CN104483306A - Novel method for measuring content of impurities in zirconyl chloride octahydrate product - Google Patents
Novel method for measuring content of impurities in zirconyl chloride octahydrate product Download PDFInfo
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- CN104483306A CN104483306A CN201410834378.1A CN201410834378A CN104483306A CN 104483306 A CN104483306 A CN 104483306A CN 201410834378 A CN201410834378 A CN 201410834378A CN 104483306 A CN104483306 A CN 104483306A
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Abstract
The invention discloses a novel method for measuring the content of impurities in a zirconyl chloride octahydrate product, and belongs to methods for testing and analyzing materials by optical means of plasma thermal excitation. The method is characterized by comprising the following steps: (1), measuring the impurity content by an inductively coupled plasma atomic emission spectrometer; (2), adding a zirconium matrix solution into an impurity standard solution for enabling the zirconium matrix concentration of the impurity standard solution to be approximate to that of a sample solution to be measured. According to the novel method provided by the invention, the operation steps are simple and convenient, a detection result is accurate, and the impurity element detection limit is relatively low; the technical problems of complicated process, tedious operation, high analytic cost, a large amount of waste liquid pollutants, low measurement result precision and poor repeatability of a spectrophotometric method due to the addition of various regents for masking, ionic valence conversion, color development and the like in a detection process in the prior art are solved; the novel method is suitable for measuring the content of metal impurity elements in zirconyl chloride octahydrate, chloride octahydrate and zirconium carbonate products.
Description
Technical field
The present invention is the new method of dirt content test in a kind of eight hydration zirconium oxychloride products.Belong to and carry out test analysis material with the optical instrument of plasma thermal excitation.
Background technology
Eight hydration zirconium oxychloride (ZrOCl
28H
2o) being important zirconium chemicals, is the raw material of synthesis zirconium dioxide and many zirconates.Can be used as coating drying agent, rubber additive, fire resistive material, ceramic paint, lubricant; Be used widely in pottery, tanning, electronics, jewelry, metallurgical industry, catalyzer, medical treatment, purifying vehicle exhaust etc.And eight hydration zirconium oxychlorides still prepare the important source material of reactor-grade metal zirconium hafnium.
Due to eight hydration zirconium oxychloride (ZrOCl
28H
2o) of many uses, domestic and international market demand constantly rises, and eight hydration zirconium oxychloride products have wide market outlook.One of 21 century the most promising new high-tech material is called as with the serial zirconium products that eight hydration zirconium oxychlorides are raw material.
Along with widening of eight hydration zirconium oxychloride markets, the demand of user to the quality, particularly Light absorbing impurty of eight hydration zirconium oxychloride products constantly promotes, increasingly strictly.Such as; Existing " People's Republic of China's chemical industry standard " HG/T2772-2012[industry eight hydration eight hydrations zirconium oxychloride (basic zirconium chloride)] in the impurity technical requirement of regulation be: iron oxide≤0.002%, silicon dioxide≤0.01%, titania≤0.001%, sodium oxide molybdena≤0.005%, calcium oxide≤0.01%; And the requirement of certain user is: iron oxide≤0.0005%, silicon dioxide≤0.001%, titania≤0.0005%, sodium oxide molybdena≤0.001%, calcium oxide≤0.0005%.
In existing " People's Republic of China's chemical industry standard " HG/T2772-2012, the test method of regulation, free silica and titania adopt spectrophotometry, and iron oxide, calcium oxide, sodium oxide molybdena three kinds of impurity adopt aas determination.There is following weak point:
1. need in spectrophotometry process to add plurality of reagents for sheltering, transforming ion valence, colour developing etc., process complexity, complex operation, analysis cost are high, waste liquor contamination thing is many, and measurement result precision is low, poor repeatability.
2. atomic absorption spectrography (AAS) detects, and when sample concentration is low, elemental signals to be measured is weak, and during sample concentration height, the Zr element disturbance in product strengthens, and affects the accuracy of testing result.
3.. the impurity analysis project such as aluminium, barium of customer requirement, not yet makes stipulations in act.std, without ready patterns to follow.
