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GB/T 11132-2022Test method for hydrocarbon types in liquid petroleum products - Fluorescent indicator adsorption (English PDF)

液体石油产品烃类的测定 荧光指示剂吸附法

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Issued by

State Administration for Market Regulation; Standardization Administration of China

Level / Type

National · Recommended

Issue date

October 12, 2022

Implementation date

October 12, 2022

Scope

GB/T 11132-2022 is the English-translated version of 液体石油产品烃类的测定 荧光指示剂吸附法.

GB/T 11132-2022 specifies the fluorescent indicator adsorption (FIA) method for determining the hydrocarbon types - total aromatics, total olefins and total saturates - in petroleum fractions boiling below 315 °C, over ranges of 5% to 99% aromatics, 1% to 55% olefins and 1% to 95% saturates by volume.

It applies to full-boiling-range petroleum products and to motor gasoline with or without oxygenates such as methanol, ethanol, MTBE, TAME and ETBE, whose results are corrected to a whole-sample basis; it does not apply to samples with dark components that obscure the bands, and its precision does not cover narrow fractions boiling near 315 °C. About 0.75 mL of sample is adsorbed on activated silica gel with a fluorescent dye layer in a glass column, desorbed with alcohol under gas pressure, and the volume fraction of each type is calculated from the length of its zone under ultraviolet light; the standard details the standard-wall and precision-bore columns and their tolerances, reagents, procedure, calculation, report and precision.

It replaces GB/T 11132-2008, deleting the significance and use clause, adding an optional threaded pressurised gas connection, a calculation note and report content for oxygenate-containing samples, and revising the sample and content ranges of the precision tables.

Issued on 12 October 2022 and in force from the same date. Classification: ICS 75.080, CCS E30. The document runs to 20 pages, delivered complete in English translation.

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Document preview — GB/T 11132-2022

National Standard of the People's Republic of China

ICS
75.080
Classification
E30
Replacing
GB/T 11132-2008

Issued by: State Administration for Market Regulation; Standardization Administration of China

Contents

  • ForewordI
  • 1 Scope1
  • 2 Normative references1
  • 3 Terms and definitions2
  • 4 Summary of the method2
  • 5 Apparatus2
  • 5.1 Adsorption column2

Foreword

This document is drafted in accordance with the rules given in GB/T 1.1-2020, Directives for standardization - Part 1: Rules for the structure and drafting of standardizing documents.

This document replaces GB/T 11132-2008, Test method for hydrocarbon types in liquid petroleum products - Fluorescent indicator adsorption. Compared with GB/T 11132-2008, apart from structural adjustments and editorial changes, the main technical changes are as follows:

- the clause "Significance and use" has been deleted (see Clause 5 of the 2008 edition);

- an optional pressurised gas connection for the adsorption column and its schematic diagram have been added (see 5.1.4 and Figure 2);

- the method of fixing the adsorption column at the end of the ruler has been deleted (see 10.2 of the 2008 edition);

- the determination of the pH value of the silica gel has been changed into a table footnote (see Table 2; 7.1 of the 2008 edition);

- a calculation note for samples containing oxygenates has been added (see 10.2);

- report content for samples containing oxygenate blending components has been added (see 11.2);

- the sample range to which the precision Tables 3 and 4 apply has been changed (see Note to Table 3 and Note 1 to Table 4; 1.4 of the 2008 edition);

- the applicable content ranges of the hydrocarbon types in Table 4 have been changed (see Table 4; Table 4 of the 2008 edition).

Attention is drawn to the possibility that some elements of this document may be the subject of patent rights. The issuing body of this document shall not be held responsible for identifying any or all such patent rights.

This document was proposed by and is under the jurisdiction of the National Technical Committee on Petroleum Products and Lubricants of Standardization Administration of China (SAC/TC 280).

Drafting organisation of this document: SINOPEC Fushun Research Institute of Petroleum and Petrochemicals (China Petroleum and Chemical Corporation).

Main drafters of this document: Zhao Bin, Geng Chenchen, Gui Xinghua and Ling Fengxiang.

The previous editions of this document and of the documents it replaces are as follows:

- first published in 1989 as GB/T 11132-1989, first revised in 2002 and revised for the second time in 2008;

- this is the third revision.

