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Measuring Hydrocarbon Oil Index

according to ISO 9377-2 (DIN H53)

Environmental Application
Gas Chromatography
Bernhard Wst

Abstract

Introduction

Agilent Technologies developed this ana-

The Hydrocarbon Oil Index (HOI) is defined

lytical method to comply with ISO 9377-2

as the total amount of compounds which

This analytical method complies with the

and DIN H53 Standards. The method

can be extracted from the sample (potable

ISO Standard 9377-2 for the determination

employs a simple instrument configuration

water, surface water and waste water)

of the Hydrocarbon Oil Index by Gas

consisting of a Gas Chromatograph (GC)

with a non-polar solvent having a boiling

Chromatography. The method is suitable for

equipped with a Split/Splitless (S/SL) inlet

point between 39C and 69C (replacing

HOI determinations in concentrations above

and Flame Ionisation Detector (FID), making

the use of halogenated solvents). In

0.1 mg/L in drinking waters, surface waters,

the method both easy to implement and

addition, the compounds must not absorb on

waste waters and waters from sewage

robust to operate. The combination of an

Florisil and must elute between n-decane

treatment plants.

Agilent GC system (see configuration

(C10H24) and n-tetracontane (C40H82)

above), selected capillary GC column,

when analysed by GC using an apolar

proprietary injection port liner, appropriate

analytical column. Restrictions on the use of

chemical standards as well as method

halogenated hydrocarbons as solvents for

installation and support by an Agilent

analytical applications combined with the

Applications Specialist, provide a complete

increasing cost of and reduced availability of

solution for the measurement of the

technical grade halogenated solvents as well

Hydrocarbon Oil Index.

as documented environmental

considerations resulted in the change to a


non-polar solvent for HOI determinations.

Publication number 5988-0621EN

Agilent Technologies

Experimental

Instrument Parameters

The Agilent 6890 and Agilent 6850 Gas


Chromatographs are well suited to the HOI
application. Both instruments use the same
Split/Splitless inlet system and identical
Flame Ionisation Detector. Discrimination
effects on higher boiling compounds are the
most critical aspect of the analysis and are
prevented by the use of a special injection
port liner which, in combination with the
Agilent S/SL inlet system, produces robust
and reliable data. Additional benefits such
as reduced maintenance time and faster
analytical cycle times are also available by
using a S/SL inlet as compared to a Cool-onColumn inlet.
The Agilent GC ChemStation standard
software is able to subtract background
signals to produce a chromatogram with
any column bleed removed. In addition, both
the Agilent 6890 and 6850 are able to save
column compensation signals in memory
and subsequently subtract the column
background from the sample data and
provide a background-subtracted signal to
the ChemStation or data integration
system. Standard ChemStation software
tools are used to control the GC and
perform the data analysis required of the
sample data. A custom report template is
included with the HOI method and
generates a report conforming to the ISO
Standard (see figure 3).

Oven temperature
profile
Inlet (S/SL)
Detector (FID)
Analytical Column
Inlet Liner
Carrier Gas
Carrier Gas
Flow Rate
Injection Mode
Injection Volume

Page 2

Isothermal 35C (1.5 min), ramp 5C/min to 60C hold 0 min,


ramp 15C/min to 350C hold 5 min.
375C Splitless Mode
375C
Agilent Part Number 19095Z-221E (HP1, 15m x 0.53mm x 0,15 m)
Agilent Part Number 5183-4647
Helium
7.4 ml/min Constant Flow Mode
Automated (Agilent 7683) Fast Injection
1.0 l

Calibration Curve
Hydrocarbon
Hydrocarbon
Index,
FID1
A Index, FID1 A
Area = -375.37592
20647.3902*Amt-375.37592
Area
20647.3902*Amt
=
Area
Area

Rel. Res%(7):-4.0289e-1

Rel.
Res%(7):
-4.0289e-1

40000

35000

30000

25000
6
20000
5
15000

10000

5000

2
1

Correlation:
Correlation:
0.99918 0.99918

0
0

0.5

1.5

Amount
Amount[mg[mq/m]
/m]l

Figure 1: Oil Standards Calibration Curve

4.207

FID1 A, (HYC2509\007F0702.D)

