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GB/T 23942-2009 English PDF (GBT23942-2009)

GB/T 23942-2009 English PDF (GBT23942-2009)

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GB/T 23942-2009: Chemical reagent -- General rules for inductively coupled plasma atomic emission spectrometry

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.
GB/T 23942-2009
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 71.040.30
G 60
Chemical reagent - General rules for inductively
coupled plasma atomic emission spectrometry
ISSUED ON. JUNE 02, 2009
IMPLEMENTED ON. FEBRUARY 01, 2010
Issued by. General Administration of Quality Supervision, Inspection and Quarantine;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Methodology ... 6
5 Reagents ... 7
6 Instruments ... 7
7 Determination ... 7
8 Recovery rate ... 10
9 Safety considerations ... 10
Appendix A (Normative) Quartz sub-boiling distillation device ... 11
Appendix B (Normative) Preparation of multi-element group standard solution ... 13
Appendix C (Informative) Test element analysis spectral line wavelength ... 14 Appendix D (Normative) Detection limit determination method ... 16
Foreword
Appendix A, Appendix B and Appendix D of this standard are normative
appendixes. Appendix C is an informative appendix.
This standard was proposed by China Petroleum and Chemical Industry
Association.
This standard shall be under the jurisdiction of the National Chemical
Standardization Technical Committee Chemical Reagents Subcommittee
(SAC/TC 63/SC 3).
Drafting organizations of this standard. China Institute of Metrology, Beijing Institute of Chemical Reagents.
Main drafters of this standard. Shi Naijie, Li Haifeng, Ma Liandi, Han Baoying. Test method for total bacterial count in electronic
grade water by membrane filters
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
GB/T 6682 Water for analytical laboratory use - Specification and test
methods (GB/T 6682-2008, ISO 3696.1987, MOD)
JJG 768 Verification regulation of emission spectrometer
3 Terms and definitions
The following terms and definitions established by GB/T 4470 apply to this standard.
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. 5.3 The standard solution shall be certified single element solution standard substance or be prepared in accordance with the provisions of GB/T 602, multi- element standard solution is prepared in accordance with Appendix B.
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. 6.2.2 Sequential inductively coupled plasma atomic emission spectrometer. 6.2.3 Full spectrum direct reading 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.
7.1.2 Incident power
SELECT the optimal power in accordance with the characteristics of the sample The amount of sample is determined based on the mass concentration of the element to be detected in the sample and the detection limit of the method; the mass concentration of the element to be detected in the sample solution shall be at least three times the detection limit of the element. The determination method of detection limit is shown in Appendix D.
7.3.2 Working curve method
PREPARE sample solution, blank test solution, and four to five standard solutions in proportion to the mass concentration in accordance with the product standard. Under the specified instrument conditions, respectively DETERMINE the corresponding strength values. USE the mass concentration of the standard solution as the abscissa, and the corresponding intensity value as the ordinate, to draw the standard working curve. FIND the mass concentration of the test element in the sample solution from the working curve.
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. Under the specified instrument conditions, respectively DETERMINE the corresponding strength value. USE the mass concentration of the standard solution as the abscissa, and the corresponding intensity value as the ordinate, to draw a curve, EXTEND the curve in the opposite direction to intersect with the horizontal axis. The intersection point is the mass concentration of the test element.
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).
Where.
?? - The value of the mass concentration of the measured element from the curve, in micrograms per milliliter (??g/mL);
V - The volume of the sample solution, in milliliters (mL);
m - The value of the sample mass, in grams (g).

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