CN108037112A - A kind of method of nickel in Flame Atomic Absorption Spectrometry method measure reduced iron powder - Google Patents
A kind of method of nickel in Flame Atomic Absorption Spectrometry method measure reduced iron powder Download PDFInfo
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Abstract
The invention discloses a kind of method that Flame Atomic Absorption Spectrometry method measures nickel in reduced iron powder, it includes the following steps：(1) sample weighing；(2) sample dissolves；(3) sample constant volume；(4) blank sample is prepared；(5) measurement standard curve；(6) sample measures；(7) measurement result is calculated.The present invention is the analysis method that nickel content is 0.005~0.50% in Flame Atomic Absorption Spectrometry Determination reduced iron powder, this method is mainly measured nickel content in reduced iron powder using Atomic absorption, the method is simple and quick, accuracy, precision and linear relationship are good, and a kind of preferable analysis method is provided for nickel content measure in measure reduced iron powder.
Description
Technical field：
The present invention relates to a kind of method for measuring nickel in reduced iron powder, surveyed more particularly to a kind of Flame Atomic Absorption Spectrometry method
Determine the method for nickel in reduced iron powder.
Background technology：
Reduced iron powder is mainly used for during hydrometallurgy zinc, the heavy copper of neutralization department displacement.The process of reduced iron powder copper removal
In should reduce other impurities element to the greatest extent and bring into, wherein, during the band membership of nickel element makes hydrometallurgy zinc technology, purifying vehicle
Between remove the difficulty increase of the element of impurities in liquid containing zinc, while increase remove zinc powder amount needed for nickel, increase production process into
This, the content for the nickel element brought into theory in whole technical process is more low better.Therefore, should when selecting reduced iron powder
The nickel content in reduced iron powder is detected, avoids reduced iron powder from bringing excessive nickel element into.
At present, nickel content in reduced iron powder is measured, without corresponding national standard analysis method, is typically used for reference《Ore and have
Non-ferrous metal analyzes handbook》Common elements chemical analysis method is analyzed in ore disclosed in page 68, but due to constituent
There are larger difference, iron Matrix effects are serious in reduced iron powder, and measurement result is inaccurate；And this method is primarily adapted for use in 1%
The analysis of above nickel element content, for nickel content in reduced iron powder 0.005~0.50%, analytical error is larger；And should
Analysis method is related to sample dissolving, filtering, the adjusting of pH value, when whole analytic process used time nearly 2 is small, is reached using reagent
10 kinds, analysis time length, reagent cost height.Therefore design one kind is needed to measure accurate, time of measuring is short, inexpensive reduced iron
The assay method of nickel content in powder.
The content of the invention：
It is an object of the invention to provide one kind measurement accurately, time of measuring is short, inexpensive Flame Atomic Absorption Spectrometry method
The method for measuring nickel in reduced iron powder.
The purpose of the present invention is implemented by following technical solution：Nickel in a kind of Flame Atomic Absorption Spectrometry method measure reduced iron powder
Method, it includes the following steps：(1) sample weighing；(2) sample dissolves；(3) sample constant volume；(4) blank sample is prepared；(5) survey
Measure standard curve；(6) sample measures；(7) measurement result is calculated；Wherein,
(2) sample dissolves：
A, Trace Silicon into sample plus in ammonium fluoride removing sample；
B, after except silicon, then hydrochloric acid, nitric acid and reduced iron powder is added to react so that iron powder is dissolved in acid；
C, after iron powder dissolving, then carbon and insoluble in hydrochloric acid and the impurity of nitric acid in sulfuric acid dissolution sample is added；
D, it is eventually adding salt in nitric acid and water sample dissolution.
