SIST EN 15199-2:2021
(Main)Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 2: Heavy distillates and residual fuels
Petroleum products - Determination of boiling range distribution by gas chromatography method - Part 2: Heavy distillates and residual fuels
This European Standard specifies a method for the determination of the boiling range distribution of petroleum products by capillary gas chromatography using flame ionisation detection. The standard is applicable to materials having a vapour pressure low enough to permit sampling at ambient temperature, and which have a boiling range of at least 100 °C. The standard is applicable to materials with initial boiling points (IBP) above 100 °C and final boiling points (FBP) above 750 °C, for example, heavy distillate fuels and residuals. The method is not applicable to bituminous samples.
The test method is not applicable for the analysis of petroleum or petroleum products containing low molecular weight components (for example naphthas, reformates, gasolines, diesel). Components containing hetero atoms (for example alcohols, ethers, acids, or esters) or residue are not to be analyzed by this test method.
NOTE For the purposes of this European Standard, the terms "% (m/m)" and "% (V/V)" are used to represent respectively the mass fraction and the volume fraction.
WARNING - The use of this European Standard may involve hazardous materials, operations and equipment. This European Standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use.
Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil 2: Schweröle und Rückstandsöle
1 Anwendungsbereich
Dieses Dokument legt ein Verfahren zur Bestimmung des Siedeverlaufes in Mineralölerzeugnissen mit Hilfe der Kapillar-Gaschromatographie mit einem Flammenionisationsdetektor (FID) fest. Die Norm ist anwendbar für Mineralölerzeugnisse mit einem für die Probenahme bei Umgebungstemperatur ausreichend niedrigen Dampfdruck und mit einem Siedebereich von mindestens 100 °C. Die Norm ist anwendbar für Mineralölerzeugnisse mit einem IBP oberhalb von 100 °C und mit einem FBP oberhalb von 750 °C, wie z. B. Schweröle und Rückstandsöle. Für bituminöse Proben ist dieses Verfahren nicht geeignet.
Das Prüfverfahren ist nicht anzuwenden für die Analyse von Mineralöl oder Mineralölerzeugnissen mit niedermolekularen Anteilen (z. B. Naphtha, Reformat, Ottokraftstoff) oder Mitteldestillaten, wie z. B. Diesel und Flug (turbinen )kraftstoff.
Mineralöl oder Mineralölerzeugnisse, die Blendkomponenten mit Heteroatomen enthalten (z. B. Alkohole, Ether, Säuren oder Ester) oder Rückstände sind mit diesem Prüfverfahren nicht zu untersuchen.
ANMERKUNG Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils einer Substanz der Ausdruck „% (m/m)“ und für den Volumenanteil einer Substanz der Ausdruck „% (V/V)“ verwendet.
WARNUNG - Die Anwendung dieses Dokuments kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Dieses Dokument beansprucht nicht, alle damit verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung des Anwenders dieser Norm, vor der Anwendung angemessene Maßnahmen in Hinblick auf Sicherheit und Gesundheit zu ergreifen und die Anwendbarkeit einschränkender Vorschriften zu ermitteln.
Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par méthode de chromatographie en phase gazeuse - Partie 2: Fiouls lourds et fiouls résiduels
Le présent document prescrit une méthode de détermination de la répartition dans l’intervalle de distillation des produits pétroliers par chromatographie en phase gazeuse capillaire avec une détection par ionisation de flamme. La norme s’applique aux produits dont la pression de vapeur est suffisamment faible pour permettre l’échantillonnage à la température ambiante et dont l’intervalle de distillation est d’au moins 100 °C. La norme s’applique aux produits dont le point d’ébullition initial (IBP) est supérieur à 100 °C et le point d’ébullition final (FBP) est supérieur à 750 °C, par exemple, les fiouls lourds et les fiouls résiduels. Cette méthode ne s’applique pas aux produits bitumineux.
Cette méthode d’essai ne s’applique pas pour l’analyse de pétrole ou de produits pétroliers ayant des composants de faible masse moléculaire (par exemple naphtas, réformats, carburants essences ou distillats moyens comme les carburants diesel et les carburéacteurs).
Le pétrole ou les produits pétroliers contenant en mélange des composés avec des hétéro-atomes (par exemple alcools, éthers, acides ou esters) ou les résidus ne peuvent pas être analysés suivant cette méthode.
NOTE Pour les besoins du présent document, les termes "% (m/m)" et "% (V/V)" sont utilisés pour représenter respectivement la fraction massique et la fraction volumique.
Naftni proizvodi - Določanje porazdelitve območja vrelišč z metodo plinske kromatografije - 2. del: Težki destilati in goriva iz destilacijskih ostankov
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 15199-2:2021
01-marec-2021
Nadomešča:
SIST EN 15199-2:2006
Naftni proizvodi - Določanje porazdelitve območja vrelišč z metodo plinske
kromatografije - 2. del: Težki destilati in goriva iz destilacijskih ostankov
Petroleum products - Determination of boiling range distribution by gas chromatography
method - Part 2: Heavy distillates and residual fuels
Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil 2:
Schweröle und Rückstandsöle
Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par
méthode de chromatographie en phase gazeuse - Partie 2: Fiouls lourds et fiouls
résiduels
Ta slovenski standard je istoveten z: EN 15199-2:2020
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
75.160.01 Goriva na splošno Fuels in general
SIST EN 15199-2:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 15199-2:2021
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SIST EN 15199-2:2021
EN 15199-2
EUROPEAN STANDARD
NORME EUROPÉENNE
December 2020
EUROPÄISCHE NORM
ICS 75.080 Supersedes EN 15199-2:2006
English Version
Petroleum products - Determination of boiling range
distribution by gas chromatography method - Part 2:
Heavy distillates and residual fuels
Produits pétroliers - Détermination de la répartition Mineralölerzeugnisse - Gaschromatographische
dans l'intervalle de distillation par méthode de Bestimmung des Siedeverlaufes - Teil 2: Schweröle und
chromatographie en phase gazeuse - Partie 2 : Fiouls Rückstandsöle
lourds et fiouls résiduels
This European Standard was approved by CEN on 23 November 2020.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 15199-2:2020 E
worldwide for CEN national Members.
