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GB/T 11060.4-2017Natural gas -- Determination of sulfur compound -- Part 4: Determination of total sulfur content by oxidative micro-coulometry method (English PDF)

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Issued by

General Administration of Quality Supervision, Inspection and Quarantine

Level / Type

National · Recommended

Issue date

December 29, 2017

Implementation date

July 1, 2018

Scope

GB/T 11060.4-2017 (Natural gas -- Determination of sulfur compound -- Part 4: Determination of total sulfur content by oxidative micro-coulometry method) is available as an English-translated PDF.

GB/T 11060.4-2017 — This part of GB/T 11060 specifies the test method of using the microcoulometry method for the determination of total sulfur in natural gas. This part applies to the determination of total sulfur in natural gas.

The measurement range is 1 mg/m3 ~ 200 mg/m3, and the measurement range can be extended to higher concentrations by dilution.

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Document preview — GB/T 11060.4-2017

National Standard of the People's Republic of China

ICS
75.060
Classification
E 24

Issued by: General Administration of Quality Supervision, Inspection and Quarantine

Contents

  • Foreword .3
  • 1 Scope ..6
  • 2 Normative references .6
  • 3 Test principles .6
  • 4 Reagents .7
  • 5 Instruments ..7
  • 6 Test preparation .8
  • 7 Test procedures ..10
  • 8 Calculation .10
  • 9 Precision.12

Foreword

GB/T 11060 "Natural gas - Determination of sulfur compound" is divided into

the following 12 parts.

- Part 1. Determination of hydrogen sulfide content by iodometric titration

method;

- Part 2. Determination of hydrogen sulfide content by methylene blue

method;

- Part 3. Determination of hydrogen sulfide content by lead acetate reaction

rate dual photo path method;

- Part 4. Determination of total sulfur content by oxidative microcoulometry

method;

- Part 5. Determination of total sulfur content by hydrogenolysis and

rateometric colorimetry method;

- Part 6. Determination of hydrogen sulfide, mercaptan sulfur and carbonyl

sulfide sulfur by potentiometry;

- Part 7. Determination of total sulfur content by Lingener combustion method;

- Part 8. Determination of total sulfur content by ultraviolet fluorescence

method;

- Part 9. Determination of mercaptan sulfur content by iodometric titration

method;

- Part 10. Determination of sulfur compounds using gas chromatography

method;

- Part 11. Determination of mercaptan sulfur content by iodometric titration

method;

- Part 12. Determination of hydrogen sulfide content by laser absorption

spectroscopy.

This part is part 4 of GB/T 11060.

This part was drafted in accordance with the rules given in GB/T 1.1-2009.

This part is an amendment to GB/T 11060.4-2010 "Natural gas - Determination

of sulfur compound - Part 4. Determination of total sulfur content by oxidative

microcoulometry method". As compared with GB/T 11060.4-2010, in addition to

editorial changes, the main technical changes of this part are as follows.

Natural gas - Determination of sulfur compound –

Part 4. Determination of total sulfur content by

oxidative microcoulometry method

Warning - This part does not cover all safety issues related to its

application. Before using this part, the user is responsible for formulating

corresponding safety and protection measures, and defining the scope of

application.

1 Scope

This part of GB/T 11060 specifies the test method of using the microcoulometry

method for the determination of total sulfur in natural gas.

This part applies to the determination of total sulfur in natural gas. The

measurement range is 1 mg/m3 ~ 200 mg/m3, and the measurement range can

be extended to higher concentrations by dilution.

2 Normative references

The following documents are essential to the application of this document. For

the dated documents, only the versions with the dates indicated are applicable

to this document; for the undated documents, only the latest version (including

all the amendments) are applicable to this standard.

GB/T 6682 Water for analytical laboratory use - Specification and test

methods (GB/T 6682-2008, ISO 3696.1987, MOD)

GB/T 8170 Rules of rounding off for numerical values & expression and

judgement of limiting values

GB/T 13609 Natural gas sampling guidelines (GB/T 13609-2017, ISO

10715.1997, MOD)

3 Test principles

Sulfur-containing natural gas is mixed and combusted with oxygen in a quartz

conversion tube, the sulfur is converted into sulfur dioxide, which enters the

titration tank with nitrogen and reacts with iodine. Iodine consumed is

supplemented by electrolytic potassium iodide. In accordance with the

Faraday's law of electrolysis, the amount of sulfur in the sample is calculated

from the amount of electricity consumed by the electrolysis and calibrated with

a gas reference material.

4 Reagents

4.1 Deionized water. Meets the specifications of level II water in GB/T 6682.

4.2 Potassium iodide. Analytically pure.

4.3 Glacial acetic acid. Analytically pure.

4.4 Oxygen. Volume fraction not less than 99.99%.

4.5 Nitrogen. Volume fraction is not less than 99.99%.

4.6 Gas reference materials. It is recommended to use the hydrogen sulfide gas

reference material in methane or nitrogen, or use the thiocarbon-oxygen gas

reference material in methane or nitrogen, which has certificate or analysis

report. The sulfur content of the gas reference material is as close as possible

to the sulfur concentration in the sample to be measured.

5 Instruments

5.1 Converter. it has three separate heating stage (combustion stage,

preheating stage and outlet stage) or one heating stage (combustion stage).

5.2 Titration cell. A pair of electrolysis electrodes and a pair of indication

reference electrodes are inserted in the cell.

5.3 Microcoulometer. When sulfur dioxide enters the titration cell and the

concentration of iodine in the cell is reduced, it can automatically (or manually)

perform contact electrolysis, to restore the iodine to its original level,

automatically record the electrolysis time and current, finally display the sulfur

content directly. The microcoulometer shall have a clear response to 1 ng of

sulfur.

5.4 Flow controller.

5.5 Electromagnetic stirrer.

5.6 Quartz conversion tube.

5.7 Needle valve.

5.8 Medical syringes. 0.25 mL, 1 mL, 2 mL and 5 mL each, which shall have a

ascertained, and re-measurement shall be performed.

7 Test procedures

7.1 Sampling

7.1.1 Sampling from natural gas pipelines

It is performed in accordance with GB/T 13609.

7.1.2 Sampling from gas cylinder

USE the sample to rinse the syringe for 3 to 5 times before formal sampling.

During sampling, it shall use the gas pressure in the bottle to push the syringe

core to the desired scale, then insert the instrument inlet, so that the sample

enters within 3 s ~ 5 s. The injection volume should be controlled between 0.25

mL ~ 5 mL.

7.1.3 Sampling from airbags

USE the sample to rinse the syringe for 3 to 5 times before formal sampling.

During sampling, it shall press the airbag to use the gas pressure in the airbag

to push the syringe core to the desired scale, then insert the instrument inlet,

so that the sample enters within 3 s ~ 5 s. The injection volume should be

controlled between 0.25 mL ~ 5 mL.

7.2 Injection and determination

SWITCH the measurement method to the sample measurement state, ENTER

the sample injection volume (calibration volume), MAKE determination against

the sample in accordance with the method in 6.7.1, then the instrument can

display the total sulfur concentration in the sample.

When the total sulfur content in the sample is higher than the measuring range

of the instrument, the sample can be diluted before measurement. It shall

describe the dilution methods in the test report.

8 Calculation

8.1 Volume conversion

8.1.1 Volume of wet base gas

The volume conversion of the wet base gas sample is performed in accordance

with the formula (1).

......

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 12 pages — is available in the English PDF.

Referenced standards

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