of Analytical Quality and the Committee of External Quality Programs of Spanish Society of Laboratory Medicine (SEQC) in collaboration with the Dutch Foundation for the Quality organized the first national category 1 External Quality Assessment Programs (EQAP) pilot study. The aim is to evaluate the standardization of serum creatinine measurements in the Spanish laboratories through a category 1 external quality assurance program with commutable material and reference method assigned values. A total of 87 Spanish laboratories were involved in this program in 2015. Each day a sample control was measured by duplicate during 6 consecutive days. Percentage deviations and coefficients of variation obtained were compared with quality specifications derived from biological variation. A total of 1044 creatinine results were obtained. Laboratories were coded in 11 different method-traceability combinations. Only enzymatic methods get all results within the acceptability limits. To participate in a category 1 EQAP is a valuable tool to assess the standardization degree in our country; a big effort should be made to promote laboratories to change their procedures and to use enzymatic creatinine methods, in order to achieve a satisfactory standardization degree for this important analyte.

Determination of steroid hormones and related compounds in filtered and unfiltered water by solid-phase extraction, derivatization, and gas chromatography with tandem mass spectrometry

USGS Publications Warehouse

Foreman, William T.; Gray, James L.; ReVello, Rhiannon C.; Lindley, Chris E.; Losche, Scott A.; Barber, Larry B.

2012-01-01

A new analytical method has been developed and implemented at the U.S. Geological Survey National Water Quality Laboratory that determines a suite of 20 steroid hormones and related compounds in filtered water (using laboratory schedule 2434) and in unfiltered water (using laboratory schedule 4434). This report documents the procedures and initial performance data for the method and provides guidance on application of the method and considerations of data quality in relation to data interpretation. The analytical method determines 6 natural and 3 synthetic estrogen compounds, 6 natural androgens, 1 natural and 1 synthetic progestin compound, and 2 sterols: cholesterol and 3--coprostanol. These two sterols have limited biological activity but typically are abundant in wastewater effluents and serve as useful tracers. Bisphenol A, an industrial chemical used primarily to produce polycarbonate plastic and epoxy resins and that has been shown to have estrogenic activity, also is determined by the method. A technique referred to as isotope-dilution quantification is used to improve quantitative accuracy by accounting for sample-specific procedural losses in the determined analyte concentration. Briefly, deuterium- or carbon-13-labeled isotope-dilution standards (IDSs), all of which are direct or chemically similar isotopic analogs of the method analytes, are added to all environmental and quality-control and quality-assurance samples before extraction. Method analytes and IDS compounds are isolated from filtered or unfiltered water by solid-phase extraction onto an octadecylsilyl disk, overlain with a graded glass-fiber filter to facilitate extraction of unfiltered sample matrices. The disks are eluted with methanol, and the extract is evaporated to dryness, reconstituted in solvent, passed through a Florisil solid-phase extraction column to remove polar organic interferences, and again evaporated to dryness in a reaction vial. The method compounds are reacted with activated -methyl--trimethylsilyl trifluoroacetamide at 65 degrees Celsius for 1 hour to form trimethylsilyl or trimethylsilyl-enol ether derivatives that are more amenable to gas chromatographic separation than the underivatized compounds. Analysis is carried out by gas chromatography with tandem mass spectrometry using calibration standards that are derivatized concurrently with the sample extracts. Analyte concentrations are quantified relative to specific IDS compounds in the sample, which directly compensate for procedural losses (incomplete recovery) in the determined and reported analyte concentrations. Thus, reported analyte concentrations (or analyte recoveries for spiked samples) are corrected based on recovery of the corresponding IDS compound during the quantification process. Recovery for each IDS compound is reported for each sample and represents an absolute recovery in a manner comparable to surrogate recoveries for other organic methods used by the National Water Quality Laboratory. Thus, IDS recoveries provide a useful tool for evaluating sample-specific analytical performance from an absolute mass recovery standpoint. IDS absolute recovery will differ and typically be lower than the corresponding analyte’s method recovery in spiked samples. However, additional correction of reported analyte concentrations is unnecessary and inappropriate because the analyte concentration (or recovery) already is compensated for by the isotope-dilution quantification procedure. Method analytes were spiked at 10 and 100 nanograms per liter (ng/L) for most analytes (10 times greater spike levels were used for bisphenol A and 100 times greater spike levels were used for 3--coprostanol and cholesterol) into the following validation-sample matrices: reagent water, wastewater-affected surface water, a secondary-treated wastewater effluent, and a primary (no biological treatment) wastewater effluent. Overall method recovery for all analytes in these matrices averaged 100 percent, with overall relative standard deviation of 28 percent. Mean recoveries of the 20 individual analytes for spiked reagent-water samples prepared along with field samples and analyzed in 2009–2010 ranged from 84–104 percent, with relative standard deviations of 6–36 percent. Concentrations for two analytes, equilin and progesterone, are reported as estimated because these analytes had excessive bias or variability, or both. Additional database coding is applied to other reported analyte data as needed, based on sample-specific IDS recovery performance. Detection levels were derived statistically by fortifying reagent water at six different levels (0.1 to 4 ng/L) and range from about 0.4 to 4 ng/L for 16 analytes. Interim reporting levels applied to analytes in this report range from 0.8 to 8 ng/L. Bisphenol A and the sterols (cholesterol and 3-beta-coprostanol) were consistently detected in laboratory and field blanks. The minimum reporting levels were set at 100 ng/L for bisphenol A and at 200 ng/L for the two sterols to prevent any bias associated with the presence of these compounds in the blanks. A minimum reporting level of 2 ng/L was set for 11-ketotestosterone to minimize false positive risk from an interfering siloxane compound emanating as chromatographic-column bleed, from vial septum material, or from other sources at no more than 1 ng/L.

21 CFR 118.8 - Testing methodology for Salmonella Enteritidis (SE).

Code of Federal Regulations, 2010 CFR

2010-04-01

... Salmonella Web site is located at http://www.fda.gov/Food/ScienceResearch/LaboratoryMethods/ucm114716.htm... you may examine a copy at the Center for Food Safety and Applied Nutrition's Library, 5100 Paint... Edition, is located at http://www.fda.gov/Food/ScienceResearch/LaboratoryMethods/BacteriologicalAnalytical...

Engineering of a miniaturized, robotic clinical laboratory

PubMed Central

Nourse, Marilyn B.; Engel, Kate; Anekal, Samartha G.; Bailey, Jocelyn A.; Bhatta, Pradeep; Bhave, Devayani P.; Chandrasekaran, Shekar; Chen, Yutao; Chow, Steven; Das, Ushati; Galil, Erez; Gong, Xinwei; Gessert, Steven F.; Ha, Kevin D.; Hu, Ran; Hyland, Laura; Jammalamadaka, Arvind; Jayasurya, Karthik; Kemp, Timothy M.; Kim, Andrew N.; Lee, Lucie S.; Liu, Yang Lily; Nguyen, Alphonso; O'Leary, Jared; Pangarkar, Chinmay H.; Patel, Paul J.; Quon, Ken; Ramachandran, Pradeep L.; Rappaport, Amy R.; Roy, Joy; Sapida, Jerald F.; Sergeev, Nikolay V.; Shee, Chandan; Shenoy, Renuka; Sivaraman, Sharada; Sosa‐Padilla, Bernardo; Tran, Lorraine; Trent, Amanda; Waggoner, Thomas C.; Wodziak, Dariusz; Yuan, Amy; Zhao, Peter; Holmes, Elizabeth A.

2018-01-01

Abstract The ability to perform laboratory testing near the patient and with smaller blood volumes would benefit patients and physicians alike. We describe our design of a miniaturized clinical laboratory system with three components: a hardware platform (ie, the miniLab) that performs preanalytical and analytical processing steps using miniaturized sample manipulation and detection modules, an assay‐configurable cartridge that provides consumable materials and assay reagents, and a server that communicates bidirectionally with the miniLab to manage assay‐specific protocols and analyze, store, and report results (i.e., the virtual analyzer). The miniLab can detect analytes in blood using multiple methods, including molecular diagnostics, immunoassays, clinical chemistry, and hematology. Analytical performance results show that our qualitative Zika virus assay has a limit of detection of 55 genomic copies/ml. For our anti‐herpes simplex virus type 2 immunoglobulin G, lipid panel, and lymphocyte subset panel assays, the miniLab has low imprecision, and method comparison results agree well with those from the United States Food and Drug Administration‐cleared devices. With its small footprint and versatility, the miniLab has the potential to provide testing of a range of analytes in decentralized locations. PMID:29376134

Engineering of a miniaturized, robotic clinical laboratory.

PubMed

Nourse, Marilyn B; Engel, Kate; Anekal, Samartha G; Bailey, Jocelyn A; Bhatta, Pradeep; Bhave, Devayani P; Chandrasekaran, Shekar; Chen, Yutao; Chow, Steven; Das, Ushati; Galil, Erez; Gong, Xinwei; Gessert, Steven F; Ha, Kevin D; Hu, Ran; Hyland, Laura; Jammalamadaka, Arvind; Jayasurya, Karthik; Kemp, Timothy M; Kim, Andrew N; Lee, Lucie S; Liu, Yang Lily; Nguyen, Alphonso; O'Leary, Jared; Pangarkar, Chinmay H; Patel, Paul J; Quon, Ken; Ramachandran, Pradeep L; Rappaport, Amy R; Roy, Joy; Sapida, Jerald F; Sergeev, Nikolay V; Shee, Chandan; Shenoy, Renuka; Sivaraman, Sharada; Sosa-Padilla, Bernardo; Tran, Lorraine; Trent, Amanda; Waggoner, Thomas C; Wodziak, Dariusz; Yuan, Amy; Zhao, Peter; Young, Daniel L; Robertson, Channing R; Holmes, Elizabeth A

2018-01-01

The ability to perform laboratory testing near the patient and with smaller blood volumes would benefit patients and physicians alike. We describe our design of a miniaturized clinical laboratory system with three components: a hardware platform (ie, the miniLab) that performs preanalytical and analytical processing steps using miniaturized sample manipulation and detection modules, an assay-configurable cartridge that provides consumable materials and assay reagents, and a server that communicates bidirectionally with the miniLab to manage assay-specific protocols and analyze, store, and report results (i.e., the virtual analyzer). The miniLab can detect analytes in blood using multiple methods, including molecular diagnostics, immunoassays, clinical chemistry, and hematology. Analytical performance results show that our qualitative Zika virus assay has a limit of detection of 55 genomic copies/ml. For our anti-herpes simplex virus type 2 immunoglobulin G, lipid panel, and lymphocyte subset panel assays, the miniLab has low imprecision, and method comparison results agree well with those from the United States Food and Drug Administration-cleared devices. With its small footprint and versatility, the miniLab has the potential to provide testing of a range of analytes in decentralized locations.

New insights into liquid chromatography for more eco-friendly analysis of pharmaceuticals.

PubMed

Shaaban, Heba

2016-10-01

Greening the analytical methods used for analysis of pharmaceuticals has been receiving great interest aimed at eliminating or minimizing the amount of organic solvents consumed daily worldwide without loss in chromatographic performance. Traditional analytical LC techniques employed in pharmaceutical analysis consume tremendous amounts of hazardous solvents and consequently generate large amounts of waste. The monetary and ecological impact of using large amounts of solvents and waste disposal motivated the analytical community to search for alternatives to replace polluting analytical methodologies with clean ones. In this context, implementing the principles of green analytical chemistry (GAC) in analytical laboratories is highly desired. This review gives a comprehensive overview on different green LC pathways for implementing GAC principles in analytical laboratories and focuses on evaluating the greenness of LC analytical procedures. This review presents green LC approaches for eco-friendly analysis of pharmaceuticals in industrial, biological, and environmental matrices. Graphical Abstract Green pathways of liquid chromatography for more eco-friendly analysis of pharmaceuticals.

National survey on intra-laboratory turnaround time for some most common routine and stat laboratory analyses in 479 laboratories in China

PubMed Central

Fei, Yang; Zeng, Rong; Wang, Wei; He, Falin; Zhong, Kun

2015-01-01

Introduction To investigate the state of the art of intra-laboratory turnaround time (intra-TAT), provide suggestions and find out whether laboratories accredited by International Organization for Standardization (ISO) 15189 or College of American Pathologists (CAP) will show better performance on intra-TAT than non-accredited ones. Materials and methods 479 Chinese clinical laboratories participating in the external quality assessment programs of chemistry, blood gas, and haematology tests organized by the National Centre for Clinical Laboratories in China were included in our study. General information and the median of intra-TAT of routine and stat tests in last one week were asked in the questionnaires. Results The response rate of clinical biochemistry, blood gas, and haematology testing were 36% (479 / 1307), 38% (228 / 598), and 36% (449 / 1250), respectively. More than 50% of laboratories indicated that they had set up intra-TAT median goals and almost 60% of laboratories declared they had monitored intra-TAT generally for every analyte they performed. Among all analytes we investigated, the intra-TAT of haematology analytes was shorter than biochemistry while the intra-TAT of blood gas analytes was the shortest. There were significant differences between median intra-TAT on different days of the week for routine tests. However, there were no significant differences in median intra-TAT reported by accredited laboratories and non-accredited laboratories. Conclusions Many laboratories in China are aware of intra-TAT control and are making effort to reach the target. There is still space for improvement. Accredited laboratories have better status on intra-TAT monitoring and target setting than the non-accredited, but there are no significant differences in median intra-TAT reported by them. PMID:26110033

Analytical control test plan and microbiological methods for the water recovery test

NASA Technical Reports Server (NTRS)

Traweek, M. S. (Editor); Tatara, J. D. (Editor)

1994-01-01

Qualitative and quantitative laboratory results are important to the decision-making process. In some cases, they may represent the only basis for deciding between two or more given options or processes. Therefore, it is essential that handling of laboratory samples and analytical operations employed are performed at a deliberate level of conscientious effort. Reporting erroneous results can lead to faulty interpretations and result in misinformed decisions. This document provides analytical control specifications which will govern future test procedures related to all Water Recovery Test (WRT) Phase 3 activities to be conducted at the National Aeronautics and Space Administration/Marshall Space Flight Center (NASA/MSFC). This document addresses the process which will be used to verify analytical data generated throughout the test period, and to identify responsibilities of key personnel and participating laboratories, the chains of communication to be followed, and ensure that approved methodology and procedures are used during WRT activities. This document does not outline specifics, but provides a minimum guideline by which sampling protocols, analysis methodologies, test site operations, and laboratory operations should be developed.

Food adulteration analysis without laboratory prepared or determined reference food adulterant values.

PubMed

Kalivas, John H; Georgiou, Constantinos A; Moira, Marianna; Tsafaras, Ilias; Petrakis, Eleftherios A; Mousdis, George A

2014-04-01

Quantitative analysis of food adulterants is an important health and economic issue that needs to be fast and simple. Spectroscopy has significantly reduced analysis time. However, still needed are preparations of analyte calibration samples matrix matched to prediction samples which can be laborious and costly. Reported in this paper is the application of a newly developed pure component Tikhonov regularization (PCTR) process that does not require laboratory prepared or reference analysis methods, and hence, is a greener calibration method. The PCTR method requires an analyte pure component spectrum and non-analyte spectra. As a food analysis example, synchronous fluorescence spectra of extra virgin olive oil samples adulterated with sunflower oil is used. Results are shown to be better than those obtained using ridge regression with reference calibration samples. The flexibility of PCTR allows including reference samples and is generic for use with other instrumental methods and food products. Copyright © 2013 Elsevier Ltd. All rights reserved.

Exhaled breath condensate – from an analytical point of view

PubMed Central

Dodig, Slavica; Čepelak, Ivana

2013-01-01

Over the past three decades, the goal of many researchers is analysis of exhaled breath condensate (EBC) as noninvasively obtained sample. A total quality in laboratory diagnostic processes in EBC analysis was investigated: pre-analytical (formation, collection, storage of EBC), analytical (sensitivity of applied methods, standardization) and post-analytical (interpretation of results) phases. EBC analysis is still used as a research tool. Limitations referred to pre-analytical, analytical, and post-analytical phases of EBC analysis are numerous, e.g. low concentrations of EBC constituents, single-analyte methods lack in sensitivity, and multi-analyte has not been fully explored, and reference values are not established. When all, pre-analytical, analytical and post-analytical requirements are met, EBC biomarkers as well as biomarker patterns can be selected and EBC analysis can hopefully be used in clinical practice, in both, the diagnosis and in the longitudinal follow-up of patients, resulting in better outcome of disease. PMID:24266297

Low-Cost Method for Quantifying Sodium in Coconut Water and Seawater for the Undergraduate Analytical Chemistry Laboratory: Flame Test, a Mobile Phone Camera, and Image Processing

ERIC Educational Resources Information Center

Moraes, Edgar P.; da Silva, Nilbert S. A.; de Morais, Camilo de L. M.; das Neves, Luiz S.; de Lima, Kassio M. G.

2014-01-01

The flame test is a classical analytical method that is often used to teach students how to identify specific metals. However, some universities in developing countries have difficulties acquiring the sophisticated instrumentation needed to demonstrate how to identify and quantify metals. In this context, a method was developed based on the flame…

Extracting laboratory test information from biomedical text

PubMed Central

Kang, Yanna Shen; Kayaalp, Mehmet

2013-01-01

Background: No previous study reported the efficacy of current natural language processing (NLP) methods for extracting laboratory test information from narrative documents. This study investigates the pathology informatics question of how accurately such information can be extracted from text with the current tools and techniques, especially machine learning and symbolic NLP methods. The study data came from a text corpus maintained by the U.S. Food and Drug Administration, containing a rich set of information on laboratory tests and test devices. Methods: The authors developed a symbolic information extraction (SIE) system to extract device and test specific information about four types of laboratory test entities: Specimens, analytes, units of measures and detection limits. They compared the performance of SIE and three prominent machine learning based NLP systems, LingPipe, GATE and BANNER, each implementing a distinct supervised machine learning method, hidden Markov models, support vector machines and conditional random fields, respectively. Results: Machine learning systems recognized laboratory test entities with moderately high recall, but low precision rates. Their recall rates were relatively higher when the number of distinct entity values (e.g., the spectrum of specimens) was very limited or when lexical morphology of the entity was distinctive (as in units of measures), yet SIE outperformed them with statistically significant margins on extracting specimen, analyte and detection limit information in both precision and F-measure. Its high recall performance was statistically significant on analyte information extraction. Conclusions: Despite its shortcomings against machine learning methods, a well-tailored symbolic system may better discern relevancy among a pile of information of the same type and may outperform a machine learning system by tapping into lexically non-local contextual information such as the document structure. PMID:24083058

EPA Region 6 Laboratory Method Specific Analytical Capabilities with Sample Concentration Range

EPA Pesticide Factsheets

EPA Region 6 Environmental Services Branch (ESB) Laboratory is capable of analyzing a wide range of samples with concentrations ranging for low part-per trillion (ppt) to low percent () levels, depending on the sample matrix.

Transfer of analytical procedures: a panel of strategies selected for risk management, with emphasis on an integrated equivalence-based comparative testing approach.

PubMed

Agut, C; Caron, A; Giordano, C; Hoffman, D; Ségalini, A

2011-09-10

In 2001, a multidisciplinary team made of analytical scientists and statisticians at Sanofi-aventis has published a methodology which has governed, from that time, the transfers from R&D sites to Manufacturing sites of the release monographs. This article provides an overview of the recent adaptations brought to this original methodology taking advantage of our experience and the new regulatory framework, and, in particular, the risk management perspective introduced by ICH Q9. Although some alternate strategies have been introduced in our practices, the comparative testing one, based equivalence testing as statistical approach, remains the standard for assays lying on very critical quality attributes. This is conducted with the concern to control the most important consumer's risk involved at two levels in analytical decisions in the frame of transfer studies: risk, for the receiving laboratory, to take poor release decisions with the analytical method and risk, for the sending laboratory, to accredit such a receiving laboratory on account of its insufficient performances with the method. Among the enhancements to the comparative studies, the manuscript presents the process settled within our company for a better integration of the transfer study into the method life-cycle, just as proposals of generic acceptance criteria and designs for assay and related substances methods. While maintaining rigor and selectivity of the original approach, these improvements tend towards an increased efficiency in the transfer operations. Copyright © 2011 Elsevier B.V. All rights reserved.

3D-MICE: integration of cross-sectional and longitudinal imputation for multi-analyte longitudinal clinical data.

PubMed

Luo, Yuan; Szolovits, Peter; Dighe, Anand S; Baron, Jason M

2018-06-01

A key challenge in clinical data mining is that most clinical datasets contain missing data. Since many commonly used machine learning algorithms require complete datasets (no missing data), clinical analytic approaches often entail an imputation procedure to "fill in" missing data. However, although most clinical datasets contain a temporal component, most commonly used imputation methods do not adequately accommodate longitudinal time-based data. We sought to develop a new imputation algorithm, 3-dimensional multiple imputation with chained equations (3D-MICE), that can perform accurate imputation of missing clinical time series data. We extracted clinical laboratory test results for 13 commonly measured analytes (clinical laboratory tests). We imputed missing test results for the 13 analytes using 3 imputation methods: multiple imputation with chained equations (MICE), Gaussian process (GP), and 3D-MICE. 3D-MICE utilizes both MICE and GP imputation to integrate cross-sectional and longitudinal information. To evaluate imputation method performance, we randomly masked selected test results and imputed these masked results alongside results missing from our original data. We compared predicted results to measured results for masked data points. 3D-MICE performed significantly better than MICE and GP-based imputation in a composite of all 13 analytes, predicting missing results with a normalized root-mean-square error of 0.342, compared to 0.373 for MICE alone and 0.358 for GP alone. 3D-MICE offers a novel and practical approach to imputing clinical laboratory time series data. 3D-MICE may provide an additional tool for use as a foundation in clinical predictive analytics and intelligent clinical decision support.

40 CFR 408.61 - Specialized definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... components of a waste water amenable to measurement by the method described in Methods for Chemical Analysis of Water and Wastes, 1971, Environmental Protection Agency, Analytical Quality Control Laboratory...

40 CFR 408.71 - Specialized definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... waste water amenable to measurement by the method described in Methods for Chemical Analysis of Water and Wastes, 1971, Environmental Protection Agency, Analytical Quality Control Laboratory, page 217. (c...

40 CFR 408.81 - Specialized definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... components of a waste water amendable to measurement by the method described in Methods for Chemical Analysis of Water and Wastes, 1971, Environmental Protection Agency, Analytical Quality Control Laboratory...

Empirical insights and considerations for the OBT inter-laboratory comparison of environmental samples.

PubMed

Kim, Sang-Bog; Roche, Jennifer

2013-08-01

Organically bound tritium (OBT) is an important tritium species that can be measured in most environmental samples, but has only recently been recognized as a species of tritium in these samples. Currently, OBT is not routinely measured by environmental monitoring laboratories around the world. There are no certified reference materials (CRMs) for environmental samples. Thus, quality assurance (QA), or verification of the accuracy of the OBT measurement, is not possible. Alternatively, quality control (QC), or verification of the precision of the OBT measurement, can be achieved. In the past, there have been differences in OBT analysis results between environmental laboratories. A possible reason for the discrepancies may be differences in analytical methods. Therefore, inter-laboratory OBT comparisons among the environmental laboratories are important and would provide a good opportunity for adopting a reference OBT analytical procedure. Due to the analytical issues, only limited information is available on OBT measurement. Previously conducted OBT inter-laboratory practices are reviewed and the findings are described. Based on our experiences, a few considerations were suggested for the international OBT inter-laboratory comparison exercise to be completed in the near future. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

The work of the European Union Reference Laboratory for Food Additives (EURL) and its support for the authorisation process of feed additives in the European Union: a review

PubMed Central

von Holst, Christoph; Robouch, Piotr; Bellorini, Stefano; de la Huebra, María José González; Ezerskis, Zigmas

2016-01-01

ABSTRACT This paper describes the operation of the European Union Reference Laboratory for Feed Additives (EURL) and its role in the authorisation procedure of feed additives in the European Union. Feed additives are authorised according to Regulation (EC) No. 1831/2003, which introduced a completely revised authorisation procedure and also established the EURL. The regulations authorising feed additives contain conditions of use such as legal limits of the feed additives, which require the availability of a suitable method of analysis for official control purposes under real world conditions. It is the task of the EURL to evaluate the suitability of analytical methods as proposed by the industry for this purpose. Moreover, the paper shows that one of the major challenges is the huge variety of the methodology applied in feed additive analysis, thus requiring expertise in quite different analytical areas. In order to cope with this challenge, the EURL is supported by a network of national reference laboratories (NRLs) and only the merged knowledge of all NRLs allows for a scientifically sound assessment of the analytical methods. PMID:26540604

Determination of Calcium in Dietary Supplements: Statistical Comparison of Methods in the Analytical Laboratory

ERIC Educational Resources Information Center

Garvey, Sarah L.; Shahmohammadi, Golbon; McLain, Derek R.; Dietz, Mark L.

2015-01-01

A laboratory experiment is described in which students compare two methods for the determination of the calcium content of commercial dietary supplement tablets. In a two-week sequence, the sample tablets are first analyzed via complexometric titration with ethylenediaminetetraacetic acid and then, following ion exchange of the calcium ion present…

Creating and Evaluating a Hypertext System of Documenting Analytical Test Methods in a Chemical Plant Quality Assurance Laboratory.

ERIC Educational Resources Information Center

White, Charles E., Jr.

The purpose of this study was to develop and implement a hypertext documentation system in an industrial laboratory and to evaluate its usefulness by participative observation and a questionnaire. Existing word-processing test method documentation was converted directly into a hypertext format or "hyperdocument." The hyperdocument was designed and…

40 CFR 417.191 - Specialized definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... methylene blue active substances amenable to measurement by the method described in “Methods for Chemical Analysis of Water and Wastes,” 1971, Environmental Protection Agency, Analytical Quality Control Laboratory...

EPA/ORD NATIONAL EXPOSURE RESEARCH LABORATORY MEASUREMENT SCIENCE SUPPORT FOR HOMELAND SECURITY

EPA Science Inventory

This product describes the National Exposure Research Laboratory research and development support for homeland security through the proposed National Exposure Measurements Center (NEMC). Key NEMC functional areas depicted in this poster are: standardized analytical method develo...

Sigma metrics as a tool for evaluating the performance of internal quality control in a clinical chemistry laboratory

PubMed Central

Kumar, B. Vinodh; Mohan, Thuthi

2018-01-01

OBJECTIVE: Six Sigma is one of the most popular quality management system tools employed for process improvement. The Six Sigma methods are usually applied when the outcome of the process can be measured. This study was done to assess the performance of individual biochemical parameters on a Sigma Scale by calculating the sigma metrics for individual parameters and to follow the Westgard guidelines for appropriate Westgard rules and levels of internal quality control (IQC) that needs to be processed to improve target analyte performance based on the sigma metrics. MATERIALS AND METHODS: This is a retrospective study, and data required for the study were extracted between July 2015 and June 2016 from a Secondary Care Government Hospital, Chennai. The data obtained for the study are IQC - coefficient of variation percentage and External Quality Assurance Scheme (EQAS) - Bias% for 16 biochemical parameters. RESULTS: For the level 1 IQC, four analytes (alkaline phosphatase, magnesium, triglyceride, and high-density lipoprotein-cholesterol) showed an ideal performance of ≥6 sigma level, five analytes (urea, total bilirubin, albumin, cholesterol, and potassium) showed an average performance of <3 sigma level and for level 2 IQCs, same four analytes of level 1 showed a performance of ≥6 sigma level, and four analytes (urea, albumin, cholesterol, and potassium) showed an average performance of <3 sigma level. For all analytes <6 sigma level, the quality goal index (QGI) was <0.8 indicating the area requiring improvement to be imprecision except cholesterol whose QGI >1.2 indicated inaccuracy. CONCLUSION: This study shows that sigma metrics is a good quality tool to assess the analytical performance of a clinical chemistry laboratory. Thus, sigma metric analysis provides a benchmark for the laboratory to design a protocol for IQC, address poor assay performance, and assess the efficiency of existing laboratory processes. PMID:29692587

Reproducibility of risk figures in 2nd-trimester maternal serum screening for down syndrome: comparison of 2 laboratories.

PubMed

Benn, Peter A; Makowski, Gregory S; Egan, James F X; Wright, Dave

2006-11-01

Analytical error affects 2nd-trimester maternal serum screening for Down syndrome risk estimation. We analyzed the between-laboratory reproducibility of risk estimates from 2 laboratories. Laboratory 1 used Bayer ACS180 immunoassays for alpha-fetoprotein (AFP) and human chorionic gonadotropin (hCG), Diagnostic Systems Laboratories (DSL) RIA for unconjugated estriol (uE3), and DSL enzyme immunoassay for inhibin-A (INH-A). Laboratory 2 used Beckman immunoassays for AFP, hCG, and uE3, and DSL enzyme immunoassay for INH-A. Analyte medians were separately established for each laboratory. We used the same computational algorithm for all risk calculations, and we used Monte Carlo methods for computer modeling. For 462 samples tested, risk figures from the 2 laboratories differed >2-fold for 44.7%, >5-fold for 7.1%, and >10-fold for 1.7%. Between-laboratory differences in analytes were greatest for uE3 and INH-A. The screen-positive rates were 9.3% for laboratory 1 and 11.5% for laboratory 2, with a significant difference in the patients identified as screen-positive vs screen-negative (McNemar test, P<0.001). Computer modeling confirmed the large between-laboratory risk differences. Differences in performance of assays and laboratory procedures can have a large effect on patient-specific risks. Screening laboratories should minimize test imprecision and ensure that each assay performs in a manner similar to that assumed in the risk computational algorithm.

Initial interlaboratory validation of an analytical method for the determination of lead in canned tuna to be used for monitoring and regulatory purposes.

PubMed

Santiago, E C; Bello, F B B

2003-06-01

The Association of Official Analytical Chemists (AOAC) Standard Method 972.23 (dry ashing and flame atomic absorption spectrophotometry (FAAS)), applied to the analysis of lead in tuna, was validated in three selected local laboratories to determine the acceptability of the method to both the Codex Alimentarius Commission (Codex) and the European Union (EU) Commission for monitoring lead in canned tuna. Initial validation showed that the standard AOAC method as performed in the three participating laboratories cannot satisfy the Codex/EU proposed criteria for the method detection limit for monitoring lead in fish at the present regulation level of 0.5 mg x kg(-1). Modification of the standard method by chelation/concentration of the digest solution before FAAS analysis showed that the modified method has the potential to meet Codex/EU criteria on sensitivity, accuracy and precision at the specified regulation level.

Expansion of the Scope of AOAC First Action Method 2012.25--Single-Laboratory Validation of Triphenylmethane Dye and Leuco Metabolite Analysis in Shrimp, Tilapia, Catfish, and Salmon by LC-MS/MS.

PubMed

Andersen, Wendy C; Casey, Christine R; Schneider, Marilyn J; Turnipseed, Sherri B

2015-01-01

Prior to conducting a collaborative study of AOAC First Action 2012.25 LC-MS/MS analytical method for the determination of residues of three triphenylmethane dyes (malachite green, crystal violet, and brilliant green) and their metabolites (leucomalachite green and leucocrystal violet) in seafood, a single-laboratory validation of method 2012.25 was performed to expand the scope of the method to other seafood matrixes including salmon, catfish, tilapia, and shrimp. The validation included the analysis of fortified and incurred residues over multiple weeks to assess analyte stability in matrix at -80°C, a comparison of calibration methods over the range 0.25 to 4 μg/kg, study of matrix effects for analyte quantification, and qualitative identification of targeted analytes. Method accuracy ranged from 88 to 112% with 13% RSD or less for samples fortified at 0.5, 1.0, and 2.0 μg/kg. Analyte identification and determination limits were determined by procedures recommended both by the U. S. Food and Drug Administration and the European Commission. Method detection limits and decision limits ranged from 0.05 to 0.24 μg/kg and 0.08 to 0.54 μg/kg, respectively. AOAC First Action Method 2012.25 with an extracted matrix calibration curve and internal standard correction is suitable for the determination of triphenylmethane dyes and leuco metabolites in salmon, catfish, tilapia, and shrimp by LC-MS/MS at a residue determination level of 0.5 μg/kg or below.

40 CFR Appendix G to Subpart A of... - UNEP Recommendations for Conditions Applied to Exemption for Essential Laboratory and Analytical...

Code of Federal Regulations, 2013 CFR

2013-07-01

... and laboratory purposes. Pursuant to Decision XI/15 of the Parties to the Montreal Protocol, effective... laboratory and analytical purposes is authorized provided that these laboratory and analytical chemicals..., restricted to laboratory use and analytical purposes and specifying that used or surplus substances should be...

40 CFR Appendix G to Subpart A of... - UNEP Recommendations for Conditions Applied to Exemption for Essential Laboratory and Analytical...

Code of Federal Regulations, 2010 CFR

2010-07-01

... and laboratory purposes. Pursuant to Decision XI/15 of the Parties to the Montreal Protocol, effective... laboratory and analytical purposes is authorized provided that these laboratory and analytical chemicals..., restricted to laboratory use and analytical purposes and specifying that used or surplus substances should be...

40 CFR Appendix G to Subpart A of... - UNEP Recommendations for Conditions Applied to Exemption for Essential Laboratory and Analytical...

Code of Federal Regulations, 2014 CFR

2014-07-01

... and laboratory purposes. Pursuant to Decision XI/15 of the Parties to the Montreal Protocol, effective... laboratory and analytical purposes is authorized provided that these laboratory and analytical chemicals..., restricted to laboratory use and analytical purposes and specifying that used or surplus substances should be...

40 CFR Appendix G to Subpart A of... - UNEP Recommendations for Conditions Applied to Exemption for Essential Laboratory and Analytical...

Code of Federal Regulations, 2012 CFR

2012-07-01

... and laboratory purposes. Pursuant to Decision XI/15 of the Parties to the Montreal Protocol, effective... laboratory and analytical purposes is authorized provided that these laboratory and analytical chemicals..., restricted to laboratory use and analytical purposes and specifying that used or surplus substances should be...

40 CFR Appendix G to Subpart A of... - UNEP Recommendations for Conditions Applied to Exemption for Essential Laboratory and Analytical...

Code of Federal Regulations, 2011 CFR

2011-07-01

... and laboratory purposes. Pursuant to Decision XI/15 of the Parties to the Montreal Protocol, effective... laboratory and analytical purposes is authorized provided that these laboratory and analytical chemicals..., restricted to laboratory use and analytical purposes and specifying that used or surplus substances should be...

Clinical laboratory analytics: Challenges and promise for an emerging discipline.

PubMed

Shirts, Brian H; Jackson, Brian R; Baird, Geoffrey S; Baron, Jason M; Clements, Bryan; Grisson, Ricky; Hauser, Ronald George; Taylor, Julie R; Terrazas, Enrique; Brimhall, Brad

2015-01-01

The clinical laboratory is a major source of health care data. Increasingly these data are being integrated with other data to inform health system-wide actions meant to improve diagnostic test utilization, service efficiency, and "meaningful use." The Academy of Clinical Laboratory Physicians and Scientists hosted a satellite meeting on clinical laboratory analytics in conjunction with their annual meeting on May 29, 2014 in San Francisco. There were 80 registrants for the clinical laboratory analytics meeting. The meeting featured short presentations on current trends in clinical laboratory analytics and several panel discussions on data science in laboratory medicine, laboratory data and its role in the larger healthcare system, integrating laboratory analytics, and data sharing for collaborative analytics. One main goal of meeting was to have an open forum of leaders that work with the "big data" clinical laboratories produce. This article summarizes the proceedings of the meeting and content discussed.

Clinical laboratory analytics: Challenges and promise for an emerging discipline

PubMed Central

Shirts, Brian H.; Jackson, Brian R.; Baird, Geoffrey S.; Baron, Jason M.; Clements, Bryan; Grisson, Ricky; Hauser, Ronald George; Taylor, Julie R.; Terrazas, Enrique; Brimhall, Brad

2015-01-01

The clinical laboratory is a major source of health care data. Increasingly these data are being integrated with other data to inform health system-wide actions meant to improve diagnostic test utilization, service efficiency, and “meaningful use.” The Academy of Clinical Laboratory Physicians and Scientists hosted a satellite meeting on clinical laboratory analytics in conjunction with their annual meeting on May 29, 2014 in San Francisco. There were 80 registrants for the clinical laboratory analytics meeting. The meeting featured short presentations on current trends in clinical laboratory analytics and several panel discussions on data science in laboratory medicine, laboratory data and its role in the larger healthcare system, integrating laboratory analytics, and data sharing for collaborative analytics. One main goal of meeting was to have an open forum of leaders that work with the “big data” clinical laboratories produce. This article summarizes the proceedings of the meeting and content discussed. PMID:25774320

The Hazardous-Drums Project: A Multiweek Laboratory Exercise for General Chemistry Involving Environmental, Quality Control, and Cost Evaluation

ERIC Educational Resources Information Center

Hayes, David; Widanski, Bozena

2013-01-01

A laboratory experiment is described that introduces students to "real-world" hazardous waste management issues chemists face. The students are required to define an analytical problem, choose a laboratory analysis method, investigate cost factors, consider quality-control issues, interpret the meaning of results, and provide management…

Overview of mycotoxin methods, present status and future needs.

PubMed

Gilbert, J

1999-01-01

This article reviews current requirements for the analysis for mycotoxins in foods and identifies legislative as well as other factors that are driving development and validation of new methods. New regulatory limits for mycotoxins and analytical quality assurance requirements for laboratories to only use validated methods are seen as major factors driving developments. Three major classes of methods are identified which serve different purposes and can be categorized as screening, official and research. In each case the present status and future needs are assessed. In addition to an overview of trends in analytical methods, some other areas of analytical quality assurance such as participation in proficiency testing and reference materials are identified.

Improvement of analytical capabilities of neutron activation analysis laboratory at the Colombian Geological Survey

NASA Astrophysics Data System (ADS)

Parrado, G.; Cañón, Y.; Peña, M.; Sierra, O.; Porras, A.; Alonso, D.; Herrera, D. C.; Orozco, J.

2016-07-01

The Neutron Activation Analysis (NAA) laboratory at the Colombian Geological Survey has developed a technique for multi-elemental analysis of soil and plant matrices, based on Instrumental Neutron Activation Analysis (INAA) using the comparator method. In order to evaluate the analytical capabilities of the technique, the laboratory has been participating in inter-comparison tests organized by Wepal (Wageningen Evaluating Programs for Analytical Laboratories). In this work, the experimental procedure and results for the multi-elemental analysis of four soil and four plant samples during participation in the first round on 2015 of Wepal proficiency test are presented. Only elements with radioactive isotopes with medium and long half-lives have been evaluated, 15 elements for soils (As, Ce, Co, Cr, Cs, Fe, K, La, Na, Rb, Sb, Sc, Th, U and Zn) and 7 elements for plants (Br, Co, Cr, Fe, K, Na and Zn). The performance assessment by Wepal based on Z-score distributions showed that most results obtained |Z-scores| ≤ 3.

Microbiological methods for the water recovery systems test, revision 1.1

NASA Technical Reports Server (NTRS)

Rhoads, Tim; Kilgore, M. V., Jr.; Mikell, A. T., Jr.

1990-01-01

Current microbiological parameters specified to verify microbiological quality of Space Station Freedom water quality include the enumeration of total bacteria, anaerobes, aerobes, yeasts and molds, enteric bacteria, gram positives, gram negatives, and E. coli. In addition, other parameters have been identified as necessary to support the Water Recovery Test activities to be conducted at the NASA/MSFC later this year. These other parameters include aerotolerant eutrophic mesophiles, legionellae, and an additional method for heterotrophic bacteria. If inter-laboratory data are to be compared to evaluate quality, analytical methods must be eliminated as a variable. Therefore, each participating laboratory must utilize the same analytical methods and procedures. Without this standardization, data can be neither compared nor validated between laboratories. Multiple laboratory participation represents a conservative approach to insure quality and completeness of data. Invariably, sample loss will occur in transport and analyses. Natural variance is a reality on any test of this magnitude and is further enhanced because biological entities, capable of growth and death, are specific parameters of interest. The large variation due to the participation of human test subjects has been noted with previous testing. The resultant data might be dismissed as 'out of control' unless intra-laboratory control is included as part of the method or if participating laboratories are not available for verification. The purpose of this document is to provide standardized laboratory procedures for the enumeration of certain microorganisms in water and wastewater specific to the water recovery systems test. The document consists of ten separate cultural methods and one direct count procedure. It is not intended nor is it implied to be a complete microbiological methods manual.

A transient laboratory method for determining the hydraulic properties of 'tight' rocks-I. Theory

USGS Publications Warehouse

Hsieh, P.A.; Tracy, J.V.; Neuzil, C.E.; Bredehoeft, J.D.; Silliman, Stephen E.

1981-01-01

Transient pulse testing has been employed increasingly in the laboratory to measure the hydraulic properties of rock samples with low permeability. Several investigators have proposed a mathematical model in terms of an initial-boundary value problem to describe fluid flow in a transient pulse test. However, the solution of this problem has not been available. In analyzing data from the transient pulse test, previous investigators have either employed analytical solutions that are derived with the use of additional, restrictive assumptions, or have resorted to numerical methods. In Part I of this paper, a general, analytical solution for the transient pulse test is presented. This solution is graphically illustrated by plots of dimensionless variables for several cases of interest. The solution is shown to contain, as limiting cases, the more restrictive analytical solutions that the previous investigators have derived. A method of computing both the permeability and specific storage of the test sample from experimental data will be presented in Part II. ?? 1981.

Importance of implementing an analytical quality control system in a core laboratory.

PubMed

Marques-Garcia, F; Garcia-Codesal, M F; Caro-Narros, M R; Contreras-SanFeliciano, T

2015-01-01

The aim of the clinical laboratory is to provide useful information for screening, diagnosis and monitoring of disease. The laboratory should ensure the quality of extra-analytical and analytical process, based on set criteria. To do this, it develops and implements a system of internal quality control, designed to detect errors, and compare its data with other laboratories, through external quality control. In this way it has a tool to detect the fulfillment of the objectives set, and in case of errors, allowing corrective actions to be made, and ensure the reliability of the results. This article sets out to describe the design and implementation of an internal quality control protocol, as well as its periodical assessment intervals (6 months) to determine compliance with pre-determined specifications (Stockholm Consensus(1)). A total of 40 biochemical and 15 immunochemical methods were evaluated using three different control materials. Next, a standard operation procedure was planned to develop a system of internal quality control that included calculating the error of the analytical process, setting quality specifications, and verifying compliance. The quality control data were then statistically depicted as means, standard deviations, and coefficients of variation, as well as systematic, random, and total errors. The quality specifications were then fixed and the operational rules to apply in the analytical process were calculated. Finally, our data were compared with those of other laboratories through an external quality assurance program. The development of an analytical quality control system is a highly structured process. This should be designed to detect errors that compromise the stability of the analytical process. The laboratory should review its quality indicators, systematic, random and total error at regular intervals, in order to ensure that they are meeting pre-determined specifications, and if not, apply the appropriate corrective actions. Copyright © 2015 SECA. Published by Elsevier Espana. All rights reserved.

Analysis of Whiskey by Dispersive Liquid-Liquid Microextraction Coupled with Gas Chromatography/Mass Spectrometry: An Upper Division Analytical Chemistry Experiment Guided by Green Chemistry

ERIC Educational Resources Information Center

Owens, Janel E.; Zimmerman, Laura B.; Gardner, Michael A.; Lowe, Luis E.

2016-01-01

Analysis of whiskey samples prepared by a green microextraction technique, dispersive liquid-liquid microextraction (DLLME), before analysis by a qualitative gas chromatography-mass spectrometry (GC/MS) method, is described as a laboratory experiment for an upper division instrumental methods of analysis laboratory course. Here, aroma compounds in…

Rapid fusion method for the determination of refractory thorium and uranium isotopes in soil samples

DOE PAGES

Maxwell, Sherrod L.; Hutchison, Jay B.; McAlister, Daniel R.

2015-02-14

Recently, approximately 80% of participating laboratories failed to accurately determine uranium isotopes in soil samples in the U.S Department of Energy Mixed Analyte Performance Evaluation Program (MAPEP) Session 30, due to incomplete dissolution of refractory particles in the samples. Failing laboratories employed acid dissolution methods, including hydrofluoric acid, to recover uranium from the soil matrix. The failures illustrate the importance of rugged soil dissolution methods for the accurate measurement of analytes in the sample matrix. A new rapid fusion method has been developed by the Savannah River National Laboratory (SRNL) to prepare 1-2 g soil sample aliquots very quickly, withmore » total dissolution of refractory particles. Soil samples are fused with sodium hydroxide at 600 ºC in zirconium crucibles to enable complete dissolution of the sample. Uranium and thorium are separated on stacked TEVA and TRU extraction chromatographic resin cartridges, prior to isotopic measurements by alpha spectrometry on cerium fluoride microprecipitation sources. Plutonium can also be separated and measured using this method. Batches of 12 samples can be prepared for measurement in <5 hours.« less

Comparison of Enzymatic Assay for HBA1C Measurement (Abbott Architect) With Capillary Electrophoresis (Sebia Minicap Flex Piercing Analyser).

PubMed

Tesija Kuna, Andrea; Dukic, Kristina; Nikolac Gabaj, Nora; Miler, Marijana; Vukasovic, Ines; Langer, Sanja; Simundic, Ana-Maria; Vrkic, Nada

2018-03-08

To compare the analytical performances of the enzymatic method (EM) and capillary electrophoresis (CE) for hemoglobin A1c (HbA1c) measurement. Imprecision, carryover, stability, linearity, method comparison, and interferences were evaluated for HbA1c via EM (Abbott Laboratories, Inc) and CE (Sebia). Both methods have shown overall within-laboratory imprecision of less than 3% for International Federation of Clinical Chemistry and Laboratory Medicine (IFCC) units (<2% National Glycohemoglobin Standardization Program [NGSP] units). Carryover effects were within acceptable criteria. The linearity of both methods has proven to be excellent (R2 = 0.999). Significant proportional and constant difference were found for EM, compared with CE, but were not clinically relevant (<5 mmol/mol; NGSP <0.5%). At the clinically relevant HbA1c concentration, stability observed with both methods was acceptable (bias, <3%). Triglyceride levels of 8.11 mmol per L or greater showed to interfere with EM and fetal hemoglobin (HbF) of 10.6% or greater with CE. The enzymatic method proved to be comparable to the CE method in analytical performances; however, certain interferences can influence the measurements of each method.

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J. Michael

2000-01-01

A microchip laboratory system and method provide fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel.

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J. Michael

2000-01-01

A microchip laboratory system and method proved fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel.

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J. Michael

2002-01-01

A microchip laboratory system and method provide fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel.

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J. Michael

1999-01-01

A microchip laboratory system and method provide fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel.

Apparatus and method for performing microfluidic manipulations for chemical analysis and synthesis

DOEpatents

Ramsey, J.M.

1999-01-12

A microchip laboratory system and method provide fluid manipulations for a variety of applications, including sample injection for microchip chemical separations. The microchip is fabricated using standard photolithographic procedures and chemical wet etching, with the substrate and cover plate joined using direct bonding. Capillary electrophoresis and electrochromatography are performed in channels formed in the substrate. Analytes are loaded into a four-way intersection of channels by electrokinetically pumping the analyte through the intersection, followed by switching of the potentials to force an analyte plug into the separation channel. 46 figs.

Complexometric Determination of Mercury Based on a Selective Masking Reaction

ERIC Educational Resources Information Center

Romero, Mercedes; Guidi, Veronica; Ibarrolaza, Agustin; Castells, Cecilia

2009-01-01

In the first analytical chemistry course, students are introduced to the concepts of equilibrium in water solutions and classical (non-instrumental) analytical methods. Our teaching experience shows that "real samples" stimulate students' enthusiasm for the laboratory work. From this diagnostic, we implemented an optional activity at the end of…

Keeping It Simple: Can We Estimate Malting Quality Potential Using an Isothermal Mashing Protocol and Common Laboratory Instrumentation?

USDA-ARS?s Scientific Manuscript database

Current methods for generating malting quality metrics have been developed largely to support commercial malting and brewing operations, providing accurate, reproducible analytical data to guide malting and brewing production. Infrastructure to support these analytical operations often involves sub...

Protein Quantification by Elemental Mass Spectrometry: An Experiment for Graduate Students

ERIC Educational Resources Information Center

Schwarz, Gunnar; Ickert, Stefanie; Wegner, Nina; Nehring, Andreas; Beck, Sebastian; Tiemann, Ruediger; Linscheid, Michael W.

2014-01-01

A multiday laboratory experiment was designed to integrate inductively coupled plasma-mass spectrometry (ICP-MS) in the context of protein quantification into an advanced practical course in analytical and environmental chemistry. Graduate students were familiar with the analytical methods employed, whereas the combination of bioanalytical assays…

A Field Study Program in Analytical Chemistry for College Seniors.

ERIC Educational Resources Information Center

Langhus, D. L.; Flinchbaugh, D. A.

1986-01-01

Describes an elective field study program at Moravian College (Pennsylvania) in which seniors in analytical chemistry obtain first-hand experience at Bethlehem Steel Corporation. Discusses the program's planning phase, some method development projects done by students, experiences received in laboratory operations, and the evaluation of student…

Visual analytics as a translational cognitive science.

PubMed

Fisher, Brian; Green, Tera Marie; Arias-Hernández, Richard

2011-07-01

Visual analytics is a new interdisciplinary field of study that calls for a more structured scientific approach to understanding the effects of interaction with complex graphical displays on human cognitive processes. Its primary goal is to support the design and evaluation of graphical information systems that better support cognitive processes in areas as diverse as scientific research and emergency management. The methodologies that make up this new field are as yet ill defined. This paper proposes a pathway for development of visual analytics as a translational cognitive science that bridges fundamental research in human/computer cognitive systems and design and evaluation of information systems in situ. Achieving this goal will require the development of enhanced field methods for conceptual decomposition of human/computer cognitive systems that maps onto laboratory studies, and improved methods for conducting laboratory investigations that might better map onto real-world cognitive processes in technology-rich environments. Copyright © 2011 Cognitive Science Society, Inc.

Data analysis considerations for pesticides determined by National Water Quality Laboratory schedule 2437

USGS Publications Warehouse

Shoda, Megan E.; Nowell, Lisa H.; Stone, Wesley W.; Sandstrom, Mark W.; Bexfield, Laura M.

2018-04-02

In 2013, the U.S. Geological Survey National Water Quality Laboratory (NWQL) made a new method available for the analysis of pesticides in filtered water samples: laboratory schedule 2437. Schedule 2437 is an improvement on previous analytical methods because it determines the concentrations of 225 fungicides, herbicides, insecticides, and associated degradates in one method at similar or lower concentrations than previously available methods. Additionally, the pesticides included in schedule 2437 were strategically identified in a prioritization analysis that assessed likelihood of occurrence, prevalence of use, and potential toxicity. When the NWQL reports pesticide concentrations for analytes in schedule 2437, the laboratory also provides supplemental information useful to data users for assessing method performance and understanding data quality. That supplemental information is discussed in this report, along with an initial analysis of analytical recovery of pesticides in water-quality samples analyzed by schedule 2437 during 2013–2015. A total of 523 field matrix spike samples and their paired environmental samples and 277 laboratory reagent spike samples were analyzed for this report (1,323 samples total). These samples were collected in the field as part of the U.S. Geological Survey National Water-Quality Assessment groundwater and surface-water studies and as part of the NWQL quality-control program. This report reviews how pesticide samples are processed by the NWQL, addresses how to obtain all the data necessary to interpret pesticide concentrations, explains the circumstances that result in a reporting level change or the occurrence of a raised reporting level, and describes the calculation and assessment of recovery. This report also discusses reasons why a data user might choose to exclude data in an interpretive analysis and outlines the approach used to identify the potential for decreased data quality in the assessment of method recovery. The information provided in this report is essential to understanding pesticide data determined by schedule 2437 and should be reviewed before interpretation of these data.

