CN110823867A - Analysis method for multi-element content in tin-lanthanum-cerium intermediate alloy - Google Patents
Analysis method for multi-element content in tin-lanthanum-cerium intermediate alloy Download PDFInfo
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Abstract
The method comprises the steps of weighing 0.1000g of a tin-lanthanum-cerium intermediate alloy sample, placing the sample in a 150mL conical flask, adding 30mL of 1+3 mixed nitrate acid, heating at a low temperature until the sample is completely dissolved, taking down, cooling to room temperature, diluting to a certain volume by using second-level or higher-level pure water, measuring the emission light intensity of an analysis element in a test solution at a recommended wavelength or other suitable wavelengths on an inductively coupled plasma atomic emission spectrometer by using a prepared tin-lanthanum-cerium series calibration solution, and calculating the mass fractions of tin, lanthanum and cerium according to a calibration curve. The invention solves the technical problem of detecting the content of tin, lanthanum and cerium in the tin, lanthanum and cerium intermediate alloy, and establishes a specific analysis method; solves the technical problems of the inductively coupled plasma atomic emission spectrometry detection method of the content of tin-free lanthanum and cerium, and the measurement of the content of antimony, bismuth, iron, arsenic, copper, silver, zinc, aluminum, cadmium, phosphorus and gold.
Description
Technical Field
The invention relates to an analysis method of multi-element content in tin-lanthanum-cerium intermediate alloy, in particular to an inductively coupled plasma atomic emission spectroscopy quantitative analysis method of the tin-lanthanum-cerium content in the tin-lanthanum-cerium intermediate alloy.
Background
The tin-lead solder has low melting point, good corrosion resistance and good wettability to copper, copper alloy and steel, is widely applied to the aspects of connection of electric parts, elements and leads, connection of common terminals and printed circuit boards and the like, and accounts for about 70-80 percent in the field of electronic industry. Pb used in the solder is difficult to recover, and the Pb harms water sources and affects human health. Nowadays, with the enhancement of environmental awareness, the limited use and prohibition of lead-containing solders is actually a matter of time, and the replacement of lead-containing solders with lead-free solders is imperative, and the development of lead-free solders is urgent.
A novel diversified rare earth soft solder product belongs to lead-free solder. The main raw materials required by the production are tin-lanthanum-cerium intermediate alloy, and the components are as follows: tin is a matrix element, lanthanum is 0.050-10.00 percent, cerium is 0.050-20.00 percent, and other impurity elements are contained.
In order to meet the production requirements of the novel product, the content and the addition amount of multiple elements in the tin-lanthanum-cerium intermediate alloy must be strictly controlled, which undoubtedly provides a difficult problem for chemical analysts and provides a challenge for the development of detection technology.
Through inquiry, the standard analysis method approved to be issued in China has about more than 1000 items.
Relevant criteria are:
① GB/T2454-2009 analysis method for measuring contents of lanthanum, cerium and magnesium in cast iron and low alloy steel by inductively coupled plasma atomic emission spectrometry
② GB/T12689.12-2004 method for chemical analysis of Zn and Zn alloy
③ YS/T806-2012 method for measuring contents of lanthanum, cerium, praseodymium, neodymium and samarium in aluminum and aluminum alloy by using X-ray fluorescence spectrometry
④ GB/T3260-2000 method for analyzing tin chemistry
⑤ GB/T10574.1-2003 determination of tin content in chemical analysis method of tin-lead solder
⑥ GB/T12689.11-2004 tribromoazoarsine spectrophotometry for measuring lanthanum and cerium content in chemical analysis method of zinc and zinc alloy
⑦ GB/T223.33-1994 & lt & gt analysis method of chemistry of steel and alloy extraction and separation-cerium content determination by azochlorophosphine mA spectrophotometry & gt
⑧ GB/T20975.24-2008 "chemical analysis method of aluminum and aluminum alloy part 24. determination of total content of rare earth" method tribromoazoarsine spectrophotometry "and" method of oxalate gravimetric method ".
⑨ GB/T10574.13-2017 chemical analysis method of tin-lead solder part 13, determination of contents of antimony, bismuth, iron, arsenic, copper, silver, zinc, aluminum, cadmium, phosphorus and gold by inductively coupled plasma atomic emission spectrometry.
