CN109211812A - The analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy - Google Patents
The analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy Download PDFInfo
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Abstract
The present invention relates to alloy macroelement analysis technical fields, to solve the problems, such as that it is big to distinguish high cost of determination, analysis time length, error for nickel, phosphorus content in traditional nickel-base alloy, provide the analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy, comprising the following steps: (1) prepared by mother liquor；(2) nickel-silicon nitride: iodine oxidation-dimethylglyoxime spectrophotometry；(3) phosphorus yield: P-Mo blue spectrophotometry.Stability of the present invention is good, chemical analysis favorable reproducibility, and data analysis is influenced small by environment temperature etc.；Analysis method is at low cost, and chemical reagent usage amount is few, and analysis time is few, highly efficient；Analysis result accuracy is high, and error is small.
Description
Technical field
The present invention relates to nickel in alloy macroelement analysis technical field more particularly to a kind of simultaneous determination nickel-base alloy,
The analysis method of phosphorus content.
Background technique
Nickel-base alloy has excellent corrosion resistance, intensity, plasticity and toughness, metallurgical stability, machinability and solderable
Connecing property is widely used in the fields such as aerospace, nuclear power and ship.Metallurgy and manufacturing technology be constantly progressive pushed it is Ni-based
Therefore the development of alloy, the performance that the content of each chemical element directly affects alloy material in nickel-base alloy accurately detect Ni-based
Alloy composition carries out the important guarantee that quality control is nickel-bass alloy material development, application and production.
The content of two kinds of nickel, phosphorus elements in nickel-base alloy is to determine whether nickel-base alloy is used as the necessary of stainless steel base-material
Element is measured, Elements in Nickel-base Alloy analysis measurement mainly has atomic emission spectrometry, atomic absorption spectrography (AAS), spectrophotometric
Method, infrared absorption spectroscopy, the analysis methods such as electrochemical methods, traditional analysis method are surveyed respectively to nickel and phosphorus
It is fixed, there is a large amount of analytical reagents are expended, the disadvantages of analysis time is long, and analytical error is big.
" a kind of analysis method for measuring platinum, palladium content in high temperature alloy ", notification number are disclosed in Chinese patent literature
For CN102435597A, which uses the superalloy coupons of hydrochloric acid, nitric acid, hydrofluoric acid treatment platiniferous, while solving nickel
The problems of dissolution of based alloy sample and analytical element platinum；By progress interference experiment, spectrum analysis, optimal analytical line is had found,
It solves the interference of the multiple elements such as Main elements nickel, tantalum, cobalt in high temperature alloy using the method for exact matching, improves measurement
Accuracy.But this method is not appropriate for the simultaneous determination to nickel, phosphorus content in nickel-base alloy.
Summary of the invention
Nickel in traditional nickel-base alloy, phosphorus content difference cost of determination is high, analysis time is long, error is big in order to overcome by the present invention
The problem of, the analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy is provided, the use of chemical reagent is greatly reduced
Amount reduces analysis cost and analysis time, provides foundation for nickel, P elements analysis in nickel-base alloy.
To achieve the goals above, the invention adopts the following technical scheme:
The analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy, comprising the following steps:
(1) prepared by mother liquor: weighing nickel-base alloy 0.1000g to be measured in the without phosphorus triangular flask of 100mL hard, the dilute king of 25mL is added
Water, the hydrofluoric acid solution 6~8 that 40wt% is added dropwise drip, and the without phosphorus triangular flask of hard is placed in dissolved samples on low temperature electric hot plate, then
Increase chloric acid 5mL and continue dissolution and be evaporated to syrupy shape, after cooling plus water 20mL boils, and then cools to room temperature, constant volume is in 100mL
It is shaken up in volumetric flask stand-by；
(2) nickel-silicon nitride: iodine oxidation-dimethylglyoxime spectrophotometry
5~10mL of mother liquor of aspiration step (1) adds the ammonium citrate solution 5mL of 25wt% in 100mL volumetric flask, shakes up and adds
The dimethylglyoxime solution 10mL of 0.05N iodine solution 5mL, 0.1wt%, add water constant volume, shake up, and place 5~10min, are with distilled water
Reference solution measures extinction value at spectrophotometer 530nm and is denoted as E1, standard specimen measurement extinction value be denoted as E0, according to following public affairs
Formula calculates content W (Ni) % of nickel in nickel-base alloy to be measured:
W (Ni) %=(A1/E0)*E1* 100%；
Wherein: A1: the nickel content of standard specimen；
E0: the extinction value of standard specimen measurement；
E1: the extinction value of nickel-base alloy to be measured.
