kSIST FprEN 15199-2:2020
(Main)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
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 auf Mineralölerzeugnisse mit einem für die Probenahme bei Umgebungstemperatur ausreichend niedrigen Dampfdruck und mit einem Siedebereich von mindestens 100 °C. Die Norm ist anwendbar auf Mineralölerzeugnisse mit einem Siedebeginn (IBP, "Initial Boiling Point") oberhalb von 100 °C und mit einem Siedeende (FBP, "Final Boiling Point") oberhalb von 750 °C, wie z. B. Schweröle und Rückstandsöle. Für bituminöse Proben ist dieses Prüfverfahren nicht geeignet.
Das Prüfverfahren ist nicht einsetzbar 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. Il 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. Le présent document 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, carburants diesels). Les composants contenant 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,µ, et la fraction volumique, φ.
AVERTISSEMENT — L’utilisation de la présente Norme européenne implique l’utilisation de produits, d’opérations et d’équipements à caractère dangereux. La présente Norme européenne n’a pas la prétention d’aborder tous les problèmes de sécurité concernés par son usage. Il est de la responsabilité de l’utilisateur de consulter et d’établir des règles de sécurité et d’hygiène appropriées et de déterminer l’applicabilité des restrictions réglementaires avant utilisation.
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
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 fuelsMineralölerzeugnisse - Gaschromatographische Bestimmung des Siedeverlaufes - Teil
2: Schweröle und RückstandsöleProduits pétroliers - Détermination de la répartition dans l'intervalle de distillation par
méthode de chromatographie en phase gazeuse - Partie 2: Fiouls lourds et fioulsrésiduels
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.
---------------------- Page: 1 ----------------------oSIST prEN 15199-2:2019
---------------------- Page: 2 ----------------------
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 Rückstandsölelourds 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.---------------------- Page: 3 ----------------------
oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
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
---------------------- Page: 4 ----------------------oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
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
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
---------------------- Page: 5 ----------------------oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
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.
---------------------- Page: 6 ----------------------oSIST prEN 15199-2:2019
prEN 15199-2:2019 (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. 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 referencesThe 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 obtained3.2
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---------------------- Page: 7 ----------------------
oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
3.3
area slice
area resulting from the integration of the chromatographic detector signal within a specified retention
time intervalNote 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) analysis3.5
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 solvent3.6
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---------------------- Page: 8 ----------------------
oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
3.7
net area
cumulative area counts for the sample minus the cumulative area count for the blank
3.8recovery
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 PrincipleA 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 20C 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).---------------------- Page: 9 ----------------------
oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
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
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 2calibration 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.
---------------------- Page: 10 ----------------------oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
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
---------------------- Page: 11 ----------------------
oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
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
---------------------- Page: 12 ----------------------
oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
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 apparatus8.1 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
with a suitable solvent, and a cleaning wire can be used.---------------------- Page: 13 ----------------------
oSIST prEN 15199-2:2019
prEN 15199-2:2019 (E)
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 preparation9.1 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
% = (1)
V
+
where
m is the mass of the test portion, in g;
m is the mass of carbon disulphide (5.7), in g;
σ is the density of the test portion at 20 °C, in kg/l;
σ is the density of carbon disulphide (5.7) at 20 °C, in kg/l; (= 1,26).
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.---------------------- Page:
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.