CN109358015A - Zinc-manganese content assaying method in a kind of generation gloomy class product - Google Patents
Zinc-manganese content assaying method in a kind of generation gloomy class product Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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Abstract
The invention discloses a kind of zinc-manganese content analysis methods.This method uses Atomic absorption, uses solution of the flame method with mixed solution (for the concentration of EDTA for 10-20mM, PH is the solution of 9.5-11.0) as sample dissolution, zinc-manganese content is detected under element lamp appropriate and wavelength.Analysis method of the invention is easy, quick, and accuracy is high, and precision is good, and saving reagent simultaneously can be reduced industrial pollution.
Description
Technical field
The present invention relates to analysis of agricultural drugs fields, in particular, being related to a kind of analysis method of atomic absorption spectrum.More specifically
Ground, the present invention relates to zinc-manganese content assaying methods in a kind of gloomy class product of generation.
Background technique
For the protection fungicide that gloomy class product is for many leaf diseases, for preventing and treating potato, tomato powdery mildew, morning
Epidemic disease and late blight etc..Having had CIPAC to the analysis method for zinc-manganese content in gloomy class product at present, (the international analysis of agricultural drugs is assisted
Make the committee) standard and national standard, but above two method is more complicated, and it is intelligent not met present industrial production
It is required with modernization, and uses potassium cyanide as screening agent in CIPAC, belong to toxic articles, safety in utilization cannot ensure, purchase
It is considerably complicated to buy program, analysis can only accurately measure Zn content with screening agent, and manganese is by subtracting Zn content and excess EDTA
Meter calculate, it is possible to include other metal ions, as in Mancozeb, Propineb all containing calcium ion and sodium from
Son causes manganese content that cannot really react its result.Right national standard analysis (GB20699-2006) zinc-manganese operating procedure is complicated, when
Between it is longer, zinc is filtered twice by G2 crucible and G4 crucible, adjusts PH twice, and gravimetric method calculates content.Manganese is after resolution
Plurality of reagents, complex steps and terminal point control is not apparent are added.
Summary of the invention
In order to solve shortcomings existing in the prior art and difficult point, the present invention provides a kind of new zinc-manganese containing measurement
Determine method, which saves artificial analytical error caused by a large amount of artificial analysis times and complex steps, analytical effect is good,
It reduces using a large amount of reagent pollution on the environments, save analysis cost, and realize intelligent operation, overcome using cyanogen
The shortcomings that changing potassium toxic articles.And veracity and precision is above the requirement of CIPAC and national standard.With CIPAC and national standard
Credit analysis comparison, content can fit like a glove, and obtain satisfied result.
The analysis method of manganese of the present invention, zinc, is achieved through the following technical solutions:
Zinc-manganese content assaying method in a kind of generation gloomy class product, uses aas determination in gloomy class product
Zinc-manganese content.
Further, the atomic absorption spectrography (AAS) is Atomic absorption flame photometry.
Further, the Detection wavelength of manganese is 279.5.
Further, the Detection wavelength of zinc is 213.9.
Further, lamp current 4.0mA.
Further, it the described method comprises the following steps:
(1) preparation of standard solution: taking zinc-manganese standard items, is redissolved, obtains after carrying out clearing up respectively after weighing completely
Standard solution draws standard curve；
(2) it the preparation of sample solution: weighs for gloomy class product sample, is mixed using the dissolution of preparation solution A, dilution, constant volume
It is spare；
(3) carry out the analysis of Atomic absorption instrument: using Atomic absorption instrument, the element lamp for measuring each substance and
Wavelength suitable for each element detects each element, manganese wavelength 279.5, zinc wavelength 213.9, lamp current 4.0MA, deducts
Background carries out atomic absorption analysis to the solution of preparation respectively, obtains zinc-manganese standard curve value correspondence and calculates corresponding content.
Further, the manganese standard items are cleared up with hydrochloric acid.
Further, the zinc standard items Sulfuric-Acid Digestion.
Further, the preparation solution A contains EDTA, and the concentration of the EDTA is 10-20mM.
Further, the pH of the preparation solution A is 9.5-11.
Beneficial effect
Compared with prior art, the invention has the following advantages that
1. the measuring method saves artificial analytical error caused by a large amount of artificial analysis times and complex steps, analytical effect
Good, reduction is endangered caused by human body using toxic reagent, and has abandoned a large amount of reagents used at present, and environment is made in reduction
At pollution, save a large amount of analysis costs, and realize intelligent operation.
