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    7 parts of chemical analysis methods for tungsten concentrate are solicited for comments

    • Last Update: 2023-01-05
    • Source: Internet
    • Author: User
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    【Chemical Machinery and Equipment Network Policies and Regulations】Recently, the 1st, 3rd, 4th, 6th, 8th, 10th, and 15th parts of the chemical analysis method of tungsten concentrate were compiled and publicly solicited for comments, and the time ended on November 18
    .
    The main drafters are Ganzhou Nonferrous Metallurgy Research Institute, National Tungsten and Rare Earth Product Quality Supervision and Inspection Center, etc
    .

     
    Tungsten concentrate is an important strategic resource, tungsten and tungsten alloy produced as an important industrial raw material, due to the characteristics of high melting point, high specific gravity and high hardness, widely used in mechanical processing, metallurgy, mining, electronic communications, construction industry, weapons industry, aerospace and other fields
    .

     
    GB/T 6150 aims to establish a complete, feasible and suitable method standard
    for chemical composition analysis of tungsten concentrate products production and trade through experimental research.
    Due to the length of the document, the demand for use, the scope of application and the technical independence between the analytical methods, GB/T 6150 is proposed to consist of
    20 parts.

     
    The series of standardization documents for chemical analysis methods of tungsten concentrate are mainly drafted
    according to the technical indicators in the tungsten concentrate product standard.
    Since 1985, two versions of GB/T 6150
    have been released.
    GB/T 6150.
    1-2008 has been issued and implemented for more than ten years, during which its applicable product standards have been revised once in 2015 (YS/T 231-2015), the content of tungsten trioxide in different grades of tungsten concentrate has been revised, and the measurement range of GB/T6150.
    1-2008 can no longer fully cover the requirements
    of product standards.
    In view of this, it is indeed necessary to revise GB/T 6150.
    1-2008 to ensure that the standard adapts to industry changes and market needs
    .

     
    Methods for chemical analysis of tungsten concentrate Part 1: Determination of tungsten trioxide content Ammonium tungstate ignition gravimetric method
     
    This document specifies the method
    for determining the content of tungsten trioxide in tungsten concentrate.
    This document is suitable for the determination of tungsten trioxide content in tungsten concentrate with molybdenum content less than 0.
    3% and phosphorus content less than 0.
    3%, and the determination range (mass fraction): >20%.


     
    This document further improves the applicability of the standard and is of great significance
    in improving the quality of tungsten concentrate products, promoting its production, trade and expanding application demand.

     
    In the presence of a small amount of ammonium fluoride, the sample is dissolved with hydrochloric acid, nitric acid and perchloric acid, concentrated to white smoke to drive out fluoride ions and nitrate, tungsten into tungsten acid precipitation, filtered, so that it is separated from most of the coexisting elements, tungsten acid is dissolved with ammonia, the filtrate is evaporated and burned, and the quality of tungsten trioxide is called by hydrofluoric acid silica again after siliconization
    .
    The mass of tungsten trioxide in the residue was determined by spectrophotometry and the results
    were corrected.

     
    Methods for chemical analysis of tungsten concentrate Part 3: Determination of phosphorus content Phosphomolybdenum yellow spectrophotometry and inductively coupled plasma atomic emission spectrometry
     
    This document expands the scope of methods and adds inductively coupled plasma atomic emission spectrometry to better meet the needs
    of the tungsten industry for product inspection.

     
    This document specifies the method
    for determining phosphorus content in tungsten concentrate.
    This document applies to the determination of phosphorus content in tungsten concentrate and contains two methods
    .
    Method 1: Phosphomolybdenum yellow spectrophotometry, determination range (mass fraction): 0.
    0050%~1.
    00%.

    Method 2: Inductively coupled plasma atomic emission spectrometry, measurement range (mass fraction): 1.
    00 %~~10.
    00 %.


     
    After the sample material is melted and leached by alkali, sulfuric acid plating is used as the carrier to separate phosphorus and hydroxide plating from other elements
    .
    In a nitric acid solution of a certain acidity, ammonium vanadate-ammonium molybdate was used as the color developer, and the absorbance was measured at 420 nm by spectrophotometer
    .
    After separation, the residual tungsten, arsenic, silicon, etc.
    do not affect the determination
    .

     
    Methods for chemical analysis of tungsten concentrate Part 4: Determination of sulfur content High-frequency induction infrared absorption method and combustion-iodine measurement method
     
    This document specifies the method
    for determining the sulfur content in tungsten concentrate.
    This document is suitable for the determination of sulfur content in tungsten concentrate, including two methods, method 1: high-frequency induction infrared absorption method, measurement range (mass fraction): 0.
    10%~4.
    00%; Method 2: combustion-iodine method, measurement range (mass fraction): 1.
    00%~~10.
    00%.