4. when impurity content to be measured is less than 0.001%, measuring error becomes large, is difficult to obtain result accurately.
The new method that a kind of simple operating steps, testing result are accurate, impurity element detects dirt content test in eight lower hydration zirconium oxychloride products of limitation is that people expected.
Summary of the invention
The object of the invention is to avoid above-mentioned weak point of the prior art, and the new method that a kind of simple operating steps, testing result are accurate, impurity element detects dirt content test in eight lower hydration zirconium oxychloride products of limitation is provided.
Object of the present invention can be reached by following measure:
The new method that in eight hydration zirconium oxychloride products of the present invention, impurity content measures, is characterized in that:
1.. adopt inductively coupled plasma atomic emission spectrometer to measure;
2.. in contamination levels solution, add zirconium Matrix Solution, to make in contamination levels solution and testing sample solution zirconium matrix concentration comparable seemingly.
Atomic emission spectrometry measures the chemical composition of material according to the spectrum of atomic emissions.Its principle makes testing sample become gaseous atom by outside energy, and make gaseous atom outer-shell electron from ground state transition to excited state, when transitting to low-energy state from high-energy state, the unnecessary energy of release is launched characteristic spectral line by atom, the radiation produced in this process carries out dispersion light splitting through spectrometer, obtains spectrogram.In the spectral intensity that material is launched after exciting and material, the composition of element is closely related.Elements Atom content in line strength of element Atom and testing sample has certain funtcional relationship.Therefore by the emission spectrographic analysis to material, the content of material can be drawn.
Atomic emission spectrometry can be fast and convenient sense cycle table on 70 multiple elements.The amount analyzed needed for sample is few, can detect multiple element simultaneously, detect that the range of linearity is wider.
Inductively coupled plasma atomic emission spectrometry method because having multielement simultaneous determination, linear model is wide, highly sensitive, precision is good, the feature such as quick and precisely, inductively coupled plasma atomic emission spectrometer can reach 10 by accurate analysis content
-9the element of level, and the detection limit of a lot of common elements reaches μ g/L level, and analysis precision is very high.The element being applicable to high low content requires Simultaneously test, is specially adapted to the test item high to Minor element precision prescribed.
The ICP-AES that the present inventor adopts is the most effective method of current trace and ultratrace composition multielement Fast Measurement.Successfully solve in the testing process that in prior art, spectrophotometric method exists and need to add plurality of reagents for sheltering, transforming ion valence, colour developing etc., process complexity, complex operation, analysis cost are high, waste liquor contamination thing is many, and measurement result precision is low, the technical matters of poor repeatability.
In contamination levels solution, add zirconium Matrix Solution, to make in contamination levels solution and testing sample solution zirconium matrix concentration comparable seemingly.
Adopt the zirconium Matrix Solution similar to testing sample technical indicator, under the same terms as far as possible, standard model and sample to be tested are measured, avoids the change of a series of condition such as activating system, monitoring system and the systematic error brought, ensure that the accuracy of analysis result.It is the technical characteristic of having made the technical contribution given prominence to for completing task of the present invention.
Object of the present invention can also be reached by following measure:
The new method that in eight hydration zirconium oxychloride products of the present invention, impurity content measures, the iCAP6300 plasma emission spectrometer of Thermo Fischer Scient Inc. of inductively coupled plasma atomic emission spectrometry Yi Shi U.S. ThermoFisher Scientific that feature is 1. described.
The new method that in eight hydration zirconium oxychloride products of the present invention, impurity content measures, the running parameter of feature 1. described inductively coupled plasma atomic emission spectrometry instrument is chosen to be: RF power is 1150W (survey sodium is 950W); Nebulizer gas flow is 0.6L/min; Assist gas flow 0.5L/min; Flush time 30S; Rinse pump speed 100rpm; Analyze pump speed 50rpm; Integral time long wave 5S, shortwave 10S.It is preferred technical scheme.
The new method that in eight hydration zirconium oxychloride products of the present invention, impurity content measures, the impurity element in described eight hydration zirconium oxychloride products is iron, titanium, silicon, aluminium, barium, calcium, sodium.According to the market demand, the content of other impurity elements more in eight hydration zirconium oxychloride products can also be measured.
