程序文件和质量手册的编写

质量手册和程序文件是实验室质量体系文件中的核心文件。文中介绍了文件的格式和编写要点。     

Chemical and physical analysis for the improvement of the dry mounting method for fragile documents

Paper lamination is a widely used method to consolidate fragile documents. Previous studies have presented a new method of lamination that allows the consolidation of documents before undertaking aqueous treatments. In this method a thin Japanese paper coated with an acrylic resin is applied on the fragile document by means of a heated press. In this work we optimised the preparation of the lamination sheets as well as the working procedures, and we were able to establish that our laboratory-made specimens are chemically stable, easily reversible and permeable to aqueous solutions. The latest property is of particular importance, since it allows a subsequent aqueous deacidification even for fragile documents. The laminated paper documents were further analysed by means of colorimetry and FTIR spectroscopy before and after accelerated ageing as well as by determination of the alkali reserve left on the coated paper, in order to compare our lamination method with other commercially available lamination sheets.     

Who touched the document?: A new overall strategy for collection and identification of DNA from the questioned documents as a supportive evidence

The questions on which judges/prosecutors apply for expertise are mostly about by whom a document was drafted/signed. In this study, a new collective strategy was constructed including a collection method, a modified-silica-based DNA isolation method, and a novel purification method on four contact traces formed on four different paper surface during writing, using PCR with AmpFlSTR®GlobalFiler™ STR kit (after experimental comparison between three different kits) and identification using CE. This collective analysis approach is more sensitive and superior to its equivalents on questioned documents in literature because quantifiable amounts of touch DNA and profiles with high loci percentages (100% on day 1, 72.72% after 1 week) were obtained up to 1 week even after the most challenging conditions of sample forming that a forensic scientist can meet; as washing hands just before drafting and using a very low pressure in a shorter time (simulating a simple contact real conditions while drafting), using no visualizing technique that damages the document. Using the strategy, four most commonly used paper types were compared, to see in which of them DNA could be recovered better. The success of this strategy was shown on the 1-day to 10-year-old real samples from a diary and some archive documents from a law office (including the mix-DNA and different ballpoint pens). Thus, it became possible to show if a person had touched the document, in high success rates up to 1 week as a secondary evidence, when primary evidences are insufficient for the detection of document fraud offenses.     

SemanticEye: a semantic web application to rationalize and enhance chemical electronic publishing

SemanticEye, an ontology with associated tools, improves the classification and open accessibility of chemical information in electronic publishing. In a manner analogous to digital music management, RDF metadata encoded as Adobe XMP can be extracted from a variety of document formats, such as PDF, and managed in an RDF repository called Sesame. Users upload electronic documents containing XMP to a central server by "dropping" them into WebDAV folders. The documents can then be navigated in a Web browser via their metadata, and multiple documents containing identical metadata can then be aggregated. SemanticEye does not actually store any documents. By including unique identifiers within the XMP, such as the DOI, associated documents can be retrieved from the Web with the help of resolving agents. The power of this metadata driven approach is illustrated by including, within the XMP, InChI identifiers for molecular structures and finding relationships between articles based on their InChIs. SemanticEye will become increasingly more comprehensive as usage becomes more widespread. Furthermore, following the Semantic Web architecture enables the reuse of open software tools, provides a "semantically intuitive" alternative to search engines, and fosters a greater sense of trust in Web-based scientific information.     

Chemical markup, XML and the World-Wide Web. 3. Toward a signed semantic chemical web of trust

We describe how a collection of documents expressed in XML-conforming languages such as CML and XHTML can be authenticated and validated against digital signatures which make use of established X.509 certificate technology. These can be associated either with specific nodes in the XML document or with the entire document. We illustrate this with two examples. An entire journal article expressed in XML has its individual components digitally signed by separate authors, and the collection is placed in an envelope and again signed. The second example involves using a software robot agent to acquire a collection of documents from a specified URL, to perform various operations and transformations on the content, including expressing molecules in CML, and to automatically sign the various components and deposit the result in a repository. We argue that these operations can used as components for building what we term an authenticated and semantic chemical web of trust.     

