CN103954610A - Method for measuring arsenic in high-chromium high-nickel steel - Google Patents
Method for measuring arsenic in high-chromium high-nickel steel Download PDFInfo
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Abstract
The invention belongs to analysis technologies for low-content elements in alloy, and relates to an analysis method for measuring arsenic in high-chromium high-nickel steel. The method comprises: adding 5 mL-15 mL of hydrochloric acid, 3 mL-8 mL of nitric acid and 10 drops-30 drops of hydrofluoric acid, heating and dissolving a sample. According to the method, hydrofluoric acid is employed for dissolve the sample, so that a clear sample solution is obtained; by performing interference experiments, an optimum analysis spectral line is determined, and the measuring accuracy is improved; the method is wide in measure scope, the measure lower limit is 0.01%, and the measure upper limit is 0.50%; by synchronously processing the sample and preparing a high-standard solution and a low-standard solution for measuring arsenic element, the analysis error is minimum and the method is good in repeatability; the recovery rate and the precision degree are relatively good; results obtained through analysis on a standard sample, method reviewing and the like are compared and indicate that the made analysis method is good in accuracy and the method is stable and completely accords with requirements on low-content element analysis; and the method disclosed by the invention is rapid in measure and simple in operation and helps to save a large amount of manpower and material resource.
Description
Technical field
The invention belongs to alloy Minor element analytical technology, relate to a kind of analytical approach of measuring arsenic in high-chromium-nickel steel.
Background technology
Steel is taking iron as essential element, and carbon content contains other elements conventionally when as follows 2%.High-chromium-nickel steel is because it is containing having an appointment 24% nickel element, and approximately 25% chromium element makes it have high intensity, corrosion resistivity and toughness.Again because the reliable performance of its cheap price becomes one of maximum material of current use, it is building industry, manufacturing industry and the people indispensable part in life that rises day.
At present, method be can find to arsenic in composition of steel both at home and abroad and arsenic iodide extraction molybdenum blue spectrophotometry, diethyl amino dithioacid silver photometry, separated photometry, graphite electrode atomic absorption spectrometry, the sub-refreshing acidimetry of metallic arsenic separation, potentiometric titration, sodium hypophosphite reduction-iodometric determination arsenic amount etc. mostly are, these method operation stepss are many, labour intensity is large, take tediously longly, be unfavorable for Fast Measurement; Simultaneously, in steel, alloying element is widely different, in method introduction, do not relate to the interference problem of essential element to element to be measured in high chrome high-nickel Steel material, if adopt said method to need lot of experiments checking, be not therefore suitable for the analysis needs of arsenic element in high-chromium-nickel steel.
The feature that inductively coupled plasma atomic emission spectrometer (ICP) analysis has accurately, quick, multielement is analyzed simultaneously; be widely used in the fields such as geology, metallurgy, machine-building, environmental protection, biomedicine, food; there is good detection limit and analytical precision; matrix disturbs little; linear dynamic range is wide; can be mixed with a series of standard with primary standard substance, and the advantage such as sample pretreating is easy.
The means that arsenic element is measured have photometry, volumetric method, potentiometric titration etc. conventionally.Can find corresponding analytical approach for the different-alloy trade mark, about the analysis of arsenic in high-chromium-nickel steel, at present both at home and abroad all without the inductively coupled plasma method of this alloy arsenic element of accurate analysis, substantially be all to apply mechanically steel or other alloy methods, using method exists that sample dissolves, the selection of analytical line is uncertain etc. causes analytical cycle longer, produces the shortcomings such as certain analytical error.
Summary of the invention
The object of the invention is: propose that a kind of analytical element content is lower, wide ranges, the analytical approach of arsenic element in the mensuration high-chromium-nickel steel of arsenic analysis of can accurately carrying out.
Technical scheme of the present invention is: adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 0.95～1.5Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 13～20L/min; Assisted gas flow: 1.0L/min; Pump speed: rinse pump speed 110～190rpm; Analyze pump speed 110～190rpm; Ultraviolet integral time: 2～10s;
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrofluorite, ρ 1.15g/mL; Top grade is pure;
(1.4), sulfuric acid, ρ 1.84g/mL; Top grade is pure;
(1.5), hydrochloric acid, 1+1;
(1.6), sulfuric acid, 1+1;
(1.7), sodium hydroxide solution, 200g/L;
(1.8), arsenic standard solution A:1.00mg/mL; Take 0.1320g standard reagent arsenic trioxide, be placed in 100mL beaker, slowly add 10mL nitric acid (1.2), heating for dissolving, after all dissolving, add 2mL sulfuric acid (1.6), slowly heating, and evaporation is removed after most of nitric acid, move to high temperature place and emit sulfuric acid cigarette, take off slightly coldly, rinse surface plate and wall of cup with water, heating is smoldered again, take off slightly cold, add about 10mL water, heating for dissolving salt, takes off after molten until complete, be cooled to room temperature, move in 100mL volumetric flask, be diluted with water to scale, shake up;
(1.9), arsenic standard solution B:0.10mg/mL; Pipette 20.00mL arsenic standard solution A (1.7), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), arsenic standard solution C:0.01mg/mL; Pipette 20.00mL arsenic standard solution B (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.11), aluminum standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 300mL beaker, adds 30mL hydrochloric acid (1.5), is heated to aluminium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.12), cobalt standard solution 1.00mg/mL; Take 1.0000g; The pure cobalt of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine copper, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.14), niobium standard solution 1.00mg/mL; Take 0.5000g; The pure niobium of > 99.99%, be placed in 300mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 5mL nitric acid (1.2), drip 5mL hydrofluorite (1.5), being heated to niobium dissolves completely, in cooling rear immigration 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.15), titanium standard solution 1.00mg/mL; Take 0.5000g; The pure titanium of > 99.99%, is placed in 300mL beaker, adds 40mL sulfuric acid (1.6), is heated to titanium and dissolves completely, drip 5 nitric acid (1.2), blow water, heating for dissolving salt, in cooling rear immigration 500mL volumetric flask, be diluted with water to scale, mix;