The chemical principle of analysis detection nickel content of the present invention is as follows:
(3) phosphorus yield: P-Mo blue spectrophotometry
The mother liquor 20mL of aspiration step (1) adds sulfuric acid solution 2mL to shake up in 50mL volumetric flask, adjusts acidity, adds 3wt% nitre
Sour bismuth solution 5mL, 3wt% ammonium molybdate solution 5mL, shakes up；Add 0.5wt% ascorbic acid (C6H8O6) 10mL, it is reduced to phosphorus molybdenum
Indigo plant shakes up and places 8min, using distilled water as reference solution, measures extinction value at spectrophotometer 680nm and is denoted as E2, standard specimen survey
Fixed extinction value is denoted as E0, content W (P) % of phosphorus in nickel-base alloy to be measured is calculated according to following formula:
W (P) %=(A2/E0)*E2* 100%；
Wherein: A2: the phosphorus content of standard specimen；
E0: the extinction value of standard specimen measurement；
E2: the extinction value of nickel-base alloy to be measured.
The chemical principle of analysis detection phosphorus content of the present invention is as follows:
2Bi(NO3)3+H3PO4+12(NH4)2MOO4+18HNO3=H3PO4·Bi2O3·12MOO3+24NH4NO3+9H2O；
H3PO4·Bi2O3·12MOO3+6C6H8O6=H3PO4·BiO3·MOO5+6C6H8O6+6H2O。
Ingredient is complex in nickel-base alloy, general main component are as follows: Ni 4~12wt%, Cr 8~18wt%, Fe 60
0.05~0.3wt% of~75wt%, Si 1~4wt%, P 0.02~0.1wt%, C 2.0~4.5wt%, S.Nickel-base alloy
The content of two kinds of middle nickel, phosphorus elements is to determine that whether nickel-base alloy be used as stainless steel base-material must measure element, for a long time with
Coming, ability domain analysis tester carries out different dissolution systems to nickel-base alloy respectively according to testing requirement and carries out pre-treatment,
Then nickel and phosphorus are measured respectively, analysis time is long, and handy a large amount of chemical reagent.The present invention is being surveyed according to nickel and phosphorus
During fixed can interdependent and commonality, provide the analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy, the party
Method can share nickel-base alloy dissolution pre-treatment system, only need to configure a kind of mother liquor, be applicable to nickel content 0.5~
20%, it is measured while nickel, phosphorus content in the nickel-base alloy of phosphorus content 0.01~0.2%, meets the survey of Beer law chemical analysis
It is fixed.
The ingredient of standard specimen selected by the present invention and source are shown in Table 1:
1. standard specimen ingredient of table and source
According to the type of nickel-base alloy to be measured, corresponding standard specimen is selected from table 1.
Preferably, dilute chloroazotic acid is formulated according to the component that following volumes matches: HCl:HNO in step (1)3:
H2O=3:1:15.
Preferably, in step (2), the configuration method of the iodine solution are as follows: weigh 6.35g iodine respectively, 12.5g potassium iodide,
Constant volume 1000mL after being dissolved in water.
Preferably, in step (2), it is molten that the dimethylglyoxime solution by dimethylglyoxime is dissolved in the ammonium hydroxide that volume ratio is 1:1
Match in liquid.
