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Bitumi e leganti bituminosi

NORMA Determinazione del contenuto di paraffina UNI EN 12606-1


E U R OP E A Parte 1: Metodo per distillazione

LUGLIO 2007

Bitumen and bituminous binders


Determination of the paraffin wax content
Part 1: Method by distillation

La norma specifica un procedimento per la determinazione del


contenuto di paraffina di bitume e leganti bituminosi mediante il
metodo DIN.

TESTO INGLESE
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La presente norma è la versione ufficiale in lingua inglese della


norma europea EN 12606-1 (edizione marzo 2007).

La presente norma è la revisione della UNI EN 12606-1:2002.

ICS 75.140; 91.100.50

UNI © UNI
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PREMESSA NAZIONALE
La presente norma costituisce il recepimento, in lingua inglese, del-
la norma europea EN 12606-1 (edizione marzo 2007), che assume
così lo status di norma nazionale italiana.

La presente norma è stata elaborata sotto la competenza dell’ente


federato all’UNI
UNICHIM - Associazione per l’Unificazione nel settore dell’In-
dustria Chimica

La presente norma è stata ratificata dal Presidente dell’UNI ed è


entrata a far parte del corpo normativo nazionale il 19 luglio 2007.

Le norme UNI sono elaborate cercando di tenere conto dei punti di vista di tutte le parti
interessate e di conciliare ogni aspetto conflittuale, per rappresentare il reale stato
dell’arte della materia ed il necessario grado di consenso.
Chiunque ritenesse, a seguito dell’applicazione di questa norma, di poter fornire sug-
gerimenti per un suo miglioramento o per un suo adeguamento ad uno stato dell’arte
in evoluzione è pregato di inviare i propri contributi all’UNI, Ente Nazionale Italiano di
Unificazione, che li terrà in considerazione per l’eventuale revisione della norma stessa.

Le norme UNI sono revisionate, quando necessario, con la pubblicazione di nuove edizioni o
di aggiornamenti.
È importante pertanto che gli utilizzatori delle stesse si accertino di essere in possesso
dell’ultima edizione e degli eventuali aggiornamenti.
Si invitano inoltre gli utilizzatori a verificare l’esistenza di norme UNI corrispondenti alle
norme EN o ISO ove citate nei riferimenti normativi.
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EUROPEAN STANDARD EN 12606-1
NORME EUROPÉENNE
EUROPÄISCHE NORM March 2007

ICS 75.140; 91.100.50 Supersedes EN 12606-1:1999

English Version

Bitumen and bituminous binders - Determination of the paraffin


wax content - Part 1: Method by distillation

Bitumes et liants bitumineux - Détermination de la teneur Bitumen und bitumenhaltige Bindemittel - Bestimmung des
en paraffines - Partie 1 : Méthode par distillation Paraffingehaltes - Teil 1: Destillationsverfahren

This European Standard was approved by CEN on 3 February 2007.

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 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 Management Centre has the same status as the
official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
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EUROPEAN COMMITTEE FOR STANDARDIZATION


COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2007 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12606-1:2007: E
worldwide for CEN national Members.

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EN 12606-1:2007 (E)

Contents Page

Foreword..............................................................................................................................................................3
1 Scope ......................................................................................................................................................4
2 Normative references ............................................................................................................................4
3 Terms and definitions ...........................................................................................................................4
4 Principle..................................................................................................................................................4
5 Reagents and materials ........................................................................................................................4
6 Apparatus ...............................................................................................................................................5

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7 Sampling.................................................................................................................................................6
8 Procedure ...............................................................................................................................................7
9 Calculation..............................................................................................................................................8
10 Expression of results ............................................................................................................................9
11 Precision.................................................................................................................................................9
12 Test report ..............................................................................................................................................9

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EN 12606-1:2007 (E)

Foreword
This document (EN 12606-1:2007) has been prepared by Technical Committee CEN/TC 336 “Bituminous
binders”, the secretariat of which is held by AFNOR.

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 September 2007, and conflicting national standards shall be
withdrawn at the latest by September 2007.

This document supersedes EN 12606-1:1999.

This draft European standard EN 12606 consists of the following parts under the general title Bitumen and
bituminous binders – Determination of the paraffin wax content

Part 1: Method by distillation

Part 2: Method by extraction

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and United Kingdom.
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EN 12606-1:2007 (E)

1 Scope
This European Standard specifies a procedure for determining the paraffin wax content of bitumen and
bituminous binder by the DIN method.

Aqueous bituminous binders, fluxed or cut-back anhydrous binders, and modified binders, whatever their
consistency, are not within the scope of the present test method.

