FSI 16-14-2 - Applicability of IMO Conventions to FPSOs and FSUs (International Transport W...) (1)
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高效液相色谱法测定固体食品中的安赛蜜刁玉华,张加稳,陈娴(昆明市食品药品检验所,昆明 650032)摘要:建立一种高效液相色谱法测定固体食品中安赛蜜的方法。
以水为提取溶剂超声波提取安赛蜜,然后在提取液中加入沉淀剂除杂,采用C18反相色谱柱,紫外检测器,以0.02mol/L乙酸铵溶液∶甲醇=90∶10(v/v)为流动相,检测波长225nm,流速1.0mL/min,柱温30℃,进样量10μL进行检测,外标法定量。
安赛蜜出峰时间为4.348min,样品的检出限为0.57mg/kg,定量限1.89mg/kg,线性范围为0.5~50.0μg/mL,相关系数0.9998,安赛蜜的加标回收率在91.3%~99.3%之间,重复性实验的相对标准偏差在2% 以下(n=6)。
建立的前处理方法具有简单、快速、准确、实用性强的特点,可用于固体食品中安赛蜜的检测。
关键词:安赛蜜;高效液相色谱;固体食品中图分类号:TS207.3/TS202.1 文献标识码:A 文章编号:1006-2513(2021)03-0090-05 doi:10.19804/j.issn1006-2513.2021.03.015Determination of acesulfame K in solid food byhigh performance liquid chromatographyDIAO Yu-hua,ZHANG Jia-wen,CHEN Xian(Kunming Institute for Food and Drag Control,Kunming 650032)Abstract:A high performance liquid chromatography for determination of acesulfame K in solid food was developed. Acesulfame K was extracted using water,assisted by ultrasound,and purified by precipitation. Zinc acetate and potassium ferrocyanide was used for preparation. Acesulfame K was separated on a C18 column using 0.02mol/L ammonium acetate methanol(90∶10,v/v)as mobile phase at a flow rate of 1.0mL/min and detected by ultraviolet detector at 225 nm. The column temperature was 30℃ and injection volume was 10μL. The quantitative detection was carried out by external standard. The retention time of acesulfame K was 4.348 min. The limit of detection was 0.57mg/ kg and limit of quantification was 1.89mg/kg. The linear range was between 0.5 and 50.0μg/mL with correlation coefficient of 0.9998. The mean spike recoveries for acesulfame K in a blank sample was between 91.3%and 99.3%,with a relative standard deviation below 2%(n=6) . The method was simple,rapid,accurate and practical. It can be used for determination of acesulfame K in solid food.Key words: acesulfame K;high performance liquid chromatography(HPLC);solid food安赛蜜,学名乙酰磺胺酸钾(Acesulfame-K)是一种健康新型高强度甜味剂。
MagMAX ™ FFPE DNA/RNA Ultra KitAutomated or manual isolation of total nucleic acid (TNA) from FFPE samples using AutoLys tubesCatalog Number A31881Pub. No. MAN0017538 Rev.A.0WARNING! Read the Safety Data Sheets (SDSs) and follow thehandling instructions. Wear appropriate protective eyewear,clothing, and gloves. Safety Data Sheets (SDSs) are available from /support .Product descriptionThe Applied Biosystems ™ MagMAX ™ FFPE DNA/RNA Ultra Kit is designed to isolate both DNA and RNA from the same section offormaldehyde- or paraformaldehyde-fixed, paraffin-embedded (FFPE)tissues. The kit also allows for flexibility to isolate DNA only, RNA only or total nucleic acid (TNA). The kit uses MagMAX ™ magnetic-bead technology, ensuring reproducible recovery of high-quality nucleic acid through manual or automated processing. The isolated nucleic acid is appropriate for use with a broad range of downstream assays, such as quantitative real-time RT-PCR and next-generation sequencing.In addition to the use of traditional solvents, the kit is compatible with Autolys M tubes that enable a faster and more convenient means of deparaffinizing FFPE samples by eliminating the need for organic solvents such as xylene or CitriSolv and ethanol. Samples are put into the tubes for protease digestion, tubes are lifted with the Auto-pliers or Auto-Lifter and then samples are spun down. The wax and debris are contained in the upper chamber while the lysate is passed through.Afterwards, the clarified lysate can be directly purified with the MagMAX ™ FFPE DNA/RNA Ultra Kit.For guides without using AutoLys M tubes for sequential DNA and RNA isolation, or DNA isolation, or RNA isolation only, seeMagMAX ™ FFPE DNA/RNA Ultra Kit User Guide (sequential DNA/RNA isolation) (Pub. No. MAN0015877), or MagMAX ™ FFPE DNA/RNA Ultra Kit User Guide (DNA isolation only) (Pub. No. MAN0015905), or MagMAX ™ FFPE DNA/RNA Ultra Kit User Guide (RNA isolation only)(Pub. No. MAN0015906), respectively.This guide describes isolation of TNA from FFPE tissue blocks or FFPE slides using AutoLys M tubes. Three optimized methods for sections or curls both up to 40 µm using AutoLys M tubes are included:•Manual sample processing.•KingFisher ™ Flex Magnetic Particle Processor with 96 Deep-Well Head (DW96; 96-well deep well setting).•KingFisher ™ Duo Prime Magnetic Particle Processor (12-well deep well setting).For sequential DNA and RNA isolation, or DNA isolation, or RNA isolation only, see MagMAX ™ FFPE DNA/RNA Ultra Kit User Guide (sequential DNA/RNA isolation) (Pub. No. MAN0017541), MagMAX ™FFPE DNA/RNA Ultra Kit User Guide (DNA isolation only)(Pub. No. MAN0017539), or MagMAX ™ FFPE DNA/RNA Ultra Kit User Guide (RNA isolation only) (Pub. No. MAN0017540), respectively.Contents and storageReagents provided in the kit are sufficient for 48 TNA isolations from sections up to 40 µm with the AutoLys workflow.Table 1 MagMAX ™ FFPE DNA/RNA Ultra Kit (Cat. No. A31881)Additional reagents are available separately; Protease Digestion Buffer, Binding Solution, and DNA Wash Buffer are also available as Cat. No. A32796. [2]Shipped at room temperature. [3]Not used in TNA workflow[4]Final volume; see “Isolate TNA“ on page 4.Required materials not suppliedUnless otherwise indicated, all materials are available through . MLS: Fisher Scientific ( ) or other major laboratory supplier.Table 2 Materials required for nucleic acid isolation (all methods)Table 3 Additional materials required for manual isolationTable 4 Additional materials required for automated isolationIf needed, download the KingFisher ™ Duo Prime or Flex programThe programs required for this protocol are not pre-installed on theKingFisher ™Duo Prime Magnetic Particle Processor or on theKingFisher ™Flex Magnetic Particle Processor 96DW.1.On the MagMAX ™ FFPE DNA/RNA Ultra Kit product web page,scroll down to the Product Literature section.2.Right-click on the appropriate program file(s) for your samplesize to download the program to your computer:3.4.Refer to the manufacturer's documentation for instructions forinstalling the program on the instrument.Procedural guidelines•Perform all steps at room temperature (20–25°C) unless otherwise noted.•When mixing samples by pipetting up and down, avoid creating bubbles.•When working with RNA:–Wear clean gloves and a clean lab coat.–Change gloves whenever you suspect that they are contaminated.–Open and close all sample tubes carefully. Avoid splashing or spraying samples.–Use a positive-displacement pipettor and RNase-free pipette tips.–Clean lab benches and equipment periodically with an RNase decontamination solution, such as RNase Zap ™ Solution (Cat.No. AM9780).•Incubation at 60°C can be extended overnight to increase DNA yields, followed by incubation at 90°C for 1 hour.•Volumes for reagent mixes are given per sample. We recommend that you prepare master mixes for larger sample numbers. To calculate volumes for master mixes, refer to the per-well volume and add 5–10% overage.Before you beginBefore first use of the kit•Prepare the Wash Solutions from the concentrates:–Add 46 mL of isopropanol to RNA Wash Buffer Concentrate ,mix, and store at room temperature.–Add 168 mL of ethanol to Wash Solution 2 Concentrate , mix,and store at room temperature.Before each use of the kit•Equilibrate the Nucleic Acid Binding Beads to room temperature.•Pre-heat the incubators or ovens to 60°C and 90°C.•Prepare the following solutions according to the following tables.Table 5 Protease solutionTable 6 TNA Binding BufferPrepare the FFPE samples•For curls from FFPE tissue blocks: proceed to “Prepare the curls from FFPE tissue blocks“ on page 3.•For FFPE slide-mounted sections: proceed to “Prepare samples from FFPE slides“ on page 3.Prepare the curls from FFPE tissue blocksa.Cut sections from FFPE tissue blocks using a microtome.Note: For miRNA extraction, we recommend using sections of 10 µm or thicker.b.Collect each section in an AutoLys M tube.1Section FFPE tissue blocks a.Add 235 µL of the Protease Solution (see Table 5).Note: If working with curls, they might stick straight up so make sure to submerge samples in theProtease Solution with a tip or a 1 mL syringe plunger or do a quick spin down at 3000 rpm for 1 minute prior to the addition of buffer to collapse the curl. Time may be extended.b.Incubate at 60°C for 1 hour or longer.Note: Use the AutoLys racks and place in an incubator or oven.c.Incubate at 90°C for 1 hour.Note: For automated isolation, set up the processing plates during the incubation.