(1.16), vanadium standard solution 1.00mg/mL; Take 1.0000g; The pure vanadium of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to vanadium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.17), tungsten standard solution 1.00mg/mL; Take the specpure tungstic acid of 0.6305g, at 800 DEG C of calcination 30min, be placed in polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, add 10mL sodium hydroxide solution (1.7), heating for dissolving.Be cooled to room temperature, move in 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.18), zirconium standard solution 0.50mg/mL; Take 0.1351g; High-purity zirconium dioxide, be placed in 50mL platinum ware, add 5mL hydrofluorite, low-temperature heat to zirconium dioxide dissolves completely, adds 10mL sulfuric acid (1.6) after cooling, heating evaporation is to emitting sulfuric acid cigarette, add a small amount of water, heating for dissolving salt, in cooling rear immigration 200mL volumetric flask, be diluted with water to scale, mix;
(1.19), silicon standard solution 0.5mg/mL; Take 1.012g; Sodium silicate, is placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, and water dissolves; Add 2mL NaOH (1.7), move in 200mL plastics volumetric flask, be diluted with water to scale, mix;
(1.20), phosphorus standard solution 0.10mg/mL; Take 0.4394g; At 105 DEG C-110 DEG C spectroscopic pure potassium dihydrogen phosphates that toast and be cooled to room temperature in exsiccator, be placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, dissolve by suitable quantity of water, move in 1000mL volumetric flask, be diluted with water to scale, mix;
(1.21), manganese standard solution 5.00mg/mL; Take 1.0000g; The pure manganese of > 99.99%, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to manganese and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.22), molybdenum standard solution 5.00mg/mL; Take 1.0000g; The pure molybdenum of > 99.99%, is placed in 400mL beaker, is blown into 10mL hydrochloric acid (1.1), and 5mL nitric acid (1.2), is heated to molybdenum and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.23), nickel standard solution 10.00mg/mL; Take 2.0000g; > 99.99% pure nickel, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to nickel and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.24), chromium standard solution 10.00mg/mL; Take 2.0000g; The pure chromium of > 99.99%, is placed in 400mL beaker, adds 40mL hydrochloric acid (1.5), is heated to chromium and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.25), iron-based liquid solution: 20.0mg/mL; Take 20.00g, > 99.99% pure iron, is placed in 500mL beaker, add 20mL water 20mL hydrochloric acid (1.5), low-temperature heat is to dissolving completely, in cooling rear immigration 1000mL volumetric flask, add hydrochloric acid 160mL(1.5), be diluted with water to scale, shake up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3), element analysis spectrum line is selected:
Prepare serial single solution, 15.0mL iron-based liquid solution (1.25), 10.0mL iron-based liquid solution (1.25), 7.5mL aluminum standard solution (1.11), 1.0mL cobalt standard solution (1.12), 5.0mL copper standard solution (1.13), 5.0mL niobium standard solution (1.14), 2.5mL titanium standard solution (1.15), 2.5mL vanadium standard solution (1.16), 5.0mL tungsten standard solution (1.17), 2.5mL zirconium standard solution (1.18), 15.0mL silicon standard solution (1.19), 1.5mL phosphorus standard solution (1.20), 5.0mL manganese standard solution (1.21), 4.0mL molybdenum standard solution (1.22), 12.5mL nickel standard solution (1.23), 12.5mL chromium standard solution (1.24), 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 2mL hydrofluorite (1.3), respectively in 50mL plastics volumetric flask, carry out above-mentioned solution respectively spectrogram scanning on the analysis spectral line of 4 arsenic, stack, therefrom Analysis on Selecting signal is strong, matrix, coexistence elements disturb minimum analytical line as separated time spectral line,
(4), sample solubility test
A. take three parts, 0.50g sample, add respectively 5mL hydrochloric acid (1.1) and 2mL nitric acid (1.2), 10mL hydrochloric acid (1.1) and 4mL nitric acid (1.2), 15mL hydrochloric acid (1.1) and 6mL nitric acid (1.2) to heat on electric furnace, sample dissolves not exclusively, has black insolubles in solution;
B. take three parts, 0.50g sample, add respectively 1. 5mL hydrochloric acid (1.1), 3mL nitric acid (1.2) and 10 hydrofluorite (1.3); 2. 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 20 hydrofluorite (1.3); 3. 15mL hydrochloric acid (1.1), 8mL nitric acid (1.2) and 30 hydrofluorite (1.3), sample dissolves completely, solution clarification;
(5), matrix interference, working curve linear test
A. prepare reagent blank working curve: get six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 2.50mL and 5.00mL arsenic standard solution (1.10), 2.50mL arsenic standard solution (1.9), 0.50mL, 1.00mL and 2.50mL arsenic standard solution (1.8) at first again, be diluted with water to scale, shake up;
B. prepare ferrous substrates working curve: get in addition six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) and 15.0mL iron-based liquid solution (1.25) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 2.50mL and 5.00mL arsenic standard solution (1.10), 2.50mL arsenic standard solution (1.9), 0.50mL, 1.00mL and 2.50mL arsenic standard solution (1.8) at first again, be diluted with water to scale, shake up;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.50g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, adopt 4(b) sample dissolution mechanism, add 5mL～15mL hydrochloric acid (1.1), 3mL～8mL nitric acid (1.2), 10～30 hydrofluorite (1.3), on electric hot plate, low-grade fever to test portion dissolves completely; Take off slightly coldly from electric hot plate, blow water walls of beaker, liquor capacity keeps about 30mL, boils dissolved salts; Cooling test solution is to room temperature; Move in 50mL volumetric flask, be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
Adopt (5) b to prepare point in ferrous substrates working curve respectively as low mark solution and high standard solution; Taking do not add arsenic standard solution a bit as low mark solution, other each points can be according to sample content range as high standard solution; Require high standard solution point must cover arsenic element analyst coverage in sample;
(6.4), measure the concentration of arsenic in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of arsenic in sample solution, draw arsenic percentage composition.
Prepare low, high standard solution or use the approaching standard model of chemical composition, after processing according to (6.1)～(6.3), be mixed with needed low, high standard solution.
Advantage of the present invention is:
1) sample preparation technology is one of advantage of the present invention, and the present invention adopts and adds 5mL～15mL hydrochloric acid (1.1), 3mL～8mL nitric acid (1.2), 10～30 hydrofluorite (1.3), and heating, dissolves sample.The present invention is dissolved sample with hydrofluorite, to obtain the sample solution of clarification;
2) by carrying out interference experiment, determine optimized analysis spectral line, improved the accuracy of measuring;
3) method measurement range is wide, and it is 0.01% that measurement is rolled off the production line, and is limited to 0.50% in measurement;
4) adopt synchronous processing sample and prepare high and low mark solution and measure arsenic element, analytical error minimum, method is reproducible;
5) addition 0.10%-0.30%, recovery 98.0%-101.0%, relative standard deviation is less than 1.5%, and the recovery, precision are better;
6) show that by the analysis result such as analysis, the method reinspection comparison of standard model made fixed analytical approach accuracy is good, method is stable, meets the requirement that low secondary element is analyzed completely;
7) the inventive method is measured fast, easy and simple to handle, has saved a large amount of man power and materials.
