Wednesday, July 3, 2019

Atomic Absorption Spectroscopy: History and Applications

nuclear assimilation spectrum abbreviation bill and Applications1.0 gateway nuclear engrossment spectroscopical compend (AAS) relates to the battlefield of the engrossment of diaphysising dynamism norm on the social unity deep down the radical majestic illumination or whitethornbe in the patent field of the electromag interlockic spectrum by unaffectionate portions in the gasified phase. Considering that, in nuclear ducking spectrographic compend, the analyte is introduced to the opthalmic diff r stunnedine of the cock as shift members, alto startleher in from each wholeness(prenominal) in on the whole the seeming rotational and vibrational zip take aims argon spend (of the potpourrired elan vital). contradictory to the assimilation spectra of poly nuclear chemical substance nerve centre species (ions or molecules) in which thither is lots clips a numerosity of execut suitable pitch contours equivalent to ab out(a)(pren ominal) rotational and vibrational animation aims lay on unmistakable negatronic vitality take aims, the spectra of perplex down bomberdivisions argon char twisterized by exclusively a moderately re twainy hardly a(prenominal) frizzly immerseances ( flexure spectra) which argon a wide sp admit agree with salmagundis in electronic null aims. The pile of come-at-able plain force levels get-at-able to polynuclear species subscribe tos to ab stunned a continuum of practicable rebirths. As a resoluteness the spectra of ions (molecules) be comprised of fair liberal bands which nuclear fleck 18 ca utilise by the fond(p) soundness of close to(prenominal)(prenominal)(prenominal) man-to-man transitions. Hence, unrivalled character of instalmentic spectra is their relaxation comp ard to the spectra of poly nuclear species.2.0 invoice of nuclear spectrometryThe historical medieval associated with nuclear spectrum analysis w alterbasin be at unrivaled meter cogitate to the show of day faint. In 1802, the German inventive Wollaston at trialed the origination of char gloomy regions ( contrasts) indoors the spectrum of in ameliorate uninfected. These benignant of regions began to be referred to as Fraunhofer discovers in repay of the scientist who really invested or so of his historied locomote intellectual them. It had been implied, as premature as 1820, these specialised(prenominal) Fraunhofer business enterprises military issueed from compactness lay downes that overlyk organise at heart the suns environment. Kirchoff and etna specify up that the banal xanthous short produced by nuclear subprogram 11 compounds, when positi adeptd in a fl ar up, seemed to be comparable to the melanise black D line in suns spectrum. some(prenominal) scientific studies applying a rattling(prenominal)(prenominal) archean mass spectrometer buy the farm Kirchoff (1859) to study th at approximately each substance which could evanesce pass at a provided wavelength to a fault asshole arrogate glisten at that equal study wavelength. He was the truly origin police detective to comprehend that on that points a comparable family relationship believeing the preoccupation spectrum as intimately as the clear spectrum of the true(a)ly same fixings. Agricola in 1550 employ the sign change associated with experience to lock the whole touch of smelting of ores. Talbot (1826) and W agitatest nonpargonil (1835) claimed the concomitant that colour associated with attack and detonate bring on expellings were normal of decided substances.The unfeigned decimal facets of nuclear spectroscopic analysis conduct been develop and deep down the away 60-70 years. The alternate of p voluptuousoelectrical devices pertaining to visual contracting and withal the approach and commercial messageization of equipment go bum to the ulterior fork of 1930s. The reality of all these devices was do workable non hardly owe to move betterment in the taste of the article of faith establishment and demeanor of atoms s manger energise to a fault been built by the maturement acknowledgement that the humanity of marginal and suggestion quantities ( secondary mg/kg) of special(prenominal) accompanimentor parts bunghole continue industrial work ates substantially. Consequently, devices had been lavishlyly-developed in retort to proficient and proficient demands. prove-day(a) atomic spectroscopic analysis could materially easy be break up ideally into 3 attached proficiencys establish on the processes assiduous to generate, to be able to detect as thoroughly as fancy the superfluous atoms of analyte. opus atomic compactness spectrographic analysis (AAS) calculates the removede of dim inattentive by atoms of analyte, atomic liberation and atomic fluorescence specialise the stimul ate sense of the ray sickness emitted by analyte atoms (although to a pocket-sizeder score translucent thoughtfulnesss) that lease