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SIST EN 15199-2:2021
EN 15199-2:2020 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 6
5 Reagents and materials . 6
6 Apparatus . 9
7 Sampling . 11
8 Preparation of the apparatus . 11
8.1 Gas chromatograph preparation . 11
8.2 System performance check . 11
9 Sample and reference material preparation . 11
10 Calibration . 12
11 Procedure . 14
12 Visual inspection of the chromatograms . 15
13 Calculation . 15
14 Expression of results . 15
15 Precision . 15
15.1 General . 15
15.2 Repeatability . 15
15.3 Reproducibility . 15
16 Test report . 17
Annex A (normative) Calculation procedure . 18
Annex B (normative) System performance check . 21
Annex C (normative) Boiling points of n-alkanes. 23
Annex D (informative) Additional guidance for the calculation algorithm . 25
Bibliography . 29
2
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SIST EN 15199-2:2021
EN 15199-2:2020 (E)
European foreword
This document (EN 15199-2:2020) has been prepared by Technical Committee CEN/TC 19 “Gaseous and
liquid fuels, lubricants and related products of petroleum, synthetic and biological origin”, the secretariat
of which is held by NEN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by June 2021, and conflicting national standards shall be
withdrawn at the latest by June 2021.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 15199-2:2006.
The main changes in this edition include:
— updated text to give better guidance to operators executing the test;
— additional clarification in the sample preparation section.
EN 15199 consists of the following parts, under the general title Petroleum products — Determination of
boiling range distribution by gas chromatography method:
— Part 1: Middle distillates and lubricating base oils;
— Part 2: Heavy distillates and residual fuels;
— Part 3: Crude oil;
— Part 4: Light fractions of crude oil.
This document specifies the determination of boiling range distribution of materials with initial boiling
points (IBP) above 100 °C and final boiling points (FBP) above 750 °C. For testing materials with initial
boiling points (IBP) above 100 °C and final boiling point (FBP) below 750 °C, Part 1 of the standard can be
used. For testing materials with initial boiling points (IBP) below 100 °C and final boiling points (FBP)
above 750 °C, such as crude oils, Part 3 is applicable. Part 4 describes the determination of boiling range
distribution of hydrocarbons up to n-nonane in crude oil.
This document is a joint development between the EI [5], ASTM [4] and CEN.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United
Kingdom
3
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EN 15199-2:2020 (E)
1 Scope
This document specifies a method for the determination of the boiling range distribution of petroleum
products by capillary gas chromatography using flame ionization detection. The standard is applicable to
materials having a vapour pressure low enough to permit sampling at ambient temperature, and which
have a boiling range of at least 100 °C. The standard is applicable to materials with initial boiling points
(IBP) above 100 °C and final boiling points (FBP) above 750 °C, for example, heavy distillate fuels and
residuals. The method is not applicable to bituminous samples.
The test method is not applicable for the analysis of petroleum or petroleum products containing low
molecular weight components (for example naphthas, reformates, gasolines) or middle distillates like
Diesel and Jet fuel.
Petroleum or petroleum products containing blending components, which contain hetero atoms (for
example alcohols, ethers, acids, or esters) or residue, are not to be analysed by this test method.
NOTE For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent respectively
the mass fraction and the volume fraction.
WARNING — The use of this document may involve hazardous materials, operations and equipment. This
document does not purport to address all of the safety problems associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety and health practices and to
determine the applicability of regulatory limitations prior to use.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170)
EN ISO 3171, Petroleum liquids — Automatic pipeline sampling (ISO 3171)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
3.1
initial boiling point
IBP
temperature corresponding to the retention time at which a net area (3.7) counts equal to 0,5 % of the
total sample area (3.6) under the chromatogram is obtained (see Figure 1)
3.2
final boiling point
FBP
temperature corresponding to the retention time at which a net area (3.7) counts equal to 99,5 % of the
total sample area (3.6) under the chromatogram is obtained (see Figure 1)
4
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EN 15199-2:2020 (E)
Key
1 start of elution 4 end of elution
2 IBP (3.1) X retention time (minutes)
3 FBP (3.2) Y response (pA)
Figure 1 — Typical chromatogram
3.3
area slice
area resulting from the integration of the chromatographic detector signal within a specified retention
time interval
Note 1 to entry: In area slice mode peak detection parameters are bypassed and the detector signal integral is
recorded as area slices of consecutive, fixed duration time interval.