    The overlapping part of the measurement range is arbitrated by Method 2
    .

     
    In the presence of flux, oxygen is introduced into the high-frequency induction furnace to make the sulfur in the sample be converted into sulfur dioxide by combustion in a high-temperature melting environment, and the signal is processed by the computer to measure the sulfur content
    in the sample after being introduced into the infrared detector.

     
    Methods for chemical analysis of tungsten concentrate Part 6: Determination of wet water content Gravimetric method
     
    This document specifies the method
    for determining the wet water content in tungsten concentrate.
    This document is suitable for the determination of wet water content in tungsten concentrate, and the determination range (mass fraction): 0.
    2%~10.
    00%.


     
    The sample material is heated at 105 °C~110 °C for a certain period of time, and the water can be completely evaporated
    .
    Weigh the mass of the sample before and after heating, and calculate the amount of
    moisture.

     
    Methods for chemical analysis of tungsten concentrate Part 8: Determination of molybdenum content Thiocyanate spectrophotometry
     
    This document specifies the method
    for determining the molybdenum content in tungsten concentrate.
    This document is suitable for the determination of molybdenum content in tungsten concentrate, and the determination range (mass fraction): 0.
    0050 % ~ 2.
    50
    %.

     
    The sample material is melted with sodium peroxide in the ground snail and leached with water to separate molybdenum from most of the iron, manganese, copper, bismuth, calcium, etc
    .
    Tungsten was masked with citric acid, copper salt was used as catalyst, molybdenum was reduced to pentavalent with thiourea in dilute sulfuric acid solution, and then an orange-red complex was formed with thiocyanate, and its absorbance
    was measured at a spectrophotometer wavelength of 460 nm.

     
    Methods for chemical analysis of tungsten concentrate Part 10: Determination of lead content Hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometry
     
    This document specifies the method
    for determining the lead content in tungsten concentrate.
    This document is applicable to the determination of lead content in tungsten concentrate and contains two methods: method 1 hydride generation atomic fluorescence spectrometry and method 2 flame atomic absorption spectrometry
    .
    Method 1 measurement range (mass fraction): 0.
    001% ~ O.
    30%, Method 2 measurement range (mass fraction): 0.
    10% ~ 0.
    50
    %.
    When there is overlap in the measurement range, method 2 is used as the arbitration method
    .

     
    The sample is decomposed with hydrochloric acid on the boiling water bath, nitric acid is added, perchloric acid is heated and dissolved to thick white smoke, in the acidic solution with a large amount of tungsten matrix removed, oxalic acid is used as an interfering element masking agent, potassium ferricyanide is used as an oxidant, in the hydride generator, lead is reduced to hydride by potassium borohydride, and its fluorescence intensity
    is measured on an atomic fluorescence spectrometer.

     
    Methods for chemical analysis of tungsten concentrate Part 15: Determination of bismuth content Hydride generation atomic fluorescence spectrometry and flame atomic absorption spectrometry
     
    By improving and changing the analytical methods in the existing standards, replacing or expanding the detection range with new testing instruments, it is the main way
    to maintain the adaptability of analytical method standards.
    This revision replaces atomic absorption spectrometry with hydride atomic fluorescence spectroscopy, which makes the lower limit of method detection lower, which can increase the applicability of this document, thereby improving the standard adoption rate, better serving and promoting production, trade and application needs
    .

     
    This document specifies the method
    for determining the bismuth content in tungsten concentrate.
    This document is applicable to the determination of bismuth content in tungsten concentrate and contains two methods: method 1 hydride generation atomic fluorescence spectrometry and method 2 flame atomic absorption spectrometry
    .
    Method 1 measurement range (mass fraction): 0.
    001%~0.
    30%, Method 2 measurement range (mass fraction): 0.
    050%~0.
    50
    %.
    When there is overlap in the measurement range, method 2 is used as the arbitration method
    .

     
    The sample was heated with hydrochloric acid, nitric acid, perchloric acid to dissolve until thick white smoke, in the acidic solution with a large amount of tungsten matrix removed, thiourea-ascorbic acid was used as a masking agent, in the hydride generator, bismuth was reduced to hydride by potassium borohydride, and its fluorescence intensity
    was determined on an atomic fluorescence spectrometer.

     
    Original: 7 parts of chemical analysis methods for tungsten concentrate solicited comments

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