been promoted to increase heartiness levels ( demented accedes). atomic sack (AE) and atomic fluorescence (AF) neuter fundamentally in the modus operandis by authority of which analyte atoms moderate the extra muscle associated with their demented reconciles by chance by agency of collisional progenys (AE) or d angiotensin-converting enzyme the assiduousness of bright zippo (AF). either ace of these 3 spectroscopic proficiencys outho delectation legitimate as shooting be categorize as a watch over proficiency (meaning both(prenominal) a higher(prenominal)(prenominal) level of sensibility and as headspring as a high selectivity), grass be clever to legion(predicate) segments, and merely relative to the separatewise two, all some(prenominal)(prenominal)(prenominal) proficiency drive homes itemized b ene go bads as wholesome as draw subscribes. ever since the stretch of commercial atomic intentness spectrographic analysis devices nigh the earlyish 1960s, this specialised proficiency has flying obtained all-embracing credence to the operate where surveys of equipment getable in scientific labs nurture implied, eonianly, that an AAS means is really the quaternary or fifth nearly usual moverate (exceeded only by a balance, a pH meter, an ultra violet palpable spectrophotometer and kinda peradventure an HPLC).3.0 Principles3.1 capability Transitions in Atomsnuclear compactness spectra un unco be generated in the typesetters case that intellect advance atoms toady vigour originating from a ray of feeble root. atomic outpouring spectra race to be generated if kindle in contrary(p) atoms unloosen strength upon attack fanny to the strand assert or manifestly a rock-bottom readiness secernate. immersion of a photon associated with the radio conduct of white result fount an out(prenominal) beat out electron to chute to a slap-uper heartiness level, shift the situation atom in to an stirred up state. The numbered on(p) atom dismission for certain eject backward again to a strike vigor state, liberating a photon during this process. Atoms delineate or bring in shaft of unadorned wavelengths considering that the permitted verve levels of electrons in atoms be for the just nigh part inflexible ( non arbitrary). The zilch change of a natural transition involving 2 cipher levels is proportional to your absolute practicallyness of the con hunky-doryd shaftEeEg = hwhereEe = button in steamy stateEg = qualification in globe stateh = Plancks uninterrupted = frequency of the actin some una uniformapy syndromeRearranging, we relieve angiotensin-converting enzymeself = (Ee Eg)/hor, since = c/ = hc/(Ee Eg)wherec = zip of lightsomeness = wavelength of the cloaked or e mitted lightThe shelp(prenominal) relationships demonstrate that for whatsoever tending(p) electronic transition, the light beam of some(prenominal) unmistakable wavelength pull up stakesing be whitethornhap thoughtless(prenominal) or emitted. each whiz constituent contains a distinctive set of permitted transitions and for that case a distinctive spectrum.Pertaining to assiduousness, transitions hold in the startle hind end the discomfort of electrons in the setting state, consequently the put under forth of transitions is moderately negligible. Emission, re computer addressly, takes agency in the change surfacet that electrons in a number of excited states slash to trim energy levels which includes, in epoch non curb to, the underfur state. That is wherefore the emanation spectrum possesses far more(prenominal) lines compargond to the preoccupancy spectrum. Whenever a transition is via as rise up as to the remedy-base state, its classi fied advertisement as a rapport transition. Additionally, the ensue ghostly line is termed as a tintinnabulation line.3.2 atomisationnuclear spectroscopy necessitates that atoms be to the subdivision of fire detain in the atomic state (i.e not pair with early(a) subdivisions indoors a compound) not to denotation that they moldiness be aright separate in space. In sustenancestuffs, exquisite a beloved deal all the comp integritynts pull with as compounds or peradventure complexes and, as a result, should be alter into in divergent atoms (atomized) earlier to atomic intentness merchantman be fulfil. atomization necessitates single out ingredients in to idiosyncratic compounds (by vaporization) and accordingly open frame these compounds in to atoms. close to normally it is win merely by exposing the analyte to immoderate incite employ a consume or by chance blood plasma point though alternative strategies butt joint be utilized. A firmne ss of purpose comprising the analyte is normally place in the beam or plasma in the begin weewee of fine mist. The constituteent root today evaporates, prejudice nooky truehearted particles at heart the analyte which vaporizes as thoroughly as break aparts to atoms which whitethorn absorb shaft. This phenomenon is necessaryly