CN103293175B - Measure the method for liquid soluble glass chemical composition - Google Patents

Measure the method for liquid soluble glass chemical composition Download PDF

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CN103293175B
CN103293175B CN201310200288.2A CN201310200288A CN103293175B CN 103293175 B CN103293175 B CN 103293175B CN 201310200288 A CN201310200288 A CN 201310200288A CN 103293175 B CN103293175 B CN 103293175B
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soluble glass
liquid soluble
sample
liquid
ray fluorescence
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CN103293175A (en
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吴浩
魏艳
吕奎清
袁艺
张佑富
朱文刚
黄志芳
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Wuhan Tiemiao Welding Materials Co Ltd
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Wuhan Tiemiao Welding Materials Co Ltd
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Abstract

The invention discloses a kind of method measuring liquid soluble glass chemical composition, comprise the following steps: the 1) definite value of liquid soluble glass standard model; 2) preparation of liquid soluble glass sample and the determination of sampling amount; 3) the x-ray fluorescence spectrometry instrument drawing curve adopted; 4) Na in liquid soluble glass sample 2o, SiO 2, K 2the mensuration of O, S content.The present invention has feature quick, accurate, simple to operate, and sample just can direct injection analysis without the need to doing special process, can measure all types of water glass well; The applications expanding of the method range of application of x-ray fluorescence spectrometry method, compared with traditional wet chemistry analysis, this law sampling is easy, analysis speed fast, precision and accuracy high, drastically increase analytical test efficiency, save testing cost.

Description

Measure the method for liquid soluble glass chemical composition
Technical field
The invention belongs to field of spectral analysis technology, relate to a kind of method measuring liquid soluble glass chemical composition.
Background technology
Liquid soluble glass is moisture sodium polysilicate, is viscous liquid, is commonly used for cement or tackifier architectural, is also one of important source material of producing acid-resistant cement.Liquid soluble glass is also important bonding agent and the arc stabilizer of welding material production, and its quality is directly connected to the quality of properties of product.To the detection of liquid soluble glass chemical composition, be all at present generally that what to adopt is chemical industry standard HG/T2830-2009 " industrial sodium potassium silicate ", adopt gravimetric determination K 2o, acid base neutralization titration method measure SiO 2and Na 2o, turbidimetry for Determination S.Wherein K 2the mensuration of O needs to use the severe corrosive such as hydrofluorite, perchloric acid reagent; SiO 2, Na 2the mensuration of O compares owing to not having liquid soluble glass standard model, and the concentration of therefore used during acid-base titration standard titration solution directly determines SiO in sample 2, Na 2the content of O, so its standard titration solution needs especially strictly control in preparation, demarcation and preservation; Turbidimetry for Determination S can only carry out semiquantitative determination.This series of detection will expend more human and material resources (water power, chemical reagent etc.), and analysis time is also long, about 2, also has certain pollution to environment.
Summary of the invention
For solving the problems of the technologies described above, the invention provides and a kind ofly relate to a kind of method measuring liquid soluble glass chemical composition, with the Na in Accurate Determining liquid soluble glass 2o, SiO 2, K 2o, S content, thus increase work efficiency, cost-saving, reduce environmental pollution.
The method of mensuration liquid soluble glass chemical composition provided by the invention, comprises the following steps:
1) definite value of liquid soluble glass standard model;
2) preparation of liquid soluble glass sample and the determination of sampling amount;
3) the x-ray fluorescence spectrometry instrument drawing curve adopted;
4) Na in liquid soluble glass sample 2o, SiO 2, K 2the mensuration of O, S content.
Preferably, wherein step 1) described in the valued methods of liquid soluble glass standard model be: according to chemical industry standard HG/T2830-2009 " industrial sodium potassium silicate " and standard GB/T/T 4209-2008 " industrial metasilicate ", to Na in all types of liquid soluble glass sample 2o, SiO 2, K 2o, S content carries out chemical analysis definite value, only has the measurement result when each test item all to meet respective specified in above standard method, could using this liquid soluble glass sample as standard model.