1 Scope

Warning - Persons using this document should have practical experience of formal laboratory work. The use of this document may involve hazardous materials, equipment and operations; this document does not purport to address all the safety problems that may be associated with its use. It is the responsibility of the user to take appropriate safety and health measures and to ensure compliance with the conditions stipulated by the relevant national regulations.

This document describes a method for the determination of hydrocarbon types in petroleum fractions boiling below 315 °C by fluorescent indicator adsorption.

This document is applicable to the determination of hydrocarbon types - total aromatics, total olefins and total saturates - in petroleum fractions boiling below 315 °C, over the following ranges: aromatics 5% to 99% by volume, olefins 1% to 55% by volume and saturates 1% to 95% by volume. This document may also be used for samples with concentrations outside these ranges, but the precision has not been determined. This document is not applicable to samples containing dark-coloured components that interfere with the reading of the hydrocarbon chromatographic bands.

This document is applicable to petroleum products of full boiling range, but statistical test data show that the precision of this document does not apply to narrow petroleum fractions boiling close to 315 °C: such samples do not separate properly and the results are unstable.

This document may also be used for automotive spark-ignition engine fuels (motor gasoline), with or without oxygenates such as alcohols and ethers (for example MTBE, ethanol), where gasoline is the main component by volume of the blend.

This document is applicable to samples containing certain oxygenate blending components. These oxygenates are methanol, ethanol, methyl tert-butyl ether (MTBE), tert-amyl methyl ether (TAME) and ethyl tert-butyl ether (ETBE); at the concentrations found in normal blended products they do not interfere with the hydrocarbon type determination, as they are eluted with the alcohol desorbent and are not detected. Other oxygenates shall be verified individually. When samples containing oxygenate blending components are analysed, the results are corrected to a whole-sample basis.

It has not been established whether this document is applicable to products derived from non-petroleum fossil fuels such as coal, shale or oil sands bitumen; its precision may or may not apply to such products.

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.

GB/T 4756 Method for manual sampling of petroleum liquids

GB/T 5816 Catalysts and adsorbents - Determination of surface area

GB/T 6003.1 Test sieves - Technical requirements and testing - Part 1: Test sieves of metal wire cloth

GB/T 6536-2010 Standard test method for distillation of petroleum products at atmospheric pressure

GB/T 27867 Petroleum liquids - Automatic pipeline sampling

NB/SH/T 0663 Determination of alcohols and ethers in gasoline - Gas chromatography

SH/T 0720 Determination of oxygenates in gasoline (gas chromatography and oxygen selective flame ionization detection)

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.

3.1 Aromatics

Monocyclic and polycyclic aromatic hydrocarbons, aromatic olefins, certain dienes, and compounds containing sulfur or nitrogen, or oxygenates of higher boiling point (except those oxygenates listed in Clause 1).

3.2 Olefins

Hydrocarbons containing carbon-carbon double bonds (olefinic bonds).

Note: including cycloolefins and certain dienes.

3.3 Saturates

The collective term for alkanes and cycloalkanes.

4 Summary of the method

Approximately 0.75 mL of the sample is introduced into a glass adsorption column packed with activated silica gel, the separation section of which contains a thin layer of silica gel impregnated with a mixture of fluorescent dyes. When the whole sample has been adsorbed on the gel, alcohol is added to desorb the sample, and pressure is applied to force the sample down the column. The hydrocarbons in the sample are separated into aromatics, olefins and saturates according to their adsorption affinities. The fluorescent dyes are also selectively separated together with the hydrocarbon types, making the boundaries of the aromatic, olefin and saturate zones clearly visible under ultraviolet light. The volume fraction of each hydrocarbon type is calculated from the length of its coloured zone in the adsorption column.

5 Apparatus

5.1 Adsorption column

5.1.1

The adsorption column is made of precision-bore glass tubing [as shown in Figure 1 b)], comprising a charger section with a capillary neck, a separation section and an analytical section; or of standard-wall glass tubing [as shown in Figure 1 a)]. The permissible dimensional tolerances of the adsorption column are given in Table 1.

Table 1 - Permissible dimensional tolerances of the adsorption column (dimensions in millimetres; standard-wall glass tubing column / precision-bore glass tubing column):

Charger section: inside diameter 12 ± 2 / 12 ± 2; height of silica gel packing approximately 75 / approximately 75; total length 150 ± 5 / 150 ± 5.