2. atomic absorption spectrometry manganese content of the invention, method accuracy reach: average recovery rate is
99.77%, precision reaches: standard deviation 0.1032%, the coefficient of variation 0.59.
3. atomic absorption spectrometry Zn content of the invention, method accuracy reach: average recovery rate is
99.24%, precision reaches: standard deviation 0.0909, the coefficient of variation 4.3.
4. atomic absorption spectrum determination method of the invention and GB20699-2006 and CIPAC analysis method compare,
The equal zinc of result error (obtains) in 0.15% range, in 0.3% range of manganese according to table 8, table 9.
Detailed description of the invention
The following drawings is merely to illustrate the present invention, of the invention not for limiting convenient for promoting the understanding of the present invention.
Fig. 1 is manganese canonical plotting.
Fig. 2 is zinc canonical plotting.
Specific embodiment
In order to preferably explain the present invention, the present invention is further explained in the light of specific embodiments.Following implementation
Instrument used in example are as follows: Agilent Atomic absorption flame spectrometer, measurement are zinc lamp, manganese lamp, high purity acetylene using element lamp
Gas, air, data processing stations and suitable concentration standard solution.
In following embodiment, (maneb, zineb, Propineb series similarly) is analyzed by taking Mancozeb as an example.Mark
Quasi- product solution be resolution after zinc standard solution and manganese standard solution obtained, be diluted to respectively concentration be 1mg/L, 2mg/L,
3mg/L.Preparation solution A is the solution that the EDTA containing various concentration and the potassium hydroxide by being saturated are adjusted to suitable pH value.
It carries out the analysis of Atomic absorption instrument: using Atomic absorption instrument, the element lamp for measuring each substance and fitting
Each element is detected in the wavelength of each element.Lamp current 4.0mA, manganese wavelength 279.5, zinc wavelength 213.9 deduct back
Scape.Standard curve is 0.5mg/L, 1mg/L, 2mg/L, 3mg/L, 4mg/L, 5mg/L: carrying out atom suction to the solution of preparation respectively
Contracture analysis obtains zinc-manganese standard curve value correspondence and calculates corresponding content.
The drafting of 1 standard curve of embodiment
It prepares standard items stock solution: accurately weighing 1.0 grams of zinc standard items (being accurate to 0.01mg), be put into 50ml volumetric flask
In, 5 milliliters of Sulfuric-Acid Digestions are added, are prepared into the standard items stock solution of 1mg/L, 2mg/L, 3mg/L.Weigh 1.0 grams of manganese standards
Product (are accurate to 0.01mg), are put into 50ml volumetric flask, and 5 milliliters of hydrochloric acid resolutions are added, are prepared into 1mg/L, 2mg/L, 3mg/L
Standard items stock solution.
Concentration point is made according to the above-mentioned method for preparing standard items stock solution in the manganese standard items for weighing different quality respectively
Not Wei 82.940mg/L, 92.130mg/L, 102.42mg/L, 112.66mg/L and 122.90mg/L manganese standard solution, and
Sample introduction, measures light absorption value, and measurement result is shown in Table 1.
Different quality zinc standard items are weighed respectively, and concentration difference is made according to the above-mentioned method for preparing standard items stock solution
For 80.332mg/L, 90.413mg/L, 100.415mg/L, 100.472mg/L and 120.537mg/L, sample introduction measures light absorption value,
Measurement result is shown in Table 2.
1 manganese content of table analyzes range of linearity measurement
| 1 | 2 | 3 | 4 | 5 | |
| It weighs sample W (g) | 0.8294 | 0.9213 | 1.0242 | 1.1266 | 1.2290 |
| Absorbance A | 0.1596 | 0.1764 | 0.1964 | 0.2134 | 0.23060 |
2 Zn content of table analyzes range of linearity measurement
| 1 | 2 | 3 | 4 | 5 | |
| It weighs sample W (mg) | 80.332 | 90.413 | 100.415 | 110.472 | 120.537 |
| Absorbance A | 0.1032 | 0.1248 | 0.1485 | 0.1724 | 0.1974 |
Sample is weighed as abscissa using manganese, and absorbance is ordinate, draws standard curve, obtains regression equation Y=0.1782x
+ 0.0123, coefficient R 2=0.9996, standard curve is shown in Fig. 1.
