CO2 SPECIFICATION GUIDE

FOR ANALYTICAL STEPS

AND FREQUENCIES
IGC Doc 76/01/E

EUROPEAN INDUSTRIAL GASES ASSOCIATION

AVENUE DES ARTS 3-5 • B – 1210 BRUSSELS

Tel : +32 2 217 70 98 • Fax : +32 2 219 85 14
E-mail : [email protected] • Internet : http://www.eiga.org
 IGC Doc 76/01/E

CO2 SPECIFICATION GUIDE

FOR ANALYTICAL STEPS
AND FREQUENCIES

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EUROPEAN INDUSTRIAL GASES ASSOCIATION

Avenue des Arts 3-5 B 1210 Brussels Tel +32 2 217 70 98 Fax +32 2 219 85 14
E-mail: [email protected] Internet: http://www.eiga.org
IGC DOC 76/01/E

Table of Contents
1 Introduction....................................................................................................................................... 1

2 Scope ............................................................................................................................................... 1

3 Source Certification .......................................................................................................................... 1

3.1 Process plants as CO2 Sources................................................................................................ 1
3.2 Natural wells / Geothermal........................................................................................................ 2
3.3 Fermentation ............................................................................................................................. 2
4 CO2 production ................................................................................................................................. 2
4.1 Design ....................................................................................................................................... 2
4.2 Analytical controls ..................................................................................................................... 2
4.3 CO2 storage tank at the plant.................................................................................................... 2
4.4 CO2 intermediate storage tanks (depots).................................................................................. 3
5 Product control ................................................................................................................................. 3

6 Frequencies...................................................................................................................................... 3
IGC DOC 76/01/E

1 Introduction

The EIGA Document 70/99/E "CO2 Source Certification, Quality Standards and Verification" presents
a standard for the CO2 specification which is in line with the CGA-CO2-Specification and the CO2-
Quality-Guidelines of the ISBT (International Society of Beverage Technologists).

The EIGA document 70/99/E is intended to be used world-wide by CO2 producers and the users,
especially the food and beverage industry.

The ISBT guidelines contain also the analytical procedure bibliography where guidance is provided for
sampling and the analytical procedures.

This document is intended to be guidance on control and analysing procedures to be implemented as

the quality assurance system of the production plants. The EIGA Document 68/99/E “Prevention of
CO2 Backfeed Contamination” gives additional guidance on the necessary precautions to be taken in
order to assure conformity of CO2 supplies.

This document will be also available to the user of the product.

2 Scope

This guidance paper will explain which analysis should be carried out on the raw gas sources and the
liquefied CO2 product.

It will give recommendations for on-line control and frequencies of analyses for the CO2 production
and the product to be delivered.

3 Source Certification

The initial assessment of the raw gas source will give an indication of the normal variations in the
composition of the raw gas. This can be used to choose the components to be analysed and the
frequency of regular analysis.

It may be necessary to reanalyse and re-evaluate the CO2 process if there is any significant change in
the raw gas composition, e.g.: a significant change would be, when the oil, which is used as feedstock
for the chemical process, of which the CO2 raw gas is taken from, is changed from a so called poor
sulfur quality to a sulfur quality.

3.1 Process plants as CO2 Sources

The CO2 raw gas is taken from different sources, as it is listed in table 2 of the EIGA document
70/99/E.

In order to select a source as a possible raw gas stream for a CO2 plant, it is necessary to assess the
process producing the raw gas. It is also necessary to assess the feed stock being used in the
process (e.g. what kind of crude oil or natural gas).

It is important to know the composition of the CO2 raw gas.

Prior to design of the CO2 plant, and periodically thereafter, raw gas samples from the relevant source
should be taken to analyse the raw gas at least for the components, which are listed in table 2 of
EIGA DOC 70/99/E.

The detection level should be the same as that used for analysis of the final product.

The results of the analyses should be discussed with the process plant operator, to check if the raw
gas composition could change under normal operation. The process operator should also inform the
CO2 plant, if there are changes in the process, which could affect the CO2 quality.

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The CO2 producer should also be informed prior to any significant change in the process (e.g. change
of feed stock).

3.2 Natural wells / Geothermal

The CO2 raw gas of natural wells needs to be assessed. It is also necessary to evaluate the
geological source and possible changes of components which may be found in the raw gas,
particularly in case of variation of extraction.

3.3 Fermentation

CO2 raw gas from fermentation need to be assessed in the same way as above.

The composition of the raw gas can vary due to apparently minor changes in the feedstock caused by
geographical variations or growing conditions.