Gasoline and Diesel Fuel Test Methods Additional Resources

EPA Pesticide Factsheets

Supporting documents on the Direct Final Rule that allows refiners and laboratories to use more current and improved fuel testing procedures for twelve American Society for Testing and Materials analytical test methods.

Utility perspective on USEPA analytical methods program redirection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koch, B.; Davis, M.K.; Krasner, S.W.

1996-11-01

The Metropolitan Water District of Southern California (Metropolitan) is a public, municipal corporation, created by the State of California, which wholesales supplemental water trough 27 member agencies (cities and water districts). Metropolitan serves nearly 16 million people in an area along the coastal plain of Southern California that covers approximately 5200 square miles. Water deliveries have averaged up to 2.5 million acre-feet per year. Metropolitan`s Water Quality Laboratory (WQL) conducts compliance monitoring of its source and finished drinking waters for chemical and microbial constituents. The laboratory maintains certification of a large number and variety of analytical procedures. The WQL operatesmore » in a 17,000-square-foot facility. The equipment is state-of-the-art analytical instrumentation. The staff consists of 40 professional chemists and microbiologists whose experience and expertise are extensive and often highly specialized. The staff turnover is very low, and the laboratory is consistently, efficiently, and expertly run.« less

Performance evaluation soil samples utilizing encapsulation technology

DOEpatents

Dahlgran, J.R.

1999-08-17

Performance evaluation soil samples and method of their preparation uses encapsulation technology to encapsulate analytes which are introduced into a soil matrix for analysis and evaluation by analytical laboratories. Target analytes are mixed in an appropriate solvent at predetermined concentrations. The mixture is emulsified in a solution of polymeric film forming material. The emulsified solution is polymerized to form microcapsules. The microcapsules are recovered, quantitated and introduced into a soil matrix in a predetermined ratio to form soil samples with the desired analyte concentration. 1 fig.

Performance evaluation soil samples utilizing encapsulation technology

DOEpatents

Dahlgran, James R.

1999-01-01

Performance evaluation soil samples and method of their preparation using encapsulation technology to encapsulate analytes which are introduced into a soil matrix for analysis and evaluation by analytical laboratories. Target analytes are mixed in an appropriate solvent at predetermined concentrations. The mixture is emulsified in a solution of polymeric film forming material. The emulsified solution is polymerized to form microcapsules. The microcapsules are recovered, quantitated and introduced into a soil matrix in a predetermined ratio to form soil samples with the desired analyte concentration.

Major advances in testing of dairy products: milk component and dairy product attribute testing.

PubMed

Barbano, D M; Lynch, J M

2006-04-01

Milk component analysis is relatively unusual in the field of quantitative analytical chemistry because an analytical test result determines the allocation of very large amounts of money between buyers and sellers of milk. Therefore, there is high incentive to develop and refine these methods to achieve a level of analytical performance rarely demanded of most methods or laboratory staff working in analytical chemistry. In the last 25 yr, well-defined statistical methods to characterize and validate analytical method performance combined with significant improvements in both the chemical and instrumental methods have allowed achievement of improved analytical performance for payment testing. A shift from marketing commodity dairy products to the development, manufacture, and marketing of value added dairy foods for specific market segments has created a need for instrumental and sensory approaches and quantitative data to support product development and marketing. Bringing together sensory data from quantitative descriptive analysis and analytical data from gas chromatography olfactometry for identification of odor-active compounds in complex natural dairy foods has enabled the sensory scientist and analytical chemist to work together to improve the consistency and quality of dairy food flavors.

Spectral multivariate calibration without laboratory prepared or determined reference analyte values.

PubMed

Ottaway, Josh; Farrell, Jeremy A; Kalivas, John H

2013-02-05

An essential part to calibration is establishing the analyte calibration reference samples. These samples must characterize the sample matrix and measurement conditions (chemical, physical, instrumental, and environmental) of any sample to be predicted. Calibration usually requires measuring spectra for numerous reference samples in addition to determining the corresponding analyte reference values. Both tasks are typically time-consuming and costly. This paper reports on a method named pure component Tikhonov regularization (PCTR) that does not require laboratory prepared or determined reference values. Instead, an analyte pure component spectrum is used in conjunction with nonanalyte spectra for calibration. Nonanalyte spectra can be from different sources including pure component interference samples, blanks, and constant analyte samples. The approach is also applicable to calibration maintenance when the analyte pure component spectrum is measured in one set of conditions and nonanalyte spectra are measured in new conditions. The PCTR method balances the trade-offs between calibration model shrinkage and the degree of orthogonality to the nonanalyte content (model direction) in order to obtain accurate predictions. Using visible and near-infrared (NIR) spectral data sets, the PCTR results are comparable to those obtained using ridge regression (RR) with reference calibration sets. The flexibility of PCTR also allows including reference samples if such samples are available.

Laboratory and quality assurance protocols for the analysis of herbicides in ground water from the Management Systems Evaluation Area, Princeton, Minnesota

USGS Publications Warehouse

Larson, S.J.; Capel, P.D.; VanderLoop, A.G.

1996-01-01

Laboratory and quality assurance procedures for the analysis of ground-water samples for herbicides at the Management Systems Evaluation Area near Princeton, Minnesota are described. The target herbicides include atrazine, de-ethylatrazine, de-isopropylatrazine, metribuzin, alachlor, 2,6-diethylaniline, and metolachlor. The analytical techniques used are solid-phase extraction, and analysis by gas chromatography with mass-selective detection. Descriptions of cleaning procedures, preparation of standard solutions, isolation of analytes from water, sample transfer methods, instrumental analysis, and data analysis are included.

Guided-inquiry laboratory experiments to improve students' analytical thinking skills

NASA Astrophysics Data System (ADS)

Wahyuni, Tutik S.; Analita, Rizki N.

2017-12-01

This study aims to improve the experiment implementation quality and analytical thinking skills of undergraduate students through guided-inquiry laboratory experiments. This study was a classroom action research conducted in three cycles. The study has been carried out with 38 undergraduate students of the second semester of Biology Education Department of State Islamic Institute (SII) of Tulungagung, as a part of Chemistry for Biology course. The research instruments were lesson plans, learning observation sheets and undergraduate students' experimental procedure. Research data were analyzed using quantitative-descriptive method. The increasing of analytical thinking skills could be measured using gain score normalized and statistical paired t-test. The results showed that guided-inquiry laboratory experiments model was able to improve both the experiment implementation quality and the analytical thinking skills. N-gain score of the analytical thinking skills was increased, in spite of just 0.03 with low increase category, indicated by experimental reports. Some of undergraduate students have had the difficulties in detecting the relation of one part to another and to an overall structure. The findings suggested that giving feedback the procedural knowledge and experimental reports were important. Revising the experimental procedure that completed by some scaffolding questions were also needed.

Food Adulteration in Switzerland: From 'Ravioli' over 'Springbok' to 'Disco Sushi'.

PubMed

Hubner, Philipp

2016-01-01

The driving force behind food adulteration is monetary profit and this has remained unchanged for at least the last hundred years. Food adulterations were and still are difficult to uncover because they occur mostly in an unpredictable and unexpected way. Very often food falsifiers take advantage of modern technology in such a way that food adulterations are difficult or sometimes even impossible to detect. Targets for food adulteration were and still are highly priced food items such as spirits, meat, seafood and olive oil. Although difficult to detect, food adulterations were in the past strong driving forces for the development of adequate detection methods in the official food control laboratories and for the enforcement of the food law. A very prominent example in this context is the 'Ravioli scandal' in Switzerland in the late 1970s which showed that cheap second-class meat could be processed into products without being discovered for long time. As a consequence the official food control laboratories in Switzerland were reinforced with more laboratory equipment and technical staff. With the introduction of new detection principles such as DNA-based analytical methods new kinds of food adulteration could and can be uncovered. Analytical methods have their limits and in some cases of food fraud there are no analytical means to detect them. In such cases the examination of trade by checking of accounts is the method of choice.

HEATED PURGE AND TRAP METHOD DEVELOPMENT AND TESTING

EPA Science Inventory

The goal of the research was to develop a heated purge and trap method that could be used in conjunction with SW-846 method 8240 for the analysis of volatile, water soluble Appendix VIII analytes. The developed method was validated according to a partial single laboratory method ...

Measurement of Henry's Law Constants Using Internal Standards: A Quantitative GC Experiment for the Instrumental Analysis or Environmental Chemistry Laboratory

ERIC Educational Resources Information Center

Ji, Chang; Boisvert, Susanne M.; Arida, Ann-Marie C.; Day, Shannon E.

2008-01-01

An internal standard method applicable to undergraduate instrumental analysis or environmental chemistry laboratory has been designed and tested to determine the Henry's law constants for a series of alkyl nitriles. In this method, a mixture of the analytes and an internal standard is prepared and used to make a standard solution (organic solvent)…

Enzymatic Spectrophotometric Reaction Rate Determination of Glucose in Fruit Drinks and Carbonated Beverages. An Analytical Chemistry Laboratory Experiment for Food Science-Oriented Students

NASA Astrophysics Data System (ADS)

Vasilarou, Argyro-Maria G.; Georgiou, Constantinos A.

2000-10-01

The glucose oxidase-horseradish peroxidase coupled reaction using phenol and 4-aminoantipyrine is used for the kinetic determination of glucose in drinks and beverages. This laboratory experiment demonstrates the implementation of reaction rate kinetic methods of analysis, the use of enzymes as selective analytical reagents for the determination of substrates, the kinetic masking of ascorbic acid interference, and the analysis of glucose in drinks and beverages. The method is optimized for student use in the temperature range of 18-28 °C and can be used in low-budget laboratories equipped with an inexpensive visible photometer. The mixed enzyme-chromogen solution that is used is stable for two months. Precision ranged from 5.1 to 12% RSD for analyses conducted during a period of two months by 48 students.

Development of analytical methodologies to assess recalcitrant pesticide bioremediation in biobeds at laboratory scale.

PubMed

Rivero, Anisleidy; Niell, Silvina; Cerdeiras, M Pía; Heinzen, Horacio; Cesio, María Verónica

2016-06-01

To assess recalcitrant pesticide bioremediation it is necessary to gradually increase the complexity of the biological system used in order to design an effective biobed assembly. Each step towards this effective biobed design needs a suitable, validated analytical methodology that allows a correct evaluation of the dissipation and bioconvertion. Low recovery yielding methods could give a false idea of a successful biodegradation process. To address this situation, different methods were developed and validated for the simultaneous determination of endosulfan, its main three metabolites, and chlorpyrifos in increasingly complex matrices where the bioconvertor basidiomycete Abortiporus biennis could grow. The matrices were culture media, bran, and finally a laboratory biomix composed of bran, peat and soil. The methodology for the analysis of the first evaluated matrix has already been reported. The methodologies developed for the other two systems are presented in this work. The targeted analytes were extracted from fungi growing over bran in semisolid media YNB (Yeast Nitrogen Based) with acetonitrile using shaker assisted extraction, The salting-out step was performed with MgSO4 and NaCl, and the extracts analyzed by GC-ECD. The best methodology was fully validated for all the evaluated analytes at 1 and 25mgkg(-1) yielding recoveries between 72% and 109% and RSDs <11% in all cases. The application of this methodology proved that A. biennis is able to dissipate 94% of endosulfan and 87% of chlorpyrifos after 90 days. Having assessed that A. biennis growing over bran can metabolize the studied pesticides, the next step faced was the development and validation of an analytical procedure to evaluate the analytes in a laboratory scale biobed composed of 50% of bran, 25% of peat and 25% of soil together with fungal micelium. From the different procedures assayed, only ultrasound assisted extraction with ethyl acetate allowed recoveries between 80% and 110% with RSDs <18%. Linearity, recovery, precision, matrix effect and LODs/LOQs of each method were studied for all the analytes: endosulfan isomers (α & β) and its metabolites (endosulfan sulfate, ether and diol) as well as for chlorpyrifos. In the first laboratory evaluation of these biobeds endosulfan was bioconverted up to 87% and chlorpyrifos more than 79% after 27 days. Copyright © 2016 Elsevier B.V. All rights reserved.

The Joint Committee for Traceability in Laboratory Medicine (JCTLM) - its history and operation.

PubMed

Jones, Graham R D; Jackson, Craig

2016-01-30

The Joint Committee for Traceability in Laboratory Medicine (JCTLM) was formed to bring together the sciences of metrology, laboratory medicine and laboratory quality management. The aim of this collaboration is to support worldwide comparability and equivalence of measurement results in clinical laboratories for the purpose of improving healthcare. The JCTLM has its origins in the activities of international metrology treaty organizations, professional societies and federations devoted to improving measurement quality in physical, chemical and medical sciences. The three founding organizations, the International Committee for Weights and Measures (CIPM), the International Federation of Clinical Chemistry and Laboratory Medicine (IFCC) and the International Laboratory Accreditation Cooperation (ILAC) are the leaders of this activity. The main service of the JCTLM is a web-based database with a list of reference materials, reference methods and reference measurement services meeting appropriate international standards. This database allows manufacturers to select references for assay traceability and provides support for suppliers of these services. As of mid 2015 the database lists 295 reference materials for 162 analytes, 170 reference measurement procedures for 79 analytes and 130 reference measurement services for 39 analytes. There remains a need for the development and implementation of metrological traceability in many areas of laboratory medicine and the JCTLM will continue to promote these activities into the future. Copyright © 2015 Elsevier B.V. All rights reserved.

Preface: 5th International Symposium on the Interface between Analytical Chemistry and Microbiology - April 19th to 21st, 2004: Hosted at Pacific Northwest National Laboratory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Allmaier, Guenter; Wunschel, David S.; Wahl, Karen L.

2004-04-19

This is an introduction to a special issue of the Journal of microbiological Methods based on a recent meeting held at PNNL: the 5th International Symposium on the Interface between Analytical Chemistry and Microbiology.

Comparison of three sampling and analytical methods for the determination of airborne hexavalent chromium.

PubMed

Boiano, J M; Wallace, M E; Sieber, W K; Groff, J H; Wang, J; Ashley, K

2000-08-01

A field study was conducted with the goal of comparing the performance of three recently developed or modified sampling and analytical methods for the determination of airborne hexavalent chromium (Cr(VI)). The study was carried out in a hard chrome electroplating facility and in a jet engine manufacturing facility where airborne Cr(VI) was expected to be present. The analytical methods evaluated included two laboratory-based procedures (OSHA Method ID-215 and NIOSH Method 7605) and a field-portable method (NIOSH Method 7703). These three methods employ an identical sampling methodology: collection of Cr(VI)-containing aerosol on a polyvinyl chloride (PVC) filter housed in a sampling cassette, which is connected to a personal sampling pump calibrated at an appropriate flow rate. The basis of the analytical methods for all three methods involves extraction of the PVC filter in alkaline buffer solution, chemical isolation of the Cr(VI) ion, complexation of the Cr(VI) ion with 1,5-diphenylcarbazide, and spectrometric measurement of the violet chromium diphenylcarbazone complex at 540 nm. However, there are notable specific differences within the sample preparation procedures used in three methods. To assess the comparability of the three measurement protocols, a total of 20 side-by-side air samples were collected, equally divided between a chromic acid electroplating operation and a spray paint operation where water soluble forms of Cr(VI) were used. A range of Cr(VI) concentrations from 0.6 to 960 microg m(-3), with Cr(VI) mass loadings ranging from 0.4 to 32 microg, was measured at the two operations. The equivalence of the means of the log-transformed Cr(VI) concentrations obtained from the different analytical methods was compared. Based on analysis of variance (ANOVA) results, no statistically significant differences were observed between mean values measured using each of the three methods. Small but statistically significant differences were observed between results obtained from performance evaluation samples for the NIOSH field method and the OSHA laboratory method.

A MASSive Laboratory Tour. An Interactive Mass Spectrometry Outreach Activity for Children

NASA Astrophysics Data System (ADS)

Jungmann, Julia H.; Mascini, Nadine E.; Kiss, Andras; Smith, Donald F.; Klinkert, Ivo; Eijkel, Gert B.; Duursma, Marc C.; Cillero Pastor, Berta; Chughtai, Kamila; Chughtai, Sanaullah; Heeren, Ron M. A.

2013-07-01

It is imperative to fascinate young children at an early stage in their education for the analytical sciences. The exposure of the public to mass spectrometry presently increases rapidly through the common media. Outreach activities can take advantage of this exposure and employ mass spectrometry as an exquisite example of an analytical science in which children can be fascinated. The presented teaching modules introduce children to mass spectrometry and give them the opportunity to experience a modern research laboratory. The modules are highly adaptable and can be applied to young children from the age of 6 to 14 y. In an interactive tour, the students explore three major scientific concepts related to mass spectrometry; the building blocks of matter, charged particle manipulation by electrostatic fields, and analyte identification by mass analysis. Also, the students carry out a mass spectrometry experiment and learn to interpret the resulting mass spectra. The multistage, inquiry-based tour contains flexible methods, which teach the students current-day research techniques and possible applications to real research topics. Besides the scientific concepts, laboratory safety and hygiene are stressed and the students are enthused for the analytical sciences by participating in "hands-on" work. The presented modules have repeatedly been successfully employed during laboratory open days. They are also found to be extremely suitable for (early) high school science classes during laboratory visit-focused field trips.

Microbial ecology laboratory procedures manual NASA/MSFC

NASA Technical Reports Server (NTRS)

Huff, Timothy L.

1990-01-01

An essential part of the efficient operation of any microbiology laboratory involved in sample analysis is a standard procedures manual. The purpose of this manual is to provide concise and well defined instructions on routine technical procedures involving sample analysis and methods for monitoring and maintaining quality control within the laboratory. Of equal importance is the safe operation of the laboratory. This manual outlines detailed procedures to be followed in the microbial ecology laboratory to assure safety, analytical control, and validity of results.

21 CFR 200.10 - Contract facilities (including consulting laboratories) utilized as extramural facilities by...

Code of Federal Regulations, 2014 CFR

2014-04-01

... Cosmetic Act specifically authorizes inspection of consulting laboratories as well as any factory... Federal Food, Drug, and Cosmetic Act. The Food and Drug Administration's position is that by the... Administration does not consider results of validation studies of analytical and assay methods and control...

21 CFR 200.10 - Contract facilities (including consulting laboratories) utilized as extramural facilities by...

Code of Federal Regulations, 2011 CFR

2011-04-01

... Cosmetic Act specifically authorizes inspection of consulting laboratories as well as any factory... Federal Food, Drug, and Cosmetic Act. The Food and Drug Administration's position is that by the... Administration does not consider results of validation studies of analytical and assay methods and control...

21 CFR 200.10 - Contract facilities (including consulting laboratories) utilized as extramural facilities by...

Code of Federal Regulations, 2013 CFR

2013-04-01

... Cosmetic Act specifically authorizes inspection of consulting laboratories as well as any factory... Federal Food, Drug, and Cosmetic Act. The Food and Drug Administration's position is that by the... Administration does not consider results of validation studies of analytical and assay methods and control...

21 CFR 200.10 - Contract facilities (including consulting laboratories) utilized as extramural facilities by...

Code of Federal Regulations, 2012 CFR

2012-04-01

... Cosmetic Act specifically authorizes inspection of consulting laboratories as well as any factory... Federal Food, Drug, and Cosmetic Act. The Food and Drug Administration's position is that by the... Administration does not consider results of validation studies of analytical and assay methods and control...

Other Resources Related to SAM

EPA Pesticide Factsheets

Learn more about websites and information related to EPA's Selected Analytical Methods for Environmental Remediation and Recovery (SAM), including key EPA collaborators, laboratories, and research centers.

Methods for collection and analysis of water samples

USGS Publications Warehouse

Rainwater, Frank Hays; Thatcher, Leland Lincoln

1960-01-01

This manual contains methods used by the U.S. Geological Survey to collect, preserve, and analyze water samples. Throughout, the emphasis is on obtaining analytical results that accurately describe the chemical composition of the water in situ. Among the topics discussed are selection of sampling sites, frequency of sampling, field equipment, preservatives and fixatives, analytical techniques of water analysis, and instruments. Seventy-seven laboratory and field procedures are given for determining fifty-three water properties.

Comparison of methods for measurement of organic compounds at ultra-trace level: analytical criteria and application to analysis of amino acids in extraterrestrial samples.

PubMed

Vandenabeele-Trambouze, O; Claeys-Bruno, M; Dobrijevic, M; Rodier, C; Borruat, G; Commeyras, A; Garrelly, L

2005-02-01

The need for criteria to compare different analytical methods for measuring extraterrestrial organic matter at ultra-trace levels in relatively small and unique samples (e.g., fragments of meteorites, micrometeorites, planetary samples) is discussed. We emphasize the need to standardize the description of future analyses, and take the first step toward a proposed international laboratory network for performance testing.

External quality assurance programs as a tool for verifying standardization of measurement procedures: Pilot collaboration in Europe.

PubMed

Perich, C; Ricós, C; Alvarez, V; Biosca, C; Boned, B; Cava, F; Doménech, M V; Fernández-Calle, P; Fernández-Fernández, P; García-Lario, J V; Minchinela, J; Simón, M; Jansen, R

2014-05-15

Current external quality assurance schemes have been classified into six categories, according to their ability to verify the degree of standardization of the participating measurement procedures. SKML (Netherlands) is a Category 1 EQA scheme (commutable EQA materials with values assigned by reference methods), whereas SEQC (Spain) is a Category 5 scheme (replicate analyses of non-commutable materials with no values assigned by reference methods). The results obtained by a group of Spanish laboratories participating in a pilot study organized by SKML are examined, with the aim of pointing out the improvements over our current scheme that a Category 1 program could provide. Imprecision and bias are calculated for each analyte and laboratory, and compared with quality specifications derived from biological variation. Of the 26 analytes studied, 9 had results comparable with those from reference methods, and 10 analytes did not have comparable results. The remaining 7 analytes measured did not have available reference method values, and in these cases, comparison with the peer group showed comparable results. The reasons for disagreement in the second group can be summarized as: use of non-standard methods (IFCC without exogenous pyridoxal phosphate for AST and ALT, Jaffé kinetic at low-normal creatinine concentrations and with eGFR); non-commutability of the reference material used to assign values to the routine calibrator (calcium, magnesium and sodium); use of reference materials without established commutability instead of reference methods for AST and GGT, and lack of a systematic effort by manufacturers to harmonize results. Results obtained in this work demonstrate the important role of external quality assurance programs using commutable materials with values assigned by reference methods to correctly monitor the standardization of laboratory tests with consequent minimization of risk to patients. Copyright © 2013 Elsevier B.V. All rights reserved.

The non-Gaussian joint probability density function of slope and elevation for a nonlinear gravity wave field. [in ocean surface

NASA Technical Reports Server (NTRS)

Huang, N. E.; Long, S. R.; Bliven, L. F.; Tung, C.-C.

1984-01-01

On the basis of the mapping method developed by Huang et al. (1983), an analytic expression for the non-Gaussian joint probability density function of slope and elevation for nonlinear gravity waves is derived. Various conditional and marginal density functions are also obtained through the joint density function. The analytic results are compared with a series of carefully controlled laboratory observations, and good agreement is noted. Furthermore, the laboratory wind wave field observations indicate that the capillary or capillary-gravity waves may not be the dominant components in determining the total roughness of the wave field. Thus, the analytic results, though derived specifically for the gravity waves, may have more general applications.

Amie Sluiter | NREL

Science.gov Websites

biomass analysis methods and is primary author on 11 Laboratory Analytical Procedures, which are ) spectroscopic analysis methods. These methods allow analysts to predict the composition of feedstock and process . Patent No. 6,737,258 (2002) Featured Publications "Improved methods for the determination of drying

37Cl/35Cl isotope ratio analysis in perchlorate by ion chromatography/multi collector -ICPMS: Analytical performance and implication for biodegradation studies.

PubMed

Zakon, Yevgeni; Ronen, Zeev; Halicz, Ludwik; Gelman, Faina

2017-10-01

In the present study we propose a new analytical method for 37 Cl/ 35 Cl analysis in perchlorate by Ion Chromatography(IC) coupled to Multicollector Inductively Coupled Plasma Mass Spectrometry (MC-ICPMS). The accuracy of the analytical method was validated by analysis of international perchlorate standard materials USGS-37 and USGS -38; analytical precision better than ±0.4‰ was achieved. 37 Cl/ 35 Cl isotope ratio analysis in perchlorate during laboratory biodegradation experiment with microbial cultures enriched from the contaminated soil in Israel resulted in isotope enrichment factor ε 37 Cl = -13.3 ± 1‰, which falls in the range reported previously for perchlorate biodegradation by pure microbial cultures. The proposed analytical method may significantly simplify the procedure for isotope analysis of perchlorate which is currently applied in environmental studies. Copyright © 2017. Published by Elsevier Ltd.

Recalibration of blood analytes over 25 years in the Atherosclerosis Risk in Communities Study: The impact of recalibration on chronic kidney disease prevalence and incidence

PubMed Central

Parrinello, Christina M.; Grams, Morgan E.; Couper, David; Ballantyne, Christie M.; Hoogeveen, Ron C.; Eckfeldt, John H.; Selvin, Elizabeth; Coresh, Josef

2016-01-01

Background Equivalence of laboratory tests over time is important for longitudinal studies. Even a small systematic difference (bias) can result in substantial misclassification. Methods We selected 200 Atherosclerosis Risk in Communities Study participants attending all 5 study visits over 25 years. Eight analytes were re-measured in 2011–13 from stored blood samples from multiple visits: creatinine, uric acid, glucose, total cholesterol, HDL-cholesterol, LDL-cholesterol, triglycerides, and high-sensitivity C-reactive protein. Original values were recalibrated to re-measured values using Deming regression. Differences >10% were considered to reflect substantial bias, and correction equations were applied to affected analytes in the total study population. We examined trends in chronic kidney disease (CKD) pre- and post-recalibration. Results Repeat measures were highly correlated with original values (Pearson’s r>0.85 after removing outliers [median 4.5% of paired measurements]), but 2 of 8 analytes (creatinine and uric acid) had differences >10%. Original values of creatinine and uric acid were recalibrated to current values using correction equations. CKD prevalence differed substantially after recalibration of creatinine (visits 1, 2, 4 and 5 pre-recalibration: 21.7%, 36.1%, 3.5%, 29.4%; post-recalibration: 1.3%, 2.2%, 6.4%, 29.4%). For HDL-cholesterol, the current direct enzymatic method differed substantially from magnesium dextran precipitation used during visits 1–4. Conclusions Analytes re-measured in samples stored for ~25 years were highly correlated with original values, but two of the 8 analytes showed substantial bias at multiple visits. Laboratory recalibration improved reproducibility of test results across visits and resulted in substantial differences in CKD prevalence. We demonstrate the importance of consistent recalibration of laboratory assays in a cohort study. PMID:25952043

ERLN Technical Support for Labs

EPA Pesticide Factsheets

The Environmental Response Laboratory Network provides policies and guidance on lab and data requirements, Standardized Analytical Methods, and technical support for water and radiological sampling and analysis

Sigma metrics as a tool for evaluating the performance of internal quality control in a clinical chemistry laboratory.

PubMed

Kumar, B Vinodh; Mohan, Thuthi

2018-01-01

Six Sigma is one of the most popular quality management system tools employed for process improvement. The Six Sigma methods are usually applied when the outcome of the process can be measured. This study was done to assess the performance of individual biochemical parameters on a Sigma Scale by calculating the sigma metrics for individual parameters and to follow the Westgard guidelines for appropriate Westgard rules and levels of internal quality control (IQC) that needs to be processed to improve target analyte performance based on the sigma metrics. This is a retrospective study, and data required for the study were extracted between July 2015 and June 2016 from a Secondary Care Government Hospital, Chennai. The data obtained for the study are IQC - coefficient of variation percentage and External Quality Assurance Scheme (EQAS) - Bias% for 16 biochemical parameters. For the level 1 IQC, four analytes (alkaline phosphatase, magnesium, triglyceride, and high-density lipoprotein-cholesterol) showed an ideal performance of ≥6 sigma level, five analytes (urea, total bilirubin, albumin, cholesterol, and potassium) showed an average performance of <3 sigma level and for level 2 IQCs, same four analytes of level 1 showed a performance of ≥6 sigma level, and four analytes (urea, albumin, cholesterol, and potassium) showed an average performance of <3 sigma level. For all analytes <6 sigma level, the quality goal index (QGI) was <0.8 indicating the area requiring improvement to be imprecision except cholesterol whose QGI >1.2 indicated inaccuracy. This study shows that sigma metrics is a good quality tool to assess the analytical performance of a clinical chemistry laboratory. Thus, sigma metric analysis provides a benchmark for the laboratory to design a protocol for IQC, address poor assay performance, and assess the efficiency of existing laboratory processes.

Modern analytical chemistry in the contemporary world

NASA Astrophysics Data System (ADS)

Šíma, Jan

2016-12-01

Students not familiar with chemistry tend to misinterpret analytical chemistry as some kind of the sorcery where analytical chemists working as modern wizards handle magical black boxes able to provide fascinating results. However, this approach is evidently improper and misleading. Therefore, the position of modern analytical chemistry among sciences and in the contemporary world is discussed. Its interdisciplinary character and the necessity of the collaboration between analytical chemists and other experts in order to effectively solve the actual problems of the human society and the environment are emphasized. The importance of the analytical method validation in order to obtain the accurate and precise results is highlighted. The invalid results are not only useless; they can often be even fatal (e.g., in clinical laboratories). The curriculum of analytical chemistry at schools and universities is discussed. It is referred to be much broader than traditional equilibrium chemistry coupled with a simple description of individual analytical methods. Actually, the schooling of analytical chemistry should closely connect theory and practice.

Dried blood spot specimen quality and validation of a new pre-analytical processing method for qualitative HIV-1 PCR, KwaZulu-Natal, South Africa

PubMed Central

Parboosing, Raveen; Siyaca, Ntombizandile; Moodley, Pravikrishnen

2016-01-01

Background Poor quality dried blood spot (DBS) specimens are usually rejected by virology laboratories, affecting early infant diagnosis of HIV. The practice of combining two incompletely-filled DBS in one specimen preparation tube during pre-analytical specimen processing (i.e., the two-spot method) has been implemented to reduce the number of specimens being rejected for insufficient volume. Objectives This study analysed laboratory data to describe the quality of DBS specimens and the use of the two-spot method over a one-year period, then validated the two-spot method against the standard (one-spot) method. Methods Data on HIV-1 PCR test requests submitted in 2014 to the Department of Virology at Inkosi Albert Luthuli Central Hospital in KwaZulu-Natal province, South Africa were analysed to describe reasons for specimen rejection, as well as results of the two-spot method. The accuracy, lower limit of detection and precision of the two-spot method were assessed. Results Of the 88 481 specimens received, 3.7% were rejected for pre-analytical problems. Of those, 48.9% were rejected as a result of insufficient specimen volume. Two health facilities had significantly more specimen rejections than other facilities. The two-spot method prevented 10 504 specimen rejections. The Pearson correlation coefficient comparing the standard to the two-spot method was 0.997. Conclusions The two-spot method was comparable with the standard method of pre-analytical specimen processing. Two health facilities were identified for targeted retraining on specimen quality. The two-spot method of DBS specimen processing can be used as an adjunct to retraining, to reduce the number of specimens rejected and improve linkage to care. PMID:28879108

Machine learning in laboratory medicine: waiting for the flood?

PubMed

Cabitza, Federico; Banfi, Giuseppe

2018-03-28

This review focuses on machine learning and on how methods and models combining data analytics and artificial intelligence have been applied to laboratory medicine so far. Although still in its infancy, the potential for applying machine learning to laboratory data for both diagnostic and prognostic purposes deserves more attention by the readership of this journal, as well as by physician-scientists who will want to take advantage of this new computer-based support in pathology and laboratory medicine.

Multilaboratory Validation of First Action Method 2016.04 for Determination of Four Arsenic Species in Fruit Juice by High-Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry.

PubMed

Kubachka, Kevin; Heitkemper, Douglas T; Conklin, Sean

2017-07-01

Before being designated AOAC First Action Official MethodSM 2016.04, the U.S. Food and Drug Administration's method, EAM 4.10 High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometric Determination of Four Arsenic Species in Fruit Juice, underwent both a single-laboratory validation and a multilaboratory validation (MLV) study. Three federal and five state regulatory laboratories participated in the MLV study, which is the primary focus of this manuscript. The method was validated for inorganic arsenic (iAs) measured as the sum of the two iAs species arsenite [As(III)] and arsenate [As(V)], dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) by analyses of 13 juice samples, including three apple juice, three apple juice concentrate, four grape juice, and three pear juice samples. In addition, two water Standard Reference Materials (SRMs) were analyzed. The method LODs and LOQs obtained among the eight laboratories were approximately 0.3 and 2 ng/g, respectively, for each of the analytes and were adequate for the intended purpose of the method. Each laboratory analyzed method blanks, fortified method blanks, reference materials, triplicate portions of each juice sample, and duplicate fortified juice samples (one for each matrix type) at three fortification levels. In general, repeatability and reproducibility of the method was ≤15% RSD for each species present at a concentration >LOQ. The average recovery of fortified analytes for all laboratories ranged from 98 to 104% iAs, DMA, and MMA for all four juice sample matrixes. The average iAs results for SRMs 1640a and 1643e agreed within the range of 96-98% of certified values for total arsenic.

Interlaboratory comparability, bias, and precision for four laboratories measuring analytes in wet deposition, October 1983-December 1984

USGS Publications Warehouse

Brooks, Myron H.; Schroder, LeRoy J.; Willoughby, Timothy C.

1987-01-01

Four laboratories involved in the routine analysis of wet-deposition samples participated in an interlaboratory comparison program managed by the U.S. Geological Survey. The four participants were: Illinois State Water Survey central analytical laboratory in Champaign, Illinois; U.S. Geological Survey national water-quality laboratories in Atlanta, Georgia, and Denver, Colorado; and Inland Waters Directorate national water-quality laboratory in Burlington, Ontario, Canada. Analyses of interlaboratory samples performed by the four laboratories from October 1983 through December 1984 were compared.Participating laboratories analyzed three types of interlaboratory samples--natural wet deposition, simulated wet deposition, and deionized water--for pH and specific conductance, and for dissolved calcium, magnesium, sodium, sodium, potassium, chloride, sulfate, nitrate, ammonium, and orthophosphate. Natural wet-deposition samples were aliquots of actual wet-deposition samples. Analyses of these samples by the four laboratories were compared using analysis of variance. Test results indicated that pH, calcium, nitrate, and ammonium results were not directly comparable among the four laboratories. Statistically significant differences between laboratory results probably only were meaningful for analyses of dissolved calcium. Simulated wet-deposition samples with known analyte concentrations were used to test each laboratory for analyte bias. Laboratory analyses of calcium, magnesium, sodium, potassium, chloride, sulfate, and nitrate were not significantly different from the known concentrations of these analytes when tested using analysis of variance. Deionized-water samples were used to test each laboratory for reporting of false positive values. The Illinois State Water Survey Laboratory reported the smallest percentage of false positive values for most analytes. Analyte precision was estimated for each laboratory from results of replicate measurements. In general, the Illinois State Water Survey laboratory achieved the greatest precision, whereas the U.S. Geological Survey laboratories achieved the least precision.

Optimisation of an analytical method and results from the inter-laboratory comparison of the migration of regulated substances from food packaging into the new mandatory European Union simulant for dry foodstuffs.

PubMed

Jakubowska, Natalia; Beldì, Giorgia; Peychès Bach, Aurélie; Simoneau, Catherine

2014-01-01

This paper presents the outcome of the development, optimisation and validation at European Union level of an analytical method for using poly(2,6-diphenyl phenylene oxide--PPPO), which is stipulated in Regulation (EU) No. 10/2011, as food simulant E for testing specific migration from plastics into dry foodstuffs. Two methods for fortifying respectively PPPO and a low-density polyethylene (LDPE) film with surrogate substances that are relevant to food contact were developed. A protocol for cleaning the PPPO and an efficient analytical method were developed for the quantification of butylhydroxytoluene (BHT), benzophenone (BP), diisobutylphthalate (DiBP), bis(2-ethylhexyl) adipate (DEHA) and 1,2-cyclohexanedicarboxylic acid, diisononyl ester (DINCH) from PPPO. A protocol for a migration test from plastics using small migration cells was also developed. The method was validated by an inter-laboratory comparison (ILC) with 16 national reference laboratories for food contact materials in the European Union. This allowed for the first time data to be obtained on the precision and laboratory performance of both migration and quantification. The results showed that the validation ILC was successful even when taking into account the complexity of the exercise. The results showed that the method performance was 7-9% repeatability standard deviation (rSD) for most substances (regardless of concentration), with 12% rSD for the high level of BHT and for DiBP at very low levels. The reproducibility standard deviation results for the 16 European Union laboratories were in the range of 20-30% for the quantification from PPPO (for the three levels of concentrations of the five substances) and 15-40% from migration experiments from the fortified plastic at 60°C for 10 days and subsequent quantification. Considering the lack of data previously available in the literature, this work has demonstrated that the validation of a method is possible both for migration from a film and for quantification into a corresponding simulant for specific migration.

Dried blood spot specimen quality and validation of a new pre-analytical processing method for qualitative HIV-1 PCR, KwaZulu-Natal, South Africa.

PubMed

Govender, Kerusha; Parboosing, Raveen; Siyaca, Ntombizandile; Moodley, Pravikrishnen

2016-01-01

Poor quality dried blood spot (DBS) specimens are usually rejected by virology laboratories, affecting early infant diagnosis of HIV. The practice of combining two incompletely-filled DBS in one specimen preparation tube during pre-analytical specimen processing (i.e., the two-spot method) has been implemented to reduce the number of specimens being rejected for insufficient volume. This study analysed laboratory data to describe the quality of DBS specimens and the use of the two-spot method over a one-year period, then validated the two-spot method against the standard (one-spot) method. Data on HIV-1 PCR test requests submitted in 2014 to the Department of Virology at Inkosi Albert Luthuli Central Hospital in KwaZulu-Natal province, South Africa were analysed to describe reasons for specimen rejection, as well as results of the two-spot method. The accuracy, lower limit of detection and precision of the two-spot method were assessed. Of the 88 481 specimens received, 3.7% were rejected for pre-analytical problems. Of those, 48.9% were rejected as a result of insufficient specimen volume. Two health facilities had significantly more specimen rejections than other facilities. The two-spot method prevented 10 504 specimen rejections. The Pearson correlation coefficient comparing the standard to the two-spot method was 0.997. The two-spot method was comparable with the standard method of pre-analytical specimen processing. Two health facilities were identified for targeted retraining on specimen quality. The two-spot method of DBS specimen processing can be used as an adjunct to retraining, to reduce the number of specimens rejected and improve linkage to care.

Capillary Zone Electrophoresis for the Analysis of Peptides: Fostering Students' Problem-Solving and Discovery Learning in an Undergraduate Laboratory Experiment

ERIC Educational Resources Information Center

Albright, Jessica C.; Beussman, Douglas J.

2017-01-01

Capillary electrophoresis is an important analytical separation method used to study a wide variety of samples, including those of biological origin. Capillary electrophoresis may be covered in the classroom, especially in advanced analytical courses, and while many students are exposed to gel electrophoresis in biology or biochemistry…

Target analyte quantification by isotope dilution LC-MS/MS directly referring to internal standard concentrations--validation for serum cortisol measurement.

PubMed

Maier, Barbara; Vogeser, Michael

2013-04-01

Isotope dilution LC-MS/MS methods used in the clinical laboratory typically involve multi-point external calibration in each analytical series. Our aim was to test the hypothesis that determination of target analyte concentrations directly derived from the relation of the target analyte peak area to the peak area of a corresponding stable isotope labelled internal standard compound [direct isotope dilution analysis (DIDA)] may be not inferior to conventional external calibration with respect to accuracy and reproducibility. Quality control samples and human serum pools were analysed in a comparative validation protocol for cortisol as an exemplary analyte by LC-MS/MS. Accuracy and reproducibility were compared between quantification either involving a six-point external calibration function, or a result calculation merely based on peak area ratios of unlabelled and labelled analyte. Both quantification approaches resulted in similar accuracy and reproducibility. For specified analytes, reliable analyte quantification directly derived from the ratio of peak areas of labelled and unlabelled analyte without the need for a time consuming multi-point calibration series is possible. This DIDA approach is of considerable practical importance for the application of LC-MS/MS in the clinical laboratory where short turnaround times often have high priority.

EVOLUTION OF AN ANALYTICAL METHOD FOR HALOGENATED FURANONES IN DRINKING WATER

EPA Science Inventory

A unified method of detection for seven halogenated furanones present in drinking waters at the ng/L level has been developed. The use of GC/ECD makes this method amenable to manyenvironmental laboratories and water treatment plants in the United States. Detection limits observe...

Chapter A5. Section 6.1.F. Wastewater, Pharmaceutical, and Antibiotic Compounds

USGS Publications Warehouse

Lewis, Michael Edward; Zaugg, Steven D.

2003-01-01

The USGS differentiates between samples collected for analysis of wastewater compounds and those collected for analysis of pharmaceutical and antibiotic compounds, based on the analytical schedule for the laboratory method. Currently, only the wastewater laboratory method for field-filtered samples (SH1433) is an approved, routine (production) method. (The unfiltered wastewater method LC 8033 also is available but requires a proposal for custom analysis.) At this time, analysis of samples for pharmaceutical and antibiotic compounds is confined to research studies and is available only on a custom basis.

Results of the first provisional technical secretariat interlaboratory comparison test

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stuff, J.R.; Hoffland, L.

1995-06-01

The principal task of this laboratory in the first Provisional Technical Secretariat (PTS) Interlaboratory Comparison Test was to verify and test the extraction and preparation procedures outlined in the Recommended Operating Procedures for Sampling and Analysis in the Verification of Chemical Disarmament in addition to our laboratory extraction methods and our laboratory analysis methods. Sample preparation began on 16 May 1994 and analysis was completed on 12 June 1994. The analytical methods used included NMR ({sup 1}H and {sup 31}P) GC/AED, GC/MS (EI and methane CI), GC/IRD, HPLC/IC, HPLC/TSP/MS, MS/MS(Electrospray), and CZE.

Results of the U. S. Geological Survey's analytical evaluation program for standard reference samples distributed in April 2001

USGS Publications Warehouse

Woodworth, M.T.; Connor, B.F.

2001-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for six standard reference samples -- T-165 (trace constituents), M-158 (major constituents), N-69 (nutrient constituents), N-70 (nutrient constituents), P-36 (low ionic-strength constituents), and Hg-32 (mercury) -- that were distributed in April 2001 to laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data received from 73 laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Results of the U. S. Geological Survey's Analytical Evaluation Program for Standard Reference Samples Distributed in March 2002

USGS Publications Warehouse

Woodworth, M.T.; Conner, B.F.

2002-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for six standard reference samples -- T- 169 (trace constituents), M- 162 (major constituents), N-73 (nutrient constituents), N-74 (nutrient constituents), P-38 (low ionic-strength constituents), and Hg-34 (mercury) -- that were distributed in March 2002 to laboratories enrolled in the U.S. Geological Survey sponsored intedaboratory testing program. Analytical data received from 93 laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Results of the U.S. Geological Survey's analytical evaluation program for standard reference samples distributed in September 2002

USGS Publications Warehouse

Woodworth, Mark T.; Connor, Brooke F.

2003-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for six standard reference samples -- T-171 (trace constituents), M-164 (major constituents), N-75 (nutrient constituents), N-76 (nutrient constituents), P-39 (low ionic-strength constituents), and Hg-35 (mercury) -- that were distributed in September 2002 to laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data received from 102 laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Results of the U.S. Geological Survey's analytical evaluation program for standard reference samples distributed in September 2001

USGS Publications Warehouse

Woodworth, Mark T.; Connor, Brooke F.

2002-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for six standard reference samples -- T-167 (trace constituents), M-160 (major constituents), N-71 (nutrient constituents), N-72 (nutrient constituents), P-37 (low ionic-strength constituents), and Hg-33 (mercury) -- that were distributed in September 2001 to laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data received from 98 laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Results of the U.S. Geological Survey's Analytical Evaluation Program for Standard Reference Samples Distributed in March 2000

USGS Publications Warehouse

Farrar, Jerry W.; Copen, Ashley M.

2000-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for six standard reference samples -- T-161 (trace constituents), M-154 (major constituents), N-65 (nutrient constituents), N-66 nutrient constituents), P-34 (low ionic strength constituents), and Hg-30 (mercury) -- that were distributed in March 2000 to 144 laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 132 of the laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Results of the U.S. Geological Survey's analytical evaluation program for standard reference samples distributed in October 1999

USGS Publications Warehouse

Farrar, T.W.

2000-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for six standard reference samples -- T-159 (trace constituents), M-152 (major constituents), N-63 (nutrient constituents), N-64 (nutrient constituents), P-33 (low ionic strength constituents), and Hg-29 (mercury) -- that were distributed in October 1999 to 149 laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 131 of the laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Results of the U.S. Geological Survey's analytical evaluation program for standard reference samples distributed in March 2003

USGS Publications Warehouse

Woodworth, Mark T.; Connor, Brooke F.

2003-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for six standard reference samples -- T-173 (trace constituents), M-166 (major constituents), N-77 (nutrient constituents), N-78 (nutrient constituents), P-40 (low ionic-strength constituents), and Hg-36 (mercury) -- that were distributed in March 2003 to laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data received from 110 laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Results of the U. S. Geological Survey's analytical evaluation program for standard reference samples distributed in October 2000

USGS Publications Warehouse

Connor, B.F.; Currier, J.P.; Woodworth, M.T.

2001-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for six standard reference samples -- T-163 (trace constituents), M-156 (major constituents), N-67 (nutrient constituents), N-68 (nutrient constituents), P-35 (low ionic strength constituents), and Hg-31 (mercury) -- that were distributed in October 2000 to 126 laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 122 of the laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

METHODS FOR EMERGING CONTAMINANT GROUPS: EXPLOSIVES AND NITROSAMINES

EPA Science Inventory

Background
In support of requirements in the Safe Drinking Water Act, the National Exposure Research Laboratory (NERL), has been developing analytical methods for chemicals on the 1998 contaminant candidate list (CCL) and for other chemicals of emerging interest. The purpose ...

Interlaboratory comparison for the determination of the soluble fraction of metals in welding fume samples.

PubMed

Berlinger, Balazs; Harper, Martin

2018-02-01

There is interest in the bioaccessible metal components of aerosols, but this has been minimally studied because standardized sampling and analytical methods have not yet been developed. An interlaboratory study (ILS) has been carried out to evaluate a method for determining the water-soluble component of realistic welding fume (WF) air samples. Replicate samples were generated in the laboratory and distributed to participating laboratories to be analyzed according to a standardized procedure. Within-laboratory precision of replicate sample analysis (repeatability) was very good. Reproducibility between laboratories was not as good, but within limits of acceptability for the analysis of typical aerosol samples. These results can be used to support the development of a standardized test method.

Promoting clinical and laboratory interaction by harmonization.

PubMed

Plebani, Mario; Panteghini, Mauro

2014-05-15

The lack of interchangeable results in current practice among clinical laboratories has underpinned greater attention to standardization and harmonization projects. Although the focus was mainly on the standardization and harmonization of measurement procedures and their results, the scope of harmonization goes beyond method and analytical results: it includes all other aspects of laboratory testing, including terminology and units, report formats, reference limits and decision thresholds, as well as test profiles and criteria for the interpretation of results. In particular, as evidence collected in last decades demonstrates that pre-pre- and post-post-analytical steps are more vulnerable to errors, harmonization initiatives should be performed to improve procedures and processes at the laboratory-clinical interface. Managing upstream demand, down-stream interpretation of laboratory results, and subsequent appropriate action through close relationships between laboratorians and clinicians remains a crucial issue of the laboratory testing process. Therefore, initiatives to improve test demand management from one hand and to harmonize procedures to improve physicians' acknowledgment of laboratory data and their interpretation from the other hand are needed in order to assure quality and safety in the total testing process. © 2013.

Toxicologic evaluation of analytes from Tank 241-C-103

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahlum, D.D.; Young, J.Y.; Weller, R.E.

1994-11-01

Westinghouse Hanford Company requested PNL to assemble a toxicology review panel (TRP) to evaluate analytical data compiled by WHC, and provide advice concerning potential health effects associated with exposure to tank-vapor constituents. The team`s objectives would be to (1) review procedures used for sampling vapors from tanks, (2) identify constituents in tank-vapor samples that could be related to symptoms reported by workers, (3) evaluate the toxicological implications of those constituents by comparison to establish toxicological databases, (4) provide advice for additional analytical efforts, and (5) support other activities as requested by WHC. The TRP represents a wide range of expertise,more » including toxicology, industrial hygiene, and occupational medicine. The TRP prepared a list of target analytes that chemists at the Oregon Graduate Institute/Sandia (OGI), Oak Ridge National Laboratory (ORNL), and PNL used to establish validated methods for quantitative analysis of head-space vapors from Tank 241-C-103. this list was used by the analytical laboratories to develop appropriate analytical methods for samples from Tank 241-C-103. Target compounds on the list included acetone, acetonitrile, ammonia, benzene, 1, 3-butadiene, butanal, n-butanol, hexane, 2-hexanone, methylene chloride, nitric oxide, nitrogen dioxide, nitrous oxide, dodecane, tridecane, propane nitrile, sulfur oxide, tributyl phosphate, and vinylidene chloride. The TRP considered constituent concentrations, current exposure limits, reliability of data relative to toxicity, consistency of the analytical data, and whether the material was carcinogenic or teratogenic. A final consideration in the analyte selection process was to include representative chemicals for each class of compounds found.« less

Assessment of analytical quality in Nordic clinical chemistry laboratories using data from contemporary national programs.

PubMed

Aronsson, T; Bjørnstad, P; Leskinen, E; Uldall, A; de Verdier, C H

1984-01-01

The aim of this investigation was primarily to assess analytical quality expressed as between-laboratory, within-laboratory, and total imprecision, not in order to detect laboratories with poor performance, but in the positive sense to provide data for improving critical steps in analytical methodology. The aim was also to establish the present state of the art in comparison with earlier investigations to see if improvement in analytical quality could be observed.

Screening of 23 β-lactams in foodstuffs by LC-MS/MS using an alkaline QuEChERS-like extraction.

PubMed

Bessaire, Thomas; Mujahid, Claudia; Beck, Andrea; Tarres, Adrienne; Savoy, Marie-Claude; Woo, Pei-Mun; Mottier, Pascal; Desmarchelier, Aurélien

2018-04-01

A fast and robust high performance LC-MS/MS screening method was developed for the analysis of β-lactam antibiotics in foods of animal origin: eggs, raw milk, processed dairy ingredients, infant formula, and meat- and fish-based products including baby foods. QuEChERS extraction with some adaptations enabled 23 drugs to be simultaneously monitored. Screening target concentrations were set at levels adequate to ensure compliance with current European, Chinese, US and Canadian regulations. The method was fully validated according to the European Community Reference Laboratories Residues Guidelines using 93 food samples of different composition. False-negative and false-positive rates were below 5% for all analytes. The method is adequate for use in high-routine laboratories. A 1-year study was additionally conducted to assess the stability of the 23 analytes in the working standard solution.

The role of light microscopy in aerospace analytical laboratories

NASA Technical Reports Server (NTRS)

Crutcher, E. R.

1977-01-01

Light microscopy has greatly reduced analytical flow time and added new dimensions to laboratory capability. Aerospace analytical laboratories are often confronted with problems involving contamination, wear, or material inhomogeneity. The detection of potential problems and the solution of those that develop necessitate the most sensitive and selective applications of sophisticated analytical techniques and instrumentation. This inevitably involves light microscopy. The microscope can characterize and often identify the cause of a problem in 5-15 minutes with confirmatory tests generally less than one hour. Light microscopy has and will make a very significant contribution to the analytical capabilities of aerospace laboratories.

