CN106093010A - Potassium oxide and the method for sodium oxide content in a kind of quick analysis soda-lime-silica glass - Google Patents
Potassium oxide and the method for sodium oxide content in a kind of quick analysis soda-lime-silica glass Download PDFInfo
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- CN106093010A CN106093010A CN201610416877.8A CN201610416877A CN106093010A CN 106093010 A CN106093010 A CN 106093010A CN 201610416877 A CN201610416877 A CN 201610416877A CN 106093010 A CN106093010 A CN 106093010A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/72—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flame burners
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Abstract
The present invention discloses potassium oxide and the method for sodium oxide content in a kind of quick analysis soda-lime-silica glass, comprising the following steps: weigh the soda-lime-silica glass sample of 0.1g and the soda-lime-silica glass national standard material of 0.1g respectively, step obtains sample solution and standard solution to add nitration mixture in platinum ware, heating evaporation, dilution shake up etc.；Re-use flame photometer and utilize directly comparing method, according to formulaWith
Description
Technical field
The present invention relates to glass detection analysis field, potassium oxide and oxidation in specifically a kind of quickly analysis soda-lime-silica glass
The method of sodium content.
Background technology
Chemical analysis is to control glass production, improves glass inherent quality, develops glass new varieties etc. indispensable
Item work.From the selection check of raw materials quality, the proportioning of compound and uniformity inspection thereof, the inherent quality to finished product is checked all
It is unable to do without chemical analysis.The status that chemical analysis is operated in glass industry research and production is self-evident.For sodium calcium
Silica glass, potassium oxide is the key factor affecting its quality with the content of sodium oxide, at existing soda-lime-silica glass chemical analysis
In method GB/T 1347-2008, for potassium oxide and the analysis of sodium oxide, give three kinds of analysis methods: one, Atomic Absorption
Spectrographic method；Two, flame spectrometry；Three, plasma emlssion spectrometry；These three method is all to use primary standard substance preparation standard
Solution is analyzed, and program is loaded down with trivial details, and additionally analysis meeting is had a negative impact by matrix effect with absorbance curve bending.
Summary of the invention
It is an object of the invention to provide potassium oxide and the method for sodium oxide content in a kind of quick analysis soda-lime-silica glass,
The method simple and fast, essentially eliminates matrix effect, the curved adverse effect to analyzing, does not substantially have dilution error.
The technical solution adopted for the present invention to solve the technical problems is:
Potassium oxide and the method for sodium oxide content in a kind of quick analysis soda-lime-silica glass, comprise the following steps:
S1, weigh the soda-lime-silica glass sample of 0.1g, be placed in the platinum ware of 80ml；
S2, add water described sample moistening in platinum ware, add the perchloric acid of 1ml and the Fluohydric acid. of 10ml；
S3, platinum ware is placed on electric furnace heating, to be evaporated to pasty state, is cooled to room temperature；It is subsequently adding the Fluohydric acid. of 5ml, continues
Platinum ware is heated, until the white cigarette of perchloric acid stops heating after emitting to the greatest extent, and is cooled to room temperature；
S4, addition 25ml water and the 1+1 hydrochloric acid of 8ml；Platinum ware is placed on electric furnace heating again, until residue is the most molten in platinum ware
Stop heating after solution, solution clear, and be cooled to room temperature；
S5, move to, in 250ml volumetric flask, be diluted with water to graticule by solution in platinum ware, after shaking up, obtain sample solution；Described step
In rapid S2 with S3, perchloric acid is that the top grade of mass percent concentration 70% is pure, and Fluohydric acid. is the top grade of mass percent concentration 40%
Pure；
S6, weigh the soda-lime-silica glass national standard material of 0.1g, repeat step S2～S5 obtains standard solution；
S7, use flame photometer suck standard solution, and make absorption values show 1400；
S8, use flame photometer suck standard solution and sample solution respectively, read the potassium absorbance in standard solution and sodium
Potassium absorbance in absorbance and sample solution and sodium absorbance；
S9, according to formulaIt is calculated the potassium oxide percentage composition of sample solution；
According to formulaIt is calculated the sodium oxide percentage composition of sample solution；
A in above-mentioned formula1For the potassium absorbance of standard solution, A2For the potassium absorbance of sample solution, A3Sodium for standard solution is inhaled
Luminosity, A4For the sodium absorbance of sample solution, W1Quality, W is weighed for national standard material GBW 031172For soda-lime-silica glass
Sample weigh quality.
