CN106940293A - A kind of method of quick measure silica - Google Patents

A kind of method of quick measure silica Download PDF

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Publication number
CN106940293A
CN106940293A CN201610004996.2A CN201610004996A CN106940293A CN 106940293 A CN106940293 A CN 106940293A CN 201610004996 A CN201610004996 A CN 201610004996A CN 106940293 A CN106940293 A CN 106940293A
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China
Prior art keywords
water
sample
solution
plus
hydrochloric acid
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CN201610004996.2A
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Inventor
赵竞泽
王晓旭
田秀梅
王炳琨
张勋
桑妍
张丽丽
雷学斌
张辉
陈英丽
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Angang Steel Co Ltd
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Angang Steel Co Ltd
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Priority to CN201610004996.2A priority Critical patent/CN106940293A/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

The present invention relates to a kind of method of quick measure silica, this method includes sample preparation, sample analysis process, by the sample sodium peroxide for the mesh of ＜ 100 of chemical analysis, fused mass is rinsed with water and dissolved in the beaker for fill hydrochloric acid, dividing after constant volume takes test solution to be placed in volumetric flask, plus watery hydrochloric acid, ammonium molybdate solution, mix, place 5-35min or heating water bath 5-40S；Add water, careless sulphur nitration mixture plus l ferrous ammonium sulfate solution, constant volume is diluted with water, on spectrophotometer, at 630-810nm wavelength, with cuvette, using water or blank solution as reference measurement absorbance.Needed for the present invention is based on iron ammonium sulfate reduction-Silicon Molybdenum Blue Spectrophotometry general principle, and only not wider applicability is applicable to the inspection of various materials, and its measurement range can cover production.Its analysis process is easy, governing factor is few, process control requirements are low, be easy to grasp, with high accuracy.

Description

A kind of method of quick measure silica
Technical field
The present invention relates to detection method, more particularly to a kind of method of quick measure silica.
Background technology
Raw mineral materials, enriched ore, flux class material used in ironmaking production etc. are various in style, and existing country's mark The measure iron ammonium sulfate reduction-Silicon Molybdenum Blue Spectrophotometry and GB/ of quasi- GB/T 6730.9-2006 iron ore silicone contents T3286.2-2012 lime stones and dolomite chemical analysis method part 2：The measure silicon molybdenum blue light splitting light of dioxide-containing silica Degree method and perchloric acid determination, although this two standards are applicable to various materials but its measurement range is narrower in ironmaking (being less than 5%), and universal material dioxide-containing silica is less than 20.00% in producing, national standard can not cover produce reality institute Need, and use national standard method analytical test personnel labor intensity is big, analytical cycle is long, and complex operation step, process control It is required that high, chemical examination high cost, environmental pollution are big.Need to develop quick, accurate, saving manpower thing in one line of guidance production at present Power, the method for inspection easy to operate meet detection requirements of one's work.
The content of the invention
The technical problems to be solved by the invention are to provide dioxy in a kind of accurate, quick, easy to operate measure material The method of SiClx, it is based on iron ammonium sulfate reduction-Silicon Molybdenum Blue Spectrophotometry general principle, is not applicable widely only Property, it is applicable to the inspection of various materials, and needed for its measurement range can cover production.
To achieve the above object, the present invention is realized using following technical scheme：
A kind of method of quick measure silica, is completed using following steps：
1) sample after drying is taken to be crushed, the sample particle after crushing is the mesh of ＜ 100；
2) sample is weighed, sample is placed in crucible, plus sodium peroxide stirs, and is subsequently placed in 650-1000 DEG C At a temperature of melt, melt into kermesinus working fluid, take out slightly cold；
3) fused mass is rinsed in filling in the beaker of hydrochloric acid with water, stirring make solution clarify after constant volume, mix, it is static after A point liquid is carried out with pipette；
4) dividing takes test solution to be placed in volumetric flask, plus watery hydrochloric acid, plus ammonium molybdate solution, mixes, and places 5-35min or water-bath adds Hot 5-40S；
5) add water, careless sulphur nitration mixture plus l ferrous ammonium sulfate solution, constant volume is diluted with water, on spectrophotometer, in 630- At 810nm wavelength, with cuvette, using water or blank solution as reference measurement absorbance；
6) after the absorbance for deducting blank test, standard is drawn with standard liquid or the absorbance and content value of standard sample bent Line, checks in dioxide-containing silica from working curve.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention is based on iron ammonium sulfate reduction-Silicon Molybdenum Blue Spectrophotometry general principle, is not applicable widely only Property, it is applicable to the inspection of various materials, and needed for its measurement range can cover production.It analyzes that process is easy, control because Element is less, process control requirements are low, be easy to grasp, with high accuracy, and round of visits can be examined by 1 people and foreshorten to 1 in more than 2 hours People examines complete for 20 minutes, can effective Instructing manufacture.Inspection cost is saved compared with GB chemical method, environment dirt is reduced Dye.
Embodiment
With reference to embodiment, the present invention is further described：
The present invention will be described in detail for following examples.These embodiments are only that preferred embodiment of the invention is entered Row description, is not limited the scope of the present invention.
A kind of method of quick measure silica, is completed using following steps：
1) a small amount of sample clean material alms bowl after drying is used, iron ore sample, which is put into, shakes grinding machine, compresses compacting, and iron ore shakes mill Sample granularity is crossed on 0.1mm standard screens (150 mesh) sieve and measured after 180S, crushing<0.5g, the iron ore particle after crushing is 150- 200 mesh.
2) reagent is configured：
Hydrochloric acid (1+50)：(ρ about 1.19g/ml) 10ml is taken to be dissolved in 500ml water.
Molybdic acid amine aqueous solution (5%)：Weigh 50g amine molybdates to be dissolved in a small amount of water, 1L is diluted to after dissolving.
Careless sulphur nitration mixture, (1+3).
Iron ammonium sulfate (4%)：Weigh 40g iron ammonium sulfates and add a small amount of water dissolves, add (1+2) sulfuric acid 30ml or dense Sulfuric acid 10ml, is diluted with water to 1000ml.
3) 0.1 ± 0.0001g samples are weighed, sample is placed in iron crucible, plus 0.6g sodium peroxides, stirred with glass bar Uniformly, it is subsequently placed in 850-900 DEG C of high temperature furnace, melts into kermesinus working fluid, takes out slightly cold.
4) fused mass is rinsed in filling in 250ml the or 500ml beakers of 10ml hydrochloric acid with about 50ml water, stirring makes solution Constant volume 250ml after clarification, is mixed, static to carry out a point liquid with 5ml pipettes afterwards.
5) divide and take 5ml test solutions to be placed in 100ml volumetric flasks, plus 15ml (1+50) hydrochloric acid, plus 5ml concentration is 5% ammonium molybdate Solution, is mixed, and places 5-35min or heating water bath 5-40S.
6) 25ml water, 15ml (1+3) grass sulphur nitration mixture are added, plus 5ml concentration is 4% l ferrous ammonium sulfate solution, is diluted with water to 100ml shakes up, on visible spectrophotometer, at 680nm wavelength, uses 1cm cuvettes, using water or blank solution as reference measurement Absorbance.
7) working curve is drawn：With three and the above standard sample different with the content of kind, examination is made by operation 1-6 Liquid measures absorbance.Using absorbance, silica mass percent as transverse and longitudinal coordinate drawing curve.(or do recurrence side Journey)
8) silica Analysis result calculation, by the absorbance for measuring sample, by checking in corresponding dioxy on working curve SiClx mass percent or by regression equation calculation silica quality percentage.
The ferrous molybdenum blue absorption spectrophotometry experimental principle of above-mentioned experiment：
Sample is dissolved with acid, silicon is changed into soluble positive silicic acid：
FeSi+2HCl+4H2O=FeCl2+H4SiO4+3H2
Under appropriate acidity, silicic acid and ammonium molybdate effect generation molybdenum yellow：
H4SiO4+12H2MoO4=H8[Si(Mo2O7)6]+10H2O
Iron ammonium sulfate is added, molybdenum yellow is reduced to silicon molybdenum blue：
H8[Si(Mo2O7)6]+4FeSO4+2H2SO4=H8[SiMo2O5(Mo2O7)5]+2Fe2(SO4)3+2H2O
Standard sample detection data are compareed with normal data is shown in Table 1：
The standard sample of table 1 detection data are compareed with normal data
Title Numbering Measured value Standard value
Iron ore (Brazilian ore deposit 2) GSB03-2026-2006 1.80 1.79
Iron ore 6 GSB 03-2858-2012 4.90 4.92
Iron ore GBW07218a 3.48 3.48
Magnetite concentrate 02-43A 1.80 1.80
Iron ore GSBH30005-97 10.20 10.24
Iron ore 9# YSBC28739-95 7.40 7.40
Iron ore sample carries out 10 measurements, its SiO2Content detection value is shown in Table 2：
The iron ore sample SiO of table 22Content detection value
It is high by the visible detection method accuracy in detection of the invention of Tables 1 and 2, can effective Instructing manufacture.