3.4
corrected area slice
area slice (3.3) corrected for baseline offset by subtraction of the exactly corresponding area slice (3.3) in
a previously recorded blank (non-sample) analysis
3.5
cumulative corrected area
accumulated sum of corrected area slices (3.4) from the beginning of the analysis through a given
retention time, ignoring any non-sample area for example of solvent
3.6
total sample area
cumulative corrected area (3.5), from the initial area point to the final area point, where the
chromatographic signal has returned to baseline after complete sample elution
3.7
net area
cumulative area counts for the sample minus the cumulative area count for the blank
5
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EN 15199-2:2020 (E)
3.8
recovery
ratio of the cumulative area count of the sample to that of the reference material (external standard)
corrected for dilution and material weights combined with the percentage of light ends, if applicable
4 Principle
A test portion is introduced into a gas chromatographic column, which separates hydrocarbons in the
order of increasing boiling point. The column temperature is raised at a linear reproducible rate and the
area under the chromatogram is recorded throughout the analysis. Boiling points are assigned to the time-
axis from a calibration curve, which is obtained by running a mixture of known n-alkanes covering the test
portion boiling range, under the same conditions. From these data, the boiling range distribution is
obtained. The recovery (3.8) at a specified temperature is determined by comparing the area under the
chromatogram with that of a reference standard which has been completely eluted. The temperature at
which the recovery was measured is recorded. If the found recovery is less than 100 %, the final boiling
point (3.2) is reported as 720 °C or 750 °C at that recovery.
Several SIMDIS methods are standardized test methods and each one is dedicated to a certain boiling point
range or product.
EN ISO 3924 [2] is limited to products having an initial boiling point greater than 55 °C, a final boiling
point lower than 538 °C and having a vapour pressure sufficiently low to permit sampling at ambient
temperature.
EN 15199-1 [1] is applicable to materials having a boiling range of at least 100 °C, an initial boiling points
(IBP) above 100 °C and final boiling points (FBP) below 750 °C, for example, middle distillates and
lubricating base stocks.
EN 15199-3 is applicable to crude oils. The boiling range distribution and recovery up to C or C can
100 120
be determined.
5 Reagents and materials
Unless otherwise stated, only chemicals of recognized analytical quality shall be used.
5.1 Carrier gas, helium, of at least 99,999 % (V/V) purity. Any oxygen present is removed by a chemical
resin filter.
WARNING — Follow the safety instructions from the filter supplier.
5.2 Hydrogen, grade suitable for flame ionization detectors.
5.3 Compressed air, suitable for flame ionization detectors.
5.4 Alkanes, n-alkanes of at least 98 % (m/m) purity from C to C , C , C , C , C , C , C and
5 10 12 14 16 18 20 24
C .
28
NOTE The calibration mixture from EN ISO 3924 [2] is also suitable.
5.5 Polywax 655 or 1000
5.6 Carbon disulfide(CS ), with a minimum purity of 99,7 % (V/V).
2
WARNING — Extremely flammable and toxic.
6
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EN 15199-2:2020 (E)
CAUTION — It is recommended that all work with CS is carried out in an explosion protected fume
2
cupboard.
Cyclohexane (C H )—(>99 % pure) can be used in place of CS for the preparation of the calibration
6 12 2
mixture. However, the precision of this method is based on calibration mixtures, reference material and
samples prepared with CS only.
2
5.7 Calibration mixture
Dissolve 0,1 g of Polywax (5.5) in 7 ml CS (5.6), warming gently if necessary. Prepare an equal volume
2
mixture of alkanes (5.4) and add 10 µl to the Polywax solution.
NOTE 1 Commercially available alkane standards are suitable for column performance checks.
NOTE 2 The calibration mix is used to determine the column resolution, skewness of the C peak, and retention
20
time versus boiling point calibration curve.
5.8 Reference materials
5.8.1 A reference material has two functions:
— External Standard: to determine the recovery (3.8) of samples by comparing the total sample area
(3.6) of the reference material with the total sample area (3.6) of the unknown sample.
— Boiling Point Distribution Standard: to check the proper functioning of the system by comparing the
results with a known boiling point distribution on a routine basis. Typical example is given in (5.8.2).
5.8.2 Reference Material 5010, a reference sample that has been analysed by laboratories
participating in the test method cooperative study. Consensus values for the boiling range distribution of
this sample are given in Table 1.
5.8.3 Binary gravimetric blend, a binary distillate mixture with boiling points ranges that gives a
baseline at the start, a baseline between the two peaks and an end time that is as close to the end of the
chromatogram as possible (see Figure 2 and B.3). This mixture is used to check the relative response of
the two distillates and to check the baselines at the start, middle and end of the chromatogram.
7
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Table 1 — Reference Material 5010
Accepted
% Maximum allowable range
Reference
recovered 95,5 % Confidence Interval
value
°C °C
IBP 428 9
5 477 3
10 493 3
15 502 3
20 510 3
25 518 4
30 524 4
35 531 4
40 537 4
45 543 4
50 548 5
55 554 4
60 560 4
65 566 4
70 572 4
75 578 5
80 585 4
85 593 4
90 602 4
95 616 4
FBP 655 18
8
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Key
Y response (pA)
X retention time (minutes)
Figure 2 — Typical chromatogram of binary gravimetric blend distillate
6 Apparatus
6.1 Gas chromatograph, with the following performance characteristics.
6.1.1 Flame ionization detector, connected to the column so as to avoid any cold spots. The detector
shall be capable of operating at a temperature at least equivalent to the maximum column temperature
employed in the method.