The new method that in eight hydration zirconium oxychloride products of the present invention, impurity content measures, the measurement line wavelength/nm of described impurity element to be measured is chosen as: iron Fe 238.2, titanium Ti334.9, silicon Si 251.6, aluminium Al 167.0, barium Ba 493.4, calcium Ca 93.3, sodium Na 589.0.It is preferred technical scheme.
The new method that in eight hydration zirconium oxychloride products of the present invention, impurity content measures, is characterized in that measuring in accordance with the following steps:
1.. zirconium Matrix Solution is prepared
Take the eight hydration zirconium oxychloride ZrOCl through three recrystallizing and refinings
28H
2o crystal 10.0000g, transfers in 100mL volumetric flask, after being diluted to scale constant volume, shakes up, and is zirconium Matrix Solution, and concentration is 100mg/mL;
2. .. impurity element standard solution preparation
A. iron Fe standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1726-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
B. titanium Ti standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1757-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
C. silicon Si standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1752-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
D aluminium Al standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1713-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
E. barium Ba standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1717-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
F. calcium Ca standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1720-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
G. sodium Na standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1738-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
3.. testing sample process
Take 50g testing sample and join constant volume in 250mL volumetric flask, get 5mL with transfer pipet and join in 100mL volumetric flask, be diluted to scale constant volume, shake up;
4. .. instrument and setting parameter thereof:
Use the iCAP6300 plasma emission spectrometer of Thermo Fischer Scient Inc. of U.S. ThermoFisher Scientific, instrument parameter is set as follows:
5.. element spectral line to be measured is selected
Selected line wavelength 167.0nm measures aluminium Al content;
Selected line wavelength 493.1nm measures barium Ba content
Selected line wavelength 393.3nm measures calcium Ca content
Selected line wavelength 238.2nm measures iron Fe content
Selected line wavelength 334.9nm measures titanium Ti content
Selected line wavelength 251.6nm measures silicon Si content
Selected line wavelength 589.0nm measures sodium Na content
6.. drawing curve
Respectively aspiration step 2. prepare iron Fe, titanium Ti, silicon Si, aluminium Al, barium Ba, calcium Ca, sodium Na seven kinds of impurity elements standard mark liquid each 0ml, 1mL, 2mL, 5mL, and move in respective 100mL volumetric flask, then, the zirconium Matrix Solution 10mL that 1. step is prepared is added in each volumetric flask, be diluted to scale constant volume, shake up; Namely in each pool-size bottle, constituent content to be measured is respectively 0mg, 0.01mg, 0.02mg, 0.05mg; Sample introduction on inductively coupled plasma atomic emission spectrometry instrument, determination data drawing curve;
7.. sample determination
Testing sample sample introduction, recording result is each constituent content to be measured, unit mg;
8.. data processing
Calculate as follows:
In formula:
W--constituent content to be measured (massfraction), numerical value represents with %;
M
1--apparatus measures result, unit is mg;
γ---element is converted into oxide coefficient;
M--sample quality, unit is g.
It is a preferred technical scheme.
In eight hydration zirconium oxychloride products of the present invention impurity content measure new method, step 1. described in the eight hydration zirconium oxychloride ZrOCl through three recrystallizing and refinings
28H
2o crystal, its technical requirement is: zirconium hafnium content is with ZrO
2massfraction>=37.00% of meter, iron, titanium, silicon, aluminium, barium, calcium, sodium impurity elements content are all less than 0.00001%.It is preferred technical scheme.
In eight hydration zirconium oxychloride products of the present invention, the application of the new method that impurity content measures, is characterized in that the mensuration of the metallic impurity elements content be applicable in eight hydration zirconium oxychlorides, zirconium dioxide, zirconium carbonate product.
The new method of dirt content test in eight hydration zirconium oxychloride products of the present invention, can produce following technique effect compared to existing technology:
1. provide a kind of simple operating steps, testing result accurately, impurity element detects the new method of dirt content test in eight lower hydration zirconium oxychloride products of limitation.