However, the national and industry standard analysis method of elements such as tin, lanthanum and cerium in the tin-lanthanum-cerium intermediate alloy is not found. In addition, no relevant applicable analysis methods have been found in the enterprise standard methods. At present, the development of a method for detecting the content of multiple elements in the tin-lanthanum-cerium intermediate alloy is still blank.
Disclosure of Invention
The present invention is to solve the above problems in the background art, and provides a method for analyzing the content of multiple elements in a tin-lanthanum-cerium intermediate alloy.
The method comprises the steps of weighing 0.1000g of a tin-lanthanum-cerium intermediate alloy sample, placing the sample in a 150mL conical flask, adding 30mL of 1+3 mixed nitrate acid, heating at a low temperature until the sample is completely dissolved, taking down, cooling to room temperature, diluting to a certain volume by using second-level or higher-level pure water, measuring the emission light intensity of an analysis element in a test solution at a recommended wavelength or other suitable wavelengths on an inductively coupled plasma atomic emission spectrometer by using a prepared tin-lanthanum-cerium series calibration solution, and calculating the mass fractions of tin, lanthanum and cerium according to a calibration curve.
The invention has the beneficial effects that:
the method for analyzing the content of multiple elements in the tin-lanthanum-cerium intermediate alloy has the following characteristics:
1. the technical problem of detecting the content of tin, lanthanum and cerium in the tin, lanthanum and cerium intermediate alloy for the innovative project of 'national development technology [ 2012 ] 778-multiple rare earth alloy soft solder' (the standing code 12C26215116037, Chongqing Jinkang tin industry development Co., Ltd.) is solved, and a specific analysis method is established;
2. the technical problem of the inductively coupled plasma atomic emission spectrometry detection method of the content of tin, lanthanum and cerium in GB/T3260-2013 tin chemical analysis method and GB/T10574.1-2003 tin content determination of tin-lead solder chemical analysis method is solved;
3. the method solves the problems of part 13 of the chemical analysis method of the tin-lead solder of GB/T10574.13-2017: the inductively coupled plasma atomic emission spectrometry detection method is adopted in the inductively coupled plasma atomic emission spectrometry for measuring the amounts of antimony, bismuth, iron, arsenic, copper, silver, zinc, aluminum, cadmium, phosphorus and gold, but the technical problem of measuring the content of tin, lanthanum and cerium cannot be solved;
4. the chemical detection method solves the problem that the chemical detection of the content of tin, lanthanum and cerium in the tin, lanthanum and cerium intermediate alloy has no existing reliable chemical analysis method of national standard, industrial standard, local standard and enterprise standard;
4. measurement range: 65 to 95 percent of Sn, 0.050 to 10.00 percent of La and 0.050 to 20.00 percent of Ce;
5. precision: the difference in analytical results between laboratories should not be greater than the allowable difference values listed in table 1.
TABLE 1 allowable Difference values
Detailed Description
Examples
The process of the present invention is further illustrated below with reference to examples.