WARNING — Use of this European standard can 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 European standard to establish appropriate
safety and health practices and determine the applicability of regulatory limitations prior to use.

2 Normative references
The following referenced documents are indispensable for the application 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 58, Bitumen and bituminous binders – Sampling bituminous binders

EN 1425, Bitumen and bituminous binders - Characterization of perceptible properties

EN 12594, Bitumen and bituminous binders – Preparation of test samples

EN ISO 3696:1995, Water for analytical laboratory use – Specification and test methods (ISO 3696:1987)

ISO 383, Laboratory glassware – Interchangeable conical ground joints

3 Terms and definitions


For the purposes of this document, the following term and definition applies.

3.1
paraffin wax
mixture of hydrocarbons crystallising in a 50 % volume fraction mixture of ether/ethanol at temperatures down
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to - 20 °C, obtained by a specified process and having a melting range of above 25 °C

4 Principle
Paraffin wax present in bitumen is determined in the distillate obtained from a specified distillation process.

5 Reagents and materials

5.1 General

Use only reagents of recognized analytical grade and water conforming to grade 3 of EN ISO 3696:1995
unless otherwise specified.

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EN 12606-1:2007 (E)

5.2 Ethoxyethane (Diethylether), anhydrous, referred to in this standard as ether.

5.3 Ethanol, absolute.

5.4 Ethanol, technical grade.

5.5 Petroleum spirit, with density of approximately 645 kg/m³ at 15 °C, and a distillation range of
approximately 30 °C to 75 °C;

5.6 Acetone, reagent grade.

5.7 Carbon dioxide, solid, finely ground.

NOTE A cryostat with a cooling effect equivalent to that of solid carbon dioxide can be used.

5.8 Ice, finely ground.

5.9 Washing liquid, a 50 % volume fraction mixture of ether/ethanol.


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6 Apparatus
Usual laboratory apparatus and glassware, together with the following:

6.1 Oven, capable of maintaining (125 ± 5) °C.

6.2 Thermometers, referred to in this standard as:

6.2.1 Sample thermometer: a solid stem thermometer, in the range - 38 °C to 50 °C, and with a subdivision
every 1 °C; total length (360 ± 5) mm, immersion (180 ± 5) mm, stem outside diameter (10 ± 0,5) mm.

6.2.2 Bath thermometer: a solid stem thermometer, in the range - 30 °C to 50 °C, and with a subdivision
every 0,5 °C, total length (220 ± 5) mm, immersion (50 ± 5) mm, stem outside diameter (8 ± 0,5) mm.

Other temperature measuring devices may be used instead of mercury stem thermometers; however, the
mercury stem thermometer is the reference device. Therefore, any alternative device employed shall be
calibrated so as to provide the same readings as would be provided by the mercury stem thermometer,
recognising and allowing for changed thermal response times compared with the mercury thermometer.

NOTE When measuring and controlling nominally constant temperatures, as in this test method, alternative devices
can indicate greater cyclic variations than mercury thermometers, depending on the cycle time of heating and the power of
the controlled heat input.

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EN 12606-1:2007 (E)

6.3 Distillation flask as shown in Figure 1, fitted with cork stopper.

6.4 Sheet metal guard ring with an approximate 18 mm inside diameter and a 65 mm outside diameter.

6.5 Test tubes, fitted with a spout and bored cork stopper; dimensions are given in Figure 2.

6.6 Test tubes, fitted with a 29/32 ground socket and a wash bottle fitted with a 29/32 ground cone
according to ISO 383; dimensions are given in Figure 2.

6.7 Erlenmeyer flask, 100 ml, to be used as distillation receiver fitted with a bored cork stopper
continuously vertically notched on the outer surface.

6.8 Filter flask, 500 ml, with vacuum unit.

6.9 Glass wash bottle, 500 ml.

6.10 Cooling bath (see an example on Figure 2), a different cooling bath with the same isolation effect can
also be used.

6.11 Funnel (in cooling bath), with a diameter of 72 mm and a total length of 200 mm.

6.12 Evaporating basin, diameter 80 mm, mark at 15 mm.

6.13 Balance, accurate to ± 10 mg.

6.14 Balance, accurate to ± 2,0 mg

6.15 Laboratory burner (see Figure 3).

6.16 Desiccator

6.17 Porcelain crucible, with a diameter of 80 mm.

6.18 Round filter, with a diameter of 110 mm, for quantitative analysis, transmission: middle close or
middle rapid flowing.

