CN102253177A - Multielement standard solution for component analysis of alloying element in steel and preparation method - Google Patents

Abstract

The invention discloses a multielement standard solution for component analysis of alloying elements in steel and a preparation method, and belongs to the technical field of metallurgical analysis. The solution comprises the following elements: 0.01 mg/mL of aluminium, 0.05 mg/mL of chromium, 0.05 mg/mL of copper, 0.20 mg/mL of manganese, 0.05 mg/mL of nickel, 0.05 mg/mL of molybdenum, 0.05 mg/mL of vanadium, 0.05 mg/mL of titanium, and 0.005 mg/mL of phosphor; the solution medium is HCl with a mass percentage concentration of 5%. Closely combined with the characteristics of alloy components of steel materials, the invention solves the standard problem of material alloy analysis for apparatuses such as ICP and the like, eliminates the interference of an iron substrate and a background, realizes the traceability, greatly shortens the analysis time, and is convenient for users.

Description

Alloy element component analysis multielement standard solution and preparation method in the iron and steel

Technical field

The invention belongs to the metallurgical analysis technical field, alloy element component analysis multielement standard solution and preparation method in a kind of specifically iron and steel.

Background technology

Recently, China's steel industry begins to pay attention to from the development of output to quality, is the important means that improves the strength of materials and toughness to the adding of alloying element in the metal material and control.To the quality control of new material alloy element, because analyzing and testing needs standard solution to use as standard with the hysteresis quality and the difficulty of material standard research.And standard solution has solved the problem of the insoluble one-tenth distributed points of material standard Gradient distribution, and applicability is strong.

Along with the development of analytical technology, large-sized analytic instruments such as ICP are more and more universal in the use of metallurgy industry, and increase gradually to the demand of standard solution in market.And the majority of standard solution in the market is a single element, needs preparation in use and adds, and needs the waste plenty of time, and in smelting iron and steel rhythm very fast today, this becomes a bottleneck.It is exactly matrix coupling and matrix interference problem that the single element standard solution also has the problem of a maximum, is difficult to eliminate the interference of iron-based body, therefore uses very inconvenient.At present, can measure the characteristics of multielement simultaneously and the multielement standard solution developed is also fewer to these large-scale instruments, and be still blank at present at the multielement standard solution of steel and alloy elemental composition analysis.

Summary of the invention

The object of the present invention is to provide alloy element component analysis multielement standard solution and preparation method in a kind of iron and steel, this standard solution can satisfy the demand of large-sized analytic instruments such as ICP to the multielement standard solution of steel and alloy elemental composition analysis usefulness, make the testing staff when calibration AAS, ICP etc. analyze instrument and evaluation analysis method, can use the multielement standard solution that definite value is accurate, stability is reliable, convenient, shorten the analysis time of ferrous materials alloying element, improve the accuracy of measuring.

Technical scheme of the present invention is: alloy element component analysis multielement standard solution in a kind of iron and steel, it is characterized in that,

Contained element is in this solution, aluminium (Al), chromium (Cr), copper (Cu), manganese (Mn), nickel (Ni), molybdenum (Mo), vanadium (V), titanium (Ti) and phosphorus (P);

The content of every kind of element is aluminium 0.01mg/mL, chromium 0.05mg/mL, copper 0.05mg/mL, manganese 0.20mg/mL, nickel 0.05mg/mL, molybdenum 0.05mg/mL, vanadium 0.05mg/mL, titanium 0.05mg/mL and phosphorus 0.005mg/mL;

Solution medium is that mass percentage concentration is 5% HCl.

The alloy element component analysis comprises the steps: with the preparation method of multielement standard solution in a kind of iron and steel

(1). set up that 20 ℃ of constant temperature, humidity are controlled at 70%～80%, cleanliness factor is ten thousand grades laboratory, set up cleanliness factor and be hundred grades testing table;

(2). take by weighing 0.1000g purity respectively and be 99.95% high-purity chromium, 0.1000g purity and be 99.99% high purity copper, 0.1000g purity and be 99.99% high purity nickel, 0.1000g purity and be 99.99% high purity titanium and 0.4000g purity and be high-purity electrolytic manganese of 99.95% in beaker, the adding mass percentage concentration is 18% hydrochloric acid 20mL, dripping mass percentage concentration is 30% hydrogen peroxide 1mL, is heated to its whole dissolvings under 150～200 ℃ of conditions;

