CN105223186A - Adopt the method for silicon content in ICP method Fast Measurement titanium or titanium alloy - Google Patents

Abstract

The invention discloses a kind of method adopting silicon content in ICP method Fast Measurement titanium or titanium alloy, the method is dissolved at low temperatures sample nitric acid and hydrofluorite, use boric acid complexing fluorine ion again, and adjust matrix content make it coupling, production standard solution curve, on indutively coupled plasma Atomic Emission Spectrometer AES, suitable element silicon analytical line is selected to carry out measuring the content of element silicon.The present invention adopts nitric acid and hydrofluoric acid dissolution test portion, then uses boric acid complexing fluorine ion, thus avoids hydrofluorite to corrode the quartz sample system of indutively coupled plasma Atomic Emission Spectrometer AES, pollutes, affect the factor of measurement accuracy to instrument.Meanwhile, the present invention adopts boric acid to stablize sample solution and standard solution acidity, not only avoid the inconsistent impact on measuring of acidity, and adjustment matrix content makes it coupling, decreases matrix effect.

Description

Adopt the method for silicon content in ICP method Fast Measurement titanium or titanium alloy

Technical field

The present invention relates to a kind of method measuring silicon content in titanium or titanium alloy, particularly relate to a kind of method adopting silicon content in ICP method Fast Measurement titanium or titanium alloy.

Background technology

Titanium is a kind of important structural metal grown up the 1950's, and intensity is high, corrosion stability good because having for titanium alloy, thermotolerance high and be widely used in Aeronautics and Astronautics field.In titanium alloy, the addition of element silicon plays an important role to the intensity of titanium alloy and heat resistance, therefore silicon content in Measurement accuracy titanium alloy, is the key of development and production control.At present, generally adopt titanium sponge, titanium or titanium alloy chemical analysis method-molybdenum blue spectrophotometric method to measure silicon amount (GB4968.3-1996), but there is the shortcomings such as measurement range narrow (0.010% ~ 0.060%), accuracy is low, complex operation, test period are long in the method, can not meet modern Production requirement.

In detection alloying element means, since inductively coupled plasma (ICP) emission spectrometer came out from 1975, the advantages such as the mutual interference just because its detectability is low, precision is high, between wide, the sample composition of the mensuration range of linearity of concentration is little, become a kind of analysis means that other analytical technology is incomparable in micro-Simultaneously test.But, in traditional method for sample pretreatment, normal employing nitric acid, hydrofluorite mixed-acid dissolution sample, hydrofluorite has corrosive attack to indutively coupled plasma Atomic Emission Spectrometer AES quartz sample system, easily instrument is polluted, the accuracy that impact measures and repeatability, and adopt the wayward sample solution of nitric acid and standard solution acidity separately, easily cause solution acidity inconsistent, affect measurement result.

Summary of the invention

The object of the invention is to: provide a kind of method fast, accurately, to silicon content in instrument free of contamination employing ICP method Fast Measurement titanium or titanium alloy, to overcome the deficiencies in the prior art.

Technical scheme of the present invention: a kind of method adopting silicon content in ICP method Fast Measurement titanium or titanium alloy, comprises the following steps:

A, take 0.1g titanium or titanium alloy sample in the teflon cup of 200mL, first add the water of 20mL, add the nitric acid that 10mL top grade is pure again, then the pure hydrofluorite of 2mL top grade is slowly added dropwise to plastic dropper, now teflon cup is placed on electric hot plate and heats, control temperature 80 DEG C, after dissolving completely to sample, teflon cup is taken off from electric hot plate and adds 20mL water, add the boric acid that 3g top grade is pure again, shake cup makes boric acid dissolve, be cooled to after room temperature until solution, solution is moved in the plastics volumetric flask of 100mL, mix with after water constant volume, then 40min is left standstill,

B, take the pure titanium consistent with matrix of samples respectively in the teflon cup of 6 200mL, then the silicon standard solution 0mL that concentration is 10 μ g/mL is pipetted respectively, 1.0mL, 5.0mL is in front 3 teflon cups, pipette the silicon standard solution 1.0mL that concentration is 100 μ g/mL respectively, 5.0mL, 10.0mL is in rear 3 teflon cups, now in each teflon cup, add the pure nitric acid of 10mL top grade, the pure hydrofluorite of 2mL top grade is slowly added dropwise to plastic dropper, now teflon cup is placed on electric hot plate and heats, control temperature 80 DEG C, after dissolving completely to sample, teflon cup is taken off from electric hot plate and adds 20mL water, add the boric acid that 3g top grade is pure again, shake cup makes boric acid dissolve, be cooled to after room temperature until solution, solution is moved in the plastics volumetric flask of 100mL, mix with after water constant volume, then 40min is left standstill, obtained standard serial solution,

C, to filter dry to standard serial solution and sample solution, and discard front 5mL, then on ICP spectrometer, according to instrument condition of work, above-mentioned standard solution is measured, with each silicon massfraction to be measured for horizontal ordinate, emissive porwer is ordinate, by computer drawing calibration curve, finally according to instrument condition of work, sample solution is measured, calculate silicone content by calibration curve.

