natgillin/translations-raw huggingface dataset:
Instrumentation:
Inštrumenti
reservoir of eluent, inert gas, degassing of the eluent, composition of the eluent, impurities,
zbiralnik za eluat, inertni plin, razplinjanje eluata, sestava eluata, nečistote,
pump, pulse dampener, injection system,
črpalka, blažilec tresljajev, injekcijski sistem,
separation columns (manufacturer, all information about the characteristics of the columns, such as pore size, kind of separation material, etc., number, length and order of the columns used),
separacijske kolone (proizvajalec, vse informacije o značilnostih kolon, kot so velikost por, vrsta separacije, material, itd., število, dolžina in zaporedje uporabljenih kolon),
number of the theoretical plates of the column (or combination), separation efficiency (resolution of the system),
število teoretičnih platojev kolone (ali kombinacije), učinkovitost separacije(resolucija sistema),
information on symmetry of the peaks,
informacije o simetriji vrhov,
column temperature, kind of temperature control,
temperatura kolone, vrste nadzora temperature,
detector (measurement principle, type, cuvette volume),
detektor (principi merjenja, tip, volumen kivete),
flowmeter if used (manufacturer, measurement principle),
merilec pretoka, če je uporabljen (proizvajalec, principi merjenja),
system to record and process data (hardware and software).
sistem zapisovanja in obdelovanja podatkov (strojna in programska oprema).
Calibration of the system:
Kalibriranje sistema
detailed description of the method used to construct the calibration curve,
podroben opis metode, uporabljene za sestavo kalibracijske krivulje,
information about quality criteria for this method (e.g. correlation coefficient, error sum of squares, etc.),
informacije o kriterijih kakovosti za to metodo (npr. korelacijski koeficient, vsota kvadratov odstopanj, itd.),
information about all extrapolations, assumptions and approximations made during the experimental procedure and the evaluation and processing of data,
informacije o vseh ekstrapolacijah, domnevah in približevanjih, opravljenih med poskusnim postopkom in ocenitev ter obdelava podatkov,
all measurements used for constructing the calibration curve have to be documented in a table which includes the following information for each calibration point:
vse uporabljene meritve za ustvarjanje kalibracijske krivulje morajo biti dokumentirane na tabeli, ki vsebuje naslednje informacije za vsako kalibracijsko točko:
name of the sample,
ime vzorca,
manufacturer of the sample,
proizvajalec vzorca,
characteristic values of the standards Mp, Mn, Mw, Mw/Mn, as provided by the manufacturer or derived by subsequent measurements, together with details about the method of determination,
značilne vrednosti standardov Mp, Mn, Mw in Mw/Mn, kot jih posreduje proizvajalec, ali kot so izpeljane iz naknadnih meritev, skupaj s podrobnostmi o metodi določanja,
injection volume and injection concentration,
injekcijski volumen in injekcijska koncentracija,
Mp value used for calibration,
Mp vrednost, uporabljena za kalibriranje,
elution volume or corrected retention time measured at the peak maxima,
elucijski volumen ali popravljeni retenzijski čas, izmerjen pri maksimumih vrha,
Mp calculated at the peak maximum,
Mp, izračunan na maksimumu vrha,
percentage error of the calculated Mp and the calibration value.
odstotek odstopanja od izračunanega Mpin kalibracijska vrednost.
Evaluation:
Ocenjevanje
evaluation on a time basis: methods used to ensure the required reproducibility (method of correction, internal standard, etc.),
ocena na časovni podlagi: metode, uporabljene za zagotovitev zahtevane obnovljivosti (metode popravljanja, interni standard, itd.),
information about whether the evaluation was effected on the basis of the elution volume or the retention time,
informacije o tem, ali je ocena izvedena na podlagi elucijskega volumna aliretenzijskega časa,
information about the limits of the evaluation if a peak is not completely analysed,
informacije o mejah ocenjevanja, če vrh ni analiziran v celoti,
description of smoothing methods, if used,
opis blažilnih metod, če so uporabljene,
preparation and pre-treatment procedures of the sample,
postopki priprave in predobdelave vzorca,
the presence of undissolved particles, if any,
prisotnost morebitnih neraztopljenih delcev,
injection volume (μl) and injection concentration (mg/ml),
injekcijski volumen (μl) in injekcijska koncentracija (mg/μl),
observations indicating effects which lead to deviations from the ideal GPC profile,
ugotovitve, ki kažejo na učinke, ki peljejo k odklonom od idealnega GPC profila,
detailed description of all modifications in the testing procedures,
podroben opis vseh sprememb v preskusnih postopkih,
details of the error ranges,
podrobnosti o stopnjah odstopanj,
any other information and observations relevant for the interpretation of the results.