The method of nickel, concrete operation step are as follows in a kind of Flame Atomic Absorption Spectrometry method measure reduced iron powder：
(1) sample weighing：Accurately 0.2000g test specimens are weighed in 250mL beakers；
(2) sample dissolves：
A, Trace Silicon in sample is removed：250g/l ammonium fluoride 2ml are added into sample, add 20ml hydrochloric acid, beyond the Great Wall band row
5min is boiled in tracheae piston, heating, removes Trace Silicon in sample；
B, iron powder dissolves：After silicon, add 5ml nitric acid and boil to 2~3ml, hydrochloric acid, nitric acid and reduced iron powder and react so that
Iron powder is dissolved in acid；
C, carbon and impurity in sample dissolution：After iron powder dissolving, (1+1) sulfuric acid 5ml is added, is boiled to 2ml, removes cooling,
In sample carbon and insoluble in the impurity of hydrochloric acid and nitric acid dissolve；
D, salt in sample dissolution：After carbon and impurity dissolving, 5ml nitric acid is added, and adds water to be boiled to 30ml, is then cooled down
To room temperature, salt dissolves in sample, obtains fluid sample；
(3) sample constant volume：Fluid sample adds water to be settled to 100mL, and sample to be tested is made；
(4) blank sample is prepared：Blank sample is prepared with sample to be tested same procedure is prepared；
(5) measurement standard curve：Take respectively nickel standard solution 0.0mL, 0.2mL of 100ug/mL, 0.4mL, 0.8mL,
1.2mL, which is put into, to be contained with the 100ml volumetric flasks of 36mL (5mg/mL) iron standard solution, is added 5mL nitric acid, is arrived with water constant volume
100mL, obtains five groups of standard solution, and the standard solution of configuration on Atomic absorption instrument using calibration curve method in being carried out more than
Measure, draws standard curve；
(6) sample measures：Sample to be tested and blank sample are demarcated with standard curve, obtains sample to be tested measured value and blank
Sample measurement；
(7) measurement result is calculated：Sample to be tested measured value subtracts the survey that blank sample measurement is worth to sample to be tested
Measure result.
Atomic absorption instrument is Metalization of skin, its best operating condition is：Wavelength 232.0nm, monochromator lead to
Band 0.2nm, fixed lamp current 4mA, air acetylene flow 13.50-2.00L/min, burn grease head highness 13.5mm, and buckle back scape is opened.
Principle：Take a certain amount of test specimen ammonium fluoride (removing a small amount of silicon in sample), hydrochloric acid (sample dissolving), nitric acid
(sample dissolving), sulfuric acid smoke (a little carbon content in sample dissolution), in nitric acid medium；In Flame Atomic Absorption Spectrometry spectrophotometer
It is measured at wavelength 232.0nm, with the absorbance of nickel in calibration curve method determination test sample, in its absorbance and sample
Nickel content is directly proportional, is quantified compared with standard series.
Advantages of the present invention：The present invention be in Flame Atomic Absorption Spectrometry Determination reduced iron powder nickel content for 0.005~
0.50% analysis method, this method are mainly measured nickel content in reduced iron powder using Atomic absorption, the method operation
Simple and fast, accuracy, precision and linear relationship are good, are provided for nickel content measure in measure reduced iron powder a kind of preferable
Analysis method.The method of the present invention agents useful for same species is few, reduces reagent cost；Analysis time by existing analysis method 2 it is small when
It shorten to 40 minutes, and it is high to analyze accuracy rate.
Embodiment：
A kind of method of nickel in Flame Atomic Absorption Spectrometry method measure reduced iron powder, key instrument and reagent used are respectively：
Instrument:Metalization of skin (AA240-FS types), attached nickel hollow cathode lamp, electronic balance (MS204S), glass
Glass vessel.
Reagent：Hydrochloric acid (analysis is pure), nitric acid (analysis is pure), sulfuric acid (analysis is pure), ammonium fluoride (analysis is pure)
Nickel standard solution is the Standard Stock solutions of 100ug/mL, and preparation method is carried out by the preparation method of standard solution.
