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GB/T 23942-2009Chemical reagent - General rules for inductively coupled plasma atomic emission spectrometry (English PDF)

化学试剂 电感耦合等离子体原子发射光谱法通则

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

June 2, 2009

Implementation date

February 1, 2010

Scope

GB/T 23942-2009 is the English-translated version of 化学试剂 电感耦合等离子体原子发射光谱法通则.

GB/T 23942-2009 is the Chinese standard "Chemical reagent - General rules for inductively coupled plasma atomic emission spectrometry".

Its scope clause reads: This standard specifies the requirements and methods for the determination of metal and non-metallic impurities in chemical reagents by inductively coupled plasma atomic emission spectrometry.

This standard applies to the liquid specimen of chemical reagents containing a variety of impurities or the direct sample injection of the sample solution after removal of the substrate which is determined by the inductively coupled plasma atomic emission spectrometry (ICP-AES).

This standard does not apply to solid sample injection. Its clauses include terms and definitions; methodology; reagents; instruments; determination; recovery rate; safety considerations.

It was issued by the General Administration of Quality Supervision, Inspection and Quarantine on JUNE 02, 2009 and took effect on FEBRUARY 01, 2010.

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Document preview — GB/T 23942-2009

National Standard of the People's Republic of China

ICS
71.040.30
Classification
G 60

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

Contents

  • Foreword3
  • 1 Scope4
  • 2 Normative references4
  • 3 Terms and definitions4
  • 4 Methodology6
  • 5 Reagents7
  • 6 Instruments7
  • 7 Determination7
  • 8 Recovery rate10
  • 9 Safety considerations10
  • Appendix A (Normative) Quartz sub-boiling distillation device11
  • Appendix B (Normative) Preparation of multi-element group standard solution13
  • Appendix C (Informative) Test element analysis spectral line wavelength14
  • Appendix D (Normative) Detection limit determination method16

Foreword

Appendix A, Appendix B and Appendix D of this standard are normative appendixes. Appendix C is an informative appendix.

1 Scope

This standard specifies the requirements and methods for the determination of metal and non-metallic impurities in chemical reagents by inductively coupled plasma atomic emission spectrometry.

This standard applies to the liquid specimen of chemical reagents containing a variety of impurities or the direct sample injection of the sample solution after removal of the substrate which is determined by the inductively coupled plasma atomic emission spectrometry (ICP-AES). This standard does not apply to solid sample injection.

2 Normative references

The provisions in following documents become the provisions of this standard through reference in this standard. For the dated references, the subsequent amendments (excluding corrections) or revisions do not apply to this standard; however, parties who reach an agreement based on this standard are encouraged to study if the latest versions of these documents are applicable.

For undated references, the latest edition of the referenced document applies.

GB/T 602 Chemical reagent - Preparations of standard solutions for impurity (GB/T 602-2002, ISO 6353-1:1982, NEQ)

GB/T 4470 Analytical spectroscopic methods - Flame emission, atomic absorption and atomic fluorescence - Vocabulary

GB/T 4842 Argon

3 Terms and definitions

The following terms and definitions established by GB/T 4470 apply to this standard.

3.1 High frequency generator

A high frequency power source that provides high frequency energy to the coupling coil and plasma.

3.2 Plasma torch

A device consisting of three layers of concentric quartz tubes to maintain a stable discharge of inductively coupled plasma (ICP).

3.3 Incident power

The net power delivered by the high frequency generator to the coupling coil and the plasma.

3.4 Observation height

Select the height of the exposed part of the plasma torch.

3.5 Coolant gas

The outermost gas flow of the torch which serves to cool the torch and maintain the plasma.

4 Methodology

The sample solution is atomized by the atomization system to form an aerosol, which is carried into the plasma by the carrier gas, evaporated, atomized, excited and ionized in a high-temperature and inert argon atmosphere.

5 Reagents

5.1 Hydrochloric acid and nitric acid shall select high-purity reagents or superior pure reagents which is subject to sub-boiling distillation (SEE Appendix A for the quartz sub-boiling distillation apparatus).

5.2 The test water shall meet the level II water specification in GB/T 6682.

6 Instruments

6.1 General requirements

The inductively coupled plasma atomic emission spectrometer shall comply with the provisions of JJG 768.

6.2 Instrument type

6.2.1 Multichannel inductively coupled plasma atomic emission spectrometer

6.3 Instrument composition

The inductively coupled plasma atomic emission spectrometer consists of an injection system, an excitation light source, a dispersion system, a detection system, and a data processing system.

7 Determination

7.1 Selection of measurement conditions

7.1.1 Analytical spectral lines of the elements under test

The wavelength of the analytical line of the element under test is given in Appendix C.

7.1.4 Gas and flow

In accordance with the torch and analysis requirements, DETERMINE the gas flow. The argon used shall meet the requirements of GB/T 4842.

7.1.5 Solution extraction rate

The extraction rate of the solution is generally (0.5 ~ 2) mL/min.

7.1.6 Analysis time

The rinse time and exposure time are determined by the instrument and analysis requirements.

7.2 Elimination of interference

7.2.1 The use of appropriate separation methods and selection of appropriate

element spectral lines, observation heights, incident power, and carrier gas flow may limit some of the interference effects in the light source to a certain level.

7.3 Measurement methods

7.3.1 Processing of samples

In accordance with the characteristics of the sample and the measurement characteristics of the instrument, the sample matrix may be removed by a separation method such as volatilization, acid digestion, alkali digestion, dry ashing, extraction, ion exchange, precipitation, or directly diluted to prepare a sample solution.

7.3.3 Standard addition method

PREPARE test solutions and blank solutions as specified in product standards.

MEASURE the same volume of the above test solution, at least four sets. DO not add standard solution in one set, ADD standard solution in proportions respectively into the rest sets, DILUTE it to the specified volume.

7.3.4 Calculation

The mass fraction of the elements to be measured is calculated by w, expressed in terms of "%" and calculated in accordance with formula (1).

8 Recovery rate

The test element recovery rate shall be controlled at 80% ~ 120%.

9 Safety considerations

9.1 High-pressure argon cylinders shall be used in accordance with the provisions for the safe operation of high-pressure cylinders.

Appendix A (Normative) Quartz sub-boiling distillation device

9.3 Pay attention to safe electricity

A.1 Quartz sub-boiling distillation device

SEE Figure A.1.

Appendix B (Normative) Preparation of multi-element group standard solution

B.1 Multi-element group standard solution shall use certified multi-element solution standard substance, the other requirements are same as clause 5.

B.2 Elements that interfere with each other chemically, produce sediments, and have spectral interferences shall be prepared in groups.

A.2 Precautions

A.2.1 The temperature shall be strictly controlled below the boiling point of the acid and the solution must not boil.

A.2.2 Distilled liquid flow rate shall be controlled at about 40 mL/h. […]

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 16 pages — is available in the English PDF.

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