Embodiment
Embodiment mono-
Measure arsenic content in high-chromium-nickel steel, adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 1.05Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 15L/min; Assisted gas flow: 1.0L/min; Pump speed: rinse pump speed 110rpm; Analyze pump speed 110rpm; Ultraviolet integral time: 5s;
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrofluorite, ρ 1.15g/mL; Top grade is pure;
(1.4), sulfuric acid, ρ 1.84g/mL; Top grade is pure;
(1.5), hydrochloric acid, 1+1;
(1.6), sulfuric acid, 1+1;
(1.7), sodium hydroxide solution, 200g/L;
(1.8), arsenic standard solution A:1.00mg/mL; Take 0.1320g standard reagent arsenic trioxide, be placed in 100mL beaker, slowly add 10mL nitric acid (1.2), heating for dissolving, after all dissolving, add 2mL sulfuric acid (1.6), slowly heating, and evaporation is removed after most of nitric acid, move to high temperature place and emit sulfuric acid cigarette, take off slightly coldly, rinse surface plate and wall of cup with water, heating is smoldered again, take off slightly cold, add about 10mL water, heating for dissolving salt, takes off after molten until complete, be cooled to room temperature, move in 100mL volumetric flask, be diluted with water to scale, shake up;
(1.9), arsenic standard solution B:0.10mg/mL; Pipette 20.00mL arsenic standard solution A (1.7), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), arsenic standard solution C:0.01mg/mL; Pipette 20.00mL arsenic standard solution B (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.11), aluminum standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 300mL beaker, adds 30mL hydrochloric acid (1.5), is heated to aluminium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.12), cobalt standard solution 1.00mg/mL; Take 1.0000g; The pure cobalt of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine copper, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.14), niobium standard solution 1.00mg/mL; Take 0.5000g; The pure niobium of > 99.99%, be placed in 300mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 5mL nitric acid (1.2), drip 5mL hydrofluorite (1.5), being heated to niobium dissolves completely, in cooling rear immigration 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.15), titanium standard solution 1.00mg/mL; Take 0.5000g; The pure titanium of > 99.99%, is placed in 300mL beaker, adds 40mL sulfuric acid (1.6), is heated to titanium and dissolves completely, drip 5 nitric acid (1.2), blow water, heating for dissolving salt, in cooling rear immigration 500mL volumetric flask, be diluted with water to scale, mix;
(1.16), vanadium standard solution 1.00mg/mL; Take 1.0000g; The pure vanadium of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to vanadium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.17), tungsten standard solution 1.00mg/mL; Take the specpure tungstic acid of 0.6305g, at 800 DEG C of calcination 30min, be placed in polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, add 10mL sodium hydroxide solution (1.7), heating for dissolving.Be cooled to room temperature, move in 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.18), zirconium standard solution 0.50mg/mL; Take 0.1351g; High-purity zirconium dioxide, be placed in 50mL platinum ware, add 5mL hydrofluorite, low-temperature heat to zirconium dioxide dissolves completely, adds 10mL sulfuric acid (1.6) after cooling, heating evaporation is to emitting sulfuric acid cigarette, add a small amount of water, heating for dissolving salt, in cooling rear immigration 200mL volumetric flask, be diluted with water to scale, mix;
(1.19), silicon standard solution 0.5mg/mL; Take 1.012g; Sodium silicate, is placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, and water dissolves; Add 2mL NaOH (1.7), move in 200mL plastics volumetric flask, be diluted with water to scale, mix;
(1.20), phosphorus standard solution 0.10mg/mL; Take 0.4394g; At 105 DEG C-110 DEG C spectroscopic pure potassium dihydrogen phosphates that toast and be cooled to room temperature in exsiccator, be placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, dissolve by suitable quantity of water, move in 1000mL volumetric flask, be diluted with water to scale, mix;
(1.21), manganese standard solution 5.00mg/mL; Take 1.0000g; The pure manganese of > 99.99%, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to manganese and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.22), molybdenum standard solution 5.00mg/mL; Take 1.0000g; The pure molybdenum of > 99.99%, is placed in 400mL beaker, is blown into 10mL hydrochloric acid (1.1), and 5mL nitric acid (1.2), is heated to molybdenum and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.23), nickel standard solution 10.00mg/mL; Take 2.0000g; > 99.99% pure nickel, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to nickel and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.24), chromium standard solution 10.00mg/mL; Take 2.0000g; The pure chromium of > 99.99%, is placed in 400mL beaker, adds 40mL hydrochloric acid (1.5), is heated to chromium and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.25), iron-based liquid solution: 20.0mg/mL; Take 20.00g, > 99.99% pure iron, is placed in 500mL beaker, add 20mL water 20mL hydrochloric acid (1.5), low-temperature heat is to dissolving completely, in cooling rear immigration 1000mL volumetric flask, add hydrochloric acid 160mL(1.5), be diluted with water to scale, shake up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3), element analysis spectrum line is selected:
Prepare serial single solution, 15.0mL iron-based liquid solution (1.25), 10.0mL iron-based liquid solution (1.25), 7.5mL aluminum standard solution (1.11), 1.0mL cobalt standard solution (1.12), 5.0mL copper standard solution (1.13), 5.0mL niobium standard solution (1.14), 2.5mL titanium standard solution (1.15), 2.5mL vanadium standard solution (1.16), 5.0mL tungsten standard solution (1.17), 2.5mL zirconium standard solution (1.18), 15.0mL silicon standard solution (1.19), 1.5mL phosphorus standard solution (1.20), 5.0mL manganese standard solution (1.21), 4.0mL molybdenum standard solution (1.22), 12.5mL nickel standard solution (1.23), 12.5mL chromium standard solution (1.24), 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 2mL hydrofluorite (1.3) are respectively in 50mL plastics volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 4 arsenic to spectrogram scanning, stack, therefrom choose 197.262 ﹛ 170 ﹜ nm as separated time spectral line,
(4), sample solubility test
A. take three parts, 0.50g sample, add respectively 5mL hydrochloric acid (1.1) and 2mL nitric acid (1.2), 10mL hydrochloric acid (1.1) and 4mL nitric acid (1.2), 15mL hydrochloric acid (1.1) and 6mL nitric acid (1.2) to heat on electric furnace, sample dissolves not exclusively, has black insolubles in solution;
B. take three parts, 0.50g sample, add respectively 1. 5mL hydrochloric acid (1.1), 3mL nitric acid (1.2) and 10 hydrofluorite (1.3); 2. 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 20 hydrofluorite (1.3); 3. 15mL hydrochloric acid (1.1), 8mL nitric acid (1.2) and 30 hydrofluorite (1.3), sample dissolves completely, solution clarification;
(5), matrix interference, working curve linear test
A. prepare reagent blank working curve; Get six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 2.50mL, 5.00mL, 7.50mL, 10.00mL and 15.00mL arsenic standard solution (1.10) to be diluted with water to scale at first again, shake up;
B. prepare ferrous substrates working curve; Get in addition six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) and 15.0mL iron-based liquid solution (1.25) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 2.50mL, 5.00mL, 7.50mL, 10.00mL and 15.00mL arsenic standard solution (1.10) at first again, be diluted with water to scale, shake up;
Research shows, containing ferro element in iron-based body running curve has inhibiting effect to the measurement of arsenic, and calibration curve should adopt iron Matrix Match; Working curve is linear, and related coefficient is 0.999916;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.50g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 5mL hydrochloric acid (1.1), 8mL nitric acid (1.2), 30 hydrofluorite (1.3), on electric hot plate, low-grade fever to test portion dissolves completely; Take off slightly coldly from electric hot plate, blow water walls of beaker, liquor capacity keeps about 30mL, boils dissolved salts; Cooling test solution is to room temperature; Move in 50mL volumetric flask, be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
(6.3.1), prepare low mark solution; Prepare low mark solution by main chemical compositions in tested high chrome high-nickel steel as follows; Pipette 15.00mL iron-based liquid solution (1.25) in 50mL plastics volumetric flask, 5mL hydrochloric acid (1.1), 8mL nitric acid (1.2), 30 hydrofluorite (1.3), be diluted with water to scale, shakes up, as low mark solution;
(6.3.2), prepare high standard solution; As follows by main chemical compositions preparation high standard solution in tested high chrome high-nickel steel; Pipette 15.00mL iron-based liquid solution (1.25) in 50mL volumetric flask, 5mL hydrochloric acid (1.1), 8mL nitric acid (1.2), 30 hydrofluorite (1.3), accurately add respectively 0.00mL, 2.50mL, 5.00mL, 7.50mL, 10.00mL and 15.00mL arsenic standard solution (1.10), be diluted with water to scale, shake up, as high standard solution;
(6.5), measure the concentration of arsenic in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of arsenic in sample solution, the content that obtains arsenic is 0.0103%.