The best conditions of instrument, is shown in Table shown in 1 Instrument measuring condition:
1 Instrument measuring condition of table
Its concrete operation step is as follows：(1) sample weighing；(2) sample dissolves；(3) sample constant volume；(4) blank sample is prepared
Product；(5) measurement standard curve；(6) sample measures；(7) measurement result is calculated；Wherein,
(1) sample weighing：Accurately 0.2000g test specimens are weighed in 250mL beakers；
(2) sample dissolves：
A, Trace Silicon in sample is removed：250g/l ammonium fluoride 2ml are added into sample, add 20ml hydrochloric acid, beyond the Great Wall band row
5min is boiled in tracheae piston, heating, removes Trace Silicon in sample；
B, iron powder dissolves：After silicon, add 5ml nitric acid and boil to 2~3ml, hydrochloric acid, nitric acid and reduced iron powder and react so that
Iron powder is dissolved in acid；
C, carbon and impurity in sample dissolution：After iron powder dissolving, (1+1) sulfuric acid 5ml is added, is boiled to 2ml, removes cooling,
In sample carbon and insoluble in the impurity of hydrochloric acid and nitric acid dissolve；
D, salt in sample dissolution：After carbon and impurity dissolving, 5ml nitric acid is added, and adds water to be boiled to 30ml, is then cooled down
To room temperature, salt dissolves in sample, obtains fluid sample；
(3) sample constant volume：Fluid sample adds water to be settled to 100mL, and sample to be tested is made；
(4) blank sample is prepared：Blank sample is prepared with sample to be tested same procedure is prepared；
(5) measurement standard curve：Take respectively nickel standard solution 0.0mL, 0.2mL of 100ug/mL, 0.4mL, 0.8mL,
1.2mL, which is put into, to be contained with the 100ml volumetric flasks of 36mL (5mg/mL) iron standard solution, is added 5mL nitric acid, is arrived with water constant volume
100mL, obtains five groups of standard solution, and the standard solution of configuration on Atomic absorption instrument using calibration curve method in being carried out more than
Measure, draws standard curve；
(6) sample measures：Sample to be tested and blank sample are demarcated with standard curve, obtains sample to be tested measured value and blank
Sample measurement；
(7) measurement result is calculated：Sample to be tested measured value subtracts the survey that blank sample measurement is worth to sample to be tested
Measure result.
For analytical instrument Atomic absorption it is very common that in ore each element measure, but to measure reduce
In iron powder for reduced iron powder, in sample handling processes, it is endless to there is dissolving also without relevant measure example in nickel element
It is complete to cause analytic process Matrix effects caused by analysis result is relatively low, iron content is high serious and the selection of analytical instrument condition, influence
The accuracy of measurement result, the application method overcome above influence factor, ensure that the accuracy of measurement result.
Contrast experiment：
First, accuracy test
Totally 10,0.2000g reduced iron powders sample accurately is weighed, weighed 10 samples are divided into 5 groups, every group of correspondence
The nickel standard of one addition 0.05mg, after being handled by the present embodiment method and step, blank test, experiment knot are done in company with sample
Fruit see the table below 2：
Table 2：The process recovery of standard addition table of comparisons
| Sample ID | Mark-on amount mg | Measured value mg | The rate of recovery (%) |
| Reduced iron powder -1 | 0.072 | ||
| Reduced iron powder -2 | 0.073 | ||
| Reduced iron powder -3 | 0.071 | ||
| Reduced iron powder -4 | 0.074 | ||
| Reduced iron powder -5 | 0.075 | ||
| Reduced iron powder -1.1 | 0.05 | 0.122 | 100 |
| Reduced iron powder -2.2 | 0.05 | 0.118 | 90 |
| Reduced iron powder -3.3 | 0.05 | 0.124 | 106 |
| Reduced iron powder -4.4 | 0.05 | 0.124 | 100 |
| Reduced iron powder -5.5 | 0.05 | 0.121 | 92 |
The method of the present invention determination sample rate of recovery is can be seen that between 90~106% by upper table data, thus illustrates this
Inventive method is feasible.
2nd, Precision Experiment
Each 10 of 0.2000g different Ni contents reduced iron powder samples are accurately weighed respectively, carry out two groups of contrast parallel tests,
To 10 nickel contents of same group of sample parallel determination, Precision test result is shown in Table 3：
3 two groups of contrast parallel test measurement results of table
The precision of nickel element is analyzing allowable error model in the method for the present invention measure reduced iron powder as can be seen from the above table
In enclosing, illustrate that the method measurement result is relatively stablized.
3rd, tested for sample problems of dissolution
Same sample weighs 20 glasss, and 10 glasss of conical beaker openings are dissolved in course of dissolution, band pipe piston on 10 cup lids
Dissolving, other operating procedures are identical with the present embodiment, and measurement result is as shown in table 4：
4 two groups of contrast test measurement results of table
Measurement result is contrasted, it is found that open processing sample impurity is more, it is more muddy, illustrate that sample dissolving is endless
Entirely；And it is limpider with the sample after the processing of pipe piston, as can be seen from Table 4, conical beaker opening is dissolved, and is caused point
It is inaccurate to analyse result, error is larger.