·For isolation using KingFisher ™ Duo Prime Magnetic Particle Processor, proceed to “Set up the processing plate“ on page 4.·For isolation using KingFisher ™ Flex Magnetic Particle Processor 96DW, proceed to “Set up the TNA processing plates“ on page 5.2Digest with Protease a.Allow samples to cool down for 3–5 minutes before proceeding to lift the tubes.e the Auto-plier for individual tube lifting or the Auto-lifter for multiple tube lifting of up to 24 tubes.c.Lock the tubes in position by hand or use the locking lid.d.Centrifuge at 2000 × g for 10 minutes in a benchtop centrifuge with plate adapters.e.Unlock the tubes by hand or remove the locking lid.e the Auto-plier or Auto-lifer to lift the inner tube for sample access.g.Proceed to purification. See “Isolate TNA“ on page 43Lift the tubesPrepare samples from FFPE slidesa.Pipet 2–4 µL of Protease Digestion Buffer depending on the tissue size evenly across the FFPE tissuesection on the slide to pre-wet the section.Note: You can adjust the volume of Protease Digestion Buffer if the tissue is smaller or larger.b.Scrape the tissue sections in a single direction with a clean razor blade or scalpel, then collect the tissueon the slide into a cohesive mass.c.Transfer the tissue mass into an AutoLys M tube with the scalpel or a pipette tip.d.Add 235 µL of the Protease Solution (see Table 5).Note: Be sure to submerge samples in the Protease Solution with a tip or a 1 mL syringe plunger e.Incubate at 60°C for 1 hour or longer.Note: Use the AutoLys racks and place in an incubator or oven.f.Incubate at 90°C for 1 hour.Note: For automated isolation, set up the processing plates during the incubation.·For isolation using KingFisher ™ Duo Prime Magnetic Particle Processor, proceed to “Set up the processing plate“ on page 4.·For isolation using KingFisher ™ Flex Magnetic Particle Processor 96DW, proceed to “Set up the TNA processing plates“ on page 5.4Scrape the samples and digest with Proteasea.Allow samples to cool down for 3–5 minutes before proceeding to lift the tubes.e the Auto-plier for individual tube lifting or the Auto-lifter for multiple tube lifting of up to 24 tubes.c.Lock the tubes in position by hand or use the locking lid.d.Centrifuge at 2000 × g for 10 minutes in a benchtop centrifuge with plate adapters.e.Unlock the tubes by hand or remove the locking lid.e the Auto-plier or Auto-lifer to lift the inner tube for sample access.g.Proceed to purification. See “Isolate TNA“ on page 45Lift the tubesIsolate TNA•To isolate TNA manually, proceed to “Isolate TNA manually“ on page 4.•To isolate TNA using the KingFisher ™Duo Prime Magnetic Particle Processor, proceed to “Isolate TNA using KingFisher ™ Duo Prime Magnetic Particle Processor“ on page 4.•To isolate TNA using the KingFisher ™Flex Magnetic Particle Processor 96DW, proceed to “Isolate TNA using KingFisher ™ Flex Magnetic Particle Processor 96DW“ on page 5.Isolate TNA manuallyUse microcentrifuge tubes to perform manual TNA isolations.a.After the Protease digestion is complete, add 20 µL of Nucleic Acid Binding Beads to the samples.b.Add 900 µL of TNA Binding Buffer (see Table 6) to the sample.c.Shake for 5 minutes at speed 10 or 1150 rpm.d.Place the sample on the magnetic stand for 2 minutes or until the solution clears and the beads are pelleted against the magnet.e.Carefully discard the supernatant with a pipette.1Bind the TNA to beadsa.Wash the beads with 500 µL of RNA Wash Buffer.b.Shake for 1 minute at speed 10 or 1150 rpm until the mixture is thoroughly chocolate brown in color.c.Place the sample on the magnetic stand for 2 minutes or until the solution clears and the beads arepelleted against the magnet.d.Carefully discard the supernatant with a pipette.e.Repeat steps a-d.f.Wash the beads with 500 µL of Wash Solution 2.g.Shake for 1 minute at speed 10 or 1150 rpm until the mixture is thoroughly chocolate brown in color.h.Place the sample on the magnetic stand for 2 minutes or until the solution clears and the beads arepelleted against the magnet.i.Carefully discard the supernatant with a pipette.j.Repeat steps f-i.k.Shake for 1–2 minutes at speed 10 or 1150 rpm to dry the beads.Do not over-dry the beads. Over-dried beads results in low TNA recovery yields.2Wash TNA on the beadsa.Add 50 µL of Elution Solution to the beads.b.Shake for 5 minutes at speed 10 or 1150 rpm and at 55°C until the mixture is thoroughly chocolatebrown in color.c.Place the sample on the magnetic stand for 2 minutes or until the solution clears and the beads arepelleted against the magnet.The supernatant contains the purified TNAThe purified TNA is ready for immediate use. Store at –20°C or –80°C for long-term storage.3Elute the TNAIsolate TNA using KingFisher ™ Duo Prime Magnetic Particle ProcessorDuring the protease incubation, add processing reagents to the wells of a MagMAX ™ Express-96 Deep WellPlate as indicated in the following table.Table 7 TNA plate setupRow on the MagMAX ™ Express-96 Deep Well Plate.4Set up the processing plate a.Ensure that the instrument is set up for processing with the deep well 96–well plates and select theappropriate program A31881_DUO_large_vol_TNA on the instrument.b.At the end of the protease incubation, add 200 µL of sample to each well in Row G of the TNA plate.c.Add 20 µL of Nucleic Acid Binding Beads to each sample well in Row G.d.Start the run and load the prepared processing plates when prompted by the instrument.5Bind, wash, rebind, and elute the TNA5Bind, wash, rebind,and elute the TNA(continued)e.At the end of the run, remove the Elution Plate from the instrument and transfer the eluted TNA(Row A of TNA plate) to a new plate and seal immediately with a new MicroAmp ™ Clear Adhesive Film.IMPORTANT! Do not allow the purified samples to sit uncovered at room temperature for more than 10minutes, to prevent evaporation and contamination.The purified TNA is ready for immediate use. Store at –20°C or –80°C for long-term storage.Isolate TNA using KingFisher ™ Flex Magnetic Particle Processor 96DWDuring the protease incubation, add processing reagents to the wells of MagMAX ™ Express-96 Plates asindicated in the following table.Table 8 TNA plates setupPosition on the instrument6Set up the TNA processing platesa.Ensure that the instrument is set up for processing with the deep well magnetic head and select theA31881_FLEX_large_vol_TNA program on the instrument.b.At the end of the protease incubation, add 200 µL of sample to each well in Plate 1.c.Add 20 µL of Nucleic Acid Binding Beads to each sample well in Plate 1.d.Start the run and load the prepared processing plates in their positions when prompted by theinstrument (see “Set up the TNA processing plates“ on page 5).e.At the end of the run, remove the Elution Plate from the instrument and seal immediately with a newMicroAmp ™ Clear Adhesive Film.IMPORTANT! Do not allow the purified samples to sit uncovered at room temperature for more than 10minutes, to prevent evaporation and contamination.The purified TNA is ready for immediate use. Store at –20°C or –80°C for long-term storage. .7Bind, wash, rebind, and elute the TNALimited product warrantyLife Technologies Corporation and/or its affiliate(s) warrant their products as set forth in the Life Technologies' General Terms and Conditions of Sale found on Life Technologies' website at /us/en/home/global/terms-and-conditions.html . If you have any questions,please contact Life Technologies at /support .Manufacturer: Life Technologies Corporation | 2130 Woodward Street | Austin, TX 78744The information in this guide is subject to change without notice.DISCLAIMER : TO THE EXTENT ALLOWED BY LAW, LIFE TECHNOLOGIES AND/OR ITS AFFILIATE(S) WILL NOT BE LIABLE FOR SPECIAL, INCIDENTAL, INDIRECT, PUNITIVE,MULTIPLE, OR CONSEQUENTIAL DAMAGES IN CONNECTION WITH OR ARISING FROM THIS DOCUMENT, INCLUDING YOUR USE OF IT.Important Licensing Information : This product may be covered by one or more Limited Use Label Licenses. By use of this product, you accept the terms and conditions of all applicable Limited Use Label Licenses.©2018 Thermo Fisher Scientific Inc. All rights reserved. All trademarks are the property of Thermo Fisher Scientific and its subsidiaries unless otherwise specified./support | /askaquestion 。