Claims (1)

1. a kind of method of quick measure silica, it is characterised in that completed using following steps：
1) sample after drying is taken to be crushed, the sample particle after crushing is the mesh of ＜ 100；
2) sample is weighed, sample is placed in crucible, plus sodium peroxide stirs, and is subsequently placed in 650-1000 DEG C of temperature It is lower to melt, kermesinus working fluid is melted into, is taken out slightly cold；
3) fused mass is rinsed in filling in the beaker of hydrochloric acid with water, stirring makes constant volume after solution clarification, mixes, static rear use is moved Liquid pipe carries out a point liquid；
4) dividing takes test solution to be placed in volumetric flask, plus watery hydrochloric acid, plus ammonium molybdate solution, mixes, and places 5-35min or heating water bath 5- 40S；
5) add water, careless sulphur nitration mixture plus l ferrous ammonium sulfate solution, constant volume is diluted with water, on spectrophotometer, in 630-810nm At wavelength, with cuvette, using water or blank solution as reference measurement absorbance；
6) after the absorbance for deducting blank test, standard curve is drawn with standard liquid or the absorbance and content value of standard sample, from Dioxide-containing silica is checked on working curve.
CN201610004996.2A 2016-01-05 2016-01-05 A kind of method of quick measure silica Pending CN106940293A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114371165A (en) * 2022-01-04 2022-04-19 杭州英普环境技术股份有限公司 Method for detecting content of silicon dioxide in high-chroma and reductive wastewater

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CN101988892A (en) * 2009-07-30 2011-03-23 中国商用飞机有限责任公司 Method for measuring silicon dioxide content in solution
CN103728261A (en) * 2013-12-14 2014-04-16 武钢集团昆明钢铁股份有限公司 Fast and accurate detection method for silicon dioxide content in limestone, kalk and dolomite

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Publication number Priority date Publication date Assignee Title
CN101988892A (en) * 2009-07-30 2011-03-23 中国商用飞机有限责任公司 Method for measuring silicon dioxide content in solution
CN103728261A (en) * 2013-12-14 2014-04-16 武钢集团昆明钢铁股份有限公司 Fast and accurate detection method for silicon dioxide content in limestone, kalk and dolomite

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114371165A (en) * 2022-01-04 2022-04-19 杭州英普环境技术股份有限公司 Method for detecting content of silicon dioxide in high-chroma and reductive wastewater

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Application publication date: 20170711