6.19 Timer

6.20 Pincers

7 Sampling
Make sure that the laboratory sample is homogeneous and is not contaminated (see EN 1425). Take all
necessary safety precautions and ensure that the test sample is representative of the laboratory sample from
which it is taken (see EN 58). The laboratory sample shall be taken in accordance with EN 58.

The test shall be carried out on two portions each of (25 ± 1) g. Prepare the test sample in accordance with
EN 12594.

6
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EN 12606-1:2007 (E)

8 Procedure
Melt each test portion in a porcelain crucible for the minimum time necessary to ensure that the sample is
completely fluid. Pour (25 ± 1) g into the distillation flask (6.3) and weigh to the nearest 10 mg (mass mB).

Heat the distillation flask with a laboratory burner with a soft flame, approximately 150 mm high, (without a
flame cone) that has just ceased to be luminous in such a way that the first distillate drop falls down after
3 min to 4 min. Fit the sheet metal guard ring (see 6.4) loosely on the distillation flask to prevent possible
burning of the cork stopper.

Ensure that the vapours produced during distillation are being condensed by weighing, to the nearest 10 mg,
the Erlenmeyer flask (6.7) into which the lower bent end of the outlet tube projects to its full length
(see Figure 2), and immerse this as far as possible into a mixture of finely ground ice and water. The rate of
distillation shall remain visible and capable of being checked.
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Adjust the distillation rate so that (15 ± 5) drops fall from the end of the outlet tube into the distillation receiver
every 10 s.

Continue heating without adjusting the laboratory burner flame, until the distillation rate slows and no drop falls
from the outlet tube over a period of 10 s or after 14 min from the start of distillation.

Continue heating for a further min with a completely non-luminous roaring flame until the flask glows red.

Complete the distillation in a maximum of 15 min. Do not transfer the condensate left in the outlet tube after
distillation to the distillation receiver.

Mix the distillate thoroughly by gently warming it whilst at the same time, carefully swirling the receiver.

Cool the receiver to ambient temperature in a desiccator and weigh the distillate contained in the receiver to
the nearest 10 mg (mass mD). Depending on the expected paraffin wax content, add 2 g to 4 g of the distillate
into a test tube (6.5) and weigh to the nearest 5 mg (mass mE).

NOTE If the paraffin wax content cannot be estimated in advance, an initial mass of distillate of approximately 3 g is
recommended.

Dissolve the weighed mass of distillate in (25 ± 1) ml of ether (5.2) and add (25 ± 1) ml of ethanol (5.3).

Close the test tube with a stopper fitted with a sample thermometer (6.2.1) extending down into the liquid and
place the test tube in a cooling bath. Cool the bath liquid by adding finely crushed solid carbon dioxide or with
a cryostat (see note to 5.7). To ensure the sample temperature is maintained at - 20 °C, which will be required
later, lower the bath temperature to (- 22 ± 1) °C. Transfer (20 ± 1) ml of the washing liquid (5.9) into the test
tube fitted with the wash bottle head and cool in the cooling bath (6.10) to (- 20 ± 0,5)°C, maintain this
temperature until filtration is complete.

Place the round filter (6.18) in the funnel standing in the cooling bath and connect it to the filter flask placed
below the cooling bath. Quickly transfer the slurry of crystals produced at (- 20 ± 0,5) °C to the filter. Rinse the
test tube with the cooled washing liquid. Re-adjust the temperature of the washing liquid to (- 20 ± 0,5) °C and
use it again for rinsing the crystal slurry into the filter. Distribute the washing liquid as uniformly as possible
between the three washing operations.

Support the filtration by a gentle vacuum process during which the pressure does not fall below 5 kPa. As
soon as filtration is complete, lift off the round filter using pincers and place it in the funnel situated over the
evaporating basin or Erlenmeyer Flask, which has been weighed previously to the nearest 0,5 mg. Dissolve
the crude paraffin wax residue by carefully spraying heated petroleum spirit over it. Dissolve in the same way
any paraffin wax that may be adhering to the thermometer or to the test tube. Evaporate the mixed filtrates in
the evaporating basin over the water bath. To prevent liquid creeping over the rim, carry out the evaporation in
a weak air stream. Dry the residue for (15 ± 1) min at (125 ± 5) °C in the oven and allow it to cool. When the

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EN 12606-1:2007 (E)

previously purified paraffin waxes have cooled down but have not quite solidified, add approximately 15 ml of
acetone.

