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GB/T 223.82-2018Steel and iron—Determination of hydrogen content—Thermal conductivity/infrared method after fusion under inert gas (English PDF)

钢铁 氢含量的测定 惰性气体熔融-热导或红外法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

May 14, 2018

Implementation date

February 1, 2019

Scope

GB/T 223.82-2018 is the English-translated version of 钢铁 氢含量的测定 惰性气体熔融-热导或红外法.

GB/T 223.82-2018 sets out how to determine the hydrogen content of steel and iron by fusing the sample under inert gas and detecting the released hydrogen by thermal conductivity or infrared absorption.

It applies to mass fractions from 0.6 µg/g to 30.0 µg/g. The sample is fused in a degassed graphite crucible, and the hydrogen passes into the carrier gas of argon, nitrogen or helium, is separated from other gases on a chromatographic column and is measured.

The standard covers reagents and materials, the analyser, sampling and sample preparation for pre-furnace, ingot, profile, powdered and other samples, the blank test, single-point and multi-point calibration, sample analysis, calculation of the result in µg/g and precision.

It replaces GB/T 223.82-2007, was issued on 14 May 2018 and has applied since 1 February 2019.

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Document preview — GB/T 223.82-2018

National Standard of the People's Republic of China

ICS
77.080.01
Classification
H 11
Replacing
GB/T 223.82-2007

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Foreword3
  • 1 Scope4
  • 2 Normative References4
  • 3 Principle4
  • 4 Reagents and Materials5
  • 5 Instruments5
  • 6 Sampling and Sample Preparation5
  • 7 Analytical Procedures7
  • 8 Result Calculation9
  • 9 Precision10
  • 10 Test Report10
  • Appendix A (informative appendix)11

Foreword

This is No. 82 part of GB/T 223.

This Part is drafted in accordance with stipulations in GB/T 1.1-2009.

This Part is drafted as a replacement of GB/T 223.82-2007 Steel and Iron - Determination of Hydrogen Content - Inert Gas Impulse Fusion Heat Conductivity Method. In comparison with GB/T 223.82-2007, there are the following main changes to the content.

---The name of the Standard is modified;

---The range of determination is modified;

---The content of infrared method is added to detection;

---The content of ultrasonic cleaning, powdered sample and crumbed sample is added to sampling and preparation of sample;

---The content of single-point calibration and multi-point calibration is added to calibration;

---"7 Analytical Procedure", previous "5.2 Instrument Preparation", "7 Calibration" and "8 Measurement" are added to Chapter 7;

---Formula of repeatability limit and reproducibility limit in "9 Precision" is modified.

1 Scope

This Part in GB/T 223 specifies methods of determining hydrogen content through thermal conductivity or infrared method after fusion under inert gas.

This Part is applicable to the determination of hydrogen content in steel and iron (mass fraction. 0.6 µg/g ~ 30.0 µg/g).

2 Normative References

The following documents are indispensable to the application of this Standard. In terms of references with a specified date, only versions with a specified date are applicable to this Standard. The latest version (including all the modifications) of references without a specified date is also applicable to this Standard.

GB/T 6379.1 Accuracy (Trueness and Precision) of Measurement Methods and Results - Part 1: General Principles and Definitions (GB/T 6379.1-2004, ISO 5725-1:1994, IDT)

GB/T 6379.2 Accuracy (Trueness and Precision) of Measurement Methods and Results - Part 2: Basic Method for the Determination of Repeatability and Reproducibility of a Standard Measurement Method (GB/T 6379.2-2004, ISO 5725-2:1994, IDT)

GB/T 20066 Steel and Iron - Sampling and Preparation of Samples for the Determination of Chemical Composition (GB/T 20066-2006, ISO 14284:1996, IDT)

3 Principle

Place reagent in a degassed graphite crucible; heat it up and fuse it under inert gas.

In reagent, hydrogen is released in the form of molecular, and enters carrier gas flow.

After isolating it from other gases with chromatographic column, conduct the detection in thermal conductivity cell.

4 Reagents and Materials

4.1 High-purity carrier gas (purity. >= 99.99%). argon, nitrogen or helium, depends on instrument manufacturer's recommendation.

4.2 Power gas, nitrogen, argon or compressed air; oil and water content < 0.5%; flammable gas is prohibited.

4.3 Carbon tetrachloride, acetone or ether (analytical purity).

4.4 Anhydrous magnesium perchlorate (granular reagent).

4.7 Graphite (electrode) crucible, disposable, made of high-purity graphite.

4.8 Hydrogen standard substance/standard sample in steel (iron).

5 Instruments

Inert gas fusion - thermal conductivity or infrared hydrogen detection analyzer, including pulsed graphite electrode furnace, analytical airflow impurity removal system, auxiliary purification system and thermal conductivity cell or infrared pool hydrogen determination system.