Preferably, wherein step 2) described in being prepared as of liquid soluble glass sample: take 30g liquid soluble glass sample, be placed in polytetrafluoroethylene beaker, liquid soluble glass viscosity is drawn by viscosity meter direct-detection, need add 30g deionized water wherein when tested viscosity is greater than 1000mPa.s, is placed in by this polytetrafluoroethylene beaker on electric hot plate with the low-temperature heat being no more than 80 DEG C, carry out stirring to promote to dissolve with glass bar simultaneously, after abundant dissolving, cool, leave standstill, for subsequent use.
Preferably, wherein step 2) described in the sampling amount of liquid soluble glass sample be defined as: consider the sample amount of pipetting produces bubbles volume size on liquid soluble glass in the impact of X-fluorescence intensity and test process, and the capacity of measuring cup, gradient test is carried out to sampling amount, thus has determined that the amount of pipetting of sample is 15g.
Preferably, wherein step 3) described in x-ray fluorescence spectrometry instrument be sharp end window type rhodium target X-ray tube; And x-ray fluorescence spectrometry instrument described in this is equipped with helium system of filling and the liquid measure cup of analyzing liquid sample; LiF200, PE002, Ge111, PX1 or other conventional analyzing crystals; Autompulse Height Analyzer; Gas proportional detector.
Preferably, wherein step 3) described in adopt the flow process of x-ray fluorescence spectrometry instrument drawing curve to be: will according to step 1) in the liquid soluble glass detected value input x-ray fluorescence spectrometry instrument inspection software of definite value, Criterion sample concentration database, filling under helium system step 1) the liquid soluble glass standard model of definite value measures, after all standard models are measured, carry out linear regression, draw out the working curve of X-ray intensity to constituent content, set up the drift correction program of working curve simultaneously, thus guarantee the stability of instrument continuous duty and the accuracy of result.
Preferably, wherein step 4) described in Na in liquid soluble glass sample 2o, SiO 2, K 2the mensuration flow process of O, S content is: at one, the carrying disk upper berth of electronic balance filter paper, liquid measure cup is placed on filter paper, accurately taking 15g according to step 2) ready liquid soluble glass sample puts into this measuring cup, covering vinyl cover, leave standstill 3 minutes, whether having this measuring cup of water suction confirmation there is no fluid sample seepage by observing filter paper, select step 3) working curve set up, measure with x-ray fluorescence spectrometry instrument, calculate, obtain a result.
The present invention can reach following technique effect:
Method provided by the present invention has feature quick, accurate, simple to operate, and sample just can direct injection analysis without the need to doing special process, can well measure all types of water glass; The applications expanding of the method range of application of x-ray fluorescence spectrometry method, compared with traditional wet chemistry analysis, easy, the analysis speed of this method sampling is fast, precision and accuracy high, by setting up the drift correction program of working curve, working curve is set up without the need to repeating, drastically increase analytical test efficiency, thus be conducive to saving testing cost.
Accompanying drawing explanation
Fig. 1 is the effect diagram of the sample amount of pipetting to Na, S measured intensity;
Fig. 2 is the effect diagram of the sample amount of pipetting to Si, K measured intensity.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, and to make those skilled in the art the present invention may be better understood and can be implemented, but illustrated embodiment is not as a limitation of the invention.
Measure a method for liquid soluble glass chemical composition, its step comprises: the 1) definite value of liquid soluble glass standard model; 2) preparation of liquid soluble glass sample and the determination of sampling amount; 3) x-ray fluorescence spectrometry instrument drawing curve is adopted; 4) Na in liquid soluble glass sample 2o, SiO 2, K 2the mensuration of O, S content.