6.1.2 Column temperature programmer, capable of linear programmed temperature operation over
a range of 10 °C above ambient to 450 °C.
6.1.3 Sample inlet system, consisting of a programmable temperature vaporizer (PTV) or cold on-
column (COC) injection port. The maximum temperature of the injection device shall be equal to, or higher
than, the final oven temperature. The minimum temperature shall be low enough to prevent sample or
solvent flashback, but high enough to allow sample focusing at the front of the column. Table 2 contains
the typical operating conditions.
6.2 Column
6.2.1 The capillary column should sit just below the flame tip and it is recommended that the orifice of
the jet should be 0,6 mm minimum to prevent frequent blocking with silicones.
6.2.2 Use a metal column with 0,53 mm internal diameter and coated with methyl silicone. Commercially
available columns with film thickness (d ) = 0,09 µm (for analysis up to C ) and (d ) = 0,17 µm (for
f 120 f
analysis up to C ) have been found to be satisfactory.
100
It is recommended that the column resolution, R, is at least 2 and not more than 4 (see B.2).
6.2.3 Use some form of column bleed compensation to obtain a stable baseline. This can be carried out by
subtraction of a column bleed profile previously obtained using exactly the same conditions as used for
the sample analysis, by injecting the same volume, using solvent for the blank run and sample dilution
from one batch taken at the same time, to avoid differences due to contamination.
9
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Table 2 — Typical operating conditions for gas chromatograph
Unit Specification
Column length m 5
Column internal diameter mm 0,53
Column material — Ultimetal
Stationary phase — Methyl silicone
Film thickness µm 0,09 or 0,17
Initial column temperature °C 35
Final column temperature °C 430
Program rate °C/min 10
Injector initial temperature °C 100
Injector final temperature °C 430
Program rate °C/min 15
Hold time min 5
Detector temperature °C 450
Detector hydrogen flow rate (5.2) ml/min 35
Detector air flow rate (5.3) ml/min 350
Carrier gas — Helium
a
Carrier gas flow rate ml/min 19
Sample size µl 1,0
Sample concentration % (m/m) 2
Injector — PTV or COC
a
A carrier gas flow rate up to 25 ml/min can be used to ensure all material elutes before the end of the
temperature program.
6.3 Carrier gas control
The chromatograph shall be able to deliver a constant carrier gas flow over the whole temperature range
of the analysis.
6.4 Micro-syringe, of appropriate volume, e.g. 10 µl, for introduction of 1 µl of the calibration mixture
and test portions. Plunger in needle syringes are not recommended due to excessive carry over of heavy
ends to the following analysis.
6.5 Volumetric flask, 10 ml capacity.
6.6 Refrigerator, shall be of an explosion-protected design.
6.7 Analytical balance, capable of weighing to the nearest 0,1 mg.
10
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7 Sampling
Samples shall be taken as specified in EN ISO 3170 or EN ISO 3171 (see the requirements of national
standards or regulations for the sampling of petroleum products for further information).
Store samples in either glass or metal containers. Plastic containers for sample storage shall not be used
as prolonged contact with the sample can cause contamination of the sample due to possible leaching of
the plasticizer.
8 Preparation of the apparatus
8.1 Gas chromatograph preparation
8.1.1 Set up and operate the gas chromatograph (6.1) in accordance with the manufacturer’s
instructions.
Typical operating conditions are shown in Table 2.
8.1.2 Deposits can form on the jet from combustion of decomposition products from the liquid
stationary phase. These will affect the characteristics of the detector and shall be removed.
NOTE The following parameters are affected by deposits on the jet: increase in inlet pressure; FID difficult to
light; increase in the CS response and an off specification reference material. To clean the jet, an ultrasonic cleaner
2
with a suitable solvent, and a cleaning wire can be used.
8.2 System performance check
Check the system performance at the intervals given and by the procedures specified in Annex B.
9 Sample and reference material preparation
9.1 Mix the sample by shaking, warming prior to shaking where necessary.
9.2 Weigh approximately 0,1 g to 0,3 g of the sample to the nearest 0,1 mg, into a clean 10 ml volumetric
flask (6.5) and add 5 ml to 7 ml CS (5.6).
2
Shake the mixture to completely dissolve the test portion and then add CS (5.6) to the mark. Immediately
2
transfer the solution to auto test portion vials, seal, and store in a refrigerator until ready for use.
If the density of the sample is known, the test portion can be prepared on a mass/mass basis, and the
following correction applied:
100m
m
1
% = (1)
V
mm
22
+
σσ
12
where
m is the mass of the test portion, in g;
1
m is the mass of CS (5.6), in g;
2
2
σ is the density of the test portion at 20 °C, in kg/l;
1
3
σ is the density of CS (5.6) at 20 °C, in kg/m ; (= 1,26).
2
2
11
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NOTE The density is quoted at 20 °C as a temperature approximately ambient in most laboratories. Appropriate
adjustments can be made if the laboratory temperature is outside (20 ± 5) °C.
9.3 Sample preparation is important to calculate the recovery (3.8) of the sample. The sample can be
prepared by weighing the sample in a 10 ml flask as specified. Using this procedure, it is not required to
know or measure the density of the sample. Due to the low boiling point and the health restrictions of CS
2
it is preferred to prepare the sample by weight and correct for the density.