2. the ICP-AES adopted is the most effective method of current trace and ultratrace composition multielement Fast Measurement.Successfully solve in the testing process that in prior art, spectrophotometric method exists and need to add plurality of reagents for sheltering, transforming ion valence, colour developing etc., process complexity, complex operation, analysis cost are high, waste liquor contamination thing is many, and measurement result precision is low, the technical matters of poor repeatability.
3. in contamination levels solution, add eight hydration zirconium oxychloride zirconium Matrix Solutions of concentration close to testing sample solution.Adopt the zirconium Matrix Solution similar to testing sample technical indicator, under the same terms as far as possible, standard model and sample to be tested are measured, avoids the change of a series of condition such as activating system, monitoring system and the systematic error brought, ensure that the accuracy of analysis result.
4. avoid atomic absorption light spectroscopic methodology to detect, when sample concentration is low, elemental signals to be measured is weak, and during sample concentration height, the Zr element disturbance in product strengthens, and affects the technical matters of the accuracy of testing result.
5. the accurate data of the impurity content such as aluminium, barium can be provided according to customer requirement.
6. solve and exist in prior art, when impurity content to be measured is less than 0.001%, measuring error becomes large, is difficult to the technical matters obtaining result accurately.
Embodiment
The present invention will now be further detailed embodiment:
Embodiment 1
The assay method of impurity content in a kind of eight hydration zirconium oxychloride products
Measure in accordance with the following steps:
1.. zirconium Matrix Solution is prepared
Take the eight hydration zirconium oxychloride ZrOCl through three recrystallizing and refinings
28H
2o crystal 10.0000g, transfers in 100mL volumetric flask, after being diluted to scale constant volume, shakes up, and is zirconium Matrix Solution, and concentration is 100mg/mL;
2. .. impurity element standard solution preparation
A. iron Fe standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1726-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
B. titanium Ti standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1757-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
C. silicon Si standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1752-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
D aluminium Al standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1713-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
E. barium Ba standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1717-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
F. calcium Ca standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1720-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
G. sodium Na standard solution 0.01mg/mL
With the national liquid standard sample of numbering GSB04-1738-2004 (1.000mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
3.. testing sample process
Take 50g testing sample and join constant volume in 250mL volumetric flask, get 5mL with transfer pipet and join in 100mL volumetric flask, be diluted to scale constant volume, shake up;
4. .. instrument and setting parameter thereof:
Use the iCAP6300 plasma emission spectrometer of Thermo Fischer Scient Inc. of U.S. ThermoFisher Scientific, instrument parameter is set as follows:
5.. element spectral line to be measured is selected
Selected line wavelength 167.0nm measures aluminium Al content;
Selected line wavelength 493.1nm measures barium Ba content
Selected line wavelength 393.3nm measures calcium Ca content
Selected line wavelength 238.2nm measures iron Fe content
Selected line wavelength 334.9nm measures titanium Ti content
Selected line wavelength 251.6nm measures silicon Si content
Selected line wavelength 589.0nm measures sodium Na content
6.. drawing curve
Respectively aspiration step 2. prepare iron Fe, titanium Ti, silicon Si, aluminium Al, barium Ba, calcium Ca, sodium Na seven kinds of impurity elements standard mark liquid each 0ml, 1mL, 2mL, 5mL, and move in respective 100mL volumetric flask, then, the zirconium Matrix Solution 10mL that 1. step is prepared is added in each volumetric flask, be diluted to scale constant volume, shake up; Namely in each pool-size bottle, constituent content to be measured is respectively 0mg, 0.01mg, 0.02mg, 0.05mg; Sample introduction on inductively coupled plasma atomic emission spectrometry instrument, determination data drawing curve;
7.. sample determination
Testing sample sample introduction, recording result is each constituent content to be measured, unit mg;
8.. data processing
Calculate as follows:
In formula:
W--element oxide content (massfraction) to be measured, numerical value represents with %;
M
1--apparatus measures result, unit is mg;
γ---element is converted into oxide coefficient;
M--sample quality, unit is g.
