GB/T 11446.6-1997 Spectrophotometric test method for electronic grade silicon dioxide in water
Some standard content:
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 Fan Yuan
National Standard of the People's Republic of China
Spectrophotometric Test Method for Silicon Dioxide in Electronic Grade Water GB/T11446.6--1997 Test method for Sio, in electronic grade water by spectrophotometer This standard specifies the spectrophotometric determination method for silicon dioxide in electronic grade water. This standard is applicable to the determination of silicon dioxide in electronic grade water, and the lower limit of analysis is 1 R/L. 2 Reference Standard
Replaces GR 11446. 6—99
The clauses contained in the following standards constitute the clauses of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards are subject to revision, and parties using this standard should explore the possibility of using the latest versions 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 Soluble silican
Soluble silicate existing in water in a single molecule state. 3.2 Total silicon
The total amount of soluble silicon in water and silicon existing in the form of colloidal silica. The difference between total silicon and soluble silicon is colloidal silicon. 4 Principle
Soluble silicon in water reacts with ammonium sulfate in an acidic medium (pH=1~2) to generate yellow silico-copper heteropoly acid (NH4H2O3)[Si(MO4O4)]H2O3. The yellow silico-molybdenum heteropoly acid is reduced to molybdenum blue by a reducing agent 1-amino-2-phenol-4-sulfonic acid, and then the absorbance of molybdenum blue is measured by a spectrophotometer. The amount of soluble silicon in water is calculated. Non-silicon in water can be dissolved with hydrofluoric acid to determine total silicon. 5 Reagents
5.1 Blank water: Should comply with GB/T11446.1 Electronic grade water EWI grade water, 5.2 Silicon standard solution:
5.2.1 1Pg/mL silicon dioxide standard stock solution: Accurately weigh 1.0000g of silicon dioxide (superior grade pure) burned at 800C and 3.0g of anhydrous sodium carbonate (superior grade pure) in a platinum crucible, mix well, heat at 1000C and completely melt, after cooling, dissolve the melt in water, dilute to 1L, store in a plastic bottle, the solution should be transparent, if turbid, it should be re-prepared. 5.2.2 1Pg/mL silicon dioxide standard solution: Prepare the silicon dioxide standard stock solution in 5.2.1 by diluting it step by step (prepared for use). www.bzxz.net
5.3 Ammonium molybdate solution: 10% (W/V). Analytically pure ammonium molybdate is purified by two recrystallizations. 5.4 Benzoic acid solution or tartaric acid or citric acid solution: 10% (W/V), approved by the State Administration of Technology Supervision on September 1997-0901
Implementation on September 1998-09-01
GB/T 11446.6---1997
5.5 1-amino-2-phenol-4-sulfonic acid reducing agent solution: Weigh 1.5 1-amino-2-phenol-4-sulfonic acid and 7g anhydrous sodium sulfite, dissolve in 200mL water, add this solution to 600mL (15% sodium bicarbonate solution, dilute with blank water to 1L (if the solution is turbid, it should be filtered) and store in a polyethylene bottle.
5.6 Hydrochloric acid: (1+1) (V/V). After evaporation Or absorb purified hydrochloric acid. 5.7 Chlorofluoric acid: 1% (V/V). Hydrofluoric acid purified by platinum distiller. 5.8 Boric acid solution: saturated solution prepared with boric acid purified by recrystallization. 6 Instruments
6.1 Spectrophotometer: working wavelength 200nm~1000nm, wavelength accuracy ±1.5nm; transmittance range (0~110)%, transmittance repeatability ±0.5%, absorbance measurement range 0.04~2, cuvette 1cm, 2cm, 5cm10 cm, 6.2 Analytical balance.