9.4 When the density is unknown and therefore no correction can be applied, the error in the recovery
calculation is minor. Not correcting for density can result in a deviation of at most 1 % on the recovery
3 3
(3.8) for the density range 700 kg/m to 1 000 kg/m .
10 Calibration
10.1 It is highly recommended to carry out the steps given in 10.2 to 10.4 each day before sample analysis.
The first run of the day shall not be a blank, a reference material or a sample, due to the possible elution
of extraneous components, which have built up in the injector, but it may be the calibration mixture (5.7).
10.2 Run the calibration mixture (5.7) as specified in Clause 11.
Take care to ensure the test portion volume chosen does not allow any peak to exceed the linear range of
the detector, or overload the column. Determine the skewness according to Annex B System Performance
(B4). A skew of > 3 indicates the sample is too concentrated and a skew of < 1 indicates an old column or
dirty liner. As a guide, 1 µl of the calibration mixture (5.7) has been found to be suitable for columns with
film thickness less than 0,17 µm.
10.3 Record the retention time of each component and plot the retention time versus the atmospheric
boiling point for each component to obtain the calibration curve.
NOTE The atmospheric boiling points of the alkanes (5.4 and 5.5) are given in Annex C.
A typical chromatogram of the calibration mixture (5.7) is given in Figure 3 and a typical calibration curve
is given in Figure 4.
10.4 Run the reference material (5.8.2) using the specified procedure in Clause 11. Calculate the boiling
range distribution of the reference material by the procedures specified in Annex A and compare this with
the consensus values for the reference material used.
If the results are not within the specified range, it is advised to carefully follow the manufacturer’s
instructions regarding chromatographic problem solving and related diagnostics.
12
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Key
Y response (pA)
X retention time (minutes)
Figure 3 — Typical chromatogram of calibration mixture
Key
Y response (pA)
X retention time (minutes)
Figure 4 — Typical calibration curve
13
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11 Procedure
11.1 Run a solvent (blank) baseline analysis before the first sample analysis, and then after every five
samples. Using the data system, merge the blank baselines and the subsequent analyses and observe the
last part of the chromatogram. The baseline shall look like example a in Figure 5.
NOTE It is good practice to follow each test portion with a CS2 (5.6) blank to prevent carryover of heavy non-volatile
material into the next analysis.
a) good baseline b) bad baseline c) bad baseline
merging parallel crossing
(high FBP) (low FBP)
Figure 5 — Baselines
The peak shape of the CS and the identification of a constant baseline at the end of the run is critical to
2
the analysis. Constant attention shall be given to all factors that influence the peak shape and the baseline
stability, e.g. column substrate bleed, septum bleed, detector temperature control, constancy of carrier gas
(5.1) flow, leaks and instrument drift. The peak shape of the CS is influenced by the cleanliness of the liner
2
and or the connection between the column and the liner (Figure 6). The baseline at the end of each analysis
shall merge with the baseline of the blank run associated with it. Both signals shall merge to confirm
integrity; if they do not, the analysis shall be repeated.
Key
A good
B bad
Figure 6 — Solvent Peak Shape
11.2 Run the calibration and the reference sample according to Clause 10 under the same analysis
circumstances, see Table 2.
11.3 Verify the system performance check as specified in Annex B, and when they passed the
...
SLOVENSKI STANDARD
oSIST prEN 15199-2:2019
01-december-2019
Naftni proizvodi - Določanje porazdelitve območja vrelišč z metodo plinske
kromatografije - 2. del: Težki destilati in goriva iz destilacijskih ostankov
Petroleum products - Determination of boiling range distribution by gas chromatography
method - Part 2: Heavy distillates and residual fuels
Mineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil
2: Schweröle und Rückstandsöle
Produits pétroliers - Détermination de la répartition dans l'intervalle de distillation par
méthode de chromatographie en phase gazeuse - Partie 2: Fiouls lourds et fiouls
résiduels
Ta slovenski standard je istoveten z: prEN 15199-2
ICS:
75.080 Naftni proizvodi na splošno Petroleum products in
general
75.160.01 Goriva na splošno Fuels in general
oSIST prEN 15199-2:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 15199-2:2019
DRAFT
EUROPEAN STANDARD
prEN 15199-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2019
ICS 75.080 Will supersede EN 15199-2:2006
English Version
Petroleum products - Determination of boiling range
distribution by gas chromatography method - Part 2:
Heavy distillates and residual fuels
Produits pétroliers - Détermination de la répartition Mineralölerzeugnisse - Gaschromatographische
dans l'intervalle de distillation par méthode de Bestimmung des Siedeverlaufes - Teil 2: Schweröle und
chromatographie en phase gazeuse - Partie 2: Fiouls Rückstandsöle
lourds et fiouls résiduels
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 19.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations
which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC
Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15199-2:2019 E
worldwide for CEN national Members.