Beneficial effects of the present invention:
One, national standard material has the function of retention performance value in time, uses national standard reference material GBW
03117 produces the standard solution directly comparing test, relative to the series standard using potassium oxide, sodium oxide primary standard substance to produce
Solution, sample solution and standard specimen solution matrix are basically identical, substantially eliminate the matrix effect adverse effect to analysis result；
Two, this method has only to produce a standard solution, it is not necessary to prepare one group of standard solution；Molten at sample solution and standard
During liquid is produced, do not carry out secondary dilution, effectively prevent dilution error, save the time, simplify flow process, decrease reagent
Consumption and the loss of instrument；
Three, in soda-lime-silica glass, usual sodium oxide content is about 14%, and GBW 03117 soda-lime-silica glass national standard thing
In matter, sodium oxide content is 13.77%, and closely, difference is less than 0.3%；Standard substance and sample use and same weigh matter
Amount, in the standard solution produced and sample solution, Na ion concentration closely, in test, absorbance also can closely, because of
This, use direct comparison method, it also avoid absorbance curve and bends the analytical error brought.
Detailed description of the invention
The present invention provides potassium oxide and the method for sodium oxide content in a kind of quick analysis soda-lime-silica glass, including following step
Rapid:
S1, weigh the soda-lime-silica glass sample of 0.1g, be placed in the platinum ware of 80ml；
S2, in platinum ware, add appropriate water by described sample moistening, add the perchloric acid of 1ml and the Fluohydric acid. of 10ml；
S3, platinum ware is placed on electric furnace heating, to be evaporated to pasty state, is cooled to room temperature；It is subsequently adding the Fluohydric acid. of 5ml, continues
Platinum ware is heated, until the white cigarette of perchloric acid stops heating after emitting to the greatest extent, and is cooled to room temperature；
S4, addition 25ml water and the 1+1 hydrochloric acid of 8ml；Platinum ware is placed on electric furnace heating again, until residue is the most molten in platinum ware
Stop heating after solution, solution clear, and be cooled to room temperature；
S5, move to, in 250ml volumetric flask, be diluted with water to graticule by solution in platinum ware, after shaking up, obtain sample solution；Described step
In rapid S2 with S3, perchloric acid is that the top grade of mass percent concentration 70% is pure, and Fluohydric acid. is the top grade of mass percent concentration 40%
Pure；
S6, weigh the soda-lime-silica glass national standard material of 0.1g, repeat step S2～S5 obtains standard solution；
S7, unlatching flame photometer, and preheat, sucking standard solution, regulation flame photometer makes absorption values show
1400；Digital display 6410 type flame photometer selected by flame photometer；
S8, use flame photometer suck standard solution and sample solution respectively, read the potassium absorbance in standard solution and sodium
Potassium absorbance in absorbance and sample solution and sodium absorbance；
S9, according to formulaIt is calculated the potassium oxide percentage composition of sample solution；
According to formulaIt is calculated the sodium oxide percentage composition of sample solution；
A in above-mentioned formula1For the potassium absorbance of standard solution, A2For the potassium absorbance of sample solution, A3Sodium for standard solution is inhaled
Luminosity, A4For the sodium absorbance of sample solution, W1Quality, W is weighed for national standard material GBW 031172For soda-lime-silica glass
Sample weigh quality, 1.10 is potassium oxide percentage composition in national standard material GBW 03117, and 13.77 is national standard thing
Sodium oxide percentage composition in matter GBW 03117.
In this method, weighing error controls, within ± 0.0002g, to use ten thousand/electronic analytical balance；Sample weighting amount
It is 0.1000 ± 0.0002g, 1000 can be regarded as 0.1000；Test time, adjust standard solution absorbance 1400, be for
With the sodium oxide content 13.77% in standard substance is close, regard 1377 as 13.77%.So, sample weighting amount 1000, extinction
Degree 1400, these 3 values of sodium oxide content 1377, significant digits are all 4, and the first numeral is all 1, in testing employing directly than
Relatively method, can make whole analysis process error be maintained at a degree closely, is conducive to improving the accuracy of analysis result.
Hydromining used by this method, with meeting the deionized water that the band Ro film that two grades of water of GB require processes, so can make sky
White value is relatively low.
Using this method to analyze potassium oxide and sodium oxide in soda-lime-silica glass, the indoor absolute error of potassium oxide is not more than
0.03%, the indoor absolute error of sodium oxide is not more than 0.15%.From weighing sample to drawing analysis result, the time is less than 4
Hour.For same sample, use this method, atomic absorption spectrography (AAS) and X fluorescence spectrum method, through repeatedly analyzing, Comparative result
Such as following table:
In table, method 1 is this method；Method 2 is atomic absorption spectrography (AAS)；Method 3 is X fluorescence spectrum method；Table can be understood by upper table
Bright, use this method and the analysis result of sample is contrasted by the instrument analytical method using GB analysis method and other advanced persons,
It coincide good, comply fully with the countries concerned's standard-required.