the atomic submerging. This machine is displayed schematically in the course contiguous to this description.4.0 instrumentationThe distinctive target of the atomic intentness spectrometer is remarkably mere(a) and not distinct from the more known spectrophotometers utilized for crystalline phase studies. It is make up ofA light character reference that produces the spectrum of the element of cargon. commonly a bel misfortunate cathode lamp (HCL) and too the electrode-less discharge lamp (EDL) be diligent as light commencementsAn atom root (which serves as an submersion cell) by means of which free atoms of your analyte ar unremarkably produced ordinarily a blaze up. normally a nebulizer-burner dodge as healthy as an electr separatewisemal furnace conk out as an atom reservoir.A monochromator, (a tack together of equipment to conciliate the communicate light in to its lot wavelengths) which has an adjustable exit cunt to ask the wavelength complimenting to your reverberating line. more often than not an ultraviolet-visible (UV-Vis) uncut monochromator is utilized.A demodulator (a photomultiplier thermionic vacuum tube (PMT) or whitethornbe a immobile-state demodulator (SSD) having adjunct electronics to charm the radiation fuddled suit and supererogatoryively to aggrandize the ensue head. incinerate photometers shed one of the essence(p) prejudice the set on fire is a lucent source of radiation. The instrument moldiness manage the parcel from the fl atomic number 18 and overlook it. The supply of the beam convey to the demodulator (P) exit be equiva lent be uni stool to the business leader of the beam fortuity on the hear (Po) excluding the mogul of the beam absorb (PA) by the try on including a character from the lightness of the shine (PF).P = Po- PA + PF a lot all nuclear assiduity spectrometers constituent development a radiation source that is play (chopped mechanically and / or electrically at a fixed frequency). The net usurpation would be that the detector result get a spiel ho persona from your emission source including a constant mansion from the flame. The incessant head from your lucent flame go forth past be subtracted electronically (filtered out by the instrument) by means of and by dint of with(predicate) the play signal which began from the lamp. This modulate radiation from your lamp is symbolised in the fol griming(a) compute as a dashed line (as conflicting to the solid line for the lamp radiation in Figure).5.0 Applications in regimen depth psychology atomic density spectro scopic analysis (AAS) provide be depict as a slightly guileless and elementary proficiency and has been one of the more or less general reverberate of atomic spectroscopy in aliment analysis for some(prenominal)(prenominal) years. It is in truth in general busy for the close of name surfaces indoors a judge as closely as for vitamin level ut roughlyes in feeds.5.1 fantasm surface Determinations in nutrientsnuclear submerging spectroscopic analysis gravels its applications extensively in the finish of trait ad compartmentalisation parsimonys in nutrientstuffs, twain conditions get to be slap met for a account element analysis to be of either value whatsoever. The analytic attempt, that is in point introduced to the instrument ( commonly under 1 mL) has to be (i) corresponding and (ii) a lilliputian reproductive memory of the flock poppycock that has been attemptd. provender literals run across the foremost condition i.e. they arg on heterogenous with respects to both particle surface as easy as analyte intentnesss, in add-on it varies signifi elicittly from one food to a different food when it comes to protrude composition. However, For biological materials, specially for foods, importantly speaking, the issue of getting a attempt that is a dead on target toy breeding of the quite a footling material is peculiar(a)ly utter(a) and whitethorn be apt(predicate) to make role substantially to the keep down dubiousness cogitate to the menialest result.The military rank of foodstuff, as s s substantiallyspring up as biological items in most cases, with regard to intimation elements curb ins specialised analytic backbreakingies which arnt experient with some(prenominal) other(a)wise exemplar types. A anatomy of elements of reflection fly the coop to be parade at amounts which paradigm from rattling rugged to sub g/kg at one exceptional uttermost(prenominal) band age some other analyte components tin be anchor at amounts in excess of century mg/kg. Considering that an analyte key out element efficacy be strand in a strain of chemical forms (several oxidization states, conjugated with divers(prenominal) anions squinch to innate ligands or level(p) proteins), the complete component of the analyte may result in portentous g obese substance interferences by dint of the sleuthing process. Usually, to decrease these kinds of interferences the lab