MAC4LDFpis Rev 04/221Product InformationMetaPolyzyme, DNA freeSuitable for Microbiome researchMAC4LDFSynonym: Multilytic Enzyme Mix Storage Temperature –20 °CProduct DescriptionMetagenomics investigates all DNA that has been isolated directly from given single samples, such as environmental samples or biological organisms.1,2Metagenomics allows for the investigation of microbes that exist in extreme environments, and which have been historically difficult to isolate, culture, andstudy.3 Metagenomics has revealed the existence of novel microbial species.4 Applications ofmetagenomics work include public health dataanalysis,5,6 discovery of novel proteins, enzymes and natural products,7,8 environmental studies,9,10 and agricultural investigations.11,12Microbes are difficult to disrupt because the cell walls may form capsules or resistant spores. DNA can be extracted by using lysing enzymes such as lyticase, chitinase, zymolase, and gluculase to induce partial spheroplast formation. Spheroplasts are subsequently lysed to release DNA.MetaPolyzyme products (Cat. Nos. MAC4L, MAC4LDF) are based on a multi-lytic enzyme mixture, originally developed by Scott Tighe, for use in microbiome and DNA extraction efficiency studies, and formulated for effective lysis of microbiome samples from extreme environments. MetaPolyzyme was originally evaluated and developed in consultation and collaboration with the Association of Biomolecular Resource Facilities (ABRF) Metagenomics and Microbiome ResearchGroup (MMRG; formerly the Metagenomics Research Group, MGRG).13-16Studies of microbial communities have beenenhanced by the use of culture-independent analytical techniques such as 16S rRNA gene sequencing and metagenomics. DNA contamination during sample preparation is a major problem of sequence-based approaches. Extraction reagents free of DNA contaminants are thus essential. MetaPolyzyme, DNA free was developed to address the need for DNA-free reagents, to minimize microbial DNA contamination from reagents. This productundergoes strict quality control testing to ensure the absence of detectable levels of contaminatingmicrobial DNA using 35 cycles PCR amplification of 16S and 18S rDNA using universal primer sets.Precautions and DisclaimerFor R&D use only. Not for drug, household, or other uses. Please consult the Safety Data Sheet for information regarding hazards and safe handling practices.ReagentThe enzymes in MetaPolyzyme, DNA free are:• Mutanolysin • Achromopeptidase • Lyticase • Chitinase • Lysostaphin •LysozymeAll the enzymes are individually tested for theabsence of contaminating DNA using 16S and 18S PCR amplification.Mutanolysin (from Streptomyces globisporus )Mutanolysin is a muralytic enzyme (muramidase) that cleaves the β-N -acetylmuramyl-(1→4)-N -acetylglucosamine linkage of the bacterial cell wall peptidoglycan-polysaccharide, particularly the β(1→4) bond in MurNAc-GlcNAc.17 Mutanolysin particularly acts on many Gram-positive bacteria, where the enzyme’s carboxy -terminal moietiesparticipate in the recognition and binding of unique cell wall structures.MAC4LDFpis Rev 04/22AchromopeptidaseAchromopeptidase (known also as β-lytic protease 18) has potent bacteriolytic activity on many Gram-positive aerobic bacteria 19 with high lytic activity, against bacterial strains with the A1α chemotype (such as Aerococcus viridans ), and the A3αchemotype (such as Staphylococcus epidermidis ) for cell wall peptidoglycan structures. The enzyme has been reported to have particular recognition for Gly-X sites in peptide sequences, and for Gly-Gly and ᴅ-Ala-X sites in peptidoglycans.20Lyticase (from Arthrobacter luteus )Lyticase is useful in digestion of linear glucosepolymers with β(1→3) linkages, of yeast glycan coats and for spheroplast formation, and of the cell wall of active yeast cells.Chitinase (from Streptomyces griseus )Chitinase degrades chitin by enzymatic hydrolysis to N-acetyl-D-glucosamine. Degradation occurs via two consecutive enzyme reactions: •Chitodextrinase-chitinase, apoly(1,4-β-[2-acetamido-2-deoxy-D-glucoside])-glycanohydrolase, removes chitobiose units from chitin.•N-acetylglucosaminidase-chitobiase cleaves the disaccharide to its monomer subunits, N-acetyl-D-glucosamine (NAGA).Lysostaphin (from Staphylococcus staphylolyticus )Lysostaphin is a lytic enzyme with activity against Staphylococcus species, including S. aureus . Lysostaphin has hexosaminidase, amidase, and endopeptidase activities. It cleaves polyglycine crosslinks in the cellular wall of Staphylococcus species, which leads to cell lysis.21,22Lysozyme (from chicken egg white)Lysozyme hydrolyzes β(1→4) linkages betweenN -acetylmuraminic acid and N -acetyl-D-glucosamine residues in peptidoglycan, and betweenN -acetyl-D-glucosamine residues in chitodextrin. Lysozyme lyses the peptidoglycan cell wall of Gram-positive bacteria.23Storage/StabilityThis product ships at cooler temperature conditions. Long-term storage at –20 °C is recommended. Reconstituted solutions of MetaPolyzyme, DNA free may be stored at –20 °C, but long-term solution stability has not been examined.Preparation InstructionsBecause of the great diversity of samples formetagenomics studies, it will be necessary for each researcher to work out particular conditions for optimal sample preparation and treatment. It is recommended to reconstitute MetaPolyzyme, DNA free in sterile PBS buffer, pH 7.5 (no EDTA, calcium or magnesium present in solution). The following is a sample procedure, to be scaled appropriately:1. Add 100 µL of sterile PBS (pH 7.5) to 1 vial ofMetaPolyzyme, DNA free.1.1. Resuspend by gentle agitation or pipetting. 1.2. Set solution aside at 2-8 °C until Step 7. 2. Thoroughly suspend sample in sterile PBS(pH 7.5). 3. Add 200 µL of sample in PBS to a 2 mLpolypropylene microcentrifuge tube. 4. Optional pellet wash:4.1. To sample tube, add 1 mL of PBS (pH 7.5). 4.2. Vortex, centrifuge and remove supernatant. 4.3. Repeat pellet wash two more times ifneeded. 5. Resuspend pelleted sample in 150 µL of PBS(pH 7.5). Vortex thoroughly.6. Optional: if solution will sit for more than 4 hours,sodium azide may be added to 0.02%. 7. Add 20 µL (*) of MetaPolyzyme, DNA free tosample solution. 8. Incubate at 35 °C for 2-24 hours.9. Continue with standard DNA extraction protocol. (*) The optimal volume and concentration of MetaPolyzyme, DNA free may vary in different experiments.References1. Gilbert, J.A., and Dupont, C.L., Ann. Rev. MarineSci., 3, 347-371 (2011). 2. Kang, H.S., and Brady, S.F., J. Am. Chem. Soc.,136(52), 18111-18119 (2014). 3. Ufarté, L. et al., Biotechnol. Adv., 33(8),1845-1854 (2015). 4. Davison, M. et al., Photosynth. Res., 126(1),135-146 (2015). 5. Afshinnekoo, E. et al., Cell Syst., 1(1), 72-87(2015).The life science business of Merck operatesas MilliporeSigma in the U.S. and Canada.Merck and Sigma-Aldrich are trademarks of Merck KGaA, Darmstadt, Germany or its affiliates.All other trademarks are the property of their respective owners. Detailed information on trademarks is available via publicly accessible resources.© 2022 Merck KGaA, Darmstadt, Germany and/or its affiliates. All Rights Reserved.MAC4LDFpis Rev 04/22 DK,DT,GCY,TJ,RBG,SBC,MAM36.The MetaSUB International Consortium,Microbiome, 4, 24 (2016). [Erratum inMicrobiome, 4, 45 (2016).]7.Trinidade, M. et al., Front. Microbiol., 6, 890(2015).8.Coughlan, L.M. et al., Front. Microbiol., 6, 672(2015).9.Palomo, A. et al., ISME J., 10(11), 2569-2581(2016).10.Pold, G. et al., Appl. Environ. Microbiol., 82(22),6518-6530 (2016).11.Mitra, N. et al., J. Gen. Virol., 97(8), 1771-1784(2016).12.Theuns, S. et al., Infect. Genet. Evol., 43,135-145 (2016).13.Baldwin, D.A. et al., "Life at the Extreme", ABRFMetagenomics Research Group Poster 2015,presented at the ABRF 2015 Conference, St.Louis, MO, USA, March 28-31, 2015.14.Baldwin, D.A. et al., "Implementing NewStandards in Metagenomics and the ExtremeMicrobiome Project", ABRF MetagenomicsResearch Group Poster 2016, presented at theABRF 2016 Conference, Fort Lauderdale, FL, USA, February 20-23, 2016.15.McIntyre, A. et al., "Life at the Extreme: TheABRF Metagenomics Research Group", ABRFMetagenomics Research Group Poster 2017,presented at the ABRF 2017 Conference, SanDiego, CA, March 25-28, 2017.16.Tighe, S. et al., J. Biomol. Tech., 28(1), 31-39(2017).17.Gründling, A., and Schneewind, O., J. Bacteriol.,188(7), 2463-2472 (2006).18.Li, S.L. et al., J. Bacteriol., 172(11), 6506-6511(1990).19.Ezaki, T., and Suzuki, S., J. Clin. Microbiol.,16(5), 844-846 (1982). 