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Contents Page
European foreword . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 7
5 Reagents and materials . 7
6 Apparatus . 10
7 Sampling procedure . 11
8 Preparation of the apparatus . 11
8.1 Gas chromatograph preparation . 11
8.2 System performance check . 12
9 Sample and reference material preparation . 12
10 Calibration . 12
11 Procedure . 14
12 Visual inspection of the chromatograms . 15
13 Calculation . 15
14 Expression of results . 15
15 Precision . 15
15.1 General . 15
15.2 Repeatability . 15
15.3 Reproducibility . 15
16 Test report . 16
Annex A (normative) Calculation procedure . 17
A.1 Application . 17
A.2 Starting conditions . 17
A.3 Zero sample or reference chromatogram . 17
A.4 Sample area . 17
A.5 Start of sample elution time . 17
A.6 End of sample elution time . 18
A.7 End of reference material elution time . 18
A.8 Corrected sample or reference material area . 18
A.9 Normalization . 18
A.10 Conversion of retention time to percent off . 18
A.10.1 Initial boiling point . 18
A.10.2 Intermediate boiling points . 19
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A.11 Conversion of retention times to boiling points . 19
Annex B (normative) System performance check . 20
B.1 Frequency . 20
B.2 Column resolution . 20
B.3 Detector response (gravimetric blend) . 20
B.4 Skewing of peak . 21
Annex C (informative) Boiling points of normal alkanes . 22
Annex D (informative) Additional guidance for the calculation algorithm . 24
D.1 Zeroing of the reference material chromatogram . 24
D.2 Zeroing of sample chromatograms . 24
D.3 Blank baseline subtraction from the sample chromatogram . 25
D.4 Quenching correction . 25
D.5 Determination of the sample final elution time (t ) . 25
FE
D.6 Determination of the sample area . 25
D.7 Response factor . 26
D.8 Calculation of the percentage recovery . 26
D.9 Determination of the boiling point distribution . 27
D.10 Calculation of cut point intervals . 27
Bibliography . 28
3
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European foreword
This document (prEN 15199-2:2019) has been prepared by Technical Committee CEN/TC 19 “Gaseous
and liquid fuels, lubricants and related products of petroleum, synthetic and biological origin”, the
secretariat of which is held by NEN.
This document is currently submitted to the CEN Enquiry.
EN 15199 consists of the following parts, under the general title Petroleum products — Determination of
boiling range distribution by gas chromatography method:
— Part 1: Middle distillates and lubricating base oils
— Part 2: Heavy distillates and residual fuels
— Part 3: Crude oil
— Part 4: Light fractions of crude oil
This part of the standard describes the determination of boiling range distribution of materials with
initial boiling points (IBP) above 100 °C and final boiling points (FBP) above 750 °C. For testing
materials with initial boiling points (IBP) above 100 °C and final boiling point (FBP) below 750 °C, Part 1
of the standard may be used. For testing materials with initial boiling points (IBP) below 100 °C and final
boiling points (FBP) above 750 °C, such as crude oils, Part 3 is applicable.
This part of the standard is a joint development between the EI [1], ASTM [2] and CEN.
This second edition cancels and replaced the first edition (EN 15199-2:2006) which is updated
editorially and contains additional clarification in the sample preparation section.
4
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1 Scope
This document specifies a method for the determination of the boiling range distribution of petroleum
products by capillary gas chromatography using flame ionization detection. This document is applicable
to materials having a vapour pressure low enough to permit sampling at ambient temperature, and
which have a boiling range of at least 100 °C. This document is applicable to materials with initial boiling
points (IBP) above 100 °C and final boiling points (FBP) above 750 °C, for example, heavy distillate fuels
and residuals. The method is not applicable to bituminous samples.
The test method is not applicable for the analysis of petroleum or petroleum products containing low
molecular weight components (for example naphthas, reformates, gasolines, diesel). Components
containing hetero atoms (for example alcohols, ethers, acids, or esters) or residue are not to be analysed
by this test method.
NOTE For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent
respectively the mass fraction, µ, and the volume fraction, φ.
WARNING — The use of this European Standard may involve hazardous materials, operations and
equipment. This European Standard does not purport to address all of the safety problems associated
with its use. It is the responsibility of the user of this standard to establish appropriate safety and health
practices and to determine the applicability of regulatory limitations prior to use.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170:2004)
EN ISO 3171, Petroleum liquids — Automatic pipeline sampling (ISO 3171:1988)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at http://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
Note 1 to entry: Explanation of some of the terms is given in Figure 1.
3.1
initial boiling point
IBP
temperature corresponding to the retention time at which a net area (3.7) counts equal to 0,5% of the
total sample area (3.6) under the chromatogram is obtained
3.2
final boiling point
FBP
temperature corresponding to the retention time at which a net area (3.7) counts equal to 99,5% of the
total sample area (3.6) under the chromatogram is obtained
5
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3.3
area slice
area resulting from the integration of the chromatographic detector signal within a specified retention
time interval
Note 1 to entry: In area slice mode peak detection parameters are bypassed and the detector signal integral is
recorded as area slices of consecutive, fixed duration time interval.