Capillary neck: inside diameter 2 ± 0.5 / 2 ± 0.5; total length 50 ± 5 / 50 ± 5.

Separation section: inside diameter 5 ± 0.5 / 5 ± 0.5; total length 190 ± 5 / 190 ± 5.

Long taper below the separation section: tip outside diameter 3.5 ± 0.5 / -; tip inside diameter 2 ± 0.5 / -; total length 25 ± 2 / -.

Analytical section: inside diameter 1.5 ± 0.5 / 1.60 to 1.65; total length 1 200 ± 30 / 1 200 ± 30.

Column end: total length - / 30 ± 5.

Figure 1 - Adsorption column: a) standard-wall glass tubing column; b) precision-bore glass tubing column, with an optional clamp arrangement shown (dimensions in millimetres). Key: 1 compressed gas; 2 28/12 ball joint; 3 height of silica gel packing; 4 charger section; 5 chromatographic silica gel; 6 long taper connection; 7 dyed silica gel; 8 separation section; 9 polyethylene tubing; 10 analytical section; 11 12/2 ball joint; 12 column end; 13 tip drawn out into a fine capillary.

5.1.2

Precision-bore glass tubing column: the inside diameter of the analytical section shall be 1.60 mm to 1.65 mm, and a mercury thread approximately 100 mm long shall not vary in length by more than 0.3 mm in any part of the analytical section. The sections of the column shall be joined by long taper connections. A small plug of glass wool is placed between the ball and socket of the 12/2 ball joint to support the silica gel in the column and to cover the outlet of the analytical section. The inside diameter of the column end connected to the socket shall be 2 mm. The ball and socket of the ball joint are held tightly together with a clamp, ensuring that the column end remains in line with the analytical section during packing and testing. For a disposable analytical section of 3 mm diameter, if its internal geometry is essentially the same as described above and it provides a smooth transition between the internal diameters of the two glass sections, a commercially available compression connector may be used to connect the bottom of the separation section (cut off square). A similar commercially available connector may also be used at the end of the 3 mm diameter analytical section, since it has an integral porous frit that can support the silica gel in the column.

5.1.3

Standard-wall glass tubing column: for convenience, a standard-wall glass tubing column [as shown in Figure 1 a)] may also be used. When standard-wall glass tubing is used as the analytical section, its inside diameter shall be uniform and the joint between the analytical section and the separation section shall be sealed. Calibration of the inside diameter of standard-wall glass tubing is not easily achieved, but its outside diameter can be measured along the tube with a vernier caliper; if the outside diameter varies by 0.5 mm or more, the inside diameter is regarded as irregular and the column shall not be used. To prevent the silica gel from running out of the glassware, one method is to draw out the lower end of the analytical section into a fine capillary. The upper end of the analytical section is connected to the separation section with a piece of polyethylene tubing (30 ± 5) mm long, ensuring that the two glass sections are in contact. To obtain a good seal between the analytical section and the polyethylene tubing, the upper end of the analytical section is heated just enough to soften the polyethylene tubing and then inserted into it; alternatively, the joint between the polyethylene tubing and the glass analytical section is sealed by winding soft metal wire tightly around it. For a disposable analytical section of 3 mm diameter, if its internal geometry is essentially the same as described above and it provides a smooth transition between the internal diameters of the two glass sections, a commercially available compression connector may be used to connect the bottom of the separation section (cut off square). A similar commercially available connector may also be used at the end of the 3 mm diameter analytical section, since it has an integral porous frit that can support the silica gel in the column.

5.1.4

As an alternative to the ball joint connection, a threaded pressurised gas connection may be used, as shown in Figure 2. Apart from the connection, all dimensions and requirements of the adsorption column remain unchanged.

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 20 pages — is available in the English PDF.

Referenced standards

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Editions of GB/T 11132

EditionTitleRevisionStatus
GB/T 11132-2022Test method for hydrocarbon types in liquid petroleum products - Fluorescent indicator adsorptioncurrent editionCurrent
GB/T 11132-2008Standard test method for hydrocarbon types in liquid petroleum products by fluorescent indicator adsorptionprevious editionSuperseded

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