CN103528879A - Method for determining iron content in nori with flame atomic absorption spectrometry - Google Patents
Method for determining iron content in nori with flame atomic absorption spectrometry Download PDFInfo
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Abstract
The invention provides a method for determining iron content in nori with a flame atomic absorption spectrometry. The method comprises the following steps: dyeing a sample at a high temperature to remove water; immersing the sample into a digestion solvent for long time and then pre-treating under high-temperature, high-pressure and closed conditions, so as to rapidly transfer iron in the sample into the digestion solvent at maximum, wherein the digestion solvent is a mixed acid of nitric acid and perchloric acid at a volume ratio of 4:1; heating and digesting by using a microwave oven so as to achieve a high temperature instantly and shorten the digestion time. According to the method provided by the invention, the problems of a traditional method that the consumed time is long and the use amount of solvents is great when the flame atomic absorption spectrometry is used for determining microelements and the environmental pollution caused by the solvents is serious are solved; the method has the advantages of rapidness and convenience, good repeatability and good accuracy, and is applicable to determining the microelements of similar materials.
Description
Technical field
The present invention relates to a kind of method of measuring iron-holder in laver, be specifically related to a kind of method with iron content in Flame Atomic Absorption Spectrometry Determination laver.
Background technology
Laver is the phycophyta on a kind of growth and shallow sea rock, be rich in protein, polysaccharide, each seed amino acid, fat, vitamin, inorganic salts and iron, magnesium, zinc, calcium, copper, etc. various trace elements, be the high nutritional health food of taste, there is higher nutritive value and medical value.Wherein ferro element has hematopoiesis function in human body, participate in the synthetic of haemproteins, cytochrome and various enzymes, promote growth, the also effect of its transportation oxygen and nutriment in blood, human body lacks iron can there is small cell anemia, immunologic function decline and metabolic disturbance, therefore, human body need to be guaranteed the intake of iron in diet.
Laver is on dining table, to obtain a kind of cuisines raw material that most people like, the content of measuring iron in laver can provide the reference data of use to dietotherapy health-care efficacy, have certain practical value.At present, detect the main GFAAS (graphite furnace atomic absorption spectrometry) of method of iron content, that GFAAS (graphite furnace atomic absorption spectrometry) has is highly sensitive, the few sample utilization factor of consumption is high, is suitable for the solution that analytical solution concentration is ppb level, but the composition unevenness of the method is larger, repeatable poor.According to iron content in laver, be not less than 0.05mg/g, meeting under the prerequisite of precision flame atomic absorption spectrometry more accurately and reliably, and convenient fast, favorable repeatability.During Flame Atomic Absorption Spectrometry Determination iron content routinely, consumption is long, and solvent use amount is large, and the environmental pollution of being introduced by solvent is also just more serious.
Summary of the invention
In order to solve the deficiency in background technology, the object of the invention is to overcome the defect of background technology, the method for iron content in the Flame Atomic Absorption Spectrometry Determination laver that a kind of minute is short, solvent use amount is little, degree contaminated environment is reduced is provided.
For achieving the above object, the technical solution used in the present invention is: a kind of method of iron content in Flame Atomic Absorption Spectrometry Determination laver, is characterized in that: comprise the following steps:
A. the collection of sample: commercially available wild laver is cleaned to the air-dry clean container of putting into, clean container is put into temperature dries to permanent quality at the constant temperature oven of 80 ~ 85 ℃, use mortar grind into powder, obtain laver sample after crossing 80 mesh sieves, be placed in exsiccator, preserve stand-by;
B. Specimen eliminating is processed: accurately take laver sample, be placed in reaction vessel, to adding in reaction vessel, quantitatively clear up solvent soaking 45 ~ 50min, after sealing, be placed in micro-wave oven and first use " low fire screen " heating and decompose 2min, use again " in high fire screen " heating and decompose 4min, take out reaction vessel after test solution is cooled to room temperature, with neutral filter paper, test solution is crossed to leaching filtrate, be placed in volumetric flask stand-by;
C. the preparation of sample solution: add redistilled water to be settled to scale in volumetric flask, be mixed with sample solution;
D. blank solution preparation: with step b, but only add the solvent of clearing up with step b equivalent, in micro-wave oven, after heating, take out reaction vessel to be cooled to room temperature, taking out blank test solution is placed in the volumetric flask with step c intermediate size, in volumetric flask, add redistilled water constant volume to determine scale, be mixed with blank solution standby;
E. standard solution preparation: the nitric acid that the concentration of take is 1% is thinning agent, the iron titer of 1mg/mL is mixed with to variable concentrations standard solution standby;
F. iron content in Instrument measuring waste gas, described instrument comprises: flame atomic absorption spectrophotometer, iron atom spectrum lamp, design parameter arranges as follows:
Lamp current: 6.0mA
Spectral band-width: 0.2nm
Burner height: 7mm
Air mass flow: 8.0mL/min
Acetylene gas flow: 1.5 L/min
Wavelength: 248.3nm
G. with blank solution calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and testing sample solution, drawing standard curve, measures the content of iron.