Key
1 start of elution
2 initial boiling point (IBP) (3.1)
3 final boiling point (FBP)
4 end of elution
X min
Y pA
Figure 1 — Typical chromatogram
3.4
corrected area slice
area slice (3.3) corrected for baseline offset by subtraction of the exactly corresponding area slice (3.3)
in a previously recorded blank (non-sample) analysis
3.5
cumulative corrected area
accumulated sum of corrected area slices (3.4) from the beginning of the analysis through a given
retention time, ignoring any non-sample area for example of solvent
3.6
total sample area
cumulative corrected area (3.5), from the initial area point to the final area point, where the
chromatographic signal has returned to baseline after complete sample elution
6
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3.7
net area
cumulative area counts for the sample minus the cumulative area count for the blank
3.8
recovery
ratio of the cumulative area count of the sample to that of the reference material (external standard)
corrected for dilution and material weights combined with the percentage of light ends, if applicable
4 Principle
A test portion is introduced into a gas chromatographic column, which separates hydrocarbons in the
order of increasing boiling point. The column temperature is raised at a linear reproducible rate and the
area under the chromatogram is recorded throughout the analysis. Boiling points are assigned to the
time-axis from a calibration curve, which is obtained by running a mixture of known normal alkanes
covering the test portion boiling range, under the same conditions. From these data, the boiling range
distribution is obtained. The recovery (3.8) at a specified temperature is determined by comparing the
area under the chromatogram with that of a reference standard which has been completely eluted. The
temperature at which the recovery (3.8) was measured is recorded.
NOTE If the found recovery is less than 100 %, the final boiling point (3.2) is reported as 720 °C or 750 °C at
that recovery.
5 Reagents and materials
Unless otherwise stated, only chemicals of recognized analytical quality shall be used.
5.1 Liquid stationary phase, a methyl silicone stationary phase for the column.
5.2 Carrier gas, helium, nitrogen or hydrogen, of at least 99,999 % (V/V) purity. Any oxygen present
is removed by a chemical resin filter.
WARNING — Follow the safety instructions from the filter supplier.
5.3 Hydrogen, grade suitable for flame ionization detectors.
5.4 Compressed air, regulated for flame ionization detectors.
5.5 Alkanes, normal alkanes of at least 98 % (m/m) purity from C to C , C , C , C , C , C ,
5 10 12 14 16 18 20
C and C to be used with Polywax 655 or 1000 (5.6).
24 28
NOTE The calibration mixture from ISO 3924 [3] is also suitable.
5.6 Polywax 655 or 1000
5.7 Carbon disulphide, with a minimum purity of 99,7 % (V/V).
WARNING — Extremely flammable and toxic.
CAUTION — It is recommended that all work with carbon disulphide is carried out in an explosion
protected fume cupboard.
To confirm the suitability of the carbon disulphide (5.7) as a solvent, it is recommended to check elution
profiles (see Figure 2).
7
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Key
good
bad
Figure 2 — Solvent peak shapes
5.8 Calibration mixture
The mixture shall contain at least one normal alkane with a boiling point lower than the IBP of the
sample, and at least one normal alkane with a boiling point close to the temperature at which the
recovery (3.8) is measured.
Dissolve 0,1 g of Polywax (5.6) in 7 ml carbon disulphide (5.7), warming gently if necessary. Prepare an
equal volume mixture of alkanes (5.5) and add 10 µl to the Polywax solution.
NOTE 1 Commercially available alkane standards are suitable for column performance checks.
NOTE 2 The calibration mix is used to determine the column resolution, skewness of the C peak, and
20
retention time versus boiling point calibration curve.
5.9 Reference materials (RM)
5.9.1 A reference material has two functions:
— External Standard: to determine the recovery (3.8) of samples by comparing the total sample area
(3.6) of the reference material with the total sample area (3.6) of the unknown sample.
— Boiling Point Distribution Standard: to check the proper functioning of the system by comparing the
results with a known boiling point distribution on a routine basis. Typical example is given in
(5.9.2).
5.9.2 Reference Material 5010, a reference sample that has been analysed by laboratories
participating in the test method cooperative study. Consensus values for the boiling range distribution of
this sample are given in Table 1.
5.9.3 Cyclohexane, (C H )—(99+ % pure) may be used in place of CS for the preparation of the
6 12 2
calibration mixture.
5.9.4 Binary gravimetric blend, a binary distillate mixture with boiling points ranges that gives a
baseline at the start, a baseline between the two peaks and an end time that is as close to the end of the
chromatogram as possible (see Figure 3 and B.3). This mixture is used to check the relative response of
the two distillates and to check the baselines at the start, middle and end of the chromatogram.
8
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Key
Y response
X retention time (min)
Figure 3 — Typical chromatogram of binary gravimetric blend distillate
Table 1 — Reference Material 5010
Maximum allowable range
Reference
% recovered
temperature
95,5 % CI
°C °C
IBP 428 9
5 477 3
10 493 3
15 502 3
20 510 3
25 518 4
30 524 4
35 531 4
40 537 4
45 543 4
50 548 5
55 554 4
60 560 4
65 566 4
70 572 4
75 578 5
80 585 4
85 593 4
90 602 4
95 616 4
FBP 655 18
9
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6 Apparatus
6.1 Gas chromatograph, with the following performance characteristics.
6.1.1 Flame ionization detector, connected to the column so as to avoid any cold spots. The detector
shall be capable of operating at a temperature at least equivalent to the maximum column temperature
employed in the method.
6.1.2 Column temperature programmer, capable of linear programmed temperature operation over
a range of 10 °C above ambient to 450 °C.
6.1.3 Sample inlet system, consisting of a programmable temperature vaporizer (PTV) or cold on-
column (COC) injection port. The maximum temperature of the injection device shall be equal to, or
higher than, the final oven temperature. The minimum temperature shall be low enough to prevent
sample or solvent flashback, but high enough to allow sample focusing at the front of the column. Table 2
contains the typical operating conditions.