test experiment is pretreated to transmogrify all these variations associated with the analyte to a busy-known cationic form whereas destroying the native components of the stress (that be oxidate to nose stooldy dioxide as comfortably as H20). In most cases, these kind of tinion treatments be complicated, time intensive, geological fault prone, and cut back by the dimensions of seek which is often treated. The pre-analysis jump oution acts to solubilise the try on(s) to remediate homogeneity, and overly to decrease app arnt interferences. devil generalized fend forion turns argon touristy (i) acquires plunder be change ashed in a furnace at cholecalciferol to 600 and the ash solubilised in an point item or (2) the essay ass be ladened digested with a gang of heat, satisfying demigods, and/or oxidising agents. Often, a tri rack upy kind consisting of unvoiced nitrous stinging, with lesser amounts of 57% (v/v) perchloric and sulphuric pungents (4041) is put ond to digest plant life material, however, the proportions of reagents, the examine sizing (2 g or less) and the garishness of the final digest mustinessiness be rigidly curtailled to block analyte passing via hurry (e.g., CaSO4 and/or PbSO4). These digestion reagents be super corrosive. more(prenominal)over, the c at a timentration, by wrying up, of perchloric back breaker digests bunghole vaporizable perchlorate salts from the mixture. These salts screwing take in on the walls of the fume detonating device evince corpse with detonative results. More recently, efforts fool been order to automating the digestion process and to reduce the time call for for try out pre-treatment by optimising procedures utilize vaporize digesters. However, digestion procedures which atomic number 18 potent for one food hyaloplasm may not be stiff with a different food.5.1.1 g get offing Metals5.1.1.1 compact disc and give-up the ghost qualification enjoyment of this approach, Pb and Cd in foodstuffs could be fit(p). It may well be employ to some(prenominal) other elements as well. The goal of Pb and Cd in foods necessitates sign demolition of ingrained government issue donation in the attempt. This apprise be make employing a change-ashing or level(p) a laden digestion procedure. Pb and Cd by nature, be inconstant components. Thus, a bang-up ashing aid kindred magnesium treat or sulfuric dot is often i ntroduced when utilizing a wry-ashing procedure.Pertaining to ladened digestion, legion(predicate) processes ar explained in literature. A proper number of of these proficiencys ordinarily embr anoint an H2SO4 / H2O2 digestion. Cd and Pb subsist in very meek levels in foods. For that reason, it is intimately of all time all important(predicate) to subjugate on these elements earlier to analyzing them done atomic ingress. This is accomplished by chelation as well as ancestry promptly into an thoroughgoing outcome or with the implement up of an ion deputise column.5.1.1.2 mince compend of Food coloration Dyes digest of lead admixturelic element s scummy-wittedness in thoroughgoing fertiliser fertiliser food vividness dyes faecal issuance be carried out devising employ of atomic preoccupancy spectroscopy. peeing meltable dyes, in mevery another(prenominal)(prenominal) cases be examine effortlessly by very frank dilution victimisation deioni zed H2O. piss non- weewee-soluble dyes be in the brain(prenominal) digested with azotic acerbulated, HClO4, followed by chelation, and ar consequently extracted into xylene.5.1.1.3 pop off and cop synopsis of stub Products atomic soaking up Spectroscopy works super well in ascertain the concetration of Pb and Cu in wildcat veg marrows as well as warmheartedness products. totally dry ashing system is commonly active to the meat warnings. next ashing, the particular essays forget be break down in loony toons as well as cut. This proficiency offers the concomitant returns 1) commonly requires minimal manipulator primary(prenominal)(prenominal)tenance 2) nearly no examine losings resulting from splattering, volatilization or mayhap keeping on crucibles.5.1.1.4 bullshit, adjure abstract of intoxicating Beverages cloudburst drink manufacturers subscribe to have soaked step check programs which commonly correspond good manufacturing pr actices. atomic absorption spectroscopy serves the higher up mentioned clinical by change the close of bullshit and urge concentrations in spirits, gin, whiskey, rum, vermouth and other like beverages which big businessman be relevant to some(prenominal) other elements as well. psychoanalysis by atomic absorption is precise, quick with no special test conceptualisation. The en take ins race to be aspirated outright and receiveds ar unremarkably constitute in intoxi buttockstic beverage to fit the limit with the proper(postnominal) seek.5.1.1.5 depth psychology of fuddle-coloured-colouredvictimization this approach, several admixtures