Sample is weighed as abscissa using zinc, and absorbance is ordinate, draws standard curve, obtains regression equation Y=
0.0023X-0.0876, coefficient R 2=0.9993, standard curve are shown in Fig. 2.
Embodiment 2
It prepares standard solution: accurately weighing 1.0 grams of zinc standard items (being accurate to 0.01mg), be put into 50ml volumetric flask,
5 milliliters of Sulfuric-Acid Digestions are added, the standard solution for being prepared into 1mg/L, 2mg/L, 3mg/L is spare.Weigh 1.0 grams of manganese standard items (essence
It really to 0.01mg), is put into 50ml volumetric flask, 5 milliliters of hydrochloric acid resolutions is added, are prepared into the standard of 1mg/L, 2mg/L, 3mg/L
Solution for standby.
It prepares sample solution: accurately weighing Mancozeb sample 100mg or so (being accurate to 0.01mg), be put into 100ml appearance
In measuring bottle, EDTA containing 20mM is added, the preparation solution A 1 that pH value is 9.8, after ultrasonic dissolution, adds the pure of non-metallic ion
Water purification is diluted to scale, is then carried out in secondary dilution to standard curve range again according to sample concentration, mixes spare.To instrument
Standard curve is measured after stabilization, and result is then calculated according to its curve.As a result are as follows: zinc 2.22%, manganese 17.66%.
Embodiment 3
It prepares standard solution: accurately weighing 1.0 grams of zinc standard items (being accurate to 0.01mg), be put into 50ml volumetric flask,
5 milliliters of Sulfuric-Acid Digestions are added, the standard solution for being prepared into 1mg/L, 2mg/L, 3mg/L is spare.Weigh 1.0 grams of manganese standard items (essence
It really to 0.01mg), is put into 50ml volumetric flask, 5 milliliters of hydrochloric acid resolutions is added, are prepared into the standard of 1mg/L, 2mg/L, 3mg/L
Solution for standby.
It prepares sample solution: accurately weighing Mancozeb sample 100mg or so (being accurate to 0.01mg), be put into 100ml appearance
In measuring bottle, EDTA containing 20mM is added, the preparation solution A 3 that pH value is 10.5, after ultrasonic dissolution, adds the pure of non-metallic ion
Water purification is diluted to scale, is then carried out in secondary dilution to standard curve range again according to sample concentration, mixes spare.To instrument
Standard curve is measured after stabilization, and result is then calculated according to its curve.As a result are as follows: zinc 2.26%, manganese 17.63%.
Embodiment 4
It prepares standard solution: accurately weighing 1.0 grams of zinc standard items (being accurate to 0.01mg), be put into 50ml volumetric flask,
5 milliliters of sulfuric acid are added, the standard solution for being prepared into 1mg/L, 2mg/L, 3mg/L is spare.1.0 grams of manganese standard items are weighed (to be accurate to
0.01mg), it is put into 50ml volumetric flask, 5 milliliters of hydrochloric acid is added, the standard solution for being prepared into 1mg/L, 2mg/L, 3mg/L is spare.
It prepares sample solution: accurately weighing Mancozeb sample 100mg or so (being accurate to 0.01mg) and be put into 100ml capacity
In bottle, EDTA containing 20mM is added, the preparation solution A 4 that pH value is 11.0, after ultrasonic dissolution, adds the pure of non-metallic ion
Water is diluted to scale, is then carried out in secondary dilution to standard curve range again according to sample concentration, mixes spare.It is steady to instrument
Standard curve is measured after fixed, result is then calculated according to its curve.As a result are as follows: zinc 2.15%, manganese 17.59%.
Embodiment 5
It prepares standard solution: accurately weighing 1.0 grams of zinc standard items (being accurate to 0.01mg), be put into 50ml volumetric flask,
5 milliliters of sulfuric acid are added, the standard solution for being prepared into 1mg/L, 2mg/L, 3mg/L is spare.1.0 grams of manganese standard items are weighed (to be accurate to
0.01mg), it is put into 50ml volumetric flask, 5 milliliters of hydrochloric acid is added, the standard solution for being prepared into 1mg/L, 2mg/L, 3mg/L is spare.