Embodiment bis-
Measure arsenic content in high-chromium-nickel steel, adopt inductively coupled plasma instrument, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 1.0Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 16L/min; Assisted gas flow: 1.0L/min; Pump speed: rinse pump speed 130rpm; Analyze pump speed 130rpm; Ultraviolet integral time: 2s; Ultimate analysis line: arsenic 197.262 ﹛ 170 ﹜ nm.
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrofluorite, ρ 1.15g/mL; Top grade is pure;
(1.4), sulfuric acid, ρ 1.84g/mL; Top grade is pure;
(1.5), hydrochloric acid, 1+1;
(1.6), sulfuric acid, 1+1;
(1.7), sodium hydroxide solution, 200g/L;
(1.8), arsenic standard solution A:1.00mg/mL; Take 0.1320g standard reagent arsenic trioxide, be placed in 100mL beaker, slowly add 10mL nitric acid (1.2), heating for dissolving, after all dissolving, add 2mL sulfuric acid (1.6), slowly heating, and evaporation is removed after most of nitric acid, move to high temperature place and emit sulfuric acid cigarette, take off slightly coldly, rinse surface plate and wall of cup with water, heating is smoldered again, take off slightly cold, add about 10mL water, heating for dissolving salt, takes off after molten until complete, be cooled to room temperature, move in 100mL volumetric flask, be diluted with water to scale, shake up;
(1.9), arsenic standard solution B:0.10mg/mL; Pipette 20.00mL arsenic standard solution A (1.7), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), arsenic standard solution C:0.01mg/mL; Pipette 20.00mL arsenic standard solution B (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.11), aluminum standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 300mL beaker, adds 30mL hydrochloric acid (1.5), is heated to aluminium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.12), cobalt standard solution 1.00mg/mL; Take 1.0000g; The pure cobalt of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine copper, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.14), niobium standard solution 1.00mg/mL; Take 0.5000g; The pure niobium of > 99.99%, be placed in 300mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 5mL nitric acid (1.2), drip 5mL hydrofluorite (1.5), being heated to niobium dissolves completely, in cooling rear immigration 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.15), titanium standard solution 1.00mg/mL; Take 0.5000g; The pure titanium of > 99.99%, is placed in 300mL beaker, adds 40mL sulfuric acid (1.6), is heated to titanium and dissolves completely, drip 5 nitric acid (1.2), blow water, heating for dissolving salt, in cooling rear immigration 500mL volumetric flask, be diluted with water to scale, mix;
(1.16), vanadium standard solution 1.00mg/mL; Take 1.0000g; The pure vanadium of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to vanadium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.17), tungsten standard solution 1.00mg/mL; Take the specpure tungstic acid of 0.6305g, at 800 DEG C of calcination 30min, be placed in polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, add 10mL sodium hydroxide solution (1.7), heating for dissolving.Be cooled to room temperature, move in 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.18), zirconium standard solution 0.50mg/mL; Take 0.1351g; High-purity zirconium dioxide, be placed in 50mL platinum ware, add 5mL hydrofluorite, low-temperature heat to zirconium dioxide dissolves completely, adds 10mL sulfuric acid (1.6) after cooling, heating evaporation is to emitting sulfuric acid cigarette, add a small amount of water, heating for dissolving salt, in cooling rear immigration 200mL volumetric flask, be diluted with water to scale, mix;
(1.19), silicon standard solution 0.5mg/mL; Take 1.012g; Sodium silicate, is placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, and water dissolves; Add 2mL NaOH (1.7), move in 200mL plastics volumetric flask, be diluted with water to scale, mix;
(1.20), phosphorus standard solution 0.10mg/mL; Take 0.4394g; At 105 DEG C-110 DEG C spectroscopic pure potassium dihydrogen phosphates that toast and be cooled to room temperature in exsiccator, be placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, dissolve by suitable quantity of water, move in 1000mL volumetric flask, be diluted with water to scale, mix;
(1.21), manganese standard solution 5.00mg/mL; Take 1.0000g; The pure manganese of > 99.99%, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to manganese and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.22), molybdenum standard solution 5.00mg/mL; Take 1.0000g; The pure molybdenum of > 99.99%, is placed in 400mL beaker, is blown into 10mL hydrochloric acid (1.1), and 5mL nitric acid (1.2), is heated to molybdenum and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.23), nickel standard solution 10.00mg/mL; Take 2.0000g; > 99.99% pure nickel, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to nickel and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.24), chromium standard solution 10.00mg/mL; Take 2.0000g; The pure chromium of > 99.99%, is placed in 400mL beaker, adds 40mL hydrochloric acid (1.5), is heated to chromium and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.25), iron-based liquid solution: 20.0mg/mL; Take 20.00g, > 99.99% pure iron, is placed in 500mL beaker, add 20mL water 20mL hydrochloric acid (1.5), low-temperature heat is to dissolving completely, in cooling rear immigration 1000mL volumetric flask, add hydrochloric acid 160mL(1.5), be diluted with water to scale, shake up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3), element analysis spectrum line is selected:
Prepare serial single solution, 15.0mL iron-based liquid solution (1.25), 10.0mL iron-based liquid solution (1.25), 7.5mL aluminum standard solution (1.11), 1.0mL cobalt standard solution (1.12), 5.0mL copper standard solution (1.13), 5.0mL niobium standard solution (1.14), 2.5mL titanium standard solution (1.15), 2.5mL vanadium standard solution (1.16), 5.0mL tungsten standard solution (1.17), 2.5mL zirconium standard solution (1.18), 15.0mL silicon standard solution (1.19), 1.5mL phosphorus standard solution (1.20), 5.0mL manganese standard solution (1.21), 4.0mL molybdenum standard solution (1.22), 12.5mL nickel standard solution (1.23), 12.5mL chromium standard solution (1.24), 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 2mL hydrofluorite (1.3) are respectively in 50mL plastics volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 4 arsenic to spectrogram scanning, stack, therefrom choose 197.262 ﹛ 170 ﹜ nm as separated time spectral line,
(4), sample solubility test
A. take three parts, 0.50g sample, add respectively 5mL hydrochloric acid (1.1) and 2mL nitric acid (1.2), 10mL hydrochloric acid (1.1) and 4mL nitric acid (1.2), 15mL hydrochloric acid (1.1) and 6mL nitric acid (1.2) to heat on electric furnace, sample dissolves not exclusively, has black insolubles in solution;
B. take three parts, 0.50g sample, add respectively 1. 5mL hydrochloric acid (1.1), 3mL nitric acid (1.2) and 10 hydrofluorite (1.3); 2. 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 20 hydrofluorite (1.3); 3. 15mL hydrochloric acid (1.1), 8mL nitric acid (1.2) and 30 hydrofluorite (1.3), sample dissolves completely, solution clarification;
(5), matrix interference, working curve linear test
A. prepare reagent blank working curve; Get six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 0.50mL, 1.00mL, 3.00mL, 4.00mL and 5.00mL arsenic standard solution (1.9) at first again, be diluted with water to scale, shake up;
B. prepare ferrous substrates working curve; Get in addition six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) and 15.0mL iron-based liquid solution (1.25) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 0.50mL, 1.00mL, 3.00mL, 4.00mL and 5.00mL arsenic standard solution (1.9) at first again, be diluted with water to scale, shake up;
Research shows, containing ferro element in iron-based body running curve has inhibiting effect to the measurement of arsenic, and calibration curve should adopt iron Matrix Match; Working curve is linear, and related coefficient is 0.999924;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.50g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 5mL hydrochloric acid (1.1), 8mL nitric acid (1.2), 30 hydrofluorite (1.3), on electric hot plate, low-grade fever to test portion dissolves completely; Take off slightly coldly from electric hot plate, blow water walls of beaker, liquor capacity keeps about 30mL, boils dissolved salts; Cooling test solution is to room temperature; Move in 50mL volumetric flask, be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
(6.3.1), prepare low mark solution; Prepare low mark solution by main chemical compositions in tested high chrome high-nickel steel as follows; Pipette 15.00mL iron-based liquid solution (1.25) in 50mL plastics volumetric flask, 5mL hydrochloric acid (1.1), 8mL nitric acid (1.2), 30 hydrofluorite (1.3), be diluted with water to scale, shakes up, as low mark solution;
(6.3.2), prepare high standard solution; As follows by main chemical compositions preparation high standard solution in tested high chrome high-nickel steel; Pipette 15.00mL iron-based liquid solution (1.25) in 50mL volumetric flask, 5mL hydrochloric acid (1.1), 8mL nitric acid (1.2), 30 hydrofluorite (1.3), accurately add respectively 0.00mL, 0.50mL, 1.00mL, 3.00mL, 4.00mL and 5.00mL arsenic standard solution (1.9), be diluted with water to scale, shake up, as high standard solution;
(6.4), measure the concentration of arsenic in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of arsenic in sample solution, the content that obtains arsenic is 0.048%.