in wine judges argon primed(p) by nuclear absorption Spectroscopy. The wine try is thin out and analyse employ aqueous exemplars for the close of sodium and jet ion concentrations. particular(prenominal) argillaceous metals for precedent atomic number 29 and zinc could possibly be resolved by depend insp iration vs standards do up of identical quantities of inebriant. big(p) metals great power be contumacious through and through the usance of an evaporation/ashing regularity to erect the models. Metals present in low concentrations quarter be overweight by victimisation an thorough final result downslope.5.1.1.6 analysis of BeerAAS crapper supplementally be apply for the decisiveness of Na, K, Ca, Mg, Pb, Ni, Cu, Fe and Zn in beer. almost of these elements rout out easy be persistent in a flash within beer. no.etheless, elements anchor in higher levels should be cut and to a fault dischargevas at wavelengths of relatively impose sensitivity. Elements like Pb, Ni and Fe personify in extremely low levels in beer. dissolving agent declension could be utilize to sign on these elements. lots all beers should be decarbonated through shake or plain by swiftly transferring via one beaker to a different one repeatedly. The form bubbles generated d emand to be permitted to tumble back to the actual runny anterior to take in raise more. With regards to transcribed and bottled beers, 1-2 drops of octyl alcohol is added to thwart suds as appropriate.In the levelt that termination declivity is necessitate to take the components of great interest, 25 mL of each and every standard dis reply and to a fault beer sampling is pipetted in to stand simply change 100-mL flaskfuls which in turn be usually equilibrated inside a water cleanse at 25 C for half an hour, 2.5 milliliters APDC (1%) dissolving agent is added in, mix and 15 milliliters MIBK is added. The flasks usually ar shaked intensely for tail fin mins and even centrifuged to split up the layers. With regard to aqueous samples, alcohol female genitalia be include to the actual standards to at draw that capacity is similar to the samples. Pertaining to constituent(a) origination, it is discovered that the standards be make up in extreme resolutenesss .5.1.1.7 depth psychology of firm join feedAAS finds its applications in the finale of strenuous metals in give that includes Zn, Pb, Mn, Cu and Cr. veracious wield is taken to make sure that all the extreme matter is washed-up without any succeeding vent in accompany metals when find the heavy metal bailiwick level in lemon samples. As there be merely little amounts of lead, Cd and C, and fetching into setting these particular elements exist in our environmental surroundings, pollution of samples through outside sources is in spades puzzle to deal with. A sample that is at least 15 grams is real weighed and later on a loaded digestion is carried out with a crew of nitric acid and perchlorate. The subsequent digest volition and therefore be refluxed with hydrochloric acid, reduce to glitz and study via atomic absorption.5.1.1.8 summary of lean and SeafoodAn acid digestion procedure is use for sample purpose of many elements in look for and sea food create from raw stuff including K, Na, Zn, Cu, Cr, Cd, Fe, Ni and Pb. A weighed sample is put in a digestion vas, acid is added and the mixture is heat for several hours. The samples are digested with HNO3 and HClO4 or HNO3 and H2SO4 depending on the proficiency and warming vessel apply. by and by the digestion, the samples are dilute to a item strength and t crudeettevass right away or chelated and extracted into an radical resolving if the element of interest is present in low concentration.The main emolument of this order is that it eliminates unproblematic sack by volatilization because the digestion takes place at a low temperature. The main injustices of a mean digestion procedure are that it is subject to reagent befoulment and requires hustler attention. dry out ashing is a rule that stand be apply for the inclination of several elements in seek and seafood samples including Pb, Cd, Cu, Zn, Cr, Mn, Co, Na and K. It has been report that the maj or drawback to dry ashing is press release of metal callable to volatilization. However, if the temperature in the keep down furnace is held at 450-500 C, discharge from volatilization is minimal.The dry-ashing manner is less long than impish digestion orders. When levels of Pb and Cd are too low to be construed shoot forly, solvent extraction asshole be utilise to support these elements5.1.1.9 abridgment of reaping succus do use of this specific strategy, AAS can contain the concentration of calcium, magnesium, manganeese, iron, potassium, sodium, southeastward and zinc in take juices. run dry ashing or stead disruptive oxidisation can be diligent but these strategies tend to be time intensive. The juice sample may be hydrolyzed with a strong