20.Li, S. et al., J. Biochem., 124(2), 332-339(1998).21.Browder, H.P. et al., Biochem. Biophys. Res.Commun., 19, 383-389 (1965).22.Robinson, J.M. et al., J. Bacteriol., 137(3),1158-1164 (1979).23.Vocaldo, D.J. et al., Nature, 412(6849), 835-838(2001).NoticeWe provide information and advice to our customers on application technologies and regulatory matters to the best of our knowledge and ability, but without obligation or liability. Existing laws and regulations are to be observed in all cases by our customers. This also applies in respect to any rights of third parties. Our information and advice do not relieve our customers of their own responsibility for checking the suitability of our products for the envisaged purpose. The information in this document is subject to change without notice and should not be construed as a commitment by the manufacturing or selling entity, or an affiliate. 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metal-organic compoundsm328#2003International Union of CrystallographyDOI:10.1107/S0108270103011703Acta Cryst.(2003).C 59,m328±m330Ferrocene compounds.XXXIX.11-FerrocenylisochromaneMario Cetina,a Senka akovicÂ,b Vladimir Rapic Âb *and Amalija GolobicÏc aFaculty of Textile Technology,University of Zagreb,Pierottijeva 6,HR-10000Zagreb,Croatia,b Laboratory of Organic Chemistry,University of Zagreb,Faculty of Food Technology and Biotechnology,Pierottijeva 6,HR-10000Zagreb,Croatia,and cLaboratory of Inorganic Chemistry,Faculty of Chemistry and Chemical Technology,University of Ljubljana,PO Box 537,SI-1001Ljubljana,Slovenia Correspondence e-mail:*************Received 14April 2003Accepted 27May 2003Online 22July 2003In the title compound,[Fe(C 5H 5)(C 14H 13O)],the plane of the heterocyclic ring is almost perpendicular to the plane of the substituted cyclopentadienyl ring,and the heterocyclic ring adopts a half-chair conformation.The conformation of the nearly parallel cyclopentadienyl (Cp)rings [the dihedral angle between their planes is 2.7(1) ]is almost halfway between eclipsed and staggered,and the rings are mutually twisted by about 19.4(2) (mean value).The mean lengths of the CÐC bonds in the substituted and unsubstituted cyclopentadienylring are 1.420(2)and 1.406(3)AÊ,respectively,and the FeÐC distances range from 2.029(2)to 2.051(2)AÊ.The phenyl and unsubstituted cyclopentadienyl rings are involved in CÐH ÁÁÁ%interactions,with intermolecular H ÁÁÁcentroiddistances of 2.85and 3.14AÊfor CÐH ÁÁÁ%(Ph),and 2.88A Êfor CÐH ÁÁÁ%(Cp).In two of these interactions,the CÐH bond points towards one of the ring bonds rather than towards the ring centroid.In the crystal structure,the CÐH ÁÁÁ%interactions connect the molecules into a three-dimensional framework.CommentOptically active ferrocene derivatives are widely employed as chiral ligands in asymmetric reactions,and there is continuing interest in the development of ef®cient procedures for the preparation of these derivatives in enantiopure forms (Gonsalves &Chen,1995;Bolm et al.,1998;Pioda &Togni,1998;Perea et al.,1999).Ferrocene derivatives exhibiting centro-and planar chirality are very convenient substrates forbiotransformations (KoÈllner et al.,1998;Richards &Locke,1998;Schwink &Knochel,1998;Patti &Nicolosi,1999;akovicÂet al.,2003).In the course of our research on enzyme-catalyzed resolution of centrochiral ferrocene compounds,racemic 2-( -hydroxyferrocenyl)benzenethanol and 1-ferro-cenylisochromane,(I),were prepared by reduction of methyl2-(ferrocenoyl)benzeneacetate ( akovicÂ,2000).The molecular structure of (I)is the ®rst reported structure to contain an isochromanyl group attached to the ferrocenyl moiety (Fig.1).Moreover,the Cambridge Structural Database (Allen,2002)lists only three structures containing an iso-chromanyl group at all (Yamato et al.,1984;Unterhalt et al.,1994;Eikawa et al.,1999).The heterocyclic six-membered ringActa Crystallographica Section CCrystal Structure CommunicationsISSN0108-2701Figure 2Part of the crystal structure of (I),showing the formation of (010)sheets built from C14ÐH14A ÁÁÁCg 1i and C18ÐH18ÁÁÁCg 2ii interactions (Cg 1and Cg 2are the centroids of rings C12/C13/C16±C19and C6±C10,respectively).CÐH ÁÁÁ%interactions are indicated by dashed lines.[Symmetry codes:(i)x ,12Ày ,z À12;(ii)1+x ,y ,1+z.]Figure 1A view of (I),with the atom-numbering scheme.Displacement ellipsoids for non-H atoms are drawn at the 20%probability level.1Part XXXVIII:Cetina et al.(2003).adopts a distorted half-chair conformation,in which atoms O1and C15are 0.426(1)and À0.348(2)AÊfrom the plane of the other ring atoms (C11±C14);the C11ÐC12ÐC13ÐC14torsion angle is 2.4(2) .The bond lengths in the heterocyclic and fused phenyl rings (Table 1)mostly agree with the equivalent bond lengths in the structures of 1,1H -oxybis(iso-chromane)(Eikawa et al.,1999)and (S )-1-(phenyl)ethyl-ammonium (S )-isochromane-1-carboxylate (Unterhalt et al.,1994).The exception is the C12ÐC13bond,which is shorter($0.04AÊ)in the latter structure.Heterocyclic ring atoms O1,C11and C15and cyclopentadienyl (Cp)ring atom C1lie in the same plane,the C15ÐO1ÐC11ÐC1torsion angle being 178.95(14) .The dihedral angle between the mean plane of these four atoms and the C1±C5Cp ring is 47.8(1) .Furthermore,the plane of the heterocyclic ring is almost perpendicular to the plane of the C1±C5ring and is parallel to the plane of the fused phenyl ring.The corresponding dihedral angles are 87.3(1)and 4.0(1) .The exocyclic C2ÐC1ÐC11bond angle is larger than the C5ÐC1ÐC11angle (Table 1).The Cp rings are planar and almost parallel to each other [the dihedral angle between their planes is 2.7(1) ],and the FeÐC distances are in the range2.034(2)±2.051(2)AÊfor the substituted (C1±C5)and 2.029(2)±2.049(2)AÊfor the unsubstituted (C6±C10)ring,the average values being 2.042(2)and 2.038(2)AÊ,respectively.The CÐC bonds are slightly longer in the substituted ring than in the unsubstituted ring [1.410(3)±1.429(2)versus 1.397(3)±1.414(3)AÊ],and the bond angles in both rings range from 107.52(15)to 108.33(18) .The geometry of the ferrocenyl moiety agrees well with the structures of ferrocene (Seiler &Dunitz,1979)and of theferrocene derivatives we have reported previously (Cetina et al.,2002,2003).The main conformational difference was observed in the orientation of the Cp rings.In (I),the rings are twisted from an eclipsed conformation by 19.4(2) (mean value).The values of the corresponding CÐCg 3ÐCg 2ÐC pseudo-torsion angles (Cg 3and Cg 2are the centroids of the C1±C5and C6±C10rings,respectively),de®ned by joining two eclipsing Cp C atoms through the ring centroids,range from 19.0(2)to 19.7(2) .The conformation is almost exactly halfway between eclipsed and staggered,as demonstrated by the C1ÐCg 3ÐCg 2ÐC9torsion angle of 163.4(1) .This angle would be 180 for a staggered conformation and 144 for a fully eclipsed conformation.The centroids of the Cp rings are almost equidistant from the Fe atom;the FeÐCg 3and FeÐCg 2distances are 1.647(1)and 1.650(1)AÊ,respectively,while the Cg 3ÐFeÐCg 2angle is 178.2(1) .There are a number of CÐH ÁÁÁ%interactions (Table 2and Fig.2).Atom H14A of the heterocyclic ring is positioned almost perpendicularly above the phenyl-ring centroid (Cg 1)of the adjacent molecule.The six relevant H ÁÁÁC distances fallin the narrow range 3.06±3.28AÊ,and the H ÁÁÁCg i distance is signi®cantly shorter than any of the H ÁÁÁC distances[symmetry code:(i)x ,12Ày ,z À12;Table 2].The CÐH ÁÁÁ%interaction between phenyl atom H18and the unsubstituted Cp ring exhibits a