Portable total reflection x-ray fluorescence analysis in the identification of unknown laboratory hazards

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Ying, E-mail: liu.ying.48r@st.kyoto-u.ac.jp; Imashuku, Susumu; Sasaki, Nobuharu

In this study, a portable total reflection x-ray fluorescence (TXRF) spectrometer was used to analyze unknown laboratory hazards that precipitated on exterior surfaces of cooling pipes and fume hood pipes in chemical laboratories. With the aim to examine the accuracy of TXRF analysis for the determination of elemental composition, analytical results were compared with those of wavelength-dispersive x-ray fluorescence spectrometry, scanning electron microscope and energy-dispersive x-ray spectrometry, energy-dispersive x-ray fluorescence spectrometry, inductively coupled plasma atomic emission spectrometry, x-ray diffraction spectrometry (XRD), and x-ray photoelectron spectroscopy (XPS). Detailed comparison of data confirmed that the TXRF method itself was not sufficient tomore » determine all the elements (Z > 11) contained in the samples. In addition, results suggest that XRD should be combined with XPS in order to accurately determine compound composition. This study demonstrates that at least two analytical methods should be used in order to analyze the composition of unknown real samples.« less

Manganese recycling in the United States in 1998

USGS Publications Warehouse

Jones, Thomas S.

2003-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for six standard reference samples -- T-163 (trace constituents), M-156 (major constituents), N-67 (nutrient constituents), N-68 (nutrient constituents), P-35 (low ionic strength constituents), and Hg-31 (mercury) -- that were distributed in October 2000 to 126 laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 122 of the laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Nationwide Multicenter Reference Interval Study for 28 Common Biochemical Analytes in China.

PubMed

Xia, Liangyu; Chen, Ming; Liu, Min; Tao, Zhihua; Li, Shijun; Wang, Liang; Cheng, Xinqi; Qin, Xuzhen; Han, Jianhua; Li, Pengchang; Hou, Li'an; Yu, Songlin; Ichihara, Kiyoshi; Qiu, Ling

2016-03-01

A nationwide multicenter study was conducted in the China to explore sources of variation of reference values and establish reference intervals for 28 common biochemical analytes, as a part of the International Federation of Clinical Chemistry and Laboratory Medicine, Committee on Reference Intervals and Decision Limits (IFCC/C-RIDL) global study on reference values. A total of 3148 apparently healthy volunteers were recruited in 6 cities covering a wide area in China. Blood samples were tested in 2 central laboratories using Beckman Coulter AU5800 chemistry analyzers. Certified reference materials and value-assigned serum panel were used for standardization of test results. Multiple regression analysis was performed to explore sources of variation. Need for partition of reference intervals was evaluated based on 3-level nested ANOVA. After secondary exclusion using the latent abnormal values exclusion method, reference intervals were derived by a parametric method using the modified Box-Cox formula. Test results of 20 analytes were made traceable to reference measurement procedures. By the ANOVA, significant sex-related and age-related differences were observed in 12 and 12 analytes, respectively. A small regional difference was observed in the results for albumin, glucose, and sodium. Multiple regression analysis revealed BMI-related changes in results of 9 analytes for man and 6 for woman. Reference intervals of 28 analytes were computed with 17 analytes partitioned by sex and/or age. In conclusion, reference intervals of 28 common chemistry analytes applicable to Chinese Han population were established by use of the latest methodology. Reference intervals of 20 analytes traceable to reference measurement procedures can be used as common reference intervals, whereas others can be used as the assay system-specific reference intervals in China.

Nationwide Multicenter Reference Interval Study for 28 Common Biochemical Analytes in China

PubMed Central

Xia, Liangyu; Chen, Ming; Liu, Min; Tao, Zhihua; Li, Shijun; Wang, Liang; Cheng, Xinqi; Qin, Xuzhen; Han, Jianhua; Li, Pengchang; Hou, Li’an; Yu, Songlin; Ichihara, Kiyoshi; Qiu, Ling

2016-01-01

Abstract A nationwide multicenter study was conducted in the China to explore sources of variation of reference values and establish reference intervals for 28 common biochemical analytes, as a part of the International Federation of Clinical Chemistry and Laboratory Medicine, Committee on Reference Intervals and Decision Limits (IFCC/C-RIDL) global study on reference values. A total of 3148 apparently healthy volunteers were recruited in 6 cities covering a wide area in China. Blood samples were tested in 2 central laboratories using Beckman Coulter AU5800 chemistry analyzers. Certified reference materials and value-assigned serum panel were used for standardization of test results. Multiple regression analysis was performed to explore sources of variation. Need for partition of reference intervals was evaluated based on 3-level nested ANOVA. After secondary exclusion using the latent abnormal values exclusion method, reference intervals were derived by a parametric method using the modified Box–Cox formula. Test results of 20 analytes were made traceable to reference measurement procedures. By the ANOVA, significant sex-related and age-related differences were observed in 12 and 12 analytes, respectively. A small regional difference was observed in the results for albumin, glucose, and sodium. Multiple regression analysis revealed BMI-related changes in results of 9 analytes for man and 6 for woman. Reference intervals of 28 analytes were computed with 17 analytes partitioned by sex and/or age. In conclusion, reference intervals of 28 common chemistry analytes applicable to Chinese Han population were established by use of the latest methodology. Reference intervals of 20 analytes traceable to reference measurement procedures can be used as common reference intervals, whereas others can be used as the assay system-specific reference intervals in China. PMID:26945390

40 CFR 408.121 - Specialized definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... those components of a waste water amenable to measurement by the method described in Methods for Chemical Analysis of Water and Wastes, 1971, Environmental Protection Agency, Analytical Quality Control Laboratory, page 217. (c) The term seafood shall mean the raw material, including freshwater and saltwater...

Performance specifications for the extra-analytical phases of laboratory testing: Why and how.

PubMed

Plebani, Mario

2017-07-01

An important priority in the current healthcare scenario should be to address errors in laboratory testing, which account for a significant proportion of diagnostic errors. Efforts made in laboratory medicine to enhance the diagnostic process have been directed toward improving technology, greater volumes and more accurate laboratory tests being achieved, but data collected in the last few years highlight the need to re-evaluate the total testing process (TTP) as the unique framework for improving quality and patient safety. Valuable quality indicators (QIs) and extra-analytical performance specifications are required for guidance in improving all TTP steps. Yet in literature no data are available on extra-analytical performance specifications based on outcomes, and nor is it possible to set any specification using calculations involving biological variability. The collection of data representing the state-of-the-art based on quality indicators is, therefore, underway. The adoption of a harmonized set of QIs, a common data collection and standardised reporting method is mandatory as it will not only allow the accreditation of clinical laboratories according to the International Standard, but also assure guidance for promoting improvement processes and guaranteeing quality care to patients. Copyright © 2017 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Chemical Synthesis Accelerated by Paper Spray: The Haloform Reaction

ERIC Educational Resources Information Center

Bain, Ryan M.; Pulliam, Christopher J.; Raab, Shannon A.; Cooks, R. Graham

2016-01-01

In this laboratory, students perform a synthetic reaction in two ways: (i) by traditional bulk-phase reaction and (ii) in the course of reactive paper spray ionization. Mass spectrometry (MS) is used both as an analytical method and a means of accelerating organic syntheses. The main focus of this laboratory exercise is that the same ionization…

Man vs. Machine: A Junior-level Laboratory Exercise Comparing Human and Instrumental Detection Limits

ERIC Educational Resources Information Center

Elias, Ryan J.; Hopfer, Helene; Hofstaedter, Amanda N.; Hayes, John E.

2017-01-01

The human nose is a very sensitive detector and is able to detect potent aroma compounds down to low ng/L levels. These levels are often below detection limits of analytical instrumentation. The following laboratory exercise is designed to compare instrumental and human methods for the detection of volatile odor active compounds. Reference…

How Work Positions Affect the Research Activity and Information Behaviour of Laboratory Scientists in the Research Lifecycle: Applying Activity Theory

ERIC Educational Resources Information Center

Kwon, Nahyun

2017-01-01

Introduction: This study was conducted to investigate the characteristics of research and information activities of laboratory scientists in different work positions throughout a research lifecycle. Activity theory was applied as the conceptual and analytical framework. Method: Taking a qualitative research approach, in-depth interviews and field…

Insights from a Modular Interdisciplinary Laboratory Course

NASA Astrophysics Data System (ADS)

Bouvier-Brown, N. C.; Carmona, V.

2016-12-01

A laboratory curriculum is naturally oriented towards "hands on" and problem-based learning. An earth science course, like chemical ecology, has the additional advantage of interdisciplinary education. Our Chemical Ecology course at Loyola Marymount University was structured as a small modular workshop. Students first gained hands-on experience with each analytical technique in the laboratory. The class then discussed these first datasets, delved into lecture topics, and tweaked their experimental procedures. Lastly, students were given time to design and execute their own experiments and present their findings. Three-to-four class periods were allotted for each laboratory topic. Detailed information and student reflections will be presented from the Spectroscopy module. Students used the Folin-Ciocalteau reagent method to extract the phenolic content of vegetation and/or soils. Because phenols are produced by plants for defense, this spectroscopic laboratory activity provided insight on allelopathy using analytical chemistry. Students were extremely engaged and learned not only the lab theory and technique, but also its application to our local ecology.

Can Unmanned Aerial Systems (Drones) Be Used for the Routine Transport of Chemistry, Hematology, and Coagulation Laboratory Specimens?

PubMed

Amukele, Timothy K; Sokoll, Lori J; Pepper, Daniel; Howard, Dana P; Street, Jeff

2015-01-01

Unmanned Aerial Systems (UAS or drones) could potentially be used for the routine transport of small goods such as diagnostic clinical laboratory specimens. To the best of our knowledge, there is no published study of the impact of UAS transportation on laboratory tests. Three paired samples were obtained from each one of 56 adult volunteers in a single phlebotomy event (336 samples total): two tubes each for chemistry, hematology, and coagulation testing respectively. 168 samples were driven to the flight field and held stationary. The other 168 samples were flown in the UAS for a range of times, from 6 to 38 minutes. After the flight, 33 of the most common chemistry, hematology, and coagulation tests were performed. Statistical methods as well as performance criteria from four distinct clinical, academic, and regulatory bodies were used to evaluate the results. Results from flown and stationary sample pairs were similar for all 33 analytes. Bias and intercepts were <10% and <13% respectively for all analytes. Bland-Altman comparisons showed a mean difference of 3.2% for Glucose and <1% for other analytes. Only bicarbonate did not meet the strictest (Royal College of Pathologists of Australasia Quality Assurance Program) performance criteria. This was due to poor precision rather than bias. There were no systematic differences between laboratory-derived (analytic) CV's and the CV's of our flown versus terrestrial sample pairs however CV's from the sample pairs tended to be slightly higher than analytic CV's. The overall concordance, based on clinical stratification (normal versus abnormal), was 97%. Length of flight had no impact on the results. Transportation of laboratory specimens via small UASs does not affect the accuracy of routine chemistry, hematology, and coagulation tests results from selfsame samples. However it results in slightly poorer precision for some analytes.

Cotinine analytical workshop report: consideration of analytical methods for determining cotinine in human body fluids as a measure of passive exposure to tobacco smoke.

PubMed Central

Watts, R R; Langone, J J; Knight, G J; Lewtas, J

1990-01-01

A two-day technical workshop was convened November 10-11, 1986, to discuss analytical approaches for determining trace amounts of cotinine in human body fluids resulting from passive exposure to environmental tobacco smoke (ETS). The workshop, jointly sponsored by the U.S. Environmental Protection Agency and Centers for Disease Control, was attended by scientists with expertise in cotinine analytical methodology and/or conduct of human monitoring studies related to ETS. The workshop format included technical presentations, separate panel discussions on chromatography and immunoassay analytical approaches, and group discussions related to the quality assurance/quality control aspects of future monitoring programs. This report presents a consensus of opinion on general issues before the workshop panel participants and also a detailed comparison of several analytical approaches being used by the various represented laboratories. The salient features of the chromatography and immunoassay analytical methods are discussed separately. PMID:2190812

Laboratory issues: use of nutritional biomarkers.

PubMed

Blanck, Heidi Michels; Bowman, Barbara A; Cooper, Gerald R; Myers, Gary L; Miller, Dayton T

2003-03-01

Biomarkers of nutritional status provide alternative measures of dietary intake. Like the error and variation associated with dietary intake measures, the magnitude and impact of both biological (preanalytical) and laboratory (analytical) variability need to be considered when one is using biomarkers. When choosing a biomarker, it is important to understand how it relates to nutritional intake and the specific time frame of exposure it reflects as well as how it is affected by sampling and laboratory procedures. Biological sources of variation that arise from genetic and disease states of an individual affect biomarkers, but they are also affected by nonbiological sources of variation arising from specimen collection and storage, seasonality, time of day, contamination, stability and laboratory quality assurance. When choosing a laboratory for biomarker assessment, researchers should try to make sure random and systematic error is minimized by inclusion of certain techniques such as blinding of laboratory staff to disease status and including external pooled standards to which laboratory staff are blinded. In addition analytic quality control should be ensured by use of internal standards or certified materials over the entire range of possible values to control method accuracy. One must consider the effect of random laboratory error on measurement precision and also understand the method's limit of detection and the laboratory cutpoints. Choosing appropriate cutpoints and reducing error is extremely important in nutritional epidemiology where weak associations are frequent. As part of this review, serum lipids are included as an example of a biomarker whereby collaborative efforts have been put forth to both understand biological sources of variation and standardize laboratory results.

Towards European urinalysis guidelines. Introduction of a project under European Confederation of Laboratory Medicine.

PubMed

Kouri, T T; Gant, V A; Fogazzi, G B; Hofmann, W; Hallander, H O; Guder, W G

2000-07-01

Improved standardized performance is needed because urinalysis continues to be one of the most frequently requested laboratory tests. Since 1997, the European Confederation of Laboratory Medicine (ECLM) has been supporting an interdisciplinary project aiming to produce European urinalysis guidelines. More than seventy clinical chemists, microbiologists and ward-based clinicians, as well as representatives of manufacturers are taking part. These guidelines aim to improve the quality and consistency of chemical urinalysis, particle counting and bacterial culture by suggesting optimal investigative processes that could be applied in Europe. The approach is based on medical needs for urinalysis. The importance of the pre-analytical stage for total quality is stressed by detailed illustrative advice for specimen collection. Attention is also given to emerging automated technology. For cost containment reasons, both optimum (ideal) procedures and minimum analytical approaches are suggested. Since urinalysis mostly lacks genuine reference methods (primary reference measurement procedures; Level 4), a novel classification of the methods is proposed: comparison measurement procedures (Level 3), quantitative routine procedures (Level 2), and ordinal scale examinations (Level 1). Stepwise strategies are suggested to save costs, applying different rules for general and specific patient populations. New analytical quality specifications have been created. After a consultation period, the final written text will be published in full as a separate document.

Results of the U.S. Geological Survey's Analytical Evaluation Program for standard reference samples distributed in March 1999

USGS Publications Warehouse

Farrar, Jerry W.; Chleboun, Kimberly M.

1999-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for 8 standard reference samples -- T-157 (trace constituents), M-150 (major constituents), N-61 (nutrient constituents), N-62 (nutrient constituents), P-32 (low ionic strength constituents), GWT-5 (ground-water trace constituents), GWM- 4 (ground-water major constituents),and Hg-28 (mercury) -- that were distributed in March 1999 to 120 laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 111 of the laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the seven reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the 8 standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

External quality assessment of medical laboratories in Croatia: preliminary evaluation of post-analytical laboratory testing.

PubMed

Krleza, Jasna Lenicek; Dorotic, Adrijana; Grzunov, Ana

2017-02-15

Proper standardization of laboratory testing requires assessment of performance after the tests are performed, known as the post-analytical phase. A nationwide external quality assessment (EQA) scheme implemented in Croatia in 2014 includes a questionnaire on post-analytical practices, and the present study examined laboratory responses in order to identify current post-analytical phase practices and identify areas for improvement. In four EQA exercises between September 2014 and December 2015, 145-174 medical laboratories across Croatia were surveyed using the Module 11 questionnaire on the post-analytical phase of testing. Based on their responses, the laboratories were evaluated on four quality indicators: turnaround time (TAT), critical values, interpretative comments and procedures in the event of abnormal results. Results were presented as absolute numbers and percentages. Just over half of laboratories (56.3%) monitored TAT. Laboratories varied substantially in how they dealt with critical values. Most laboratories (65-97%) issued interpretative comments with test results. One third of medical laboratories (30.6-33.3%) issued abnormal test results without confirming them in additional testing. Our results suggest that the nationwide post-analytical EQA scheme launched in 2014 in Croatia has yet to be implemented to the full. To close the gaps between existing recommendations and laboratory practice, laboratory professionals should focus on ensuring that TAT is monitored and lists of critical values are established within laboratories. Professional bodies/institutions should focus on clarify and harmonized rules to standardized practices and applied for adding interpretative comments to laboratory test results and for dealing with abnormal test results.

ENVIRONMENTAL IMMUNOCHEMISTRY AT THE U.S. EPA, NATIONAL EXPOSURE RESEARCH LABORATORY'S HUMAN EXPOSURE BRANCH

EPA Science Inventory

Immunoehemical methods are responding to the changing needs of regulatory and monitoring programs and are meeting new analytical challenges as they arise. Recent advances in environmental immunoehemistry have expanded the role of immunoassays from field screening methods to hig...

Per- and Polyfluoroalkyl Substances (PFAS): Sampling ...

EPA Pesticide Factsheets

Per- and polyfluoroalkyl substances (PFAS) are a large group of manufactured compounds used in a variety of industries, such as aerospace, automotive, textiles, and electronics, and are used in some food packaging and firefighting materials. For example, they may be used to make products more resistant to stains, grease and water. In the environment, some PFAS break down very slowly, if at all, allowing bioaccumulation (concentration) to occur in humans and wildlife. Some have been found to be toxic to laboratory animals, producing reproductive, developmental, and systemic effects in laboratory tests. EPA's methods for analyzing PFAS in environmental media are in various stages of development. This technical brief summarizes the work being done to develop robust analytical methods for groundwater, surface water, wastewater, and solids, including soils, sediments, and biosolids. The U.S. Environmental Protection Agency’s (EPA) methods for analyzing PFAS in environmental media are in various stages of development. EPA is working to develop robust analytical methods for groundwater, surface water, wastewater, and solids, including soils, sediments, and biosolids.

High Throughput Analytical Techniques for the Determination and Confirmation of Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea by GC/MS, GC/MS/MS, and LC/MS/MS: Collaborative Study, First Action 2014.09.

PubMed

Pang, Guo-Fang; Fan, Chun-Lin; Cao, Yan-Zhong; Yan, Fang; Li, Yan; Kang, Jian; Chen, Hui; Chang, Qiao-Ying

2015-01-01

Thirty laboratories from fom North and South America, Europe, and Asia participated in this AOAC collaborative study (15 from China; five from Germany; two each from Italy and the United States; and one each from the Republic of Korea, Canada, Spain, Japan, Belgium, and India). Participants represented government regulatory, commercial testing, university, research institute, and private laboratories. The single-laboratory validated (SLV) tea method was evaluated in the collaborative study to determine the recovery and reproducibility of the method under multilaboratory conditions. Since there were no restrictions regarding the type of analytical instrumentation to use for the analyses, laboratories used a combination of equipment that included GC/MS, GC/MS/MS, and LC/MS/MS instruments from 22 different manufacturers, 21 brands of GC and LC columns, 13 different GC temperature programming profiles, 11 LC gradient elution programs, and six different vendor manufactured SPE cartridges. Even though all the analytical performance parameters for all the 653 compounds had been determined in the SLV study, guidance was obtained from an expert review panel of the AOAC Method-Centric Committee on Pesticide Residues to conduct the multilaboratory collaborative study based on 20 selected compounds that can be analyzed by GC/MS and 20 compounds that can be analyzed by LC/MS/MS. Altogether, 560 samples covering the 40 selected pesticides were analyzed in the study. These samples included green tea and oolong tea samples fortified typically at the European Union maximum residue limit for regulatory guidance and compliance, aged tea samples incurred with 20 pesticides, and green tea and oolong tea samples incurred with five pesticides. The analysis of the 560 samples generated a total of 82 459 test results by the 30 participating laboratories. One laboratory failed to meet the proficiency requirements in the precollaborative study. Therefore, its data submitted for the collaborative study were excluded from further analysis and interpretation. The results presented are therefore the 6638 analytical results obtained from the 29 remaining laboratories, which included 1977 results generated by GC/MS, 1704 results by GC/MS/MS, and 2957 results by LC/MS/MS. It was determined after application of the Grubbs and Dixon tests for outliers to the data sets that there were 65 outlier results from the 1977 GC/MS results (3.3%), 65 outlier results from the 1704 GC/MS/MS results (3.8%), and 57 outlier results out of 2957 LC/MS/MS results (1.9%), representing 0.98, 0.98, and 0.86%, respectively, of the 6638 results generated in the study. Analysis with the AOAC statistical software package also confirmed that the method is rugged, and average recovery, average concentration, RSDr, RSDR, and HorRat values all meet recovery and reproducibility criteria for use in multiple laboratories. The Study Director is recommending this method for adoption as an AOAC First Action Official MethodSM.

Analytical methods of the U.S. Geological Survey's New York District Water-Analysis Laboratory

USGS Publications Warehouse

Lawrence, Gregory B.; Lincoln, Tricia A.; Horan-Ross, Debra A.; Olson, Mark L.; Waldron, Laura A.

1995-01-01

The New York District of the U.S. Geological Survey (USGS) in Troy, N.Y., operates a water-analysis laboratory for USGS watershed-research projects in the Northeast that require analyses of precipitation and of dilute surface water and soil water for major ions; it also provides analyses of certain chemical constituents in soils and soil gas samples.This report presents the methods for chemical analyses of water samples, soil-water samples, and soil-gas samples collected in wateshed-research projects. The introduction describes the general materials and technicques for each method and explains the USGS quality-assurance program and data-management procedures; it also explains the use of cross reference to the three most commonly used methods manuals for analysis of dilute waters. The body of the report describes the analytical procedures for (1) solution analysis, (2) soil analysis, and (3) soil-gas analysis. The methods are presented in alphabetical order by constituent. The method for each constituent is preceded by (1) reference codes for pertinent sections of the three manuals mentioned above, (2) a list of the method's applications, and (3) a summary of the procedure. The methods section for each constitutent contains the following categories: instrumentation and equipment, sample preservation and storage, reagents and standards, analytical procedures, quality control, maintenance, interferences, safety considerations, and references. Sufficient information is presented for each method to allow the resulting data to be appropriately used in environmental investigations.

Development of Gold Standard Ion-Selective Electrode-Based Methods for Fluoride Analysis

PubMed Central

Martínez-Mier, E.A.; Cury, J.A.; Heilman, J.R.; Katz, B.P.; Levy, S.M.; Li, Y.; Maguire, A.; Margineda, J.; O’Mullane, D.; Phantumvanit, P.; Soto-Rojas, A.E.; Stookey, G.K.; Villa, A.; Wefel, J.S.; Whelton, H.; Whitford, G.M.; Zero, D.T.; Zhang, W.; Zohouri, V.

2011-01-01

Background/Aims: Currently available techniques for fluoride analysis are not standardized. Therefore, this study was designed to develop standardized methods for analyzing fluoride in biological and nonbiological samples used for dental research. Methods A group of nine laboratories analyzed a set of standardized samples for fluoride concentration using their own methods. The group then reviewed existing analytical techniques for fluoride analysis, identified inconsistencies in the use of these techniques and conducted testing to resolve differences. Based on the results of the testing undertaken to define the best approaches for the analysis, the group developed recommendations for direct and microdiffusion methods using the fluoride ion-selective electrode. Results Initial results demonstrated that there was no consensus regarding the choice of analytical techniques for different types of samples. Although for several types of samples, the results of the fluoride analyses were similar among some laboratories, greater differences were observed for saliva, food and beverage samples. In spite of these initial differences, precise and true values of fluoride concentration, as well as smaller differences between laboratories, were obtained once the standardized methodologies were used. Intraclass correlation coefficients ranged from 0.90 to 0.93, for the analysis of a certified reference material, using the standardized methodologies. Conclusion The results of this study demonstrate that the development and use of standardized protocols for F analysis significantly decreased differences among laboratories and resulted in more precise and true values. PMID:21160184

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; arsenic speciation in natural-water samples using laboratory and field methods

USGS Publications Warehouse

Garbarino, John R.; Bednar, Anthony J.; Burkhardt, Mark R.

2002-01-01

Analytical methods for the determination of arsenite [As(III)], arsenate [As(V)], dimethylarsinate (DMA), monomethylarsonate (MMA), and roxarsone in filtered natural-water samples are described. Various analytical methods can be used for the determination, depending on the arsenic species being determined. Arsenic concentration is determined by using inductively coupled plasma-mass spectrometry (ICP-MS) as an arsenic-specific detector for all methods. Laboratory-speciation methods are described that use an ion chromatographic column to separate the arsenic species; the column length, column packing, and mobile phase are dependent on the species of interest. Regardless of the separation technique, the arsenic species are introduced into plasma by eithe rpneumatic nebulization or arsine generation. Analysis times range from 2 to 8 minutes and method detection limits range from 0.1 to 0.6 microgram-arsenic per liter (ug-As/L), 10 to 60 picograms absolute (for a 100-microliter injection), depending on the arsenic species determined and the analytical method used. A field-generation specciation method also is described that uses a strong anion exchange cartridge to separate As(III) from As(V) in the field. As(III) in the eluate and the As(V) in the cartridge extract are determined by direct nebulization ICP-MS. Methylated arsenic species that also are retained on the cartridge will positively bias As(V) results without further laboratory separations. The method detection limit for field speciation is 0.3 ug-As/L. The distribution of arsenic species must be preserved in the field to eliminate changes caused by photochemical oxidation or metal oxyhydroxide precipitation. Preservation techniques, such as refrigeration, the addition of acides, or the additoin of ethylene-diaminetetraacetic acid (EDTA) and the effects of ambient light were tested. Of the preservatives evaluated, EDTA was found to work best with the laboratory- and field-speciation methods for all sample matrices tested. Storing the samples in opaque polytethylene bottles eliminated the effects of photochemical oxidation. The percentage change in As(III):As(V) ratios for an EDTA-preserved acid mine drainage (AMD) sample and ground-water sample during a 3-month period was -5 percent and +3 percent, respectively. The bias and variability of the methods were evaluated by comparing results for total arsenic and As(III), As(V), DMA, and MMA concentrations in ground water, AMD, and surface water. Seventy-one ground-water, 10 AMD, and 24 surface-water samples were analyzed. Concentrations in ground-water samples reached 720 ug-As/L for As(III) and 1080 ug-As/L for As(V); AMD samples reached 12800 ug-As/L for As(III) and 7050 ug-As/L for As(V); and surface-water samples reached 5 ug-As/L for As(III) and As(V). Inorganic arsenic species distribution in the samples ranged from 0 to 90 percent As(III). DMA and MMA were present only in surface-water samples from agricultural areas where the herbicide monosodium methylarsonate was applied; concentrations never exceeded 6 ug-As/L. Statistical analyses indicated that the difference between As(III) and As(V) concentrations for samples preserved with EDTA in opaque bottles and field-speciation results were analytically insignificant at the 95-percent confidence interval. There was no significant difference among the methods tested for total arsenic concentration. Percentage recovery for field samples spiked at 50 ug-As/L and analyzed by the laboratory-speciation method (n=2) ranged from 82 to 100 percent for As(III), 97 to 102 percent for As(V), 90 to 104 percent for DMA, and 81 to 96 percent for MMA; recoveries for samples spiked at 100 ug-As/L and analyzed by the field-speciation method ranged from 102 to 107 percent for As(III) and 105 to 106 percent for As(V). Laboratory-speciation results for Environment Canada reference material SLRS-2 closely matched reported concentrations. Laboratory-speciation metho

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of selected carbamate pesticides in water by high-performance liquid chromatography

USGS Publications Warehouse

Werner, S.L.; Johnson, S.M.

1994-01-01

As part of its primary responsibility concerning water as a national resource, the U.S. Geological Survey collects and analyzes samples of ground water and surface water to determine water quality. This report describes the method used since June 1987 to determine selected total-recoverable carbamate pesticides present in water samples. High- performance liquid chromatography is used to separate N-methyl carbamates, N-methyl carbamoyloximes, and an N-phenyl carbamate which have been extracted from water and concentrated in dichloromethane. Analytes, surrogate compounds, and reference compounds are eluted from the analytical column within 25 minutes. Two modes of analyte detection are used: (1) a photodiode-array detector measures and records ultraviolet-absorbance profiles, and (2) a fluorescence detector measures and records fluorescence from an analyte derivative produced when analyte hydrolysis is combined with chemical derivatization. Analytes are identified and confirmed in a three-stage process by use of chromatographic retention time, ultraviolet (UV) spectral comparison, and derivatization/fluorescence detection. Quantitative results are based on the integration of single-wavelength UV-absorbance chromatograms and on comparison with calibration curves derived from external analyte standards that are run with samples as part of an instrumental analytical sequence. Estimated method detection limits vary for each analyte, depending on the sample matrix conditions, and range from 0.5 microgram per liter to as low as 0.01 microgram per liter. Reporting levels for all analytes have been set at 0.5 microgram per liter for this method. Corrections on the basis of percentage recoveries of analytes spiked into distilled water are not applied to values calculated for analyte concentration in samples. These values for analyte concentrations instead indicate the quantities recovered by the method from a particular sample matrix.

Sampling and sample processing in pesticide residue analysis.

PubMed

Lehotay, Steven J; Cook, Jo Marie

2015-05-13

Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion.

Uptake of recommended common reference intervals for chemical pathology in Australia.

PubMed

Jones, Graham Rd; Koetsier, Sabrina

2017-05-01

Background Reference intervals are a vital part of reporting numerical pathology results. It is known, however, that variation in reference intervals between laboratories is common, even when analytical methods support common reference intervals. In response to this, in Australia, the Australasian Association of Clinical Biochemists together with the Royal College of Pathologists of Australasia published in 2014 a set of recommended common reference intervals for 11 common serum analytes (sodium, potassium, chloride, bicarbonate, creatinine male, creatinine female, calcium, calcium adjusted for albumin, phosphate, magnesium, lactate dehydrogenase, alkaline phosphatase and total protein). Methods Uptake of recommended common reference intervals in Australian laboratories was assessed using data from four annual cycles of the RCPAQAP reference intervals external quality assurance programme. Results Over three years, from 2013 to 2016, the use of the recommended upper and lower reference limits has increased from 40% to 83%. Nearly half of the intervals in use by enrolled laboratories in 2016 have been changed in this time period, indicating an active response to the guidelines. Conclusions These data support the activities of the Australasian Association of Clinical Biochemists and Royal College of Pathologists of Australasia in demonstrating a change in laboratory behaviour to reduce unnecessary variation in reference intervals and thus provide a consistent message to doctor and patients irrespective of the laboratory used.

EPA Method 1615. Measurement of Enterovirus and Norovirus Occurrence in Water by Culture and RT-qPCR. II. Total Culturable Virus Assay

EPA Science Inventory

A standardized method is required when national studies on virus occurrence in environmental and drinking waters utilize multiple analytical laboratories. The U.S Environmental Protection Agency’s (USEPA) Method 1615 was developed with the goal of providing such a standard ...

Evaluation of a multiclass, multiresidue liquid chromatography-tandem mass spectrometry method for analysis of 120 veterinary drugs in bovine kidney

USDA-ARS?s Scientific Manuscript database

Traditionally, regulatory monitoring of veterinary drug residues in food animal tissues involves the use of several single-class methods to cover a wide analytical scope. Multiclass, multiresidue methods of analysis tend to provide greater overall laboratory efficiency than the use of multiple meth...

Atomic spectrometry and trends in clinical laboratory medicine

NASA Astrophysics Data System (ADS)

Parsons, Patrick J.; Barbosa, Fernando

2007-09-01

Increasing numbers of clinical laboratories are transitioning away from flame and electrothermal AAS methods to those based on ICP-MS. Still, for many laboratories, the choice of instrumentation is based upon (a) the element(s) to be determined, (b) the matrix/matrices to be analyzed, and (c) the expected concentration(s) of the analytes in the matrix. Most clinical laboratories specialize in measuring Se, Zn, Cu, and Al in serum, and/or Pb, Cd, Hg, As, and Cr in blood and/or urine, while other trace elements (e.g., Pt, Au etc.) are measured for therapeutic purposes. Quantitative measurement of elemental species is becoming more widely accepted for nutritional and/or toxicological screening purposes, and ICP-MS interfaced with separation techniques, such as liquid chromatography or capillary electrophoresis, offers the advantage of on-line species determination coupled with very low detection limits. Polyatomic interferences for some key elements such as Se, As, and Cr require instrumentation equipped with dynamic reaction cell or collision cell technologies, or might even necessitate the use of sector field ICP-MS, to assure accurate results. Nonetheless, whatever analytical method is selected for the task, careful consideration must be given both to specimen collection procedures and to the control of pre-analytical variables. Finally, all methods benefit from access to reliable certified reference materials (CRMs). While a variety of reference materials (RMs) are available for trace element measurements in clinical matrices, not all can be classified as CRMs. The major metrological organizations (e.g., NIST, IRMM, NIES) provide a limited number of clinical CRMs, however, secondary reference materials are readily available from commercial organizations and organizers of external quality assessment schemes.

Avoiding pitfalls in the determination of halocarboxylic acids: the photochemistry of methylation.

PubMed

Rubio, F J; Urbansky, E T; Magnuson, M L

2000-06-01

Haloethanoic (haloacetic) acids are formed during chlorination of drinking water and are regulated by the Environmental Protection Agency (EPA). These compounds are normally quantified by gas chromatography with electron capture detection (GC-ECD) as the methyl esters. EPA Method 552 uses diazomethane (CH2N2) for this purpose, but has only been validated by EPA for HAA6: chloro-, dichloro-, bromo-, dibromo-, bromochloro- and trichloroacetic acids. EPA Method 552.2 was developed and validated for all nine analytes (HAA9 = HAA6 + dibromochloro-, bromodichloro- and tribromoethanoic acids). Since the promulgation of Method 552.2, which uses acidic methanol, a debate has ensued over discrepancies observed by various laboratories when using diazomethane instead. In an effort to identify and eliminate potential sources for these discrepancies, a comparative study was undertaken for HAA9. Better accuracy and precision were observed for all HAA9 species by Method 552.2; recoveries were satisfactory in de-ionized and tap water. Method 552 remains satisfactory for HAA6. Systematic differences in instrumental response are observed for the two methods, but these are precise and may be accounted for using similarly treated standards and analyte-fortified (spiked) samples. That notwithstanding, Method 552 (CH2N2) was shown to be unsuitable for dibromochloro-, bromodichloro- and tribromoethanoic acids (HAA9-6). The primary problem appears to be a photoactivated reaction between diazomethane and the HAA9-6 analytes; however, side reactions were found to occur even in the dark. Analyte loss is most pronounced under typical laboratory lighting (white F40 fluorescent lamps + sunlight), but it is also observed under Philips gold F40 lamps (lambda > or = 520 nm), and in the dark.

Analytical method for nitroaromatic explosives in radiologically contaminated soil for ISO/IEC 17025 accreditation

DOE PAGES

Boggess, Andrew; Crump, Stephen; Gregory, Clint; ...

2017-12-06

Here, unique hazards are presented in the analysis of radiologically contaminated samples. Strenuous safety and security precautions must be in place to protect the analyst, laboratory, and instrumentation used to perform analyses. A validated method has been optimized for the analysis of select nitroaromatic explosives and degradative products using gas chromatography/mass spectrometry via sonication extraction of radiologically contaminated soils, for samples requiring ISO/IEC 17025 laboratory conformance. Target analytes included 2-nitrotoluene, 4-nitrotoluene, 2,6-dinitrotoluene, and 2,4,6-trinitrotoluene, as well as the degradative product 4-amino-2,6-dinitrotoluene. Analytes were extracted from soil in methylene chloride by sonication. Administrative and engineering controls, as well as instrument automationmore » and quality control measures, were utilized to minimize potential human exposure to radiation at all times and at all stages of analysis, from receiving through disposition. Though thermal instability increased uncertainties of these selected compounds, a mean lower quantitative limit of 2.37 µg/mL and mean accuracy of 2.3% relative error and 3.1% relative standard deviation were achieved. Quadratic regression was found to be optimal for calibration of all analytes, with compounds of lower hydrophobicity displaying greater parabolic curve. Blind proficiency testing (PT) of spiked soil samples demonstrated a mean relative error of 9.8%. Matrix spiked analyses of PT samples demonstrated that 99% recovery of target analytes was achieved. To the knowledge of the authors, this represents the first safe, accurate, and reproducible quantitative method for nitroaromatic explosives in soil for specific use on radiologically contaminated samples within the constraints of a nuclear analytical lab.« less

Analytical method for nitroaromatic explosives in radiologically contaminated soil for ISO/IEC 17025 accreditation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boggess, Andrew; Crump, Stephen; Gregory, Clint

Here, unique hazards are presented in the analysis of radiologically contaminated samples. Strenuous safety and security precautions must be in place to protect the analyst, laboratory, and instrumentation used to perform analyses. A validated method has been optimized for the analysis of select nitroaromatic explosives and degradative products using gas chromatography/mass spectrometry via sonication extraction of radiologically contaminated soils, for samples requiring ISO/IEC 17025 laboratory conformance. Target analytes included 2-nitrotoluene, 4-nitrotoluene, 2,6-dinitrotoluene, and 2,4,6-trinitrotoluene, as well as the degradative product 4-amino-2,6-dinitrotoluene. Analytes were extracted from soil in methylene chloride by sonication. Administrative and engineering controls, as well as instrument automationmore » and quality control measures, were utilized to minimize potential human exposure to radiation at all times and at all stages of analysis, from receiving through disposition. Though thermal instability increased uncertainties of these selected compounds, a mean lower quantitative limit of 2.37 µg/mL and mean accuracy of 2.3% relative error and 3.1% relative standard deviation were achieved. Quadratic regression was found to be optimal for calibration of all analytes, with compounds of lower hydrophobicity displaying greater parabolic curve. Blind proficiency testing (PT) of spiked soil samples demonstrated a mean relative error of 9.8%. Matrix spiked analyses of PT samples demonstrated that 99% recovery of target analytes was achieved. To the knowledge of the authors, this represents the first safe, accurate, and reproducible quantitative method for nitroaromatic explosives in soil for specific use on radiologically contaminated samples within the constraints of a nuclear analytical lab.« less

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by Carbopak-B solid-phase extraction and high-preformance liquid chromatography

USGS Publications Warehouse

Werner, Stephen L.; Burkhardt, Mark R.; DeRusseau, Sabrina N.

1996-01-01

In accordance with the needs of the National Water-Quality Assessment Program (NAWQA), the U.S. Geological Survey has developed and implemented a graphitized carbon-based solid-phase extraction and high-performance liquid chromatographic analytical method. The method is used to determine 41 pesticides and pesticide metabolites that are not readily amenable to gas chromatography or other high-temperature analytical techniques. Pesticides are extracted from filtered environmental water samples using a 0.5-gram graphitized carbon-based solid-phase cartridge, eluted from the cartridge into two analytical fractions, and analyzed using high-performance liquid chromatography with photodiode-array detection. The upper concentration limit is 1.6 micrograms per liter (=B5g/L) for most compounds. Single-operator method detection limits in organic-free water samples ranged from 0.006 to 0.032 =B5g/L= Recoveries in organic-free water samples ranged from 37 to 88 percent. Recoveries in ground- and surface-water samples ranged from 29 to 94 percent. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time of 7 days.

Determination of Selected Perfluorinated Alkyl Acids in ...

EPA Pesticide Factsheets

The 1996 amendments to the Safe Drinking Water Act (SDWA) required EPA to establish a Contaminant Candidate List (CCL), that contains a list of drinking water contaminants that the Agency will consider for future regulation. EPA must make a regulatory determination on a minimum of five contaminants every five years. The first CCL was published in 1998, and updates were anticipated every five years thereafter. One of the key pieces of information that must be available in order to make a regulatory determination is nationwide occurrence data for the chemical contaminants under consideration. Historically, EPA has collected the necessary occurrence data under its Unregulated Contaminant Monitoring Regulations (UCMR). Under the UCMR, monitoring is conducted at selected drinking water utilities for specific contaminants of interest. The chemical analyses are usually performed by the utilities or by commercial laboratories. To meet the requirements of monitoring under the UCMR program, the analytical methods developed should be specific, sensitive, and practical enough for application in commercial laboratories. This task will focus on the development of analytical methods for chemicals identified on future CCLs or emerging contaminants not yet listed on the CCL. These methods will be used for the collection of occurrence data under future UCMRs. The objective of this research effort is to develop analytical methods to be used to measure the occurrence of

[Enzymatic analysis of the quality of foodstuffs].

PubMed

Kolesnov, A Iu

1997-01-01

Enzymatic analysis is an independent and separate branch of enzymology and analytical chemistry. It has become one of the most important methodologies used in food analysis. Enzymatic analysis allows the quick, reliable determination of many food ingredients. Often these contents cannot be determined by conventional methods, or if methods are available, they are determined only with limited accuracy. Today, methods of enzymatic analysis are being increasingly used in the investigation of foodstuffs. Enzymatic measurement techniques are used in industry, scientific and food inspection laboratories for quality analysis. This article describes the requirements of an optimal analytical method: specificity, sample preparation, assay performance, precision, sensitivity, time requirement, analysis cost, safety of reagents.

BIOSENSORS FOR ENVIRONMENTAL MONITORING: A REGULATORY PERSPECTIVE

EPA Science Inventory

Biosensors show the potential to complement laboratory-based analytical methods for environmental applications. Although biosensors for potential environmental-monitoring applications have been reported for a wide range of environmental pollutants, from a regulatory perspective, ...

Low/Medium Volatile Data Validation

EPA Pesticide Factsheets

Document designed to offer data reviewers guidance in determining the validity of analytical data generated through the US EPA Contract Laboratory Program Statement of Work ISM01.X Inorganic Superfund Methods (Multi-Media, Multi-Concentration)

Body fluid analysis: clinical utility and applicability of published studies to guide interpretation of today's laboratory testing in serous fluids.

PubMed

Block, Darci R; Algeciras-Schimnich, Alicia

2013-01-01

Requests for testing various analytes in serous fluids (e.g., pleural, peritoneal, pericardial effusions) are submitted daily to clinical laboratories. Testing of these fluids deviates from assay manufacturers' specifications, as most laboratory assays are optimized for testing blood or urine specimens. These requests add a burden to clinical laboratories, which need to validate assay performance characteristics in these fluids to exclude matrix interferences (given the different composition of body fluids) while maintaining regulatory compliance. Body fluid testing for a number of analytes has been reported in the literature; however, understanding the clinical utility of these analytes is critical because laboratories must address the analytic and clinical validation requirements, while educating clinicians on proper test utilization. In this article, we review the published data to evaluate the clinical utility of testing for numerous analytes in body fluid specimens. We also highlight the pre-analytic and analytic variables that need to be considered when reviewing published studies in body fluid testing. Finally, we provide guidance on how published studies might (or might not) guide interpretation of test results in today's clinical laboratories.

Bias Assessment of General Chemistry Analytes using Commutable Samples.

PubMed

Koerbin, Gus; Tate, Jillian R; Ryan, Julie; Jones, Graham Rd; Sikaris, Ken A; Kanowski, David; Reed, Maxine; Gill, Janice; Koumantakis, George; Yen, Tina; St John, Andrew; Hickman, Peter E; Simpson, Aaron; Graham, Peter

2014-11-01

Harmonisation of reference intervals for routine general chemistry analytes has been a goal for many years. Analytical bias may prevent this harmonisation. To determine if analytical bias is present when comparing methods, the use of commutable samples, or samples that have the same properties as the clinical samples routinely analysed, should be used as reference samples to eliminate the possibility of matrix effect. The use of commutable samples has improved the identification of unacceptable analytical performance in the Netherlands and Spain. The International Federation of Clinical Chemistry and Laboratory Medicine (IFCC) has undertaken a pilot study using commutable samples in an attempt to determine not only country specific reference intervals but to make them comparable between countries. Australia and New Zealand, through the Australasian Association of Clinical Biochemists (AACB), have also undertaken an assessment of analytical bias using commutable samples and determined that of the 27 general chemistry analytes studied, 19 showed sufficiently small between method biases as to not prevent harmonisation of reference intervals. Application of evidence based approaches including the determination of analytical bias using commutable material is necessary when seeking to harmonise reference intervals.

40 CFR 408.141 - Specialized definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... apply to this subpart. (b) The term oil and grease shall mean those components of a waste water amenable to measurement by the method described in Methods for Chemical Analysis of Water and Wastes, 1971, Environmental Protection Agency, Analytical Quality Control Laboratory, page 217. (c) The term seafood shall...

40 CFR 408.11 - Specialized definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... apply to this subpart. (b) The term oil and grease shall mean those components of a waste water amenable to measurement by the method described in Methods for Chemical Analysis of Water and Wastes, 1971, Environmental Protection Agency, Analytical Quality Control Laboratory, page 217. (c) The term seafood shall...

40 CFR 408.51 - Specialized definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... apply to this subpart. (b) The term oil and grease shall mean those components of a waste water amenable to measurement by the method described in Methods for Chemical Analysis of Water and Wastes, 1971, Environmental Protection Agency, Analytical Quality Control Laboratory, page 217. (c) The term seafood shall...

European specialist porphyria laboratories: diagnostic strategies, analytical quality, clinical interpretation, and reporting as assessed by an external quality assurance program.

PubMed

Aarsand, Aasne K; Villanger, Jørild H; Støle, Egil; Deybach, Jean-Charles; Marsden, Joanne; To-Figueras, Jordi; Badminton, Mike; Elder, George H; Sandberg, Sverre

2011-11-01

The porphyrias are a group of rare metabolic disorders whose diagnosis depends on identification of specific patterns of porphyrin precursor and porphyrin accumulation in urine, blood, and feces. Diagnostic tests for porphyria are performed by specialized laboratories in many countries. Data regarding the analytical and diagnostic performance of these laboratories are scarce. We distributed 5 sets of multispecimen samples from different porphyria patients accompanied by clinical case histories to 18-21 European specialist porphyria laboratories/centers as part of a European Porphyria Network organized external analytical and postanalytical quality assessment (EQA) program. The laboratories stated which analyses they would normally have performed given the case histories and reported results of all porphyria-related analyses available, interpretative comments, and diagnoses. Reported diagnostic strategies initially showed considerable diversity, but the number of laboratories applying adequate diagnostic strategies increased during the study period. We found an average interlaboratory CV of 50% (range 12%-152%) for analytes in absolute concentrations. Result normalization by forming ratios to the upper reference limits did not reduce this variation. Sixty-five percent of reported results were within biological variation-based analytical quality specifications. Clinical interpretation of the obtained analytical results was accurate, and most laboratories established the correct diagnosis in all distributions. Based on a case-based EQA scheme, variations were apparent in analytical and diagnostic performance between European specialist porphyria laboratories. Our findings reinforce the use of EQA schemes as an essential tool to assess both analytical and diagnostic processes and thereby to improve patient care in rare diseases.

Chemicals of emerging concern in water and bottom sediment in the Great Lakes Basin, 2012: collection methods, analytical methods, quality assurance, and study data

USGS Publications Warehouse

Lee, Kathy E.; Langer, Susan K.; Menheer, Michael A.; Hansen, Donald S.; Foreman, William T.; Furlong, Edward T.; Jorgenson, Zachary G.; Choy, Steven J.; Moore, Jeremy N.; Banda, JoAnn; Gefell, Daniel J.

2015-01-01

During this study, 53 environmental samples, 4 field duplicate samples, and 8 field spike samples of bottom sediment and laboratory matrix-spike samples were analyzed for a wide variety of CECs at the USGS National Water Quality Laboratory using laboratory schedule 5433 for wastewater indicators; research method 6434 for steroid hormones, sterols, and bisphenol A; and research method 9008 for human-use pharmaceuticals and antidepressants. Forty of the 57 chemicals analyzed using laboratory schedule 5433 had detectable concentrations ranging from 1 to 49,000 micrograms per kilogram. Fourteen of the 20 chemicals analyzed using research method 6434 had detectable concentrations ranging from 0.04 to 24,940 nanograms per gram. Ten of the 20 chemicals analyzed using research method 9008 had detectable concentrations ranging from 0.59 to 197.5 micrograms per kilogram. Five of the 11 chemicals analyzed using research method 9008 had detectable concentrations ranging from 1.16 to 25.0 micrograms per kilogram.

Multi-Agency Radiological Laboratory Analytical Protocols Manual (MARLAP)

EPA Pesticide Factsheets

The Multi-Agency Radiological Laboratory Analytical Protocols Manual (MARLAP) provides guidance for the planning, implementation and assessment phases of projects that require laboratory analysis of radionuclides.

Steroid hormone analysis in diagnosis and treatment of DSD: position paper of EU COST Action BM 1303 'DSDnet'.

PubMed

Kulle, A; Krone, N; Holterhus, P M; Schuler, G; Greaves, R F; Juul, A; de Rijke, Y B; Hartmann, M F; Saba, A; Hiort, O; Wudy, S A

2017-05-01

Disorders or differences in sex development (DSD) comprise a heterogeneous group of conditions with an atypical sex development. For optimal diagnosis, highly specialised laboratory analyses are required across European countries. Working group 3 of EU COST (European Cooperation in Science and Technology) Action BM 1303 'DSDnet' 'Harmonisation of Laboratory Assessment' has developed recommendations on laboratory assessment for DSD regarding the use of technologies and analytes to be investigated. This position paper on steroid hormone analysis in diagnosis and treatment of DSD was compiled by a group of specialists in DSD and/or hormonal analysis, either from participating European countries or international partner countries. The topics discussed comprised analytical methods (immunoassay/mass spectrometry-based methods), matrices (urine/serum/saliva) and harmonisation of laboratory tests. The following positions were agreed upon: support of the appropriate use of immunoassay- and mass spectrometry-based methods for diagnosis and monitoring of DSD. Serum/plasma and urine are established matrices for analysis. Laboratories performing analyses for DSD need to operate within a quality framework and actively engage in harmonisation processes so that results and their interpretation are the same irrespective of the laboratory they are performed in. Participation in activities of peer comparison such as sample exchange or when available subscribing to a relevant external quality assurance program should be achieved. The ultimate aim of the guidelines is the implementation of clinical standards for diagnosis and appropriate treatment of DSD to achieve the best outcome for patients, no matter where patients are investigated or managed. © 2017 The authors.

Analytical and clinical evaluation of the Abbott RealTime hepatitis B sequencing assay.

PubMed

Huh, Hee Jae; Kim, Ji-Youn; Lee, Myoung-Keun; Lee, Nam Yong; Kim, Jong-Won; Ki, Chang-Seok

2016-12-01

Long-term nucleoside analogue (NA) treatment leads to selection for drug-resistant mutations in patients undergoing hepatitis B virus (HBV) therapy. The Abbott RealTime HBV Sequencing assay (Abbott assay; Abbott Molecular Inc., Des Plaines, IL, USA) targets the reverse transcriptase region of the polymerase gene and as such has the ability to detect NA resistance-associated mutations in HBV. We evaluated the analytical performance of the Abbott assay and compared its diagnostic performance to that of a laboratory-developed nested-PCR and sequencing method. The analytical sensitivity of the Abbott assay was determined using a serially-diluted WHO International Standard. To validate the clinical performances of the Abbott assay and the laboratory-developed assay, 89 clinical plasma samples with various levels of HBV DNA were tested using both assays. The limit of detection of the Abbott assay, was 210IU/ml and it successfully detected mutations when the mutant types were present at levels ≥20%. Among 89 clinical specimens, 43 and 42 were amplification positive in the Abbott and laboratory-developed assays, respectively, with 87.6% overall agreement (78/89; 95% confidence interval [CI], 78.6-93.4). The Abbott assay failed to detect the minor mutant populations in two specimens, and therefore overall concordance was 85.3% (76/89), and the kappa value was 0.79 (95% CI, 0.67-0.90). The Abbott assay showed comparable diagnostic performance to laboratory-developed nested PCR followed by direct sequencing, and may be useful as a routine method for detecting HBV NA resistance-associated mutations in clinical laboratory settings. Copyright © 2016 Elsevier B.V. All rights reserved.