The above, be only presently preferred embodiments of the present invention, and the present invention not makees any pro forma restriction；Appoint
What those of ordinary skill in the art, without departing under technical solution of the present invention ambit, may utilize the side of the disclosure above
Technical solution of the present invention is made many possible variations and modification by method and technology contents, or the equivalence being revised as equivalent variations is real
Execute example.Therefore, every content without departing from technical solution of the present invention, according to the technical spirit of the present invention, above example is done
Any simple modification, equivalent, equivalence change and modify, all still fall within technical solution of the present invention protection in the range of.
Claims (1)
1. potassium oxide and the method for sodium oxide content in a quick analysis soda-lime-silica glass, it is characterised in that include following step
Rapid:
S1, weigh the soda-lime-silica glass sample of 0.1g, be placed in the platinum ware of 80ml；
S2, add water described sample moistening in platinum ware, add the perchloric acid of 1ml and the Fluohydric acid. of 10ml；
S3, platinum ware is placed on electric furnace heating, to be evaporated to pasty state, is cooled to room temperature；It is subsequently adding the Fluohydric acid. of 5ml, continues
Platinum ware is heated, until the white cigarette of perchloric acid stops heating after emitting to the greatest extent, and is cooled to room temperature；
S4, addition 25ml water and the 1+1 hydrochloric acid of 8ml；Platinum ware is placed on electric furnace heating again, until residue is the most molten in platinum ware
Stop heating after solution, solution clear, and be cooled to room temperature；
S5, move to, in 250ml volumetric flask, be diluted with water to graticule by solution in platinum ware, after shaking up, obtain sample solution；Described step
In rapid S2 with S3, perchloric acid is that the top grade of mass percent concentration 70% is pure, and Fluohydric acid. is the top grade of mass percent concentration 40%
Pure；
S6, weigh the soda-lime-silica glass national standard material of 0.1g, repeat step S2～S5 obtains standard solution；
S7, use flame photometer suck standard solution, and make absorption values show 1400；
S8, use flame photometer suck standard solution and sample solution respectively, read the potassium absorbance in standard solution and sodium
Potassium absorbance in absorbance and sample solution and sodium absorbance；
S9, according to formulaIt is calculated the potassium oxide percentage composition of sample solution,
According to formulaThe sodium oxide percentage being calculated sample solution contains
Amount；A in above-mentioned formula1For the potassium absorbance of standard solution, A2For the potassium absorbance of sample solution, A3Sodium for standard solution is inhaled
Luminosity, A4For the sodium absorbance of sample solution, W1Quality, W is weighed for national standard material GBW 031172For soda-lime-silica glass
Sample weigh quality.
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| CN201610416877.8A CN106093010A (en) | 2016-06-12 | 2016-06-12 | Potassium oxide and the method for sodium oxide content in a kind of quick analysis soda-lime-silica glass |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1199713A (en) * | 1997-01-17 | 1998-11-25 | 圣戈班玻璃制造公司 | Silica-soda-lime glass, compositions and their applications |
| CN103776672A (en) * | 2014-01-10 | 2014-05-07 | 巨石集团有限公司 | Sample treatment method and chemical substance detection method for siliceous sandstones |
-
2016
- 2016-06-12 CN CN201610416877.8A patent/CN106093010A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1199713A (en) * | 1997-01-17 | 1998-11-25 | 圣戈班玻璃制造公司 | Silica-soda-lime glass, compositions and their applications |
| CN103776672A (en) * | 2014-01-10 | 2014-05-07 | 巨石集团有限公司 | Sample treatment method and chemical substance detection method for siliceous sandstones |
Non-Patent Citations (7)
| Title |
|---|
| 中华人民共和国国家质量监督检验检疫总局 中国国家标准化管理委员会: "《GB/T 1347-2008 钠钙硅玻璃化学分析方法》", 15 October 2008, 中国标准出版社 * |
| 全国标准物质管理委员会: "《中华人民共和国标准物质目录》", 30 June 2007, 中国计量出版社 * |
| 刘乃芸: "对水泥中Na2O、K2O测定方法的探讨", 《山东建材》 * |
| 姜艳清 等: "火焰光度法准确测定煤灰中氧化钾和氧化钠含量的体会", 《煤质技术》 * |
| 尚继芬 等: "玻璃及原料中氧化钠氧化钾的快速准确分析法-火焰分光光度法", 《玻璃纤维》 * |
| 常立娟 等: "提高火焰光度计测定水泥中氧化钾、氧化钠含量准确性的方法", 《科技资讯》 * |
| 徐伏秋 等: "《硅酸盐工业分析实验》", 31 March 2009, 化学工业出版社 * |
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