completely different geometry.The H18ÁÁÁC7ii distance is shorter than the H ÁÁÁCg ii distance [symmetry code:(ii)1+x ,y ,1+z ].The second shortest H ÁÁÁC contact is that to atom C6,and the CÐH bond points towards the C6ÐC7bond of the Cp ring rather than towards the ring centroid (Cg 2).Similarly,the longest interaction,C5ÐH5ÁÁÁCg 1iii [symmetry code:(iii)1Àx ,Ày ,2Àz ],points towards the C12ÐC13bond.Both the H5ÁÁÁC12iii and the H5ÁÁÁC13iii contacts are shorter than the H ÁÁÁCg iii distance.The molecules linked by these CÐH ÁÁÁ%interactions build a three-dimensional framework (Fig.3).ExperimentalNaBH 4(253mg,6.7mmol)was added gradually to a solution of methyl 2-(ferrocenoyl)benzeneacetate (326mg,0.9mmol)in a mixture of EtOH and Et 2O (1:1v /v ;5ml).The mixture was re¯uxed for 2h and worked up in the usual manner.Separation by preparative thin-layer chromatography on silica gel (Merck,Kieselgel 60HF 254)yielded 2-( -hydroxyferrocenyl)benzeneethanol (237mg;yield 78%)and orange crystals of 1-ferrocenylisochromane (57mg;yield 20%;m.p.365±366K).Single crystals of the title compound were obtained by slow evaporation from a cyclohexane solution at room tempera-ture.IR (CH 2Cl 2,cm À1):)3081(w )and 3020(w )(CÐH,ferrocene),2942(m )(CÐH,aliphatic),1278(m )(CÐOÐC);1H NMR (DMSO,p.p.m.): 7.18(d ,1H,H16),7.12(d ,1H,H17),7.14(d ,1H,H18),7.16(d ,1H,H19),4.23(s ,5H,unsubstituted ferrocene ring),4.13±4.20(m ,4H,substituted ferrocene ring),3.97(m ,1H,H15A ),3.77(m ,1H,H15B ),2.78(m ,2H,H14),5.58(s ,1H,H11);13C NMR (DMSO,p.p.m.): 137.29(C12),132.91(C13),128.5(C17),126.25(C18),125.98(C16),125.36(C19),90.21(C1),73.63(C11),68.62(unsub-stituted ferrocene ring),68.56±66.31(substituted ferrocene ring),61.55(C15),27.99(C14).Acta Cryst.(2003).C 59,m328±m330Mario Cetina et al.[Fe(C 5H 5)(C 14H 13O)]m329metal-organic compoundsFigure 3Part of the crystal structure of (I),showing the cyclic motif generated by the C5ÐH5ÁÁÁCg 1iii interaction (Cg 1is the centroid of ring C12/C13/C16±C19),which links the (010)sheets into a three-dimensional framework.CÐH ÁÁÁ%interactions are indicated by dashed lines,and the unit-cell box has been omitted for clarity.[Symmetry code:(iii)1Àx ,Ày ,2Àz .]metal-organic compoundsm330Mario Cetina et al.[Fe(C 5H 5)(C 14H 13O)]Acta Cryst.(2003).C 59,m328±m330Crystal data[Fe(C 5H 5)(C 14H 13O)]M r =318.18Monoclinic,P 21a ca =11.5053(2)A Êb =18.5095(3)A Êc =7.1941(1)AÊ =106.933(1)V =1465.62(4)AÊ3Z =4D x =1.442Mg m À3Mo K radiationCell parameters from 3411re¯ections =2.6±27.5 "=1.02mm À1T =293(2)K Prism,orange0.80Â0.40Â0.15mm Data collectionNonius KappaCCD area-detector diffractometer 9and 3scansAbsorption correction:multi-scan (DENZO±SMN ;Otwinowski &Minor,1997)T min =0.630,T max =0.85716885measured re¯ections3334independent re¯ections 2662re¯ections with I >2'(I )R int =0.064 max =27.4 h =À14314k =À23323l =À939Re®nementRe®nement on F 2R [F 2>2'(F 2)]=0.030wR (F 2)=0.076S =1.033334re¯ections 190parametersH-atom parameters constrainedw =1/['2(F 2o )+(0.0341P )2+0.3545P ]where P =(F 2o +2F 2c )/3(Á/')max =0.001Á&max =0.25e A ÊÀ3Á&min =À0.23e AÊÀ3All H atoms were included in calculated positions as riding atoms,with SHELXL 97(Sheldrick,1997)defaults viz.CÐH =0.93AÊfor aromatic H atoms,0.98AÊfor methine H atoms,and 0.97A Êfor methylene H atoms.For all H atoms,the isotropic displacement parameters were set at 1.2times the equivalent anisotropic displacement parameters of the attached non-H atoms.Data collection:COLLECT (Nonius,2000);cell re®nement:DENZO±SMN (Otwinowski &Minor,1997);data reduction:DENZO±SMN ;program(s)used to solve structure:SHELXS 97(Sheldrick,1997);program(s)used to re®ne structure:SHELXL 97(Sheldrick,1997);molecular graphics:PLATON (Spek,2003);soft-ware used to prepare material for publication:SHELXL 97.The re¯ection data were collected at the Faculty of Chem-istry and Chemical Technology,University of Ljubljana,Slovenia.We acknowledge with thanks the ®nancial contri-bution of the Ministry of Education,Science and Sport of the Republic of Slovenia (grant Nos.X-2000and PS-511-103),which made the purchase of the apparatus possible.Supplementary data for this paper are available from the IUCr electronic archives (Reference:GD1251).Services for accessing these data are described at the back of the journal.ReferencesAllen,F.H.(2002).Acta Cryst.B 58,380±388.Bolm,C.,MunÄiz-Ferna Ândez,K.,Seger,A.,Raabe,G.&Gunther,K.(1998).Chem.63,7860±7867.Cetina,M.,Hergold-BrundicÂ,A.,Nagl,A.,Jukic Â,M.&Rapic Â,V .(2003).Struct.Chem.14,289±293.Cetina,M.,MrvosÏ-Sermek,D.,Jukic Â,M.&Rapic Â,V .(2002).Acta Cryst.E 58,m676±m678.akovicÂ,S.(2000).PhD thesis,University of Zagreb,Croatia. akovicÂ,S.,Lapic Â,J.&Rapic Â,V .(2003).Biocatal.Biotransform.In the press.Eikawa,M.,Sakaguchi,S.&Ishii,Y.(1999).Chem.64,4676±4679.Gonsalves,K.E.&Chen,X.(1995).Ferrocenes ,edited by A.Togni &T.Hayashi,ch.10,pp.497±527.Weinheim:VCH.KoÈllner,C.,Pugin,B.&Togni,A.(1998).J.Am.Chem.Soc.120,10274±10275.Nonius (2000).COLLECT.Nonius BV ,Delft,The Netherlands.Otwinowski,Z.&Minor,W.(1997).Methods in Enzymology ,Vol.276,Macromolecular Crystallography ,Part A,edited by C.W.Carter Jr &R.M.Sweet,pp.307±326.New York:Academic Press.Patti,A.&Nicolosi,G.(1999).Tetrahedron :Asymmetry ,10,2651±2654.Perea,J.J.A.,Lotz,M.&Knochel,P .(1999).Tetrahedron :Asymmetry ,10,375±384.Pioda,G.&Togni,A.(1998).Tetrahedron :Asymmetry ,9,3903±3910.Richards,C.J.&Locke,A.(1998).Tetrahedron :Asymmetry ,9,2377±2407.Schwink,L.&Knochel,P .(1998).Chem.Eur.J.4,950±968.Seiler,P .&Dunitz,J.D.(1979).Acta Cryst.B 35,2020±2032.Sheldrick,G.M.(1997).SHELXS 97and SHELXL 97.University ofGoÈttingen,Germany.Spek,A.L.(2003).J.Appl.Cryst.36,7±13.Unterhalt,B.,Krebs,B.,Lage,M.&Nocon,B.(1994).Arch.Pharm.327,799±804.Yamato,M.,Hashigaki,K.,Kokubu,N.&Nakato,Y.(1984).J.Chem.Soc.Perkin Trans.1,pp.1301±1304.Table 2Hydrogen-bonding geometry (AÊ, ).Cg 1and Cg 2are the centroids of rings C12/C13/C16±C19and C6±C10,respectively.D ÐH ÁÁÁA D ÐH H ÁÁÁA D ÁÁÁA D ÐH ÁÁÁA C14ÐH14A ÁÁÁCg 1i 0.97 2.85 3.627(2)138C18ÐH18ÁÁÁCg 2ii 0.93 2.88 3.660(2)142C18ÐH18ÁÁÁC7ii 0.93 2.86 3.760(3)163C18ÐH18ÁÁÁC6ii 0.93 3.03 3.874(3)151C5ÐH5ÁÁÁCg 1iii 0.93 3.14 3.984(2)152C5ÐH5ÁÁÁC12iii 0.93 2.98 3.840(2)154C5ÐH5ÁÁÁC13iii0.933.023.949(2)177Symmetry codes:(i)x Y 12Ày Y z À12;(ii)1 x Y y Y 1 z ;(iii)1Àx Y Ày Y 2Àz .Table 1Selected geometric parameters (AÊ, ).O1ÐC111.4236(19)O1ÐC15 1.432(2)C1ÐC11 1.503(2)C11ÐC12 1.523(2)C12ÐC16 1.388(2)C12ÐC13 1.397(2)C13ÐC19 1.392(3)C13ÐC14 1.504(3)C14ÐC15 1.501(3)C16ÐC17 1.384(3)C17ÐC18 1.380(3)C18ÐC19 1.379(3)C11ÐO1ÐC15110.39(13)C2ÐC1ÐC11127.61(14)C5ÐC1ÐC11124.78(14)O1ÐC11ÐC1109.37(13)O1ÐC11ÐC12111.64(13)C1ÐC11ÐC12112.14(13)C13ÐC12ÐC11119.77(14)C12ÐC13ÐC14120.38(16)C15ÐC14ÐC13111.24(15)O1ÐC15ÐC14110.04(15)。
Pipe & Hangers TechnicalIndustry Standards & Test MethodsPage 83Suitable for Oil-Free air handling to 25 psi, not for distribution of compressed air or gasSpears ® Manufacturing Company See Spears ® Product Sourcebook for product offerings Spears ® products are manufactured in strict compliance with applicable industry standards and specifications to ensure strength, durability and safety. Although not inclusive, the following list of internationally recognized standards, specifications, test methods and practices relate to PVC and CPVC thermoplastic piping products and related components.ASTM STANDARD SPECIFICATIONSASTM D 1784Standard Specification for Rigid Poly (Vinyl Chloride) (PVC) Compounds and Chlorinated Poly (Vinyl Chloride) (CPVC) Compounds ASTM D 1785Standard Specification for Poly (Vinyl Chloride) (PVC) Plastic Pipe- Schedules 40- 80 and 120ASTM D 2241Standard Specification for Poly (Vinyl Chloride) (PVC) Pressure Rated Pipe (SDR Series)ASTM D 2464Standard Specification for Threaded Poly (Vinyl Chloride) (PVC) Plastic Pipe Fittings- Schedule 80ASTM D 2466Standard Specification for Poly (Vinyl Chloride) (PVC) Plastic Pipe Fittings- Schedule 40ASTM D 2467Standard Specification for Poly (Vinyl Chloride) (PVC) Plastic Pipe Fittings- Schedule 80ASTM D 2665Standard Specification for Poly (Vinyl Chloride) (PVC) Plastic Drain-Waste- and Vent Pipe and Fittings ASTM D 2672Standard Specification for Joints for IPS PVC Pipe Using Solvent Cement ASTM D 2846Standard Specification