Below measure according to upper method the eight hydration zirconium oxychloride Product checking records that Guang Tong company lot number is 09-101
Table 1 be the analysis spectral line of element to be measured and buckle back sight spot and the linearly dependent coefficient of curve of working
Table 1
Table 2 is the recovery and the relative standard deviation of assay method
Table 2
| Element | Al | Ca | Ba | Fe | Ti | Si | Na |
| Recovery % | 99 | 101 | 100 | 100 | 99 | 101 | 103 |
| RSD％ | 1.95 | 0.89 | 1.87 | 0.95 | 0.85 | 1.43 | 0.51 |
The recovery of each element of this assay method, between 99%-103%, illustrates that assay method of the present invention detects each element free of losses.Relative standard deviation (RSD) is less than 2%, has repeatability and accuracy preferably.
The lot number taking Zibo Guangtong Chemical Industry "Promplast-14" Co., Ltd's in September, 2014 production is the eight hydration zirconium oxychloride product 5.0035g of 09-101, and measurement result is as table 3
Calculate as follows:
W---element oxide content (massfraction) to be measured, numerical value represents with %;
M
1---apparatus measures result, unit is mg;
γ---element is converted into oxide coefficient;
M---sample quality, unit is g.
Table 3 is measurement and calculation results
Table 3
| Element | Al | Ca | Ba | Fe | Ti | Si | Na |
| Apparatus measures result, mg | 0.00079 | 0.0014 | 0.0013 | 0.00084 | 0.0013 | 0.0084 | 0.011 |
| Reduction coefficient γ | 1.89 | 1.40 | / | 1.43 | 1.67 | 2.14 | 1.35 |
| Result of calculation, % | 0.00015 | 0.00020 | 0.00013 | 0.00012 | 0.00022 | 0.0018 | 0.0015 |
Table 4 is these measurement results and " People's Republic of China's chemical industry standard eight hydration zirconium oxychloride " that by standard No. be " HG/T 2772-2012 " prescriptive procedure detects and Japanese Electric, China Aluminum Corporation ICP-MS detect this batch products Comparative result
Table 4
Claims (8)
1. the new method that in eight hydration zirconium oxychloride products, impurity content measures, is characterized in that:
1.. adopt inductively coupled plasma atomic emission spectrometer to measure;
2.. in contamination levels solution, add zirconium Matrix Solution, to make in contamination levels solution and testing sample solution zirconium matrix concentration comparable seemingly.
2., according to the new method that impurity content in eight hydration zirconium oxychloride products of claim 1 measures, it is characterized in that the iCAP6300 plasma emission spectrometer of Thermo Fischer Scient Inc. of inductively coupled plasma atomic emission spectrometry Yi Shi U.S. ThermoFisherScientific that feature is 1. described.
3., according to the new method that impurity content in eight hydration zirconium oxychloride products of claim 1 and claim 2 measures, it is characterized in that the running parameter of feature 1. described inductively coupled plasma atomic emission spectrometry instrument is chosen to be: RF power is 1150W (survey sodium is 950W); Nebulizer gas flow is 0.6L/min; Assist gas flow 0.5L/min; Flush time 30S; Rinse pump speed 100rpm; Analyze pump speed 50rpm; Integral time long wave 5S, shortwave 10S.
4., according to the new method that impurity content in eight hydration zirconium oxychloride products of claim 1 measures, it is characterized in that the impurity element in described eight hydration zirconium oxychloride products is iron, titanium, silicon, aluminium, barium, calcium, sodium.
5. according to the new method that impurity content in eight hydration zirconium oxychloride products of claim 4 measures, it is characterized in that the measurement line wavelength/nm of described impurity element to be measured is chosen as: iron Fe 238.2, titanium Ti334.9, silicon Si 251.6, aluminium Al167.0, barium Ba 493.4, calcium Ca 93.3, sodium Na 589.0.