6 Sampling and Sample Preparation

6.1 General Requirements

Sampling and preparation of sample shall comply with stipulations in GB/T 20066.

6.2 Pre-furnace Sampling and Sample Preparation

Pre-furnace sampling shall adopt exclusive sampling devices. Before adopting a new pre-furnace sampling method or a new sampling device, its reliability and availability shall be evaluated; an evaluation report shall be issued for the record.

6.3 Sampling and Sample Preparation on Steel Ingot or Profile

In terms of forged or casted workpiece, the mode of sawing, digging and wire-electrode cutting is recommended for sampling. The mode of water soldering open flame cutting is not recommended for sampling.

6.4 Powdered Sample

Powdered sample needs to be taken from a great deal of evenly mixed powder. After sampling, store the sample in a clean plastic zip lock bag for a short time; store it in a vacuum bag, argon bag or sealed glass bottle for a long time. Since paper bag is water and gas permeable, it is not recommended here.

6.5 Crumbed Sample

Crumbed sample that is taken from profit or casted workpiece cannot be adopted as hydrogen determination sample, because of hydrogen transfer during the processing.

6.6 Other Samples

Materials in abnormal shapes shall be sampled in accordance with the materials. The operation of sampling can adopt certain modes of processing, such as cutting, sawing and wire-electrode cutting. Avoid overheat and contamination. Wire materials can be directly sampled.

7 Analytical Procedures

7.1 Instrument Preparation

7.1.1 Initiate the instrument in accordance with requirements in the instruction for use provided by instrument manufacturer; confirm that flow meter and pressure gauge on the instrument are indicating the specified position.

7.1.2 If necessary, conduct air-leak check of the instrument while the power is connected, and the water-cooling system is initiated.

7.1.3 Configurate parameters of the instrument; pre-heat and stabilize the instrument. The following analytical conditions are recommended.

7.2 Blank Test

Conduct blank test before the procedure of analysis and determination. Conduct at least 3 blank value determinations; replace a new crucible in each determination. The deduction of blank value can be automatic or manual.

7.3 Calibration (any calibration procedure can be adopted)

7.3.1 Single-point calibration

7.3.1.1 Select hydrogen standard substance/standard sample (4.8) in 2 types of steel (iron); its hydrogen content shall be higher or close to the hydrogen content of the sample to be tested; the detection range of this method shall not be exceeded.

7.3.2 Multi-point calibration

7.3.2.1 Select hydrogen standard substance/standard sample (4.8) in at least 4 types of steel (iron); its hydrogen content shall be different and within the detection range of this method.

7.3.2.2 Conduct multi-point calibration in accordance with requirements in the instruction for use of the instrument. Analyze at least 3 standard substances/standard samples (7.3.2.1); each standard substance/standard sample shall be analyzed for 3 times; respectively take the average value; determine calibration curve slope and intercept through multiple points of of hydrogen content.

7.3.2.5 In accordance with the procedure described in the instruction for use of the instrument, store this calibration in the form of method; name this method.

7.3.3 Calibration frequency requirements

Instrument shall be calibrated for at least 1 time every year. When any of the abnormal circumstances emerge, instrument shall be re-calibrated to guarantee the reliability and validity of measurement.

7.4 Sample Analysis

7.4.1 Select a suitable analytical method (7.3.1.5 or 7.3.2.5). The adopted analytical conditions shall maintain consistency with the analytical conditions adopted for calibration. If the sample to be determined is powdered, corresponding standard substance/standard sample shall be adopted for calibration.

7.4.2 Input sample information in accordance with the procedure required in the instruction for use of the instrument.

7.4.3 Weigh-take 0.5 g ~ 1.0 g of sample (accurate to 0.001 g) (if there are any special […]

8 Result Calculation

Hydrogen content shall be calculated by mass fraction (µg/g).

9 Precision

In the precision test of this method, 10 cooperative organizations and 10 laboratories shall determine 6 content levels of hydrogen element. Each laboratory shall determine 2 ~ 3 times of each content level under the repeatability conditions stipulated in GB/T 6379.1. […]

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.

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Editions of GB/T 223.82

EditionTitleRevisionStatus
GB/T 223.82-2018Steel and iron—Determination of hydrogen content—Thermal conductivity/infrared method after fusion under inert gascurrent editionCurrent
GB/T 223.82-2007Steel and iron—Determination of hydrogen content—Thermal conductivity/infrared method after fusion under inert gasprevious editionSuperseded

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