It prepares sample solution: accurately weighing Mancozeb sample 100mg or so (being accurate to 0.01mg) and be put into 100ml capacity
In bottle, EDTA containing 18mM is added, the preparation solution A 5 that pH value is 11.0, after ultrasonic dissolution, adds the pure of non-metallic ion
Water is diluted to concentration appropriate, then takes 1ml in 25ml volumetric flask, and pure water dilution is settled to scale, mixes spare.To instrument
Standard curve is measured after stabilization, and result is then calculated according to its curve.As a result are as follows: zinc 2.49%, manganese 17.65%.
Embodiment 6
It prepares standard solution: accurately weighing 1.0 grams of zinc standard items (being accurate to 0.01mg), be put into 50ml volumetric flask,
5 milliliters of sulfuric acid are added, the standard solution for being prepared into 1mg/L, 2mg/L, 3mg/L is spare.1.0 grams of manganese standard items are weighed (to be accurate to
0.01mg), it is put into 50ml volumetric flask, 5 milliliters of hydrochloric acid is added, the standard solution for being prepared into 1mg/L, 2mg/L, 3mg/L is spare.
It prepares sample solution: accurately weighing Mancozeb sample 100mg or so (being accurate to 0.01mg) in 100ml volumetric flask
In, EDTA containing 15mM is added, the solution for preparing that pH value is 11.0, after ultrasonic dissolution, the pure water for adding non-metallic ion is dilute
It releases to concentration appropriate, mixes spare.Standard curve is measured after instrument stabilizer, and result is then calculated according to its curve.Knot
Fruit are as follows: zinc 2.35%, manganese 16.51%.
7 precision test of embodiment
Weighing the Mancozeb specimen sample of different quality respectively, (batch: 17012) preparing manganese sample solution, and sample introduction is gone forward side by side
Row detection, measures absorbance, and goes out the content of manganese in each specimen sample according to the standard curve regression equation calculation of embodiment 1,
And calculate its precision.The result is shown in tables 3.
Manganese content precision measurement result in 3 sample of table
The Mancozeb specimen sample for weighing different quality respectively (batch: 17012), prepares zinc sample solution, sample introduction is simultaneously
It is detected, measures absorbance, and containing for zinc in each specimen sample according to the standard curve regression equation calculation of embodiment 1
Amount, and calculate its precision.The result is shown in tables 4.
Zn content precision measurement result in 4 sample of table
The results show that the standard deviation of manganese content is 0.1032% in the sample obtained, the coefficient of variation 0.59.Zn content
Standard deviation 0.0909%, the coefficient of variation 4.3.
8 accuracy of embodiment experiment
Different amounts of manganese standard items are added in sample solution respectively, are made into sample known to standard items content, sample introduction is simultaneously
It is detected, measures light absorption value, be measured according to embodiment 1 and calculate its rate of recovery.The result is shown in tables 5.
Manganese content quantitative analysis accuracy determination result in 5 sample of table
Different amounts of zinc standard items are added in the sample respectively, be configured to sample feeding known to standard items content and carry out
Detection measures light absorption value, is measured according to example 1 and calculates its rate of recovery, the result is shown in tables 6.
Zn content quantitative analysis accuracy determination result in 6 sample of table
Manganese average recovery rate 99.77%, zinc average recovery rate 99.24% in sample.Show using atomic absorption spectrography (AAS)
It is high to measure the accuracy of zinc-manganese content.
The comparison of the different analysis methods of embodiment 9
Data and conclusion in following table are the time required for analyzing in national standard GB20699-2006 and CIPAC method
And data are used, zinc-manganese Atomic absorption data are reflected in embodiment 2-6 in table 8 and table 9, and data are seen in table
Manganese distribution is 20-22, and zinc is between 2.6-3.1, this data be by content be 80% effective component it is scaled come, than
Such as manganese 17.66/0.8=20.07 in embodiment 2, zinc 2.22/0.8=2.77.