In a preferred embodiment of the present invention, further comprise that described reaction vessel is teflon microwave supercharging digester.
In a preferred embodiment of the present invention, further comprise that the solvent of clearing up in described step b is that volume ratio is nitric acid, the perchloric acid mixed solution of 3.5 ~ 4.5:1.
In a preferred embodiment of the present invention, further comprise that the solvent of clearing up in described step b is that volume ratio is nitric acid, the perchloric acid mixed solution of 4:1.
In a preferred embodiment of the present invention, further comprise in described mixed solution that nitric acid and perchloric acid are top grade pure.
In a preferred embodiment of the present invention, further comprise that in step b, testing sample is 1:14.45 with the volume mass of clearing up solvent than g/mL.
Usefulness of the present invention is: 1, the method for iron content in Flame Atomic Absorption Spectrometry Determination laver of the present invention, testing sample is placed in to be cleared up solvent and first soaks 30 ~ 50min, make sample and clear up solvent and fully react, can make the iron of indissoluble fully clear up fast
2, utilize microwave heating to assist and clear up, microwave energy directly penetrates sample inside, and inside and outside heating simultaneously, can reach higher temperature moment, shortens digestion time;
3, the Mixed Acids Digestion solvent of designated volume ratio oxidisability under high pressure, sealed environment strengthens greatly, sample reagent is cleared up at short notice, blank value is low, when further shortening digestion time, clear up solvent use amount little, meanwhile, by the environmental pollution of clearing up solvent introducing, also greatly reduced;
4, utilize when microwave heating is auxiliary clears up, for fear of clearing up reaction too violent and micro-leakage occurs, will clear up solvent and divide two stepwise heatings to make to clear up smoothly to complete.
Embodiment
In order to make those skilled in the art person understand better the present invention program, and above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with embodiment, the present invention is further detailed explanation.
A method for iron content in Flame Atomic Absorption Spectrometry Determination laver, comprises the following steps:
A. the collection of sample: commercially available wild laver is cleaned to the air-dry clean container of putting into, clean container is put into temperature dries to permanent quality at the constant temperature oven of 80 ~ 85 ℃, use mortar grind into powder, obtain laver sample after crossing 80 mesh sieves, be placed in exsiccator, preserve stand-by;
B. Specimen eliminating is processed: accurately take laver sample, be placed in reaction vessel, to adding in reaction vessel, quantitatively clear up solvent soaking 45 ~ 50min, after sealing, be placed in micro-wave oven and first use " low fire screen " heating and decompose 2min, use again " in high fire screen " heating and decompose 4min, take out reaction vessel after test solution is cooled to room temperature, with neutral filter paper, test solution is crossed to leaching filtrate, be placed in volumetric flask stand-by;
C. the preparation of sample solution: add redistilled water to be settled to scale in volumetric flask, be mixed with sample solution;
D. blank solution preparation: with step b, but only add the solvent of clearing up with step b equivalent, in micro-wave oven, after heating, take out reaction vessel to be cooled to room temperature, taking out blank test solution is placed in the volumetric flask with step c intermediate size, in volumetric flask, add redistilled water constant volume to determine scale, be mixed with blank solution standby;
E. standard solution preparation: the nitric acid that the concentration of take is 1% is thinning agent, the iron titer of 1mg/mL is mixed with to variable concentrations standard solution standby;
F. iron content in Instrument measuring waste gas, described instrument comprises: flame atomic absorption spectrophotometer, iron atom spectrum lamp, design parameter arranges as follows:
Lamp current: 6.0mA
Spectral band-width: 0.2nm
Burner height: 7mm
Air mass flow: 8.0mL/min
Acetylene gas flow: 1.5 L/min
Wavelength: 248.3nm
G. with blank solution calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and testing sample solution, drawing standard curve, measures the content of iron.