The evaluation of an analytical protocol for the determination of substances in waste for hazard classification

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hennebert, Pierre, E-mail: pierre.hennebert@ineris.fr; Papin, Arnaud; Padox, Jean-Marie

Highlights: • Knowledge of wastes in substances will be necessary to assess HP1–HP15 hazard properties. • A new analytical protocol is proposed for this and tested by two service laboratories on 32 samples. • Sixty-three percentage of the samples have a satisfactory analytical balance between 90% and 110%. • Eighty-four percentage of the samples were classified identically (Seveso Directive) for their hazardousness by the two laboratories. • The method, in progress, is being normalized in France and is be proposed to CEN. - Abstract: The classification of waste as hazardous could soon be assessed in Europe using largely the hazardmore » properties of its constituents, according to the the Classification, Labelling and Packaging (CLP) regulation. Comprehensive knowledge of the component constituents of a given waste will therefore be necessary. An analytical protocol for determining waste composition is proposed, which includes using inductively coupled plasma (ICP) screening methods to identify major elements and gas chromatography/mass spectrometry (GC–MS) screening techniques to measure organic compounds. The method includes a gross or indicator measure of ‘pools’ of higher molecular weight organic substances that are taken to be less bioactive and less hazardous, and of unresolved ‘mass’ during the chromatography of volatile and semi-volatile compounds. The concentration of some elements and specific compounds that are linked to specific hazard properties and are subject to specific regulation (examples include: heavy metals, chromium(VI), cyanides, organo-halogens, and PCBs) are determined by classical quantitative analysis. To check the consistency of the analysis, the sum of the concentrations (including unresolved ‘pools’) should give a mass balance between 90% and 110%. Thirty-two laboratory samples comprising different industrial wastes (liquids and solids) were tested by two routine service laboratories, to give circa 7000 parameter results. Despite discrepancies in some parameters, a satisfactory sum of estimated or measured concentrations (analytical balance) of 90% was reached for 20 samples (63% of the overall total) during this first test exercise, with identified reasons for most of the unsatisfactory results. Regular use of this protocol (which is now included in the French legislation) has enabled service laboratories to reach a 90% mass balance for nearly all the solid samples tested, and most of liquid samples (difficulties were caused in some samples from polymers in solution and vegetable oil). The protocol is submitted to French and European normalization bodies (AFNOR and CEN) and further improvements are awaited.« less

Practical solution for control of the pre-analytical phase in decentralized clinical laboratories for meeting the requirements of the medical laboratory accreditation standard DIN EN ISO 15189.

PubMed

Vacata, Vladimir; Jahns-Streubel, Gerlinde; Baldus, Mirjana; Wood, William Graham

2007-01-01

This report was written in response to the article by Wood published recently in this journal. It describes a practical solution to the problems of controlling the pre-analytical phase in the clinical diagnostic laboratory. As an indicator of quality in the pre-analytical phase of sample processing, a target analyte was chosen which is sensitive to delay in centrifugation and/or analysis. The results of analyses of the samples sent by satellite medical practitioners were compared with those from an on-site hospital laboratory with a controllable optimized pre-analytical phase. The aim of the comparison was: (a) to identify those medical practices whose mean/median sample values significantly deviate from those of the control situation in the hospital laboratory due to the possible problems in the pre-analytical phase; (b) to aid these laboratories in the process of rectifying these problems. A Microsoft Excel-based Pre-Analytical Survey tool (PAS tool) has been developed which addresses the above mentioned problems. It has been tested on serum potassium which is known to be sensitive to delay and/or irregularities in sample treatment. The PAS tool has been shown to be one possibility for improving the quality of the analyses by identifying the sources of problems within the pre-analytical phase, thus allowing them to be rectified. Additionally, the PAS tool has an educational value and can also be adopted for use in other decentralized laboratories.

Trueness verification of actual creatinine assays in the European market demonstrates a disappointing variability that needs substantial improvement. An international study in the framework of the EC4 creatinine standardization working group.

PubMed

Delanghe, Joris R; Cobbaert, Christa; Galteau, Marie-Madeleine; Harmoinen, Aimo; Jansen, Rob; Kruse, Rolf; Laitinen, Päivi; Thienpont, Linda M; Wuyts, Birgitte; Weykamp, Cas; Panteghini, Mauro

2008-01-01

The European In Vitro Diagnostics (IVD) directive requires traceability to reference methods and materials of analytes. It is a task of the profession to verify the trueness of results and IVD compatibility. The results of a trueness verification study by the European Communities Confederation of Clinical Chemistry (EC4) working group on creatinine standardization are described, in which 189 European laboratories analyzed serum creatinine in a commutable serum-based material, using analytical systems from seven companies. Values were targeted using isotope dilution gas chromatography/mass spectrometry. Results were tested on their compliance to a set of three criteria: trueness, i.e., no significant bias relative to the target value, between-laboratory variation and within-laboratory variation relative to the maximum allowable error. For the lower and intermediate level, values differed significantly from the target value in the Jaffe and the dry chemistry methods. At the high level, dry chemistry yielded higher results. Between-laboratory coefficients of variation ranged from 4.37% to 8.74%. Total error budget was mainly consumed by the bias. Non-compensated Jaffe methods largely exceeded the total error budget. Best results were obtained for the enzymatic method. The dry chemistry method consumed a large part of its error budget due to calibration bias. Despite the European IVD directive and the growing needs for creatinine standardization, an unacceptable inter-laboratory variation was observed, which was mainly due to calibration differences. The calibration variation has major clinical consequences, in particular in pediatrics, where reference ranges for serum and plasma creatinine are low, and in the estimation of glomerular filtration rate.

Validation of pharmaceutical potency determinations by quantitative nuclear magnetic resonance spectrometry.

PubMed

Webster, Gregory K; Marsden, Ian; Pommerening, Cynthia A; Tyrakowski, Christina M

2010-05-01

With the changing development paradigms in the pharmaceutical industry, laboratories are challenged to release materials for clinical studies with rapid turnaround times. To minimize cost demands, many businesses are looking to develop ways of using early Good Manufacturing Practice (GMP) materials of active pharmaceutical ingredients (API) for Good Laboratory Practice (GLP) toxicology studies. To make this happen, the analytical laboratory releases the material by one of three scenarios: (1) holding the GLP release until full GMP testing is ready, (2) issuing a separate lot number for a portion of the GMP material and releasing the material for GLP use, or (3) releasing the lot of material for GLP using alternate (equivalent) method(s) not specified for GMP release testing. Many companies are finding the third scenario to be advantageous in terms of cost and efficiency through the use of quantitative nuclear magnetic resonance (q-NMR). The use of q-NMR has proved to be a single-point replacement for routine early development testing that previously combined elements of identity testing, chromatographic assay, moisture analysis, residual solvent analysis, and elemental analysis. This study highlights that q-NMR can be validated to meet current regulatory analytical method guidelines for routine pharmaceutical analysis.

42 CFR 493.959 - Immunohematology.

Code of Federal Regulations, 2014 CFR

2014-10-01

... challenges per testing event a program must provide for each analyte or test procedure is five. Analyte or... Compatibility testing Antibody identification (d) Evaluation of a laboratory's analyte or test performance. HHS... program must compare the laboratory's response for each analyte with the response that reflects agreement...

42 CFR 493.959 - Immunohematology.

Code of Federal Regulations, 2013 CFR

2013-10-01

... challenges per testing event a program must provide for each analyte or test procedure is five. Analyte or... Compatibility testing Antibody identification (d) Evaluation of a laboratory's analyte or test performance. HHS... program must compare the laboratory's response for each analyte with the response that reflects agreement...

42 CFR 493.959 - Immunohematology.

Code of Federal Regulations, 2012 CFR

2012-10-01

... challenges per testing event a program must provide for each analyte or test procedure is five. Analyte or... Compatibility testing Antibody identification (d) Evaluation of a laboratory's analyte or test performance. HHS... program must compare the laboratory's response for each analyte with the response that reflects agreement...

42 CFR 493.959 - Immunohematology.

Code of Federal Regulations, 2011 CFR

2011-10-01

... challenges per testing event a program must provide for each analyte or test procedure is five. Analyte or... Compatibility testing Antibody identification (d) Evaluation of a laboratory's analyte or test performance. HHS... program must compare the laboratory's response for each analyte with the response that reflects agreement...

Results of the U.S. Geological Survey's Analytical Evaluation Program for standard reference samples: T-155 (trace constituents), M-148 (major constituents), N-59 (nutrient constituents), N-60 (nutrient constituents), P-31 (low ionic strength constituents), GWT-4 (ground-water trace constituents) and Hg-27 (Mercury) distributed in September 1998

USGS Publications Warehouse

Farrar, Jerry W.

1999-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for seven standard reference samples -- T-155 (trace constituents), M-148 (major constituents), N-59 (nutrient constituents), N-60 (nutrient constituents), P-31 (low ionic strength constituents), GWT-4 (ground-water trace constituents), and Hg- 27 (mercury) -- which were distributed in September 1998 to 162 laboratories enrolled in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 136 of the laboratories were evaluated with respect to overall laboratory performance and relative laboratory performance for each analyte in the seven reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the seven standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Quantitative trace analysis of polyfluorinated alkyl substances (PFAS) in ambient air samples from Mace Head (Ireland): A method intercomparison

NASA Astrophysics Data System (ADS)

Jahnke, Annika; Barber, Jonathan L.; Jones, Kevin C.; Temme, Christian

A method intercomparison study of analytical methods for the determination of neutral, volatile polyfluorinated alkyl substances (PFAS) was carried out in March, 2006. Environmental air samples were collected in triplicate at the European background site Mace Head on the west coast of Ireland, a site dominated by 'clean' westerly winds coming across the Atlantic. Extraction and analysis were performed at two laboratories active in PFAS research using their in-house methods. Airborne polyfluorinated telomer alcohols (FTOHs), fluorooctane sulfonamides and sulfonamidoethanols (FOSAs/FOSEs) as well as additional polyfluorinated compounds were investigated. Different native and isotope-labelled internal standards (IS) were applied at various steps in the analytical procedure to evaluate the different quantification strategies. Field blanks revealed no major blank problems. European background concentrations observed at Mace Head were found to be in a similar range to Arctic data reported in the literature. Due to trace-levels at the remote site, only FTOH data sets were complete and could therefore be compared between the laboratories. Additionally, FOSEs could partly be included. Data comparison revealed that despite the challenges inherent in analysis of airborne PFAS and the low concentrations, all methods applied in this study obtained similar results. However, application of isotope-labelled IS early in the analytical procedure leads to more precise results and is therefore recommended.

Develop cost effective field monitoring and laboratory methods to measure groups of contaminants of emerging concern and/or legacy chemicals and pathogens

EPA Science Inventory

Analytical chemistry methods were developed to quantify numerous emerging contaminants (ECs), such as pharmaceuticals (i.e., tamoxifen, tamoxifen metabolites, aromatase inhibitors, antibiotics, illicit drugs, over-the-counter drugs) in aqueous samples (wastewater, surface waters)...

77 FR 14814 - Tobacco Product Analysis; Scientific Workshop; Request for Comments

Federal Register 2010, 2011, 2012, 2013, 2014

2012-03-13

... work to develop tobacco reference products that are not currently available for laboratory use. Discuss... methods used to analyze tobacco products. FDA will invite speakers to address scientific and technical matters relating to the testing of tobacco reference products and the analytical methods used to measure...

40 CFR 408.41 - Specialized definitions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... shall apply to this subpart. (b) The term oil and grease shall mean those components of a waste water amenable to measurement by the method described in Methods for Chemical Analysis of Water and Wastes, 1971, Environmental Protection Agency, Analytical Quality Control Laboratory, page 217. (c) The term seafood shall...

Quality control for federal clean water act and safe drinking water act regulatory compliance.

PubMed

Askew, Ed

2013-01-01

QC sample results are required in order to have confidence in the results from analytical tests. Some of the AOAC water methods include specific QC procedures, frequencies, and acceptance criteria. These are considered to be the minimum controls needed to perform the method successfully. Some regulatory programs, such as those in 40 CFR Part 136.7, require additional QC or have alternative acceptance limits. Essential QC measures include method calibration, reagent standardization, assessment of each analyst's capabilities, analysis of blind check samples, determination of the method's sensitivity (method detection level or quantification limit), and daily evaluation of bias, precision, and the presence of laboratory contamination or other analytical interference. The details of these procedures, their performance frequency, and expected ranges of results are set out in this manuscript. The specific regulatory requirements of 40 CFR Part 136.7 for the Clean Water Act, the laboratory certification requirements of 40 CFR Part 141 for the Safe Drinking Water Act, and the ISO 17025 accreditation requirements under The NELAC Institute are listed.

21 CFR 200.10 - Contract facilities (including consulting laboratories) utilized as extramural facilities by...

Code of Federal Regulations, 2010 CFR

2010-04-01

... (IND) Application, any information obtained during the inspection of an extramural facility having a... Administration does not consider results of validation studies of analytical and assay methods and control...

Report on the U.S. Geological Survey's Evaluation Program Standard Reference Samples Distributed in October 1995: T-137 (Trace Constituents), M-136 (Major Constituents), N-47 (Nutrient Constituents), N-48 (Nutrient Constituents), P-25 (Low Ionic Strength Constituents), and Hg-21 (Mercury)

USGS Publications Warehouse

Farrar, Jerry W.; Long, H. Keith

1996-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for 6 standard reference samples--T-137 (trace constituents), M-136 (major constituents), N-47 (nutrient constituents), N-48 (nutrient constituents), P-25 (low ionic strength constituents), and Hg-21 (mercury)--that were distributed in October 1995 to 149 laboratories registered in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 136 of the laboratories were evaluated with respect to: overall laboratory performance and relative laboratory performance for each analyte in the six reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the six standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Report on the U.S. Geological Survey's evaluation program for standard reference samples distributed in April 1994; T-129 (trace constituents), M-130 (major constituents), N-42 (nutrients), P-22 (low ionic strength), and Hg-18 (mercury)

USGS Publications Warehouse

Long, H. Keith; Farrar, Jerry W.

1994-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for five standard reference samples--T-129 (trace constituents), M-130 (major constituents), N-42 (nutrients), P-22 (low ionic strength), Hg-18(mercury),--that were distributed in April 1994 to 157 laboratories registered in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 133 of the laboratories were evaluated with respect to: overall laboratory performance and relative laboratory performance for each analyte in the five reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the five standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Report of the U.S. Geological Survey's evaluation program for standard reference samples distributed in April 1993; T-123 (trace constituents), T-125 (trace constituents), M-126 (major constituents, N-38 (nutrients), N-39 (nutrients), P-20 (low ionic strength, and Hg-16 (mercury)

USGS Publications Warehouse

Long, H.K.; Farrar, J.W.

1993-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for seven standard reference samples--T-123 (trace constituents), T-125 (trace constituents), M-126 (major constituents), N-38 (nutrients), N-39 (Nutrients), P-20 (precipitation-low ionic strength), and Hg-16 (mercury)--that were distributed in April 1993 to 175 laboratories registered in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data received from 131 of the laboratories were evaluated with respect to: overall laboratory performance and relative laboratory performance for each analyte in the 7 reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the seven standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

The Spanish external quality assessment scheme for mercury in urine.

PubMed

Quintana, M J; Mazarrasa, O

1996-01-01

In 1986 the Instituto Nacional de Seguridad e Higiene en el Trabajo (INSHT), established the "Programa interlaboratorios de control de calidad de mercurio en orina (PICC-HgU)". The operation of this scheme is explained, criteria for evaluation of laboratory performance are defined and some results obtained are reviewed. Since the scheme started, an improvement in the overall performance of laboratories has been observed. The differences in the analytical methods used by laboratories do not seem to have a clear influence on the results.

Evaluation of analytical errors in a clinical chemistry laboratory: a 3 year experience.

PubMed

Sakyi, As; Laing, Ef; Ephraim, Rk; Asibey, Of; Sadique, Ok

2015-01-01

Proficient laboratory service is the cornerstone of modern healthcare systems and has an impact on over 70% of medical decisions on admission, discharge, and medications. In recent years, there is an increasing awareness of the importance of errors in laboratory practice and their possible negative impact on patient outcomes. We retrospectively analyzed data spanning a period of 3 years on analytical errors observed in our laboratory. The data covered errors over the whole testing cycle including pre-, intra-, and post-analytical phases and discussed strategies pertinent to our settings to minimize their occurrence. We described the occurrence of pre-analytical, analytical and post-analytical errors observed at the Komfo Anokye Teaching Hospital clinical biochemistry laboratory during a 3-year period from January, 2010 to December, 2012. Data were analyzed with Graph Pad Prism 5(GraphPad Software Inc. CA USA). A total of 589,510 tests was performed on 188,503 outpatients and hospitalized patients. The overall error rate for the 3 years was 4.7% (27,520/58,950). Pre-analytical, analytical and post-analytical errors contributed 3.7% (2210/58,950), 0.1% (108/58,950), and 0.9% (512/58,950), respectively. The number of tests reduced significantly over the 3-year period, but this did not correspond with a reduction in the overall error rate (P = 0.90) along with the years. Analytical errors are embedded within our total process setup especially pre-analytical and post-analytical phases. Strategic measures including quality assessment programs for staff involved in pre-analytical processes should be intensified.

Prevalence of Pre-Analytical Errors in Clinical Chemistry Diagnostic Labs in Sulaimani City of Iraqi Kurdistan

PubMed Central

2017-01-01

Background Laboratory testing is roughly divided into three phases: a pre-analytical phase, an analytical phase and a post-analytical phase. Most analytical errors have been attributed to the analytical phase. However, recent studies have shown that up to 70% of analytical errors reflect the pre-analytical phase. The pre-analytical phase comprises all processes from the time a laboratory request is made by a physician until the specimen is analyzed at the lab. Generally, the pre-analytical phase includes patient preparation, specimen transportation, specimen collection and storage. In the present study, we report the first comprehensive assessment of the frequency and types of pre-analytical errors at the Sulaimani diagnostic labs in Iraqi Kurdistan. Materials and Methods Over 2 months, 5500 venous blood samples were observed in 10 public diagnostic labs of Sulaimani City. The percentages of rejected samples and types of sample inappropriateness were evaluated. The percentage of each of the following pre-analytical errors were recorded: delay in sample transportation, clotted samples, expired reagents, hemolyzed samples, samples not on ice, incorrect sample identification, insufficient sample, tube broken in centrifuge, request procedure errors, sample mix-ups, communication conflicts, misinterpreted orders, lipemic samples, contaminated samples and missed physician’s request orders. The difference between the relative frequencies of errors observed in the hospitals considered was tested using a proportional Z test. In particular, the survey aimed to discover whether analytical errors were recorded and examine the types of platforms used in the selected diagnostic labs. Results The analysis showed a high prevalence of improper sample handling during the pre-analytical phase. In appropriate samples, the percentage error was as high as 39%. The major reasons for rejection were hemolyzed samples (9%), incorrect sample identification (8%) and clotted samples (6%). Most quality control schemes at Sulaimani hospitals focus only on the analytical phase, and none of the pre-analytical errors were recorded. Interestingly, none of the labs were internationally accredited; therefore, corrective actions are needed at these hospitals to ensure better health outcomes. Internal and External Quality Assessment Schemes (EQAS) for the pre-analytical phase at Sulaimani clinical laboratories should be implemented at public hospitals. Furthermore, lab personnel, particularly phlebotomists, need continuous training on the importance of sample quality to obtain accurate test results. PMID:28107395

An interlaboratory transfer of a multi-analyte assay between continents.

PubMed

Georgiou, Alexandra; Dong, Kelly; Hughes, Stephen; Barfield, Matthew

2015-01-01

Alex has worked at GlaxoSmithKline for the past 15 years and currently works within the bioanalytical and toxicokinetic group in the United Kingdom. Alex's role in previous years has been the in-house support of preclinical and clinical bioanalysis, from method development through to sample analysis activities as well as acting as PI for GLP bioanalysis and toxicokinetics. For the past two years, Alex has applied this analytical and regulatory experience to focus on the outsourcing of preclinical bioanalysis, toxicokinetics and clinical bioanalysis, working closely with multiple bioanalytical and in-life CRO partners worldwide. Alex works to support DMPK and Safety Assessment outsourcing activities for GSK across multiple therapeutic areas, from the first GLP study through to late stage clinical PK studies. Transfer and cross-validation of an existing analytical assay between a laboratory providing current analytical support, and a laboratory needed for new or additional support, can present the bioanalyst with numerous challenges. These challenges can be technical or logistical in nature and may prove to be significant when transferring an assay between laboratories in different continents. Part of GlaxoSmithKline's strategy to improve confidence in providing quality data, is to cross-validate between laboratories. If the cross-validation fails predefined acceptance criteria, then a subsequent investigation would follow. This may also prove to be challenging. The importance of thorough planning and good communication throughout assay transfer, cross-validation and any subsequent investigations is illustrated in this case study.

Techniques of Water-Resources Investigations of the United States Geological Survey. Book 5, Laboratory Analysis. Chapter A5, Methods for Determination of Radioactive Substances in Water and Fluvial Sediments.

ERIC Educational Resources Information Center

Thatcher, L. L.; And Others

Analytical methods for determining important components of fission and natural radioactivity found in water are reported. The discussion of each method includes conditions for application of the method, a summary of the method, interferences, required apparatus, procedures, calculations and estimation of precision. Isotopes considered are…

Quantifying the measurement uncertainty of results from environmental analytical methods.

PubMed

Moser, J; Wegscheider, W; Sperka-Gottlieb, C

2001-07-01

The Eurachem-CITAC Guide Quantifying Uncertainty in Analytical Measurement was put into practice in a public laboratory devoted to environmental analytical measurements. In doing so due regard was given to the provisions of ISO 17025 and an attempt was made to base the entire estimation of measurement uncertainty on available data from the literature or from previously performed validation studies. Most environmental analytical procedures laid down in national or international standards are the result of cooperative efforts and put into effect as part of a compromise between all parties involved, public and private, that also encompasses environmental standards and statutory limits. Central to many procedures is the focus on the measurement of environmental effects rather than on individual chemical species. In this situation it is particularly important to understand the measurement process well enough to produce a realistic uncertainty statement. Environmental analytical methods will be examined as far as necessary, but reference will also be made to analytical methods in general and to physical measurement methods where appropriate. This paper describes ways and means of quantifying uncertainty for frequently practised methods of environmental analysis. It will be shown that operationally defined measurands are no obstacle to the estimation process as described in the Eurachem/CITAC Guide if it is accepted that the dominating component of uncertainty comes from the actual practice of the method as a reproducibility standard deviation.

Keeping the Momentum and Nuclear Forensics at Los Alamos National Laboratory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Steiner, Robert Ernest; Dion, Heather M.; Dry, Donald E.

LANL has 70 years of experience in nuclear forensics and supports the community through a wide variety of efforts and leveraged capabilities: Expanding the understanding of nuclear forensics, providing training on nuclear forensics methods, and developing bilateral relationships to expand our understanding of nuclear forensic science. LANL remains highly supportive of several key organizations tasked with carrying forth the Nuclear Security Summit messages: IAEA, GICNT, and INTERPOL. Analytical chemistry measurements on plutonium and uranium matrices are critical to numerous programs including safeguards accountancy verification measurements. Los Alamos National Laboratory operates capable actinide analytical chemistry and material science laboratories suitable formore » nuclear material and environmental forensic characterization. Los Alamos National Laboratory uses numerous means to validate and independently verify that measurement data quality objectives are met. Numerous LANL nuclear facilities support the nuclear material handling, preparation, and analysis capabilities necessary to evaluate samples containing nearly any mass of an actinide (attogram to kilogram levels).« less

A Six Sigma Trial For Reduction of Error Rates in Pathology Laboratory.

PubMed

Tosuner, Zeynep; Gücin, Zühal; Kiran, Tuğçe; Büyükpinarbaşili, Nur; Turna, Seval; Taşkiran, Olcay; Arici, Dilek Sema

2016-01-01

A major target of quality assurance is the minimization of error rates in order to enhance patient safety. Six Sigma is a method targeting zero error (3.4 errors per million events) used in industry. The five main principles of Six Sigma are defining, measuring, analysis, improvement and control. Using this methodology, the causes of errors can be examined and process improvement strategies can be identified. The aim of our study was to evaluate the utility of Six Sigma methodology in error reduction in our pathology laboratory. The errors encountered between April 2014 and April 2015 were recorded by the pathology personnel. Error follow-up forms were examined by the quality control supervisor, administrative supervisor and the head of the department. Using Six Sigma methodology, the rate of errors was measured monthly and the distribution of errors at the preanalytic, analytic and postanalytical phases was analysed. Improvement strategies were reclaimed in the monthly intradepartmental meetings and the control of the units with high error rates was provided. Fifty-six (52.4%) of 107 recorded errors in total were at the pre-analytic phase. Forty-five errors (42%) were recorded as analytical and 6 errors (5.6%) as post-analytical. Two of the 45 errors were major irrevocable errors. The error rate was 6.8 per million in the first half of the year and 1.3 per million in the second half, decreasing by 79.77%. The Six Sigma trial in our pathology laboratory provided the reduction of the error rates mainly in the pre-analytic and analytic phases.

State-of-the-Art of (Bio)Chemical Sensor Developments in Analytical Spanish Groups

PubMed Central

Plata, María Reyes; Contento, Ana María; Ríos, Angel

2010-01-01

(Bio)chemical sensors are one of the most exciting fields in analytical chemistry today. The development of these analytical devices simplifies and miniaturizes the whole analytical process. Although the initial expectation of the massive incorporation of sensors in routine analytical work has been truncated to some extent, in many other cases analytical methods based on sensor technology have solved important analytical problems. Many research groups are working in this field world-wide, reporting interesting results so far. Modestly, Spanish researchers have contributed to these recent developments. In this review, we summarize the more representative achievements carried out for these groups. They cover a wide variety of sensors, including optical, electrochemical, piezoelectric or electro-mechanical devices, used for laboratory or field analyses. The capabilities to be used in different applied areas are also critically discussed. PMID:22319260

Analysis of environmental contamination resulting from catastrophic incidents: part 2. Building laboratory capability by selecting and developing analytical methodologies.

PubMed

Magnuson, Matthew; Campisano, Romy; Griggs, John; Fitz-James, Schatzi; Hall, Kathy; Mapp, Latisha; Mullins, Marissa; Nichols, Tonya; Shah, Sanjiv; Silvestri, Erin; Smith, Terry; Willison, Stuart; Ernst, Hiba

2014-11-01

Catastrophic incidents can generate a large number of samples of analytically diverse types, including forensic, clinical, environmental, food, and others. Environmental samples include water, wastewater, soil, air, urban building and infrastructure materials, and surface residue. Such samples may arise not only from contamination from the incident but also from the multitude of activities surrounding the response to the incident, including decontamination. This document summarizes a range of activities to help build laboratory capability in preparation for sample analysis following a catastrophic incident, including selection and development of fit-for-purpose analytical methods for chemical, biological, and radiological contaminants. Fit-for-purpose methods are those which have been selected to meet project specific data quality objectives. For example, methods could be fit for screening contamination in the early phases of investigation of contamination incidents because they are rapid and easily implemented, but those same methods may not be fit for the purpose of remediating the environment to acceptable levels when a more sensitive method is required. While the exact data quality objectives defining fitness-for-purpose can vary with each incident, a governing principle of the method selection and development process for environmental remediation and recovery is based on achieving high throughput while maintaining high quality analytical results. This paper illustrates the result of applying this principle, in the form of a compendium of analytical methods for contaminants of interest. The compendium is based on experience with actual incidents, where appropriate and available. This paper also discusses efforts aimed at adaptation of existing methods to increase fitness-for-purpose and development of innovative methods when necessary. The contaminants of interest are primarily those potentially released through catastrophes resulting from malicious activity. However, the same techniques discussed could also have application to catastrophes resulting from other incidents, such as natural disasters or industrial accidents. Further, the high sample throughput enabled by the techniques discussed could be employed for conventional environmental studies and compliance monitoring, potentially decreasing costs and/or increasing the quantity of data available to decision-makers. Published by Elsevier Ltd.

Contacts in the Office of Pesticide Programs, Biological and Economic Analysis Division

EPA Pesticide Factsheets

BEAD provides pesticide use-related information and economic analyses in support of pesticide regulatory activities. BEAD's laboratories validate analytical methods and test public health antimicrobials to ensure that they work as intended.

Determination of Total Carbohydrates in Algal Biomass: Laboratory Analytical Procedure (LAP)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Van Wychen, Stefanie; Laurens, Lieve M. L.

This procedure uses two-step sulfuric acid hydrolysis to hydrolyze the polymeric forms of carbohydrates in algal biomass into monomeric subunits. The monomers are then quantified by either HPLC or a suitable spectrophotometric method.

Adjustment of Pesticide Concentrations for Temporal Changes in Analytical Recovery, 1992-2006

USGS Publications Warehouse

Martin, Jeffrey D.; Stone, Wesley W.; Wydoski, Duane S.; Sandstrom, Mark W.

2009-01-01

Recovery is the proportion of a target analyte that is quantified by an analytical method and is a primary indicator of the analytical bias of a measurement. Recovery is measured by analysis of quality-control (QC) water samples that have known amounts of target analytes added ('spiked' QC samples). For pesticides, recovery is the measured amount of pesticide in the spiked QC sample expressed as percentage of the amount spiked, ideally 100 percent. Temporal changes in recovery have the potential to adversely affect time-trend analysis of pesticide concentrations by introducing trends in environmental concentrations that are caused by trends in performance of the analytical method rather than by trends in pesticide use or other environmental conditions. This report examines temporal changes in the recovery of 44 pesticides and 8 pesticide degradates (hereafter referred to as 'pesticides') that were selected for a national analysis of time trends in pesticide concentrations in streams. Water samples were analyzed for these pesticides from 1992 to 2006 by gas chromatography/mass spectrometry. Recovery was measured by analysis of pesticide-spiked QC water samples. Temporal changes in pesticide recovery were investigated by calculating robust, locally weighted scatterplot smooths (lowess smooths) for the time series of pesticide recoveries in 5,132 laboratory reagent spikes; 1,234 stream-water matrix spikes; and 863 groundwater matrix spikes. A 10-percent smoothing window was selected to show broad, 6- to 12-month time scale changes in recovery for most of the 52 pesticides. Temporal patterns in recovery were similar (in phase) for laboratory reagent spikes and for matrix spikes for most pesticides. In-phase temporal changes among spike types support the hypothesis that temporal change in method performance is the primary cause of temporal change in recovery. Although temporal patterns of recovery were in phase for most pesticides, recovery in matrix spikes was greater than recovery in reagent spikes for nearly every pesticide. Models of recovery based on matrix spikes are deemed more appropriate for adjusting concentrations of pesticides measured in groundwater and stream-water samples than models based on laboratory reagent spikes because (1) matrix spikes are expected to more closely match the matrix of environmental water samples than are reagent spikes and (2) method performance is often matrix dependent, as was shown by higher recovery in matrix spikes for most of the pesticides. Models of recovery, based on lowess smooths of matrix spikes, were developed separately for groundwater and stream-water samples. The models of recovery can be used to adjust concentrations of pesticides measured in groundwater or stream-water samples to 100 percent recovery to compensate for temporal changes in the performance (bias) of the analytical method.

Electronic laboratory notebooks progress and challenges in implementation.

PubMed

Machina, Hari K; Wild, David J

2013-08-01

Electronic laboratory notebooks (ELNs) are increasingly replacing paper notebooks in life science laboratories, including those in industry, academic settings, and hospitals. ELNs offer significant advantages over paper notebooks, but adopting them in a predominantly paper-based environment is usually disruptive. The benefits of ELN increase when they are integrated with other laboratory informatics tools such as laboratory information management systems, chromatography data systems, analytical instrumentation, and scientific data management systems, but there is no well-established path for effective integration of these tools. In this article, we review and evaluate some of the approaches that have been taken thus far and also some radical new methods of integration that are emerging.

Improvement and validation of the method to determine neutral detergent fiber in feed.

PubMed

Hiraoka, Hisaaki; Fukunaka, Rie; Ishikuro, Eiichi; Enishi, Osamu; Goto, Tetsuhisa

2012-10-01

To improve the performance of the analytical method for neutral detergent fiber in feed with heat-stable α-amylase treatment (aNDFom), the process of adding heat-stable α-amylase, as well as other analytical conditions, were examined. In this new process, the starch in the samples was removed by adding amylase to neutral detergent (ND) solution twice, just after the start of heating and immediately after refluxing. We also examined the effects of the use of sodium sulfite, and drying and ashing conditions for aNDFom analysis by this modified amylase addition method. A collaborative study to validate this new method was carried out with 15 laboratories. These laboratories analyzed two samples, alfalfa pellet and dairy mixed feed, with blind duplicates. Ten laboratories used a conventional apparatus and five used a Fibertec(®) type apparatus. There were no significant differences in aNDFom values between these two refluxing apparatuses. The aNDFom values in alfalfa pellet and dairy mixed feed were 388 g/kg and 145 g/kg, the coefficients of variation for the repeatability and reproducibility (CV(r) and CV(R) ) were 1.3% and 2.9%, and the HorRat values were 0.8 and 1.1, respectively. This new method was validated with 5.8% uncertainty (k = 2) from the collaborative study. © 2012 The Authors. Animal Science Journal © 2012 Japanese Society of Animal Science.

The Efficacy of Problem-Based Learning in an Analytical Laboratory Course for Pre-Service Chemistry Teachers

ERIC Educational Resources Information Center

Yoon, Heojeong; Woo, Ae Ja; Treagust, David; Chandrasegaran, A. L.

2014-01-01

The efficacy of problem-based learning (PBL) in an analytical chemistry laboratory course was studied using a programme that was designed and implemented with 20 students in a treatment group over 10 weeks. Data from 26 students in a traditional analytical chemistry laboratory course were used for comparison. Differences in the creative thinking…

Multielement trace determination in SiC powders: assessment of interlaboratory comparisons aimed at the validation and standardization of analytical procedures with direct solid sampling based on ETV ICP OES and DC arc OES.

PubMed

Matschat, Ralf; Hassler, Jürgen; Traub, Heike; Dette, Angelika

2005-12-01

The members of the committee NMP 264 "Chemical analysis of non-oxidic raw and basic materials" of the German Standards Institute (DIN) have organized two interlaboratory comparisons for multielement determination of trace elements in silicon carbide (SiC) powders via direct solid sampling methods. One of the interlaboratory comparisons was based on the application of inductively coupled plasma optical emission spectrometry with electrothermal vaporization (ETV ICP OES), and the other on the application of optical emission spectrometry with direct current arc (DC arc OES). The interlaboratory comparisons were organized and performed in the framework of the development of two standards related to "the determination of mass fractions of metallic impurities in powders and grain sizes of ceramic raw and basic materials" by both methods. SiC powders were used as typical examples of this category of material. The aim of the interlaboratory comparisons was to determine the repeatability and reproducibility of both analytical methods to be standardized. This was an important contribution to the practical applicability of both draft standards. Eight laboratories participated in the interlaboratory comparison with ETV ICP OES and nine in the interlaboratory comparison with DC arc OES. Ten analytes were investigated by ETV ICP OES and eleven by DC arc OES. Six different SiC powders were used for the calibration. The mass fractions of their relevant trace elements were determined after wet chemical digestion. All participants followed the analytical requirements described in the draft standards. In the calculation process, three of the calibration materials were used successively as analytical samples. This was managed in the following manner: the material that had just been used as the analytical sample was excluded from the calibration, so the five other materials were used to establish the calibration plot. The results from the interlaboratory comparisons were summarized and used to determine the repeatability and the reproducibility (expressed as standard deviations) of both methods. The calculation was carried out according to the related standard. The results are specified and discussed in this paper, as are the optimized analytical conditions determined and used by the authors of this paper. For both methods, the repeatability relative standard deviations were <25%, usually ~10%, and the reproducibility relative standard deviations were <35%, usually ~15%. These results were regarded as satifactory for both methods intended for rapid analysis of materials for which decomposition is difficult and time-consuming. Also described are some results from an interlaboratory comparison used to certify one of the materials that had been previously used for validation in both interlaboratory comparisons. Thirty laboratories (from eight countries) participated in this interlaboratory comparison for certification. As examples, accepted results are shown from laboratories that used ETV ICP OES or DC arc OES and had performed calibrations by using solutions or oxides, respectively. The certified mass fractions of the certified reference materials were also compared with the mass fractions determined in the interlaboratory comparisons performed within the framework of method standardization. Good agreement was found for most of the analytes.

Reference Intervals of Common Clinical Chemistry Analytes for Adults in Hong Kong.

PubMed

Lo, Y C; Armbruster, David A

2012-04-01

Defining reference intervals is a major challenge because of the difficulty in recruiting volunteers to participate and testing samples from a significant number of healthy reference individuals. Historical literature citation intervals are often suboptimal because they're be based on obsolete methods and/or only a small number of poorly defined reference samples. Blood donors in Hong Kong gave permission for additional blood to be collected for reference interval testing. The samples were tested for twenty-five routine analytes on the Abbott ARCHITECT clinical chemistry system. Results were analyzed using the Rhoads EP evaluator software program, which is based on the CLSI/IFCC C28-A guideline, and defines the reference interval as the 95% central range. Method specific reference intervals were established for twenty-five common clinical chemistry analytes for a Chinese ethnic population. The intervals were defined for each gender separately and for genders combined. Gender specific or combined gender intervals were adapted as appropriate for each analyte. A large number of healthy, apparently normal blood donors from a local ethnic population were tested to provide current reference intervals for a new clinical chemistry system. Intervals were determined following an accepted international guideline. Laboratories using the same or similar methodologies may adapt these intervals if deemed validated and deemed suitable for their patient population. Laboratories using different methodologies may be able to successfully adapt the intervals for their facilities using the reference interval transference technique based on a method comparison study.

Direct total and free testosterone measurement by liquid chromatography tandem mass spectrometry across two different platforms.

PubMed

Rhea, Jeanne M; French, Deborah; Molinaro, Ross J

2013-05-01

To develop and validate liquid chromatography tandem mass spectrometry (LC-MS/MS) methods for the direct measurement of total and free testosterone in patient samples on two different analytical systems. An API 4000 and 5000 triple quadropoles were used and compared; the former is reported to be 3-5 times less sensitive, as was used to set the quantitation limits. Free testosterone was separated from the protein-bound fraction by equilibrium dialysis followed by derivatization. Either free or total testosterone, and a deuterated internal standard (d3-testosterone) were extracted by liquid-liquid extraction. The validation results were compared to two different clinical laboratories. The use of d2-testosterone was found to be unacceptable for our method. The total testosterone LC-MS/MS methods on both systems were linear over a wide concentration range of 1.5-2000ng/dL. Free testosterone was measured directly using equilibrium dialysis coupled LC-MS/MS and linear over the concentration range of 2.5-2500pg/mL. Good correlation (total testosterone, R(2)=0.96; free testosterone, R(2)=0.98) was observed between our LC-MS/MS systems and comparator laboratory. However, differences in absolute values for both free and total testosterone measurements were observed while a comparison to a second published LC-MS/MS method showed excellent correlation. Free and total testosterone measurements correlated well with clinical observations. To our knowledge, this is the first published validation of free and total testosterone methods across two analytical systems of different analytical sensitivities. A less sensitive system does not sacrifice analytical or clinical sensitivity to directly measure free and total testosterone in patient samples. Copyright © 2013 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Harmonization of urine albumin/creatinine ratio (ACR) results: a study based on an external quality assessment program in Polish laboratories.

PubMed

Ćwiklińska, Agnieszka; Dąbrowska, Hanna; Kowalski, Robert; Kuchta, Agnieszka; Kortas-Stempak, Barbara; Fijałkowska, Aleksandra; Bednarczuk, Gabriela; Jankowski, Maciej

2018-05-11

The ratio of albumin to creatinine (ACR) is an important parameter used for detection of albuminuria in patients with early kidney damage. The aim of the study was to evaluate the harmonization of ACR results among Polish participants in an international external quality assessment (EQA) program, and to evaluate the impact of albumin and creatinine analytical performance on the harmonization of ACR results. We analyzed 182 results of albumin, 202 of creatinine, and 180 of ACR obtained from Polish laboratories in an EQA program organized by Labquality. The dispersion of the results in surveys and percentage differences between the results and target values were calculated. Moreover, differences between method groups were assessed. The inter-laboratory coefficient of variation (CV) for ACR was 36%. Only 74% of results of Polish laboratories were within the target limits; for 11% of the results, an incorrect albuminuria category would have been reported. The inter-laboratory CV for albumin was 20%, 2.6-fold higher than for creatinine. Significant differences between method groups for albumin determination have been observed, even when the same measurement technique was used. The greatest difference between two groups was 23%, 2.5-fold greater in comparison to creatinine. There is an insufficient harmonization of ACR values among Polish laboratories, caused mainly by urine albumin analytical performance. Given the important role of ACR in the classification, monitoring and treatment of kidney damage, the harmonization of albumin measurements is crucial and urgently needed.

Electromigrative separation techniques in forensic science: combining selectivity, sensitivity, and robustness.

PubMed

Posch, Tjorben Nils; Pütz, Michael; Martin, Nathalie; Huhn, Carolin

2015-01-01

In this review we introduce the advantages and limitations of electromigrative separation techniques in forensic toxicology. We thus present a summary of illustrative studies and our own experience in the field together with established methods from the German Federal Criminal Police Office rather than a complete survey. We focus on the analytical aspects of analytes' physicochemical characteristics (e.g. polarity, stereoisomers) and analytical challenges including matrix tolerance, separation from compounds present in large excess, sample volumes, and orthogonality. For these aspects we want to reveal the specific advantages over more traditional methods. Both detailed studies and profiling and screening studies are taken into account. Care was taken to nearly exclusively document well-validated methods outstanding for the analytical challenge discussed. Special attention was paid to aspects exclusive to electromigrative separation techniques, including the use of the mobility axis, the potential for on-site instrumentation, and the capillary format for immunoassays. The review concludes with an introductory guide to method development for different separation modes, presenting typical buffer systems as starting points for different analyte classes. The objective of this review is to provide an orientation for users in separation science considering using capillary electrophoresis in their laboratory in the future.

Single-laboratory validation of a saponification method for the determination of four polycyclic aromatic hydrocarbons in edible oils by HPLC-fluorescence detection.

PubMed

Akdoğan, Abdullah; Buttinger, Gerhard; Wenzl, Thomas

2016-01-01

An analytical method is reported for the determination of four polycyclic aromatic hydrocarbons (benzo[a]pyrene (BaP), benz[a]anthracene (BaA), benzo[b]fluoranthene (BbF) and chrysene (CHR)) in edible oils (sesame, maize, sunflower and olive oil) by high-performance liquid chromatography. Sample preparation is based on three steps including saponification, liquid-liquid partitioning and, finally, clean-up by solid phase extraction on 2 g of silica. Guidance on single-laboratory validation of the proposed analysis method was taken from the second edition of the Eurachem guide on method validation. The lower level of the working range of the method was determined by the limits of quantification of the individual analytes, and the upper level was equal to 5.0 µg kg(-1). The limits of detection and quantification of the four PAHs ranged from 0.06 to 0.12 µg kg(-1) and from 0.13 to 0.24 µg kg(-1). Recoveries of more than 84.8% were achieved for all four PAHs at two concentration levels (2.5 and 5.0 µg kg(-1)), and expanded relative measurement uncertainties were below 20%. The performance of the validated method was in all aspects compliant with provisions set in European Union legislation for the performance of analytical methods employed in the official control of food. The applicability of the method to routine samples was evaluated based on a limited number of commercial edible oil samples.

Report on the U.S. Geological Survey's evaluation program for standard reference samples distributed in October 1993 : T-127 (trace constituents), M-128 (major constituents), N-40 (nutrients), N-41 (nutrients), P-21 (low ionic strength), Hg-17 (mercury), AMW-3 (acid mine water), and WW-1 (whole water)

USGS Publications Warehouse

Long, H.K.; Farrar, J.W.

1994-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for eight standard reference samples--T-127 (trace constituents), M-128 (major constituents), N-40 (nutrients), N-41 (nutrients), P-21 (low ionic strength), Hg-17 (mercury), AMW-3 (acid mine water), and WW-1 (whole water)--that were distributed in October 1993 to 158 laboratories registered in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 145 of the laboratories were evaluated with respect to: overall laboratory performance and relative laboratory performance for each analyte in the eight reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the eight standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Report on the U.S. Geological Survey's evaluation program for standard reference samples distributed in October 1994 : T-131 (trace constituents), T-133 (trace constituents), M-132 (major constituents), N-43 (nutrients), N-44 (nutrients), P-23 (low ionic strength) and Hg-19 (mercury)

USGS Publications Warehouse

Long, H. Keith; Farrar, Jerry W.

1995-01-01

This report presents the results of the U.S. Geological Survey's analytical evaluation program for 7 standard reference samples--T-131 (trace constituents), T-133 (trace constituents), M-132 (major constituents), N-43 (nutrients), N-44 (nutrients), P-23 (low ionic strength), and Hg-19 (mercury). The samples were distributed in October 1994 to 131 laboratories registered in the U.S. Geological Survey sponsored interlaboratory testing program. Analytical data that were received from 121 of the laboratories were evaluated with respect to: overall laboratory performance and relative laboratory performance for each analyte in the seven reference samples. Results of these evaluations are presented in tabular form. Also presented are tables and graphs summarizing the analytical data provided by each laboratory for each analyte in the seven standard reference samples. The most probable value for each analyte was determined using nonparametric statistics.

Development and validation of a multi-analyte method for the regulatory control of carotenoids used as feed additives in fish and poultry feed.

PubMed

Vincent, Ursula; Serano, Federica; von Holst, Christoph

2017-08-01

Carotenoids are used in animal nutrition mainly as sensory additives that favourably affect the colour of fish, birds and food of animal origin. Various analytical methods exist for their quantification in compound feed, reflecting the different physico-chemical characteristics of the carotenoid and the corresponding feed additives. They may be natural products or specific formulations containing the target carotenoids produced by chemical synthesis. In this study a multi-analyte method was developed that can be applied to the determination of all 10 carotenoids currently authorised within the European Union for compound feedingstuffs. The method functions regardless of whether the carotenoids have been added to the compound feed via natural products or specific formulations. It is comprised of three steps: (1) digestion of the feed sample with an enzyme; (2) pressurised liquid extraction; and (3) quantification of the analytes by reversed-phase HPLC coupled to a photodiode array detector in the visible range. The method was single-laboratory validated for poultry and fish feed covering a mass fraction range of the target analyte from 2.5 to 300 mg kg - 1 . The following method performance characteristics were obtained: the recovery rate varied from 82% to 129% and precision expressed as the relative standard deviation of intermediate precision varied from 1.6% to 15%. Based on the acceptable performance obtained in the validation study, the multi-analyte method is considered fit for the intended purpose.

Instrumentation development for drug detection on the breath

DOT National Transportation Integrated Search

1972-09-01

Based on a survey of candidate analytical methods, mass spectrometry was identified as a promising technique for drug detection on the breath. To demonstrate its capabilities, an existing laboratory mass spectrometer was modified by the addition of a...

RAPID ON-SITE METHODS OF CHEMICAL ANALYSIS

EPA Science Inventory

The analysis of potentially hazardous air, water and soil samples collected and shipped to service laboratories off-site is time consuming and expensive. This Chapter addresses the practical alternative of performing the requisite analytical services on-site. The most significant...

HUMAN EXPOSURE ASSESSMENT USING IMMUNOASSAY

EPA Science Inventory

The National Exposure Research Laboratory-Las Vegas is developing analytical methods for human exposure assessment studies. Critical exposure studies generate a large number of samples which must be analyzed in a reliable, cost-effective and timely manner. TCP (3,5,6-trichlor...

Increasing productivity for the analysis of trace contaminants in food by gas chromatography-mass spectrometry using automated liner exchange, backflushing and heart-cutting.

PubMed

David, Frank; Tienpont, Bart; Devos, Christophe; Lerch, Oliver; Sandra, Pat

2013-10-25

Laboratories focusing on residue analysis in food are continuously seeking to increase sample throughput by minimizing sample preparation. Generic sample extraction methods such as QuEChERS lack selectivity and consequently extracts are not free from non-volatile material that contaminates the analytical system. Co-extracted matrix constituents interfere with target analytes, even if highly sensitive and selective GC-MS/MS is used. A number of GC approaches are described that can be used to increase laboratory productivity. These techniques include automated inlet liner exchange and column backflushing for preservation of the performance of the analytical system and heart-cutting two-dimensional GC for increasing sensitivity and selectivity. The application of these tools is illustrated by the analysis of pesticides in vegetables and fruits, PCBs in milk powder and coplanar PCBs in fish. It is demonstrated that considerable increase in productivity can be achieved by decreasing instrument down-time, while analytical performance is equal or better compared to conventional trace contaminant analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

Optimization and single-laboratory validation of a method for the determination of flavonolignans in milk thistle seeds by high-performance liquid chromatography with ultraviolet detection.

PubMed

Mudge, Elizabeth; Paley, Lori; Schieber, Andreas; Brown, Paula N

2015-10-01

Seeds of milk thistle, Silybum marianum (L.) Gaertn., are used for treatment and prevention of liver disorders and were identified as a high priority ingredient requiring a validated analytical method. An AOAC International expert panel reviewed existing methods and made recommendations concerning method optimization prior to validation. A series of extraction and separation studies were undertaken on the selected method for determining flavonolignans from milk thistle seeds and finished products to address the review panel recommendations. Once optimized, a single-laboratory validation study was conducted. The method was assessed for repeatability, accuracy, selectivity, LOD, LOQ, analyte stability, and linearity. Flavonolignan content ranged from 1.40 to 52.86% in raw materials and dry finished products and ranged from 36.16 to 1570.7 μg/mL in liquid tinctures. Repeatability for the individual flavonolignans in raw materials and finished products ranged from 1.03 to 9.88% RSDr, with HorRat values between 0.21 and 1.55. Calibration curves for all flavonolignan concentrations had correlation coefficients of >99.8%. The LODs for the flavonolignans ranged from 0.20 to 0.48 μg/mL at 288 nm. Based on the results of this single-laboratory validation, this method is suitable for the quantitation of the six major flavonolignans in milk thistle raw materials and finished products, as well as multicomponent products containing dandelion, schizandra berry, and artichoke extracts. It is recommended that this method be adopted as First Action Official Method status by AOAC International.

Residual Stress Reversal in Highly Strained Shot Peened Structural Elements. Degree awarded by Florida Univ.

NASA Technical Reports Server (NTRS)

Mitchell, William S.; Throckmorton, David (Technical Monitor)

2002-01-01

The purpose of this research was to further the understanding of a crack initiation problem in a highly strained pressure containment housing. Finite Element Analysis methods were used to model the behavior of shot peened materials undergoing plastic deformation. Analytical results are in agreement with laboratory tensile tests that simulated the actual housing load conditions. These results further validate the original investigation finding that the shot peened residual stress had reversed, changing from compressive to tensile, and demonstrate that analytical finite element methods can be used to predict this behavior.

A candidate reference method for serum potassium measurement by inductively coupled plasma mass spectrometry.

PubMed

Yan, Ying; Han, Bingqing; Zeng, Jie; Zhou, Weiyan; Zhang, Tianjiao; Zhang, Jiangtao; Chen, Wenxiang; Zhang, Chuanbao

2017-08-28

Potassium is an important serum ion that is frequently assayed in clinical laboratories. Quality assurance requires reference methods; thus, the establishment of a candidate reference method for serum potassium measurements is important. An inductively coupled plasma mass spectrometry (ICP-MS) method was developed. Serum samples were gravimetrically spiked with an aluminum internal standard, digested with 69% ultrapure nitric acid, and diluted to the required concentration. The 39K/27Al ratios were measured by ICP-MS in hydrogen mode. The method was calibrated using 5% nitric acid matrix calibrators, and the calibration function was established using the bracketing method. The correlation coefficients between the measured 39K/27Al ratios and the analyte concentration ratios were >0.9999. The coefficients of variation were 0.40%, 0.68%, and 0.22% for the three serum samples, and the analytical recovery was 99.8%. The accuracy of the measurement was also verified by measuring certified reference materials, SRM909b and SRM956b. Comparison with the ion selective electrode routine method and international inter-laboratory comparisons gave satisfied results. The new ICP-MS method is specific, precise, simple, and low-cost, and it may be used as a candidate reference method for standardizing serum potassium measurements.