for Chlorinated Poly (Vinyl Chloride) (CPVC) Plastic Hot- and Cold-Water Distribution Systems ASTM D 3139Standard Specification for Joints for Plastic Pressure Pipes Using Flexible Elastomeric Seals ASTM D 3311Standard Specification for Drain, Waste, and Vent (DWV) Plastic Fittings Patterns ASTM F 437Standard Specification for Threaded Chlorinated Poly (Vinyl Chloride) (CPVC) Plastic Pipe Fittings- Schedule 80ASTM F 438Standard Specification for Socket-Type Chlorinated Poly (Vinyl Chloride) (CPVC) Plastic Pipe Fittings- Schedule 40ASTM F 439Standard Specification for Socket-Type Chlorinated Poly (Vinyl Chloride) (CPVC) Plastic Pipe Fittings- Schedule 80ASTM F 441Standard Specification for Chlorinated Poly (Vinyl Chloride) (CPVC) Plastic Pipe- Schedules 40 and 80ASTM F 442Standard Specification for Chlorinated Poly (Vinyl Chloride) (CPVC) Plastic Pipe (SDR-PR)ASTM F 477Standard Specification for Elastomeric Seals (Gaskets) for Joining Plastic Pipe ASTM F 493Standard Specification for Solvent Cements for Chlorinated Poly (Vinyl Chloride) (CPVC) Plastic Pipe and Fittings ASTM F 656Standard Specification for Primers for Use in Solvent Cement Joints of Poly (Vinyl Chloride) (PVC) Plastic Pipe and Fittings ASTM F 913Standard Specification for Thermoplastic Elastomeric Seals (Gaskets) for Joining Plastic Pipe ASTM F 1498Standard Specification for Taper Pipe Threads 60° for Thermoplastic Pipe and Fittings ASTM F 1866Standard Specification for Poly (Vinyl Chloride) (PVC) Plastic Schedule 40 Drainage and DWV Fabricated Fittings ASTM F 1970Standard Specification for Special Engineered Fittings, Appurtenances or Valves for use in Poly (Vinyl Chloride) (PVC) or Chlorinated Poly (Vinyl Chloride) (CPVC) Systems ASTM F 2618Standard Specification for Chlorinated Poly (Vinyl Chloride) (CPVC) Pipe and Fittings for Chemical Waste Drainage Systems ASTM STANDARD TEST METHODS ASTM D 1598Standard Test Method for Time-to-Failure of Plastic Pipe Under Constant Internal Pressure ASTM D 1599Standard Test Method for Resistance to Short-Time Hydraulic Pressure of Plastic Pipe & Fittings ASTM D 2122Standard Test Method for Determining Dimensions of Thermoplastic Pipe & Fittings ASTM D 2152Standard Test Method for Adequacy of Fusion by Acetone Immersion ASTM D 2412Standard Test Method for Determination of External Loading Characteristics of Plastic Pipe by Parallel-Plate Loading ASTM D 2444Standard Test Method for Determination of the Impact Resistance of Thermoplastic Pipe and Fittings by Means of a Tup (Falling Weight)ASTM D 2564Standard Specification for Solvent Cements for Poly (Vinyl Chloride) (PVC) Plastic Piping Systems ASTM D 2837Standard Test Method for Obtaining Hydrostatic Design Basis for Thermoplastic Pipe Materials ASTM F 610Standard Test Method for Evaluating the Quality of Molded Poly (Vinyl Chloride) (PVC) Plastic Pipe Fittings by the Heat Reversion Technique ASTM STANDARD PRACTICES ASTM D 2321Standard Practice for Underground Installation of Thermoplastic Pipe for Sewers and Other Gravity-Flow Applications ASTM D 2774Standard Practice for Underground Installation of Thermoplastic Pressure Piping ASTM D 2855Standard Practice for Making Solvent-Cemented Joints with Poly (Vinyl Chloride) (PVC) Pipe and Fittings ASTM F 402Standard Practice for Safe Handling of Solvent Cements- Primers- and Cleaners Used for Joining Thermoplastics Pipe and Fittings ASTM F 645Standard Guide for Selection- Design- and Installation of Thermoplastic Water Pressure Systems ASTM F 690Standard Practice for Underground Installation of Thermoplastic Pressure Piping Irrigation System ASTM F 1057Standard Practice for Evaluating the Quality of Extruded Poly (Vinyl Chloride) (PVC) Pipe by the Heat Reversion TechniqueCSA STANDARD CSA B137.3-99Rigid Polyvinyl Chloride (PVC) Pipe for Pressure ApplicationsFIRE PERFORMANCEULC-S102.2-M88Standard Method of Test for Surface Burning Characteristics of Flooring- Floor Covering- and Miscellaneous Materials and AssembliesUL 94Test for Flammability of Plastic Materials for Parts in Devices and AppliancesUL 723Test for Surface Burning Characteristics of Building MaterialsUL 1821Thermoplastic Sprinkler Pipe and Fittings for Fire Protection ServiceUL 1887Standard for Safety for Fire Test of Plastic Sprinkler Pipe for Flame and Smoke CharacteristicsFM 1635Plastic Pipe & Fittings for Automatic Sprinkler SystemsASTM D 635Standard Test Method for Rate of Burning and/or Extent and Time of Burning of Manufacturing in a Horizontal PositionASTM D 2863Standard Test Method for Measuring the Minimum Oxygen Concentration to Support Candle-Like Combustion of Manufacturing (Oxygen Index)ASTM E 84Standard Test Method for Surface Burning Characteristics of Building MaterialsASTM E 162Standard Test Method for Surface Flammability of Materials Using a Radiant Heat Energy Source TOXICOLOGYNSF ® Standard 14Manufacturing 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Fluid-Structure Interaction Fluid-structure interaction (FSI) is a complex and challenging problem in engineering and physics, involving the interaction between a fluid and a solid structure. This interaction occurs in many real-world scenarios, such as the flow of air over an aircraft wing, the behavior of blood flow in arteries, and the movement of water around a marine structure. Understanding and accurately modeling FSI is crucial for designing and optimizing engineering systems, as well as for predicting and preventing potential failures. One of the key challenges in FSI is the need to accurately capture the two-way coupling between the fluid and the structure. This requires sophisticated numerical methods and computational tools that can solve the governing equations for both the fluid and the solid, while also accounting for their mutual interactions. Traditional approaches to FSI modeling often involve simplifications and assumptions that can limit the accuracy and applicability of the results. As a result, there is a growing demand for advanced FSI simulation techniques that can provide more realistic and reliable predictions. From a fluid dynamics perspective, FSI is important because it can significantly affect the behavior of the fluid flow. The presence of a solid structure can alter the flow patterns, create turbulence, and induce pressure fluctuations, which in turn can have a feedback effect on the structure itself. This mutual influence between the fluid and the structure can lead to complex and non-linear phenomena, such as vortex shedding, flow-induced vibrations, and fluid-elastic instabilities. Understanding these effects is essential for optimizing the performance and safety of engineering systems, such as aircraft, bridges, and offshore platforms. On the other hand, from a structural mechanics perspective, FSI is important because it can introduce additional loads and stresses on the solid structure. The forces exerted by the fluid, such as drag, lift, and added mass, can cause deformation, fatigue, and ultimately structural failure. Moreover, the dynamic response of the structure to the fluid-induced forces can lead to resonance, fatigue, and other forms of structural damage. Therefore, accurately predicting the FSI effects is crucial for ensuring the structural integrity and longevity of engineering systems. In the field of biomedical engineering, FSI plays a critical role in understanding the behavior of biological fluids, such asblood, within the human body. For example, the interaction between blood flow and the arterial walls is a key factor in the development of cardiovascular diseases, such as atherosclerosis and aneurysms. By accurately modeling FSI in blood vessels, researchers and clinicians can gain insights into the underlying mechanisms ofthese diseases, as well as develop more effective diagnostic and treatment methods. In conclusion, fluid-structure interaction is a multifaceted problem that requiresa holistic understanding of fluid dynamics, structural mechanics, and their mutual interactions. Addressing the challenges of FSI requires the development ofadvanced numerical methods, high-performance computing tools, and experimental techniques that can capture the complex and non-linear behavior of fluid-structure systems. By advancing our understanding of FSI, we can not only improve the design and performance of engineering systems, but also deepen our insights into the behavior of biological fluids in the human body.。