vse druge informacije in ugotovitve, ki so pomembne za interpretacijo rezultatov.
DIN 55672(1995) Gelpermeationschromatographie (GPC) mit Tetrahydrofuran (THF) als Elutionsmittel, Teil 1.
DIN 55672 (1995) Gelpermeationschromatographie (GPC) mit Tetrahydrofuran (THF) als Elutionsmittel, Teil 1.
ASTM D 5296-92, (1992) Standard Test Method for Molecular Weight Averages and Molecular Weight Distribution of Polystyrene by High Performance Size-Exclusion Chromatography.
ASTM D 5296-92, (1992). Standard Test Method for Molecular Weight Averages and Molecular Weight Distribution of Polystyrene by High Performance Size – Exclusion Chromatography.
Examples of other methods for determination of number average molecular weight (Mn) for polymers
Primeri drugih metod za določanje povprečnega števila molekulske mase (Mn) za polimere
Gel permeation chromatography (GPC) is the preferred method for determination of Mn, especially when a set of standards are available, whose structure are comparable with the polymer structure.
Gelska permeacijska kromatografija (GPC) je priljubljena metoda za določanje Mn, zlasti kadar je na razpolago niz standardov, katerih struktura je primerljiva s strukturo polimera.
However, where there are practical difficulties in using GPC or there is already an expectation that the substance will fail a regulatory Mn criterion (and which needs confirming), alternative methods are available, such as:
Vendar pa v primeru, kadar naletimo pri uporabi metode GPC na izvedbene težave ali kadar lahko pričakujemo, da snov ne bo izpolnila regularnega Mn kriterija (in ki ga je potrebno potrditi), so na razpolago druge metode, kot so:
Use of colligative properties
Uporaba koligativnih lastnosti
Ebullioscopy/Cryoscopy
Ebulioskopija/krioskopija
involves measurement of boiling point elevation (ebullioscopy) or freezing point depression (cryoscopy) of a solvent, when the polymer is added.
vključuje meritev zvišanja vrelišča (ebulioskopija) ali znižanja strdišča (krioskopija) topila ob dodajanju polimera.
The method relies on the fact that the effect of the dissolved polymer on the boiling/freezing point of the liquid is dependent on the molecular weight of the polymer (1) (2).
Metoda se zanaša na dejstvo, da je učinek raztopljenega polimera na točki vrelišča/strdišča tekočine odvisen od molekulske mase polimera (1) (2).
Applicability, Mn < 20000.
Nanos: Mn < 20000.
Lowering of vapour pressure
Nižanje pritiska hlapov
involves the measurement of the vapour pressure of a chosen reference liquid before and after the addition of known quantities of polymer (1) (2).
vključuje meritev pritiska hlapov izbrane referenčne tekočine pred in po dodajanju znanih količin polimera (1) (2).
Applicability, Mn < 20000 (theoretically; in practice however of limited value).
Nanos: Mn < 20000 (teoretično; v praksi gre za mejno vrednost).
Membrane osmometry
Membranska osmometrija
relies on the principle of osmosis, i.e. the natural tendency of solvent molecules to pass through a semi-permeable membrane from a dilute to a concentrated solution to achieve equilibrium.
se zanaša na osmozo, t.j. naravno nagnjenost raztapljajočih se molekul, da predrejo skozi polprepustno membrano iz razredčila v koncentrirano raztopino, da bi se doseglo ravnovesje.