The definite value of liquid soluble glass standard model: according to the requirement of test event and scope, according to chemical industry standard HG/T2830-2009 " industrial sodium potassium silicate " and standard GB/T/T 4209-2008 " industrial metasilicate ", to Na in existing liquid soluble glass sample 2o, SiO 2, K 2o, S content carries out chemical analysis definite value, only has the measurement result when each test item all to meet respective specified in above standard method, just can using this water glass sample as standard model drawing curve.According to the needs of drawing curve, have finally chosen the standard model of 11 liquid soluble glass samples as drawing curve, sensing range is in table 1, and its each component content is in table 2.The concentration of standard model covers the concentration range of whole quantitative test.
Table 1 measurement range
Table 2 standard model value data
The service condition of x-ray fluorescence spectrometry instrument: the service condition of instrument should meet GB/T 16597 " metallurgic product analysis method x-ray fluorescence spectrometry method general rule ".
The configuration of x-ray fluorescence spectrometry instrument: sharp end window type rhodium target X-ray tube; This x-ray fluorescence spectrometry instrument is equipped with helium system of filling and the liquid measure cup of analyzing liquid sample; LiF200, PE002, Ge111, PX1 or other conventional analyzing crystals; Autompulse Height Analyzer; Gas proportional detector.
The determination of x-ray fluorescence spectrometry instrument measurement parameter: select optimum measurement parameter according to element to be analyzed and spectral line disturbed condition.The Wavelength dispersion type X fluorescence spectrometer in this laboratory measures Na 2o, SiO 2, K 2when O, S, selected measurement spectral line is respectively: K-K α, Na-K α, Si-K α, S-K α.According to X fluorescence spectrum law theory, there is the interference of other element a large amount of in above-mentioned spectral line, and interference type has overlap of spectral lines, α absorbs/strengthens, β absorbs/strengthens.For finding out the interference element that may exist, making sample with water glass, in the channel setting of program, angle scanning being carried out to the element that may exist, find interference element mainly P and Ca existed.Independent deionized water carries out same scanning as sample again simultaneously, finds that the peak position intensity of P and Ca is about the same with peak position intensity when making sample with water glass.It can thus be appreciated that P and Ca comes from support liq mylar used.Owing to must use mylar when measuring liquid, therefore each measurement all can have P and Ca to disturb, so in the channel setting of program, also added the Measurement channel of P and Ca except the Measurement channel of element to be measured, for later curvature correction.Design parameter is in table 3.
Table 3 apparatus measures parameter
Note: PHD is pulse height distribution, and FLOW is gas proportional detector.
The determination of liquid soluble glass sampling amount: in liquid soluble glass, more than 50% is water, belongs to light matrix sample, and X ray has penetration capacity to light matrix sample, the measured intensity of the amount of pipetting to analytical element of sample has a certain impact.Choose the liquid soluble glass that each analytical element content is all moderate, get 5g, 10g, 15g, 20g, 25g and put into the measuring cup measuring liquid respectively, the X-fluorescence intensity of determination and analysis element.Choose element Na, S, K, Si to be measured and investigate the size of the sample amount of pipetting to the impact (see Fig. 1, Fig. 2) of X-fluorescence intensity.Known, when the sample amount of pipetting is more than or equal to 10g, sample is infinite thickness substantially, and now X ray can not penetrate the fluorescence intensity of sample and impact analysis element.Due to the irradiation of X ray, liquid soluble glass is heated, and can produce bubble bottom measuring cup.Bubble has a certain impact to X-fluorescence intensity, therefore should reduce the generation of bubble as far as possible.Under same illuminate condition, sample size is larger, and its temperature increase is less, and the generation of bubble is fewer.Consider the impact of the sample amount of pipetting on the impact of X-fluorescence intensity and bubble generation, and the capacity of measuring cup, finally determine that the amount of pipetting of sample is 15g.