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS 2016年第35卷第4期·1074·化工进展石油馏分中酸性物质的组成分析肖丽霞,吕涯(华东理工大学石油加工研究所,上海 200237)摘要:针对某炼厂酮苯脱蜡装置原料油(减三线)中酸性物质组成特殊(对装置产生严重的腐蚀)的情况,采用碱醇法提取其中的酸性物质,借助负离子电喷雾-傅里叶变换离子回旋共振质谱(negative-ion ESI FT-ICR MS)研究其酸性组分的组成及分布,并与工业级脱脂环酸进行比较,从分子层面上揭示了其特殊之处。
Negative-ion ESI FT-ICR MS结果表明,减三线酸性化合物主要的特点为O2类化合物中脂肪酸(Z=0)占明显优势,缩合度较大的Z=−8和Z=−10的O2类化合物中有些碳数的物质相对丰度也比较大,碳数分布有两个中心;O1类杂原子化合物的相对丰度仅次于O2类化合物,且大大高出其他类杂原子化合物,O1类化合物中,烷基酚类化合物占绝对优势。
减三线酸性化合物的特殊组成将对进一步探究腐蚀机理和寻求解决设备腐蚀的途径有重要的指导意义。
关键词:石油馏分;腐蚀;酸性物质;负离子电喷雾-傅里叶变换离子回旋共振质谱;组成中图分类号:TE 622 文献标志码:A 文章编号:1000–6613(2016)04–1074–07DOI:10.16085/j.issn.1000-6613.2016.04.017Composition of acidic compounds in petroleum fractionXIAO Lixia,LÜ Ya(Institute of Petroleum Processing,East China University of Science and Technology,Shanghai 200237,China)Abstract:The acidic compounds in the feedstock of a refinery(vacuum cut 3) made devices corroded seriously,so the composition and distribution of the acidic compounds were analyzed by negative-ion electrospray ionization Fourier transform ion cyclotron resonance mass spectroscopy (negative-ion ESI FT-ICR MS). The acid fraction was extracted by alkaline-ethanol extraction prior to analysis,and compared with the industrial-grade naphthenic acids. The specialty of the acidic compounds in the feedstock of the refinery was explained from the molecular level. Negative-ion ESI FT-ICR MS revealed that the O2 class of the extracted acid fraction in the feedstock was dominated by acyclic carboxylic acids (belong to Z=0 family),and those had higher relative abundance of some compounds belonged to Z=−8 and −10 families of the O2 class,which leads the carbon number distribution curve has two peaks. The relative abundance of O1 class was much higher than that of other classes except for O2 class. The O1 class was dominated by alkylphenols. The special composition and distribution of acidic compounds has an important guiding significance to study the mechanism of corrosion and seek treatments for equipment corrosion.Key words:petroleum fractions;corrosion;acidic species;negative-ion electrospray ionization Fourier transform ion cyclotron resonance mass spectroscopy(negative-ion ESI-FT-ICR MS);composition随着石油资源的不断消耗,含酸或高酸原油的处理量越来越大,对石油加工过程产生很多影响,例如加工时引起装置严重腐蚀、影响产品质量等[1-2],深入研究石油及馏分中的酸性物质成为石油化学研究的热点之一。
Vol.53 No.4Apr.,2021第53卷第4期2021年4月无机盐工业INORGANIC CHEMICALS INDUSTRYDoi:10.11962/1006-4990.2020-0318开放科学(资源服务)标志识码(OSID)改性球形活性炭对氨气吸附性能的研究金青青袁梁晓烽,张佳楠,周晓龙(华东理工大学化工学院,上海200237)摘 要:研究了不同金属盐溶液浸渍改性的球形活性炭对氨气的吸附性能以及同种浸渍剂的最佳浸渍比。
采用 扫描电镜、透射电镜、X 射线衍射仪、康塔吸附仪探究了不同浸渍比对浸渍炭样品的表面形貌、物相结构及孔径分布的影响。
通过固定床吸附装置对基炭和浸渍炭进行了氨气吸附性能的研究。
结果表明:浸渍剂种类对氨气吸附效果 有很大影响,同等浸渍条件下,氯化钻浸渍的活性炭具有最优氨气吸附效果,氯化钻浸渍比为50%的样品对氨气的吸附量最高,可达54.05 mg/mL ,为基炭的37倍。
对吸附氨气后样品的物化性质进行分析以及程序升温脱附表征,结 果表明氯化钻与氨气反应生成了 [Co (NH 3)6]Cl 3。
关键词:球形活性炭;氯化钻;浸渍炭;氨气;吸附性能中图分类号:0647.32 文献标识码:A 文章编号:1006-4990(2021)04-0061-06Study on adsorption performance of modified spherical activated carbon for ammoniaJin Qingqing ,Liang Xiaoyi 袁Zhang Jia'nan ,Zhou Xiaolong(School of Chemical Engineering , East China University of S cience and Technology , Shanghai 200237, China)Abstract : The adsorption performance of spherical activated carbon impregnated with different metal salt solutions for ammonia and the optimal ratio of the same impregnant were studied.The influence of different impregnation ratio on the surface morpho-logy ,phase structure and pore size distribution on impregnated carbon samples were investigated by scanning electron micro scopy , transmission electron microscopy , X-ray diffraction and Quanta adsorption instrument.The adsorption performance of the unmodified carbon and impregnated carbon for ammonia was studied by the fixed bed adsorption device.The results showedthat the type of impregnant had a great influence on the adsorption performance of ammonia.Under the same impregnation conditions , the activated carbon impregnated with cobalt chloride had the best adsorption performance for ammonia.The samplewith 50% impregnation ratio of cobalt chloride had the highest ammonia adsorption capacity up to 54.05 mg/mL , which was 37 times of the unmodified carbon.The physicochemical properties and temperature programmed desorption characteristics ofthe samples after ammonia adsorption were analyzed.The results showed that[Co(NH 3)6]Cl 3 was formed by the reaction of co balt chloride with ammonia.Key words : spherical activated carbon ; cobalt chloride ; impregnated carbon ; ammonia ; adsorption capacity氨气渊NH 3 )是一种有毒的碱性气体,对人类健 康和环境均造成严重危害[1]。
第43 卷第 5 期2024 年5 月Vol.43 No.5674~681分析测试学报FENXI CESHI XUEBAO(Journal of Instrumental Analysis)氮掺杂Ti3C2 MXene量子点荧光探针用于α-葡萄糖苷酶活性检测李军1,杨新杰1,罗焰1,李泉1,宗玉红1,张艳丽1*,王红斌1,杨文荣1,2,庞鹏飞1*(1.云南民族大学化学与环境学院,云南省教育厅环境功能材料重点实验室,云南昆明650504;2.迪肯大学生命与环境科学学院,澳大利亚维多利亚州吉朗3217)摘要:α-葡萄糖苷酶是生物体糖代谢途径中不可或缺的一类酶,发展简单、灵敏、准确的α-葡萄糖苷酶活性检测及抑制剂筛选方法对于糖尿病的治疗与预防具有重要意义。
该文基于氮掺杂Ti3C2 MXene量子点(N-Ti3C2 MQDs)荧光探针和内滤效应(IFE),构建了一种“开-关-开”型荧光传感α-葡萄糖苷酶活性检测及抑制剂筛选的新方法。
研究发现,N-Ti3C2 MQDs发射蓝色荧光(λem = 440 nm),荧光量子产率为15.7%。
其检测机理为:α-葡萄糖苷酶水解底物对硝基苯基-α-D-吡喃葡萄糖苷,水解产物对硝基苯酚通过内滤效应导致N-Ti3C2 MQDs荧光猝灭;而抑制剂阿卡波糖可使α-葡萄糖苷酶的活性受到抑制,水解产物减少,N-Ti3C2 MQDs 荧光恢复。
结果显示,N-Ti3C2 MQDs探针荧光强度与α-葡萄糖苷酶浓度在5~300 U/L范围内呈良好线性关系,检出限为2.5 U/L(S/N = 3),对阿卡波糖的半最大抑制浓度(IC50)为178.5 μmol/L。
该方法具有成本低、操作简单、灵敏度高、选择性好等特点,已成功用于人血清中α-葡萄糖苷酶活性的测定。
关键词:α-葡萄糖苷酶;氮掺杂Ti3C2 MXene;量子点;荧光探针中图分类号:O657.3;O629.8文献标识码:A 文章编号:1004-4957(2024)05-0674-08 Fluorescent Probe for Detection of α-Glucosidase Activity Based onN-Doped Ti3C2MXene Quantum DotsLI Jun1,YANG Xin-jie1,LUO Yan1,LI Quan1,ZONG Yu-hong1,ZHANG Yan-li1*,WANG Hong-bin1,YANG Wen-rong1,2,PANG Peng-fei1*(1.Key Laboratory of Environmental Functional Materials of Yunnan Province Education Department,School ofChemistry and Environment,Yunnan Minzu University,Kunming 650504,China;2.School of Life andEnvironmental Sciences,Deakin University,Geelong VIC 3217,Australia)Abstract:α-Glucosidase is an indispensable enzyme in the glucose metabolism pathway of organ⁃isms. The development of simple,sensitive and accurate detection methods for α-glucosidase activi⁃ty and inhibitors screening are of great significance for the treatment and prevention of diabetes. In this work,a novel fluorescent "on-off-on" method for detection of α-glucosidase activity and its in⁃hibitors screening was developed based on N-doped Ti3C2 MXene quantum dots(N-Ti3C2 MQDs) and internal filtration effect(IFE). The prepared N-Ti3C2 MQDs emitted blue fluorescence(λem = 440 nm)with a fluorescence quantum yield of 15.7%.α-Glucosidase can hydrolyze substrate p-nitrophenyl-α-D-glucopyranoside to produce p-nitrophenol,which causes fluorescence quenching of the N-Ti3C2 MQDs through IFE.After adding the acarbose inhibitor,the activity of α-glucosidase is inhibited and the produced p-nitrophenol by hydrolysis is reduced,resulting in fluorescence recovery of N-Ti3C2 MQDs. Fluorescent intensity of N-Ti3C2 MQDs probe is proportional to α-glucosidase concentra⁃tion in the range of 5-300 U/L,with a detection limit of 2.5 U/L(S/N = 3). The half-maximal inhibi⁃tory concentration of inhibitor(IC50) value is calculated to be 178.5 μmol/L for acarbose. This pro⁃posed method has the advantages of low cost,simple operation,high sensitivity,and good selectivi⁃ty,which has been successfully used for determination of α-glucosidase activity in human serum.doi:10.12452/j.fxcsxb.24010503收稿日期:2024-01-05;修回日期:2024-02-18基金项目:国家自然科学基金资助项目(21665027,21565031);云南省科技厅应用基础研究项目(202001AT070012)∗通讯作者:张艳丽,博士,教授,研究方向:化学与生物传感,E-mail:ylzhang@庞鹏飞,博士,教授,研究方向:荧光传感分析,E-mail:pfpang@第 5 期李军等:氮掺杂Ti3C2 MXene量子点荧光探针用于α-葡萄糖苷酶活性检测Key words:α-glucosidase;N-doped Ti3C2 MXene;quantum dots;fluorescent probe糖尿病作为一种影响多种慢性病的重要因素,因发病率高,引起了广泛的关注。