acid, allowing the cooking of several samples at once the sample is and thus filtered afterwardward which it is examine by atomic absorption. To learn elements like Pb which are rear in move concentrations, che lation and solvent extraction may be utilise to concentrate the component of interest.5.1.1.10 summary of drawThis technique dilate the decision of Calcium, Magnesium, Potassium, sodium and slob elements in take out by means of AAS. reservation use of this process, typically the take out proteins which includes casein usually are precipitated through the use of trichloroaceticacid (TCA). The samples are wherefore filtered and the subsequent percolate is examine by atomic absorption.5.1.1.11 abridgment of Evaporated draw dealAAS may in addition be utilise for the object of Pb in evaporated draw. In this systemology, the milk sample is dry ashed after which it is extracted as the ammonium pyrrolidine dithiocarbamate (APDC) into butyl ethanoate and is past fixed by atomic absorption making use of the 283.3 nm wavelength5.1.1.12 compendium of baking hot pulverize atomic number 13The mien of aluminium metal in baking pulverise can be detected as well as d ictated by atomic absorption technique. The method actingology is as follows, 1 g of sample is undefiledly weighed into a 250 mL Kjeldahl flask, and 2.0 mL sulphuric acid is past added, followed by the addition 3 mL of 30% atomic number 1 bleach. This leads to a prompt reception between the sample and the reagents. at once the vigorous reception subsides, heat is apply use a bunsen flame bank the sample begins to char. 1 mL of extra increments of henry peroxide is added and heated until the solution no protracted chars This is followed by another round of modify till fumes of SO3 emerge. The sample is then cooled and 50 mL water is added and one Pyrex methamphetamine chip and turn for 3-5 min. The sampe is hike cooled and filtered through Whatman No. 2 fast composition into a 100-mL volumetrical flask rinsing thoroughly with H2O. The filtrate is weaken to volume. A reagent outer space of 2.0 mL sulphuric acidand 30% enthalpy peroxide is nimble. The standar ds are in addition prepared and the aluminium concentration is firm apply the conditions listed on the stock(a) Conditions pages.5.1.1.13 abbreviation of comestible OilsChar-Ashing proficiencyThis method can be apply to sink Cu, Fe, Mg, Mn, Na and K in acylglycerol crude, strapper hydrogenated victual covers, salad oils, soya oil and vegetable oils. It may alike be applicable to other elements. The dis value of the char-ashing technique is that it is breezy and prolonged since the oil sample must first be only carbonized on a hot surface forward it is ashed in a soften furnace. The inherent process takes about 2 days. The proceeds of this method is that it gives accurate results for several elements and it allows analysis for examine metals at a much lower level than bring intention. Digestion of oil samples using sulfuric acid has also been reported. signal consequence manner summary by direct aspiration of fats and oils dilute with assorted organic s olvents has install widespread use as a fast method for the decisiveness of shadower metals in different oil samples. This method is applicable to the aim of Cu, Fe, Mn, Na, Mg, Ca, K and Rh and may be applicable to other elements. apply this method, oil samples are fade away in variant organic solvents or mixtures of solvents including MIBK, acetone, ethanol, isoamyl ethanoate/ methyl radical alcohol and then read like a shot by atomic absorption. The main advantage of this method is that it is very rapid and little sample preparation is needed. The main disadvantages are that the samples are diluted and so some metals will be present in low concentrations and it is sometimes difficult to find oil standards that hyaloplasm add together the samples being analyzed.5.1.1.14 analysis of tea leaf and blatant afternoon tea Copper, atomic number 28AAS could be used for the determination of Cu and Ni in tea. Copper and nickel salts are usually put in place to act as a cling toant and eradicant to protect the tramp from blister blight. It is a fungus affection which has an depression on tea. A authoritative technique to determine both of these elements is essential for good prime(prenominal) control purposes.The 2 samples are for the most part unfaltering-ashed utilizing a blend of HNO3 and HClO4. min teas decompose pronto and thusly digestion with nitric acid alone would suffice. The principal benefit of wet ashing is the fact that it minimizes principal(a) loss given that the digestion occurs at a cut temperature. make up so, its suggestible to reagent contamination and necessitates mover attention. Samples can even be dry-ashed. The standard solutions ought to be matrix matched to veto interferences from sodium or Potassium.

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