Measure the impact of dielectric gas residual quantity: Xray fluorescence spectrometer is filling under helium system state and directly can carry out analytical test to liquid, when gas condition is changed, helium condition is changed into by air conditions, if the time transformed is too short, then gas residue can have a great impact testing result, found through experiments, and the time will be set as 70s, conversion can be carried out fully, can ensureing that gas is changed completely.
The drafting of working curve: working curve is that according to least square method, intensity and concentration fitting operation are drawn by the clean intensity (Net Rate) of ultimate analysis line each in series of standards sample and its normal concentration C.By in the liquid soluble glass detected value input x-ray fluorescence spectrometry instrument inspection software of 11 definite values, Criterion sample concentration database, the liquid soluble glass standard model of chemical definite value is measured filling under helium system, under the measurement parameter collected, standard model is measured one by one, after all standard models are measured, carry out linear regression, draw out the working curve of X-ray intensity to constituent content.
The drift correction of working curve: in instrument use procedure, by the impact that self and external condition change, may be there is certain change in spectrometer state, apply drift correction sample for this reason and correct instrument, thus guarantee the stability of instrument continuous duty and the accuracy of result.
Embodiment 1
To detect the high mould liquid soluble glass sample that certain factory produces:
First high mould liquid soluble glass viscosity is detected, its viscosity is 3850mPa.s after testing, therefore needs to dilute this sample, accurately takes this high mould liquid soluble glass sample of 30g, be placed in polytetrafluoroethylene beaker, add 30g deionized water wherein, this polytetrafluoroethylene beaker is placed in low-temperature heat on electric hot plate, temperature is no more than 80 DEG C, carry out stirring to promote to dissolve with glass bar simultaneously, after abundant dissolving, cool, leave standstill, for subsequent use.
At one, the carrying disk upper berth of electronic balance filter paper, liquid measure cup is placed on filter paper, takes the ready liquid soluble glass sample of 15g and put into measuring cup, cover vinyl cover, leaving standstill 3 minutes, whether having water suction confirmation measuring cup there is no fluid sample seepage by observing filter paper.
Start instrument and carry working software, before measurement, analysis medium is become helium, the parameters of inspection apparatus, after start is stable, starts paced work tracing analysis program, application drift correction sample corrects instrument, from standard model, choose arbitrarily a standard model as sample for reference, if measured value and standard value there was no significant difference, then instrument can be directly used in analysis.
Get out the measuring cup that testing liquid water glass is housed, select the paced work tracing analysis program set up, start to measure with x-ray fluorescence spectrometry instrument, analyzing the complete time used is 80s, carries software directly export measurement result by instrument.Compare with traditional wet chemistry analysis result, the comparison result of two kinds of methods is in table 4:
Table 4 method comparison result
As can be seen from the comparison result of table 4, analysis result conforms to traditional wet chemistry value, and this law acquired results meets analytical test requirement completely.
Embodiment 2
To detect the low mould liquid soluble glass sample that certain factory produces:
First detect low mould liquid soluble glass viscosity, its viscosity is 500mPa.s after testing, therefore without the need to diluting this sample.
At one, the carrying disk upper berth of electronic balance filter paper, liquid measure cup being placed on filter paper, taking 15g liquid soluble glass sample and put into measuring cup, cover vinyl cover, leave standstill 3 minutes, whether having water suction confirmation measuring cup there is no fluid sample seepage by observing filter paper.
Start instrument and carry working software, before measurement, analysis medium is become helium, the parameters of inspection apparatus, after start is stable, starts paced work tracing analysis program, application drift correction sample corrects instrument, from standard model, choose arbitrarily a standard model as sample for reference, if measured value and standard value there was no significant difference, then instrument can be directly used in analysis.
Get out the measuring cup that testing liquid water glass is housed, select the paced work tracing analysis program set up, start to measure with x-ray fluorescence spectrometry instrument, analyzing the complete time used is 80s, carries software directly export measurement result by instrument.With wet chemical analysis results contrast, the comparison result of two kinds of methods is in table 5:
Table 5 method comparison result
As can be seen from the comparison result of table 5, analysis result conforms to wet chemistry value, and this law acquired results meets analytical test requirement completely.