Table 2 — Typical operating conditions for gas chromatograph
Unit Specification
Column length m 5
Column internal diameter mm 0,53
Column material — Ultimetal
Stationary phase — Methyl silicone
Film thickness µm 0,09 or 0,17
Initial column temperature °C 35
Final column temperature °C 430
Program rate °C/min 10
Injector initial temperature °C 100
Injector final temperature °C 430
Program rate °C/min 15
Hold time min 5
Detector temperature °C 450
Detector hydrogen flow (5.3) ml/min 35
Detector air flow (5.4) ml/min 350
Carrier gas — He
Carrier gas flow rate ml/min 19
Sample size µl 1,0
Sample concentration % (m/m) 2
Injector — PTV or COC
10
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6.2 Column
6.2.1 The capillary column should sit just below the flame tip and it is recommended that the orifice of
the jet should be 0,6 mm minimum to prevent frequent blocking with silicones.
6.2.2 Use a metal column with 0,53 mm internal diameter and coated with methyl silicone (5.1).
Commercially available columns with film thickness (d ) = 0,09 µm (for analysis up to C ) and
f 120
(d ) = 0,17 µm (for analysis up to C ) have been found to be satisfactory.
f 100
It is recommended that the column resolution, R, is at least 2 and not more than 4 (see B.2).
6.2.3 Use some form of column bleed compensation to obtain a stable baseline.
This may be carried out by subtraction of a column bleed profile previously obtained using exactly the
same conditions as used for the sample analysis, by injecting the same volume, using solvent for the
blank run and sample dilution from one batch taken at the same time, to avoid differences due to
contamination.
6.3 Carrier gas control
The chromatograph shall be able to deliver a constant carrier gas (5.2) flow over the whole temperature
range of the analysis.
6.4 Micro-syringe, of appropriate volume, e.g. 10 µl, for introduction of 1 µl of the calibration mixture
and test portions.
Plunger in needle syringes are not recommended due to excessive carry over of heavy ends to the
following analysis.
6.5 Volumetric flask, 10 ml capacity.
6.6 Refrigerator, shall be of an explosion-protected design.
6.7 Analytical balance, able to weigh with a precision of 0,1 mg.
7 Sampling procedure
Samples shall be taken as described in EN ISO 3170 or EN ISO 3171. Store samples in either glass or
metal containers. Plastic containers for sample storage shall not be used as prolonged contact with the
sample can cause contamination of the sample due to possible leaching of the plasticizer.
8 Preparation of the apparatus
8.1 Gas chromatograph preparation
8.1.1 Set up and operate the gas chromatograph (6.1) in accordance with the manufacturer’s
instructions.
Typical operating conditions are shown in Table 2.
8.1.2 Deposits may form on the jet from combustion of decomposition products from the liquid
stationary phase (5.1). These will affect the characteristics of the detector and shall be removed.
NOTE The following parameters are affected by deposits on the jet: increase in inlet pressure; FID difficult to
light; increase in the CS response and an off specification reference material. To clean the jet, an ultrasonic cleaner
2
with a suitable solvent, and a cleaning wire can be used.
11
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8.2 System performance check
Check the system performance at the intervals given and by the procedures specified in Annex B.
9 Sample and reference material preparation
9.1 Mix the sample by shaking, warming prior to shaking where necessary.
9.2 Weigh approximately 0,1 g to 0,3 g of the sample to the nearest 0,1 mg, into a clean 10 ml
volumetric flask (6.5) and add 5 ml to 7 ml carbon disulphide (5.7).
Shake the mixture to completely dissolve the test portion and then add carbon disulphide (5.7) to the
mark. Immediately transfer the solution to auto test portion vials, seal, and store in a refrigerator until
ready for use.
If the density of the sample is known, the test portion may be prepared on a mass/mass basis, and the
following correction applied:
100m
m
1
% = (1)
V
mm
22
+
σσ
12
where
m is the mass of the test portion, in g;
1
m is the mass of carbon disulphide (5.7), in g;
2
σ is the density of the test portion at 20 °C, in kg/l;
1
σ is the density of carbon disulphide (5.7) at 20 °C, in kg/l; (= 1,26).
2
The density is quoted at 20 °C as a temperature approximately ambient in most laboratories.
Appropriate adjustments may be made if the laboratory temperature is outside (20 ± 5) °C.
Sample preparation is important to calculate the recovery (3.8) of the sample. The sample can be
prepared by weighing the sample in a 10 ml flask as described. Using this procedure, it is not required to
know or measure the density of the sample. Due to the low boiling point and the health restrictions of
CS2 it is preferred to prepare the sample by weight and correct for the density.
When the density is unknown and therefore no correction can be applied, the error in the recovery
calculation is minor. Not correcting for density can result in a deviation of at most 1 % on the recovery
3 3
(3.8) for the density range 700 kg/m to 1 000 kg/m .
10 Calibration
10.1 Proceed in accordance with 10.2 to 10.4 each day before sample analysis. The first run of the day
shall not be a blank, a reference standard (5.9) or a test portion, but it may be the calibration mixture
(5.8).
10.2 Run the calibration mixture (5.8) using the specified procedure described in Clause 11.
Take care to ensure the test portion volume chosen does not allow any peak to exceed the linear range of
the detector, or overload the column. A skew of > 3 indicates the sample is too concentrated and a skew
of < 1 indicates an old column or dirty liner. As a guide, 1 µl of the calibration mixture (5.8) has been
found to be suitable for columns with film thickness less than 0,17 µm.
12
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