Dissolve the paraffin waxes by gently heating and carefully swirling the evaporating basin. Make up any
acetone lost by evaporation. Cool the acetone/paraffin wax solution in a water bath to (15,0 ± 0,5) °C and
separate by filtering the paraffin waxes that crystallize out. Wash the evaporating basin, the thermometer and
the filter several times with acetone brought to (15 ± 0,5) °C from a wash bottle ensuring that the total volume
of washing liquid is (30 ± 1) ml. The washing liquid shall be discarded.

Dissolve the paraffin waxes purified in this way by carefully spraying them with heated petroleum spirit and
collect them again in the same evaporating basin. Evaporate the petroleum spirit/paraffin wax solution in a
weak air stream over the water bath.

Dry the crystallised paraffin waxes obtained for (15 ± 1) min at (125 ± 5) °C in the oven and, after cooling in
the desiccator, determine the mass to the nearest 0,5 mg (mass mA).

If the final mass is outside the range 65 mg to 85 mg, reject the result and repeat the test with an appropriately
adjusted initial mass of the same distillate (mass mE).

If the initial mass, which is required to give a final mass between 65 mg and 85 mg, is below 2 g or above 4 g,
record this in the test report.

NOTE For cooling purposes an automatic cooling device can be used provided the same results are obtained.

For routine tests, the procedure of distillation can be carried out on one portion of (25 ± 1) g.

Depending on the expected paraffin wax content, add 2 g to 4 g (e.g. 2,5 g, 3 g and 3,5 g) of the distillate into
the three test tubes and weigh them to the nearest 5 mg. Continue the procedure with these three samples of
distillate.

If one or more of the final masses of the paraffin waxes are inside the range 65 mg to 85 mg, calculate the
paraffin wax content for the two masses, which are the closest to 75 mg and if possible on both sides of the
average. If all of the final masses are outside the range of 65 mg to 85 mg, reject the results and repeat the
test with one new portion of (25 ± 1) g, adjusting initial masses of the distillate.

9 Calculation
Calculate the paraffin wax content Cp, for each test portion, expressed as a percentage by mass, using the
following equation:

mD × mA
Cp = × 100 (1)
mB × mE

where
mB is the initial mass of bitumen, in grams;
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mD is the mass of distillate, in grams;

mE is the initial mass of distillate, in grams;

mA is the final mass of paraffin wax, in grams.

If the values measured for both test portions do not differ by more than 0,3 % mass fraction, determine the
mean of the two values. Otherwise, carry out a determination on a third test portion of approximately 25 g and
take the mean of the two closest values. These values, however, shall not differ by more than 0,3 % mass
fraction. If the first two values are equidistant from the third, specify the third value.

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If it is not possible to obtain a mean value from these three values under the specified conditions, reject all
three values and repeat the test on two further test portions.

NOTE In the case of routine tests draw a graph, where the final mass is shown on the x-axis and paraffin wax
content is shown on the y-axis. Place the results into the graph. Read the final paraffin wax content from the graph at the
point, where the final mass is 75 mg.

10 Expression of results
Express the paraffin wax content as a percentage by mass, rounded to the nearest 0,1 %.

11 Precision

11.1 Repeatability

The difference between two test results obtained by the same operator with the same apparatus under
constant operating conditions on identical test material would, in the long run, in the normal and correct
operation of the test method, exceed 0,3 % by mass absolute.

11.2 Reproducibility

The difference between two single and independent test results obtained by different operators working in
different laboratories on identical test material would, in the long run, in the normal and correct operation of
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the test method, exceed 0,5 % by mass absolute.

NOTE These precision data are not automatically applicable to modified bitumen or industrial bitumens. For modified
bitumen they should only be used for guidance, until criteria data are available.

12 Test report
The test report shall contain at least the following information:

a) type and identification of the sample under test;

b) reference to this European Standard;

c) result of the test (see Clauses 9 and 10);

d) any deviation, by agreement or otherwise, from the procedure specified;

e) date of the test.

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Dimensions in millimetres

Figure 1 — Distillation flask for paraffin wax determination

10
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Dimensions in millimetres

Precision is equal to ± 1 mm if not mentioned

Key

1. Air cushion 6. Opening for insertion


for solid carbon dioxide
2. Opening for funnel
7. Opening for insertion
3. Test tube of thermometer

4. Bath liquid 8. Bored corked stopper

5. Connector for filter flask 9. Spout

Figure 2 — Test tubes, cooling bath and funnel (example)

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11

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Key

1. Inlet for gas tubing

2. Needle valve
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3. Air regulator

Figure 3 — Laboratory burner

12

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EN 12606-1:2007 (E)
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Key

1 Cooling bath

2. Guard ring

Figure 4 — Schematic diagram of distillation set up

13

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