In the test, the dilute solution is at zero concentration, whereas the concentrated solution contains the polymer.
V preskusu je razredčena raztopina na nični koncentraciji, medtem ko koncentrirana raztopina vsebuje polimer.
The effect of drawing solvent through the membrane causes a pressure differential that is dependent on the concentration and the molecular weight of the polymer (1) (3) (4).
Učinek prehajanja topila skozi membrano povzroča diferencial pritiska, ki je odvisen od koncentracije in molekulske mase polimera (1) (3) (4).
Applicability, Mn between 20000 - 200000.
Nanos: Mn med 20000–200000.
Vapour phase osmometry
Osmometrija v hlapni fazi
involves comparison of the rate of evaporation of a pure solvent aerosol to at least three aerosols containing the polymer at different concentrations (1)(2)(4).
vključuje primerjavo stopnje hlapenja čistega raztopljenega aerosola na najmanj tri aerosole, ki vsebujejo polimer na različnih koncentracijah (1) (5) (6).
End-group analysis
Analiza končnih skupin
To use this method, knowledge of both the overall structure of the polymer and the nature of the chain terminating end groups is needed (which must be distinguishable from the main skeleton by, e.g. NMR or titration/derivatisation).
Da bi uporabili to metodo, sta potrebna tako celotna struktura polimera in narava verige, ki zaključuje končne skupine (ta se mora razlikovati od glavnega ogrodja po, na primer, NMR ali titriranju/derivatizaciji).
The determination of the molecular concentration of the end groups present on the polymer can lead to a value for the molecular weight (7) (8) (9).
Z določitvijo molekulske koncentracije končnih skupin, prisotnih na polimeru, lahko pridemo do vrednosti molekulske mase (7) (8) (9).
Applicability, Mn up to 50000 (with decreasing reliability).
Nanos: Mn do 50000 (z naraščajočo zanesljivostjo).
Slade, Jr. ed., Marcel Dekker, New York.
Slade, Jr. ed., Marcel Dekker, New York.
Coll, H. (1989) Membrane Osmometry.
Coll, H. (1989). membrane Osmometry.
Morris, C.E.M., (1989) Vapour Pressure Osmometry.
Morris, C.E.M., (1989). Vapour Pressure Osmometry.
This Gel Permeation Chromatographic method is a replicate of the OECD TG 119 (1996).
Ta gelska permeacijska kromatografija metoda je posnetek OECD smernice 119 (1996).
The fundamental principles and further technical information are given in the references.
Temeljna načela in nadaljnje tehnične informacije so navedene v literaturi 1.
Low molecular weight is arbitrarily defined as a molecular weight below 1000 dalton.
Nizka molekulska masa je arbitrarno opredeljena kot molekulska masa pod 1000 daltoni.
the level of the detector signal from the baseline for the retention volume Vi,
stopnja signala detektorja od osnovne črte za retenzijski volumen Vi
the molecular weight of the polymer fraction at the retention volume Vi, and n is the number of data points
molekulska masa frakcije polimera pri retenzijskem volumnu Vi in n število podatkovnih točk.
Since GPC is a relative method, calibration must be undertaken.
Ker je GPC relativna metoda, je treba opraviti kalibriranje.
Narrowly distributed, linearly constructed polystyrene standards with known average molecular weights Mn and Mw and a known molecular weight distribution are normally used for this.
Običajno za to uporabimo ozko porazdeljene, linearno strukturirane vzorce polistirena z znanimi povprečnimi molekulskimi masami Mn in Mw in znano porazdelitvijo molekulske mase.
Detection is effected by e.g. refractive index or UV-absorption and yields a simple distribution curve.
Ugotavljanje izvedemo, npr., na osnovi refrakcijskega indeksa ali UV absorpcije in dobimo preprosto distribucijsko krivuljo.
However, to attribute actual molecular weight values to the curve, it is necessary to calibrate the column by passing down polymers of known molecular weight and, ideally, of broadly similar structure, e.g. various polystyrene standards.