Compared with prior art, the invention has the advantages that: the present invention adopts nitric acid and hydrofluoric acid dissolution test portion, use boric acid complexing fluorine ion again, thus avoid hydrofluorite to corrode the quartz sample system of indutively coupled plasma Atomic Emission Spectrometer AES, instrument is polluted, affects the factor of measurement accuracy.Meanwhile, the present invention adopts boric acid to stablize sample solution and standard solution acidity, not only avoid the inconsistent impact on measuring of acidity, and adjustment matrix content makes it coupling, decreases matrix effect.Be proven, method of the present invention is adopted to measure the massfraction of titanium or titanium alloy silicon content in 0.010% ~ 1.00% scope, expand the measurement range (0.010% ~ 0.060%) of GB4968.3-1996 method, solve the mensuration of all trade mark element silicons of titanium or titanium alloy, and the RSD of element silicon measurement result is all less than 5%, precision is better, and accuracy in detection is high, for production control, scientific research provide indissoluble nickel base superalloy chemical element compositional data accurately.

Embodiment

In order to make the object of the invention, technical scheme and advantage clearly, below in conjunction with embodiment, the present invention is described in further detail.

Embodiment

A kind of method adopting silicon content in ICP method Fast Measurement titanium or titanium alloy of the present invention, comprises the following steps:

A, take 0.1g titanium or titanium alloy sample in the teflon cup of 200mL, first add the water of 20mL, add the nitric acid that 10mL top grade is pure again, then the pure hydrofluorite of 2mL top grade is slowly added dropwise to plastic dropper, now teflon cup is placed on electric hot plate and heats, control temperature 80 DEG C, after dissolving completely to sample, teflon cup is taken off from electric hot plate and adds 20mL water, add the boric acid that 3g top grade is pure again, shake cup makes boric acid dissolve, be cooled to after room temperature until solution, solution is moved in the plastics volumetric flask of 100mL, mix with after water constant volume, then 40min is left standstill,

B, take the pure titanium consistent with matrix of samples respectively in the teflon cup of 6 200mL, then the silicon standard solution 0mL that concentration is 10 μ g/mL is pipetted respectively, 1.0mL, 5.0mL is in front 3 teflon cups, pipette the silicon standard solution 1.0mL that concentration is 100 μ g/mL respectively, 5.0mL, 10.0mL is in rear 3 teflon cups, now in each teflon cup, add the pure nitric acid of 10mL top grade, the pure hydrofluorite of 2mL top grade is slowly added dropwise to plastic dropper, now teflon cup is placed on electric hot plate and heats, control temperature 80 DEG C, after dissolving completely to sample, teflon cup is taken off from electric hot plate and adds 20mL water, add the boric acid that 3g top grade is pure again, shake cup makes boric acid dissolve, be cooled to after room temperature until solution, solution is moved in the plastics volumetric flask of 100mL, mix with after water constant volume, then 40min is left standstill, obtained standard serial solution,

C, to filter dry to standard serial solution and sample solution, and discard front 5mL, then on ICP spectrometer, according to instrument condition of work, above-mentioned standard solution is measured, with each silicon massfraction to be measured for horizontal ordinate, emissive porwer is ordinate, by computer drawing calibration curve, finally according to instrument condition of work, sample solution is measured, calculate silicone content by calibration curve.

Be proven, method of the present invention is adopted to measure the massfraction of titanium or titanium alloy silicon content in 0.010% ~ 1.00% scope, expand the measurement range (0.010% ~ 0.060%) of GB4968.3-1996 method, solve the mensuration of all trade mark element silicons of titanium or titanium alloy, and the RSD of element silicon measurement result is all less than 5%, precision is better, and accuracy in detection is high, for production control, scientific research provide indissoluble nickel base superalloy chemical element compositional data accurately.

Claims (1)

1. adopt a method for silicon content in ICP method Fast Measurement titanium or titanium alloy, it is characterized in that comprising the following steps:

A, take 0.1g titanium or titanium alloy sample in the teflon cup of 200mL, first add the water of 20mL, add the nitric acid that 10mL top grade is pure again, then the pure hydrofluorite of 2mL top grade is slowly added dropwise to plastic dropper, now teflon cup is placed on electric hot plate and heats, control temperature 80 DEG C, after dissolving completely to sample, teflon cup is taken off from electric hot plate and adds 20mL water, add the boric acid that 3g top grade is pure again, shake cup makes boric acid dissolve, be cooled to after room temperature until solution, solution is moved in the plastics volumetric flask of 100mL, mix with after water constant volume, then 40min is left standstill,

B, take the pure titanium consistent with matrix of samples respectively in the teflon cup of 6 200mL, then the silicon standard solution 0mL that concentration is 10 μ g/mL is pipetted respectively, 1.0mL, 5.0mL is in front 3 teflon cups, pipette the silicon standard solution 1.0mL that concentration is 100 μ g/mL respectively, 5.0mL, 10.0mL is in rear 3 teflon cups, now in each teflon cup, add the pure nitric acid of 10mL top grade, the pure hydrofluorite of 2mL top grade is slowly added dropwise to plastic dropper, now teflon cup is placed on electric hot plate and heats, control temperature 80 DEG C, after dissolving completely to sample, teflon cup is taken off from electric hot plate and adds 20mL water, add the boric acid that 3g top grade is pure again, shake cup makes boric acid dissolve, be cooled to after room temperature until solution, solution is moved in the plastics volumetric flask of 100mL, mix with after water constant volume, then 40min is left standstill, obtained standard serial solution,

C, to filter dry to standard serial solution and sample solution, and discard front 5mL, then on ICP spectrometer, according to instrument condition of work, above-mentioned standard solution is measured, with each silicon massfraction to be measured for horizontal ordinate, emissive porwer is ordinate, by computer drawing calibration curve, finally according to instrument condition of work, sample solution is measured, calculate silicone content by calibration curve.