This standard specifies the test method for the determination of trace metals copper, nickel, sodium and potassium in electronic grade water using a flameless (or flame) atomic absorption spectrophotometer. GB/T 11446.5-1997 Atomic absorption spectrophotometric test method for trace metals in electronic grade water GB/T11446.5-1997 Standard download decompression password: www.bzxz.net

GB/T 11446.3-11446.10-1997 GB/T11446.3~11446.10-1997 are respectively GB11446.3-89 "General Rules for Testing Methods of Electronic Grade Water", GB11446.4-89 "Test Methods for Resistivity of Electronic Grade Water", GB11446.5-89 "Atomic Absorption Spectrophotometric Test Methods for Trace Metals in Electronic Grade Water", GB11446.6-89 "Spectrophotometric Test Methods for Trace Silica in Electronic Grade Water", GB11446.7-89 "Ion Chromatographic Test Methods for Trace Ions in Electronic Grade Water", GB11446.8-89 "Test Methods for Total Organic Carbon in Electronic Grade Water", GB11446.9: 89 Instrumental Test Method for Particles in Electronic Grade Water". GB11446.10-89 "Filter Culture Test Method for Total Bacteria in Electronic Grade Water" has been revised.
Since GB/T11446.1 has added technical indicators for the leaving factory of metal nickel, nitrate ions, phosphate ions, and sulfur rubber ions, this standard has added the test methods for the determination of metal nickel by atomic absorption spectrophotometry and the determination of nitrate, phosphate, and sulfate by ion chromatography. The test method for bacteria only uses the filter culture method, and the method for measuring total organic carbon has also been completely rewritten. The general principles of test methods, the method for measuring resistivity, and the method for determining total silicon have all been revised and rewritten. This standard is implemented from the date of implementation, and G13 11446.3~11446.1089.
This standard is proposed by the Ministry of Electronics Industry of the People's Republic of China. This standard is submitted by the Standardization Institute of the Ministry of Electronics Industry of the People's Republic of China. The drafting units of this standard are: Institute of Semiconductors, Chinese Academy of Sciences, and Standardization Institute of the Ministry of Electronics Industry. The main drafters of this standard are: Wen Ruimei, Li Xiaoying, Wang Zaizhong, Xu Xuemin, You Pan, Liu Renzhong, and Xu Xiuxin. ..com1 Scope
National Standard of the People's Republic of China
Test method for measuring trace metals in electronicgrade water by atomic absorption spectrophotometryGB/T 11446.5-1997
Replaces GB11446.5-89
This standard specifies the test method for determining trace metals of copper, zinc, nickel, sodium and potassium in electronic grade water using flame (or flame) atomic absorption spectrophotometer.
Non-flame atomic absorption spectrophotometry is applicable to the determination of trace metals in D- to I-grade electronic grade water. The detection limit of the method is less than 10-1%.
Fire-roasted atomic absorption spectrophotometry is applicable to the determination of trace metals in I-grade electronic grade water. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard by reference in this standard. The versions shown are valid at the time of publication of this standard. All standards will be revised. All parties using this standard should explore the possibility of using the following standards to promote the latest version. GB/T 11446.1-1997 Electronic Grade Water
GB/T11446.3-1997 General Rules for Testing Methods of Electronic Grade Water 3 Principle
The determination of trace metals by atomic absorption spectrophotometry is based on the absorption of light with characteristic spectral lines of the elements to be measured from the light source by atoms of the elements to be measured in the ground state in the sample vapor, and the content of the elements to be measured in the sample is determined according to the degree of attenuation of the radiated characteristic spectral line light.
This method uses a flameless (or flame-melting) atomic absorption spectrophotometer at wavelengths of 324.7nm, 213.9nmml, 232.0mm, 589.nm766.5nm to measure the absorbance of metal elements such as copper, zinc, nickel, sodium, potassium, etc. in the water sample to be measured, and then the content of the elements to be measured corresponding to each absorbance is obtained from the standard curve. 4 Reagents
4.1 Blank water: water in accordance with GB/T11446.1 electronic grade water. 4.2 Carbon nitrate: MOS grade.
4.3 Hydrochloric acid: (I+1)(V/V).MOS grade.
4.4 Standard solution: Use secondary standard substances approved by the State Technical Supervision Bureau. The standard substances for water component analysis GBW(E) are copper (080122), zinc (080130), nickel (080141), sodium (080127), potassium (080125). Or national standard substances BW series water quality standard solution provided by the research center.
Approved by the State Administration of Technical Supervision on September 1, 1997 and implemented on September 1, 1998
5 Instruments and blood
GB/T11446.5-1997
5.1 Atomic absorption spectrophotometer: including four parts: hollow cathode lamp, atomization system, graphite furnace (or flame atomizer), spectrophotometer system and detection and recording system.
5.2 Sampler: automatic sampler or microsampler, flame atomization sprayer. 5.3 Polyethylene bottle: 25 ml, 50 mL, 100 mL. 5.4 Pipette, 0.2 mL~5.0 mL
5.5 Volumetric flask: 25.0 mL~-100.0 ml. 6 Test steps
6.1 Selection of instrument conditions
For the selection of the best instrument parameters (lamp current, slit width, etc.) according to different instrument models, see Appendix A (suggestive appendix). For the selection of operating conditions of the stone furnace atomizer, see Appendix A (suggestive appendix). 6.2 Injection volume
The injection volume is determined according to the sensitivity of the element to be measured and the content of metal elements in the water sample. 20μL~1pl. is generally selected for graphite furnace injection. When the content is extremely low, multiple injections can be used to reduce the lower limit of determination: when performing flame analysis, the sample is sprayed into the flame until a stable maximum absorption value is obtained.
6.3. Drawing of working curves
6.3.1 Preparation of standard series working solutions: Prepare the standard solutions into the corresponding series by step-by-step dilution, see Table 1. Table 1 Standard series solutions
6.3.2 Drawing of working curves: Prepare the standard series working solutions by step-by-step dilution, see Table 1. The quasi-series L working solutions are measured under the optimal conditions of the above instruments, and the measured absorbance (generally the height) is used as the ordinate and the corresponding temperature is used as the abscissa to draw a graph, and the slope of the working curve is obtained. 6.4 Determination of water samples
Absorb a certain amount of water sample into a stone tube (or spray the water sample into a flame towel), and after measuring the absorbance, find out the light element content corresponding to the absorbance from the working curve.
7 Precision
The precision of this method is shown in Table 2.
8 Test report
CB/T11446.5-1997
The report format of the content of the measured elements in the sample is in accordance with the requirements of Chapter 6 of GB/T11446.3--1997. 9 PrecautionsWww.bzxZ.net
9.1 Whether the laboratory air is purified or not has a great influence on the analysis results, and it is best to be carried out in a clean room. 9.2 Before adding each sample, the graphite furnace must be burned to zero reading, or a blank test must be performed. Standard deviation
3 After measuring a certain number of samples, a standard sample should be analyzed to check the life of the graphite tube. If there is any impact, a new graphite tube should be replaced. 9.3
9.4 Water samples should be analyzed as soon as possible. The longer they are stored, the greater the possibility of contamination. If it is not possible to analyze immediately, it should be stored in a refrigerator. Drying stage GB/T 11446. 5—1997 Appendix A (suggestive appendix) Instrument working conditions Lamp protection HGA-500 graphite furnace working conditions Ashing stage Heating time/holding time Heating time/holding time Spectral passband width Atomization stage Heating time/holding time Note: When the injection volume is 20μl, the drying holding time is 30%; the hydrogen flow is 50mL/min in the atomization stage and 300ml/min in other stages.
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