Preferably, the sulfuric acid solution is according to volume proportion H in step (3)2SO4:H2O=1:4 is configured.
Therefore, the invention has the following beneficial effects:
(1) this method stability is good, chemical analysis favorable reproducibility, and data analysis is influenced small by environment temperature etc.；
(2) analysis method is at low cost, and chemical reagent usage amount is few, and analysis time is few, highly efficient；
(3) analysis result accuracy is high, and error is small.
Detailed description of the invention
Fig. 1 is the extinction value-A- nickel content Ni% curve of standard specimen.
Fig. 2 is the extinction value-A- phosphorus content P% curve of standard specimen.
Specific embodiment
Below by specific embodiment, and in conjunction with attached drawing, the technical solutions of the present invention will be further described.
In the present invention, if not refering in particular to, all devices and raw material is commercially available or the industry is common are following
Method in embodiment is unless otherwise instructed conventional method in that art.
Standard specimen used in the embodiment of the present invention is as shown in table 1:
1. standard specimen ingredient of table and source
It draws the extinction value-A- nickel content Ni% curve of standard specimen: weighing each standard specimen 0.1000g, draw and survey nickel, in triplicate, survey
0 point of curve is obtained, as shown in Figure 1, analysis obtains:
The extinction value of alloy cast iron YSBC3705A-1 is 0.058,0.058,0.06；
The extinction value of stainless steel YSBC11307-93 is 0.253,0.254,0.255；
The extinction value of stainless steel 301YSBC37370-13 is 0.323,0.324,0.324.
Draw the extinction value-A- phosphorus content P% curve of standard specimen:
It draws the extinction value-A- phosphorus content P% curve of standard specimen: weighing each standard specimen 0.1000g, draw survey phosphorus and measure in triplicate
0 point of curve was arrived, as shown in Fig. 2, analysis obtains:
The extinction value of alloy cast iron YSBC3705A-1 (P 0.048) is 0.191,0.192,0.192；
The extinction value of stainless steel YSBC11307-93 (P 0.099) is 0.399,0.400,0.399；
The extinction value of stainless steel 301YSBC37370-13 (P 0.028) is 0.115,0.114,0.115.
Embodiment 1
(1) prepared by mother liquor: weighing nickel-base alloy 0.1000g to be measured in the without phosphorus triangular flask of 100mL hard, alkene chloroazotic acid is added
(HCl:HNO3:H2O=3:1:15, volume ratio) 25mL, according to product silicon content be added dropwise hydrofluoric acid (40wt%) 6 drip, by hard without
Phosphorus triangular flask is placed in dissolved samples on low temperature electric hot plate, then increase chloric acid (ρ=1.67) 5mL continue dissolution be evaporated to syrup
Shape, after cooling plus water 20mL boils, and dissolved salts then cool to room temperature, and constant volume shakes up for use in 100mL volumetric flask；
(2) nickel-silicon nitride: iodine oxidation-dimethylglyoxime spectrophotometry
Mother liquor 5mL is drawn in 100mL volumetric flask, adding citric acid ammonium (25wt%) 5mL shakes up and adds iodine solution (0.05N) 5mL, fourth
Two ketoxime solutions (0.1wt%) 10mL, adds water constant volume, shakes up, and places 5min, using distilled water as reference solution, is divided in 722 types
Extinction value E is measured at photometer 530nm1=0.324, the content of nickel is calculated by standard specimen:
W (Ni) %=(A1/E0)*E1* 100%=6.21wt%；
A1: the nickel content of stainless steel 301YSBC37370-13 standard specimen；
E0: the extinction value of stainless steel 301YSBC37370-13 standard specimen measurement, referring to Fig. 1；
E1: the extinction value of nickel-base alloy to be measured；
(3) phosphorus yield: P-Mo blue spectrophotometry
Mother liquor 20mL is drawn in 50mL volumetric flask, adds sulfuric acid (H2SO4:H2O=1:4, volume ratio) 2mL shakes up, add bismuth nitrate
(3wt%) 5mL, ammonium molybdate (3wt%) 5mL, shake up；Add ascorbic acid (0.5wt%) 10mL, shake up and place 8min, with distillation
Water is reference solution, and extinction value E is measured at 722 type spectrophotometer 680nm2=0.153, containing for phosphorus is calculated by standard specimen
Amount:
W (P) %=(A2/E0)*E1* 100%=0.037wt%；
A2: the nickel content of stainless steel 301YSBC37370-13 standard specimen；
E0: the extinction value of stainless steel 301YSBC37370-13 standard specimen measurement, referring to fig. 2；
E2: the extinction value of nickel-base alloy to be measured.