For reasons of economy, this document is printed in a limited number. Delegates arekindly asked to bring their copies to meetings and not to request additional copies.INTERNATIONAL MARITIME ORGANIZATIONIMOESUB-COMMITTEE ON FLAG STATEIMPLEMENTATION16th sessionAgenda item 14 FSI 16/14/2 27 March 2008Original: ENGLISHREVIEW OF THE CODE FOR THE IMPLEMENTATIONOF MANDATORY IMO INSTRUMENTSApplicability of IMO Conventions to FPSOs and FSUsSubmitted by the International Transport Workers' Federation (ITF)SUMMARYExecutive summary: This document requests a clarification on the applicability of theSOLAS Convention and the ISM Code to FPSOs and FSUsdesigned to be released from their moorings and operate undertheir own powerStrategic Direction: 2High-Level Action: 2.1.1Planned Output: 2.1.1.5Action to be taken: Paragraph 19Related documents:Resolution MEPC.139(53); resolution MEPC.142(54);MEPC/Circ.406; MEPC 56/6/9; MEPC 56/WP.10; MSC 74/21/3;MSC 76/23; MSC 83/27/8; MSC 83/28; STW 39/11/8;STW 39/12; ISM Code and STCW and SOLAS ConventionsIntroduction1 Since 2001, the Marine Environment Protection Committee (MEPC) has worked on amendments to Annex I of MARPOL to exempt floating production, storage and offloading facilities (FPSOs) and floating storage units (FSUs) from many of the requirements applicable to an oil tanker as defined in regulation 1 of Annex I of MARPOL.2 In the annex to resolution MEPC.139(53), adopted on 22 July 2005, in introducing the Guidelines issued as MEPC/Circ.406, the following was recorded:.1 MEPC 49 noted the complex issues involved in applying Annex I of MARPOLto FPSOs and FSUs, the arrangements, functions and operations of which fallunder the over-riding control of coastal States;FSI 16/14/2 - 2 -.2 FPSOs and FSUs are a form of floating platform and do not fall under the definition of oil tanker in regulation 1.5 of the revised Annex I of MARPOL; and.3 the MEPC noted that the environmental hazards associated with the quantities of produced oil stored on board operational FPSOs and FSUs are similar to some ofthe hazards related to oil tankers.3 At MEPC 56, in reply to document MEPC 56/6/9 (ICFTU), it was confirmed that article 2 of MARPOL on the definition of a ship was applicable, for the purposes of the Convention, to FPSOs and FSUs (MEPC 56/WP.10, paragraph 6.50). This could be taken to mean that companies cannot just consider the vessel as a production platform and take fully into consideration its operational requirements as a ship.4 Following the proposal by Australia (MSC 74/21/3) to develop international requirements for the design, construction, survey and operation of FPSOs and FSUs, the Maritime Safety Committee (MSC), at its seventy-fourth session, forwarded the matter to the Sub-Committee on Bulk Liquid and Gases (BLG) for consideration. Based on the BLG’s advice, MSC 76 decided that, for the time being, it was not necessary to apply mandatory IMO instruments to address safety-related issues for FPSOs and FSUs, as the existing safety regime was adequate (MSC 76/23, paragraph 10.3).5 MSC 83 considered the proposal by ITF (MSC 83/27/8) that, in light of MEPC 56’s decision confirming that article 2 of the MARPOL Convention (definition of a ship) was applicable for the purposes of the MARPOL Convention to FPSOs and FSUs, the Committee should reconsider the above-mentioned MSC 76’s decision.6 While there was wide support for developing adequate safety criteria for FPSOs and FSUs, it was recognized that these criteria should not prejudice the rights of the coastal State. Accordingly, the Committee agreed to forward document MSC 83/27/8 (ITF) to FSI 16 and STW 39 for consideration and advice to MSC 85 on the applicability of IMO conventions to FPSOs and FSUs, before establishing any new work programme item for the sub-committees.7 The Sub-Committee on Standards of Training and Watchkeeping, at its thirty-ninth session, agreed that requirements of the STCW Convention applied to releasable FPSOs and FSUs when they were underway and invited MSC 85 to take this into account when deciding on safety criteria for FPSOs and FSUs (STW 39/12, paragraph 11.35).Discussion8 The status of FPSOs and FSUs as ships is particularly relevant where these vessels have the provision to disconnect their moorings in an emergency and in extreme weather conditions, to operate under their own power and, possibly, to transit into international waters.9 It appears that in the views of some Administrations, whilst these vessels must be capable, and regularly required, to operate as ships they are exempted from all the IMO safety conventions. This is particularly problematic where the interface between the production and the maritime requirements are not easily defined and the maritime crews, without being part of the vessel management process, are expected to assume full responsibility with little notice.- 3 - FSI 16/14/2 10 Recent incidents have exposed the dangers that this lack of clarity and good operating practice permits and, in one case, it came close to allowing 12,000 tonnes of crude oil to pollute the shoreline. This particular vessel had been released five times in one year, had excessive hull growth due to the lack of docking and an engine that had been de-rated and unsuitable to deal with the prevailing weather conditions.11 Some Administrations have amended their Petroleum Act (or equivalent) so that their Navigation Act (or equivalent) no longer applies to FPSOs or FSUs whilst moored on location. However, when they disconnect, the Navigation Act does apply and the designated master and chief engineer must bear the statutory responsibility. In fact, the safety case for these vessels requires them to be able to disconnect and to flee a cyclone under their own propulsion.12 Increasingly, the master and chief engineer will operate as process maintenance technicians totally outside the management team with a decreasing number of other maritime qualified technicians. This management team will make all the decisions which are usually under the responsibility of a master and chief engineer whilst moored on location.13 When a cyclone strikes, the management team will divest themselves of all responsibilities to the technicians designated as the master and the chief engineer, thus inverting the job structure in an emergency. This clearly requires the competency and gives the responsibility to these technicians without the authority to rectify problems regarding machinery or seaworthiness.14 This clearly does not comply with sections A-II/2 and A-III/2 of the STCW Code or the provisions of SOLAS chapter IX and, given that these vessels are required to flee a cyclone or extreme weather under their own power, gives scant regard to a safety management system, as defined in the International Safety Management Code (ISM Code).15 Increasingly, the oil production industry is giving little consideration to the normal maritime minimum competency or operational requirements of crews that are integrated into the production process and have reduced qualified marine crew on these vessels. These matters have been addressed at some length for special offshore vessels such as the provisions within the Mobile Offshore Drilling Unit Code (MODU Code) but are totally absent in respect of FPSOs and FSUs. Guidance from the oil production industry seems inadequate or largely ineffective. Summary16 ITF is of the view that any FPSO or FSU, capable and required to operate as a ship, and defined as a ship under article 2 of MARPOL, should also be in compliance with the minimum requirements of the STCW Convention and should be able, at all times, to show compliance with the relevant IMO instruments, in particular, the ISM Code.17 It would only seem realistic that, where the master and crew are expected to take on the responsibilities of operating a vessel in what is usually a dangerous situation, they must, at all times, have primary input into the maintenance and operating requirements.18 The provisions of the STCW Convention and the ISM Code are no less relevant for these large vessels which are full of oil and capable of operating under their own power in both national and international waters.FSI 16/14/2 - 4 -Action requested of the Sub-Committee19 The Sub-Committee is invited to recommend the reconsideration of the decision of MSC 76 in order to establish safety criteria for FPSOs and FSUs at all times, taking particular note of the applicability of the SOLAS and STCW Conventions and the ISM Code to FPSOs and FSUs._____________。