Da pa bi na krivulji opredelili dejanske vrednosti molekulske mase, moramo kalibrirati kolono, tako da skoznjo pretečejo polimeri z znano molekulsko maso in, v idealnem primeru, v glavnem podobno strukturo, npr. različni standardi polistirena.
The low molecular weight content is derived from this curve.
Vsebnost nizke molekulske mase izhaja iz te krivulje.
The calculation can only be accurate if the low molecular weight species respond equivalently on a per mass basis to the polymer as a whole.
Izračun je lahko točen le, če se vrste z nizko molekulsko maso ekvivalentno na osnovi mase odzivajo na polimer kot celota.
Correction for content of impurities and additives
Korekcija vsebnosti nečistot in aditivov
Correction of the content of species of M < 1000 for the contribution from non-polymer specific components present (e.g. impurities and/or additives) is usually necessary, unless the measured content is already < 1 %.
Ponavadi je nujno opraviti korekcijo vsebnosti vrst z M < 1000 za prispevek prisotnih nepolimerskih specifičnih sestavin (npr. nečistote in/ali aditivi), razen če je izmerjena vsebnost že < 1 %.
This is achieved by direct analysis of the polymer solution or the GPC eluate.
To izvedemo z direktno analizo polimerske raztopine ali GPC eluata.
In cases where the eluate, after passage through the column, is too dilute for a further analysis it must be concentrated.
V primerih, kadar je eluat pri prehajanju skozi kolono preveč razredčen za nadaljnjo analizo, ga je treba koncentrirati.
It may be necessary to evaporate the eluate to dryness and dissolve it again.
Mogoče bo potrebno izhlapeti eluat do suhega stanja in ga še enkrat raztopiti.
Concentration of the eluate must be effected under conditions which ensure that no changes occur in the eluate.
Koncentriranje eluata se mora izvesti v pogojih, ki zagotavljajo, da na eluatu ne pride do nikakršnih sprememb.
The treatment of the eluate after the GPC step is dependent on the analytical method used for the quantitative determination.
Tretiranje eluata po opravljeni GPC je odvisno od analitične metode, uporabljene za kvantitativno določitev.
GPC apparatus comprises the following components:
GPC aparat vsebuje naslednje komparente:
Selection of the separation gel or the length of the column is dependent on both the properties of the sample (hydrodynamic volumes, molecular weight distribution) and the specific conditions for separation such as solvent, temperature and flow rate (1) (2) (3).
Izbor separacijskega gela ali dolžine kolone je odvisen tako od lastnosti vzorca (hidrodinamični volumni, porazdelitev molekulske mase) in specifičnih pogojev za separacijo, kot so topilo, temperatura in pretok (1) (2) (3).
the peak widths at the base-1ine
širini vrha pri osnovni črti
the molecular weights at the peak maximum (should differ by a factor of 10).
molekulski masi pri maksimumu vrha (naj se razlikujeta s faktorjem 10).
The R-value for the column system should be greater than 1,7 (4).
R-vrednost sistema kolone mora biti večja od 1,7 (4).
It should not be larger than 10 μl except for light scattering and viscosity detectors.
Razen v primeru disperzije svetlobe in detektorjev viskoznosti ne sme presegati 10 μl.
Differential refractometry is usually used for detection.
Za detekcijo se navadno uporablja diferencialna refraktometrija.
In all cases it is essential to determine also data from blanks, treated under the same conditions as the sample.
V vseh primerih je bistveno, da določimo tudi podatke iz praznih polj, s katerimi smo ravnali v enakih pogojih kot vzorec.
If any insoluble polymer is retained on the column, its molecular weight is likely to be higher than that of the soluble fraction, and if not considered would result in an overestimation of the low molecular weight content.
Če na koloni ostane kak netopen polimer, bo njegova molekulska masa verjetno višja od mase topne frakcije; v kolikor je ne bi upoštevali, bi to lahko pripeljalo do previsoke ocene vsebnosti nizke molekulske mase.
Guidance for correcting the low molecular weight content for insoluble polymer is provided in the Appendix.
Smernice za korekcijo vsebnosti nizke molekulske mase za netopen polimer se nahajajo v Prilogi.