Modular workcells: modern methods for laboratory automation.

PubMed

Felder, R A

1998-12-01

Laboratory automation is beginning to become an indispensable survival tool for laboratories facing difficult market competition. However, estimates suggest that only 8% of laboratories will be able to afford total laboratory automation systems. Therefore, automation vendors have developed alternative hardware configurations called 'modular automation', to fit the smaller laboratory. Modular automation consists of consolidated analyzers, integrated analyzers, modular workcells, and pre- and post-analytical automation. These terms will be defined in this paper. Using a modular automation model, the automated core laboratory will become a site where laboratory data is evaluated by trained professionals to provide diagnostic information to practising physicians. Modem software information management and process control tools will complement modular hardware. Proper standardization that will allow vendor-independent modular configurations will assure success of this revolutionary new technology.

Analytical validation of a novel multiplex test for detection of advanced adenoma and colorectal cancer in symptomatic patients.

PubMed

Dillon, Roslyn; Croner, Lisa J; Bucci, John; Kairs, Stefanie N; You, Jia; Beasley, Sharon; Blimline, Mark; Carino, Rochele B; Chan, Vicky C; Cuevas, Danissa; Diggs, Jeff; Jennings, Megan; Levy, Jacob; Mina, Ginger; Yee, Alvin; Wilcox, Bruce

2018-05-30

Early detection of colorectal cancer (CRC) is key to reducing associated mortality. Despite the importance of early detection, approximately 40% of individuals in the United States between the ages of 50-75 have never been screened for CRC. The low compliance with colonoscopy and fecal-based screening may be addressed with a non-invasive alternative such as a blood-based test. We describe here the analytical validation of a multiplexed blood-based assay that measures the plasma concentrations of 15 proteins to assess advanced adenoma (AA) and CRC risk in symptomatic patients. The test was developed on an electrochemiluminescent immunoassay platform employing four multi-marker panels, to be implemented in the clinic as a laboratory developed test (LDT). Under the Clinical Laboratory Improvement Amendments (CLIA) and College of American Pathologists (CAP) regulations, a United States-based clinical laboratory utilizing an LDT must establish performance characteristics relating to analytical validity prior to releasing patient test results. This report describes a series of studies demonstrating the precision, accuracy, analytical sensitivity, and analytical specificity for each of the 15 assays, as required by CLIA/CAP. In addition, the report describes studies characterizing each of the assays' dynamic range, parallelism, tolerance to common interfering substances, spike recovery, and stability to sample freeze-thaw cycles. Upon completion of the analytical characterization, a clinical accuracy study was performed to evaluate concordance of AA and CRC classifier model calls using the analytical method intended for use in the clinic. Of 434 symptomatic patient samples tested, the percent agreement with original CRC and AA calls was 87% and 92% respectively. All studies followed CLSI guidelines and met the regulatory requirements for implementation of a new LDT. The results provide the analytical evidence to support the implementation of the novel multi-marker test as a clinical test for evaluating CRC and AA risk in symptomatic individuals. Copyright © 2018 Elsevier B.V. All rights reserved.

Analytical Validation of Quantitative Real-Time PCR Methods for Quantification of Trypanosoma cruzi DNA in Blood Samples from Chagas Disease Patients

PubMed Central

Ramírez, Juan Carlos; Cura, Carolina Inés; Moreira, Otacilio da Cruz; Lages-Silva, Eliane; Juiz, Natalia; Velázquez, Elsa; Ramírez, Juan David; Alberti, Anahí; Pavia, Paula; Flores-Chávez, María Delmans; Muñoz-Calderón, Arturo; Pérez-Morales, Deyanira; Santalla, José; Guedes, Paulo Marcos da Matta; Peneau, Julie; Marcet, Paula; Padilla, Carlos; Cruz-Robles, David; Valencia, Edward; Crisante, Gladys Elena; Greif, Gonzalo; Zulantay, Inés; Costales, Jaime Alfredo; Alvarez-Martínez, Miriam; Martínez, Norma Edith; Villarroel, Rodrigo; Villarroel, Sandro; Sánchez, Zunilda; Bisio, Margarita; Parrado, Rudy; Galvão, Lúcia Maria da Cunha; da Câmara, Antonia Cláudia Jácome; Espinoza, Bertha; de Noya, Belkisyole Alarcón; Puerta, Concepción; Riarte, Adelina; Diosque, Patricio; Sosa-Estani, Sergio; Guhl, Felipe; Ribeiro, Isabela; Aznar, Christine; Britto, Constança; Yadón, Zaida Estela; Schijman, Alejandro G.

2015-01-01

An international study was performed by 26 experienced PCR laboratories from 14 countries to assess the performance of duplex quantitative real-time PCR (qPCR) strategies on the basis of TaqMan probes for detection and quantification of parasitic loads in peripheral blood samples from Chagas disease patients. Two methods were studied: Satellite DNA (SatDNA) qPCR and kinetoplastid DNA (kDNA) qPCR. Both methods included an internal amplification control. Reportable range, analytical sensitivity, limits of detection and quantification, and precision were estimated according to international guidelines. In addition, inclusivity and exclusivity were estimated with DNA from stocks representing the different Trypanosoma cruzi discrete typing units and Trypanosoma rangeli and Leishmania spp. Both methods were challenged against 156 blood samples provided by the participant laboratories, including samples from acute and chronic patients with varied clinical findings, infected by oral route or vectorial transmission. kDNA qPCR showed better analytical sensitivity than SatDNA qPCR with limits of detection of 0.23 and 0.70 parasite equivalents/mL, respectively. Analyses of clinical samples revealed a high concordance in terms of sensitivity and parasitic loads determined by both SatDNA and kDNA qPCRs. This effort is a major step toward international validation of qPCR methods for the quantification of T. cruzi DNA in human blood samples, aiming to provide an accurate surrogate biomarker for diagnosis and treatment monitoring for patients with Chagas disease. PMID:26320872

No Impact of the Analytical Method Used for Determining Cystatin C on Estimating Glomerular Filtration Rate in Children.

PubMed

Alberer, Martin; Hoefele, Julia; Benz, Marcus R; Bökenkamp, Arend; Weber, Lutz T

2017-01-01

Measurement of inulin clearance is considered to be the gold standard for determining kidney function in children, but this method is time consuming and expensive. The glomerular filtration rate (GFR) is on the other hand easier to calculate by using various creatinine- and/or cystatin C (Cys C)-based formulas. However, for the determination of serum creatinine (Scr) and Cys C, different and non-interchangeable analytical methods exist. Given the fact that different analytical methods for the determination of creatinine and Cys C were used in order to validate existing GFR formulas, clinicians should be aware of the type used in their local laboratory. In this study, we compared GFR results calculated on the basis of different GFR formulas and either used Scr and Cys C values as determined by the analytical method originally employed for validation or values obtained by an alternative analytical method to evaluate any possible effects on the performance. Cys C values determined by means of an immunoturbidimetric assay were used for calculating the GFR using equations in which this analytical method had originally been used for validation. Additionally, these same values were then used in other GFR formulas that had originally been validated using a nephelometric immunoassay for determining Cys C. The effect of using either the compatible or the possibly incompatible analytical method for determining Cys C in the calculation of GFR was assessed in comparison with the GFR measured by creatinine clearance (CrCl). Unexpectedly, using GFR equations that employed Cys C values derived from a possibly incompatible analytical method did not result in a significant difference concerning the classification of patients as having normal or reduced GFR compared to the classification obtained on the basis of CrCl. Sensitivity and specificity were adequate. On the other hand, formulas using Cys C values derived from a compatible analytical method partly showed insufficient performance when compared to CrCl. Although clinicians should be aware of applying a GFR formula that is compatible with the locally used analytical method for determining Cys C and creatinine, other factors might be more crucial for the calculation of correct GFR values.

Auditing of chromatographic data.

PubMed

Mabie, J T

1998-01-01

During a data audit, it is important to ensure that there is clear documentation and an audit trail. The Quality Assurance Unit should review all areas, including the laboratory, during the conduct of the sample analyses. The analytical methodology that is developed should be documented prior to sample analyses. This is an important document for the auditor, as it is the instrumental piece used by the laboratory personnel to maintain integrity throughout the process. It is expected that this document will give insight into the sample analysis, run controls, run sequencing, instrument parameters, and acceptance criteria for the samples. The sample analysis and all supporting documentation should be audited in conjunction with this written analytical method and any supporting Standard Operating Procedures to ensure the quality and integrity of the data.

Uranium and Calcium Isotope Ratio Measurements using the Modified Total Evaporation Method in TIMS

NASA Astrophysics Data System (ADS)

Richter, S.; Kuehn, H.; Berglund, M.; Hennessy, C.

2010-12-01

A new version of the "modified total evaporation" (MTE) method for isotopic analysis by multi-collector thermal ionization mass spectrometry (TIMS), with high analytical performance and designed in a more user-friendly and routinely applicable way, is described in detail. It is mainly being used for nuclear safeguards measurements of U and Pu and nuclear metrology, but can readily be applied to other scientific tasks in geochemistry, e.g. for Sr, Nd and Ca, as well. The development of the MTE method was organized in collaboration of several "key nuclear mass spectrometry laboratories", namely the New Brunswick Laboratory (NBL), the Institute for Transuranium Elements (ITU), the Safeguards Analytical Laboratory (now Safeguards Analytical Services, SGAS) of the International Atomic Energy Agency (IAEA) and the Institute for Reference Materials and Measurements (IRMM), with IRMM taking the leading role. The manufacturer of the TRITON TIMS instrument, Thermo Fisher Scientific, integrated this method into the software of the instrument. The development has now reached its goal to become a user-friendly and routinely useable method for uranium isotope ratio measurements with high precision and accuracy. Due to the use of the “total evaporation” (TE) method the measurement of the "major" uranium isotope ratio 235U/238U is routinely being performed with a precision of 0.01% to 0.02%. The use of a (certified) reference material measured under comparable conditions is emphasized to achieve an accuracy at a level of 0.02% - depending on the stated uncertainty of the certified value of the reference material. In contrast to the total evaporation method (TE), in the MTE method the total evaporation sequence is interrupted on a regular basis to allow for correction for background from peak tailing, internal calibration of a secondary electron multiplier (SEM) detector versus the Faraday cups, and ion source re-focusing. Therefore, the most significant improvement using the MTE method is in the analytical performance achieved for the "minor" ratios 234U/238U and 236U/238U. The MTE method is now routinely used at all collaborating laboratories and possibly more in the future. Additional applications for the MTE method, e.g. to take advantage of the good external precision in combination with the possibilities of internal background and detector calibrations or mass jumps between different cup configurations, are presented as well. One interesting application concerns new absolute isotope ratio measurements for Ca with an unprecedented level of accuracy. This is important because up to now most reported Ca isotope data are only calculated as relative deviations from a standard like NIST-SRM 915. Using the MTE method measurements on new gravimetrically prepared Ca isotope mixtures were performed. A significantly improved level of accuracy at the level of about 0.02% for both the 42Ca/40Ca and 44Ca/40Ca ratios was obtained.

Impact of Educational Activities in Reducing Pre-Analytical Laboratory Errors

PubMed Central

Al-Ghaithi, Hamed; Pathare, Anil; Al-Mamari, Sahimah; Villacrucis, Rodrigo; Fawaz, Naglaa; Alkindi, Salam

2017-01-01

Objectives Pre-analytic errors during diagnostic laboratory investigations can lead to increased patient morbidity and mortality. This study aimed to ascertain the effect of educational nursing activities on the incidence of pre-analytical errors resulting in non-conforming blood samples. Methods This study was conducted between January 2008 and December 2015. All specimens received at the Haematology Laboratory of the Sultan Qaboos University Hospital, Muscat, Oman, during this period were prospectively collected and analysed. Similar data from 2007 were collected retrospectively and used as a baseline for comparison. Non-conforming samples were defined as either clotted samples, haemolysed samples, use of the wrong anticoagulant, insufficient quantities of blood collected, incorrect/lack of labelling on a sample or lack of delivery of a sample in spite of a sample request. From 2008 onwards, multiple educational training activities directed at the hospital nursing staff and nursing students primarily responsible for blood collection were implemented on a regular basis. Results After initiating corrective measures in 2008, a progressive reduction in the percentage of non-conforming samples was observed from 2009 onwards. Despite a 127.84% increase in the total number of specimens received, there was a significant reduction in non-conforming samples from 0.29% in 2007 to 0.07% in 2015, resulting in an improvement of 75.86% (P <0.050). In particular, specimen identification errors decreased by 0.056%, with a 96.55% improvement. Conclusion Targeted educational activities directed primarily towards hospital nursing staff had a positive impact on the quality of laboratory specimens by significantly reducing pre-analytical errors. PMID:29062553

SECOND FLOOR PLAN OF REMOTE ANALYTICAL FACILITY (CPP627) WARM LABORATORY ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

SECOND FLOOR PLAN OF REMOTE ANALYTICAL FACILITY (CPP-627) WARM LABORATORY ROOM, DECONTAMINATION ROOM, HOT CHEMISTRY LABORATORY, AND MULTICURIE CELL ROOM. INL DRAWING NUMBER 200-0627-00-098-105066. ALTERNATE ID NUMBER 4272-14-103. - Idaho National Engineering Laboratory, Idaho Chemical Processing Plant, Fuel Reprocessing Complex, Scoville, Butte County, ID

Standardization of chemical analytical techniques for pyrolysis bio-oil: history, challenges, and current status of methods

DOE PAGES

Ferrell, Jack R.; Olarte, Mariefel V.; Christensen, Earl D.; ...

2016-07-05

Here, we discuss the standardization of analytical techniques for pyrolysis bio-oils, including the current status of methods, and our opinions on future directions. First, the history of past standardization efforts is summarized, and both successful and unsuccessful validation of analytical techniques highlighted. The majority of analytical standardization studies to-date has tested only physical characterization techniques. In this paper, we present results from an international round robin on the validation of chemical characterization techniques for bio-oils. Techniques tested included acid number, carbonyl titrations using two different methods (one at room temperature and one at 80 °C), 31P NMR for determination ofmore » hydroxyl groups, and a quantitative gas chromatography–mass spectrometry (GC-MS) method. Both carbonyl titration and acid number methods have yielded acceptable inter-laboratory variabilities. 31P NMR produced acceptable results for aliphatic and phenolic hydroxyl groups, but not for carboxylic hydroxyl groups. As shown in previous round robins, GC-MS results were more variable. Reliable chemical characterization of bio-oils will enable upgrading research and allow for detailed comparisons of bio-oils produced at different facilities. Reliable analytics are also needed to enable an emerging bioenergy industry, as processing facilities often have different analytical needs and capabilities than research facilities. We feel that correlations in reliable characterizations of bio-oils will help strike a balance between research and industry, and will ultimately help to -determine metrics for bio-oil quality. Lastly, the standardization of additional analytical methods is needed, particularly for upgraded bio-oils.« less

Standardization of chemical analytical techniques for pyrolysis bio-oil: history, challenges, and current status of methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferrell, Jack R.; Olarte, Mariefel V.; Christensen, Earl D.

Here, we discuss the standardization of analytical techniques for pyrolysis bio-oils, including the current status of methods, and our opinions on future directions. First, the history of past standardization efforts is summarized, and both successful and unsuccessful validation of analytical techniques highlighted. The majority of analytical standardization studies to-date has tested only physical characterization techniques. In this paper, we present results from an international round robin on the validation of chemical characterization techniques for bio-oils. Techniques tested included acid number, carbonyl titrations using two different methods (one at room temperature and one at 80 °C), 31P NMR for determination ofmore » hydroxyl groups, and a quantitative gas chromatography–mass spectrometry (GC-MS) method. Both carbonyl titration and acid number methods have yielded acceptable inter-laboratory variabilities. 31P NMR produced acceptable results for aliphatic and phenolic hydroxyl groups, but not for carboxylic hydroxyl groups. As shown in previous round robins, GC-MS results were more variable. Reliable chemical characterization of bio-oils will enable upgrading research and allow for detailed comparisons of bio-oils produced at different facilities. Reliable analytics are also needed to enable an emerging bioenergy industry, as processing facilities often have different analytical needs and capabilities than research facilities. We feel that correlations in reliable characterizations of bio-oils will help strike a balance between research and industry, and will ultimately help to -determine metrics for bio-oil quality. Lastly, the standardization of additional analytical methods is needed, particularly for upgraded bio-oils.« less

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of chromium in water by graphite furnace atomic absorption spectrophotometry

USGS Publications Warehouse

McLain, B.J.

1993-01-01

Graphite furnace atomic absorption spectrophotometry is a sensitive, precise, and accurate method for the determination of chromium in natural water samples. The detection limit for this analytical method is 0.4 microg/L with a working linear limit of 25.0 microg/L. The precision at the detection limit ranges from 20 to 57 percent relative standard deviation (RSD) with an improvement to 4.6 percent RSD for concentrations more than 3 microg/L. Accuracy of this method was determined for a variety of reference standards that was representative of the analytical range. The results were within the established standard deviations. Samples were spiked with known concentrations of chromium with recoveries ranging from 84 to 122 percent. In addition, a comparison of data between graphite furnace atomic absorption spectrophotometry and direct-current plasma atomic emission spectrometry resulted in suitable agreement between the two methods, with an average deviation of +/- 2.0 microg/L throughout the analytical range.

77 FR 6471 - Bacillus thuringiensis Cry2Ae Protein in Cotton; Exemption from the Requirement of a Tolerance

Federal Register 2010, 2011, 2012, 2013, 2014

2012-02-08

... analytical method using enzyme- linked immunosorbent assay (ELISA) analyses for the qualitative detection of... study conducted by an independent third party laboratory to evaluate the ELISA test kit's performance as...

IN-SITU OXIDATION OF 1,4-DIOXANE (LABORATORY RESULTS)

EPA Science Inventory

Interest in the solvent stabilizer, 1,4-dioxane, is increasing because analytical detection limits have decreased indicating its presence at chlorinated volatile organic compound contaminated sites. The most common method for removing 1,4-dioxane from contaminated water is advanc...

Literature review : an analysis of laboratory fatigue tests.

DOT National Transportation Integrated Search

1975-01-01

This report discusses the various types of fatigue tests, grouped by the type of specimen (beam, plate, Marshall, etc.) used. The discussion under each type of specimen covers the test, and the analytical methods used in evaluating the data. The test...

LABORATORY MISCONDUCT - WHAT CAN HAPPEN TO YOU?

EPA Science Inventory

Contracted laboratories perform a vast number of routine and special analytical services that are the foundation of decisions upon which rests the fate of the environment. Guiding these laboratories in the generation of environmental data has been the analytical protocols and ...

Tank Vapor Characterization Project: Tank 241-S-102 fourth temporal study: Headspace gas and vapor characterization results from samples collected on December 19, 1996

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pool, K.H.; Evans, J.C.; Olsen, K.B.

1997-08-01

This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-S-102 (Tank S-102) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Service Corporation (SESC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. Ammonia was determined to be above the immediate notification limit of 150 ppm as specified by the sampling and analysis planmore » (SAP). Hydrogen was the principal flammable constituent of the Tank S-102 headspace, determined to be present at approximately 2.410% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of the LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Table S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.« less

Hyphenated analytical techniques for materials characterisation

NASA Astrophysics Data System (ADS)

Armstrong, Gordon; Kailas, Lekshmi

2017-09-01

This topical review will provide a survey of the current state of the art in ‘hyphenated’ techniques for characterisation of bulk materials, surface, and interfaces, whereby two or more analytical methods investigating different properties are applied simultaneously to the same sample to better characterise the sample than can be achieved by conducting separate analyses in series using different instruments. It is intended for final year undergraduates and recent graduates, who may have some background knowledge of standard analytical techniques, but are not familiar with ‘hyphenated’ techniques or hybrid instrumentation. The review will begin by defining ‘complementary’, ‘hybrid’ and ‘hyphenated’ techniques, as there is not a broad consensus among analytical scientists as to what each term means. The motivating factors driving increased development of hyphenated analytical methods will also be discussed. This introduction will conclude with a brief discussion of gas chromatography-mass spectroscopy and energy dispersive x-ray analysis in electron microscopy as two examples, in the context that combining complementary techniques for chemical analysis were among the earliest examples of hyphenated characterisation methods. The emphasis of the main review will be on techniques which are sufficiently well-established that the instrumentation is commercially available, to examine physical properties including physical, mechanical, electrical and thermal, in addition to variations in composition, rather than methods solely to identify and quantify chemical species. Therefore, the proposed topical review will address three broad categories of techniques that the reader may expect to encounter in a well-equipped materials characterisation laboratory: microscopy based techniques, scanning probe-based techniques, and thermal analysis based techniques. Examples drawn from recent literature, and a concluding case study, will be used to explain the practical issues that arise in combining different techniques. We will consider how the complementary and varied information obtained by combining these techniques may be interpreted together to better understand the sample in greater detail than that was possible before, and also how combining different techniques can simplify sample preparation and ensure reliable comparisons are made between multiple analyses on the same samples—a topic of particular importance as nanoscale technologies become more prevalent in applied and industrial research and development (R&D). The review will conclude with a brief outline of the emerging state of the art in the research laboratory, and a suggested approach to using hyphenated techniques, whether in the teaching, quality control or R&D laboratory.

An easy, rapid and inexpensive method to monitor tributyltin (TBT) toxicity in the laboratory.

PubMed

Cruz, Andreia; Moreira, Rafael; Mendo, Sónia

2014-05-01

Tributyltin (TBT) contamination remains a major problem worldwide. Many laboratories are committed to the development of remediation methodologies that could help reduce the negative impact of this compound in the environment. Furthermore, it is important to have at hand simple methodologies for evaluating TBT toxicity in the laboratory, besides the use of complex and costly analytical instrumentation. With that purpose, a method was adapted that is based on the inhibition of growth of an indicator strain, Micrococcus luteus ATCC 9341, under TBT. Different types of matrices, of TBT concentrations and sample treatments were tested. The results herein reported show that the bioassay method can be applied for both aqueous and soil samples and also for a high range of TBT concentrations (at least up to 500 μmol/L). Besides being cheap and easy to perform, it can be performed in any laboratory. Additionally, one possible application of the method to monitor TBT degradation is presented as an example.

Manual of analytical methods for the Environmental Health Laboratory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gray, C. E.

1975-06-01

This manual was compiled from techniques used In the Environmental Health Laboratory of Sandia Laboratories at Albuquerque. New Mexico, and is a revision of an earlier publication (SC-M-07-3044) edited by Lial W. Brewer. The procedures arc similar to those used in other laboratories devoted to Environmental Health practices. Some of the methods are standard and others are modified to suit our needs; others were developed at Sandia. The author has attempted to present all methods in a simple and concise manner, but in sufficient detail to make them readily usable. It is not inferred that the methods are universal formore » any type of sample, but they have been found very reliable for the types of samples mentioned. The author will welcome inquiry for clarification of any part of this manual. It is the desire of the author that this manual will be of use and service to others. New and revised procedures will be issued as supplements to this document.« less

The detection of problem analytes in a single proficiency test challenge in the absence of the Health Care Financing Administration rule violations.

PubMed

Cembrowski, G S; Hackney, J R; Carey, N

1993-04-01

The Clinical Laboratory Improvement Act of 1988 (CLIA 88) has dramatically changed proficiency testing (PT) practices having mandated (1) satisfactory PT for certain analytes as a condition of laboratory operation, (2) fixed PT limits for many of these "regulated" analytes, and (3) an increased number of PT specimens (n = 5) for each testing cycle. For many of these analytes, the fixed limits are much broader than the previously employed Standard Deviation Index (SDI) criteria. Paradoxically, there may be less incentive to identify and evaluate analytically significant outliers to improve the analytical process. Previously described "control rules" to evaluate these PT results are unworkable as they consider only two or three results. We used Monte Carlo simulations of Kodak Ektachem analyzers participating in PT to determine optimal control rules for the identification of PT results that are inconsistent with those from other laboratories using the same methods. The analysis of three representative analytes, potassium, creatine kinase, and iron was simulated with varying intrainstrument and interinstrument standard deviations (si and sg, respectively) obtained from the College of American Pathologists (Northfield, Ill) Quality Assurance Services data and Proficiency Test data, respectively. Analytical errors were simulated in each of the analytes and evaluated in terms of multiples of the interlaboratory SDI. Simple control rules for detecting systematic and random error were evaluated with power function graphs, graphs of probability of error detected vs magnitude of error. Based on the simulation results, we recommend screening all analytes for the occurrence of two or more observations exceeding the same +/- 1 SDI limit. For any analyte satisfying this condition, the mean of the observations should be calculated. For analytes with sg/si ratios between 1.0 and 1.5, a significant systematic error is signaled by the mean exceeding 1.0 SDI. Significant random error is signaled by one observation exceeding the +/- 3-SDI limit or the range of the observations exceeding 4 SDIs. For analytes with higher sg/si, significant systematic or random error is signaled by violation of the screening rule (having at least two observations exceeding the same +/- 1 SDI limit). Random error can also be signaled by one observation exceeding the +/- 1.5-SDI limit or the range of the observations exceeding 3 SDIs. We present a practical approach to the workup of apparent PT errors.

42 CFR 493.807 - Condition: Reinstatement of laboratories performing nonwaived testing.

Code of Federal Regulations, 2012 CFR

2012-10-01

..., subspecialties, analyte or test, or voluntarily withdraws its certification under CLIA for the failed specialty, subspecialty, or analyte, the laboratory must then demonstrate sustained satisfactory performance on two... reinstatement for certification and Medicare or Medicaid approval in that specialty, subspecialty, analyte or...

42 CFR 493.807 - Condition: Reinstatement of laboratories performing nonwaived testing.

Code of Federal Regulations, 2014 CFR

2014-10-01

..., subspecialties, analyte or test, or voluntarily withdraws its certification under CLIA for the failed specialty, subspecialty, or analyte, the laboratory must then demonstrate sustained satisfactory performance on two... reinstatement for certification and Medicare or Medicaid approval in that specialty, subspecialty, analyte or...

42 CFR 493.807 - Condition: Reinstatement of laboratories performing nonwaived testing.

Code of Federal Regulations, 2013 CFR

2013-10-01

..., subspecialties, analyte or test, or voluntarily withdraws its certification under CLIA for the failed specialty, subspecialty, or analyte, the laboratory must then demonstrate sustained satisfactory performance on two... reinstatement for certification and Medicare or Medicaid approval in that specialty, subspecialty, analyte or...

Working towards accreditation by the International Standards Organization 15189 Standard: how to validate an in-house developed method an example of lead determination in whole blood by electrothermal atomic absorption spectrometry.

PubMed

Garcia Hejl, Carine; Ramirez, Jose Manuel; Vest, Philippe; Chianea, Denis; Renard, Christophe

2014-09-01

Laboratories working towards accreditation by the International Standards Organization (ISO) 15189 standard are required to demonstrate the validity of their analytical methods. The different guidelines set by various accreditation organizations make it difficult to provide objective evidence that an in-house method is fit for the intended purpose. Besides, the required performance characteristics tests and acceptance criteria are not always detailed. The laboratory must choose the most suitable validation protocol and set the acceptance criteria. Therefore, we propose a validation protocol to evaluate the performance of an in-house method. As an example, we validated the process for the detection and quantification of lead in whole blood by electrothermal absorption spectrometry. The fundamental parameters tested were, selectivity, calibration model, precision, accuracy (and uncertainty of measurement), contamination, stability of the sample, reference interval, and analytical interference. We have developed a protocol that has been applied successfully to quantify lead in whole blood by electrothermal atomic absorption spectrometry (ETAAS). In particular, our method is selective, linear, accurate, and precise, making it suitable for use in routine diagnostics.

Development and single-laboratory validation of an HPLC method for the determination of cyclamate sweetener in foodstuffs.

PubMed

Scotter, M J; Castle, L; Roberts, D P T; Macarthur, R; Brereton, P A; Hasnip, S K; Katz, N

2009-05-01

A method for the determination of cyclamate has been developed and single-laboratory validated for a range of foodstuffs including carbonated and fruit-juice drinks, fruit preserves, spreads, and dairy desserts. The method uses the peroxide oxidation of cyclamate to cyclohexylamine followed by derivatization with trinitrobenzenesulfonic acid and analysis by a modified reversed-phase high-performance liquid chromatography-ultraviolet light (HPLC-UV). Cycloheptylamine is used as an internal standard. The limits of detection were in the range 1-20 mg kg(-1) and the analysis was linear up to 1300 mg kg(-1) cyclamic acid in foods and up to 67 mg l(-1) in beverages. Analytical recovery was between 82% and 123%, and results were recovery corrected. Precision was within experimentally predicted levels for all of the matrices tested and Horrat values for the combined standard uncertainty associated with the measurement of cyclamate between 0.4 (water-based drinks) and 1.7 (spreads). The method was used successfully to test three soft drink samples for homogeneity before analytical performance assessment. The method is recommended for use in monitoring compliance and for formal testing by collaborative trial.

Recent advances in immunosensor for narcotic drug detection

PubMed Central

Gandhi, Sonu; Suman, Pankaj; Kumar, Ashok; Sharma, Prince; Capalash, Neena; Suri, C. Raman

2015-01-01

Introduction: Immunosensor for illicit drugs have gained immense interest and have found several applications for drug abuse monitoring. This technology has offered a low cost detection of narcotics; thereby, providing a confirmatory platform to compliment the existing analytical methods. Methods: In this minireview, we define the basic concept of transducer for immunosensor development that utilizes antibodies and low molecular mass hapten (opiate) molecules. Results: This article emphasizes on recent advances in immunoanalytical techniques for monitoring of opiate drugs. Our results demonstrate that high quality antibodies can be used for immunosensor development against target analyte with greater sensitivity, specificity and precision than other available analytical methods. Conclusion: In this review we highlight the fundamentals of different transducer technologies and its applications for immunosensor development currently being developed in our laboratory using rapid screening via immunochromatographic kit, label free optical detection via enzyme, fluorescence, gold nanoparticles and carbon nanotubes based immunosensing for sensitive and specific monitoring of opiates. PMID:26929925

DOE Office of Scientific and Technical Information (OSTI.GOV)

Song, Ehwang; Gao, Yuqian; Wu, Chaochao

Here, mass spectrometry (MS) based targeted proteomic methods such as selected reaction monitoring (SRM) are becoming the method of choice for preclinical verification of candidate protein biomarkers. The Clinical Proteomic Tumor Analysis Consortium (CPTAC) of the National Cancer Institute has investigated the standardization and analytical validation of the SRM assays and demonstrated robust analytical performance on different instruments across different laboratories. An Assay Portal has also been established by CPTAC to provide the research community a resource consisting of large set of targeted MS-based assays, and a depository to share assays publicly, providing that assays meet the guidelines proposed bymore » CPTAC. Herein, we report 98 SRM assays covering 70 candidate protein biomarkers previously reported as associated with ovarian cancer that have been thoroughly characterized according to the CPTAC Assay Characterization Guidance Document. The experiments, methods and results for characterizing these SRM assays for their MS response, repeatability, selectivity, stability, and reproducible detection of endogenous analytes are described in detail.« less

Smart phone: a popular device supports amylase activity assay in fisheries research.

PubMed

Thongprajukaew, Karun; Choodum, Aree; Sa-E, Barunee; Hayee, Ummah

2014-11-15

Colourimetric determinations of amylase activity were developed based on a standard dinitrosalicylic acid (DNS) staining method, using maltose as the analyte. Intensities and absorbances of red, green and blue (RGB) were obtained with iPhone imaging and Adobe Photoshop image analysis. Correlation of green and analyte concentrations was highly significant, and the accuracy of the developed method was excellent in analytical performance. The common iPhone has sufficient imaging ability for accurate quantification of maltose concentrations. Detection limits, sensitivity and linearity were comparable to a spectrophotometric method, but provided better inter-day precision. In quantifying amylase specific activity from a commercial source (P>0.02) and fish samples (P>0.05), differences compared with spectrophotometric measurements were not significant. We have demonstrated that iPhone imaging with image analysis in Adobe Photoshop has potential for field and laboratory studies of amylase. Copyright © 2014 Elsevier Ltd. All rights reserved.

Ultraviolet, Visible, and Fluorescence Spectroscopy

NASA Astrophysics Data System (ADS)

Penner, Michael H.

Spectroscopy in the ultraviolet-visible (UV-Vis) range is one of the most commonly encountered laboratory techniques in food analysis. Diverse examples, such as the quantification of macrocomponents (total carbohydrate by the phenol-sulfuric acid method), quantification of microcomponents, (thiamin by the thiochrome fluorometric procedure), estimates of rancidity (lipid oxidation status by the thiobarbituric acid test), and surveillance testing (enzyme-linked immunoassays), are presented in this text. In each of these cases, the analytical signal for which the assay is based is either the emission or absorption of radiation in the UV-Vis range. This signal may be inherent in the analyte, such as the absorbance of radiation in the visible range by pigments, or a result of a chemical reaction involving the analyte, such as the colorimetric copper-based Lowry method for the analysis of soluble protein.

Quality in laboratory medicine: 50years on.

PubMed

Plebani, Mario

2017-02-01

The last 50years have seen substantial changes in the landscape of laboratory medicine: its role in modern medicine is in evolution and the quality of laboratory services is changing. The need to control and improve quality in clinical laboratories has grown hand in hand with the growth in technological developments leading to an impressive reduction of analytical errors over time. An essential cause of this impressive improvement has been the introduction and monitoring of quality indicators (QIs) such as the analytical performance specifications (in particular bias and imprecision) based on well-established goals. The evolving landscape of quality and errors in clinical laboratories moved first from analytical errors to all errors performed within the laboratory walls, subsequently to errors in laboratory medicine (including errors in test requesting and result interpretation), and finally, to a focus on errors more frequently associated with adverse events (laboratory-associated errors). After decades in which clinical laboratories have focused on monitoring and improving internal indicators of analytical quality, efficiency and productivity, it is time to shift toward indicators of total quality, clinical effectiveness and patient outcomes. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Nondestructive assessment of timber bridges using a vibration-based method

Treesearch

Xiping Wang; James P. Wacker; Robert J. Ross; Brian K. Brashaw

2005-01-01

This paper describes an effort to develop a global dynamic testing technique for evaluating the overall stiffness of timber bridge superstructures. A forced vibration method was used to measure the natural frequency of single-span timber bridges in the laboratory and field. An analytical model based on simple beam theory was proposed to represent the relationship...

Investigating Arsenic Contents in Surface and Drinking Water by Voltammetry and the Method of Standard Additions

ERIC Educational Resources Information Center

Cheng, Anran; Tyne, Rebecca; Kwok, Yu Ting; Rees, Louis; Craig, Lorraine; Lapinee, Chaipat; D'Arcy, Mitch; Weiss, Dominik J.; Salau¨n, Pascal

2016-01-01

Testing water samples for arsenic contamination has become an important water quality issue worldwide. Arsenic usually occurs in very small concentrations, and a sensitive analytical method is needed. We present here a 1-day laboratory module developed to introduce Earth Sciences and/or Chemistry student undergraduates to key aspects of this…

Determination of Copper and Zinc in Brass: Two Basic Methods

ERIC Educational Resources Information Center

Fabre, Paul-Louis; Reynes, Olivier

2010-01-01

In this experiment, the concentrations of copper and zinc in brass are obtained by two methods. This experiment does not require advanced instrumentation, uses inexpensive chemicals, and can be easily carried out during a 3-h upper-level undergraduate laboratory. Pedagogically, the basic concepts of analytical chemistry in solutions, such as pH,…

USGS Laboratory Review Program Ensures Analytical Quality

USGS Publications Warehouse

Erdmann, David E.

1995-01-01

The USGS operates a review program for laboratories that analyze samples for USGS environmental investigations. This program has been effective in providing QA feedback to laboratories while ensuring that analytical data are consistent, of satisfactory quality, and meet the data objectives of the investigation.

Rapid determination of residues of pesticides in honey by µGC-ECD and GC-MS/MS: Method validation and estimation of measurement uncertainty according to document No. SANCO/12571/2013.

PubMed

Paoloni, Angela; Alunni, Sabrina; Pelliccia, Alessandro; Pecorelli, Ivan

2016-01-01

A simple and straightforward method for simultaneous determination of residues of 13 pesticides in honey samples (acrinathrin, bifenthrin, bromopropylate, cyhalothrin-lambda, cypermethrin, chlorfenvinphos, chlorpyrifos, coumaphos, deltamethrin, fluvalinate-tau, malathion, permethrin and tetradifon) from different pesticide classes has been developed and validated. The analytical method provides dissolution of honey in water and an extraction of pesticide residues by n-Hexane followed by clean-up on a Florisil SPE column. The extract was evaporated and taken up by a solution of an injection internal standard (I-IS), ethion, and finally analyzed by capillary gas chromatography with electron capture detection (GC-µECD). Identification for qualitative purpose was conducted by gas chromatography with triple quadrupole mass spectrometer (GC-MS/MS). A matrix-matched calibration curve was performed for quantitative purposes by plotting the area ratio (analyte/I-IS) against concentration using a GC-µECD instrument. According to document No. SANCO/12571/2013, the method was validated by testing the following parameters: linearity, matrix effect, specificity, precision, trueness (bias) and measurement uncertainty. The analytical process was validated analyzing blank honey samples spiked at levels equal to and greater than 0.010 mg/kg (limit of quantification). All parameters were satisfactorily compared with the values established by document No. SANCO/12571/2013. The analytical performance was verified by participating in eight multi-residue proficiency tests organized by BIPEA, obtaining satisfactory z-scores in all 70 determinations. Measurement uncertainty was estimated according to the top-down approaches described in Appendix C of the SANCO document using the within-laboratory reproducibility relative standard deviation combined with laboratory bias using the proficiency test data.

Closing the brain-to-brain loop in laboratory testing.

PubMed

Plebani, Mario; Lippi, Giuseppe

2011-07-01

Abstract The delivery of laboratory services has been described 40 years ago and defined with the foremost concept of "brain-to-brain turnaround time loop". This concept consists of several processes, including the final step which is the action undertaken on the patient based on laboratory information. Unfortunately, the need for systematic feedback to improve the value of laboratory services has been poorly understood and, even more risky, poorly applied in daily laboratory practice. Currently, major problems arise from the unavailability of consensually accepted quality specifications for the extra-analytical phase of laboratory testing. This, in turn, does not allow clinical laboratories to calculate a budget for the "patient-related total error". The definition and use of the term "total error" refers only to the analytical phase, and should be better defined as "total analytical error" to avoid any confusion and misinterpretation. According to the hierarchical approach to classify strategies to set analytical quality specifications, the "assessment of the effect of analytical performance on specific clinical decision-making" is comprehensively at the top and therefore should be applied as much as possible to address analytical efforts towards effective goals. In addition, an increasing number of laboratories worldwide are adopting risk management strategies such as FMEA, FRACAS, LEAN and Six Sigma since these techniques allow the identification of the most critical steps in the total testing process, and to reduce the patient-related risk of error. As a matter of fact, an increasing number of laboratory professionals recognize the importance of understanding and monitoring any step in the total testing process, including the appropriateness of the test request as well as the appropriate interpretation and utilization of test results.

Can current analytical quality performance of UK clinical laboratories support evidence-based guidelines for diabetes and ischaemic heart disease?--A pilot study and a proposal.

PubMed

Jassam, Nuthar; Yundt-Pacheco, John; Jansen, Rob; Thomas, Annette; Barth, Julian H

2013-08-01

The implementation of national and international guidelines is beginning to standardise clinical practice. However, since many guidelines have decision limits based on laboratory tests, there is an urgent need to ensure that different laboratories obtain the same analytical result on any sample. A scientifically-based quality control process will be a pre-requisite to provide this level of analytical performance which will support evidence-based guidelines and movement of patients across boundaries while maintaining standardised outcomes. We discuss the finding of a pilot study performed to assess UK clinical laboratories readiness to work to a higher grade quality specifications such as biological variation-based quality specifications. Internal quality control (IQC) data for HbA1c, glucose, creatinine, cholesterol and high density lipoprotein (HDL)-cholesterol were collected from UK laboratories participating in the Bio-Rad Unity QC programme. The median of the coefficient of variation (CV%) of the participating laboratories was evaluated against the CV% based on biological variation. Except creatinine, the other four analytes had a variable degree of compliance with the biological variation-based quality specifications. More than 75% of the laboratories met the biological variation-based quality specifications for glucose, cholesterol and HDL-cholesterol. Slightly over 50% of the laboratories met the analytical goal for HBA1c. Only one analyte (cholesterol) had a performance achieving the higher quality specifications consistent with 5σ. Our data from IQC do not consistently demonstrate that the results from clinical laboratories meet evidence-based quality specifications. Therefore, we propose that a graded scale of quality specifications may be needed at this stage.

HPLC and chemometrics-assisted UV-spectroscopy methods for the simultaneous determination of ambroxol and doxycycline in capsule

NASA Astrophysics Data System (ADS)

Hadad, Ghada M.; El-Gindy, Alaa; Mahmoud, Waleed M. M.

2008-08-01

High-performance liquid chromatography (HPLC) and multivariate spectrophotometric methods are described for the simultaneous determination of ambroxol hydrochloride (AM) and doxycycline (DX) in combined pharmaceutical capsules. The chromatographic separation was achieved on reversed-phase C 18 analytical column with a mobile phase consisting of a mixture of 20 mM potassium dihydrogen phosphate, pH 6-acetonitrile in ratio of (1:1, v/v) and UV detection at 245 nm. Also, the resolution has been accomplished by using numerical spectrophotometric methods as classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS-1) applied to the UV spectra of the mixture and graphical spectrophotometric method as first derivative of the ratio spectra ( 1DD) method. Analytical figures of merit (FOM), such as sensitivity, selectivity, analytical sensitivity, limit of quantitation and limit of detection were determined for CLS, PLS-1 and PCR methods. The proposed methods were validated and successfully applied for the analysis of pharmaceutical formulation and laboratory-prepared mixtures containing the two component combination.

HPLC and chemometrics-assisted UV-spectroscopy methods for the simultaneous determination of ambroxol and doxycycline in capsule.

PubMed

Hadad, Ghada M; El-Gindy, Alaa; Mahmoud, Waleed M M

2008-08-01

High-performance liquid chromatography (HPLC) and multivariate spectrophotometric methods are described for the simultaneous determination of ambroxol hydrochloride (AM) and doxycycline (DX) in combined pharmaceutical capsules. The chromatographic separation was achieved on reversed-phase C(18) analytical column with a mobile phase consisting of a mixture of 20mM potassium dihydrogen phosphate, pH 6-acetonitrile in ratio of (1:1, v/v) and UV detection at 245 nm. Also, the resolution has been accomplished by using numerical spectrophotometric methods as classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS-1) applied to the UV spectra of the mixture and graphical spectrophotometric method as first derivative of the ratio spectra ((1)DD) method. Analytical figures of merit (FOM), such as sensitivity, selectivity, analytical sensitivity, limit of quantitation and limit of detection were determined for CLS, PLS-1 and PCR methods. The proposed methods were validated and successfully applied for the analysis of pharmaceutical formulation and laboratory-prepared mixtures containing the two component combination.

15. VIEW OF LABORATORY EQUIPMENT IN THE BUILDING 771 ANALYTICAL ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

15. VIEW OF LABORATORY EQUIPMENT IN THE BUILDING 771 ANALYTICAL LABORATORY. THE LAB ANALYZED SAMPLES FOR PLUTONIUM, AMERICIUM, URANIUM, NEPTUNIUM, AND OTHER RADIOACTIVE ISOTOPES. (9/25/62) - Rocky Flats Plant, Plutonium Recovery & Fabrication Facility, North-central section of plant, Golden, Jefferson County, CO

Merging Old and New: An Instrumentation-Based Introductory Analytical Laboratory

ERIC Educational Resources Information Center

Jensen, Mark B.

2015-01-01

An instrumentation-based laboratory curriculum combining traditional unknown analyses with student-designed projects has been developed for an introductory analytical chemistry course. In the first half of the course, students develop laboratory skills and instrumental proficiency by rotating through six different instruments performing…

Method of Analysis by the U.S. Geological Survey California District Sacramento Laboratory-- Determination of Dissolved Organic Carbon in Water by High Temperature Catalytic Oxidation, Method Validation, and Quality-Control Practices

USGS Publications Warehouse

Bird, Susan M.; Fram, Miranda S.; Crepeau, Kathryn L.

2003-01-01

An analytical method has been developed for the determination of dissolved organic carbon concentration in water samples. This method includes the results of the tests used to validate the method and the quality-control practices used for dissolved organic carbon analysis. Prior to analysis, water samples are filtered to remove suspended particulate matter. A Shimadzu TOC-5000A Total Organic Carbon Analyzer in the nonpurgeable organic carbon mode is used to analyze the samples by high temperature catalytic oxidation. The analysis usually is completed within 48 hours of sample collection. The laboratory reporting level is 0.22 milligrams per liter.

Reporting Results of Molecular Tests: A Retrospective Examination of BRAF Mutation Reporting.

PubMed

Treece, Amanda L; Gulley, Margaret L; Vasalos, Patricia; Paquette, Cherie; Lindeman, Neal I; Jennings, Lawrence J; Bartley, Angela N

2017-05-01

- With enormous growth in the field of molecular pathology, the reporting of results gleaned from this testing is essential to guide patient care. - To examine molecular reports from laboratories participating in proficiency testing for required elements to convey molecular laboratory test results to clinicians and patients. - Molecular laboratories participating in the College of American Pathologists (CAP) proficiency testing program for BRAF mutation analysis were solicited to submit examples of final reports from 2 separate proficiency testing reporting cycles. Reports were reviewed for the presence or absence of relevant components. - A total of 107 evaluable reports were received (57 demonstrating a positive result for the BRAF V600E mutation and 50 negative). Methods for BRAF testing varied, with 95% (102 of 107) of reports adequately describing their assay methods and 87% (93 of 107) of reports adequately describing the target(s) of their assays. Information on the analytic sensitivity of the assay was present in 74% (79 of 107) of reports and 83% (89 of 107) reported at least 1 assay limitation, though only 34% (36 of 107) reported on variants not detected by their assays. Analytic and clinical interpretive comments were included in 99% (106 of 107) and 90% (96 of 107) of reports, respectively. Of participants that perform a laboratory-developed test, 88% (88 of 100) included language addressing the development of the assay. - Laboratories participating in BRAF proficiency testing through the CAP are including most of the required reporting elements to unambiguously convey molecular results. Laboratories should continue to strive to report these results in a concise and comprehensive manner.

FIRST FLOOR PLAN OF REMOTE ANALYTICAL FACILITY (CPP627) SHOWING REMOTE ...

Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

FIRST FLOOR PLAN OF REMOTE ANALYTICAL FACILITY (CPP-627) SHOWING REMOTE ANALYTICAL LABORATORY, DECONTAMINATION ROOM, AND MULTICURIE CELL ROOM. INL DRAWING NUMBER 200-0627-00-008-105065. ALTERNATE ID NUMBER 4272-14-102. - Idaho National Engineering Laboratory, Idaho Chemical Processing Plant, Fuel Reprocessing Complex, Scoville, Butte County, ID

Evaluation of Brazilian Sugarcane Bagasse Characterization: An Interlaboratory Comparison Study

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sluiter, Justin B.; Chum, Helena; Gomes, Absai C.

2016-05-01

This paper describes a study of the variability of measured composition for a single bulk sugarcane bagasse conducted across eight laboratories using similar analytical methods, with the purpose of determining the expected variation for compositional analysis performed by different laboratories. The results show good agreement of measured composition within a single laboratory, but greater variability when results are compared among laboratories. These interlaboratory variabilities do not seem to be associated with a specific method or technique or any single piece of instrumentation. The summary censored statistics provide mean values and pooled standard deviations as follows: total extractives 6.7% (0.6%), wholemore » ash 1.5% (0.2%), glucan 42.3% (1.2%), xylan 22.3% (0.5%), total lignin 21.3% (0.4%), and total mass closure 99.4% (2.9%).« less

A field study of selected U.S. Geological Survey analytical methods for measuring pesticides in filtered stream water, June - September 2012

USGS Publications Warehouse

Martin, Jeffrey D.; Norman, Julia E.; Sandstrom, Mark W.; Rose, Claire E.

2017-09-06

U.S. Geological Survey monitoring programs extensively used two analytical methods, gas chromatography/mass spectrometry and liquid chromatography/mass spectrometry, to measure pesticides in filtered water samples during 1992–2012. In October 2012, the monitoring programs began using direct aqueous-injection liquid chromatography tandem mass spectrometry as a new analytical method for pesticides. The change in analytical methods, however, has the potential to inadvertently introduce bias in analysis of datasets that span the change.A field study was designed to document performance of the new method in a variety of stream-water matrices and to quantify any potential changes in measurement bias or variability that could be attributed to changes in analytical methods. The goals of the field study were to (1) summarize performance (bias and variability of pesticide recovery) of the new method in a variety of stream-water matrices; (2) compare performance of the new method in laboratory blank water (laboratory reagent spikes) to that in a variety of stream-water matrices; (3) compare performance (analytical recovery) of the new method to that of the old methods in a variety of stream-water matrices; (4) compare pesticide detections and concentrations measured by the new method to those of the old methods in a variety of stream-water matrices; (5) compare contamination measured by field blank water samples in old and new methods; (6) summarize the variability of pesticide detections and concentrations measured by the new method in field duplicate water samples; and (7) identify matrix characteristics of environmental water samples that adversely influence the performance of the new method. Stream-water samples and a variety of field quality-control samples were collected at 48 sites in the U.S. Geological Survey monitoring networks during June–September 2012. Stream sites were located across the United States and included sites in agricultural and urban land-use settings, as well as sites on major rivers.The results of the field study identified several challenges for the analysis and interpretation of data analyzed by both old and new methods, particularly when data span the change in methods and are combined for analysis of temporal trends in water quality. The main challenges identified are large (greater than 30 percent), statistically significant differences in analytical recovery, detection capability, and (or) measured concentrations for selected pesticides. These challenges are documented and discussed, but specific guidance or statistical methods to resolve these differences in methods are beyond the scope of the report. The results of the field study indicate that the implications of the change in analytical methods must be assessed individually for each pesticide and method.Understanding the possible causes of the systematic differences in concentrations between methods that remain after recovery adjustment might be necessary to determine how to account for the differences in data analysis. Because recoveries for each method are independently determined from separate reference standards and spiking solutions, the differences might be due to an error in one of the reference standards or solutions or some other basic aspect of standard procedure in the analytical process. Further investigation of the possible causes is needed, which will lead to specific decisions on how to compensate for these differences in concentrations in data analysis. In the event that further investigations do not provide insight into the causes of systematic differences in concentrations between methods, the authors recommend continuing to collect and analyze paired environmental water samples by both old and new methods. This effort should be targeted to seasons, sites, and expected concentrations to supplement those concentrations already assessed and to compare the ongoing analytical recovery of old and new methods to those observed in the summer and fall of 2012.