(3). take by weighing 0.04395g purity and be 99.99% benchmark potassium dihydrogen phosphate in beaker, add three distilled water of 30mL and make its dissolving;

(4). take by weighing 0.0200g purity and be 99.99% rafifinal in polytetrafluoroethylene beaker, add 1g NaOH and three distilled water of 10mL and make its dissolving, adding the 10mL mass percentage concentration then is that 34% nitric acid carries out acidifying;

(5). take by weighing 0.1000g purity and be high-purity molybdenum of 99.99% in beaker, add the 2mL mass percentage concentration and be 36% hydrochloric acid and 3mL mass percentage concentration and be 68% nitric acid, heating makes its dissolving under 150～200 ℃ of conditions;

(6). get 0.1785g purity and be 99.99% high purity vanadic anhydride in polytetrafluoroethylene beaker, add 5mL concentration, add the 10mL mass percentage concentration then and be 18% hydrochloric acid and carry out acidifying for the 100g/L sodium hydroxide solution makes its dissolving;

(7). above solution is transferred in the 2000mL volumetric flask, is that 5% hydrochloric acid is diluted to scale and shakes up with mass percentage concentration in the time of 20 ℃;

(8). store and packing, stock solution can be stored in the 2000mL volumetric flask, is placed in the environment of 20 ℃ of cleanings of temperature to store; The import vinyon bottle of also available 500mL or two kinds of specifications of 50mL packs, and Packaging Bottle will be carried out cleaning before use and handled, sealed and packed after, be placed on temperature and be in 20 ℃ the clean environment and store.

The invention has the beneficial effects as follows that the combine closely characteristics of ferrous materials alloying component of the present invention have solved the typical problem that instruments such as ICP are analyzed for material alloys, eliminated the interference of iron-based body and background, realize traceability, shortened analysis time greatly, made things convenient for the user.This multielement standard solution uses through how tame unit, consistent think this serial multielement standard solution value accurately, job requirements such as good stability, easy to use, the calibration that can satisfy instruments such as ICP, AAS, test.Be applied to the material analysis and the quality control of more domestic iron and steel enterprises (as Ji steel, Laigang, blue or green steel etc.),, reduced quality objection to produce vital role for guaranteeing the ferrous materials quality; This multielement standard solution is examined by State Bureau of Technical Supervision, uses as national standard substance issue, also is applied to metrological service and uses as the standard of instrument calibration and instrument calibrating, has realized the magnitude tracing of instruments such as ICP.The present invention has good economic benefit and social benefit.

Embodiment

The alloy element component analysis with contained element in the multielement standard solution is in a kind of iron and steel, aluminium (Al), chromium (Cr), copper (Cu), manganese (Mn), nickel (Ni), molybdenum (Mo), vanadium (V), titanium (Ti), phosphorus (P);

The content of every kind of element sees Table 1.

The alloy element component analysis content of every kind of element of multielement standard solution in table 1 iron and steel

The alloy element component analysis with the preparation method of multielement standard solution is in a kind of iron and steel:

(1). set up that 20 ℃ of constant temperature, humidity are controlled at 70%～80%, cleanliness factor is ten thousand grades laboratory, set up cleanliness factor and be hundred grades testing table;

(2). take by weighing 0.1000g purity respectively and be 99.95% high-purity chromium, 0.1000g purity and be 99.99% high purity copper, 0.1000g purity and be 99.99% high purity nickel, 0.1000g purity and be 99.99% high purity titanium and 0.4000g purity and be high-purity electrolytic manganese of 99.99% in beaker, the adding mass percentage concentration is 18% hydrochloric acid 20mL, dripping mass percentage concentration is 30% hydrogen peroxide 1mL, is heated to whole dissolvings under 150～200 ℃ of conditions;

(3). take by weighing 0.04395g purity and be 99.99% benchmark potassium dihydrogen phosphate in beaker, add three distilled water of 30mL and make its dissolving;

(4). take by weighing 0.0200g purity and be 99.99% rafifinal in polytetrafluoroethylene beaker, add 1g NaOH and three distilled water of 10mL and make its dissolving, adding the 10mL mass percentage concentration then is that 34% nitric acid carries out acidifying;