Embodiment tri-
Adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 1.1Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 15L/min; Assisted gas flow: 0.50L/min; Pump speed: rinse pump speed 130rpm; Analyze pump speed 130rpm; Ultraviolet integral time: 6s; Ultimate analysis line: arsenic 197.262 ﹛ 170 ﹜ nm.
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrofluorite, ρ 1.15g/mL; Top grade is pure;
(1.4), sulfuric acid, ρ 1.84g/mL; Top grade is pure;
(1.5), hydrochloric acid, 1+1;
(1.6), sulfuric acid, 1+1;
(1.7), sodium hydroxide solution, 200g/L;
(1.8), arsenic standard solution A:1.00mg/mL; Take 0.1320g standard reagent arsenic trioxide, be placed in 100mL beaker, slowly add 10mL nitric acid (1.2), heating for dissolving, after all dissolving, add 2mL sulfuric acid (1.6), slowly heating, and evaporation is removed after most of nitric acid, move to high temperature place and emit sulfuric acid cigarette, take off slightly coldly, rinse surface plate and wall of cup with water, heating is smoldered again, take off slightly cold, add about 10mL water, heating for dissolving salt, takes off after molten until complete, be cooled to room temperature, move in 100mL volumetric flask, be diluted with water to scale, shake up;
(1.9), arsenic standard solution B:0.10mg/mL; Pipette 20.00mL arsenic standard solution A (1.7), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), arsenic standard solution C:0.01mg/mL; Pipette 20.00mL arsenic standard solution B (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.11), aluminum standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 300mL beaker, adds 30mL hydrochloric acid (1.5), is heated to aluminium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.12), cobalt standard solution 1.00mg/mL; Take 1.0000g; The pure cobalt of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine copper, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.14), niobium standard solution 1.00mg/mL; Take 0.5000g; The pure niobium of > 99.99%, be placed in 300mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 5mL nitric acid (1.2), drip 5mL hydrofluorite (1.5), being heated to niobium dissolves completely, in cooling rear immigration 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.15), titanium standard solution 1.00mg/mL; Take 0.5000g; The pure titanium of > 99.99%, is placed in 300mL beaker, adds 40mL sulfuric acid (1.6), is heated to titanium and dissolves completely, drip 5 nitric acid (1.2), blow water, heating for dissolving salt, in cooling rear immigration 500mL volumetric flask, be diluted with water to scale, mix;
(1.16), vanadium standard solution 1.00mg/mL; Take 1.0000g; The pure vanadium of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to vanadium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.17), tungsten standard solution 1.00mg/mL; Take the specpure tungstic acid of 0.6305g, at 800 DEG C of calcination 30min, be placed in polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, add 10mL sodium hydroxide solution (1.7), heating for dissolving.Be cooled to room temperature, move in 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.18), zirconium standard solution 0.50mg/mL; Take 0.1351g; High-purity zirconium dioxide, be placed in 50mL platinum ware, add 5mL hydrofluorite, low-temperature heat to zirconium dioxide dissolves completely, adds 10mL sulfuric acid (1.6) after cooling, heating evaporation is to emitting sulfuric acid cigarette, add a small amount of water, heating for dissolving salt, in cooling rear immigration 200mL volumetric flask, be diluted with water to scale, mix;
(1.19), silicon standard solution 0.5mg/mL; Take 1.012g; Sodium silicate, is placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, and water dissolves; Add 2mL NaOH (1.7), move in 200mL plastics volumetric flask, be diluted with water to scale, mix;
(1.20), phosphorus standard solution 0.10mg/mL; Take 0.4394g; At 105 DEG C-110 DEG C spectroscopic pure potassium dihydrogen phosphates that toast and be cooled to room temperature in exsiccator, be placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, dissolve by suitable quantity of water, move in 1000mL volumetric flask, be diluted with water to scale, mix;
(1.21), manganese standard solution 5.00mg/mL; Take 1.0000g; The pure manganese of > 99.99%, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to manganese and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.22), molybdenum standard solution 5.00mg/mL; Take 1.0000g; The pure molybdenum of > 99.99%, is placed in 400mL beaker, is blown into 10mL hydrochloric acid (1.1), and 5mL nitric acid (1.2), is heated to molybdenum and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.23), nickel standard solution 10.00mg/mL; Take 2.0000g; > 99.99% pure nickel, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to nickel and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.24), chromium standard solution 10.00mg/mL; Take 2.0000g; The pure chromium of > 99.99%, is placed in 400mL beaker, adds 40mL hydrochloric acid (1.5), is heated to chromium and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.25), iron-based liquid solution: 20.0mg/mL; Take 20.00g, > 99.99% pure iron, is placed in 500mL beaker, add 20mL water 20mL hydrochloric acid (1.5), low-temperature heat is to dissolving completely, in cooling rear immigration 1000mL volumetric flask, add hydrochloric acid 160mL(1.5), be diluted with water to scale, shake up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3), element analysis spectrum line is selected:
Prepare serial single solution, 15.0mL iron-based liquid solution (1.25), 10.0mL iron-based liquid solution (1.25), 7.5mL aluminum standard solution (1.11), 1.0mL cobalt standard solution (1.12), 5.0mL copper standard solution (1.13), 5.0mL niobium standard solution (1.14), 2.5mL titanium standard solution (1.15), 2.5mL vanadium standard solution (1.16), 5.0mL tungsten standard solution (1.17), 2.5mL zirconium standard solution (1.18), 15.0mL silicon standard solution (1.19), 1.5mL phosphorus standard solution (1.20), 5.0mL manganese standard solution (1.21), 4.0mL molybdenum standard solution (1.22), 12.5mL nickel standard solution (1.23), 12.5mL chromium standard solution (1.24), 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 2mL hydrofluorite (1.3) are respectively in 50mL plastics volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 4 arsenic to spectrogram scanning, stack, therefrom choose 197.262 ﹛ 170 ﹜ nm as separated time spectral line,
(4), sample solubility test
A. take three parts, 0.50g sample, add respectively 5mL hydrochloric acid (1.1) and 2mL nitric acid (1.2), 10mL hydrochloric acid (1.1) and 4mL nitric acid (1.2), 15mL hydrochloric acid (1.1) and 6mL nitric acid (1.2) to heat on electric furnace, sample dissolves not exclusively, has black insolubles in solution;
B. take three parts, 0.50g sample, add respectively 1. 5mL hydrochloric acid (1.1), 3mL nitric acid (1.2) and 10 hydrofluorite (1.3); 2. 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 20 hydrofluorite (1.3); 3. 15mL hydrochloric acid (1.1), 8mL nitric acid (1.2) and 30 hydrofluorite (1.3), sample dissolves completely, solution clarification;
(5), matrix interference, working curve linear test
A. prepare reagent blank working curve; Get six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 1.00mL, 3.00mL, 5.00mL, 7.00mL and 10.00mL arsenic standard solution (1.9) at first again, be diluted with water to scale, shake up;