Clinical Chemistry Laboratory Automation in the 21st Century - Amat Victoria curam (Victory loves careful preparation)

PubMed Central

Armbruster, David A; Overcash, David R; Reyes, Jaime

2014-01-01

The era of automation arrived with the introduction of the AutoAnalyzer using continuous flow analysis and the Robot Chemist that automated the traditional manual analytical steps. Successive generations of stand-alone analysers increased analytical speed, offered the ability to test high volumes of patient specimens, and provided large assay menus. A dichotomy developed, with a group of analysers devoted to performing routine clinical chemistry tests and another group dedicated to performing immunoassays using a variety of methodologies. Development of integrated systems greatly improved the analytical phase of clinical laboratory testing and further automation was developed for pre-analytical procedures, such as sample identification, sorting, and centrifugation, and post-analytical procedures, such as specimen storage and archiving. All phases of testing were ultimately combined in total laboratory automation (TLA) through which all modules involved are physically linked by some kind of track system, moving samples through the process from beginning-to-end. A newer and very powerful, analytical methodology is liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). LC-MS/MS has been automated but a future automation challenge will be to incorporate LC-MS/MS into TLA configurations. Another important facet of automation is informatics, including middleware, which interfaces the analyser software to a laboratory information systems (LIS) and/or hospital information systems (HIS). This software includes control of the overall operation of a TLA configuration and combines analytical results with patient demographic information to provide additional clinically useful information. This review describes automation relevant to clinical chemistry, but it must be recognised that automation applies to other specialties in the laboratory, e.g. haematology, urinalysis, microbiology. It is a given that automation will continue to evolve in the clinical laboratory, limited only by the imagination and ingenuity of laboratory scientists. PMID:25336760

Clinical Chemistry Laboratory Automation in the 21st Century - Amat Victoria curam (Victory loves careful preparation).

PubMed

Armbruster, David A; Overcash, David R; Reyes, Jaime

2014-08-01

The era of automation arrived with the introduction of the AutoAnalyzer using continuous flow analysis and the Robot Chemist that automated the traditional manual analytical steps. Successive generations of stand-alone analysers increased analytical speed, offered the ability to test high volumes of patient specimens, and provided large assay menus. A dichotomy developed, with a group of analysers devoted to performing routine clinical chemistry tests and another group dedicated to performing immunoassays using a variety of methodologies. Development of integrated systems greatly improved the analytical phase of clinical laboratory testing and further automation was developed for pre-analytical procedures, such as sample identification, sorting, and centrifugation, and post-analytical procedures, such as specimen storage and archiving. All phases of testing were ultimately combined in total laboratory automation (TLA) through which all modules involved are physically linked by some kind of track system, moving samples through the process from beginning-to-end. A newer and very powerful, analytical methodology is liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). LC-MS/MS has been automated but a future automation challenge will be to incorporate LC-MS/MS into TLA configurations. Another important facet of automation is informatics, including middleware, which interfaces the analyser software to a laboratory information systems (LIS) and/or hospital information systems (HIS). This software includes control of the overall operation of a TLA configuration and combines analytical results with patient demographic information to provide additional clinically useful information. This review describes automation relevant to clinical chemistry, but it must be recognised that automation applies to other specialties in the laboratory, e.g. haematology, urinalysis, microbiology. It is a given that automation will continue to evolve in the clinical laboratory, limited only by the imagination and ingenuity of laboratory scientists.

Green analytical chemistry introduction to chloropropanols determination at no economic and analytical performance costs?

PubMed

Jędrkiewicz, Renata; Orłowski, Aleksander; Namieśnik, Jacek; Tobiszewski, Marek

2016-01-15

In this study we perform ranking of analytical procedures for 3-monochloropropane-1,2-diol determination in soy sauces by PROMETHEE method. Multicriteria decision analysis was performed for three different scenarios - metrological, economic and environmental, by application of different weights to decision making criteria. All three scenarios indicate capillary electrophoresis-based procedure as the most preferable. Apart from that the details of ranking results differ for these three scenarios. The second run of rankings was done for scenarios that include metrological, economic and environmental criteria only, neglecting others. These results show that green analytical chemistry-based selection correlates with economic, while there is no correlation with metrological ones. This is an implication that green analytical chemistry can be brought into laboratories without analytical performance costs and it is even supported by economic reasons. Copyright © 2015 Elsevier B.V. All rights reserved.

1990 National Water Quality Laboratory Services Catalog

USGS Publications Warehouse

Pritt, Jeffrey; Jones, Berwyn E.

1989-01-01

PREFACE This catalog provides information about analytical services available from the National Water Quality Laboratory (NWQL) to support programs of the Water Resources Division of the U.S. Geological Survey. To assist personnel in the selection of analytical services, the catalog lists cost, sample volume, applicable concentration range, detection level, precision of analysis, and preservation techniques for samples to be submitted for analysis. Prices for services reflect operationa1 costs, the complexity of each analytical procedure, and the costs to ensure analytical quality control. The catalog consists of five parts. Part 1 is a glossary of terminology; Part 2 lists the bottles, containers, solutions, and other materials that are available through the NWQL; Part 3 describes the field processing of samples to be submitted for analysis; Part 4 describes analytical services that are available; and Part 5 contains indices of analytical methodology and Chemical Abstract Services (CAS) numbers. Nomenclature used in the catalog is consistent with WATSTORE and STORET. The user is provided with laboratory codes and schedules that consist of groupings of parameters which are measured together in the NWQL. In cases where more than one analytical range is offered for a single element or compound, different laboratory codes are given. Book 5 of the series 'Techniques of Water Resources Investigations of the U.S. Geological Survey' should be consulted for more information about the analytical procedures included in the tabulations. This catalog supersedes U.S. Geological Survey Open-File Report 86-232 '1986-87-88 National Water Quality Laboratory Services Catalog', October 1985.

Environmental Response Laboratory Network (ERLN) Data Submission Requirements

EPA Pesticide Factsheets

These Environmental Response Laboratory Network specifications are essential to the mission of providing consistent analytical data of know and documented quality for each Analytical Service Request (ASR).

External quality-assurance results for the National Atmospheric Deposition Program and the National Trends Network during 1986

USGS Publications Warehouse

See, Randolph B.; Schroder, LeRoy J.; Willoughby, Timothy C.

1988-01-01

During 1986, the U.S. Geological Survey operated three programs to provide external quality-assurance monitoring of the National Atmospheric Deposition Program and National Trends Network. An intersite-comparison program was used to assess the accuracy of onsite pH and specific-conductance determinations at quarterly intervals. The blind-audit program was used to assess the effect of routine sample handling on the precision and bias of program and network wet-deposition data. Analytical results from four laboratories, which routinely analyze wet-deposition samples, were examined to determine if differences existed between laboratory analytical results and to provide estimates of the analytical precision of each laboratory. An average of 78 and 89 percent of the site operators participating in the intersite-comparison met the network goals for pH and specific conductance. A comparison of analytical values versus actual values for samples submitted as part of the blind-audit program indicated that analytical values were slightly but significantly (a = 0.01) larger than actual values for pH, magnesium, sodium, and sulfate; analytical values for specific conductance were slightly less than actual values. The decreased precision in the analyses of blind-audit samples when compared to interlaboratory studies indicates that a large amount of uncertainty in network deposition data may be a result of routine field operations. The results of the interlaboratory comparison study indicated that the magnitude of the difference between laboratory analyses was small for all analytes. Analyses of deionized, distilled water blanks by participating laboratories indicated that the laboratories had difficulty measuring analyte concentrations near their reported detection limits. (USGS)

Response to comment on “Persistence of pharmaceutical compounds and other organic wastewater contaminants in a conventional drinking-water-treatment plant”

USGS Publications Warehouse

Stackelberg, Paul E.; Furlong, Edward T.; Meyer, Michael T.; Zaugg, Steven D.; Henderson, Alden K.; Reissman, Dori B.

2006-01-01

The U.S. Geological Survey (USGS) and the Centers for Disease Control thank Dr. Till for her comments concerning our research (Till, 2005) and welcome the opportunity to respond. The primary objective of our study was to evaluate the potential for organic wastewater-related contaminants (OWCs), including pharmaceuticals, to survive a conventional drinking-water-treatment process and persist in potable-water supplies (Stackelberg et al., 2004). Our study was supported by two USGS laboratories: the National Water Quality Laboratory (NWQL), which provided the HPLC/ESI-MS and CLLE GC/MS data and the Ocala Water Quality and Research Laboratory (OWQRL), which provided the LC/MS data (Stackelberg et al., 2004). Although discussed as distinct techniques by Dr. Till and indicated by differing acronyms to distinguish the laboratories producing the data, as described in our paper, the two LC/MS methods are very similar; they consist of a solid-phase extraction method with analysis of the extract produced using high-performance liquid chromatography coupled to an electrospray ionization mass spectrometer operated in the positive mode. The NWQL and OWQRL report ‘trace’ and ‘ultratrace’ determinations of analytes that provide significant benefit for describing the presence and fate of low-level contaminants. For mass spectral methods, an analyte is qualitatively identified by its retention time on the chromatographic column as well as the presence of two or more confirming ions with area ratios that match that of the reference standard compounds. Because of a recognized increased risk of false positives, these qualitative identification criteria are used in conjunction with abundant quality-control samples (detailed below) to confirm detection prior to making an estimate of the concentration. These qualitative identification criteria must be met before a compound is considered present (or detected) in a sample (Oblinger Childress et al., 1999). When a compound has been qualitatively identified in an environmental sample (whether above or below its reporting level [RL]), it is assessed in context with associated field and laboratory blanks, field and laboratory replicates, and other data, such as appropriate laboratory reagent spikes. An environmental concentration is calculated only after determining that field and laboratory procedures did not contaminate the samples. The concentrations are then calculated from 5- to 8-point calibration curves using internal standard quantitation. Our lowest calibration standard is intentionally much lower than the RL, typically 10 times lower. The most abundant molecular or fragment ion is used for quantitation, and, for the two LC/MS methods, at least one, and where possible two, qualifier ions are used for confirmation. For the GC/MS method, with its greater degree of fragmentation, one quantitation and two qualifier ions are used. When any of the abovementioned qualitative identification criteria are not met, the analyte is considered not present and is reported as “less than” the RL.

Useful measures and models for analytical quality management in medical laboratories.

PubMed

Westgard, James O

2016-02-01

The 2014 Milan Conference "Defining analytical performance goals 15 years after the Stockholm Conference" initiated a new discussion of issues concerning goals for precision, trueness or bias, total analytical error (TAE), and measurement uncertainty (MU). Goal-setting models are critical for analytical quality management, along with error models, quality-assessment models, quality-planning models, as well as comprehensive models for quality management systems. There are also critical underlying issues, such as an emphasis on MU to the possible exclusion of TAE and a corresponding preference for separate precision and bias goals instead of a combined total error goal. This opinion recommends careful consideration of the differences in the concepts of accuracy and traceability and the appropriateness of different measures, particularly TAE as a measure of accuracy and MU as a measure of traceability. TAE is essential to manage quality within a medical laboratory and MU and trueness are essential to achieve comparability of results across laboratories. With this perspective, laboratory scientists can better understand the many measures and models needed for analytical quality management and assess their usefulness for practical applications in medical laboratories.

An improved method of chemical analysis for low levels of nitrogen in forest streams or in rainwater.

Treesearch

Elly E. Holcombe; Duane G. Moore; Richard L. Fredriksen

1986-01-01

A modification of the macro-Kjeldahl method that provides increased sensitivity was developed for determining very low levels of nitrogen in forest streams and in rain-water. The method is suitable as a routine laboratory procedure. Analytical range of the method is 0.02 to 1.5 mg/L with high recovery and excellent precision and ac-curacy. The range can be increased to...

Certification of elements in and use of standard reference material 3280 multivitamin/multielement tablets.

PubMed

Turk, Gregory C; Sharpless, Katherine E; Cleveland, Danielle; Jongsma, Candice; Mackey, Elizabeth A; Marlow, Anthony F; Oflaz, Rabia; Paul, Rick L; Sieber, John R; Thompson, Robert Q; Wood, Laura J; Yu, Lee L; Zeisler, Rolf; Wise, Stephen A; Yen, James H; Christopher, Steven J; Day, Russell D; Long, Stephen E; Greene, Ella; Harnly, James; Ho, I-Pin; Betz, Joseph M

2013-01-01

Standard Reference Material 3280 Multivitamin/ Multielement Tablets was issued by the National Institute of Standards and Technology in 2009, and has certified and reference mass fraction values for 13 vitamins, 26 elements, and two carotenoids. Elements were measured using two or more analytical methods at NIST with additional data contributed by collaborating laboratories. This reference material is expected to serve a dual purpose: to provide quality assurance in support of a database of dietary supplement products and to provide a means for analysts, dietary supplement manufacturers, and researchers to assess the appropriateness and validity of their analytical methods and the accuracy of their results.

The quality of veterinary in-clinic and reference laboratory biochemical testing.

PubMed

Rishniw, Mark; Pion, Paul D; Maher, Tammy

2012-03-01

Although evaluation of biochemical analytes in blood is common in veterinary practice, studies assessing the global quality of veterinary in-clinic and reference laboratory testing have not been reported. The aim of this study was to assess the quality of biochemical testing in veterinary laboratories using results obtained from analyses of 3 levels of assayed quality control materials over 5 days. Quality was assessed by comparison of calculated total error with quality requirements, determination of sigma metrics, use of a quality goal index to determine factors contributing to poor performance, and agreement between in-clinic and reference laboratory mean results. The suitability of in-clinic and reference laboratory instruments for statistical quality control was determined using adaptations from the computerized program, EZRules3. Reference laboratories were able to achieve desirable quality requirements more frequently than in-clinic laboratories. Across all 3 materials, > 50% of in-clinic analyzers achieved a sigma metric ≥ 6.0 for measurement of 2 analytes, whereas > 50% of reference laboratory analyzers achieved a sigma metric ≥ 6.0 for measurement of 6 analytes. Expanded uncertainty of measurement and ± total allowable error resulted in the highest mean percentages of analytes demonstrating agreement between in-clinic and reference laboratories. Owing to marked variation in bias and coefficient of variation between analyzers of the same and different types, the percentages of analytes suitable for statistical quality control varied widely. These findings reflect the current state-of-the-art with regard to in-clinic and reference laboratory analyzer performance and provide a baseline for future evaluations of the quality of veterinary laboratory testing. © 2012 American Society for Veterinary Clinical Pathology.

National survey on the pre-analytical variability in a representative cohort of Italian laboratories.

PubMed

Lippi, Giuseppe; Montagnana, Martina; Giavarina, Davide

2006-01-01

Owing to remarkable advances in automation, laboratory technology and informatics, the pre-analytical phase has become the major source of variability in laboratory testing. The present survey investigated the development of several pre-analytical processes within a representative cohort of Italian clinical laboratories. A seven-point questionnaire was designed to investigate the following issues: 1a) the mean outpatient waiting time before check-in and 1b) the mean time from check-in to sample collection; 2) the mean time from sample collection to analysis; 3) the type of specimen collected for clinical chemistry testing; 4) the degree of pre-analytical automation; 5a) the number of samples shipped to other laboratories and 5b) the availability of standardised protocols for transportation; 6) the conditions for specimen storage; and 7) the availability and type of guidelines for management of unsuitable specimens. The questionnaire was administered to 150 laboratory specialists attending the SIMEL (Italian Society of Laboratory Medicine) National Meeting in June 2006. 107 questionnaires (71.3%) were returned. Data analysis revealed a high degree of variability among laboratories for the time required for check-in, outpatient sampling, sample transportation to the referral laboratory and analysis upon the arrival. Only 31% of laboratories have automated some pre-analytical steps. Of the 87% of laboratories that ship specimens to other facilities without sample preparation, 19% have no standardised protocol for transportation. For conventional clinical chemistry testing, 74% of the laboratories use serum evacuated tubes (59% with and 15% without serum separator), whereas the remaining 26% use lithium-heparin evacuated tubes (11% with and 15% without plasma separator). The storage period and conditions for rerun/retest vary widely. Only 63% of laboratories have a codified procedure for the management of unsuitable specimens, which are recognised by visual inspection (69%) or automatic detection (29%). Only 56% of the laboratories have standardised procedures for the management of unsuitable specimens, which vary widely on a local basis. The survey highlights broad heterogeneity in several pre-analytical processes among Italian laboratories. The lack of reliable guidelines encompassing evidence-based practice is a major problem for the standardisation of this crucial part of the testing process and represents a major challenge for laboratory medicine in the 2000s.

Quality-assurance results for field pH and specific-conductance measurements, and for laboratory analysis, National Atmospheric Deposition Program and National Trends Network; January 1980-September 1984

USGS Publications Warehouse

Schroder, L.J.; Brooks, M.H.; Malo, B.A.; Willoughby, T.C.

1986-01-01

Five intersite comparison studies for the field determination of pH and specific conductance, using simulated-precipitation samples, were conducted by the U.S.G.S. for the National Atmospheric Deposition Program and National Trends Network. These comparisons were performed to estimate the precision of pH and specific conductance determinations made by sampling-site operators. Simulated-precipitation samples were prepared from nitric acid and deionized water. The estimated standard deviation for site-operator determination of pH was 0.25 for pH values ranging from 3.79 to 4.64; the estimated standard deviation for specific conductance was 4.6 microsiemens/cm at 25 C for specific-conductance values ranging from 10.4 to 59.0 microsiemens/cm at 25 C. Performance-audit samples with known analyte concentrations were prepared by the U.S.G.S.and distributed to the National Atmospheric Deposition Program 's Central Analytical Laboratory. The differences between the National Atmospheric Deposition Program and national Trends Network-reported analyte concentrations and known analyte concentrations were calculated, and the bias and precision were determined. For 1983, concentrations of calcium, magnesium, sodium, and chloride were biased at the 99% confidence limit; concentrations of potassium and sulfate were unbiased at the 99% confidence limit. Four analytical laboratories routinely analyzing precipitation were evaluated in their analysis of identical natural- and simulated precipitation samples. Analyte bias for each laboratory was examined using analysis of variance coupled with Duncan 's multiple-range test on data produced by these laboratories, from the analysis of identical simulated-precipitation samples. Analyte precision for each laboratory has been estimated by calculating a pooled variance for each analyte. Interlaboratory comparability results may be used to normalize natural-precipitation chemistry data obtained from two or more of these laboratories. (Author 's abstract)

A simplified method for monomeric carbohydrate analysis of corn stover biomass

USDA-ARS?s Scientific Manuscript database

Constituent determination of biomass for theoretical ethanol yield (TEY) estimation requires the removal of non-structural carbohydrates prior to analysis to prevent interference with the analytical procedure. According to the accepted U.S. Dept. of Energy-National Renewable Energy Laboratory (NREL)...

A SIMPLE COLORIMETRIC METHOD TO DETECT BIOLOGICAL EVIDENCE OF HUMAN EXPOSURE TO MICROCYSTINS

EPA Science Inventory

Toxic cyanobacteria are contaminants of surface waters worldwide. Microcystins are some of the most commonly detected toxins. Biological evidence of human exposure may be difficult to obtain due to limitations associated with cost, laboratory capacity, analytic support, and exp...

40 CFR 80.47 - Performance-based Analytical Test Method Approach.

Code of Federal Regulations, 2014 CFR

2014-07-01

... chemistry and statistics, or at least a bachelor's degree in chemical engineering, from an accredited... be compensated for any known chemical interferences using good laboratory practices. (3) The test... section, individual test results shall be compensated for any known chemical interferences using good...

Teaching Chemical Technique: A Review of the Literature.

ERIC Educational Resources Information Center

DeMeo, Stephen

2001-01-01

Determines through an historical review of the literature some of the most effective ways to teach manipulative skills in chemistry. Reviews chemical education journals, laboratory manuals, early American chemistry textbooks, analytical chemistry texts, and science education textbooks and journals that address instructional methods for teaching…

BetaScint{trademark} fiber-optic sensor for detecting strontium-90 and uranium-238 in soil. Innovative technology summary report

DOE Office of Scientific and Technical Information (OSTI.GOV)

NONE

1998-12-01

Accurate measurements of radioactivity in soils contaminated with Strontium-90 (Sr-90) or Uranium-238 (U-238) are essential for many DOE site remediation programs. These crucial measurements determine if excavation and soil removal is necessary, where remediation efforts should be focused, and/or if a site has reached closure. Measuring soil contamination by standard EPA laboratory methods typically takes a week (accelerated analytical test turnaround) or a month (standard analytical test turnaround). The time delay extends to operations involving heavy excavation equipment and associated personnel which are the main costs of remediation. This report describes an application of the BetaScint{trademark} fiber-optic sensor that measuresmore » Sr-90 or U-238 contamination in soil samples on site in about 20 minutes, at a much lower cost than time-consuming laboratory methods, to greatly facilitate remediation. This report describes the technology, its performance, its uses, cost, regulatory and policy issues, and lessons learned.« less

Green Chemistry Metrics with Special Reference to Green Analytical Chemistry.

PubMed

Tobiszewski, Marek; Marć, Mariusz; Gałuszka, Agnieszka; Namieśnik, Jacek

2015-06-12

The concept of green chemistry is widely recognized in chemical laboratories. To properly measure an environmental impact of chemical processes, dedicated assessment tools are required. This paper summarizes the current state of knowledge in the field of development of green chemistry and green analytical chemistry metrics. The diverse methods used for evaluation of the greenness of organic synthesis, such as eco-footprint, E-Factor, EATOS, and Eco-Scale are described. Both the well-established and recently developed green analytical chemistry metrics, including NEMI labeling and analytical Eco-scale, are presented. Additionally, this paper focuses on the possibility of the use of multivariate statistics in evaluation of environmental impact of analytical procedures. All the above metrics are compared and discussed in terms of their advantages and disadvantages. The current needs and future perspectives in green chemistry metrics are also discussed.

Collection methods and quality assessment for Esche-richia coli, water quality, and microbial source tracking data within Tumacácori National Historical Park and the upper Santa Cruz River, Arizona, 2015-16

USGS Publications Warehouse

Paretti, Nicholas; Coes, Alissa L.; Kephart, Christopher M.; Mayo, Justine

2018-03-05

Tumacácori National Historical Park protects the culturally important Mission, San José de Tumacácori, while also managing a portion of the ecologically diverse riparian corridor of the Santa Cruz River. This report describes the methods and quality assurance procedures used in the collection of water samples for the analysis of Escherichia coli (E. coli), microbial source tracking markers, suspended sediment, water-quality parameters, turbidity, and the data collection for discharge and stage; the process for data review and approval is also described. Finally, this report provides a quantitative assessment of the quality of the E. coli, microbial source tracking, and suspended sediment data.The data-quality assessment revealed that bias attributed to field and laboratory contamination was minimal, with E. coli detections in only 3 out of 33 field blank samples analyzed. Concentrations in the field blanks were several orders of magnitude lower than environmental concentrations. The microbial source tracking (MST) field blank was below the detection limit for all MST markers analyzed. Laboratory blanks for E. coli at the USGS Arizona Water Science Center and laboratory blanks for MST markers at the USGS Ohio Water Microbiology Laboratory were all below the detection limit. Irreplicate data for E. coli and suspended sediment indicated that bias was not introduced to the data by combining samples collected using discrete sampling methods with samples collected using automatic sampling methods.The split and sequential E. coli replicate data showed consistent analytical variability and a single equation was developed to explain the variability of E. coli concentrations. An additional analysis of analytical variability for E. coli indicated analytical variability around 18 percent relative standard deviation and no trend was observed in the concentration during the processing and analysis of multiple split-replicates. Two replicate samples were collected for MST and individual markers were compared for a base flow and flood sample. For the markers found in common between the two types of samples, the relative standard deviation for the base flow sample was more than 3 times greater than the markers in the flood sample. Sequential suspended sediment replicates had a relative standard deviation of about 1.3 percent, indicating that environmental and analytical variability was minimal.A holding time review and laboratory study analysis supported the extended holding times required for this investigation. Most concentrations for flood and base-flow samples were within the theoretical variability specified in the most probable number approach suggesting that extended hold times did not overly influence the final concentrations reported.

Evaluation of chemical data from selected sites in the Surface-Water Ambient Monitoring Program (SWAMP) in Florida

USGS Publications Warehouse

Katz, B.G.; Collins, J.J.

1998-01-01

A cooperative study between the Florida Department of Environmental Protection (FDEP) and the U.S. Geological Survey was conducted to assess the integrity of selected water-quality data collected at 150 sites in the FDEP Surface-Water Ambient Monitoring Program (SWAMP) in Florida. The assessment included determining the consistency of the water-quality data collected statewide, including commonality of monitoring procedures and analytes, screening of the gross validity of a chemical analysis, and quality assurance and quality control (QA/QC) procedures. Four tests were used to screen data at selected SWAMP sites to estimate the gross validity of selected chemical data: (1) the ratio of dissolved solids (in milligrams per liter) to specific conductance (in microsiemens per centimeter); (2) the ratio of total cations (in milliequivalents per liter) multiplied by 100 to specific conductance (in microsiemens per centimeter); (3) the ratio of total anions (in milliequivalents per liter) multiplied by 100 to specific conductance (in microsiemens per centimeter); and (4) the ionic charge-balance error. Although the results of the four screening tests indicate that the chemical data generally are quite reliable, the extremely small number of samples (less than 5 percent of the total number of samples) with sufficient chemical information to run the tests may not provide a representative indication of the analytical accuracy of all laboratories in the program. In addition to the four screening tests, unusually low or high values were flagged for field and laboratory pH (less than 4.0 and greater than 9.0) and specific conductance (less than 10 and greater than 10,000 microsiemens per centimeter). The numbers of flagged data were less than 1 percent of the 19,937 water samples with pH values and less than 0.6 percent of the 16,553 water samples with specific conductance values. Thirty-four agencies responded to a detailed questionnaire that was sent to more than 60 agencies involved in the collection and analysis of surface-water-quality data for SWAMP. The purpose of the survey was to evaluate quality assurance methods and consistency of methods statewide. Information was compiled and summarized on monitoring network design, data review and upload procedures, laboratory and field sampling methods, and data practices. Currently, most agencies that responded to the survey follow FDEP-approved QA/QC protocol for sampling and have quality assurance practices for recording and reporting data. Also, most agencies responded that calibration procedures were followed in the laboratory for analysis of data, but no responses were given about the specific procedures. Approximately 50 percent of the respondents indicated that laboratory analysis methods have changed over time. With so many laboratories involved in analyzing samples for SWAMP, it is difficult to compare water quality from one site to another due to different reporting conventions for chemical constituents and different analytical methods over time. Most agencies responded that calibration methods are followed in the field, but no specific details were provided. Grab samples are the most common method of collection. Other data screening procedures are necessary to further evaluate the validity of chemical data collected at SWAMP sites. High variability in the concentration of targeted constituents may signal analytical problems, but more likely changes in concentration are related to hydrologic conditions. This underscores the need for accurate measurements of discharge, lake stage, tidal stage at the time of sampling so that changes in constituent concentrations can be properly evaluated and fluxes (loads) of nutrients or metals, for example, can be calculated and compared over time.

Chiral Analysis by Tandem Mass Spectrometry Using the Kinetic Method, by Polarimetry, and by [Superscript 1]H NMR Spectroscopy

ERIC Educational Resources Information Center

Fedick, Patrick W.; Bain, Ryan M.; Bain, Kinsey; Cooks, R. Graham

2017-01-01

The goal of this laboratory exercise was for students to understand the concept of chirality and how enantiomeric excess (ee) is experimentally determined using the analysis of ibuprofen as an example. Students determined the enantiomeric excess of the analyte by three different instrumental methods: mass spectrometry, nuclear magnetic resonance…

Nondestructive assessment of single-span timber bridges using a vibration- based method

Treesearch

Xiping Wang; James P. Wacker; Angus M. Morison; John W. Forsman; John R. Erickson; Robert J. Ross

2005-01-01

This paper describes an effort to develop a global dynamic testing technique for evaluating the overall stiffness of timber bridge superstructures. A forced vibration method was used to measure the natural frequency of single-span timber bridges in the laboratory and field. An analytical model based on simple beam theory was proposed to represent the relationship...

DEVELOPMERNT OF A LOW-LEVEL ANALYTICAL METHOD FOR CO-PLANAR PCB CONGENERS IN SOIL/SEDIMENT MATRICES USING GC/ECD.

EPA Science Inventory

The method development is on-going in the Region 10 Laboratory. The conditions of the separation technique is complete. The MDLs have been determined to be between 3 to 6 ppt in marine sediment for co-planar PCB congeners #77; #81; #126 and #169. The procedure has been used fo...

Determination of Total Solids and Ash in Algal Biomass: Laboratory Analytical Procedure (LAP)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Van Wychen, Stefanie; Laurens, Lieve M. L.

2016-01-13

This procedure describes the methods used to determine the amount of moisture or total solids present in a freeze-dried algal biomass sample, as well as the ash content. A traditional convection oven drying procedure is covered for total solids content, and a dry oxidation method at 575 deg. C is covered for ash content.

Which Method Is Most Precise; Which Is Most Accurate? An Undergraduate Experiment

ERIC Educational Resources Information Center

Jordan, A. D.

2007-01-01

A simple experiment, the determination of the density of a liquid by several methods, is presented. Since the concept of density is a familiar one, the experiment is suitable for the introductory laboratory period of a first- or second-year course in physical or analytical chemistry. The main objective of the experiment is to familiarize students…

Analytical performance specifications for external quality assessment - definitions and descriptions.

PubMed

Jones, Graham R D; Albarede, Stephanie; Kesseler, Dagmar; MacKenzie, Finlay; Mammen, Joy; Pedersen, Morten; Stavelin, Anne; Thelen, Marc; Thomas, Annette; Twomey, Patrick J; Ventura, Emma; Panteghini, Mauro

2017-06-27

External Quality Assurance (EQA) is vital to ensure acceptable analytical quality in medical laboratories. A key component of an EQA scheme is an analytical performance specification (APS) for each measurand that a laboratory can use to assess the extent of deviation of the obtained results from the target value. A consensus conference held in Milan in 2014 has proposed three models to set APS and these can be applied to setting APS for EQA. A goal arising from this conference is the harmonisation of EQA APS between different schemes to deliver consistent quality messages to laboratories irrespective of location and the choice of EQA provider. At this time there are wide differences in the APS used in different EQA schemes for the same measurands. Contributing factors to this variation are that the APS in different schemes are established using different criteria, applied to different types of data (e.g. single data points, multiple data points), used for different goals (e.g. improvement of analytical quality; licensing), and with the aim of eliciting different responses from participants. This paper provides recommendations from the European Federation of Laboratory Medicine (EFLM) Task and Finish Group on Performance Specifications for External Quality Assurance Schemes (TFG-APSEQA) and on clear terminology for EQA APS. The recommended terminology covers six elements required to understand APS: 1) a statement on the EQA material matrix and its commutability; 2) the method used to assign the target value; 3) the data set to which APS are applied; 4) the applicable analytical property being assessed (i.e. total error, bias, imprecision, uncertainty); 5) the rationale for the selection of the APS; and 6) the type of the Milan model(s) used to set the APS. The terminology is required for EQA participants and other interested parties to understand the meaning of meeting or not meeting APS.

Destructive analysis capabilities for plutonium and uranium characterization at Los Alamos National Laboratory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tandon, Lav; Kuhn, Kevin J; Drake, Lawrence R

Los Alamos National Laboratory's (LANL) Actinide Analytical Chemistry (AAC) group has been in existence since the Manhattan Project. It maintains a complete set of analytical capabilities for performing complete characterization (elemental assay, isotopic, metallic and non metallic trace impurities) of uranium and plutonium samples in different forms. For a majority of the customers there are strong quality assurance (QA) and quality control (QC) objectives including highest accuracy and precision with well defined uncertainties associated with the analytical results. Los Alamos participates in various international and national programs such as the Plutonium Metal Exchange Program, New Brunswick Laboratory's (NBL' s) Safeguardsmore » Measurement Evaluation Program (SME) and several other inter-laboratory round robin exercises to monitor and evaluate the data quality generated by AAC. These programs also provide independent verification of analytical measurement capabilities, and allow any technical problems with analytical measurements to be identified and corrected. This presentation will focus on key analytical capabilities for destructive analysis in AAC and also comparative data between LANL and peer groups for Pu assay and isotopic analysis.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Parrado, G., E-mail: gparrado@sgc.gov.co; Cañón, Y.; Peña, M., E-mail: mlpena@sgc.gov.co

The Neutron Activation Analysis (NAA) laboratory at the Colombian Geological Survey has developed a technique for multi-elemental analysis of soil and plant matrices, based on Instrumental Neutron Activation Analysis (INAA) using the comparator method. In order to evaluate the analytical capabilities of the technique, the laboratory has been participating in inter-comparison tests organized by Wepal (Wageningen Evaluating Programs for Analytical Laboratories). In this work, the experimental procedure and results for the multi-elemental analysis of four soil and four plant samples during participation in the first round on 2015 of Wepal proficiency test are presented. Only elements with radioactive isotopes withmore » medium and long half-lives have been evaluated, 15 elements for soils (As, Ce, Co, Cr, Cs, Fe, K, La, Na, Rb, Sb, Sc, Th, U and Zn) and 7 elements for plants (Br, Co, Cr, Fe, K, Na and Zn). The performance assessment by Wepal based on Z-score distributions showed that most results obtained |Z-scores| ≤ 3.« less

Quality systems in veterinary diagnostics laboratories.

PubMed

de Branco, Freitas Maia L M

2007-01-01

Quality assurance of services provided by veterinary diagnostics laboratories is a fundamental element promoted by international animal health organizations to establish trust, confidence and transparency needed for the trade of animals and their products at domestic and international levels. It requires, among other things, trained personnel, consistent and rigorous methodology, choice of suitable methods as well as appropriate calibration and traceability procedures. An important part of laboratory quality management is addressed by ISO/IEC 17025, which aims to facilitate cooperation among laboratories and their associated parties by assuring the generation of credible and consistent information derived from analytical results. Currently, according to OIE recommendation, veterinary diagnostics laboratories are only subject to voluntary compliance with standard ISO/IEC 17025; however, it is proposed here that OIE reference laboratories and collaboration centres strongly consider its adoption.

Role and Evaluation of Interlaboratory Comparison Results in Laboratory Accreditation

NASA Astrophysics Data System (ADS)

Bode, P.

2008-08-01

Participation in interlaboratory comparisons provides laboratories an opportunity for independent assessment of their analytical performance, both in absolute way and in comparison with those by other techniques. However, such comparisons are hindered by differences in the way laboratories participate, e.g. at best measurement capability or under routine conditions. Neutron activation analysis laboratories, determining total mass fractions, often see themselves classified as `outliers' since the majority of other participants employ techniques with incomplete digestion methods. These considerations are discussed in relation to the way results from interlaboratory comparisons are evaluated by accreditation bodies following the requirements of Clause 5.9.1 of the ISO/IEC 17025:2005. The discussion and conclusions come largely forth from experiences in the author's own laboratory.

Analytical and pre-analytical performance characteristics of a novel cartridge-type blood gas analyzer for point-of-care and laboratory testing.

PubMed

Oyaert, Matthijs; Van Maerken, Tom; Bridts, Silke; Van Loon, Silvi; Laverge, Heleen; Stove, Veronique

2018-03-01

Point-of-care blood gas test results may benefit therapeutic decision making by their immediate impact on patient care. We evaluated the (pre-)analytical performance of a novel cartridge-type blood gas analyzer, the GEM Premier 5000 (Werfen), for the determination of pH, partial carbon dioxide pressure (pCO 2 ), partial oxygen pressure (pO 2 ), sodium (Na + ), potassium (K + ), chloride (Cl - ), ionized calcium ( i Ca 2+ ), glucose, lactate, and total hemoglobin (tHb). Total imprecision was estimated according to the CLSI EP5-A2 protocol. The estimated total error was calculated based on the mean of the range claimed by the manufacturer. Based on the CLSI EP9-A2 evaluation protocol, a method comparison with the Siemens RapidPoint 500 and Abbott i-STAT CG8+ was performed. Obtained data were compared against preset quality specifications. Interference of potential pre-analytical confounders on co-oximetry and electrolyte concentrations were studied. The analytical performance was acceptable for all parameters tested. Method comparison demonstrated good agreement to the RapidPoint 500 and i-STAT CG8+, except for some parameters (RapidPoint 500: pCO 2 , K + , lactate and tHb; i-STAT CG8+: pO 2 , Na + , i Ca 2+ and tHb) for which significant differences between analyzers were recorded. No interference of lipemia or methylene blue on CO-oximetry results was found. On the contrary, significant interference for benzalkonium and hemolysis on electrolyte measurements were found, for which the user is notified by an interferent specific flag. Identification of sample errors from pre-analytical sources, such as interferences and automatic corrective actions, along with the analytical performance, ease of use and low maintenance time of the instrument, makes the evaluated instrument a suitable blood gas analyzer for both POCT and laboratory use. Copyright © 2018 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Characterization and measurement of natural gas trace constituents. Volume 1. Arsenic. Final report, June 1989-October 1993

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chao, S.S.; Attari, A.

1995-01-01

The discovery of arsenic compounds, as alkylarsines, in natural gas prompted this research program to develop reliable measurement techniques needed to assess the efficiency of removal processes for these environmentally sensitive substances. These techniques include sampling, speciation, quantitation and on-line instrumental methods for monitoring the total arsenic concentration. The current program has yielded many products, including calibration standards, arsenic-specific sorbents, sensitive analytical methods and instrumentation. Four laboratory analytical methods have been developed and successfully employed for arsenic determination in natural gas. These methods use GC-AED and GC-MS instruments to speciate alkylarsines, and peroxydisulfate extraction with FIAS, special carbon sorbent withmore » XRF and an IGT developed sorbent with GFAA for total arsenic measurement.« less

ASVCP quality assurance guidelines: control of general analytical factors in veterinary laboratories.

PubMed

Flatland, Bente; Freeman, Kathy P; Friedrichs, Kristen R; Vap, Linda M; Getzy, Karen M; Evans, Ellen W; Harr, Kendal E

2010-09-01

Owing to lack of governmental regulation of veterinary laboratory performance, veterinarians ideally should demonstrate a commitment to self-monitoring and regulation of laboratory performance from within the profession. In response to member concerns about quality management in veterinary laboratories, the American Society for Veterinary Clinical Pathology (ASVCP) formed a Quality Assurance and Laboratory Standards (QAS) committee in 1996. This committee recently published updated and peer-reviewed Quality Assurance Guidelines on the ASVCP website. The Quality Assurance Guidelines are intended for use by veterinary diagnostic laboratories and veterinary research laboratories that are not covered by the US Food and Drug Administration Good Laboratory Practice standards (Code of Federal Regulations Title 21, Chapter 58). The guidelines have been divided into 3 reports on 1) general analytic factors for veterinary laboratory performance and comparisons, 2) hematology and hemostasis, and 3) clinical chemistry, endocrine assessment, and urinalysis. This report documents recommendations for control of general analytical factors within veterinary clinical laboratories and is based on section 2.1 (Analytical Factors Important In Veterinary Clinical Pathology, General) of the newly revised ASVCP QAS Guidelines. These guidelines are not intended to be all-inclusive; rather, they provide minimum guidelines for quality assurance and quality control for veterinary laboratory testing. It is hoped that these guidelines will provide a basis for laboratories to assess their current practices, determine areas for improvement, and guide continuing professional development and education efforts. ©2010 American Society for Veterinary Clinical Pathology.

Determination of Ivermectin in Medicated Feeds by Liquid Chromatography with Fluorescence Detection

PubMed Central

2013-01-01

A labour- and time-effective analytical procedure for determination of ivermectin in medicated feed at recommended level of 2.0 mg kg−1 has been developed and validated. The analyte was extracted from grinded feed samples with acetonitrile and derivatisated with N-methylimidazole and trifluoracetic anhydride. The fluorescent derivatives were analysed by liquid chromatography method using C8 column. The isocratic conditions using acetonitrile, methanol, water, and tetrahydrofuran were applied. Fluorescence detection was performed at 365 nm (excitation) and 475 nm (emission) wavelengths. The total analysis time was 10 min. The validation results of the method (within-laboratory reproducibility 4.0% CV, mean recovery 100.1%) confirm the appropriate precision and accuracy of the developed method. PMID:24453835

[The development and validation of the methods for the quantitative determination of sibutramine derivatives in dietary supplements].

PubMed

Stern, K I; Malkova, T L

The objective of the present study was the development and validation of sibutramine demethylated derivatives, desmethyl sibutramine and didesmethyl sibutramine. Gas-liquid chromatography with the flame ionization detector was used for the quantitative determination of the above substances in dietary supplements. The conditions for the chromatographic determination of the analytes in the presence of the reference standard, methyl stearate, were proposed allowing to achieve the efficient separation. The method has the necessary sensitivity, specificity, linearity, accuracy, and precision (on the intra-day and inter-day basis) which suggests its good validation characteristics. The proposed method can be employed in the analytical laboratories for the quantitative determination of sibutramine derivatives in biologically active dietary supplements.

Protocol for Detection of Yersinia pestis in Environmental ...

EPA Pesticide Factsheets

Methods Report This is the first ever open-access and detailed protocol available to all government departments and agencies, and their contractors to detect Yersinia pestis, the pathogen that causes plague, from multiple environmental sample types including water. Each analytical method includes sample processing procedure for each sample type in a step-by-step manner. It includes real-time PCR, traditional microbiological culture, and the Rapid Viability PCR (RV-PCR) analytical methods. For large volume water samples it also includes an ultra-filtration-based sample concentration procedure. Because of such a non-restrictive availability of this protocol to all government departments and agencies, and their contractors, the nation will now have increased laboratory capacity to analyze large number of samples during a wide-area plague incident.

Laboratory Workhorse: The Analytical Balance.

ERIC Educational Resources Information Center

Clark, Douglas W.

1979-01-01

This report explains the importance of various analytical balances in the water or wastewater laboratory. Stressed is the proper procedure for utilizing the equipment as well as the mechanics involved in its operation. (CS)

Participation and performance in INSTAND multi-analyte molecular genetics external quality assessment schemes from 2006 to 2012.

PubMed

Maly, Friedrich E; Fried, Roman; Spannagl, Michael

2014-01-01

INSTAND e.V. has provided Molecular Genetics Multi-Analyte EQA schemes since 2006. EQA participation and performance were assessed from 2006 - 2012. From 2006 to 2012, the number of analytes in the Multi-Analyte EQA schemes rose from 17 to 53. Total number of results returned rose from 168 in January 2006 to 824 in August 2012. The overall error rate was 1.40 +/- 0.84% (mean +/- SD, N = 24 EQA dates). From 2006 to 2012, no analyte was reported 100% correctly. Individual participant performance was analysed for one common analyte, Lactase (LCT) T-13910C. From 2006 to 2012, 114 laboratories participated in this EQA. Of these, 10 laboratories (8.8%) reported at least one wrong result during the whole observation period. All laboratories reported correct results after their failure incident. In spite of the low overall error rate, EQA will continue to be important for Molecular Genetics.

Defining the challenges of the Modern Analytical Laboratory (CPSA USA 2014): the risks and reality of personalized healthcare.

PubMed

Weng, Naidong; Needham, Shane; Lee, Mike

2015-01-01

The 17th Annual Symposium on Clinical and Pharmaceutical Solutions through Analysis (CPSA) 29 September-2 October 2014, was held at the Sheraton Bucks County Hotel, Langhorne, PA, USA. The CPSA USA 2014 brought the various analytical fields defining the challenges of the modern analytical laboratory. Ongoing discussions focused on the future application of bioanalysis and other disciplines to support investigational new drugs (INDs) and new drug application (NDA) submissions, clinical diagnostics and pathology laboratory personnel that support patient sample analysis, and the clinical researchers that provide insights into new biomarkers within the context of the modern laboratory and personalized medicine.

40 CFR 141.852 - Analytical methods and laboratory certification.

Code of Federal Regulations, 2014 CFR

2014-07-01

.... All approved material is available for inspection either electronically at www.regulations.gov, in....gov/federal_register/code_of_federal_regulations/ibr_ locations.html. (1) American Public Health..., “Enzyme Substrate Test”, Colilert® and Colisure®. (2) Charm Sciences, Inc., 659 Andover Street, Lawrence...

40 CFR 141.852 - Analytical methods and laboratory certification.

Code of Federal Regulations, 2013 CFR

2013-07-01

.... All approved material is available for inspection either electronically at www.regulations.gov, in....gov/federal_register/code_of_federal_regulations/ibr_ locations.html. (1) American Public Health..., “Enzyme Substrate Test”, Colilert® and Colisure®. (2) Charm Sciences, Inc., 659 Andover Street, Lawrence...

RECOVERY OF SEMI-VOLATILE ORGANIC COMPOUNDS DURING SAMPLE PREPARATION: IMPLICATIONS FOR CHARACTERIZATION OF AIRBORNE PARTICULATE MATTER

EPA Science Inventory

Semi-volatile compounds present special analytical challenges not met by conventional methods for analysis of ambient particulate matter (PM). Accurate quantification of PM-associated organic compounds requires validation of the laboratory procedures for recovery over a wide v...

Algorithms and software for U-Pb geochronology by LA-ICPMS

NASA Astrophysics Data System (ADS)

McLean, Noah M.; Bowring, James F.; Gehrels, George

2016-07-01

The past 15 years have produced numerous innovations in geochronology, including experimental methods, instrumentation, and software that are revolutionizing the acquisition and application of geochronological data. For example, exciting advances are being driven by Laser-Ablation ICP Mass Spectrometry (LA-ICPMS), which allows for rapid determination of U-Th-Pb ages with 10s of micrometer-scale spatial resolution. This method has become the most commonly applied tool for dating zircons, constraining a host of geological problems. The LA-ICPMS community is now faced with archiving these data with associated analytical results and, more importantly, ensuring that data meet the highest standards for precision and accuracy and that interlaboratory biases are minimized. However, there is little consensus with regard to analytical strategies and data reduction protocols for LA-ICPMS geochronology. The result is systematic interlaboratory bias and both underestimation and overestimation of uncertainties on calculated dates that, in turn, decrease the value of data in repositories such as EarthChem, which archives data and analytical results from participating laboratories. We present free open-source software that implements new algorithms for evaluating and resolving many of these discrepancies. This solution is the result of a collaborative effort to extend the U-Pb_Redux software for the ID-TIMS community to the LA-ICPMS community. Now named ET_Redux, our new software automates the analytical and scientific workflows of data acquisition, statistical filtering, data analysis and interpretation, publication, community-based archiving, and the compilation and comparison of data from different laboratories to support collaborative science.

Analytical performance of 17 general chemistry analytes across countries and across manufacturers in the INPUtS project of EQA organizers in Italy, the Netherlands, Portugal, United Kingdom and Spain.

PubMed

Weykamp, Cas; Secchiero, Sandra; Plebani, Mario; Thelen, Marc; Cobbaert, Christa; Thomas, Annette; Jassam, Nuthar; Barth, Julian H; Perich, Carmen; Ricós, Carmen; Faria, Ana Paula

2017-02-01

Optimum patient care in relation to laboratory medicine is achieved when results of laboratory tests are equivalent, irrespective of the analytical platform used or the country where the laboratory is located. Standardization and harmonization minimize differences and the success of efforts to achieve this can be monitored with international category 1 external quality assessment (EQA) programs. An EQA project with commutable samples, targeted with reference measurement procedures (RMPs) was organized by EQA institutes in Italy, the Netherlands, Portugal, UK, and Spain. Results of 17 general chemistry analytes were evaluated across countries and across manufacturers according to performance specifications derived from biological variation (BV). For K, uric acid, glucose, cholesterol and high-density density (HDL) cholesterol, the minimum performance specification was met in all countries and by all manufacturers. For Na, Cl, and Ca, the minimum performance specifications were met by none of the countries and manufacturers. For enzymes, the situation was complicated, as standardization of results of enzymes toward RMPs was still not achieved in 20% of the laboratories and questionable in the remaining 80%. The overall performance of the measurement of 17 general chemistry analytes in European medical laboratories met the minimum performance specifications. In this general picture, there were no significant differences per country and no significant differences per manufacturer. There were major differences between the analytes. There were six analytes for which the minimum quality specifications were not met and manufacturers should improve their performance for these analytes. Standardization of results of enzymes requires ongoing efforts.

Analytical methods for toxic gases from thermal degradation of polymers

NASA Technical Reports Server (NTRS)

Hsu, M.-T. S.

1977-01-01

Toxic gases evolved from the thermal oxidative degradation of synthetic or natural polymers in small laboratory chambers or in large scale fire tests are measured by several different analytical methods. Gas detector tubes are used for fast on-site detection of suspect toxic gases. The infrared spectroscopic method is an excellent qualitative and quantitative analysis for some toxic gases. Permanent gases such as carbon monoxide, carbon dioxide, methane and ethylene, can be quantitatively determined by gas chromatography. Highly toxic and corrosive gases such as nitrogen oxides, hydrogen cyanide, hydrogen fluoride, hydrogen chloride and sulfur dioxide should be passed into a scrubbing solution for subsequent analysis by either specific ion electrodes or spectrophotometric methods. Low-concentration toxic organic vapors can be concentrated in a cold trap and then analyzed by gas chromatography and mass spectrometry. The limitations of different methods are discussed.

A simple method for the small scale synthesis and solid-phase extraction purification of steroid sulfates.

PubMed

Waller, Christopher C; McLeod, Malcolm D

2014-12-01

Steroid sulfates are a major class of steroid metabolite that are of growing importance in fields such as anti-doping analysis, the detection of residues in agricultural produce or medicine. Despite this, many steroid sulfate reference materials may have limited or no availability hampering the development of analytical methods. We report simple protocols for the rapid synthesis and purification of steroid sulfates that are suitable for adoption by analytical laboratories. Central to this approach is the use of solid-phase extraction (SPE) for purification, a technique routinely used for sample preparation in analytical laboratories around the world. The sulfate conjugates of sixteen steroid compounds encompassing a wide range of steroid substitution patterns and configurations are prepared, including the previously unreported sulfate conjugates of the designer steroids furazadrol (17β-hydroxyandrostan[2,3-d]isoxazole), isofurazadrol (17β-hydroxyandrostan[3,2-c]isoxazole) and trenazone (17β-hydroxyestra-4,9-dien-3-one). Structural characterization data, together with NMR and mass spectra are reported for all steroid sulfates, often for the first time. The scope of this approach for small scale synthesis is highlighted by the sulfation of 1μg of testosterone (17β-hydroxyandrost-4-en-3-one) as monitored by liquid chromatography-mass spectrometry (LCMS). Copyright © 2014 Elsevier Inc. All rights reserved.

Standardization of glycohemoglobin results and reference values in whole blood studied in 103 laboratories using 20 methods.

PubMed

Weykamp, C W; Penders, T J; Miedema, K; Muskiet, F A; van der Slik, W

1995-01-01

We investigated the effect of calibration with lyophilized calibrators on whole-blood glycohemoglobin (glyHb) results. One hundred three laboratories, using 20 different methods, determined glyHb in two lyophilized calibrators and two whole-blood samples. For whole-blood samples with low (5%) and high (9%) glyHb percentages, respectively, calibration decreased overall interlaboratory variation (CV) from 16% to 9% and from 11% to 6% and decreased intermethod variation from 14% to 6% and from 12% to 5%. Forty-seven laboratories, using 14 different methods, determined mean glyHb percentages in self-selected groups of 10 nondiabetic volunteers each. With calibration their overall mean (2SD) was 5.0% (0.5%), very close to the 5.0% (0.3%) derived from the reference method used in the Diabetes Control and Complications Trial. In both experiments the Abbott IMx and Vision showed deviating results. We conclude that, irrespective of the analytical method used, calibration enables standardization of glyHb results, reference values, and interpretation criteria.

Comparison of radium-228 determination in water among Australian laboratories.

PubMed

Zawadzki, Atun; Cook, Megan; Cutmore, Brodie; Evans, Fiona; Fierro, Daniela; Gedz, Alicea; Harrison, Jennifer J; Loosz, Tom; Medley, Peter; Mokhber-Shahin, Lida; Mullins, Sarah; Sdraulig, Sandra

2017-11-01

The National Health and Medical Research Council and Natural Resource Management Ministerial Council of Australia developed the current Australian Drinking Water Guidelines which recommend an annual radiation dose value of 1 mSv year -1 . One of the potential major contributors to the radiation dose from drinking water is radium-228, a naturally occurring radionuclide arising from the thorium decay series. Various methods of analysing for radium-228 in water have been established and adapted by analytical radiochemistry laboratories. Seven laboratories in Australia participated in analysing radium-228 spiked water samples with activity concentrations ranging from 6 mBq L -1 to 20 Bq L -1 . The aim of the exercise was to compare and evaluate radium-228 results reported by the participating laboratories, the methods used and the detection limits. This paper presents the outcome of the exercise. Crown Copyright © 2017. Published by Elsevier Ltd. All rights reserved.