The invention relates to a method for analyzing the content of multiple elements in a tin-lanthanum-cerium intermediate alloy, which comprises the following steps:
the method comprises the following steps: reagent preparation
Adding 200mL of pure water into a 500mL beaker, adding hydrochloric acid and nitric acid, and uniformly stirring by using a glass rod;
step two: pretreatment of sample
Weighing 0.1000g of tin-lanthanum-cerium intermediate alloy sample, placing the sample in a 150mL conical flask, adding 30mL of 1+3 mixed salt-nitrate acid, heating at low temperature until the sample is completely dissolved, taking down, cooling to room temperature, transferring into a 100mL volumetric flask, inserting a glass rod into the volumetric flask during the transfer process, enabling the opening of the conical flask to be inclined and tightly close to the glass rod, enabling the solution to slowly flow along the glass rod, enabling the lower end of the glass rod to be close to the inner wall of the bottleneck but not too close to the opening of the bottleneck so as to avoid overflowing the solution, after the solution flows out, slightly lifting the conical flask along the glass rod, standing vertically, enabling a drop of the solution attached to the opening of the conical flask to flow back into the beaker, washing a small amount of the solution in the conical flask with a small amount of more than two-level water for 3-4 times, transferring the washing solution into the volumetric flask according to the method, adding more than two-level water, and diluting to about 3/4 volume, the volumetric flask is horizontally shaken for several times to be primarily mixed, then water of more than two levels is continuously added, the water is carefully added dropwise when the water is close to the marked line until a meniscus of the solution is tangent to the marked line, the stopper is tightly covered, the left index finger presses the stopper, the right finger tip props against the bottom edge of the flask, the volumetric flask is inverted and swirled, the volumetric flask is inverted again, bubbles rise to the top, and the process is repeated for 10-15 times to be mixed uniformly;
step three: optimization of instrument operating conditions
Optimizing the working conditions of the IRIS Intrepid II XSP type inductively coupled plasma atomic emission spectrometer according to the instrument specification, selecting proper measuring conditions such as argon pressure, observation height, analysis line, washing time, integration time and the like, and taking the selected optimized measuring conditions as recommended working parameters-/-
RF power: 1150W; atomizing gas pressure: 0.2 MPa; pump speed: 100 r/min; auxiliary air flow rate: 0.5L/min; plasma torch observation height: 15 mm; integration time: 10 s; argon purity: not less than 99.99%;
step four: detection wavelength selection
After the working conditions of the instrument are optimized according to the instrument specification, in the element measurement wavelength spectral line, comprehensive consideration is carried out according to the detection range, the linear relation, the recovery rate and the accuracy of the detection result, and a proper measurement wavelength is selected, wherein the selected measurement wavelength is as follows:
Sn 189.989{176}nm、189.989{177}nm、、283.999{118}nm；
La 394.910{85}nm、398.852{84}nm、408.672{82}nm；
Ce 413.380{81}nm、413.765{81}nm、418.660{80}nm；
step five: preparation of series calibration curves
The content of the element to be detected in the calibration curve solution is slightly higher than that of the element in the sample, the quantity of the calibration curve solution is determined by the precision requirement, generally 3-5, and the standard solution for drawing the calibration curve is shown in table 2;
table 2 series of calibration solutions for plotting calibration curves
Step six: inductively coupled plasma atomic emission spectrometry detection
Measuring the spectral intensity of tin, lanthanum and cerium in a series of calibration curve solutions and a sample solution on an inductively coupled plasma emission spectrometer, repeatedly measuring each solution for 2-3 times, calculating the average value, taking the average value of the spectral intensity minus the average value of the spectral intensity of zero concentration as the ordinate, taking the concentration of the series of calibration curve solutions as the abscissa, respectively drawing the calibration curves of tin, lanthanum and cerium, taking the average value of the spectral intensity of a test solution minus the average value of the spectral intensity of a blank solution as the net spectral intensity, converting the net spectral intensity into the mass concentration of the tin, lanthanum and cerium in the sample solution according to the calibration curve, expressing the mass concentration of the tin, lanthanum and cerium in the sample solution in mg/mL, and converting to obtain the mass fractions w of the tin, lanthanum and cerium in the sampleBIn% by weight, the values are expressed;
step seven: calculation of analysis results
Converting the net spectral intensity into mass concentrations of the tin, the lanthanum and the cerium in the sample solution according to a calibration curve, wherein the mass concentrations are expressed in mg/mL, and the contents of the tin, the lanthanum and the cerium in the sample are expressed by mass fraction wBIn% by weight, the value is calculated according to formula (1):
in the formula:
ρB-the mass concentration of tin, lanthanum and cerium in the test solution is expressed in milligrams per milliliter (mg/mL);
v is the value of the volume of the liquid to be tested in milliliters (mL);
m is the value of the mass of the sample in grams (g).