6., according to the new method that impurity content in eight hydration zirconium oxychloride products of claim 1 measures, it is characterized in that measuring in accordance with the following steps:
1.. zirconium Matrix Solution is prepared
Take the eight hydration zirconium oxychloride ZrOCl through three recrystallizing and refinings
28H
2o crystal 10.0000g, transfers in 100mL volumetric flask, after being diluted to scale constant volume, shakes up, and is zirconium Matrix Solution, and concentration is 100mg/mL;
2. .. impurity element standard solution preparation
A. iron Fe standard solution 1.000mg/mL
With the national liquid standard sample of numbering GSB04-1726-2004 (0.1mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
B. titanium Ti standard solution 1.000mg/mL
With the national liquid standard sample of numbering GSB04-1757-2004 (0.1mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
C. silicon Si standard solution 1.000mg/mL
With the national liquid standard sample of numbering GSB04-1752-2004 (0.1mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
D aluminium Al standard solution 1.000mg/mL
With the national liquid standard sample of numbering GSB04-1713-2004 (0.1mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
E. barium Ba standard solution 1.000mg/mL
With the national liquid standard sample of numbering GSB04-1717-2004 (0.1mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
F. calcium Ca standard solution 1.000mg/mL
With the national liquid standard sample of numbering GSB04-1720-2004 (0.1mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
G. sodium Na standard solution 1.000mg/mL
With the national liquid standard sample of numbering GSB04-1738-2004 (0.1mg/ml) for standard specimen, draw this standard model 1ml, move in 100ml volumetric flask, be diluted to scale constant volume, shake up;
3.. testing sample process
Take 50g testing sample and join constant volume in 250mL volumetric flask, get 5mL with transfer pipet and join in 100mL volumetric flask, be diluted to scale constant volume, shake up;
4. .. instrument and setting parameter thereof:
Use the iCAP6300 plasma emission spectrometer of Thermo Fischer Scient Inc. of U.S. ThermoFisher Scientific, instrument parameter is set as follows:
5.. element spectral line to be measured is selected
Selected line wavelength 167.0nm measures aluminium Al content;
Selected line wavelength 493.1nm measures barium Ba content
Selected line wavelength 393.3nm measures calcium Ca content
Selected line wavelength 238.2nm measures iron Fe content
Selected line wavelength 334.9nm measures titanium Ti content
Selected line wavelength 251.6nm measures silicon Si content
Selected line wavelength 589.0nm measures sodium Na content
6.. drawing curve
Respectively aspiration step 2. prepare iron Fe, titanium Ti, silicon Si, aluminium Al, barium Ba, calcium Ca, sodium Na seven kinds of impurity elements standard mark liquid each 0ml, 1mL, 2mL, 5mL, and move in respective 100mL volumetric flask, then, the zirconium Matrix Solution 10mL that 1. step is prepared is added in each volumetric flask, be diluted to scale constant volume, shake up; Namely in each pool-size bottle, constituent content to be measured is respectively 0mg, 0.01mg, 0.02mg, 0.05mg; Sample introduction on inductively coupled plasma atomic emission spectrometry instrument, determination data drawing curve;
7.. sample determination
Testing sample sample introduction, recording result is each constituent content to be measured, unit mg;
8.. data processing
Calculate as follows:
In formula:
W--constituent content to be measured (massfraction), numerical value represents with %;
M
1--apparatus measures result, unit is mg;
γ---element is converted to oxide coefficient
M--sample quality, unit is g.
7., according to the new method that impurity content in eight hydration zirconium oxychloride products of claim 1 and claim 6 measures, it is characterized in that the eight hydration zirconium oxychloride ZrOCl through three recrystallizing and refinings described in step 1.
28H
2o crystal, its technical requirement is: zirconium hafnium content is with ZrO
2massfraction>=37.00% of meter, iron, titanium, silicon, aluminium, barium, calcium, sodium impurity elements content are all less than 0.00001%.
8. in eight hydration zirconium oxychloride products of claim 1, the application of the new method that impurity content measures, is characterized in that the mensuration of the metallic impurity elements content be applicable in eight hydration zirconium oxychlorides, zirconium dioxide, zirconium carbonate product.
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| CN105510306A (en) * | 2015-12-01 | 2016-04-20 | 贵州黎阳航空动力有限公司 | Method for measuring trace element content of nano-ZrO2 |
| CN115584501A (en) * | 2022-10-26 | 2023-01-10 | 中国航发沈阳黎明航空发动机有限责任公司 | Corrosive for showing macroscopic crystal defects of nickel-based superalloy single crystal blade and application thereof |
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