B. prepare ferrous substrates working curve; Get in addition six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) and 15.0mL iron-based liquid solution (1.25) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 1.00mL, 3.00mL, 5.00mL, 7.00mL and 10.00mL arsenic standard solution (1.9) at first again, be diluted with water to scale, shake up;
Research shows, containing ferro element in iron-based body running curve has inhibiting effect to the measurement of arsenic, and calibration curve should adopt iron Matrix Match; Working curve is linear, and related coefficient is 0.999849;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.50g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 10 hydrofluorite (1.3), on electric hot plate, low-grade fever to test portion dissolves completely; Take off slightly coldly from electric hot plate, blow water walls of beaker, liquor capacity keeps about 30mL, boils dissolved salts; Cooling test solution is to room temperature; Move in 50mL volumetric flask, be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
(6.3.1), prepare low mark solution; Prepare low mark solution by main chemical compositions in tested high chrome high-nickel steel as follows; Pipette 15.00mL iron-based liquid solution (1.25) in 50mL plastics volumetric flask, 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 10 hydrofluorite (1.3), be diluted with water to scale, shakes up, as low mark solution;
(6.3.2), prepare high standard solution; As follows by main chemical compositions preparation high standard solution in tested high chrome high-nickel steel; Pipette 15.00mL iron-based liquid solution (1.25) in 50mL volumetric flask, 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 10 hydrofluorite (1.3), 10.00mL arsenic standard solution (1.9), is diluted with water to scale, shake up, as high standard solution;
(6.4), measure the concentration of arsenic in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of arsenic in sample solution, computation and measurement result, the content that obtains arsenic is 0.090%.
Embodiment tetra-
Adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 1.15Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 15L/min; Assisted gas flow: 0.5L/min; Pump speed: rinse pump speed 160rpm; Analyze pump speed 160rpm; Ultraviolet integral time: 10s; Ultimate analysis line: arsenic 197.262 ﹛ 170 ﹜ nm.
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrofluorite, ρ 1.15g/mL; Top grade is pure;
(1.4), sulfuric acid, ρ 1.84g/mL; Top grade is pure;
(1.5), hydrochloric acid, 1+1;
(1.6), sulfuric acid, 1+1;
(1.7), sodium hydroxide solution, 200g/L;
(1.8), arsenic standard solution A:1.00mg/mL; Take 0.1320g standard reagent arsenic trioxide, be placed in 100mL beaker, slowly add 10mL nitric acid (1.2), heating for dissolving, after all dissolving, add 2mL sulfuric acid (1.6), slowly heating, and evaporation is removed after most of nitric acid, move to high temperature place and emit sulfuric acid cigarette, take off slightly coldly, rinse surface plate and wall of cup with water, heating is smoldered again, take off slightly cold, add about 10mL water, heating for dissolving salt, takes off after molten until complete, be cooled to room temperature, move in 100mL volumetric flask, be diluted with water to scale, shake up;
(1.9), arsenic standard solution B:0.10mg/mL; Pipette 20.00mL arsenic standard solution A (1.7), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), arsenic standard solution C:0.01mg/mL; Pipette 20.00mL arsenic standard solution B (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.11), aluminum standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 300mL beaker, adds 30mL hydrochloric acid (1.5), is heated to aluminium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.12), cobalt standard solution 1.00mg/mL; Take 1.0000g; The pure cobalt of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine copper, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.14), niobium standard solution 1.00mg/mL; Take 0.5000g; The pure niobium of > 99.99%, be placed in 300mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 5mL nitric acid (1.2), drip 5mL hydrofluorite (1.5), being heated to niobium dissolves completely, in cooling rear immigration 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.15), titanium standard solution 1.00mg/mL; Take 0.5000g; The pure titanium of > 99.99%, is placed in 300mL beaker, adds 40mL sulfuric acid (1.6), is heated to titanium and dissolves completely, drip 5 nitric acid (1.2), blow water, heating for dissolving salt, in cooling rear immigration 500mL volumetric flask, be diluted with water to scale, mix;
(1.16), vanadium standard solution 1.00mg/mL; Take 1.0000g; The pure vanadium of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to vanadium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.17), tungsten standard solution 1.00mg/mL; Take the specpure tungstic acid of 0.6305g, at 800 DEG C of calcination 30min, be placed in polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, add 10mL sodium hydroxide solution (1.7), heating for dissolving.Be cooled to room temperature, move in 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.18), zirconium standard solution 0.50mg/mL; Take 0.1351g; High-purity zirconium dioxide, be placed in 50mL platinum ware, add 5mL hydrofluorite, low-temperature heat to zirconium dioxide dissolves completely, adds 10mL sulfuric acid (1.6) after cooling, heating evaporation is to emitting sulfuric acid cigarette, add a small amount of water, heating for dissolving salt, in cooling rear immigration 200mL volumetric flask, be diluted with water to scale, mix;
(1.19), silicon standard solution 0.5mg/mL; Take 1.012g; Sodium silicate, is placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, and water dissolves; Add 2mL NaOH (1.7), move in 200mL plastics volumetric flask, be diluted with water to scale, mix;
(1.20), phosphorus standard solution 0.10mg/mL; Take 0.4394g; At 105 DEG C-110 DEG C spectroscopic pure potassium dihydrogen phosphates that toast and be cooled to room temperature in exsiccator, be placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, dissolve by suitable quantity of water, move in 1000mL volumetric flask, be diluted with water to scale, mix;
(1.21), manganese standard solution 5.00mg/mL; Take 1.0000g; The pure manganese of > 99.99%, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to manganese and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.22), molybdenum standard solution 5.00mg/mL; Take 1.0000g; The pure molybdenum of > 99.99%, is placed in 400mL beaker, is blown into 10mL hydrochloric acid (1.1), and 5mL nitric acid (1.2), is heated to molybdenum and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.23), nickel standard solution 10.00mg/mL; Take 2.0000g; > 99.99% pure nickel, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to nickel and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.24), chromium standard solution 10.00mg/mL; Take 2.0000g; The pure chromium of > 99.99%, is placed in 400mL beaker, adds 40mL hydrochloric acid (1.5), is heated to chromium and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.25), iron-based liquid solution: 20.0mg/mL; Take 20.00g, > 99.99% pure iron, is placed in 500mL beaker, add 20mL water 20mL hydrochloric acid (1.5), low-temperature heat is to dissolving completely, in cooling rear immigration 1000mL volumetric flask, add hydrochloric acid 160mL(1.5), be diluted with water to scale, shake up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3), element analysis spectrum line is selected:
Prepare serial single solution, 15.0mL iron-based liquid solution (1.25), 10.0mL iron-based liquid solution (1.25), 7.5mL aluminum standard solution (1.11), 1.0mL cobalt standard solution (1.12), 5.0mL copper standard solution (1.13), 5.0mL niobium standard solution (1.14), 2.5mL titanium standard solution (1.15), 2.5mL vanadium standard solution (1.16), 5.0mL tungsten standard solution (1.17), 2.5mL zirconium standard solution (1.18), 15.0mL silicon standard solution (1.19), 1.5mL phosphorus standard solution (1.20), 5.0mL manganese standard solution (1.21), 4.0mL molybdenum standard solution (1.22), 12.5mL nickel standard solution (1.23), 12.5mL chromium standard solution (1.24), 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 2mL hydrofluorite (1.3) are respectively in 50mL plastics volumetric flask, respectively above-mentioned solution is carried out on the analysis spectral line of 4 arsenic to spectrogram scanning, stack, therefrom choose 197.262 ﹛ 170 ﹜ nm as separated time spectral line,
(4), sample solubility test
A. take three parts, 0.50g sample, add respectively 5mL hydrochloric acid (1.1) and 2mL nitric acid (1.2), 10mL hydrochloric acid (1.1) and 4mL nitric acid (1.2), 15mL hydrochloric acid (1.1) and 6mL nitric acid (1.2) to heat on electric furnace, sample dissolves not exclusively, has black insolubles in solution;
B. take three parts, 0.50g sample, add respectively 1. 5mL hydrochloric acid (1.1), 3mL nitric acid (1.2) and 10 hydrofluorite (1.3); 2. 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 20 hydrofluorite (1.3); 3. 15mL hydrochloric acid (1.1), 8mL nitric acid (1.2) and 30 hydrofluorite (1.3), sample dissolves completely, solution clarification;
(5), matrix interference, working curve linear test
A. prepare reagent blank working curve; Get six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 1.00mL, 1.50mL, 2.00mL, 2.50mL and 3.00mL arsenic standard solution (1.8) at first again, be diluted with water to scale, shake up;
B. prepare ferrous substrates working curve; Get in addition six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) and 15.0mL iron-based liquid solution (1.25) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 1.00mL, 1.50mL, 2.00mL, 2.50mL and 3.00mL arsenic standard solution (1.8) at first again, be diluted with water to scale, shake up;
Research shows, containing ferro element in iron-based body running curve has inhibiting effect to the measurement of arsenic, and calibration curve should adopt iron Matrix Match; Working curve is linear, and related coefficient is 0.999769;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.50g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 10 hydrofluorite (1.3), on electric hot plate, low-grade fever to test portion dissolves completely; Take off slightly coldly from electric hot plate, blow water walls of beaker, liquor capacity keeps about 30mL, boils dissolved salts; Cooling test solution is to room temperature; Move in 50mL volumetric flask, be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
(6.3.1), prepare low mark solution; Prepare low mark solution by main chemical compositions in tested high chrome high-nickel steel as follows; Pipette 15.00mL iron-based liquid solution (1.25) in 50mL plastics volumetric flask, 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 10 hydrofluorite (1.3), be diluted with water to scale, shakes up, as low mark solution;
(6.3.2), prepare high standard solution; Take standard substance 0.50g sample by main chemical compositions in tested high chrome high-nickel steel, be accurate to 0.0001g, be placed in 150mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, carry out sample dissolution according to (6.3), move in 50mL volumetric flask, add 3.00mL arsenic standard solution (1.8), be diluted with water to scale, shake up, as high standard solution;
(6.4), measure the concentration of arsenic in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of arsenic in sample solution, computation and measurement result, the content that obtains arsenic is 0.518%.
Claims (2)
1. an analytical approach of measuring arsenic element in high-chromium-nickel steel, is characterized in that: adopt inductive coupling plasma emission spectrograph, condition of work and the analytical line of instrument are as follows: high frequency frequency: 40.68MHz; Incident power: 0.95～1.5Kw; Reflective power: < 15W; Argon flow amount: cooling gas flow: 13～20L/min; Assisted gas flow: 1.0L/min; Pump speed: rinse pump speed 110～190rpm; Analyze pump speed 110～190rpm; Ultraviolet integral time: 2～10s;
(1) reagent, using in mensuration process is as follows:
(1.1), hydrochloric acid, ρ 1.19g/mL; Top grade is pure;
(1.2), nitric acid, ρ 1.42g/mL; Top grade is pure;
(1.3), hydrofluorite, ρ 1.15g/mL; Top grade is pure;
(1.4), sulfuric acid, ρ 1.84g/mL; Top grade is pure;
(1.5), hydrochloric acid, 1+1;
(1.6), sulfuric acid, 1+1;
(1.7), sodium hydroxide solution, 200g/L;
(1.8), arsenic standard solution A:1.00mg/mL; Take 0.1320g standard reagent arsenic trioxide, be placed in 100mL beaker, slowly add 10mL nitric acid (1.2), heating for dissolving, after all dissolving, add 2mL sulfuric acid (1.6), slowly heating, and evaporation is removed after most of nitric acid, move to high temperature place and emit sulfuric acid cigarette, take off slightly coldly, rinse surface plate and wall of cup with water, heating is smoldered again, take off slightly cold, add about 10mL water, heating for dissolving salt, takes off after molten until complete, be cooled to room temperature, move in 100mL volumetric flask, be diluted with water to scale, shake up;
(1.9), arsenic standard solution B:0.10mg/mL; Pipette 20.00mL arsenic standard solution A (1.7), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.10), arsenic standard solution C:0.01mg/mL; Pipette 20.00mL arsenic standard solution B (1.8), be placed in 200mL volumetric flask, be diluted with water to scale, shake up;
(1.11), aluminum standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine aluminium, is placed in 300mL beaker, adds 30mL hydrochloric acid (1.5), is heated to aluminium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.12), cobalt standard solution 1.00mg/mL; Take 1.0000g; The pure cobalt of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.13), copper standard solution 1.00mg/mL; Take 1.0000g; > 99.99% fine copper, is placed in 300mL beaker, is blown into intermediate water 30mL, adds 30mL nitric acid (1.2), is heated to cobalt and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.14), niobium standard solution 1.00mg/mL; Take 0.5000g; The pure niobium of > 99.99%, be placed in 300mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, add 5mL nitric acid (1.2), drip 5mL hydrofluorite (1.5), being heated to niobium dissolves completely, in cooling rear immigration 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.15), titanium standard solution 1.00mg/mL; Take 0.5000g; The pure titanium of > 99.99%, is placed in 300mL beaker, adds 40mL sulfuric acid (1.6), is heated to titanium and dissolves completely, drip 5 nitric acid (1.2), blow water, heating for dissolving salt, in cooling rear immigration 500mL volumetric flask, be diluted with water to scale, mix;
(1.16), vanadium standard solution 1.00mg/mL; Take 1.0000g; The pure vanadium of > 99.99%, is placed in 300mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to vanadium and dissolves completely, in cooling rear immigration 1000mL volumetric flask, is diluted with water to scale, mixes;