(5). take by weighing 0.1000g purity and be high-purity molybdenum of 99.99% in beaker, add the 2mL mass percentage concentration and be 36% hydrochloric acid and 3mL mass percentage concentration and be 68% nitric acid, heating makes its dissolving under 150～200 ℃ of conditions;

(6). get 0.1785g purity and be 99.99% high purity vanadic anhydride in polytetrafluoroethylene beaker, add 5mL concentration, add the 10mL mass percentage concentration then and be 18% hydrochloric acid and carry out acidifying for the 100g/L sodium hydroxide solution makes its dissolving;

(7). above solution is transferred in the 2000mL volumetric flask, is that 5% hydrochloric acid is diluted to scale and shakes up with mass percentage concentration in the time of 20 ℃;

(8). store and packing, stock solution can be stored in the 2000mL volumetric flask, is placed in the environment of 20 ℃ of cleanings of temperature to store; The import vinyon bottle of also available 500mL or two kinds of specifications of 50mL packs, and Packaging Bottle will be carried out cleaning before use and handled, sealed and packed after, be placed on temperature and be in 20 ℃ the clean environment and store.

The alloy element component analysis sees Table 2 with multielement standard solution analysis of the accuracy in this kind iron and steel.

Alloy element component analysis multielement standard solution analysis of the accuracy table in table 2 iron and steel

Claims (2)

1. alloy element component analysis multielement standard solution in the iron and steel is characterized in that,

Contained element is in this solution, aluminium, chromium, copper, manganese, nickel, molybdenum, vanadium, titanium and phosphorus;

The content of every kind of element is aluminium 0.01mg/mL, chromium 0.05mg/mL, copper 0.05mg/mL, manganese 0.20mg/mL, nickel 0.05mg/mL, molybdenum 0.05mg/mL, vanadium 0.05mg/mL, titanium 0.05mg/mL and phosphorus 0.005mg/mL;

Solution medium is that mass percentage concentration is 5% HCl.

2. the alloy element component analysis is characterized in that with the preparation method of multielement standard solution in a kind of iron and steel as claimed in claim 1, comprises the steps:

(1). set up that 20 ℃ of constant temperature, humidity are controlled at 70%～80%, cleanliness factor is ten thousand grades laboratory, set up cleanliness factor and be hundred grades testing table;

(2). take by weighing 0.1000g purity respectively and be 99.95% high-purity chromium, 0.1000g purity and be 99.99% high purity copper, 0.1000g purity and be 99.99% high purity nickel, 0.1000g purity and be 99.99% high purity titanium and 0.4000g purity and be high-purity electrolytic manganese of 99.95% in beaker, the adding mass percentage concentration is 18% hydrochloric acid 20mL, dripping mass percentage concentration is 30% hydrogen peroxide 1mL, is heated to its whole dissolvings under 150～200 ℃ of conditions;

(3). take by weighing 0.04395g purity and be 99.99% benchmark potassium dihydrogen phosphate in beaker, add three distilled water of 30mL and make its dissolving;

(4). take by weighing 0.0200g purity and be 99.99% rafifinal in polytetrafluoroethylene beaker, add 1g NaOH and three distilled water of 10mL and make its dissolving, adding the 10mL mass percentage concentration then is that 34% nitric acid carries out acidifying;

(5). take by weighing 0.1000g purity and be high-purity molybdenum of 99.99% in beaker, add the 2mL mass percentage concentration and be 36% hydrochloric acid and 3mL mass percentage concentration and be 68% nitric acid, heating makes its dissolving under 150～200 ℃ of conditions;

(6). get 0.1785g purity and be 99.99% high purity vanadic anhydride in polytetrafluoroethylene beaker, add 5mL concentration, add the 10mL mass percentage concentration then and be 18% hydrochloric acid and carry out acidifying for the 100g/L sodium hydroxide solution makes its dissolving;

(7). above solution is transferred in the 2000mL volumetric flask, is that 5% hydrochloric acid is diluted to scale and shakes up with mass percentage concentration in the time of 20 ℃;

(8). store and packing, stock solution can be stored in the 2000mL volumetric flask, is placed in the environment of 20 ℃ of cleanings of temperature to store; The import vinyon bottle of also available 500mL or two kinds of specifications of 50mL packs, and Packaging Bottle will be carried out cleaning before use and handled, sealed and packed after, be placed on temperature and be in 20 ℃ the clean environment and store.