Accreditation of reference material producers

 The use of reference materials is the most pragmatic means by which the analyst can achieve comparability of data. Reference material producers therefore need to have adequate quality systems in place for ensuring the reliability of their materials. In order to provide guidance to both producers and assessors, ISO Guide 34 has recently been produced detailing the quality system requirements for the production of reference materials. CITAC, REMCO and ILAC are now collaborating in the revision of this guide to produce a free-standing document detailing the general requirements for the competence of reference material producers. This paper discusses some of the more important issues described in these documents. The possible formation of an international register containing details of a reference material producer's quality system status is also discussed.     

Uniform Colloidal Polymer Rods by Stabilizer-Assisted Liquid-Crystallization-Driven Self-Assembly

The synthesis of anisotropic colloidal building blocks is essential for their self-assembly into hierarchical materials. Here, a highly efficient stabilizer-assisted liquid-crystallization-driven self-assembly (SA-LCDSA) strategy was developed to achieve monodisperse colloidal polymer rods. This strategy does not require the use of block copolymers, but only homopolymers or random copolymers. The resulting rods have tunable size and aspect ratios, as well as well-defined columnar liquid crystal structures. The integrated triphenylene units enable the rods to exhibit unusual photo-induced fluorescence enhancement and accompanying irradiation memory effect, which, as demonstrated, are attractive for information encryption/decryption of paper documents. In particular, unwanted document decryption during delivery can be examined by fluorescence kinetics. This SA-LCDSA-based approach can be extended to synthesize other functional particles with desired π-molecular units.     

The use of laser desorption/ionization mass spectrometry in the analysis of inks in questioned documents

Determination of the age of a handwritten or ink printed questioned document can be an important consideration in forensic cases. Most often the age of a document is determined by the chemical behavior of the dyes that make up the ink. Exposure of the dyes to environmental factors such as oxygen and ultraviolet or visible light cause them to degrade. Often this degradation can be correlated to the time since the exposure of the ink to the elements began. A number of methods have been used to track the aging of inks on paper. This paper reports the use of laser desorption mass spectrometry as a valuable tool in not only elucidating the structures of dyes used in inks but tracking the change in their chemistry as they age. This study also explores methods for artificially aging documents using ultraviolet and visible light.     

Document authentication at molecular levels using desorption atmospheric pressure chemical ionization mass spectrometry imaging

Molecular images of documents were obtained by sequentially scanning the surface of the document using desorption atmospheric pressure chemical ionization mass spectrometry (DAPCI‐MS), which was operated in either a gasless, solvent‐free or methanol vapor‐assisted mode. The decay process of the ink used for handwriting was monitored by following the signal intensities recorded by DAPCI‐MS. Handwritings made using four types of inks on four kinds of paper surfaces were tested. By studying the dynamic decay of the inks, DAPCI‐MS imaging differentiated a 10‐min old from two 4 h old samples. Non‐destructive forensic analysis of forged signatures either handwritten or computer‐assisted was achieved according to the difference of the contour in DAPCI images, which was attributed to the strength personalized by different writers. Distinction of the order of writing/stamping on documents and detection of illegal printings were accomplished with a spatial resolution of about 140 µm. A Matlab® written program was developed to facilitate the visualization of the similarity between signature images obtained by DAPCI‐MS. The experimental results show that DAPCI‐MS imaging provides rich information at the molecular level and thus can be used for the reliable document analysis in forensic applications. © 2013 The Authors. Journal of Mass Spectrometry published by John Wiley & Sons, Ltd.     

The U.S. Department of Energy (DOE) Sampling and Analytical Chemistry Guide: Doe Methods for Evaluating Environmental and Waste Management Samples

Abstract

DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) is a guidance/methods document to support sampling and analysis activities at DOE sites. DOE Methods is intended to supplement existing guidance documents (e.g., EPA's Test Methods for Evaluating Solid Waste, SW-846), which generally apply to low-level or nonradioactive samples. DOE Methods targets the complexities of DOE radioactive mixed waste and environmental samples. The document contains quality assurance (QA), quality control (QC), safety, sampling, organic analysis, inorganic analysis, and radioanalytical guidance as well as sampling and analytical methods. An addendum is distributed every six months (April and October) with updated guidance and additional methods.