(1.17), tungsten standard solution 1.00mg/mL; Take the specpure tungstic acid of 0.6305g, at 800 DEG C of calcination 30min, be placed in polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, add 10mL sodium hydroxide solution (1.7), heating for dissolving.Be cooled to room temperature, move in 500mL plastics volumetric flask, be diluted with water to scale, mix;
(1.18), zirconium standard solution 0.50mg/mL; Take 0.1351g; High-purity zirconium dioxide, be placed in 50mL platinum ware, add 5mL hydrofluorite, low-temperature heat to zirconium dioxide dissolves completely, adds 10mL sulfuric acid (1.6) after cooling, heating evaporation is to emitting sulfuric acid cigarette, add a small amount of water, heating for dissolving salt, in cooling rear immigration 200mL volumetric flask, be diluted with water to scale, mix;
(1.19), silicon standard solution 0.5mg/mL; Take 1.012g; Sodium silicate, is placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, and water dissolves; Add 2mL NaOH (1.7), move in 200mL plastics volumetric flask, be diluted with water to scale, mix;
(1.20), phosphorus standard solution 0.10mg/mL; Take 0.4394g; At 105 DEG C-110 DEG C spectroscopic pure potassium dihydrogen phosphates that toast and be cooled to room temperature in exsiccator, be placed in 100mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker in advance, dissolve by suitable quantity of water, move in 1000mL volumetric flask, be diluted with water to scale, mix;
(1.21), manganese standard solution 5.00mg/mL; Take 1.0000g; The pure manganese of > 99.99%, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to manganese and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.22), molybdenum standard solution 5.00mg/mL; Take 1.0000g; The pure molybdenum of > 99.99%, is placed in 400mL beaker, adds 10mL hydrochloric acid (1.1), and 5mL nitric acid (1.2), is heated to molybdenum and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.23), nickel standard solution 10.00mg/mL; Take 2.0000g; > 99.99% pure nickel, is placed in 400mL beaker, is blown into intermediate water 20mL, adds 20mL nitric acid (1.2), is heated to nickel and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.24), chromium standard solution 10.00mg/mL; Take 2.0000g; The pure chromium of > 99.99%, is placed in 400mL beaker, adds 40mL hydrochloric acid (1.5), is heated to chromium and dissolves completely, in cooling rear immigration 200mL volumetric flask, is diluted with water to scale, mixes;
(1.25), iron-based liquid solution: 20.0mg/mL; Take 20.00g, > 99.99% pure iron, is placed in 500mL beaker, add 20mL water 20mL hydrochloric acid (1.5), low-temperature heat is to dissolving completely, in cooling rear immigration 1000mL volumetric flask, add hydrochloric acid 160mL(1.5), be diluted with water to scale, shake up;
(2), sampling and sample preparation; The sample of analyzing use samples and sample preparation according to the requirement of HB/Z205;
(3), element analysis spectrum line is selected:
Prepare serial single solution, 15.0mL iron-based liquid solution (1.25), 10.0mL iron-based liquid solution (1.25), 7.5mL aluminum standard solution (1.11), 1.0mL cobalt standard solution (1.12), 5.0mL copper standard solution (1.13), 5.0mL niobium standard solution (1.14), 2.5mL titanium standard solution (1.15), 2.5mL vanadium standard solution (1.16), 5.0mL tungsten standard solution (1.17), 2.5mL zirconium standard solution (1.18), 15.0mL silicon standard solution (1.19), 1.5mL phosphorus standard solution (1.20), 5.0mL manganese standard solution (1.21), 4.0mL molybdenum standard solution (1.22), 12.5mL nickel standard solution (1.23), 12.5mL chromium standard solution (1.24), 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 2mL hydrofluorite (1.3), respectively in 50mL plastics volumetric flask, carry out above-mentioned solution respectively spectrogram scanning on the analysis spectral line of 4 arsenic, stack, therefrom Analysis on Selecting signal is strong, matrix, coexistence elements disturb minimum analytical line as separated time spectral line,
(4), sample solubility test
A. take three parts, 0.50g sample, add respectively 5mL hydrochloric acid (1.1) and 2mL nitric acid (1.2), 10mL hydrochloric acid (1.1) and 4mL nitric acid (1.2), 15mL hydrochloric acid (1.1) and 6mL nitric acid (1.2) to heat on electric furnace, sample dissolves not exclusively, has black insolubles in solution;
B. take three parts, 0.50g sample, add respectively 1. 5mL hydrochloric acid (1.1), 3mL nitric acid (1.2) and 10 hydrofluorite (1.3); 2. 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2) and 20 hydrofluorite (1.3); 3. 15mL hydrochloric acid (1.1), 8mL nitric acid (1.2) and 30 hydrofluorite (1.3), sample dissolves completely, solution clarification;
(5), matrix interference, working curve linear test
A. prepare reagent blank working curve: get six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 2.50mL and 5.00mL arsenic standard solution (1.10), 2.50mL arsenic standard solution (1.9), 0.50mL, 1.00mL and 2.50mL arsenic standard solution (1.8) at first again, be diluted with water to scale, shake up;
B. prepare ferrous substrates working curve: get in addition six 50mL plastics volumetric flasks, to the 6th volumetric flask, add 10mL hydrochloric acid (1.1), 5mL nitric acid (1.2), 20 hydrofluorite (1.3) and 15.0mL iron-based liquid solution (1.25) at first respectively, to the 6th volumetric flask, accurately add respectively 0.00mL, 2.50mL and 5.00mL arsenic standard solution (1.10), 2.50mL arsenic standard solution (1.9), 0.50mL, 1.00mL and 2.50mL arsenic standard solution (1.8) at first again, be diluted with water to scale, shake up;
(6), analytical procedure is as follows:
(6.1), test portion: take 0.50g sample, be accurate to 0.0001g;
(6.2), prepare sample solution: the test portion of analytical procedure (6.1) is placed in to 150mL polytetrafluoroethyl-ne polytetrafluoroethylene beaker, adopt 4(b) sample dissolution mechanism, add 5mL～15mL hydrochloric acid (1.1), 3mL～8mL nitric acid (1.2), 10～30 hydrofluorite (1.3), on electric hot plate, low-grade fever to test portion dissolves completely; Take off slightly coldly from electric hot plate, blow water walls of beaker, liquor capacity keeps about 30mL, boils dissolved salts; Cooling test solution is to room temperature; Move in 50mL volumetric flask, be diluted with water to scale, shake up;
(6.3), preparation calibration solution;
Adopt (5) b to prepare point in ferrous substrates working curve respectively as low mark solution and high standard solution; Taking do not add arsenic standard solution a bit as low mark solution, other each points can be according to sample content range as high standard solution; Require high standard solution point must cover arsenic element analyst coverage in sample;
(6.4), measure the concentration of arsenic in sample solution; Press the selected condition of work of inductively coupled plasma atomic emission spectrometer, adopt successively low mark solution and high standard solution to carry out standardization to instrument, then, measure the concentration of arsenic in sample solution, draw arsenic percentage composition.
2. a kind of method of measuring arsenic in high-chromium-nickel steel according to claim 1, is characterized in that, prepares low, high standard solution or uses the approaching standard model of chemical composition, after processing, is mixed with needed low, high standard solution according to (6.1)～(6.2).
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