Information on the low molecular weight polymer content:
Informacije o vsebnosti nizke molekulske mase
description of the methods used in the analysis and the way in which the experiments were conducted,
opis uporabljenih metod pri analizi in način izvedbe poskusov,
information about the percentage of the low molecular weight species content (w/w) related to the total sample,
informacije o odstotkih vsebnosti vrst nizke molekulske mase (w/w), ki se nanaša na celotni vzorec,
information about impurities, additives and other non-polymer species in percentage by weight related to the total sample.
informacije o nečistotah, aditivih in drugih nepolimerskih vrstah v odstotkih po teži, ki se nanašajo na celoten vzorec.
evaluation on a time basis: all methods to ensure the required reproducibility (method of correction, internal standard etc.),
ocena na časovni podlagi: metode, uporabljene za zagotovitev zahtevane obnovljivosti (metode popravljanja, interni standard, itd.),
ASTM D 5296-92, (1992) Standard Test method for Molecular Weight Averages and Molecular Weight Distribution of Polystyrene by High Performance Size-Exclusion Chromatography.
ASTM D 5296-92, (1992). Standard Test method for Molecular Weight Averages and Molecular Weight Distribution of Polystyrene by High Performance Size-Exclusion Chromatography.
Guidance for correcting low molecular content for the presence of insoluble polymer
Smernice za korekcijo vsebnosti nizke molekulske mase pri prisotnosti netopnega polimera
When insoluble polymer is present in a sample, it results in mass loss during the GPC analysis.
Kadar je v vzorcu prisoten netopen polimer, lahko to povzroči izgubo mase v teku GPC analize.
The insoluble polymer is irreversibly retained on the column or sample filter while the soluble portion of the sample passes through the column.
Netopen polimer se lahko nepovratno ohrani na koloni ali filtru vzorca, medtem ko raztopni delež vzorca predre skozi kolono.
In the case where the refractive index increment (dn/dc) of the polymer can be estimated or measured, one can estimate the sample mass lost on the column.
V primeru, kadar je mogoče porast refrakcijskega indeksa (dn/dc) polimera oceniti ali izmeriti, lahko ocenimo maso vzorca, izgubljeno na koloni.
In that case, one makes a correction using an external calibration with standard materials of known concentration and dn/dc to calibrate the response of the refractometer.
V tem primeru, lahko opravimo korekcijo z uporabo zunanjega kalibriranja s standardnimi materiali znane koncentracije in dn/dc, da bi kalibrirali odziv refraktometra.
In the example hereafter a poly(methyl methacrylate) (pMMA) standard is used.
V naslednjem primeru je uporabljen standard poli(metil metakrilat) (pMMA).
In the external calibration for analysis of acrylic polymers, a pMMA standard of known concentration in tetrahydrofuran, is analysed by GPC and the resulting data are used to find the refractometer constant according to the equation:
Pri zunanjem kalibriranju za analizo akrilnih polimerov, z GPC analiziramo pMMA standard znane koncentracije v tetrahidrofuranu, dobljene podatke pa uporabimo, da poiščemo konstanto na refraktometru, v skladu z enačbo:
K the refractometer constant (in microvolt second/ml),
K konstanta refraktometra (v mikrovoltsekundah/ml),
R the response of the pMMA standard (in microvolt/second),
R odziv pMMA standarda (v mikrovoltsekundah),
C the concentration of the pMMA standard (in mg/ml),
C koncentracija pMMA standarda (v mg/ml),
V the injection volume (in ml), and
V injekcijski volumen (v ml) in
dn/dc the refractive index increment for pMMA in tetrahydrofuran (in ml/mg).
dn/dc porast refrakcijskega indeksa za pMMA v tetrahidrofuranu (v ml/mg)
The following data are typical for a pMMA standard:
Naslednji podatki so značilni za pMMA standard:
dn/dc 9 × 10-5 ml/mg
dn/dc = 9 × 10-5 ml/mg
The resulting K value, 3,05 × 1011 is then used to calculate the theoretical detector response if 100 % of the polymer injected had eluted through the detector.