Embodiment 2
(1) prepared by mother liquor: weighing nickel-base alloy 0.1000g to be measured in the without phosphorus triangular flask of 100mL hard, alkene chloroazotic acid is added
(HCl:HNO3:H2O=3:1:15, volume ratio) 25mL, according to product silicon content be added dropwise hydrofluoric acid (40wt%) 8 drip, by hard without
Phosphorus triangular flask is placed in dissolved samples on low temperature electric hot plate, then increase chloric acid (ρ=1.67) 5mL continue dissolution be evaporated to syrup
Shape, after cooling plus water 20mL boils, and dissolved salts then cool to room temperature, and constant volume shakes up for use in 100mL volumetric flask；
(2) nickel-silicon nitride: iodine oxidation-dimethylglyoxime spectrophotometry
Mother liquor 10mL is drawn in 100mL volumetric flask, adding citric acid ammonium (25wt%) 5mL shakes up and adds iodine solution (0.05N) 5mL, fourth
Two ketoxime solutions (0.1wt%) 10mL, adds water constant volume, shakes up, and places 10min, using distilled water as reference solution, in 722 types point
Extinction value E is measured at light photometer 530nm1=0.311, the content of nickel is calculated by standard specimen:
W (Ni) %=(A1/E0)*E1* 100%=5.97wt%；
A1: the nickel content of stainless steel 301YSBC37370-13 standard specimen；
E0: the extinction value of stainless steel 301YSBC37370-13 standard specimen measurement, referring to Fig. 1；
E1: the extinction value of nickel-base alloy to be measured；
(3) phosphorus yield: P-Mo blue spectrophotometry
Mother liquor 20mL is drawn in 50mL volumetric flask, adds sulfuric acid (H2SO4:H2O=1:4, volume ratio) 2mL shakes up, add bismuth nitrate
(3wt%) 5mL, ammonium molybdate (3wt%) 5mL, shake up；Add ascorbic acid (0.5wt%) 10mL, shake up and place 8min, with distillation
Water is reference solution, and extinction value E is measured at 722 type spectrophotometer 680nm2=0.246, containing for phosphorus is calculated by standard specimen
Amount:
W (P) %=(A2/E0)*E1* 100%=0.060wt%；
A2: the nickel content of stainless steel 301YSBC37370-13 standard specimen；
E0: the extinction value of stainless steel 301YSBC37370-13 standard specimen measurement, referring to fig. 2；
E2: the extinction value of nickel-base alloy to be measured.
Comparative example
(1) measurement of nickel content: identical as 1 step of embodiment (1) and (2)；
(2) measurement of phosphorus content: weighing nickel-base alloy 0.1000g to be measured, using 10 milliliters of hydrochloric acid, 5 milliliters of nitric acid, hydrofluoric acid 2
Milliliter, 5 milliliters of perchloric acid, molten sample is evaporated the sulfuric acid heating that 20 milliliters of 1:4 are added completely, and 2% potassium permanganate 4 is added to drip muddiness
Afterwards, add sodium nitrite to limpid, 10 milliliters are drawn in 100 milliliters of volumetric flasks of constant volume, the step of specific continuous mode is with embodiment 1
(3)。
Embodiment 1 merges into the same step relative to comparative example, by the molten sample step of nickel, phosphorus yield, simplifies survey
Determine step, shares measurement mother liquor, disturbing factor is few, and analysis method is at low cost, and chemical reagent usage amount is few, and analysis time is few, more
It is efficient；Analysis result is more accurate, and error is small.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, and is not surpassing
There are also other variations and modifications under the premise of technical solution documented by claim out.