Preferably, reaction vessel is teflon microwave supercharging digester, it can give the environment that high temperature, high pressure, sealing are provided of clearing up of sample, in digester, in testing sample, the iron of indissoluble can quick, maximizedly be cleared up, thereby improve the accuracy of measuring, accelerate the speed of whole mensuration, shorten experimental period.
Preferably, the solvent of clearing up in step b is that volume ratio is nitric acid, the perchloric acid mixed solution of 3.5 ~ 4.5:1, the acid mixture that the present invention adopts special ratios as clear up reagent with respect to traditional simple with nitric acid as clearing up reagent, digestion effect is good, the recovery is high, the use amount of reagent is few, and the environmental pollution of introducing greatly reduces.
Preferably, the solvent of clearing up in step b is that volume ratio is nitric acid, the perchloric acid mixed solution of 4:1, through experiment repeatedly, when the volume ratio of acid mixture is 4:1, under set experiment condition, can obtain transparent digestion solution, and digestion effect is good, and the recovery is high.
Preferably, clearing up in the mixed solution of reagent nitric acid and perchloric acid, to be top grade pure, and purity is high, and oxidisability is strong.
Preferably, in step b, testing sample is 1:14.45 with the volume mass of clearing up solvent than g/mL.
Embodiment 1:
Commercially available wild laver is cleaned to the air-dry clean container of putting into, clean container is put into temperature and at the constant temperature oven of 80 ~ 85 ℃, dry to permanent quality, use mortar grind into powder, excessively after 80 mesh sieves, obtain laver sample, accurately take 1.38g laver sample, put into teflon microwave supercharging digester, adding volume ratio is the nitric acid of 4:1, perchloric acid mixed solution 20mL soaks 45 ~ 50min, then after digester being sealed, be placed in micro-wave oven and first use " low fire screen " heating and decompose 2min, use again " in high fire screen " heating and decompose 4min, after taking out reaction vessel, in fuming cupboard, be cooled to room temperature, twist the lid off, check that obtaining digestion solution is transparence, with neutral filter paper, test solution is crossed to leaching filtrate and be placed in 50mL volumetric flask, in volumetric flask, add redistilled water dilution to be settled to scale again, be configured to sample solution.
Preparation blank solution: to add volume ratio in the teflon microwave supercharging digester of laver sample be the nitric acid of 3.5:1, the mixed solution of perchloric acid 20mL to not placing, then after digester being sealed, be placed in micro-wave oven and first use " low fire screen " heating and decompose 2min, use again " in high fire screen " heating and decompose 4min, after taking out reaction vessel, in fuming cupboard, be cooled to room temperature, twist the lid off, remove test solution and be placed in 50mL volumetric flask, in volumetric flask, add redistilled water dilution to be settled to scale again, be mixed with blank solution.
Preparing standard solution drawing standard working curve: the nitric acid that the concentration of take is 1% is thinning agent, be mixed with the iron titer (being provided by State center for standard matter) of 1mg/mL respectively that concentration A is 0.0,1.0,2.0,3.0,4.0, the series standard solution of 5.0ug/mL.
Above-mentioned blank solution is measured according to above-mentioned set parameter with Japanese Shimadzu 6800 type flame atomic absorption spectrophotometers (attached computing machine and printer), proofread and correct spectrometer zero point, sequentially determining series standard solution again, instrument automatic data processing, and display standard curve, the absorbance result recording is as follows: C=-0.2045,5.2493,11.0631,16.6969,22.3307,27.9645
According to the corresponding relation of A and C, by Mathematical Fitting, obtain an equation of linear regression, as follows:
A=0.1775C+0.0363, related coefficient is r=0.9978.