DOE Methods provides a vehicle for technology transfer within the environmental restoration (ER) and waste management (WM) (collectively known as EM) community. As DOE Methods evolves, its usefulness and applicability are anticipated to grow to meet the demands of the DOE/EM mission. At the present time, DOE Methods contains methods and guidance information supplied by DOE sites. Because the EM activities in DOE are not unique to the United States, the international environmental community could benefit from the information gathered for the DOE program. This information could provide additional resources for their EM activities.     

DATINK pilot study: An effective methodology for ballpoint pen ink dating in questioned documents

Establishing the approximate age of an ink entry from a questioned document is often a complicated task and a controversial issue in forensic sciences. Among the existing approaches, the analysis of solvents in ballpoint inks may be a useful parameter for determining the age of ink on paper. In recent years, several ink dating methods have been proposed. These methods have been based on the analysis of common ink solvents using gas chromatography/mass spectrometry (GC/MS) as the analytical platform. Despite these recent methods, several questions remain. The aim of this work was to develop an ink dating methodology (DATINK) for documents written by ballpoint pens based on the disappearance of volatile solvents from the ink entry. Multiple solid-phase microextraction (MHS-SPME) coupled to GC/MS was used to measure the solvents from ink entries made with four BIC^® ballpoint pens. The β parameter, the remaining fraction of the analyte in the system after one equilibration, corresponding to the successive extractions was considered for modelling a mathematical equation for later ink age dating. Preliminary tests of DATINK method showed that it was possible to detect the presence of ink solvents on documents up to the studied five years. The analyses of different real samples of known age were analyzed in terms of β values, which provided a mean relative error of 21%. The proposed use of β parameter for estimating the absolute age of ballpoint ink entries has shown promising results with a standard deviation of β ranging from 0.002 to 0.004.     

Update on the activities of the National Cooperation for Laboratory Accreditation

 The efforts to form a laboratory accreditation cooperation in the United States and North America are described, including activities of the Laboratory Accreditation Working Group and the interim board of the National Cooperation for Laboratory Accreditation. The vision, mission, and guiding principles developed by the two groups are presented, along with the operational documents, such as bylaws, the recognition document, guidance documents and the quality manual drafted by the interim board. Received: 8 June 1998 · Accepted: 16 June 1998     

如何撰写高质量化学领域专利申请文件

本文根据笔者在专利审查工作中的实际经验,对我国高等院校和科研机构在专利申请文件撰写中容易出现的问题进行了梳理,重点阐述了化学领域专利申请中常见的说明书公开不充分、权利要求中的非必要技术特征限定、技术术语缺少定义等问题,并分析了问题产生的原因,提出了相应的应对策略,以期能够帮助科研人员更加合理地撰写发明专利申请文件,使申请人的利益得到更好的保护。     

Blood banking quality: minimum requirements for TQM

In 1995, the Council of Europe published a guide with recommendations providing transfusion services with a set of guidelines and principles relating to the preparation, use and quality assurance of blood components. As a blood transfusion service is at the same time a supplier of blood products and a test laboratory the quality management system must include good medical practice, good manufacturing practice and good laboratory service, all of which are closely linked. We made a critical evaluation of the content of the guide and analysed requirements and recommendations in comparison with quality management systems applied by the concerned partners. As a major critic we observed that the guide does not take into account any quality system of the in vitro diagnostic (IVD) supplier and/or distributor. With the addition of some items outlined in ISO 25 and ISO 9000, the Council of Europe document can be improved so that it complies with internationally accepted quality management standard recommendations.     