Claims (1)
1. A method for analyzing the content of multiple elements in a tin-lanthanum-cerium intermediate alloy comprises the following steps:
the method comprises the following steps: reagent preparation
Adding 200mL of pure water into a 500mL beaker, adding hydrochloric acid and nitric acid, and uniformly stirring by using a glass rod;
step two: pretreatment of sample
Weighing 0.1000g of tin-lanthanum-cerium intermediate alloy sample, placing the sample in a 150mL conical flask, adding 30mL of 1+3 mixed salt-nitrate acid, heating at low temperature until the sample is completely dissolved, taking down, cooling to room temperature, transferring into a 100mL volumetric flask, inserting a glass rod into the volumetric flask during the transfer process, enabling the opening of the conical flask to be inclined and tightly close to the glass rod, enabling the solution to slowly flow along the glass rod, enabling the lower end of the glass rod to be close to the inner wall of the bottleneck but not too close to the opening of the bottleneck so as to avoid overflowing the solution, after the solution flows out, slightly lifting the conical flask along the glass rod, standing vertically, enabling a drop of the solution attached to the opening of the conical flask to flow back into the beaker, washing a small amount of the solution in the conical flask with a small amount of more than two-level water for 3-4 times, transferring the washing solution into the volumetric flask according to the method, adding more than two-level water, and diluting to about 3/4 volume, the volumetric flask is horizontally shaken for several times to be primarily mixed, then water of more than two levels is continuously added, the water is carefully added dropwise when the water is close to the marked line until a meniscus of the solution is tangent to the marked line, the stopper is tightly covered, the left index finger presses the stopper, the right finger tip props against the bottom edge of the flask, the volumetric flask is inverted and swirled, the volumetric flask is inverted again, bubbles rise to the top, and the process is repeated for 10-15 times to be mixed uniformly;
step three: optimization of instrument operating conditions
Optimizing the working conditions of the IRIS Intrepid II XSP type inductively coupled plasma atomic emission spectrometer according to the instrument specification, selecting proper measuring conditions such as argon pressure, observation height, analysis line, washing time, integration time and the like, and taking the selected optimized measuring conditions as recommended working parameters-/-
RF power: 1150W; atomizing gas pressure: 0.2 MPa; pump speed: 100 r/min; auxiliary air flow rate: 0.5L/min; plasma torch observation height: 15 mm; integration time: 10 s; argon purity: not less than 99.99%;
step four: detection wavelength selection
After the working conditions of the instrument are optimized according to the instrument specification, in the element measurement wavelength spectral line, comprehensive consideration is carried out according to the detection range, the linear relation, the recovery rate and the accuracy of the detection result, and a proper measurement wavelength is selected, wherein the selected measurement wavelength is as follows:
Sn 189.989{176}nm、189.989{177}nm、、283.999{118}nm；
La 394.910{85}nm、398.852{84}nm、408.672{82}nm；
Ce 413.380{81}nm、413.765{81}nm、418.660{80}nm；
step five: preparation of series calibration curves
The content of the element to be detected in the calibration curve solution is slightly higher than that of the element in the sample, the quantity of the calibration curve solution is determined by the precision requirement, generally 3-5, and the standard solution for drawing the calibration curve is shown in table 2;
table 2 series of calibration solutions for plotting calibration curves
Step six: inductively coupled plasma atomic emission spectrometry detection
Measuring the spectral intensity of tin, lanthanum and cerium in a series of calibration curve solutions and a sample solution on an inductively coupled plasma emission spectrometer, repeatedly measuring each solution for 2-3 times, calculating the average value of the measured spectral intensities, taking the average value of the spectral intensities minus the average value of the zero concentration spectral intensity as the ordinate, taking the concentration of the series of calibration curve solutions as the abscissa, and respectively drawing the tin, lanthanum and ceriumAnd calculating a calibration curve of cerium, wherein the average value of the spectral intensity of the test solution minus the average value of the spectral intensity of the blank solution is the net spectral intensity, the net spectral intensity is converted into the mass concentration of tin, lanthanum and cerium in the sample solution according to the calibration curve, the mass concentration is expressed in mg/mL, and the contents of tin, lanthanum and cerium in the sample are obtained through conversion according to the mass fraction wBIn% by weight, the values are expressed;
step seven: calculation of analysis results
Converting the net spectral intensity into mass concentrations of the tin, the lanthanum and the cerium in the sample solution according to a calibration curve, wherein the mass concentrations are expressed in mg/mL, and the contents of the tin, the lanthanum and the cerium in the sample are expressed by mass fraction wBIn% by weight, the value is calculated according to formula (1):
in the formula:
ρB-the mass concentration of tin, lanthanum and cerium in the test solution is expressed in milligrams per milliliter (mg/mL);
v is the value of the volume of the liquid to be tested in milliliters (mL);
m is the value of the mass of the sample in grams (g).
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