Claims (5)
1. the analysis method of nickel, phosphorus content in a kind of simultaneous determination nickel-base alloy, which comprises the following steps:
(1) prepared by mother liquor: weighing nickel-base alloy 0.1000g to be measured in the without phosphorus triangular flask of 100mL hard, the dilute king of 25mL is added
Water, the hydrofluoric acid solution 6~8 that 40wt% is added dropwise drip, and the without phosphorus triangular flask of hard is placed in dissolved samples on low temperature electric hot plate, then
Increase chloric acid 5mL and continue dissolution and be evaporated to syrupy shape, after cooling plus water 20mL boils, and then cools to room temperature, constant volume is in 100mL
It is shaken up in volumetric flask stand-by；
(2) nickel-silicon nitride: iodine oxidation-dimethylglyoxime spectrophotometry
5~10mL of mother liquor of aspiration step (1) adds the ammonium citrate solution 5mL of 25wt% in 100mL volumetric flask, shakes up and adds
The dimethylglyoxime solution 10mL of 0.05N iodine solution 5mL, 0.1wt%, add water constant volume, shake up, and place 5~10min, are with distilled water
Reference solution measures extinction value at spectrophotometer 530nm and is denoted as E1, standard specimen measurement extinction value be denoted as E0, according to following public affairs
Formula calculates content W (Ni) % of nickel in nickel-base alloy to be measured:
W (Ni) %=(A1/E0)*E1* 100%；
Wherein: A1: the nickel content of standard specimen；
E0: the extinction value of standard specimen measurement；
E1: the extinction value of nickel-base alloy to be measured；
(3) phosphorus yield: P-Mo blue spectrophotometry
The mother liquor 20mL of aspiration step (1) adds sulfuric acid solution 2mL to shake up in 50mL volumetric flask, adds 3wt% bismuth nitrate solution
5mL, 3wt% ammonium molybdate solution 5mL, shake up；Add 0.5wt% ascorbic acid 10mL, shakes up and place 8min, using distilled water as reference
Solution measures extinction value at spectrophotometer 680nm and is denoted as E2, standard specimen measurement extinction value be denoted as E0, according to following formula meter
Calculate content W (P) % of phosphorus in nickel-base alloy to be measured:
W (P) %=(A2/E0)*E2* 100%；
Wherein: A2: the phosphorus content of standard specimen；
E0: the extinction value of standard specimen measurement；
E2: the extinction value of nickel-base alloy to be measured.
2. the analysis method of nickel, phosphorus content, feature exist in a kind of simultaneous determination nickel-base alloy according to claim 1
In in step (1), dilute chloroazotic acid is formulated according to the component that following volumes matches: HCl:HNO3:H2O=3:1:15.
3. the analysis method of nickel, phosphorus content, feature exist in a kind of simultaneous determination nickel-base alloy according to claim 1
In, in step (2), the configuration method of the iodine solution are as follows: weigh 6.35g iodine, 12.5g potassium iodide, constant volume after being dissolved in water respectively
1000mL。
4. the analysis method of nickel, phosphorus content, feature exist in a kind of simultaneous determination nickel-base alloy according to claim 1
In in step (2), the dimethylglyoxime solution, which is dissolved in the ammonia spirit that volume ratio is 1:1 by dimethylglyoxime, matches.
5. the analysis method of nickel, phosphorus content, feature exist in a kind of simultaneous determination nickel-base alloy according to claim 1
In in step (3), the sulfuric acid solution is according to volume proportion H2SO4:H2O=1:4 is configured.
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