Utilizing global data to estimate analytical performance on the Sigma scale: A global comparative analysis of methods, instruments, and manufacturers through external quality assurance and proficiency testing programs.

PubMed

Westgard, Sten A

2016-06-01

To assess the analytical performance of instruments and methods through external quality assessment and proficiency testing data on the Sigma scale. A representative report from five different EQA/PT programs around the world (2 US, 1 Canadian, 1 UK, and 1 Australasian) was accessed. The instrument group standard deviations were used as surrogate estimates of instrument imprecision. Performance specifications from the US CLIA proficiency testing criteria were used to establish a common quality goal. Then Sigma-metrics were calculated to grade the analytical performance. Different methods have different Sigma-metrics for each analyte reviewed. Summary Sigma-metrics estimate the percentage of the chemistry analytes that are expected to perform above Five Sigma, which is where optimized QC design can be implemented. The range of performance varies from 37% to 88%, exhibiting significant differentiation between instruments and manufacturers. Median Sigmas for the different manufacturers in three analytes (albumin, glucose, sodium) showed significant differentiation. Chemistry tests are not commodities. Quality varies significantly from manufacturer to manufacturer, instrument to instrument, and method to method. The Sigma-assessments from multiple EQA/PT programs provide more insight into the performance of methods and instruments than any single program by itself. It is possible to produce a ranking of performance by manufacturer, instrument and individual method. Laboratories seeking optimal instrumentation would do well to consult this data as part of their decision-making process. To confirm that these assessments are stable and reliable, a longer term study should be conducted that examines more results over a longer time period. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Managing the Pre- and Post-analytical Phases of the Total Testing Process

PubMed Central

2012-01-01

For many years, the clinical laboratory's focus on analytical quality has resulted in an error rate of 4-5 sigma, which surpasses most other areas in healthcare. However, greater appreciation of the prevalence of errors in the pre- and post-analytical phases and their potential for patient harm has led to increasing requirements for laboratories to take greater responsibility for activities outside their immediate control. Accreditation bodies such as the Joint Commission International (JCI) and the College of American Pathologists (CAP) now require clear and effective procedures for patient/sample identification and communication of critical results. There are a variety of free on-line resources available to aid in managing the extra-analytical phase and the recent publication of quality indicators and proposed performance levels by the International Federation of Clinical Chemistry and Laboratory Medicine (IFCC) working group on laboratory errors and patient safety provides particularly useful benchmarking data. Managing the extra-laboratory phase of the total testing cycle is the next challenge for laboratory medicine. By building on its existing quality management expertise, quantitative scientific background and familiarity with information technology, the clinical laboratory is well suited to play a greater role in reducing errors and improving patient safety outside the confines of the laboratory. PMID:22259773

Multicentric Comparative Analytical Performance Study for Molecular Detection of Low Amounts of Toxoplasma gondii from Simulated Specimens▿ †

PubMed Central

Sterkers, Yvon; Varlet-Marie, Emmanuelle; Cassaing, Sophie; Brenier-Pinchart, Marie-Pierre; Brun, Sophie; Dalle, Frédéric; Delhaes, Laurence; Filisetti, Denis; Pelloux, Hervé; Yera, Hélène; Bastien, Patrick

2010-01-01

Although screening for maternal toxoplasmic seroconversion during pregnancy is based on immunodiagnostic assays, the diagnosis of clinically relevant toxoplasmosis greatly relies upon molecular methods. A problem is that this molecular diagnosis is subject to variation of performances, mainly due to a large diversity of PCR methods and primers and the lack of standardization. The present multicentric prospective study, involving eight laboratories proficient in the molecular prenatal diagnosis of toxoplasmosis, was a first step toward the harmonization of this diagnosis among university hospitals in France. Its aim was to compare the analytical performances of different PCR protocols used for Toxoplasma detection. Each center extracted the same concentrated Toxoplasma gondii suspension and tested serial dilutions of the DNA using its own assays. Differences in analytical sensitivities were observed between assays, particularly at low parasite concentrations (≤2 T. gondii genomes per reaction tube), with “performance scores” differing by a 20-fold factor among laboratories. Our data stress the fact that differences do exist in the performances of molecular assays in spite of expertise in the matter; we propose that laboratories work toward a detection threshold defined for a best sensitivity of this diagnosis. Moreover, on the one hand, intralaboratory comparisons confirmed previous studies showing that rep529 is a more adequate DNA target for this diagnosis than the widely used B1 gene. But, on the other hand, interlaboratory comparisons showed differences that appear independent of the target, primers, or technology and that hence rely essentially on proficiency and care in the optimization of PCR conditions. PMID:20610670

Laboratory safety and the WHO World Alliance for Patient Safety.

PubMed

McCay, Layla; Lemer, Claire; Wu, Albert W

2009-06-01

Laboratory medicine has been a pioneer in the field of patient safety; indeed, the College of American Pathology first called attention to the issue in 1946. Delivering reliable laboratory results has long been considered a priority, as the data produced in laboratory medicine have the potential to critically influence individual patients' diagnosis and management. Until recently, most attention on laboratory safety has focused on the analytic stage of laboratory medicine. Addressing this stage has led to significant and impressive improvements in the areas over which laboratories have direct control. However, recent data demonstrate that pre- and post-analytical phases are at least as vulnerable to errors; to further improve patient safety in laboratory medicine, attention must now be focused on the pre- and post-analytic phases, and the concept of patient safety as a multi-disciplinary, multi-stage and multi-system concept better understood. The World Alliance for Patient Safety (WAPS) supports improvement of patient safety globally and provides a potential framework for considering the total testing process.

CSF biomarker variability in the Alzheimer’s Association quality control program

PubMed Central

Mattsson, Niklas; Andreasson, Ulf; Persson, Staffan; Carrillo, Maria C.; Collins, Steven; Chalbot, Sonia; Cutler, Neal; Dufour-Rainfray, Diane; Fagan, Anne M.; Heegaard, Niels H. H.; Hsiung, Ging-Yuek Robin; Hyman, Bradley; Iqbal, Khalid; Lachno, D. Richard; Lleó, Alberto; Lewczuk, Piotr; Molinuevo, José L.; Parchi, Piero; Regeniter, Axel; Rissman, Robert; Rosenmann, Hanna; Sancesario, Giuseppe; Schröder, Johannes; Shaw, Leslie M.; Teunissen, Charlotte E.; Trojanowski, John Q.; Vanderstichele, Hugo; Vandijck, Manu; Verbeek, Marcel M.; Zetterberg, Henrik; Blennow, Kaj; Käser, Stephan A.

2013-01-01

Background The cerebrospinal fluid (CSF) biomarkers amyloid beta 1–42, total tau, and phosphorylated tau are used increasingly for Alzheimer’s disease (AD) research and patient management. However, there are large variations in biomarker measurements among and within laboratories. Methods Data from the first nine rounds of the Alzheimer’s Association quality control program was used to define the extent and sources of analytical variability. In each round, three CSF samples prepared at the Clinical Neurochemistry Laboratory (Mölndal, Sweden) were analyzed by single-analyte enzyme-linked immunosorbent assay (ELISA), a multiplexing xMAP assay, or an immunoassay with electrochemoluminescence detection. Results A total of 84 laboratories participated. Coefficients of variation (CVs) between laboratories were around 20% to 30%; within-run CVs, less than 5% to 10%; and longitudinal within-laboratory CVs, 5% to 19%. Interestingly, longitudinal within-laboratory CV differed between biomarkers at individual laboratories, suggesting that a component of it was assay dependent. Variability between kit lots and between laboratories both had a major influence on amyloid beta 1–42 measurements, but for total tau and phosphorylated tau, between-kit lot effects were much less than between-laboratory effects. Despite the measurement variability, the between-laboratory consistency in classification of samples (using prehoc-derived cutoffs for AD) was high (>90% in 15 of 18 samples for ELISA and in 12 of 18 samples for xMAP). Conclusions The overall variability remains too high to allow assignment of universal biomarker cutoff values for a specific intended use. Each laboratory must ensure longitudinal stability in its measurements and use internally qualified cutoff levels. Further standardization of laboratory procedures and improvement of kit performance will likely increase the usefulness of CSF AD biomarkers for researchers and clinicians. PMID:23622690

Construction of measurement uncertainty profiles for quantitative analysis of genetically modified organisms based on interlaboratory validation data.

PubMed

Macarthur, Roy; Feinberg, Max; Bertheau, Yves

2010-01-01

A method is presented for estimating the size of uncertainty associated with the measurement of products derived from genetically modified organisms (GMOs). The method is based on the uncertainty profile, which is an extension, for the estimation of uncertainty, of a recent graphical statistical tool called an accuracy profile that was developed for the validation of quantitative analytical methods. The application of uncertainty profiles as an aid to decision making and assessment of fitness for purpose is also presented. Results of the measurement of the quantity of GMOs in flour by PCR-based methods collected through a number of interlaboratory studies followed the log-normal distribution. Uncertainty profiles built using the results generally give an expected range for measurement results of 50-200% of reference concentrations for materials that contain at least 1% GMO. This range is consistent with European Network of GM Laboratories and the European Union (EU) Community Reference Laboratory validation criteria and can be used as a fitness for purpose criterion for measurement methods. The effect on the enforcement of EU labeling regulations is that, in general, an individual analytical result needs to be < 0.45% to demonstrate compliance, and > 1.8% to demonstrate noncompliance with a labeling threshold of 0.9%.

Simultaneous determination of thirteen different steroid hormones using micro UHPLC-MS/MS with on-line SPE system.

PubMed

Márta, Zoltán; Bobály, Balázs; Fekete, Jenő; Magda, Balázs; Imre, Tímea; Mészáros, Katalin Viola; Bálint, Mária; Szabó, Pál Tamás

2018-02-20

Ultratrace analysis of sample components requires excellent analytical performance in terms of limits of quantitation (LOQ). Micro UHPLC coupled to sensitive tandem mass spectrometry provides state of the art solution for such analytical problems. Using on-line SPE with column switching on a micro UHPLC-MS/MS system allowed to decrease LOQ without any complex sample preparation protocol. The presented method is capable of reaching satisfactory low LOQ values for analysis of thirteen different steroid molecules from human plasma without the most commonly used off-line SPE or compound derivatization. Steroids were determined by using two simple sample preparation methods, based on lower and higher plasma steroid concentrations. In the first method, higher analyte concentrations were directly determined after protein precipitation with methanol. The organic phase obtained from the precipitation was diluted with water and directly injected into the LC-MS system. In the second method, low steroid levels were determined by concentrating the organic phase after steroid extraction. In this case, analytes were extracted with ethyl acetate and reconstituted in 90/10 water/acetonitrile following evaporation to dryness. This step provided much lower LOQs, outperforming previously published values. The method has been validated and subsequently applied to clinical laboratory measurement. Copyright © 2017 Elsevier B.V. All rights reserved.

Round-robin pretest analyses of a 1:6-scale reinforced concrete containment model subject to static internal pressurization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clauss, D.B.

Analyses of a 1:6-scale reinforced concrete containment model that will be tested to failure at Sandia National Laboratories in the spring of 1987 were conducted by the following organizations in the United States and Europe: Sandia National Laboratories (USA), Argonne National Laboratory (USA), Electric Power Research Institute (USA), Commissariat a L'Energie Atomique (France), HM Nuclear Installations Inspectorate (UK), Comitato Nazionale per la ricerca e per lo sviluppo dell'Energia Nucleare e delle Energie Alternative (Italy), UK Atomic Energy Authority, Safety and Reliability Directorate (UK), Gesellschaft fuer Reaktorsicherheit (FRG), Brookhaven National Laboratory (USA), and Central Electricity Generating Board (UK). Each organization wasmore » supplied with a standard information package, which included construction drawings and actual material properties for most of the materials used in the model. Each organization worked independently using their own analytical methods. This report includes descriptions of the various analytical approaches and pretest predictions submitted by each organization. Significant milestones that occur with increasing pressure, such as damage to the concrete (cracking and crushing) and yielding of the steel components, and the failure pressure (capacity) and failure mechanism are described. Analytical predictions for pressure histories of strain in the liner and rebar and displacements are compared at locations where experimental results will be available after the test. Thus, these predictions can be compared to one another and to experimental results after the test.« less

Laboratory Medicine Best Practice Guideline: Vitamins A, E and the Carotenoids in Blood

PubMed Central

Greaves, Ronda F; Woollard, Gerald A; Hoad, Kirsten E; Walmsley, Trevor A; Johnson, Lambro A; Briscoe, Scott; Koetsier, Sabrina; Harrower, Tamantha; Gill, Janice P

2014-01-01

Despite apparent method similarities between laboratories there appear to be confounding factors inhibiting uniform reporting and standardisation of vitamin assays. The Australasian Association of Clinical Biochemists (AACB) Vitamins Working Party, in conjunction with The Royal College of Pathologists of Australasia Quality Assurance Programs, has formulated a guideline to improve performance, reproducibility and accuracy of fat-soluble vitamin results. The aim of the guideline is to identify critical pre-analytical, analytical and post-analytical components of the analysis of vitamins A, E and carotenoids in blood to promote best practice and harmonisation. This best practice guideline has been developed with reference to the Centers for Disease Control and Prevention (CDC) “Laboratory Medicine Best Practices: Developing an Evidence-Based Review and Evaluation Process”. The CDC document cites an evaluation framework for generating best practice recommendations that are specific to laboratory medicine. These 50 recommendations proposed herein, were generated from a comprehensive literature search and the extensive combined experience of the AACB Vitamins Working Party members. They were formulated based on comparison between an impact assessment rating and strength of evidence and were classified as either: (1) strongly recommend, (2) recommend, (3) no recommendation for or against, or (4) recommend against. These best practice recommendations represent the consensus views, in association with peer reviewed evidence of the AACB Vitamins Working Party, towards best practice for the collection, analysis and interpretation of vitamins A, E and carotenoids in blood. PMID:25210208

Validation conform ISO-15189 of assays in the field of autoimmunity: Joint efforts in The Netherlands.

PubMed

Mulder, Leontine; van der Molen, Renate; Koelman, Carin; van Leeuwen, Ester; Roos, Anja; Damoiseaux, Jan

2018-05-01

ISO 15189:2012 requires validation of methods used in the medical laboratory, and lists a series of performance parameters for consideration to include. Although these performance parameters are feasible for clinical chemistry analytes, application in the validation of autoimmunity tests is a challenge. Lack of gold standards or reference methods in combination with the scarcity of well-defined diagnostic samples of patients with rare diseases make validation of new assays difficult. The present manuscript describes the initiative of Dutch medical immunology laboratory specialists to combine efforts and perform multi-center validation studies of new assays in the field of autoimmunity. Validation data and reports are made available to interested Dutch laboratory specialists. Copyright © 2018 Elsevier B.V. All rights reserved.

Recommendation for the review of biological reference intervals in medical laboratories.

PubMed

Henny, Joseph; Vassault, Anne; Boursier, Guilaine; Vukasovic, Ines; Mesko Brguljan, Pika; Lohmander, Maria; Ghita, Irina; Andreu, Francisco A Bernabeu; Kroupis, Christos; Sprongl, Ludek; Thelen, Marc H M; Vanstapel, Florent J L A; Vodnik, Tatjana; Huisman, Willem; Vaubourdolle, Michel

2016-12-01

This document is based on the original recommendation of the Expert Panel on the Theory of Reference Values of the International Federation of Clinical Chemistry and Laboratory Medicine (IFCC), updated guidelines were recently published under the auspices of the IFCC and the Clinical and Laboratory Standards Institute (CLSI). This document summarizes proposals for recommendations on: (i) The terminology, which is often confusing, noticeably concerning the terms of reference limits and decision limits. (ii) The method for the determination of reference limits according to the original procedure and the conditions, which should be used. (iii) A simple procedure allowing the medical laboratories to fulfill the requirements of the regulation and standards. The updated document proposes to verify that published reference limits are applicable to the laboratory involved. Finally, the strengths and limits of the revised recommendations (especially the selection of the reference population, the maintenance of the analytical quality, the choice of the statistical method used…) will be briefly discussed.

Pre-Analytical Components of Risk in Four Branches of Clinical Laboratory in Romania--Prospective Study.

PubMed

David, Remona E; Dobreanu, Minodora

2016-01-01

Development of quality measurement principles is a strategic point for each clinical laboratory. Preexamination process is the most critical and the most difficult to be managed. The aim of this study is to identify, quantify, and monitor the nonconformities of the pre-analytical process using quality indicators that can affect the patient's health safety in four different locations of a Romanian private clinical laboratory. The study group consisted of all the analysis requests received by the departments of biochemistry, hematology, and coagulation from January through March 2015. In order to collect the pre-analytical nonconformities, we created a "Risk Budget", using the entries from the "Evidence notebook--non-conform samples" from the above mentioned departments. The laboratory established the quality indicators by means of the risk management technique in order to identify and control the sources of errors, FMEA (Failure Modes and Effects Analyses), which had been implemented and monitored for its purposes and special needs. For the assessment of the control level over the processes, the results were transformed on the Six Sigma scale, using the Westgard calculation method and being obtained in this way the frequency with which an error may occur. (https://www.westgard. com/six-sigma-calculators.htm). The obtained results prove that the quantification and monitoring of the indicators can be a control instrument for the pre-analytic activities. The calculation of the Six Sigma value adds extra information to the study because it allows the detection of the processes which need improvement (Sigma value higher than 4 represents a well controlled process). The highest rates were observed for the hemolyzed and the lipemic samples, in the department of biochemistry and hemolyzed, insufficient sample volume, or clotted samples for the department of hematology and coagulation. Significant statistical differences between laboratories participating in the study have been recorded for these indicators. The elaborated study between the four branches of a Romanian private clinical laboratory was a challenge, and it helped in choosing strategic decisions regarding the improvement of the patient's health safety in the institution, corresponding to the accreditation requirements in accordance with ISO 15189:2013.

Art, Meet Chemistry; Chemistry, Meet Art: Case Studies, Current Literature, and Instrumental Methods Combined to Create a Hands-On Experience for Nonmajors and Instrumental Analysis Students

ERIC Educational Resources Information Center

Nivens, Delana A.; Padgett, Clifford W.; Chase, Jeffery M.; Verges, Katie J.; Jamieson, Deborah S.

2010-01-01

Case studies and current literature are combined with spectroscopic analysis to provide a unique chemistry experience for art history students and to provide a unique inquiry-based laboratory experiment for analytical chemistry students. The XRF analysis method was used to demonstrate to nonscience majors (art history students) a powerful…

Expansion of the scope of AOAC first action method 2012.25 - single-laboratory validation of triphenylmethane dye and leuco metabolite analysis in shrimp, tilapia, catfish, and salmon by LC-MS/MS

USDA-ARS?s Scientific Manuscript database

Prior to conducting a collaborative study of AOAC First Action 2012.25 LC-MS/MS analytical method for the determination of residues of three triphenylmethane dyes (malachite green, crystal violet, and brilliant green) and their metabolites (leucomalachite green and leucocrystal violet) in seafood, a...

Laboratory Investigations Of Mechanisms For 1,4-Dioxane Destruction By Ozone In Water (Presentation)

EPA Science Inventory

Advances in analytical detection methods have made it possible to quantify 1,4-dioxane contamination in groundwater, even a well-characterized sites where it had not been previously detected. Although 1,4-dioxane is difficult to treat because of its chemical and physical propert...

Evaluation of PLS, LS-SVM, and LWR for quantitative spectroscopic analysis of soils

USDA-ARS?s Scientific Manuscript database

Soil testing requires the analysis of large numbers of samples in laboratory that are often time consuming and expensive. Mid-infrared spectroscopy (mid-IR) and near-infrared spectroscopy (NIRS) are fast, non-destructive, and inexpensive analytical methods that have been used for soil analysis, in l...

Laboratory Investigation Of Mechanisms For 1,4-Dioxane Destruction By Ozone In Water

EPA Science Inventory

Advances in analytical detection methods have made it possible to quantify 1,4-dioxane contamination in groundwater, even at well-characterized sites where it had not been previously detected. Although 1,4-dioxane is difficult to treat because of its chemical and physical proper...

Evaluation of a reduced centrifugation time and higher centrifugal force on various general chemistry and immunochemistry analytes in plasma and serum.

PubMed

Møller, Mette F; Søndergaard, Tove R; Kristensen, Helle T; Münster, Anna-Marie B

2017-09-01

Background Centrifugation of blood samples is an essential preanalytical step in the clinical biochemistry laboratory. Centrifugation settings are often altered to optimize sample flow and turnaround time. Few studies have addressed the effect of altering centrifugation settings on analytical quality, and almost all studies have been done using collection tubes with gel separator. Methods In this study, we compared a centrifugation time of 5 min at 3000 ×  g to a standard protocol of 10 min at 2200 ×  g. Nine selected general chemistry and immunochemistry analytes and interference indices were studied in lithium heparin plasma tubes and serum tubes without gel separator. Results were evaluated using mean bias, difference plots and coefficient of variation, compared with maximum allowable bias and coefficient of variation used in laboratory routine quality control. Results For all analytes except lactate dehydrogenase, the results were within the predefined acceptance criteria, indicating that the analytical quality was not compromised. Lactate dehydrogenase showed higher values after centrifugation for 5 min at 3000 ×  g, mean bias was 6.3 ± 2.2% and the coefficient of variation was 5%. Conclusions We found that a centrifugation protocol of 5 min at 3000 ×  g can be used for the general chemistry and immunochemistry analytes studied, with the possible exception of lactate dehydrogenase, which requires further assessment.

Fourier Transform Infrared Absorption Spectroscopy for Quantitative Analysis of Gas Mixtures at Low Temperatures for Homeland Security Applications.

PubMed

Meier, D C; Benkstein, K D; Hurst, W S; Chu, P M

2017-05-01

Performance standard specifications for point chemical vapor detectors are established in ASTM E 2885-13 and ASTM E 2933-13. The performance evaluation of the detectors requires the accurate delivery of known concentrations of the chemical target to the system under test. Referee methods enable the analyte test concentration and associated uncertainties in the analyte test concentration to be validated by independent analysis, which is especially important for reactive analytes. This work extends the capability of a previously demonstrated method for using Fourier transform infrared (FT-IR) absorption spectroscopy for quantitatively evaluating the composition of vapor streams containing hazardous materials at Acute Exposure Guideline Levels (AEGL) to include test conditions colder than laboratory ambient temperatures. The described method covers the use of primary reference spectra to establish analyte concentrations, the generation of secondary reference spectra suitable for measuring analyte concentrations under specified testing environments, and the use of additional reference spectra and spectral profile strategies to mitigate the uncertainties due to impurities and water condensation within the low-temperature (7 °C, -5 °C) test cell. Important benefits of this approach include verification of the test analyte concentration with characterized uncertainties by in situ measurements co-located with the detector under test, near-real-time feedback, and broad applicability to toxic industrial chemicals.

Fourier Transform Infrared Absorption Spectroscopy for Quantitative Analysis of Gas Mixtures at Low Temperatures for Homeland Security Applications

PubMed Central

Meier, D.C.; Benkstein, K.D.; Hurst, W.S.; Chu, P.M.

2016-01-01

Performance standard specifications for point chemical vapor detectors are established in ASTM E 2885-13 and ASTM E 2933-13. The performance evaluation of the detectors requires the accurate delivery of known concentrations of the chemical target to the system under test. Referee methods enable the analyte test concentration and associated uncertainties in the analyte test concentration to be validated by independent analysis, which is especially important for reactive analytes. This work extends the capability of a previously demonstrated method for using Fourier transform infrared (FT-IR) absorption spectroscopy for quantitatively evaluating the composition of vapor streams containing hazardous materials at Acute Exposure Guideline Levels (AEGL) to include test conditions colder than laboratory ambient temperatures. The described method covers the use of primary reference spectra to establish analyte concentrations, the generation of secondary reference spectra suitable for measuring analyte concentrations under specified testing environments, and the use of additional reference spectra and spectral profile strategies to mitigate the uncertainties due to impurities and water condensation within the low-temperature (7 °C, −5 °C) test cell. Important benefits of this approach include verification of the test analyte concentration with characterized uncertainties by in situ measurements co-located with the detector under test, near-real-time feedback, and broad applicability to toxic industrial chemicals. PMID:28090126

Hemolysis indexes for biochemical tests and immunoassays on Roche analyzers: determination of allowable interference limits according to different calculation methods.

PubMed

Monneret, Denis; Mestari, Fouzi; Atlan, Gregory; Corlouer, Camille; Ramani, Zo; Jaffre, Jeremy; Dever, Sylvie; Fressart, Veronique; Alkouri, Rana; Lamari, Foudil; Devilliers, Catherine; Imbert-Bismut, Françoise; Bonnefont-Rousselot, Dominique

2015-04-01

To determine the hemolysis interference on biochemical tests and immunoassays performed on Roche Diagnostics analyzers, according to different maximum allowable limits. Heparinized plasma and serum pools, free of interferences, were overloaded by increasing amounts of a hemoglobin-titrated hemolysate. This interference was evaluated for 45 analytes using Modular(®) and Cobas(®) analyzers. For each parameter, the hemolysis index (HI) corresponding to the traditional ± 10% change of concentrations from baseline (± 10%Δ) was determined, as well as those corresponding to the analytical change limit (ACL), and to the reference change value (RCV). Then, the relative frequencies distribution (% RFD) of hemolyzed tests performed in a hospital laboratory over a 25-day period were established for each HI as allowable limit. Considering the ± 10%Δ, the analyte concentrations enhanced by hemolysis were: Lactate dehydrogenase (LDH), aspartate aminotransferase (AST), folate, potassium, creatine kinase, phosphorus, iron, alanine aminotransferase, lipase, magnesium and triglycerides, decreasingly. The analyte concentrations decreased by hemolysis were: Haptoglobin, high-sensitive troponin T and alkaline phosphatase. Over the 25-day period, the % RFD of tests impacted more than 10%Δ by hemolysis were < 7% for LDH; < 5% for AST, folates and iron; and < 1% for the other analytes. Considering the ACL, HI were lower, giving % RFD substantially increased for many analytes, whereas only four analytes remain sensitive to hemolysis when considering RCV. This study proposes new HI based on different allowable limits, and can therefore serve as a starting point for future harmonization of hemolysis interference evaluation needed in routine laboratory practice.

Pilot proficiency testing study for second tier congenital adrenal hyperplasia newborn screening.

PubMed

De Jesús, Víctor R; Simms, David A; Schiffer, Jarad; Kennedy, Meredith; Mei, Joanne V; Hannon, W Harry

2010-11-11

Congenital adrenal hyperplasia (CAH) is caused by inherited defects in steroid biosynthesis. The Newborn Screening Quality Assurance Program (NSQAP) initiated a pilot, dried-blood spot (DBS)-based proficiency testing program designed to investigate materials and laboratory performance for second tier CAH screening by tandem mass spectrometry (MS/MS). The ratio of 17-α-hydroxyprogesterone (17-OHP), androstenedione (4-AD) and cortisol is used as an indicator of CAH in laboratory protocols for second tier analysis of DBS specimens. DBS prepared by NSQAP contained a range of steroid concentrations resulting in different clinical ratios. Laboratories received blind-coded DBS specimens and reported results to NSQAP for evaluation. Quantitative values reported by participants for 17-OHP, 4-AD, and cortisol, reflected small differences in their analytical methods. Average quantitative values for 17-OHP increased from 81% to 107% recovery over the 3.5-year period; cortisol recoveries increased from 61.9% to 89.5%; and 4-AD recoveries decreased from 184% to 68%. Laboratory participation in the CAH second tier proficiency testing program has resulted in improved analyte recoveries and enhanced sample preparation methodologies. NSQAP services for the second tier CAH analysis in DBS demonstrate the need for surveillance to ensure harmonization and continuous improvements, and to achieve sustained high-performance of newborn screening laboratories worldwide. Published by Elsevier B.V.

A Comprehensive Microfluidics Device Construction and Characterization Module for the Advanced Undergraduate Analytical Chemistry Laboratory

ERIC Educational Resources Information Center

Piunno, Paul A. E.; Zetina, Adrian; Chu, Norman; Tavares, Anthony J.; Noor, M. Omair; Petryayeva, Eleonora; Uddayasankar, Uvaraj; Veglio, Andrew

2014-01-01

An advanced analytical chemistry undergraduate laboratory module on microfluidics that spans 4 weeks (4 h per week) is presented. The laboratory module focuses on comprehensive experiential learning of microfluidic device fabrication and the core characteristics of microfluidic devices as they pertain to fluid flow and the manipulation of samples.…

Targeted proteomic assays for quantitation of proteins identified by proteogenomic analysis of ovarian cancer

DOE PAGES

Song, Ehwang; Gao, Yuqian; Wu, Chaochao; ...

2017-07-19

Here, mass spectrometry (MS) based targeted proteomic methods such as selected reaction monitoring (SRM) are becoming the method of choice for preclinical verification of candidate protein biomarkers. The Clinical Proteomic Tumor Analysis Consortium (CPTAC) of the National Cancer Institute has investigated the standardization and analytical validation of the SRM assays and demonstrated robust analytical performance on different instruments across different laboratories. An Assay Portal has also been established by CPTAC to provide the research community a resource consisting of large set of targeted MS-based assays, and a depository to share assays publicly, providing that assays meet the guidelines proposed bymore » CPTAC. Herein, we report 98 SRM assays covering 70 candidate protein biomarkers previously reported as associated with ovarian cancer that have been thoroughly characterized according to the CPTAC Assay Characterization Guidance Document. The experiments, methods and results for characterizing these SRM assays for their MS response, repeatability, selectivity, stability, and reproducible detection of endogenous analytes are described in detail.« less

The Analytical Chemistry of Drug Monitoring in Athletes

NASA Astrophysics Data System (ADS)

Bowers, Larry D.

2009-07-01

The detection and deterrence of the abuse of performance-enhancing drugs in sport are important to maintaining a level playing field among athletes and to decreasing the risk to athletes’ health. The World Anti-Doping Program consists of six documents, three of which play a role in analytical development: The World Anti-Doping Code, The List of Prohibited Substances and Methods, and The International Standard for Laboratories. Among the classes of prohibited substances, three have given rise to the most recent analytical developments in the field: anabolic agents; peptide and protein hormones; and methods to increase oxygen delivery to the tissues, including recombinant erythropoietin. Methods for anabolic agents, including designer steroids, have been enhanced through the use of liquid chromatography/tandem mass spectrometry and gas chromatography/combustion/isotope-ratio mass spectrometry. Protein and peptide identification and quantification have benefited from advances in liquid chromatography/tandem mass spectrometry. Incorporation of techniques such as flow cytometry and isoelectric focusing have supported the detection of blood doping.

Determination of fenoterol in human plasma by HPLC with fluorescence detection after derivatization.

PubMed

Meineke, Ingolf; Steinmetz, Hannelore; Kramer, Skaidrit; Gleiter, Christoph H

2002-06-20

A new method for the determination of fenoterol is described, which uses HPLC separation with fluorescence detection. Dobutamine is employed as an internal standard. The separation was achieved on a short reversed phase column with a mobile phase consisting of water, acetonitrile and methanol. Prior to chromatography both analytes are derivatized with 9-chloroformyl-carbazole. Isolation of the analytes from plasma is carried out by liquid-liquid extraction into 2-butanol after protein precipitation with acetonitrile. The method is capable of estimating fenoterol concentrations in the sub-nanogram per ml range with sufficient accuracy and precision. The determination of fenoterol can now be carried out in the average laboratory without radiolabelled material.

Sigma metric analysis for performance of creatinine with fresh frozen serum.

PubMed

Kang, Fengfeng; Zhang, Chuanbao; Wang, Wei; Wang, Zhiguo

2016-01-01

Six sigma provides an objective and quantitative methodology to describe the laboratory testing performance. In this study, we conducted a national trueness verification scheme with fresh frozen serum (FFS) for serum creatinine to evaluate its performance in China. Two different concentration levels of FFS, targeted with reference method, were sent to 98 laboratories in China. Imprecision and bias of the measurement procedure were calculated for each participant to further evaluate the sigma value. Quality goal index (QGI) analysis was used to investigate the reason of unacceptable performance for laboratories with σ < 3. Our study indicated that the sample with high concentration of creatinine had preferable sigma values. For the enzymatic method, 7.0% (5/71) to 45.1% (32/71) of the laboratories need to improve their measurement procedures (σ < 3). And for the Jaffe method, the percentages were from 11.5% (3/26) to 73.1% (19/26). QGI analysis suggested that most of the laboratories (62.5% for the enzymatic method and 68.4% for the Jaffe method) should make an effort to improve the trueness (QGI > 1.2). Only 3.1-5.3% of the laboratories should improve both of the precision and trueness. Sigma metric analysis of the serum creatinine assays is disappointing, which was mainly due to the unacceptable analytical bias according to the QGI analysis. Further effort is needed to enhance the trueness of the creatinine measurement.

The new interactive CESAR

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, P.B.; Yatabe, M.

1987-01-01

In this report the Nuclear Criticality Safety Analytical Methods Resource Center describes a new interactive version of CESAR, a critical experiments storage and retrieval program available on the Nuclear Criticality Information System (NCIS) database at Lawrence Livermore National Laboratory. The original version of CESAR did not include interactive search capabilities. The CESAR database was developed to provide a convenient, readily accessible means of storing and retrieving code input data for the SCALE Criticality Safety Analytical Sequences and the codes comprising those sequences. The database includes data for both cross section preparation and criticality safety calculations. 3 refs., 1 tab.

New interactive CESAR

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, P.B.; Yatabe, M.

1987-01-01

The Nuclear Criticality Safety Analytical Methods Resource Center announces the availability of a new interactive version of CESAR, a critical experiments storage and retrieval program available on the Nuclear Criticality Information System (NCIS) data base at Lawrence Livermore National Laboratory. The original version of CESAR did not include interactive search capabilities. The CESAR data base was developed to provide a convenient, readily accessible means of storing and retrieving code input data for the SCALE criticality safety analytical sequences and the codes comprising those sequences. The data base includes data for both cross-section preparation and criticality safety calculations.

Magnetic scavengers as carriers of analytes for flowing atmospheric pressure afterglow mass spectrometry (FAPA-MS).

PubMed

Cegłowski, Michał; Kurczewska, Joanna; Smoluch, Marek; Reszke, Edward; Silberring, Jerzy; Schroeder, Grzegorz

2015-09-07

In this paper, a procedure for the preconcentration and transport of mixtures of acids, bases, and drug components to a mass spectrometer using magnetic scavengers is presented. Flowing atmospheric pressure afterglow mass spectrometry (FAPA-MS) was used as an analytical method for identification of the compounds by thermal desorption from the scavengers. The proposed procedure is fast and cheap, and does not involve time-consuming purification steps. The developed methodology can be applied for trapping harmful substances in minute quantities, to transport them to specialized, remotely located laboratories.

Resolution of plasma sample mix-ups through comparison of patient antibody patterns to E. coli.

PubMed

Vetter, Beatrice N; Orlowski, Vanessa; Schüpbach, Jörg; Böni, Jürg; Rühe, Bettina; Huder, Jon B

2015-12-01

Accidental sample mix-ups and the need for their swift resolution is a challenge faced by every analytical laboratory. To this end, we developed a simple immunoblot-based method, making use of a patient's characteristic plasma antibody profile to Escherichia coli (E. coli) proteins. Nitrocellulose strips of size-separated proteins from E. coli whole-cell lysates were incubated with patient plasma and visualised with an enzyme-coupled secondary antibody and substrate. Plasma samples of 20 random patients as well as five longitudinal samples of three patients were analysed for antibody band patterns, to evaluate uniqueness and consistency over time, respectively. For sample mix-ups, antibody band patterns of questionable samples were compared with samples of known identity. Comparison of anti-E. coli antibody patterns of 20 random patients showed a unique antibody profile for each patient. Antibody profiles remained consistent over time, as shown for three patients over several years. Three example cases demonstrate the use of this methodology in mis-labelling or -pipetting incidences. Our simple method for resolving plasma sample mix-ups between non-related individuals can be performed with basic laboratory equipment and thus can easily be adopted by analytical laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

Improved compliance by BPM-driven workflow automation.

PubMed

Holzmüller-Laue, Silke; Göde, Bernd; Fleischer, Heidi; Thurow, Kerstin

2014-12-01

Using methods and technologies of business process management (BPM) for the laboratory automation has important benefits (i.e., the agility of high-level automation processes, rapid interdisciplinary prototyping and implementation of laboratory tasks and procedures, and efficient real-time process documentation). A principal goal of the model-driven development is the improved transparency of processes and the alignment of process diagrams and technical code. First experiences of using the business process model and notation (BPMN) show that easy-to-read graphical process models can achieve and provide standardization of laboratory workflows. The model-based development allows one to change processes quickly and an easy adaption to changing requirements. The process models are able to host work procedures and their scheduling in compliance with predefined guidelines and policies. Finally, the process-controlled documentation of complex workflow results addresses modern laboratory needs of quality assurance. BPMN 2.0 as an automation language to control every kind of activity or subprocess is directed to complete workflows in end-to-end relationships. BPMN is applicable as a system-independent and cross-disciplinary graphical language to document all methods in laboratories (i.e., screening procedures or analytical processes). That means, with the BPM standard, a communication method of sharing process knowledge of laboratories is also available. © 2014 Society for Laboratory Automation and Screening.

Short communication: Analytical method and amount of preservative added to milk samples may alter milk urea nitrogen measurements.

PubMed

Weeks, Holley L; Hristov, Alexander N

2017-02-01

Milk urea N (MUN) is used by dairy nutritionists and producers to monitor dietary protein intake and is indicative of N utilization in lactating dairy cows. Two experiments were conducted to explore discrepancies in MUN results provided by 3 milk processing laboratories using different methods. An additional experiment was conducted to evaluate the effect of 2-bromo-2-nitropropane-1, 3-diol (bronopol) on MUN analysis. In experiment 1, 10 replicates of bulk tank milk samples, collected from the Pennsylvania State University's Dairy Center over 5 consecutive days, were sent to 3 milk processing laboratories in Pennsylvania. Average MUN differed between laboratory A (14.9 ± 0.40 mg/dL; analyzed on MilkoScan 4000; Foss, Hillerød, Denmark), laboratory B (6.5 ± 0.17 mg/dL; MilkoScan FT + 6000), and laboratory C (7.4 ± 0.36 mg/dL; MilkoScan 6000). In experiment 2, milk samples were spiked with urea at 0 (7.3 to 15.0 mg/dL, depending on the laboratory analyzing the samples), 17.2, 34.2, and 51.5 mg/dL of milk. Two 35-mL samples from each urea level were sent to the 3 laboratories used in experiment 1. Average analyzed MUN was greater than predicted (calculated for each laboratory based on the control; 0 mg of added urea): for laboratory A (23.2 vs. 21.0 mg/dL), laboratory B (18.0 vs. 13.3 mg/dL), and laboratory C (20.6 vs. 15.2 mg/dL). In experiment 3, replicated milk samples were preserved with 0 to 1.35 mg of bronopol/mL of milk and submitted to one milk processing laboratory that analyzed MUN using 2 different methods. Milk samples with increasing amounts of bronopol ranged in MUN concentration from 7.7 to 11.9 mg/dL and from 9.0 to 9.3 mg/dL when analyzed on MilkoScan 4000 or CL 10 (EuroChem, Moscow, Russia), respectively. In conclusion, measured MUN concentrations varied due to analytical procedure used by milk processing laboratories and were affected by the amount of bronopol used to preserve milk sample, when milk was analyzed using a mid-infrared analyzer. Thus, it is important to maintain consistency in milk sample preservation and analysis to ensure precision of MUN results. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Calculating cost savings in utilization management.

PubMed

MacMillan, Donna

2014-01-01

A major motivation for managing the utilization of laboratory testing is to reduce the cost of medical care. For this reason it is important to understand the basic principles of cost accounting in the clinical laboratory. The process of laboratory testing includes three distinct components termed the pre-analytic, analytic and post-analytic phases. Utilization management efforts may impact the cost structure of these three phases in different ways depending on the specific details of the initiative. Estimates of cost savings resulting from utilization management programs reported in the literature have often been fundamentally flawed due to a failure to understand basic concepts such as the difference between laboratory costs versus charges and the impact of reducing laboratory test volumes on the average versus marginal cost structure in the laboratory. This article will provide an overview of basic cost accounting principles in the clinical laboratory including both job order and process cost accounting. Specific examples will be presented to illustrate these concepts in various different scenarios. © 2013.

USGS Blind Sample Project: monitoring and evaluating laboratory analytical quality

USGS Publications Warehouse

Ludtke, Amy S.; Woodworth, Mark T.

1997-01-01

The U.S. Geological Survey (USGS) collects and disseminates information about the Nation's water resources. Surface- and ground-water samples are collected and sent to USGS laboratories for chemical analyses. The laboratories identify and quantify the constituents in the water samples. Random and systematic errors occur during sample handling, chemical analysis, and data processing. Although all errors cannot be eliminated from measurements, the magnitude of their uncertainty can be estimated and tracked over time. Since 1981, the USGS has operated an independent, external, quality-assurance project called the Blind Sample Project (BSP). The purpose of the BSP is to monitor and evaluate the quality of laboratory analytical results through the use of double-blind quality-control (QC) samples. The information provided by the BSP assists the laboratories in detecting and correcting problems in the analytical procedures. The information also can aid laboratory users in estimating the extent that laboratory errors contribute to the overall errors in their environmental data.

CLSI-based transference and verification of CALIPER pediatric reference intervals for 29 Ortho VITROS 5600 chemistry assays.

PubMed

Higgins, Victoria; Truong, Dorothy; Woroch, Amy; Chan, Man Khun; Tahmasebi, Houman; Adeli, Khosrow

2018-03-01

Evidence-based reference intervals (RIs) are essential to accurately interpret pediatric laboratory test results. To fill gaps in pediatric RIs, the Canadian Laboratory Initiative on Pediatric Reference Intervals (CALIPER) project developed an age- and sex-specific pediatric RI database based on healthy pediatric subjects. Originally established for Abbott ARCHITECT assays, CALIPER RIs were transferred to assays on Beckman, Roche, Siemens, and Ortho analytical platforms. This study provides transferred reference intervals for 29 biochemical assays for the Ortho VITROS 5600 Chemistry System (Ortho). Based on Clinical Laboratory Standards Institute (CLSI) guidelines, a method comparison analysis was performed by measuring approximately 200 patient serum samples using Abbott and Ortho assays. The equation of the line of best fit was calculated and the appropriateness of the linear model was assessed. This equation was used to transfer RIs from Abbott to Ortho assays. Transferred RIs were verified using 84 healthy pediatric serum samples from the CALIPER cohort. RIs for most chemistry analytes successfully transferred from Abbott to Ortho assays. Calcium and CO 2 did not meet statistical criteria for transference (r 2 <0.70). Of the 32 transferred reference intervals, 29 successfully verified with approximately 90% of results from reference samples falling within transferred confidence limits. Transferred RIs for total bilirubin, magnesium, and LDH did not meet verification criteria and are not reported. This study broadens the utility of the CALIPER pediatric RI database to laboratories using Ortho VITROS 5600 biochemical assays. Clinical laboratories should verify CALIPER reference intervals for their specific analytical platform and local population as recommended by CLSI. Copyright © 2018 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

National survey on intra-laboratory turnaround time for some most common routine and stat laboratory analyses in 479 laboratories in China.

PubMed

Fei, Yang; Zeng, Rong; Wang, Wei; He, Falin; Zhong, Kun; Wang, Zhiguo

2015-01-01

To investigate the state of the art of intra-laboratory turnaround time (intra-TAT), provide suggestions and find out whether laboratories accredited by International Organization for Standardization (ISO) 15189 or College of American Pathologists (CAP) will show better performance on intra-TAT than non-accredited ones. 479 Chinese clinical laboratories participating in the external quality assessment programs of chemistry, blood gas, and haematology tests organized by the National Centre for Clinical Laboratories in China were included in our study. General information and the median of intra-TAT of routine and stat tests in last one week were asked in the questionnaires. The response rate of clinical biochemistry, blood gas, and haematology testing were 36% (479/1307), 38% (228/598), and 36% (449/1250), respectively. More than 50% of laboratories indicated that they had set up intra-TAT median goals and almost 60% of laboratories declared they had monitored intra-TAT generally for every analyte they performed. Among all analytes we investigated, the intra-TAT of haematology analytes was shorter than biochemistry while the intra-TAT of blood gas analytes was the shortest. There were significant differences between median intra-TAT on different days of the week for routine tests. However, there were no significant differences in median intra-TAT reported by accredited laboratories and non-accredited laboratories. Many laboratories in China are aware of intra-TAT control and are making effort to reach the target. There is still space for improvement. Accredited laboratories have better status on intra-TAT monitoring and target setting than the non-accredited, but there are no significant differences in median intra-TAT reported by them.

Analytical methods for determination of mycotoxins: a review.

PubMed

Turner, Nicholas W; Subrahmanyam, Sreenath; Piletsky, Sergey A

2009-01-26

Mycotoxins are small (MW approximately 700), toxic chemical products formed as secondary metabolites by a few fungal species that readily colonise crops and contaminate them with toxins in the field or after harvest. Ochratoxins and Aflatoxins are mycotoxins of major significance and hence there has been significant research on broad range of analytical and detection techniques that could be useful and practical. Due to the variety of structures of these toxins, it is impossible to use one standard technique for analysis and/or detection. Practical requirements for high-sensitivity analysis and the need for a specialist laboratory setting create challenges for routine analysis. Several existing analytical techniques, which offer flexible and broad-based methods of analysis and in some cases detection, have been discussed in this manuscript. There are a number of methods used, of which many are lab-based, but to our knowledge there seems to be no single technique that stands out above the rest, although analytical liquid chromatography, commonly linked with mass spectroscopy is likely to be popular. This review manuscript discusses (a) sample pre-treatment methods such as liquid-liquid extraction (LLE), supercritical fluid extraction (SFE), solid phase extraction (SPE), (b) separation methods such as (TLC), high performance liquid chromatography (HPLC), gas chromatography (GC), and capillary electrophoresis (CE) and (c) others such as ELISA. Further currents trends, advantages and disadvantages and future prospects of these methods have been discussed.

Results of a Saxitoxin Proficiency Test Including Characterization of Reference Material and Stability Studies

PubMed Central

Harju, Kirsi; Rapinoja, Marja-Leena; Avondet, Marc-André; Arnold, Werner; Schär, Martin; Luginbühl, Werner; Kremp, Anke; Suikkanen, Sanna; Kankaanpää, Harri; Burrell, Stephen; Söderström, Martin; Vanninen, Paula

2015-01-01

A saxitoxin (STX) proficiency test (PT) was organized as part of the Establishment of Quality Assurance for the Detection of Biological Toxins of Potential Bioterrorism Risk (EQuATox) project. The aim of this PT was to provide an evaluation of existing methods and the European laboratories’ capabilities for the analysis of STX and some of its analogues in real samples. Homogenized mussel material and algal cell materials containing paralytic shellfish poisoning (PSP) toxins were produced as reference sample matrices. The reference material was characterized using various analytical methods. Acidified algal extract samples at two concentration levels were prepared from a bulk culture of PSP toxins producing dinoflagellate Alexandrium ostenfeldii. The homogeneity and stability of the prepared PT samples were studied and found to be fit-for-purpose. Thereafter, eight STX PT samples were sent to ten participating laboratories from eight countries. The PT offered the participating laboratories the possibility to assess their performance regarding the qualitative and quantitative detection of PSP toxins. Various techniques such as official Association of Official Analytical Chemists (AOAC) methods, immunoassays, and liquid chromatography-mass spectrometry were used for sample analyses. PMID:26602927

Request Pattern, Pre-Analytical and Analytical Conditions of Urinalysis in Primary Care: Lessons from a One-Year Large-Scale Multicenter Study.

PubMed

Salinas, Maria; Lopez-Garrigos, Maite; Flores, Emilio; Leiva-Salinas, Carlos

2018-06-01

To study the urinalysis request, pre-analytical sample conditions, and analytical procedures. Laboratories were asked to provide the number of primary care urinalyses requested, and to fill out a questionnaire regarding pre-analytical conditions and analytical procedures. 110 laboratories participated in the study. 232.5 urinalyses/1,000 inhabitants were reported. 75.4% used the first morning urine. The sample reached the laboratory in less than 2 hours in 18.8%, between 2 - 4 hours in 78.3%, and between 4 - 6 hours in the remaining 2.9%. 92.5% combined the use of test strip and particle analysis, and only 7.5% used the strip exclusively. All participants except one performed automated particle analysis depending on strip results; in 16.2% the procedure was only manual. Urinalysis was highly requested. There was a lack of compliance with guidelines regarding time between micturition and analysis that usually involved the combination of strip followed by particle analysis.

Collaborative trial validation study of two methods, one based on high performance liquid chromatography-tandem mass spectrometry and on gas chromatography-mass spectrometry for the determination of acrylamide in bakery and potato products.

PubMed

Wenzl, Thomas; Karasek, Lubomir; Rosen, Johan; Hellenaes, Karl-Erik; Crews, Colin; Castle, Laurence; Anklam, Elke

2006-11-03

A European inter-laboratory study was conducted to validate two analytical procedures for the determination of acrylamide in bakery ware (crispbreads, biscuits) and potato products (chips), within a concentration range from about 20 microg/kg to about 9000 microgg/kg. The methods are based on gas chromatography-mass spectrometry (GC-MS) of the derivatised analyte and on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) of native acrylamide. Isotope dilution with isotopically labelled acrylamide was an integral part of both methods. The study was evaluated according to internationally accepted guidelines. The performance of the HPLC-MS/MS method was found to be superior to that of the GC-MS method and to be fit-for-the-purpose.

Analytical investigation of a three-dimensional FRP-retrofitted reinforced concrete structure's behaviour under earthquake load effect in ANSYS program

NASA Astrophysics Data System (ADS)

Altun, F.; Birdal, F.

2012-12-01

In this study, a 1:3 scaled, three-storey, FRP (Fiber Reinforced Polymer) retrofitted reinforced concrete model structure whose behaviour and crack development were identified experimentally in the laboratory was investigated analytically. Determination of structural behaviour under earthquake load is only possible in a laboratory environment with a specific scale, as carrying out structural experiments is difficult due to the evaluation of increased parameter numbers and because it requires an expensive laboratory setup. In an analytical study, structure was modelled using ANSYS Finite Element Package Program (2007), and its behaviour and crack development were revealed. When experimental difficulties are taken into consideration, analytical investigation of structure behaviour is more economic and much faster. At the end of the study, experimental results of structural behaviour and crack development were compared with analytical data. It was concluded that in a model structure retrofitted with FRP, the behaviour and cracking model can be determined without testing by determining the reasons for the points where analytical results are not converged with experimental data. Better understanding of structural behaviour is analytically enabled with the study.

Analysis of Environmental Contamination resulting from ...

EPA Pesticide Factsheets

Catastrophic incidents can generate a large number of samples with analytically diverse types including forensic, clinical, environmental, food, and others. Environmental samples include water, wastewater, soil, air, urban building and infrastructure materials, and surface residue. Such samples may arise not only from contamination from the incident but also from the multitude of activities surrounding the response to the incident, including decontamination. This document summarizes a range of activities to help build laboratory capability in preparation for analysis following a catastrophic incident, including selection and development of fit-for-purpose analytical methods for chemical, biological, and radiological contaminants. Fit-for-purpose methods are those which have been selected to meet project specific data quality objectives. For example, methods could be fit for screening contamination in the early phases of investigation of contamination incidents because they are rapid and easily implemented, but those same methods may not be fit for the purpose of remediating the environment to safe levels when a more sensitive method is required. While the exact data quality objectives defining fitness-for-purpose can vary with each incident, a governing principle of the method selection and development process for environmental remediation and recovery is based on achieving high throughput while maintaining high quality analytical results. This paper illu

VALIDATION OF ANALYTICAL METHODS AND INSTRUMENTATION FOR BERYLLIUM MEASUREMENT: REVIEW AND SUMMARY OF AVAILABLE GUIDES, PROCEDURES, AND PROTOCOLS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ekechukwu, A.

