This standard specifies the ion chromatography test method for trace chloride ions (CL-), nitrate ions (NO3-), phosphate ions (PO43-), and sulfate ions (SO42-) in electronic grade water. This standard is applicable to the detection of trace chloride ions, nitrate ions, phosphate ions, and sulfate ions in electronic grade water. GB/T 11446.7-1997 Ion chromatography test method for trace chloride ions, nitrate ions, phosphate ions, and sulfate ions in electronic grade water GB/T11446.7-1997 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. ..com1Scope
National Standard of the People's Republic of China
Test method for trace chloride, nitrate, phosphate, suifate in electronic grade water by ion-chromatography
GB/T 11446.7—1997
Replaces GB 11416.7—89
This standard specifies the ion chromatography test method for trace chloride ions (CI-), nitrate ions (VO,-), phosphate ions (PO\) and sulfate ions (SO,\-) in electronic grade water. This standard is applicable to the detection of trace fluoride ions, nitrate ions, phosphate ions and sulfur ions in electronic grade water. 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard before being cited in this standard. When this standard was published, the versions shown were all valid. All standards will be revised. All parties using this standard should explore the possibility of using the latest version of the following standards. GB/T11446.1-1997 Electronic Grade Water
GB/T11446.3-1997 General Rules for Testing Methods of Electronic Grade Water 3 Definitions
3.1 Ion Chromatography Ion chromatography is a special liquid chromatography technique that uses the principle of high-performance ion exchange chromatography and conductivity identification method to suppress background conductivity to separate and determine ions. It can be used to measure trace anions in high-purity water. 4 Method Principle
Ion chromatograph consists of eluent reservoir, pump, injection valve, separation house, suppression column, conductivity detector and data processing. When analyzing anions in water, the separation house is filled with cation exchange resin with low exchange capacity, while the suppression column is filled with strong acid cation exchange resin (H' type) with high exchange capacity, and the eluent is a dilute alkaline solution. When the eluent and the sample flow through the separation column, the cations in the sample and the eluent pass smoothly. The anions A (ACI-, NO:, PO”, SO\- ions) in the sample compete with the anions in the eluent to replace the position of the hydroxyl (OH-) on the resin (RN+(H) in the separation column. The reaction is: RN+-OH-+A---→RN+-A-+OH
The different affinities of the anions with the resin filled in the column separate the anions and They flow out from the bottom of the separation column in sequence. When the separated splashed ions and the eluent enter the suppression column together, the following reaction occurs on the suppression column R--SO-H-+Na+IICO or (Na'OH-)-→R—SO,-Na++H,CO(or H,O)R-SO,-H++Na+A-—+R-SO,-Na'+HANational Technical Supervision High 1997-09-01 approved 1998-09-01 implementation
..comGB/T 11446.7-1997
The cations in the test solution and the eluent are adsorbed by the cation exchange resin in the column, while the sodium hydroxide or bicarbonate with high conductivity in the eluent is converted into carbonic acid or water with very low ionization degree in the suppression column. The separated anions pass through the suppression column smoothly and flow out in the form of acid with high conductivity. The chromatogram of ions such as sodium ions, nitrate ions, phosphate ions, and sulfate ions can be recorded by the conductivity detector within a few minutes, thereby quantitatively measuring the content of each anion in the sample. 5 Reagentsbzxz.net
5.1 Blank water: It should comply with the GB/T11446.1 Electronic grade water level 1 standard. 5.2 Standard preparation
5.2.1 Sodium fluoride (reference substance) standard stock solution: Accurately weigh 0.1650g of sodium chloride reference substance, dilute it to 11. volumetric flask with blank water, and prepare 0.1 tmg/mL standard stock solution containing fluoride ions 5.2.2 Sodium sulfate standard stock solution: Accurately weigh 0.1480g of high-grade pure anhydrous sodium sulfate (bake to constant temperature at 105℃~110℃C), dilute to volume with blank water in a 1 L volumetric flask, this solution contains 0.1 mg/mL sulfate ions 5.2.3 Potassium nitrate standard stock solution: Accurately weigh 0.1630g of high-grade potassium nitrate (bake to constant temperature at 120℃~130C) and dilute to 1 1 with blank water. This solution contains 0.1 mg nitrate ions /mL. 5.2.4 Sodium phosphate standard stock solution, accurately weigh 0.1727g of high-grade pure sodium phosphate and dissolve it in water, dilute it to 1L with blank water. This solution contains 0.1mg/mnL of phosphate ions
5.3 Eluent, weigh 6.30g of sodium bicarbonate (high-grade pure) and dissolve it in blank water, then add 21.20g of sodium carbonate (high-grade pure), mix well and dilute it to 1L with blank water to prepare a elution stock solution containing 0.075mol/L sodium bicarbonate and 0.200mol/L sodium carbonate. Dilute it 100 times with blank water when using.
5.4 Regeneration solution: Dissolve 280ml of concentrated sulfuric acid (MOS grade pure) in an appropriate amount of blank water, make it 4L, and prepare a 1.25mol/l sulfuric acid stock solution. Dilute it 100 times with blank water when using. 6 Instruments
6.1 High-performance ion chromatograph and accessories such as high-performance anion separation column, trace analysis column, suppression column, guard column, conductivity detector and recording system.
6.2 Adjustable polypropylene sample injector.
6.3 Glassware IIIL with complete specifications.
7 Test steps
7.1 Preparation of standard series solutions: Accurately measure an appropriate amount of standard stock solution, dilute it step by step in sequence, and prepare a corresponding series of mixed standard solutions containing chloride ions, nitrate ions, phosphate ions, and sulfate ions. 7.2 Selection of instrument working conditions: Connect the power supply and gas source according to the requirements of the instrument manual, and debug the instrument to put it in the best working state. Preheat the instrument for a sufficient time to obtain a stable baseline. 7.3 Selection of measurement conditions: Select a suitable anion separation column, the concentration and flow rate of the eluent and regeneration solution, the injection volume, and the appropriate sensitivity of the electronic detector.
7.4 Drawing of working curve: Under the best working conditions of the instrument, measure the standard series of solutions, record the peak value of the conductivity of each chromatogram, and draw the working curve with concentration as the horizontal axis and conductivity as the vertical axis. 7.5 Analysis of water samples: Under the same conditions as drawing the working curve, analyze and measure the water samples, and obtain the contents of chloride ion, nitrate ion, phosphate ion and sulfate ion in the water samples from the measured conductivity values ​​on the standard working curve. 8 Precision
The precision of this method is shown in Table 1.
Anions
Chloride ion
Nitrate
Phosphate
Sulfate
Test report
GB/T 11446.7—1997
Table 1 Relative standard deviation and recovery rate of anions Concentration
Refers to the relative standard deviation of detection
The format of the test report is in accordance with the requirements of Chapter 6 of GB/I11446.3—1997. 10 Precautions
10.1 Environmental conditions must be strictly controlled, and the instrument should be placed in an ultra-clean environment with adjustable temperature. When analyzing the sample, blank water should be injected immediately after each analysis of the sample. 10.2
Recovery
10.3 The chromatogram of anions changes with the instrument parameters and working conditions. Each measurement should be calibrated with standard solutions to determine the position of each anion chromatogram.
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