4 CO2 production

4.1 Design

The CO2 raw gas composition will determine the design of the plant, especially the purification steps
and procedures and also the analytical controls during the process.

The purification process will need analytical controls for the process, if no other relevant parameters
can be used, to assure that the purification step is functioning.

E.g.: a catalytic oxidation step is monitored by the process temperature and Oxygen surplus to ensure
that volatile hydrocarbon components are reduced to the necessary level. The measured Oxygen
surplus including the high temperature indicates the absence of non methane hydrocarbons.

E.g.: a sulphur purification step will be monitored by analysing either total sulphur or the relevant
sulphur compound after the purification process.

4.2 Analytical controls

Analytical controls during the process may be continuous using on-line instruments or based on spot
checks. This choice and the selection of the frequency for checks will depend on:

a) the component to be measured

b) the likely concentration of the component
c) the importance of the component to the perceived quality of the CO2
d) the ease of measurement
e) risk assessment of the purification process designed to remove the component to acceptable
levels.
f) regulatory mandates and/or individual guide.

The frequency of checks will vary markedly depending on consideration of these factors and may
typically be from one per hour to two per year.

Most CO2 plants use on line moisture meters to check the performance of the drying process. Other
common controls include sulphur compounds (as total sulphur or separately determined as individual
sulphur compounds), volatile hydrocarbons, carbon monoxide and nitrogen oxides. Risk assessment
may indicate that other controls are required e.g. aromatic hydrocarbons or acetaldehyde if there is a
possibility that the raw gas may contain these components.

4.3 CO2 storage tank at the plant

The CO2 is liquefied and pumped into one or more storage tanks. At some CO2 plants it is possible to
use each tank (or a cluster of tanks) as a batch. This gives the possibility to analyse the storage

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before the storage is used for filling of the tankers. The analysis of a batch will refer to the compounds
of the raw gas of the production plant, as prescribed in 4.2. The batch analysis can reduce the online-
analysis in the plant to a minimum.

However, many plant storage tanks are operated in a continuous manner and batch analysis is not
practical. Conformity of the storage is assured by analysis of the incoming product to the tank.

In case of a non-conformity, a procedure of quality assurance has to be implemented in order to stop

tanker filling and delivery, effect appropriate rectification or disposal of the non conforming product
and re-establish normal operation once conformity has been re-established. If there is a lot numbering
system, a new lot number will then be given to the storage content.

4.4 CO2 intermediate storage tanks (depots)

As CO2 cannot be produced everywhere, it is common for the CO2-distributor to use CO2-storages,
where usually the product is transported by rail, tankship or road, filled into the central storage and
distributed by road tankers to customers. The conformity of the storage is assured by importing into
the tank only products which comply with the specifications.

5 Product control

Analysis of the CO2 to the complete specification should be conducted at least as listed. Where
possible it should be sampled and analysed by a recognised test-laboratory independent from the
production plant. This gives the possibility to crosscheck the results of the production plant.

When CO2 production plants are operated under a quality assurance system, a conformity certificate
may be given at each delivery in order to prove compliance to customers.

6 Frequencies

Depending on the plant characteristics, analytical frequencies are proposed in the following table.

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 IGC DOC 76/01/E

Control Frequencies

Frequencies Online or Yearly ** When Notes

Daily or changes
Batchwise at the
source

Components
Raw gas 1
source
Purity 1 1
Dew point 1 1
(moisture)
Acidity 1
Ammonia 2 1
Oxygen 2 1 Daily if at critical level
Oxides of Nitrogen 2 1
Non volatile 2 1
residue
(particulates)
Non volatile 2 1
organic residue
Phosphine 2 1 Only if raw gas is from phosphate rock
Total volatile 1 1
hydrocarbon
Acetaldehyde 2 1
Benzene 2 1
Carbon Monoxide 2 1
Methanol 2 1 Daily if at critical level
Hydrogen Cyanide 2 1 Only if raw gas is from coal gasification
sources
Total Sulphur 2 1
Taste and odour in 1 1
water
Others* 2 1

1 Mandatory
2 Analysis is not required at this frequency if a formal risk assessment has been undertaken
which has concluded that the specified maximum level for each component in the CO2
product cannot be exceeded in normal operation or in a failure mode.

* See table 2 (EIGA-DOC "CO2 Source Certification, Quality Standards and Verification"
Possible Trace Impurities.)

** The yearly control is done as a general check by a recognised test-laboratory, independent

from production plants, see item 5.