This document proposes to provide a listing of available sources which can be used to validate analytical methods and/or instrumentation for beryllium determination. A literature review was conducted of available standard methods and publications used for method validation and/or quality control. A comprehensive listing of the articles, papers, and books reviewed is given in Appendix 1. Available validation documents and guides are listed in the appendix; each has a brief description of application and use. In the referenced sources, there are varying approaches to validation and varying descriptions of validation at different stages in method development. This discussion focuses onmore » validation and verification of fully developed methods and instrumentation that have been offered up for use or approval by other laboratories or official consensus bodies such as ASTM International, the International Standards Organization (ISO) and the Association of Official Analytical Chemists (AOAC). This review was conducted as part of a collaborative effort to investigate and improve the state of validation for measuring beryllium in the workplace and the environment. Documents and publications from the United States and Europe are included. Unless otherwise specified, all documents were published in English.« less

[ABOUT UNIFICATION OF LABORATORY CRITERIA OF DIFFERENTIATION OF BACTERIAL VAGINOSIS].

PubMed

Mavzutov, A R; Tsvetkova, A V; Muretdinova, L A

2015-06-01

The article presents analysis of laboratory criteria and classifcations used to interpret results of laboratory analysis by technique of microscopy on bacterial vaginosis or dysbacteriosis of vagina. Their advantages and restrictions are demonstrated The unified criteria of evaluation are proposed concerning results of microscopy of mucosal discharge of vagina and corresponding classification. Thereafter, three degrees of bacterial vaginosis (dysbacteriosis of vagina) are differentiated: first degree--compensated dysbacteriosis of vagina, second degree--sub compensated dysbacteriosis of vagina and third degree--decompensated dysbacteriosis of vagina. The corresponding laboratory report of physician is formulated. The proposals are presented concerning development of common unified requirements to stages (pre-analytical, analytical, post-analytical) of laboratory diagnostic of bacterial vaginosis (dysbacteriosis of vagina) with purpose of their unambiguous understanding by clinicians and hence their decision making concerning necessity and tactics of management of patient.

The Abbott Architect c8000: analytical performance and productivity characteristics of a new analyzer applied to general chemistry testing.

PubMed

Pauli, Daniela; Seyfarth, Michael; Dibbelt, Leif

2005-01-01

Applying basic potentiometric and photometric assays, we evaluated the fully automated random access chemistry analyzer Architect c8000, a new member of the Abbott Architect system family, with respect to both its analytical and operational performance and compared it to an established high-throughput chemistry platform, the Abbott Aeroset. Our results demonstrate that intra- and inter-assay imprecision, inaccuracy, lower limit of detection and linear range of the c8000 generally meet actual requirements of laboratory diagnosis; there were only rare exceptions, e.g. assays for plasma lipase or urine uric acid which apparently need to be improved by additional rinsing of reagent pipettors. Even with plasma exhibiting CK activities as high as 40.000 U/l, sample carryover by the c8000 could not be detected. Comparison of methods run on the c8000 and the Aeroset revealed correlation coefficients of 0.98-1.00; if identical chemistries were applied on both analyzers, slopes of regression lines approached unity. With typical laboratory workloads including 10-20% STAT samples and up to 10% samples with high analyte concentrations demanding dilutional reruns, steady-state throughput numbers of 700 to 800 tests per hour were obtained with the c8000. The system generally responded to STAT orders within 2 minutes yielding analytical STAT order completion times of 5 to 15 minutes depending on the type and number of assays requested per sample. Due to its extended test and sample processing capabilities and highly comfortable software, the c8000 may meet the varying needs of clinical laboratories rather well.

[Validation of measurement methods and estimation of uncertainty of measurement of chemical agents in the air at workstations].

PubMed

Dobecki, Marek

2012-01-01

This paper reviews the requirements for measurement methods of chemical agents in the air at workstations. European standards, which have a status of Polish standards, comprise some requirements and information on sampling strategy, measuring techniques, type of samplers, sampling pumps and methods of occupational exposure evaluation at a given technological process. Measurement methods, including air sampling and analytical procedure in a laboratory, should be appropriately validated before intended use. In the validation process, selected methods are tested and budget of uncertainty is set up. The validation procedure that should be implemented in the laboratory together with suitable statistical tools and major components of uncertainity to be taken into consideration, were presented in this paper. Methods of quality control, including sampling and laboratory analyses were discussed. Relative expanded uncertainty for each measurement expressed as a percentage, should not exceed the limit of values set depending on the type of occupational exposure (short-term or long-term) and the magnitude of exposure to chemical agents in the work environment.

Optimization of detection conditions and single-laboratory validation of a multiresidue method for the determination of 135 pesticides and 25 organic pollutants in grapes and wine by gas chromatography time-of-flight mass spectrometry.

PubMed

Dasgupta, Soma; Banerjee, Kaushik; Dhumal, Kondiba N; Adsule, Pandurang G

2011-01-01

This paper describes single-laboratory validation of a multiresidue method for the determination of 135 pesticides, 12 dioxin-like polychlorinated biphenyls, 12 polyaromatic hydrocarbons, and bisphenol A in grapes and wine by GC/time-of-flight MS in a total run time of 48 min. The method is based on extraction with ethyl acetate in a sample-to-solvent ratio of 1:1, followed by selective dispersive SPE cleanup for grapes and wine. The GC/MS conditions were optimized for the chromatographic separation and to achieve highest S/N for all 160 target analytes, including the temperature-sensitive compounds, like captan and captafol, that are prone to degradation during analysis. An average recovery of 80-120% with RSD < 10% could be attained for all analytes except 17, for which the average recoveries were 70-80%. LOQ ranged within 10-50 ng/g, with < 25% expanded uncertainties, for 155 compounds in grapes and 151 in wine. In the incurred grape and wine samples, the residues of buprofezin, chlorpyriphos, metalaxyl, and myclobutanil were detected, with an RSD of < 5% (n = 6); the results were statistically similar to previously reported validated methods.

Chemical analysis of pharmaceuticals and explosives in fingermarks using matrix-assisted laser desorption ionization/time-of-flight mass spectrometry.

PubMed

Kaplan-Sandquist, Kimberly; LeBeau, Marc A; Miller, Mark L

2014-02-01

Chemical analysis of latent fingermarks, "touch chemistry," has the potential of providing intelligence or forensically relevant information. Matrix-assisted laser desorption ionization/time-of-flight mass spectrometry (MALDI/TOF MS) was used as an analytical platform for obtaining mass spectra and chemical images of target drugs and explosives in fingermark residues following conventional fingerprint development methods and MALDI matrix processing. There were two main purposes of this research: (1) develop effective laboratory methods for detecting drugs and explosives in fingermark residues and (2) determine the feasibility of detecting drugs and explosives after casual contact with pills, powders, and residues. Further, synthetic latent print reference pads were evaluated as mimics of natural fingermark residue to determine if the pads could be used for method development and quality control. The results suggest that artificial amino acid and sebaceous oil residue pads are not suitable to adequately simulate natural fingermark chemistry for MALDI/TOF MS analysis. However, the pads were useful for designing experiments and setting instrumental parameters. Based on the natural fingermark residue experiments, handling whole or broken pills did not transfer sufficient quantities of drugs to allow for definitive detection. Transferring drugs or explosives in the form of powders and residues was successful for preparing analytes for detection after contact with fingers and deposition of fingermark residue. One downfall to handling powders was that the analyte particles were easily spread beyond the original fingermark during development. Analyte particles were confined in the original fingermark when using transfer residues. The MALDI/TOF MS was able to detect procaine, pseudoephedrine, TNT, and RDX from contact residue under laboratory conditions with the integration of conventional fingerprint development methods and MALDI matrix. MALDI/TOF MS is a nondestructive technique which provides chemical information in both the mass spectra and chemical images. Published by Elsevier Ireland Ltd.

Radioactive Waste Characterization Strategies; Comparisons Between AK/PK, Dose to Curie Modeling, Gamma Spectroscopy, and Laboratory Analysis Methods- 12194

DOE Office of Scientific and Technical Information (OSTI.GOV)

Singledecker, Steven J.; Jones, Scotty W.; Dorries, Alison M.

2012-07-01

In the coming fiscal years of potentially declining budgets, Department of Energy facilities such as the Los Alamos National Laboratory (LANL) will be looking to reduce the cost of radioactive waste characterization, management, and disposal processes. At the core of this cost reduction process will be choosing the most cost effective, efficient, and accurate methods of radioactive waste characterization. Central to every radioactive waste management program is an effective and accurate waste characterization program. Choosing between methods can determine what is classified as low level radioactive waste (LLRW), transuranic waste (TRU), waste that can be disposed of under an Authorizedmore » Release Limit (ARL), industrial waste, and waste that can be disposed of in municipal landfills. The cost benefits of an accurate radioactive waste characterization program cannot be overstated. In addition, inaccurate radioactive waste characterization of radioactive waste can result in the incorrect classification of radioactive waste leading to higher disposal costs, Department of Transportation (DOT) violations, Notice of Violations (NOVs) from Federal and State regulatory agencies, waste rejection from disposal facilities, loss of operational capabilities, and loss of disposal options. Any one of these events could result in the program that mischaracterized the waste losing its ability to perform it primary operational mission. Generators that produce radioactive waste have four characterization strategies at their disposal: - Acceptable Knowledge/Process Knowledge (AK/PK); - Indirect characterization using a software application or other dose to curie methodologies; - Non-Destructive Analysis (NDA) tools such as gamma spectroscopy; - Direct sampling (e.g. grab samples or Surface Contaminated Object smears) and laboratory analytical; Each method has specific advantages and disadvantages. This paper will evaluate each method detailing those advantages and disadvantages including; - Cost benefit analysis (basic materials costs, overall program operations costs, man-hours per sample analyzed, etc.); - Radiation Exposure As Low As Reasonably Achievable (ALARA) program considerations; - Industrial Health and Safety risks; - Overall Analytical Confidence Level. The concepts in this paper apply to any organization with significant radioactive waste characterization and management activities working to within budget constraints and seeking to optimize their waste characterization strategies while reducing analytical costs. (authors)« less

Colorimetric Detection of Water Vapor Using Metal-Organic Framework Composites.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Allendorf, Mark D.

Purpose: Water vapor trapped in encapsulation materials or enclosed volumes leads to corrosion issues for critical NW components. Sandia National Laboratories has created a new diagnostic to indicate the presence of water in weapon systems. Impact: Component exposure to water now can be determined instantly, without need for costly, time-consuming analytical methods.

Making and Using a Sensing Polymeric Material for Cu[superscript 2+

ERIC Educational Resources Information Center

Paddock, Jean R.; Maghasi, Anne T.; Heineman, William R.; Seliskar, Carl J.

2005-01-01

A simple chemical sensor-related experiment rooted in the synthesis of polymeric materials for use in either an advanced high-school or undergraduate college laboratory is presented. Students are introduced to and combine to the concepts of the chemical sensor, polymer chemistry, spectroscopy, metal chelates, and quantitative analytical methods.

Utility of NIST Whole-Genome Reference Materials for the Technical Validation of a Multigene Next-Generation Sequencing Test.

PubMed

Shum, Bennett O V; Henner, Ilya; Belluoccio, Daniele; Hinchcliffe, Marcus J

2017-07-01

The sensitivity and specificity of next-generation sequencing laboratory developed tests (LDTs) are typically determined by an analyte-specific approach. Analyte-specific validations use disease-specific controls to assess an LDT's ability to detect known pathogenic variants. Alternatively, a methods-based approach can be used for LDT technical validations. Methods-focused validations do not use disease-specific controls but use benchmark reference DNA that contains known variants (benign, variants of unknown significance, and pathogenic) to assess variant calling accuracy of a next-generation sequencing workflow. Recently, four whole-genome reference materials (RMs) from the National Institute of Standards and Technology (NIST) were released to standardize methods-based validations of next-generation sequencing panels across laboratories. We provide a practical method for using NIST RMs to validate multigene panels. We analyzed the utility of RMs in validating a novel newborn screening test that targets 70 genes, called NEO1. Despite the NIST RM variant truth set originating from multiple sequencing platforms, replicates, and library types, we discovered a 5.2% false-negative variant detection rate in the RM truth set genes that were assessed in our validation. We developed a strategy using complementary non-RM controls to demonstrate 99.6% sensitivity of the NEO1 test in detecting variants. Our findings have implications for laboratories or proficiency testing organizations using whole-genome NIST RMs for testing. Copyright © 2017 American Society for Investigative Pathology and the Association for Molecular Pathology. Published by Elsevier Inc. All rights reserved.

Analysis of polyphosphates in fish and shrimps tissues by two different ion chromatography methods: implications on false-negative and -positive findings.

PubMed

Kaufmann, A; Maden, K; Leisser, W; Matera, M; Gude, T

2005-11-01

Inorganic polyphosphates (di-, tri- and higher polyphosphates) can be used to treat fish, fish fillets and shrimps in order to improve their water-binding capacity. The practical relevance of this treatment is a significant gain of weight caused by the retention/uptake of water and natural juice into the fish tissues. This practice is legal; however, the use of phosphates has to be declared. The routine control testing of fish for the presence of polyphosphates, produced some results that were difficult to explain. One of the two analytical methods used determined low diphosphate concentrations in a number of untreated samples, while the other ion chromatography (IC) method did not detect them. This initiated a number of investigations: results showed that polyphosphates in fish and shrimps tissue undergo a rapid enzymatic degradation, producing the ubiquitous orthophosphate. This led to the conclusion that sensitive analytical methods are required in order to detect previous polyphosphate treatment of a sample. The polyphosphate concentrations detected by one of the analytical methods could not be explained by the degradation of endogenous high-energy nucleotides like ATP into diphosphate, but by a coeluting compound. Further investigations by LC-MS-MS proved that the substance responsible for the observed peak was inosine monophsosphate (IMP) and not as thought the inorganic diphosphate. The method producing the false-positive result was modified and both methods were ultimately able to detect polyphosphates well separated from natural nucleotides. Polyphosphates could no longer be detected (<0.5 mg kg-1) after modification of the analytical methodology. The relevance of these findings lies in the fact that similar analytical methods are employed in various control laboratories, which might lead to false interpretation of measurements.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lindahl, P.C.

A proposed American Society for Testing and Materials (ASTM) method for the determination of arsenic and selenium content in coal has been used and evaluated in the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) as part of an interlaboratory study. Coal is conducted with Eschka's mixture (MgO + Na/sub 2/CO/sub 3/), followed by determination of the aresnic and selenium content by hydride generation/atomic absorption spectrophotometry. The method was evaluated on a series of coals, including two National Bureau of Standards-Standards Reference Material (NBS-SRM) coals and twelve ASTM coal samples. Comparison of ACL/ANL arsenic and selenium data for themore » suite of coal analyzed showed excellent agreement with certified values for the NBS-SRM coals and with interlaboratory data from five other laboratories for the ASTM coals. 11 refs., 3 figs., 6 tabs.« less

Cocaine profiling for strategic intelligence, a cross-border project between France and Switzerland: part II. Validation of the statistical methodology for the profiling of cocaine.

PubMed

Lociciro, S; Esseiva, P; Hayoz, P; Dujourdy, L; Besacier, F; Margot, P

2008-05-20

Harmonisation and optimization of analytical and statistical methodologies were carried out between two forensic laboratories (Lausanne, Switzerland and Lyon, France) in order to provide drug intelligence for cross-border cocaine seizures. Part I dealt with the optimization of the analytical method and its robustness. This second part investigates statistical methodologies that will provide reliable comparison of cocaine seizures analysed on two different gas chromatographs interfaced with a flame ionisation detectors (GC-FIDs) in two distinct laboratories. Sixty-six statistical combinations (ten data pre-treatments followed by six different distance measurements and correlation coefficients) were applied. One pre-treatment (N+S: area of each peak is divided by its standard deviation calculated from the whole data set) followed by the Cosine or Pearson correlation coefficients were found to be the best statistical compromise for optimal discrimination of linked and non-linked samples. The centralisation of the analyses in one single laboratory is not a required condition anymore to compare samples seized in different countries. This allows collaboration, but also, jurisdictional control over data.

Analytical methods for PCBs and organochlorine pesticides in environmental monitoring and surveillance: a critical appraisal

PubMed Central

Sverko, Ed

2006-01-01

Analytical methods for the analysis of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) are widely available and are the result of a vast amount of environmental analytical method development and research on persistent organic pollutants (POPs) over the past 30–40 years. This review summarizes procedures and examines new approaches for extraction, isolation, identification and quantification of individual congeners/isomers of the PCBs and OCPs. Critical to the successful application of this methodology is the collection, preparation, and storage of samples, as well as specific quality control and reporting criteria, and therefore these are also discussed. With the signing of the Stockholm convention on POPs and the development of global monitoring programs, there is an increased need for laboratories in developing countries to determine PCBs and OCPs. Thus, while this review attempts to summarize the current best practices for analysis of PCBs and OCPs, a major focus is the need for low-cost methods that can be easily implemented in developing countries. A “performance based” process is described whereby individual laboratories can adapt methods best suited to their situations. Access to modern capillary gas chromatography (GC) equipment with either electron capture or low-resolution mass spectrometry (MS) detection to separate and quantify OCP/PCBs is essential. However, screening of samples, especially in areas of known use of OCPs or PCBs, could be accomplished with bioanalytical methods such as specific commercially available enzyme-linked immunoabsorbent assays and thus this topic is also reviewed. New analytical techniques such two-dimensional GC (2D-GC) and “fast GC” using GC–ECD may be well-suited for broader use in routine PCB/OCP analysis in the near future given their relatively low costs and ability to provide high-resolution separations of PCB/OCPs. Procedures with low environmental impact (SPME, microscale, low solvent use, etc.) are increasingly being used and may be particularly suited to developing countries. Electronic supplementary material Supplementary material is available in the online version of this article at http://dx.doi.org/10.1007/s00216-006-0765-y and is accessible for authorized users. PMID:17047943

Inter-laboratory exercise on antibiotic drugs analysis in aqueous samples.

PubMed

Roig, B; Brogat, M; Mompelat, S; Leveque, J; Cadiere, A; Thomas, O

2012-08-30

An inter-laboratory exercise was organized under the PHARMAS EU project, by the Advanced School of Public Health (EHESP), in order to evaluate the performances of analytical methods for the measurement of antibiotics in waters (surface and tap). This is the first time such an exercise on antibiotics has been organized in Europe, using different kinds of analytical methods and devices. In this exercise thirteen laboratories from five countries (Canada, France, Italy, the Netherlands and Portugal) participated, and a total number of 78 samples were distributed. During the exercise, 2 testing samples (3 bottles of each) prepared from tap water and river water, respectively, spiked with antibiotics, were sent to participants and analyzed over a period of one month. A final number of 77 (98.7%) testing samples were considered. Depending on substances studied by each participant, 305 values in duplicate were collected, with the results for each sample being expressed as the target concentration. A statistical study was initiated using 611 results. The mean value, standard deviation, coefficient of variation, standard uncertainty of the mean, median, the minimum and maximum values of each series as well as the 95% confidence interval were obtained from each participant laboratory. In this exercise, 36 results (6% of accounted values) were outliers according to the distribution over the median (box plot). The outlier results were excluded. In order to establish the stability of testing samples in the course of the exercise, differences between variances obtained for every type of sample at different intervals were evaluated. The results showed no representative variations and it can be considered that all samples were stable during the exercise. The goals of this inter-laboratory study were to assess results variability when analysis is conducted by different laboratories, to evaluate the influence of different matrix samples, and to determine the rate at which participating laboratories successfully completed the tests initiated. Copyright © 2012 Elsevier B.V. All rights reserved.

New, small, fast acting blood glucose meters--an analytical laboratory evaluation.

PubMed

Weitgasser, Raimund; Hofmann, Manuela; Gappmayer, Brigitta; Garstenauer, Christa

2007-09-22

Patients and medical personnel are eager to use blood glucose meters that are easy to handle and fast acting. We questioned whether accuracy and precision of these new, small and light weight devices would meet analytical laboratory standards and tested four meters with the above mentioned conditions. Approximately 300 capillary blood samples were collected and tested using two devices of each brand and two different types of glucose test strips. Blood from the same samples was used for comparison. Results were evaluated using maximum deviation of 5% and 10% from the comparative method, the error grid analysis, the overall deviation of the devices, the linear regression analysis as well as the CVs for measurement in series. Of all 1196 measurements a deviation of less than 5% resp. 10% from the reference method was found for the FreeStyle (FS) meter in 69.5% and 96%, the Glucocard X Meter (GX) in 44% and 75%, the One Touch Ultra (OT) in 29% and 60%, the Wellion True Track (WT) in 28.5% and 58%. The error grid analysis gave 99.7% for FS, 99% for GX, 98% for OT and 97% for WT in zone A. The remainder of the values lay within zone B. Linear regression analysis resembled these results. CVs for measurement in series showed higher deviations for OT and WT compared to FS and GX. The four new, small and fast acting glucose meters fulfil clinically relevant analytical laboratory requirements making them appropriate for use by medical personnel. However, with regard to the tight and restrictive limits of the ADA recommendations, the devices are still in need of improvement. This should be taken into account when the devices are used by primarily inexperienced persons and is relevant for further industrial development of such devices.

A comparison of analytical laboratory and optical in situ methods for the measurement of nitrate in north Florida water bodies

NASA Astrophysics Data System (ADS)

Rozin, A. G.; Clark, M. W.

2013-12-01

Assessing the impact of nutrient concentrations on aquatic ecosystems requires an in depth understanding of dynamic biogeochemical cycles that are often a challenge to monitor at the high spatial and temporal resolution necessary to understand these complex processes. Traditional sampling approaches involving discrete samples and laboratory analyses can be constrained by analytical costs, field time, and logistical details that can fail to accurately capture both spatial and temporal changes. Optical in situ instruments may provide the opportunity to continuously monitor a variety of water quality parameters at a high spatial or temporal resolution. This work explores the suitability of a Submersible Ultraviolet Nitrate Analyzer (SUNA), produced by Satlantic, to accurately assess in situ nitrate concentration in several freshwater systems in north Florida. The SUNA was deployed to measure nitrate at five different water bodies selected to represent a range of watershed land uses and water chemistry in the region. In situ nitrate measurements were compared to standard laboratory methods to evaluate the effectiveness of the SUNA's operation. Other optical sensors were used to measure the spectral properties of absorbance, fluorescence, and turbidity (scatter) in the same Florida water bodies. Data from these additional sensors were collected to quantify possible interferences that may affect SUNA performance. In addition, data from the SUNA and other sensors are being used to infer information about the quality and quantity of aqueous constituents besides nitrate. A better understanding of the capabilities and possible limitations of these relatively new analytical instruments will allow researchers to more effectively investigate biogeochemical processes and nutrient transport and enhance decision-making to protect our water bodies.

Analytical Characterization of Erythritol Tetranitrate, an Improvised Explosive.

PubMed

Matyáš, Robert; Lyčka, Antonín; Jirásko, Robert; Jakový, Zdeněk; Maixner, Jaroslav; Mišková, Linda; Künzel, Martin

2016-05-01

Erythritol tetranitrate (ETN), an ester of nitric acid and erythritol, is a solid crystalline explosive with high explosive performance. Although it has never been used in any industrial or military application, it has become one of the most prepared and misused improvise explosives. In this study, several analytical techniques were explored to facilitate analysis in forensic laboratories. FTIR and Raman spectrometry measurements expand existing data and bring more detailed assignment of bands through the parallel study of erythritol [(15) N4 ] tetranitrate. In the case of powder diffraction, recently published data were verified, and (1) H, (13) C, and (15) N NMR spectra are discussed in detail. The technique of electrospray ionization tandem mass spectrometry was successfully used for the analysis of ETN. Described methods allow fast, versatile, and reliable detection or analysis of samples containing erythritol tetranitrate in forensic laboratories. © 2016 American Academy of Forensic Sciences.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

This purpose of this report is to summarize the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for Fiscal Year 1990. The ACL has four technical groups -- Chemical Analysis, Instrumental Analysis, Organic Analysis, and Environmental Analysis. The Chemical Analysis Group uses wet-chemical and instrumental methods for elemental, compositional, and isotopic analyses of solid, liquid, and gaseous samples and provides specialized analytical services. The Instrumental Analysis Group uses nuclear counting techniques in radiochemical analyses over a wide range of sample types from low-level environmental samples to samples of high radioactivity. The Organic Analysis Group uses amore » number of complementary techniques to separate and to quantitatively and qualitatively analyze complex organic mixtures and compounds at the trace level, including synthetic fuels, toxic substances, fossil-fuel residues and emissions, pollutants, biologically active compounds, pesticides, and drugs. The Environmental Analysis Group performs analyses of inorganic environmental and hazardous waste and coal samples.« less

Progress Towards an Open Data Ecosystem for Australian Geochemistry and Geochronology Data

NASA Astrophysics Data System (ADS)

McInnes, B.; Rawling, T.; Brown, W.; Liffers, M.; Wyborn, L. A.; Brown, A.; Cox, S. J. D.

2016-12-01

Technological improvements in laboratory automation and microanalytical methods are producing an unprecedented volume of high-value geochemical data for use by geoscientists in understanding geological and planetary processes. In contrast, the research infrastructure necessary to systematically manage, deliver and archive analytical data has not progressed much beyond the minimum effort necessary to produce a peer-reviewed publication. Anecdotal evidence indicates that the majority of publically funded data is underreported, and what is published is relatively undiscoverable to experienced researchers let alone the general public. Government-funded "open data" initiatives have a role to play in the development of networks of data management and delivery ecosystems and practices allowing access to publically funded data. This paper reports on progress in Australia towards creation of an open data ecosystem involving multiple academic and government research institutions cooperating to create an open data architecture linking researchers, physical samples, sample metadata, laboratory metadata, analytical data and consumers.

Fully automatic method for the determination of fat soluble vitamins and vitamin D metabolites in serum.

PubMed

Mata-Granados, J M; Quesada Gómez, J M; Luque de Castro, M D

2009-05-01

Fat soluble vitamins and vitamin D metabolites are key compounds in bone metabolism. Unfortunately, variability among 25(OH)D assays limits clinician ability to monitor vitamin D status, supplementation, and toxicity. 0.5 ml serum was mixed with 0.5 ml 60% acetonitrile 150 mM sodium dodecyl sulfate, vortexed for 30 s and injected into an automatic solid-phase extraction (SPE) system for cleanup-preconcentration, then on-line transferred to a reversed-phase analytical column by a 15% methanol-acetonitrile mobile phase at 1.0 ml/min for individual separation of the target analytes. Ultraviolet detection was performed at 265 nm, 325 nm and 292 for vitamin D metabolites, vitamin A and alpha- and delta-tocopherols, respectively. Detection limits were between 0.0015 and 0.26 microg/ml for the target compounds, the precision (expressed as relative standard deviation) between 0.83 and 3.6% for repeatability and between 1.8 and 4.62% for within laboratory reproducibility. Recoveries between 97-100.2% and 95-99% were obtained for low and high concentrations of the target analytes in serum. The total analysis time was 20 min. The on-line coupling of SPE-HPLC endows the proposed method with reliability, robustness, and user unattendance, making it a useful tool for high-throughput analysis in clinical and research laboratories.

Clinical performance evaluation of total protein measurement by digital refractometry and characterization of non-protein solute interferences.

PubMed

Hunsaker, Joshua J H; Wyness, Sara P; Snow, Taylor M; Genzen, Jonathan R

2016-12-01

Refractometric methods to measure total protein (TP) in serum and plasma specimens have been replaced by automated biuret methods in virtually all routine clinical testing. A subset of laboratories, however, still report using refractometry to measure TP in conjunction with serum protein electrophoresis. The objective of this study was therefore to conduct a modern performance evaluation of a digital refractometer for TP measurement. Performance evaluation of a MISCO Palm Abbe™ digital refractometer was conducted through device familiarization, carryover, precision, accuracy, linearity, analytical sensitivity, analytical specificity, and reference interval verification. Comparison assays included a manual refractometer and an automated biuret assay. Carryover risk was eliminated using a demineralized distilled water (ddH 2 O) wash step. Precision studies demonstrated overall imprecision of 2.2% CV (low TP pool) and 0.5% CV (high TP pool). Accuracy studies demonstrated correlation to both manual refractometry and the biuret method. An overall positive bias (+5.0%) was observed versus the biuret method. On average, outlier specimens had an increased triglyceride concentration. Linearity was verified using mixed dilutions of: a) low and high concentration patient pools, or b) albumin-spiked ddH 2 O and high concentration patient pool. Decreased recovery was observed using ddH 2 O dilutions at low TP concentrations. Significant interference was detected at high concentrations of glucose (>267 mg/dL) and triglycerides (>580 mg/dL). Current laboratory reference intervals for TP were verified. Performance characteristics of this digital refractometer were validated in a clinical laboratory setting. Biuret method remains the preferred assay for TP measurement in routine clinical analyses.

Multiresidue analytical method for pharmaceuticals and personal care products in sewage and sewage sludge by online direct immersion SPME on-fiber derivatization - GCMS.

PubMed

López-Serna, Rebeca; Marín-de-Jesús, David; Irusta-Mata, Rubén; García-Encina, Pedro Antonio; Lebrero, Raquel; Fdez-Polanco, María; Muñoz, Raúl

2018-08-15

The work here presented aimed at developing an analytical method for the simultaneous determination of 22 pharmaceuticals and personal care products, including 3 transformation products, in sewage and sludge. A meticulous method optimization, involving an experimental design, was carried out. The developed method was fully automated and consisted of the online extraction of 17 mL of water sample by Direct Immersion Solid Phase MicroExtraction followed by On-fiber Derivatization coupled to Gas Chromatography - Mass Spectrometry (DI-SPME - On-fiber Derivatization - GC - MS). This methodology was validated for 12 of the initial compounds as a reliable (relative recoveries above 90% for sewage and 70% for sludge; repeatability as %RSD below 10% in all cases), sensitive (LODs below 20 ng L -1 in sewage and 10 ng g -1 in sludge), versatile (sewage and sewage-sludge samples up to 15,000 ng L -1 and 900 ng g -1 , respectively) and green analytical alternative for many medium-tech routine laboratories around the world to keep up with both current and forecast environmental regulations requirements. The remaining 10 analytes initially considered showed insufficient suitability to be included in the final method. The methodology was successfully applied to real samples generated in a pilot scale sewage treatment reactor. Copyright © 2018 Elsevier B.V. All rights reserved.

Optimization of two-dimensional gas chromatography time-of-flight mass spectrometry for separation and estimation of the residues of 160 pesticides and 25 persistent organic pollutants in grape and wine.

PubMed

Dasgupta, Soma; Banerjee, Kaushik; Patil, Sangram H; Ghaste, Manoj; Dhumal, K N; Adsule, Pandurang G

2010-06-11

Two-dimensional gas chromatography (GCxGC) coupled with time-of-flight mass spectrometric (TOFMS) method was optimized for simultaneous analysis of 160 pesticides, 12 dioxin-like polychlorinated biphenyls (PCBs), 12 polyaromatic hydrocarbons (PAHs) and bisphenol A in grape and wine. GCxGC-TOFMS could separate all the 185 analytes within 38min with >85% NIST library-based mass spectral confirmations. The matrix effect quantified as the ratio of the slope of matrix-matched to solvent calibrations was within 0.5-1.5 for most analytes. LOQ of most of the analytes was < or =10microg/L with nine exceptions having LOQs of 12.5-25microg/L. Recoveries ranged between 70 and 120% with <20% expanded uncertainties for 151 and 148 compounds in grape and wine, respectively, with intra-laboratory Horwitz ratio <0.2 for all analytes. The method was evaluated in the incurred grape samples where residues of cypermethrin, permethrin, chlorpyriphos, metalaxyl and etophenprox were detected at below MRL. Copyright 2010 Elsevier B.V. All rights reserved.

Planned Variation in Preanalytical Conditions to Evaluate Biospecimen Stability in the National Children’s Study (NCS)

PubMed Central

Mechanic, Leah; Mendez, Armando; Merrill, Lori; Rogers, John; Layton, Marnie; Todd, Deborah; Varanasi, Arti; O’Brien, Barbara; Meyer, William A.; Zhang, Ming; Schleicher, Rosemary L.; Moye, Jack

2014-01-01

BACKGROUND Preanalytical conditions encountered during collection, processing, and storage of biospecimens may influence laboratory results. The National Children’s Study (NCS) is a planned prospective cohort study of 100,000 families to examine the influence of a wide variety of exposures on child health. In developing biospecimen collection, processing, and storage procedures for the NCS, we identified several analytes of different biochemical categories for which it was unclear to what extent deviations from NCS procedures could influence measurement results. METHODS A pilot study was performed to examine effects of preanalytic sample handling conditions (delays in centrifugation, freezing delays, delays in separation from cells, additive delay, and tube type) on concentrations of eight different analytes. 2,825 measurements were made to assess 15 unique combinations of analyte and handling conditions in blood collected from 151 women of childbearing age (≥20 individuals per handling condition). RESULTS The majority of analytes were stable under the conditions evaluated. However, levels of plasma interleukin-6 and serum insulin were decreased in response to sample centrifugation delays of up to 5.5 hours post collection (P<0.0001). In addition, delays in freezing centrifuged plasma samples (comparing 24, 48 and 72 hours to immediate freezing) resulted in increased levels of adrenocorticotropic hormone (P=0.0014). CONCLUSIONS Determining stability of proposed analytes in response to preanalytical conditions and handling helps to ensure high-quality specimens for study now and in the future. The results inform development of procedures, plans for measurement of analytes, and interpretation of laboratory results. PMID:23924524

Field demonstration of on-site analytical methods for TNT and RDX in ground water

DOE Office of Scientific and Technical Information (OSTI.GOV)

Craig, H.; Ferguson, G.; Markos, A.

1996-12-31

A field demonstration was conducted to assess the performance of eight commercially-available and emerging colorimetric, immunoassay, and biosensor on-site analytical methods for explosives 2,4,6-trinitrotoluene (TNT) and hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in ground water and leachate at the Umatilla Army Depot Activity, Hermiston, Oregon and US Naval Submarine Base, Bangor, Washington, Superfund sites. Ground water samples were analyzed by each of the on-site methods and results compared to laboratory analysis using high performance liquid chromatography (HPLC) with EPA SW-846 Method 8330. The commercial methods evaluated include the EnSys, Inc., TNT and RDX colorimetric test kits (EPA SW-846 Methods 8515 and 8510) with amore » solid phase extraction (SPE) step, the DTECH/EM Science TNT and RDX immunoassay test kits (EPA SW-846 Methods 4050 and 4051), and the Ohmicron TNT immunoassay test kit. The emerging methods tested include the antibody-based Naval Research Laboratory (NRL) Continuous Flow Immunosensor (CFI) for TNT and RDX, and the Fiber Optic Biosensor (FOB) for TNT. Accuracy of the on-site methods were evaluated using linear regression analysis and relative percent difference (RPD) comparison criteria. Over the range of conditions tested, the colorimetric methods for TNT and RDX showed the highest accuracy of the emerging methods for TNT and RDX. The colorimetric method was selected for routine ground water monitoring at the Umatilla site, and further field testing on the NRL CFI and FOB biosensors will continue at both Superfund sites.« less

Sequim Marine Research Laboratory routine environmental measurements during CY-1976

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fix, J.J.; Blumer, P.J.

1977-05-01

Beginning in 1976, a routine environmental program was established at the Marine Research Laboratory (MRL) at Sequim, Washington. The program is designed, primarily, to determine levels of radioactivity present in selected biota in Sequim Bay. The biota were selected because of their presence near the laboratory and their capacity to concentrate trace elements. Other samples were obtained to determine the radionuclides in Sequim Bay and laboratory drinking water, as well as the ambient radiation exposure levels and surface deposition of fallout radionuclides for the laboratory area. A summary of the analytical methods used is included. The present document includes datamore » obtained during CY 1976, the first year of the program. Radionuclides present in samples are attributed to fallout. Data are included on content of oil and Cu in seawater samples.« less

Shedding light on food fraud: spectrophotometric and spectroscopic methods as a tool against economically motivated adulteration of food

NASA Astrophysics Data System (ADS)

Petronijević, R. B.; Velebit, B.; Baltić, T.

2017-09-01

Intentional modification of food or substitution of food ingredients with the aim of gaining profit is food fraud or economically motivated adulteration (EMA). EMA appeared in the food supply chain, and following the global expansion of the food market, has become a world-scale problem for the global economy. Food frauds have involved oils, milk and meat products, infant formula, honey, juices, spices, etc. New legislation was enacted in the last decade in order to fight EMA. Effective analytical methods for food fraud detection are few and still in development. The majority of the methods in common use today for EMA detection are time consuming and inappropriate for use on the production line or out of the laboratory. The next step in the evolution of analytical techniques to combat food fraud is development of fast, accurate methods applicable using portable or handheld devices. Spectrophotometric and spectroscopic methods combined with chemometric analysis, and perhaps in combination with other rapid physico-chemical techniques, could be the answer. This review discusses some analytical techniques based on spectrophotometry and spectroscopy, which are used to reveal food fraud and EMA.

Harmonization in laboratory medicine: Requests, samples, measurements and reports.

PubMed

Plebani, Mario

2016-01-01

In laboratory medicine, the terms "standardization" and "harmonization" are frequently used interchangeably as the final goal is the same: the equivalence of measurement results among different routine measurement procedures over time and space according to defined analytical and clinical quality specifications. However, the terms define two distinct, albeit closely linked, concepts based on traceability principles. The word "standardization" is used when results for a measurement are equivalent and traceable to the International System of Units (SI) through a high-order primary reference material and/or a reference measurement procedure (RMP). "Harmonization" is generally used when results are equivalent, but neither a high-order primary reference material nor a reference measurement procedure is available. Harmonization is a fundamental aspect of quality in laboratory medicine as its ultimate goal is to improve patient outcomes through the provision of accurate and actionable laboratory information. Patients, clinicians and other healthcare professionals assume that clinical laboratory tests performed by different laboratories at different times on the same sample and specimen can be compared, and that results can be reliably and consistently interpreted. Unfortunately, this is not necessarily the case, because many laboratory test results are still highly variable and poorly standardized and harmonized. Although the initial focus was mainly on harmonizing and standardizing analytical processes and methods, the scope of harmonization now also includes all other aspects of the total testing process (TTP), such as terminology and units, report formats, reference intervals and decision limits as well as tests and test profiles, requests and criteria for interpretation. Several projects and initiatives aiming to improve standardization and harmonization in the testing process are now underway. Laboratory professionals should therefore step up their efforts to provide interchangeable and comparable laboratory information in order to ultimately assure better diagnosis and treatment in patient care.

Measurements for 8 common analytes in native sera identify inadequate standardization among 6 routine laboratory assays.

PubMed

Stepman, Hedwig C M; Tiikkainen, Ulla; Stöckl, Dietmar; Vesper, Hubert W; Edwards, Selvin H; Laitinen, Harri; Pelanti, Jonna; Thienpont, Linda M

2014-06-01

External quality assessment (EQA) with commutable samples is essential for assessing the quality of assays performed by laboratories, particularly when the emphasis is on their standardization status and interchangeability of results. We used a panel of 20 fresh-frozen single-donation serum samples to assess assays for the measurement of creatinine, glucose, phosphate, uric acid, total cholesterol, HDL cholesterol, LDL cholesterol, and triglycerides. The commercial random access platforms included: Abbott Architect, Beckman Coulter AU, Ortho Vitros, Roche Cobas, Siemens Advia, and Thermo Scientific Konelab. The assessment was done at the peer group level and by comparison against the all-method trimmed mean or reference method values, where available. The considered quality indicators were intraassay imprecision, combined imprecision (including sample-matrix interference), bias, and total error. Fail/pass decisions were based on limits reflecting state-of-the-art performance, but also limits related to biological variation. Most assays showed excellent peer performance attributes, except for HDL- and LDL cholesterol. Cases in which individual assays had biases exceeding the used limits were the Siemens Advia creatinine (-4.2%), Ortho Vitros phosphate (8.9%), Beckman Coulter AU triglycerides (5.4%), and Thermo Scientific Konelab uric acid (6.4%), which lead to considerable interassay discrepancies. Additionally, large laboratory effects were observed that caused interlaboratory differences of >30%. The design of the EQA study was well suited for monitoring different quality attributes of assays performed in daily laboratory practice. There is a need for improvement, even for simple clinical chemistry analytes. In particular, the interchangeability of results remains jeopardized both by assay standardization issues and individual laboratory effects. © 2014 The American Association for Clinical Chemistry.

Quantitative Determination of Caffeine in Beverages Using a Combined SPME-GC/MS Method

NASA Astrophysics Data System (ADS)

Pawliszyn, Janusz; Yang, Min J.; Orton, Maureen L.

1997-09-01

Solid-phase microextraction (SPME) combined with gas chromatography/mass spectrometry (GC/MS) has been applied to the analysis of various caffeinated beverages. Unlike the current methods, this technique is solvent free and requires no pH adjustments. The simplicity of the SPME-GC/MS method lends itself to a good undergraduate laboratory practice. This publication describes the analytical conditions and presents the data for determination of caffeine in coffee, tea, and coke. Quantitation by isotopic dilution is also illustrated.

Considerations in As analysis and speciation

USGS Publications Warehouse

Edwards, M.; Patel, S.; McNeil, L.; Chen, H.W.; Frey, M.; Eaton, A.D.; Antweiler, Ronald C.; Taylor, Howard E.

1998-01-01

This article summarizes recent experiences in arsenic (As) quantification, preservation, and speciation developed during AWWA Research Foundation (AWWARF) and Water Industry Technical Action Fund (WITAF) projects. The goal of this article is to alert analysts and decision-makers to potential problems in As analysis and speciation, because there appear to be several unresolved problems with routine analytical approaches. In true split drinking water samples As was quantified by three accepted analytical methods in three laboratories. The techniques used were graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma mass spectrometry (ICP-MS), and hydride generation inductively coupled plasma-emission spectrometry (HG-ICP-AES). Experimental findings are organized into sections on As analysis, particulate As in water supplies, and examination of As speciation methods.

[Analysis of the results of the SEIMC External Quality Control Program for HIV-1 and HCV viral loads. Year 2008].

PubMed

Mira, Nieves Orta; Serrano, María del Remedio Guna; Martínez, José Carlos Latorre; Ovies, María Rosario; Pérez, José L; Cardona, Concepción Gimeno

2010-01-01

Human immunodeficiency virus type 1 (HIV-1) and hepatitis C virus (HCV) viral load determinations are among the most relevant markers for the follow up of patients infected with these viruses. External quality control tools are crucial to ensure the accuracy of results obtained by microbiology laboratories. This article summarized the results obtained from the 2008 SEIMC External Quality Control Program for HIV-1 and HCV viral loads. In the HIV-1 program, a total of five standards were sent. One standard consisted in seronegative human plasma, while the remaining four contained plasma from 3 different viremic patients, in the range of 2-5 log(10) copies/mL; two of these standards were identical aiming to determine repeatability. The specificity was complete for all commercial methods, and no false positive results were reported by the participants. A significant proportion of the laboratories (24% on average) obtained values out of the accepted range (mean +/- 0.2 log(10) copies/mL), depending on the standard and on the method used for quantification. Repeatability was very good, with up to 95% of laboratories reporting results within the limits (D < 0.5 log(10) copias/mL). The HCV program consisted of two standards with different viral load contents. Most of the participants (88,7%) obtained results within the accepted range (mean +/- 1.96 SD log(10) UI/mL). Post-analytical errors due to mistranscription of the results were detected for HCV, but not for the HIV-1 program. Data from this analysis reinforce the utility of proficiency programmes to ensure the quality of the results obtained by a particular laboratory, as well as the importance of the post-analytical phase on the overall quality. Due to the remarkable interlaboratory variability, it is advisable to use the same method and the same laboratory for patient follow up. 2010 Elsevier España S.L. All rights reserved.

HPV Genotyping of Modified General Primer-Amplicons Is More Analytically Sensitive and Specific by Sequencing than by Hybridization

PubMed Central

Meisal, Roger; Rounge, Trine Ballestad; Christiansen, Irene Kraus; Eieland, Alexander Kirkeby; Worren, Merete Molton; Molden, Tor Faksvaag; Kommedal, Øyvind; Hovig, Eivind; Leegaard, Truls Michael

2017-01-01

Sensitive and specific genotyping of human papillomaviruses (HPVs) is important for population-based surveillance of carcinogenic HPV types and for monitoring vaccine effectiveness. Here we compare HPV genotyping by Next Generation Sequencing (NGS) to an established DNA hybridization method. In DNA isolated from urine, the overall analytical sensitivity of NGS was found to be 22% higher than that of hybridization. NGS was also found to be the most specific method and expanded the detection repertoire beyond the 37 types of the DNA hybridization assay. Furthermore, NGS provided an increased resolution by identifying genetic variants of individual HPV types. The same Modified General Primers (MGP)-amplicon was used in both methods. The NGS method is described in detail to facilitate implementation in the clinical microbiology laboratory and includes suggestions for new standards for detection and calling of types and variants with improved resolution. PMID:28045981

HPV Genotyping of Modified General Primer-Amplicons Is More Analytically Sensitive and Specific by Sequencing than by Hybridization.

PubMed

Meisal, Roger; Rounge, Trine Ballestad; Christiansen, Irene Kraus; Eieland, Alexander Kirkeby; Worren, Merete Molton; Molden, Tor Faksvaag; Kommedal, Øyvind; Hovig, Eivind; Leegaard, Truls Michael; Ambur, Ole Herman

2017-01-01

Sensitive and specific genotyping of human papillomaviruses (HPVs) is important for population-based surveillance of carcinogenic HPV types and for monitoring vaccine effectiveness. Here we compare HPV genotyping by Next Generation Sequencing (NGS) to an established DNA hybridization method. In DNA isolated from urine, the overall analytical sensitivity of NGS was found to be 22% higher than that of hybridization. NGS was also found to be the most specific method and expanded the detection repertoire beyond the 37 types of the DNA hybridization assay. Furthermore, NGS provided an increased resolution by identifying genetic variants of individual HPV types. The same Modified General Primers (MGP)-amplicon was used in both methods. The NGS method is described in detail to facilitate implementation in the clinical microbiology laboratory and includes suggestions for new standards for detection and calling of types and variants with improved resolution.

Development and in-line validation of a Process Analytical Technology to facilitate the scale up of coating processes.

PubMed

Wirges, M; Funke, A; Serno, P; Knop, K; Kleinebudde, P

2013-05-05

Incorporation of an active pharmaceutical ingredient (API) into the coating layer of film-coated tablets is a method mainly used to formulate fixed-dose combinations. Uniform and precise spray-coating of an API represents a substantial challenge, which could be overcome by applying Raman spectroscopy as process analytical tool. In pharmaceutical industry, Raman spectroscopy is still mainly used as a bench top laboratory analytical method and usually not implemented in the production process. Concerning the application in the production process, a lot of scientific approaches stop at the level of feasibility studies and do not manage the step to production scale and process applications. The present work puts the scale up of an active coating process into focus, which is a step of highest importance during the pharmaceutical development. Active coating experiments were performed at lab and production scale. Using partial least squares (PLS), a multivariate model was constructed by correlating in-line measured Raman spectral data with the coated amount of API. By transferring this model, being implemented for a lab scale process, to a production scale process, the robustness of this analytical method and thus its applicability as a Process Analytical Technology (PAT) tool for the correct endpoint determination in pharmaceutical manufacturing could be shown. Finally, this method was validated according to the European Medicine Agency (EMA) guideline with respect to the special requirements of the applied in-line model development strategy. Copyright © 2013 Elsevier B.V. All rights reserved.

Interlaboratory study of a liquid chromatography method for erythromycin: determination of uncertainty.

PubMed

Dehouck, P; Vander Heyden, Y; Smeyers-Verbeke, J; Massart, D L; Marini, R D; Chiap, P; Hubert, Ph; Crommen, J; Van de Wauw, W; De Beer, J; Cox, R; Mathieu, G; Reepmeyer, J C; Voigt, B; Estevenon, O; Nicolas, A; Van Schepdael, A; Adams, E; Hoogmartens, J

2003-08-22

Erythromycin is a mixture of macrolide antibiotics produced by Saccharopolyspora erythreas during fermentation. A new method for the analysis of erythromycin by liquid chromatography has previously been developed. It makes use of an Astec C18 polymeric column. After validation in one laboratory, the method was now validated in an interlaboratory study. Validation studies are commonly used to test the fitness of the analytical method prior to its use for routine quality testing. The data derived in the interlaboratory study can be used to make an uncertainty statement as well. The relationship between validation and uncertainty statement is not clear for many analysts and there is a need to show how the existing data, derived during validation, can be used in practice. Eight laboratories participated in this interlaboratory study. The set-up allowed the determination of the repeatability variance, s(2)r and the between-laboratory variance, s(2)L. Combination of s(2)r and s(2)L results in the reproducibility variance s(2)R. It has been shown how these data can be used in future by a single laboratory that wants to make an uncertainty statement concerning the same analysis.

Phosphorus Concentrations in Stream-Water and Reference Samples - An Assessment of Laboratory Comparability

USGS Publications Warehouse

McHale, Michael R.; McChesney, Dennis

2007-01-01

In 2003, a study was conducted to evaluate the accuracy and precision of 10 laboratories that analyze water-quality samples for phosphorus concentrations in the Catskill Mountain region of New York State. Many environmental studies in this region rely on data from these different laboratories for water-quality analyses, and the data may be used in watershed modeling and management decisions. Therefore, it is important to determine whether the data reported by these laboratories are of comparable accuracy and precision. Each laboratory was sent 12 samples for triplicate analysis for total phosphorus, total dissolved phosphorus, and soluble reactive phosphorus. Eight of these laboratories reported results that met comparability criteria for all samples; the remaining two laboratories met comparability criteria for only about half of the analyses. Neither the analytical method used nor the sample concentration ranges appeared to affect the comparability of results. The laboratories whose results were comparable gave consistently comparable results throughout the concentration range analyzed, and the differences among methods did not diminish comparability. All laboratories had high data precision as indicated by sample triplicate results. In addition, the laboratories consistently reported total phosphorus values greater than total dissolved phosphorus values, and total dissolved phosphorus values greater than soluble reactive phosphorus values, as would be expected. The results of this study emphasize the importance of regular laboratory participation in sample-exchange programs.

Sigma metrics used to assess analytical quality of clinical chemistry assays: importance of the allowable total error (TEa) target.

PubMed

Hens, Koen; Berth, Mario; Armbruster, Dave; Westgard, Sten

2014-07-01

Six Sigma metrics were used to assess the analytical quality of automated clinical chemistry and immunoassay tests in a large Belgian clinical laboratory and to explore the importance of the source used for estimation of the allowable total error. Clinical laboratories are continually challenged to maintain analytical quality. However, it is difficult to measure assay quality objectively and quantitatively. The Sigma metric is a single number that estimates quality based on the traditional parameters used in the clinical laboratory: allowable total error (TEa), precision and bias. In this study, Sigma metrics were calculated for 41 clinical chemistry assays for serum and urine on five ARCHITECT c16000 chemistry analyzers. Controls at two analyte concentrations were tested and Sigma metrics were calculated using three different TEa targets (Ricos biological variability, CLIA, and RiliBÄK). Sigma metrics varied with analyte concentration, the TEa target, and between/among analyzers. Sigma values identified those assays that are analytically robust and require minimal quality control rules and those that exhibit more variability and require more complex rules. The analyzer to analyzer variability was assessed on the basis of Sigma metrics. Six Sigma is a more efficient way to control quality, but the lack of TEa targets for many analytes and the sometimes inconsistent TEa targets from different sources are important variables for the interpretation and the application of Sigma metrics in a routine clinical laboratory. Sigma metrics are a valuable means of comparing the analytical quality of two or more analyzers to ensure the comparability of patient test results.