Gamma radiation effects on physical properties of parchment documents: Assessment of Dmax

Parchments are important documents that give testimony for History; therefore these materials should be respected and preserved. Considering incremental biodeterioration problems that have to be faced daily, the Archive of the University of Coimbra (AUC) is involved in different scientific projects in order to evaluate and determine new methods for document decontamination and preservation.The aim of this study was to evaluate gamma radiation effects on the colour and texture of the AUC parchment documents. The assessment of these effects was used to estimate the maximum gamma radiation dose (D_max) that could guarantee parchment documents′ decontamination treatment, without significant alteration of their physical properties. Parchment samples were exposed to gamma radiation doses ranging from 10 to 30 kGy. The texture and colour of samples were assessed before and after the irradiation procedure, using a texture analyser and an electronic colorimeter. Hardness and springiness were determined based on texture spectra. Lightness (L?), Chroma (C), greenness vs. redness (a*) and yellowness vs. blueness (b*) values were obtained from colorimetric measures. Results indicate no significant effects of gamma radiation on the texture and colour of parchment for the studied doses.     

25 years of Science Citation Index--some experiences

Science Citation Index (SCI) depends for intellectual content entirely on citations by authors, who are sometimes prodded by editors and referees. Its patchiness is therefore not surprising, but frequently it gives access to relevant and up-to-date documents not easily accessible by other means. Two contrasting "citation families" are described. The first family, dealing with the various ascorbic acid derivatives having C substitution at C-2, actually retrieved very nearly all the relevant documents (other than patent specifications) that were retrieved by a CAS ONLINE substructure search. Organic chemists are clearly careful authors. The second family, dealing with amino acid residues covalently bound in soil organic matter, yielded documents having surprisingly little overlap with those retrieved by using a carefully devised Boolean "profile" on the general subject index of Chemical Abstracts. This was only partly because SCI is beset by language-barrier problems to which Chemical Abstracts is immune. The SCI management might extend its journal coverage, but otherwise improvement can only come from a more serious attitude to placing references in primary publications. SCI remains a complement to, not a substitute for, other data-bases.     

Utilization of statistical analysis of FT-IR spectra in forensic examination of paper

Studying of paper carriers of information has become increasingly important in forensic practice. This is caused by growing number of bogus or in other manner fraudulently alternated documents. An identification of individual paper sheets and studying their differences are the parts of forensic analysis of multiple sheets documents. This paper focuses on the possibilities of processing of mathematical and statistical data obtained by measurements of FT-IR spectral characteristics of individual paper sheets in a studied document. The spectral data were used to create data matrix which contains values of absorbance and interval of wavenumber. The method of differentiation is based on the comparison of maximum absorbance values within the range of wavenumbers from 1562 to 1215 cm^?1. This spectrum range is specific in occurrence of absorption bands that belong to calcium carbonate CaCO₃—an element of paper added into it in relatively high amounts in the form of filler which content or percentage occurrence may be different considering to the paper producer or production technology. Based on the above-said, the paper sheets originating from different producers or from various production technology units can be differentiated one from another using a robust statistical analysis.     

Towards interactive 3D graphics in chemistry publications

In this paper, we describe how it is possible to extend the visualization and publishing capabilities of the ubiquitous Adobe portable document format (PDF) from the static 2-dimensional (2D) pictures to interactive 3-dimensional (3D) models, 3D-PDF. Embedding 3D scenes of molecules and molecular properties into the electronic Computational Chemistry publications could be very important for visualization of complex molecular properties. No additional 3D-rendering software is required, because the 3D information has been already integrated within the PDF document, which can be displayed by any computer with up-to-date Adobe Acrobat software installed. We briefly describe a computer program, Jamberoo, which can be used for creating 3D-PDF documents and demonstrate several simple examples of integrated 3D models within the PDF. Finally, we show some possibilities of Acrobat JavaScript programming for creating dynamic 3D-PDF content with the elements of the Graphical User Interface (GUI).     

The quality-management system in research implemented in the food and food process quality research laboratory of the French Food Safety Agency

The French Food Safety Agency is a public body incorporating 12 laboratories that perform research to support expertise and public decisions taken in the fields of sanitary safety of food, animal health, and veterinary drugs. On the request of the General Management of the Agency a quality-management system in research (QMSR) is being implemented in the Food and Food Process Quality Research Laboratory. The experimental QMSR is based on existing standards and documents, describing the provisions required for scientific and technical competence, quality management, and project management. Furthermore, this QMSR also incorporates specific notions of great importance for research activities such as the positive and negative non-conformities, the non-confirmation of hypotheses, and the principle of evaluation of a research activity by peers for both quality and scientific aspects.