Dobljeno K vrednost 3,05 × 1011 nato uporabimo za izračun odziva teoretičnega detektorja, če je 100 % vbrizganega polimera eluirano skozi detektor.
The method described is a replicate of the revised version of OECD TG 120 (1997).
Opisana metoda je v skladu s revidirano različico OECD smernice 120 (1997).
Further technical information is given in reference (1).
Nadaljnje tehnične informacije so navedene v literaturi (1).
For certain polymers, such as emulsion polymers, initial preparatory work may be necessary before the method set out hereafter can be used.
Za določene polimere, kot so emulzijski polimeri, bo mogoče potrebno opraviti začetno pripravo, preden se uporabi tukaj podana metoda.
The method is not applicable to liquid polymers and to polymers that react with water under the test conditions.
Metoda se ne uporablja pri tekočinskih polimerih in polimerih, ki v preskusnih pogojih reagirajo z vodo.
When the method is not practical or not possible, the solution/extraction behaviour may be investigated by means of other methods.
Kadar metoda ni izvedljiva ali mogoča, lahko obnašanje raztopine/izvlečka raziščemo s pomočjo drugih metod.
The solution/extraction behaviour of polymers in an aqueous medium is determined using the flask method (see A.6 Water Solubility, Flask method) with the modifications described below.
Obnašanje raztopine/izvlečka polimerov v vodnem gojišču določimo z uporabo metode z bučko (glej A.6 vodna topnost, metoda z bučko), upoštevajoč spodaj opisane spremembe.
The following equipment is required for the method:
Za metodo je potrebna naslednja oprema:
crushing device, e.g. grinder for the production of particles of known size,
drobilna naprava, npr. mlinček za proizvajanje delcev znane velikosti,
apparatus for shaking with possibility of temperature control,
aparat za tresenje z možnostjo nadzora temperature,
membrane filter system,
sistem membranskega filtra,
appropriate analytical equipment,
ustrezna oprema za analizo,
standardised sieves.
standardizirana sita.
A representative sample has first to be reduced to a particle size between 0,125 and 0,25 mm using appropriate sieves.
Reprezentativni vzorec je treba najprej z uporabo ustreznih sit zmanjšati na velikost delca med 0,125 in 0,25 mm.
Cooling may be required for the stability of the sample or for the grinding process.
Mogoče bo potrebno hlajenje, da se doseže stabilnost vzorca ali zaradi procesa drobitve.
Materials of a rubbery nature can be crushed at liquid nitrogen temperature (1).
Materiali gumijaste narave se lahko na temperaturi tekočega dušika zdrobijo (1).
If the required particle size fraction is not attainable, action should be taken to reduce the particle size as much as possible, and the result reported.
Če zahtevane frakcije velikosti delca ni mogoče doseči, je treba velikost delca zmanjšati, kolikor je mogoče, in poročati o rezultatu.
In the report, it is necessary to indicate the way in which the crushed sample was stored prior to the test
V poročilu je treba označiti, kako smo zdrobljen vzorec hranili pred preskusom.
Three samples of 10 g of the test substance are weighed into each of three vessels fitted with glass stoppers and 1000 ml of water is added to each vessel.
Tri vzorce po 10 g preskusne snovi odmerimo v vsako izmed treh posod, zaprtih s steklenimi zamaški, in v vsako posodo dodamo 1000 ml vode.
If handling an amount of 10 g polymer proves impracticable, the next highest amount which can be handled should be used and the volume of water adjusted accordingly.
Če se izkaže, da je ravnanje s količino 10 g polimera neizvedljivo, je treba uporabiti naslednjo najvišjo količino, s katero je mogoče ravnati, in temu ustrezno prilagoditi količino vode.
The vessels are tightly stoppered and then agitated at 20 oC.
Posode tesno zamašimo in jih pretresemo pri 20 oC.
A shaking or stirring device capable of operating at constant temperature should be used.
Uporabiti moramo napravo za tresenje ali mešanje, ki lahko deluje na stalni temperaturi.