Table 7
Table 8 (the manganese data that different analysis methods obtain are with 80% Mancozeb content meter)
| Lot number | 17012 | 17014 | 17015 | 18020 | 18021 | 18022 | 18023 |
| CIPAC | 21.66 | 21.87 | 22.08 | 22.19 | 20.94 | 22.41 | 21.67 |
| Atomic absorption | 22.07 | 22.04 | 21.99 | 22.07 | 20.64 | 22.09 | 21.96 |
| National standard | 22.11 | 22.31 | 22.11 | 21.99 | 21.02 | 23.47 | 22.23 |
Table 9 (the 80% Mancozeb content meter of zinc data that different analysis methods obtain)
| Lot number | 17012 | 17014 | 17015 | 18020 | 18021 | 18022 | 18023 |
| CIPAC | 2.68 | 2.72 | 2.59 | 2.97 | 3.09 | 3.00 | 2.64 |
| Atomic absorption | 2.77 | 2.83 | 2.69 | 3.11 | 2.94 | 3.14 | 2.93 |
| National standard | 2.52 | 2.59 | 2.73 | 2.89 | 2.83 | 2.89 | 2.91 |
Table 7, table 8 and table 9 show that veracity and precision of the invention is above the requirement of CIPAC and national standard.With
CIPAC and the comparison of national standard chemical analysis, content can fit like a glove, and obtain satisfied result.
Although some exemplary embodiments of the invention have shown and described, those skilled in the art should know
Dawn, without departing from the principles and spirit of the present invention, change can be made to these exemplary embodiments, it is of the invention
Range is limited by claim and its equivalent.
Claims (10)
1. zinc-manganese content assaying method in a kind of generation gloomy class product, which is characterized in that using aas determination for gloomy
Zinc-manganese content in class product.
2. zinc-manganese content assaying method in generation gloomy class product according to claim 1, which is characterized in that the Atomic absorption
Spectroscopic methodology is Atomic absorption flame photometry.
3. zinc-manganese content assaying method in generation gloomy class product according to claim 1, which is characterized in that the Detection wavelength of manganese
It is 279.5.
4. zinc-manganese content assaying method in generation gloomy class product according to claim 1, which is characterized in that the Detection wavelength of zinc
It is 213.9.
5. zinc-manganese content assaying method in generation gloomy class product according to claim 1, which is characterized in that lamp current 4.0
mA。
6. zinc-manganese content assaying method in generation gloomy class product according to claim 1, which is characterized in that the method includes
Following steps:
(1) preparation of standard solution: taking zinc-manganese standard items, is redissolved after carrying out clearing up respectively after weighing completely, obtains standard
Product solution draws standard curve；
(2) it the preparation of sample solution: weighs for gloomy class product sample, is mixed using the dissolution of preparation solution A, dilution, constant volume spare；
(3) it carries out the analysis of Atomic absorption instrument: using Atomic absorption instrument, the element lamp for measuring each substance and being suitable for
The wavelength of each element detects each element, manganese wavelength 279.5, zinc wavelength 213.9, lamp current 4.0MA, deducts back
Scape carries out atomic absorption analysis to the solution of preparation respectively, obtains zinc-manganese standard curve value correspondence and calculates corresponding content.
7. zinc-manganese content assaying method in generation gloomy class product according to claim 6, which is characterized in that the manganese standard
Product are cleared up with hydrochloric acid.
8. zinc-manganese content assaying method in generation gloomy class product according to claim 6, which is characterized in that the zinc standard
Product Sulfuric-Acid Digestion.
9. zinc-manganese content assaying method in generation gloomy class product according to claim 6, which is characterized in that described to prepare solution
A contains EDTA, and the concentration of the EDTA is 10-20mM.
10. zinc-manganese content assaying method in generation gloomy class product according to claim 6, which is characterized in that it is described prepare it is molten
The pH of liquid A is 9.5-11.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458605A (en) * | 2014-11-04 | 2015-03-25 | 安徽农业大学 | Method for detecting content of heavy metals in plant sample |
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- 2018-12-20 CN CN201811562065.XA patent/CN109358015A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458605A (en) * | 2014-11-04 | 2015-03-25 | 安徽农业大学 | Method for detecting content of heavy metals in plant sample |
Non-Patent Citations (2)
| Title |
|---|
| 孙春香等: "微波消解-火焰原子吸收光谱法测定黄花菜、薇菜和核桃仁中的铜、锌、铁、锰 ", 《常熟理工学院学报》 * |
| 王光等: "火焰原子吸收法间接测定代森锰锌中有效成份的方法研究", 《光谱实验室》 * |
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Application publication date: 20190219 |