4th, contrast test is carried out for sample matrices disturbed condition
Two sets of standard solution are configured, have the matrix standard series to be：Take respectively 100ug/mL nickel standard solution 0.0mL,
0.2mL, 0.4mL, 0.8mL, 1.2mL, which are put into, to be contained with the 100ml volumetric flasks of 36mL (5mg/mL) iron standard solution, is added
5mL nitric acid, with water constant volume to 100mL, obtaining five groups has matrix standard solution, and foundation has matrix standard curve；Without matrix standard
Series is：Nickel standard solution 0.0mL, 0.2mL, 0.4mL, 0.8mL, 1.2mL of 100ug/mL is taken to be put into 100ml volumetric flasks respectively
In, 5mL nitric acid is added, with water constant volume to 100mL, five groups is obtained without matrix standard solution, establishes no matrix standard curve；Then
Using there is 0.4mL groups in matrix standard series to have matrix standard solution as sample, the replication 10 in no matrix standard curve
It is secondary；0.4mL groups in no matrix standard series are repeated survey as sample without matrix standard solution in having matrix standard curve again
It is 10 times fixed；There are 0.4mL groups in matrix standard series to have matrix standard solution as sample, repeat to survey in having matrix standard curve
It is 10 times fixed；Testing result is as shown in table 5：
Table 5 carries out the testing result of contrast test for sample matrices disturbed condition
| Test group | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| (1) | 0.81 | 0.82 | 0.78 | 0.79 | 0.82 | 0.81 | 0.82 | 0.80 | 0.79 | 0.81 |
| (2) | 0.25 | 0.26 | 0.24 | 0.25 | 0.26 | 0.28 | 0.25 | 0.24 | 0.26 | 0.26 |
| (3) | 0.41 | 0.42 | 0.40 | 0.41 | 0.41 | 0.40 | 0.41 | 0.41 | 0.40 | 0.40 |
Note：
(1) is that have 0.4mL groups in matrix standard series to have matrix standard solution as sample in table 5, in no matrix standard
The measurement result of replication 10 times, unit mg/l in curve；
In table 5 (2) be in no matrix standard series 0.4mL groups without matrix standard solution as sample, having matrix standard
The measurement result of replication 10 times, unit mg/l in curve；
(3) are that have 0.4mL groups in matrix standard series to have matrix standard solution as sample in table 5, are there is matrix standard
The measurement result of replication 10 times, unit mg/l in curve；
As can be seen from Table 5, carry out that standard is counter surveys before determination sample, no matrix in the standard curve for have matrix
Standard solution be measured as sample, as a result measured value is less than one times or so of standard value；Then again the standard for having matrix
Solution is measured as sample in the standard curve of no matrix, and measurement result value is higher than one times or so of standard value；There is base
The standard solution for having matrix is measured as sample in the standard curve of body, measurement result value is consistent substantially with standard value.
As can be seen from the above results, sample Matrix effects in continuous mode are more serious, and the present invention is using molten in standard
Matrix is added in liquid, effectively avoids the interference of the matrix in continuous mode so that measurement result is more accurate.
5th, instrument condition comparative selection is tested
20, the identical reduced iron powder samples of 0.2000g are accurately weighed respectively, are divided into 2 groups, every group 10, are carried out to having a competition
Test, select instrument to recommend optimal conditions, test group buckle back scape is opened, control group buckle back Jing Guan, other steps and the present embodiment step
Identical, measurement result is as shown in table 6：
6 instrument condition comparative selection of table tests measurement result
| Sample number into spectrum | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Control group (%) | 0.210 | 0.221 | 0.230 | 0.214 | 0.215 | 0.208 | 0.210 | 0.219 | 0.220 | 0.214 |
| Test group (%) | 0.040 | 0.042 | 0.044 | 0.041 | 0.042 | 0.042 | 0.041 | 0.040 | 0.039 | 0.042 |
As can be seen from the above results, sample continuous mode Instrumental buckle back Jing Guan has a great influence analysis result, instrument
It is inaccurate that buckle back scape closes measurement result.
6th, existing detection method and the present embodiment detection method contrast test
5 groups of different Ni contents reduced iron powders are taken respectively, every group 2 parts, are detected respectively with existing detection method and the present embodiment
Method is detected, and testing result is as shown in table 7：
7 existing detection method of table and the present embodiment detection method contrast test testing result
As can be seen from the above data, the present embodiment is compared with nickel element content value in existing detection method analysis-reduction iron powder
Method measured value is integrally higher by one times, and existing detection method testing result is inaccurate.