6.3 Constant temperature water bath crucible.
6.4 Platinum crucible.
6.5 Polyethylene bottle (cup): 100mL, 1000mL. 6.6 Glassware of complete specifications,
7 Sampling
7.1 The water container used for silicon analysis must be polyethylene or other plastic containers. Follow Chapter 4 of GB/T11446.1-1997. 8 Test steps
8.11. Plotting the curve
Sequentially take 0.0, 0.1, 0.2, 0.5, 0.8, 1.0, 2.0, 5.0, 10.0 mL of standard solution containing 1 μg/L of silicon dioxide and dissolve it in 50 mL Dilute to the mark with blank water in a volumetric flask, shake the hook, pour the above solutions into a polyethylene beaker, add 1mL hydrochloric acid (1+1) and 3mL 10% ammonium hydroxide solution, shake the spoon, let it stand for 10min, add 2mL 10% oxalic acid solution, pry the spoon, let it stand for 2㎡m, add 2mL 1-amino-2-phenol-4-sulfonic acid reducing agent solution, shake well. Let it stand for another 10ml. Take the blank solution as the reference, use 5 cm or 10 cm solution, and measure at a wavelength of 815nm with a spectrophotometer. Draw a curve with absorbance as the coordinate and silicon monoxide as the horizontal axis. 8.2 Reagent vacuum deduction
8.2.1 Inject 50mL and 43mL blank water into two polyethylene beakers respectively. Add single reagent and double reagent according to step 8.1, take blank water as the reference, and the difference in absorbance of the two solutions is the reagent vacuum absorbance, single reagent: 50 mL of blank water plus 1.0 mL of hydrochloric acid (1+1) plus 3.0 mL of 10% ammonium platinate plus 2.0 mL of 10% oxalic acid plus 2.0 mL of reducing agent. The absorbance of the bath is A1. Double reagent: 43.0 mL of blank water plus 1.0 mL of hydrochloric acid (1+1) 6.0 mL of 10% ammonium molybdate plus 4.0 ml of 10% oxalic acid scale, reducing agent. The absorbance of the bath is A2c8. 2. 2 When all silicon is used; in a polyethylene cup, add 2. 5 mL of saturated boric acid and 1. 0 mL hydrofluoric acid (1 + 1), add 39.5 mL of water, and then add reagents according to the steps in 8.1. Take blank water as the reference, and measure the absorbance of the liquid as A. The absorbance produced by hydrofluoric acid plus boric acid is A:-A1.
8.2.3 When determining soluble silicon, the reagent blank is Az-4, and when determining total silicon, the reagent blank is A-A+A-A:=A+A-2.At.
8.3 Determination of water samples
8.3.1 Determination of soluble silicon
50m!. The water sample is placed in a polyethylene bottle and operated according to the steps of drawing a working curve. Use blank water as a reference for photometric determination. From the working curve, find the silicon dioxide content corresponding to the difference between the absorbance of the reagent and the absorbance of the reagent blank, which is the content of soluble silicon in the water sample.
8.3.2 Determination of total silicon in water
GB/T 11446.6—1997
Add 1.0 mL hydrofluoric acid to a 50 mL water sample in a polyethylene bottle with a cap, cover the bottle and shake well, heat 15 mL in boiling water, cool to room temperature, add 2.5 mL saturated 1% acid solution and stir well. See the determination of soluble silicon below. Find the silicon dioxide content corresponding to the difference between the absorbance of the sample and the absorbance of the reagent blank on the T curve, which is the total content of silicon dioxide in the water sample. 9 Elimination of interference
9.1 Phosphoric acid and arsenate generate corresponding blue heteropoly acids under the determination conditions. Hydroxyl acids such as oxalic acid and diethyl ether can be used to eliminate the interference of phosphorus and phosphorus.
9.2 When determining the total silicon in water, use hydrofluoric acid to convert insoluble silicon into soluble silicon. Hydrofluoric acid has negative interference, which can be eliminated by adding saturated boric acid.
10 Method detection limit and relative deviation
This method analyzes the content of silicon dioxide in electrolyte water. The method detection limit is 1 /L. For the analysis of 10 μg/L (silicon monoxide) water, the relative deviation is 8%.
11 Test report
The format of the test report is in accordance with the requirements of Chapter 6 of GB/T11446.3-1997. ..com
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