22.535

pA
90

80

13.331

70

60

50

40

22.641

10

4.103

20

2.045
2.158
2.250
2.6012.513
2.783
3.011
3.128
3.494 3.377
3.647

30

Figure 2: 0.6 mg/ml Oil Standard

10

15

20

25

30 min

Publication number 5988-0621EN

Discrimination Test:
25 sequential injections of a standard
containing tetracontane C-40 and decane
C-10 were run to test for discrimination
effects within the analytical system. The
data obtained is presented in Figure 3 and
demonstrates the robustness of the method
and that the analytical system clearly
passes the discrimination test specified in
the ISO Standard.

Agilent Technologies

Page 3

150.0

140.0

130.0

120.0

110.0

100.0

90.0

80.0

70.0

50.0
1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

A mount / Run No. [Decane C10]

10.0

11.0

12.0

13.0

14.0

15.0

16.0

A mount / Run No. [Tetrac ontane C40]

17.0

18.0

19.0

Amount ( Mean )

20.0

21.0

22.0

23.0

24.0

A mount ( Mean )

Figure 3: Discrimination Test


Data file
: C:\HPCHEM\1\DATA\HYC2509\008F0802.D
Sample Name : 1000 mg/l
1
===================================================================
Injection Date
: 9/26/2000 3:23:50 AM
Seq Line : 8
Sample Name
: 1.0 mg/ml
Vial No. : 8
Acq Operator
: berwuest
Inj. No. : 2

Acq.Method
Analysis Method
Last Changed

Inj. Vol. : : HYCA04.M


: C:\HPCHEM\1\METHODS\ISO93774.M
: Fri, 29. Sep. 2000, 10:04:10 am

Analysis of Hydrocarbon Index according to Iso 9377-4 and


DIN H53

13.332

FID1 A, (HYC2509\008F0802.D)
4.207

pA
80

22.533

70

60

50

40

2.512

30

20

2.044
2.156
2.248

The Agilent 6890 and 6850 Gas


Chromatographs equipped with a
Split/Splitless inlet and Flame Ionisation
Detector can be used for Hydrocarbon Oil
Index determinations in accordance with ISO
9377-2 (DIN H53) standard. In addition, the
analytical system is easy to operate and
requires minimal maintenance. Together, the
Agilent GC, analytical capillary column,
special inlet liner, custom report template,
selected chemical standards and Agilent
applications expertise provide a complete
analytical solution for Hydrocarbon Oil Index
determinations.

60.0

2.599
2.781
3.009
3.2543.127
3.378
3.492
3.645
4.101

Results and Dicussion

10

10

15

20

30
25

min

============================================================================
Hydrocarbon Index Report
============================================================================
Calib. Data Modified
: Fri, 29. Sep. 2000,08:25:56 am
Multiplier
: 1.000000
Hydrocarbon Index
Low Boilers
High Boilers

1.052 mg/ml
9.061 mg/l
not detectable

mg/l

============================================================================
Detailed Report
============================================================================
Name
StartTime EndTime Ret Time Total Area Res.F
Amount
---------------------------------------------------------------------------Low Boilers
2.00
4.00
239.48
0.03784 9.06
Decane C10
4.21
213.73
0.03784 8.09
Hydrocarbon Index
4.31
22.37
13.33 15408.08
0.00006 1.05
Tetracontane C40
22.53
205.67
0.03247 7.94
High Boilers
n.d.
============================================================================

Figure 4: Report Printout

Bernhard Wst is an application chemist


based at
Agilent Technologies GmbH
Hewlett Packard Str. 8
76337 Waldbronn
Germany

For more information on our products and


services, visit our website at:
www.agilent.com/chem

Copyright 2000 Agilent Technologies


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Information, descriptions and
specifications in this publication are
subject to change without notice.
Publication Number 5988-0621EN