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XB/T 601.5-2008: Chemical analysis methods of lanthanum boride - Determination of acid dissolving silicon content - Silicon molybdenum blue spectral luminosity method
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Chemical analysis methods of lanthanum boride - Determination of acid dissolving silicon content - Silicon molybdenum blue spectral luminosity method
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XB/T 601.5-2008
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Basic data | Standard ID | XB/T 601.5-2008 (XB/T601.5-2008) | | Description (Translated English) | Chemical analysis methods of lanthanum boride - Determination of acid dissolving silicon content - Silicon molybdenum blue spectral luminosity method | | Sector / Industry | Rare Earth Metal Industry Standard (Recommended) | | Classification of Chinese Standard | H65 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 7,744 | | Date of Issue | 2008-02-01 | | Date of Implementation | 2008-07-01 | | Older Standard (superseded by this standard) | XB/T 601.6-1993 | | Regulation (derived from) | NDRC Announcement No. 11 of 2008; Ministry of Industry and Information Technology Announcement No. 23 of 2017 | | Issuing agency(ies) | National Development and Reform Commission of the People's Republic of China | | Summary | This standard specifies the method for determining the acid-soluble silicon content in lanthanum hexaboride. This standard applies to the determination of acid-soluble silicon content in lanthanum hexaboride. Measuring range: 0.002 0%��0.10%. | XB/T 601.5-2008: Chemical analysis methods of lanthanum boride - Determination of acid dissolving silicon content - Silicon molybdenum blue spectral luminosity method
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Chemical analysis methods of lanthanum boride-Determination of acid dissolving silicon content-Silicon molybdenum blue spectral luminosity method
Book People's Republic of China Rare Earth Industry Standard
XB/T 601.5-2008
Replace XB/T 601.6-1993
Chemical analysis method of lanthanum hexaboride
Determination of acid-soluble silicon
Silicon molybdenum blue spectrophotometry
2008-02-01 released
Implementation of.2008-07-01
Issued by the National Development and Reform Commission of the People's Republic of China
Foreword
This standard is divided into the following 5 parts.
XB/T 601.1-2008 Methods for chemical analysis of lanthanum hexaboride. Determination of boron content. Acid-base titration
XB/T 601.2-2008 Methods for chemical analysis of lanthanum hexaboride Determination of iron, calcium, magnesium, chromium, manganese, and copper content inductively coupled plasma
Emission spectroscopy
XB/T 601.3-2008 Methods for chemical analysis of lanthanum hexaboride-Determination of tungsten content-Inductively coupled plasma emission spectrometry
XB/T 601.4-2008 Methods for chemical analysis of lanthanum hexaboride. Determination of carbon content. High frequency induction combustion infrared absorption method
XB/T 601.5-2008 Methods for chemical analysis of lanthanum hexaboride-Determination of acid-soluble silicon content-Silicon molybdenum blue spectrophotometric method
This part is part 5.This part is a reference to XB/T 601.6-1993 "Methods for chemical analysis of lanthanum hexaboride, silicon molybdenum blue spectrophotometric method
Revision of "Determination of Acid Soluble Silicon Amount". Compared with XB/T 601.6-1993, the main changes are as follows.
---Edited the standard text;
--- Added precision (repeatability) clause.
This part was proposed and managed by the National Rare Earth Standardization Technical Committee.
This part was drafted by Hunan Rare Earth Metal Materials Research Institute.
This part was drafted by Baotou Rare Earth Research Institute and Beijing Nonferrous Metal Research Institute.
The main drafters of this section. Liu Rongli, Weng Guoqing, Cui Yixin.
Participating drafters of this section. Gao Lizhen, Zhang Lifeng, Chen Yunhong, Yang Ping.
The previous standard editions replaced by this standard are as follows.
---XB/T 601.6-1993.
XB/T 601.5-2008
Chemical analysis method of lanthanum hexaboride
Determination of acid-soluble silicon content-Silicon molybdenum blue spectrophotometric method
1 scope
This section specifies the method for determining the acid-soluble silicon content in lanthanum hexaboride.
This section applies to the determination of acid-soluble silicon content in lanthanum hexaboride. Measurement range. 0.0020%～0.10%.
2 Principles of the method
The sample is decomposed by dilute nitric acid. In a 0.1mol/L sulfuric acid medium, orthosilicic acid and ammonium molybdate generate yellow silicomolybdenum heteropoly acid, which improves sulfuric acid.
Concentration to 1.2mol/L to eliminate the interference of phosphorus and arsenic, use ascorbic acid to reduce silicomolybdenum yellow to silicomolybdenum blue, with a spectrophotometer wavelength of 660nm
Measure the absorbance at the place. Use the working curve to find the silicon content.
3 Reagents
3.1 Nitric acid (1+1), pure superior grade.
3.2 Hydrochloric acid (1+1), excellent grade pure.
3.3 Sulfuric acid (1+1), pure superior grade.
3.4 Sulfuric acid (1 + 17), pure superior grade, stored in plastic bottles.
3.5 Ammonia (1+1), ultra-pure, stored in a plastic bottle.
3.6 Ammonium molybdate [(NH4)6Mo7O24·4H2O] solution (50g/L), stored in a plastic bottle.
3.7 Ascorbic acid solution (30g/L), prepared when used.
3.8 Silicon standard stock solution. Weigh 0.2139g of spectrally pure dioxygen that has been pre-fired at 950°C for 2h and cooled to room temperature in a desiccator
Add 5g of anhydrous sodium carbonate (superior grade) to the silicide in a platinum crucible, and melt it at 1000°C until it becomes transparent. After cooling, it is leached with hot water and heated to dissolve it.
Cool to room temperature, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix. Store in a plastic bottle, this solution is 1mL
Contains 100μg silicon.
3.9 Silicon standard solution. Pipette 50.0mL silicon standard stock solution (3.8) into a 1000mL volumetric flask, dilute to the mark with water, and mix
Evenly, store in a plastic bottle. This solution 1mL contains 5μg silicon.
3.10 p-nitrophenol solution (1g/L).
4 Instruments and utensils
4.1 Spectrophotometer.
4.2 Teflon beaker with a capacity of 100 mL.
5 Sample
The sample is mixed and dried at 105°C to 110°C for 1 h, then cooled to room temperature in a desiccator and weighed immediately.
6 Analysis steps
6.1 Sample
Weigh the sample (5) according to Table 1, with an accuracy of 0.0001g.
XB/T 601.5-2008
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