Claims (3)
1. a kind of method of nickel in Flame Atomic Absorption Spectrometry method measure reduced iron powder, it is characterised in that it includes the following steps：
(1) sample weighing；(2) sample dissolves；(3) sample constant volume；(4) blank sample is prepared；(5) measurement standard curve；(6) sample is surveyed
It is fixed；(7) measurement result is calculated；Wherein,
(2) sample dissolves：
A, Trace Silicon into sample plus in ammonium fluoride removing sample；
B, after except silicon, then hydrochloric acid, nitric acid and reduced iron powder is added to react so that iron powder is dissolved in acid；
C, after iron powder dissolving, then carbon and insoluble in hydrochloric acid and the impurity of nitric acid in sulfuric acid dissolution sample is added；
D, it is eventually adding salt in nitric acid and water sample dissolution.
2. the method for nickel, its feature exist in a kind of Flame Atomic Absorption Spectrometry method measure reduced iron powder according to claim 1
In concrete operation step is as follows：
(1) sample weighing：Accurately 0.2000g test specimens are weighed in 250mL beakers；
(2) sample dissolves：
A, Trace Silicon in sample is removed：250g/l ammonium fluoride 2ml are added into sample, add 20ml hydrochloric acid, beyond the Great Wall band exhaust pipe
5min is boiled in piston, heating, removes Trace Silicon in sample；
B, iron powder dissolves：After silicon, add 5ml nitric acid and boil to 2~3ml, hydrochloric acid, nitric acid and reduced iron powder and react so that iron powder
It is dissolved in acid；
C, carbon and impurity in sample dissolution：After iron powder dissolving, (1+1) sulfuric acid 5ml is added, is boiled to 2ml, removes cooling, sample
Middle carbon and insoluble in the impurity of hydrochloric acid and nitric acid dissolve；
D, salt in sample dissolution：After carbon and impurity dissolving, 5ml nitric acid is added, and adds water to be boiled to 30ml, is subsequently cooled to room
Temperature, salt dissolves in sample, obtains fluid sample；
(3) sample constant volume：Fluid sample adds water to be settled to 100mL, and sample to be tested is made；
(4) blank sample is prepared：Blank sample is prepared with sample to be tested same procedure is prepared；
(5) measurement standard curve：Nickel standard solution 0.0mL, 0.2mL, 0.4mL, 0.8mL, 1.2mL of 100ug/mL is taken to put respectively
In the 100ml volumetric flasks for entering to be contained with 36mL (5mg/mL) iron standard solution, 5mL nitric acid is added, with water constant volume to 100mL, is obtained
To five groups of standard solution, the standard solution of configuration is painted in being measured on Atomic absorption instrument using calibration curve method more than
Standard curve processed；
(6) sample measures：With standard curve determination sample to be tested and blank sample, sample to be tested measured value and blank sample are obtained
Measured value；
(7) measurement result is calculated：Sample to be tested measured value subtracts the measurement knot that blank sample measurement is worth to sample to be tested
Fruit.
3. the method for nickel, its feature exist in a kind of Flame Atomic Absorption Spectrometry method measure reduced iron powder according to claim 2
In Atomic absorption instrument is Metalization of skin, its best operating condition is：Wavelength 232.0nm, monochromator passband
0.2nm, fixed lamp current 4mA, air acetylene flow 13.50-2.00L/min, burn grease head highness 13.5mm, and buckle back scape is opened.
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| CN108569675A (en) * | 2018-06-04 | 2018-09-25 | 合肥师范学院 | A kind of acid solution and the method using its dissolving iron powder |
| CN110132867A (en) * | 2019-06-06 | 2019-08-16 | 鑫联环保科技股份有限公司 | The measuring method of micro-nickel in a kind of regenerated zinc raw material zinc hydrometallurgy solution |
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| CN108569675A (en) * | 2018-06-04 | 2018-09-25 | 合肥师范学院 | A kind of acid solution and the method using its dissolving iron powder |
| CN110132867A (en) * | 2019-06-06 | 2019-08-16 | 鑫联环保科技股份有限公司 | The measuring method of micro-nickel in a kind of regenerated zinc raw material zinc hydrometallurgy solution |
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Application publication date: 20180515 |