The above embodiment is only that protection scope of the present invention is not limited thereto in order to absolutely prove the preferred embodiment that the present invention lifts.The equivalent alternative or conversion that those skilled in the art do on basis of the present invention, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.

Claims (2)

1. measure a method for liquid soluble glass chemical composition, it is characterized in that, comprise the following steps:
1) definite value of liquid soluble glass standard model: according to chemical industry standard HG/T2830-2009 " industrial sodium potassium silicate " and standard GB/T/T 4209-2008 " industrial metasilicate ", to Na in all types of liquid soluble glass sample 2o, SiO 2, K 2o, S content carries out chemical analysis definite value, only has the measurement result when each test item all to meet respective specified in above standard method, could using this liquid soluble glass sample as standard model;
2) preparation of liquid soluble glass sample and the determination of sampling amount: take 30g liquid soluble glass sample, be placed in polytetrafluoroethylene beaker, liquid soluble glass viscosity is drawn by viscosity meter direct-detection, 30g deionized water need be added wherein when tested viscosity is greater than 1000mPa.s, this polytetrafluoroethylene beaker is placed in the low-temperature heat being no more than 80 DEG C on electric hot plate, carries out stirring to promote to dissolve, after fully dissolving with glass bar simultaneously, cool, leave standstill, for subsequent use; Consider the sample amount of pipetting produces bubbles volume size on liquid soluble glass in the impact of X-fluorescence intensity and test process, and the capacity of measuring cup, gradient test is carried out to sampling amount, thus has determined that the amount of pipetting of sample is 15g;
3) x-ray fluorescence spectrometry instrument drawing curve is adopted: will according to step 1) in the liquid soluble glass detected value input x-ray fluorescence spectrometry instrument inspection software of definite value, Criterion sample concentration database, filling under helium system step 1) the liquid soluble glass standard model of definite value measures, after all standard models are measured, carry out linear regression, draw out the working curve of X-ray intensity to constituent content, set up the drift correction program of working curve simultaneously, thus guarantee the stability of instrument continuous duty and the accuracy of result;
4) Na in liquid soluble glass sample 2o, SiO 2, K 2the mensuration of O, S content: at one, the carrying disk upper berth of electronic balance filter paper, liquid measure cup is placed on filter paper, accurately taking 15g according to step 2) ready liquid soluble glass sample puts into this measuring cup, covering vinyl cover, leave standstill 3 minutes, whether having this measuring cup of water suction confirmation there is no fluid sample seepage by observing filter paper, select step 3) working curve set up, measure with x-ray fluorescence spectrometry instrument, calculate, obtain a result.
2. the method for mensuration liquid soluble glass chemical composition according to claim 1, is characterized in that, step 3) described in x-ray fluorescence spectrometry instrument be sharp end window type rhodium target X-ray tube; And x-ray fluorescence spectrometry instrument described in this be equipped with analyzing liquid sample fill helium system, liquid measure cup, analyzing crystal, autompulse Height Analyzer and gas proportional detector, wherein analyzing crystal is LiF200 or PE002 or Ge111 or PX1.
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CN104483338A (en) * 2014-12-23 2015-04-01 山东省第四地质矿产勘查院 Method for measuring bromine in brine through filter paper method sample preparation and X-ray fluorescent spectrometry
CN104634803B (en) * 2015-03-03 2017-07-04 四川西冶新材料股份有限公司 The method that lower illuminated Xray fluorescence spectrometer determines liquid soluble glass
CN106290439B (en) * 2016-09-21 2018-10-16 海南中航特玻科技有限公司 Quickly measure Na in saltcake2SO4、NaCl、Fe2O3The method of content
CN109738472A (en) * 2019-02-27 2019-05-10 上海精谱科技有限公司 A kind of method that x-ray fluorescence measures light element in silica sol liquid

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