Under arranging, above-mentioned same parameters carries out the mensuration of sample solution, prepare 6 parts of parallel sample solutions and digestion solution, by the absorbance of ferro element in spectrometer difference working sample, according to equation of linear regression, calculate respectively the content of ferro element in this 6 duplicate samples, average.The iron content recording is respectively: 553.61ug/g, 548.92 ug/g, 552.39 ug/g, 554.36 ug/g, 551.08 ug/g, 553.46 ug/g, and calculating mean value is 552.30 ug/g, the content that draws iron in laver is 552.30 ug/g.
Embodiment 2
Only be with the difference of embodiment 1: add to clear up the volume ratio of nitric acid and perchloric acid in solvent be 3.5:1, after twisting the lid off, check the digestion solution shape that is translucent.
Other experiment condition is consistent with embodiment 1, prepares 6 parts of parallel sample solutions and digestion solution, by the absorbance of ferro element in spectrometer difference working sample, calculates respectively the content of ferro element in this 6 duplicate samples according to equation of linear regression, averages.The iron content recording is respectively: 542.38 ug/g, 539.43 ug/g, 540.42 ug/g, 541.08 ug/g, 540.29 ug/g, 552.41 ug/g, calculating mean value is 542.67 ug/g, relative embodiment 1, in the laver recording, the content of ferro element is on the low side, comprehensive analysis, clearing up under solvent of the nitric acid that to draw in volume ratio be 3:1 and perchloric acid, iron dissolves completely.
Embodiment 3
Only be with the difference of embodiment 1: add to clear up the volume ratio of nitric acid and perchloric acid in solvent be 4.5:1, after twisting the lid off, check, digestion solution is transparence.
Other experiment condition is consistent with embodiment 1, prepares 6 parts of parallel sample solutions and digestion solution, by the absorbance of ferro element in spectrometer difference working sample, calculates respectively the content of ferro element in this 6 duplicate samples according to equation of linear regression, averages.The iron content recording is respectively: 553.48 ug/g, 549.32 ug/g, 551.89 ug/g, 554.73 ug/g, 551.23 ug/g, 553.26 ug/g, calculating mean value is 552.31 ug/g, record result and embodiment 1 is consistent, illustrate that clearing up in solvent ferro element when the volume ratio of nitric acid and perchloric acid is 4:1 dissolves completely, in order not waste, to clear up solvent and reduce the pollution to environment simultaneously, optimal proportion of the present invention is 4:1.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not limited by the examples; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify and all should be equivalent substitute mode, within being included in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claim was defined.
Claims (6)
1. a method for iron content in Flame Atomic Absorption Spectrometry Determination laver, is characterized in that: comprise the following steps:
A. the collection of sample: commercially available wild laver is cleaned to the air-dry clean container of putting into, clean container is put into temperature dries to permanent quality at the constant temperature oven of 80 ~ 85 ℃, use mortar grind into powder, obtain laver sample after crossing 80 mesh sieves, be placed in exsiccator, preserve stand-by;
B. Specimen eliminating is processed: accurately take laver sample, be placed in reaction vessel, to adding in reaction vessel, quantitatively clear up solvent soaking 45 ~ 50min, after sealing, be placed in micro-wave oven and first use " low fire screen " heating and decompose 2min, use again " in high fire screen " heating and decompose 4min, take out reaction vessel after test solution is cooled to room temperature, with neutral filter paper, test solution is crossed to leaching filtrate, be placed in volumetric flask stand-by;
C. the preparation of sample solution: add redistilled water to be settled to scale in volumetric flask, be mixed with sample solution;
D. blank solution preparation: with step b, but only add the solvent of clearing up with step b equivalent, in micro-wave oven, after heating, take out reaction vessel to be cooled to room temperature, taking out blank test solution is placed in the volumetric flask with step c intermediate size, in volumetric flask, add redistilled water constant volume to determine scale, be mixed with blank solution standby;
E. standard solution preparation: the nitric acid that the concentration of take is 1% is thinning agent, the iron titer of 1mg/mL is mixed with to variable concentrations standard solution standby;
F. iron content in Instrument measuring waste gas, described instrument comprises: flame atomic absorption spectrophotometer, iron atom spectrum lamp, design parameter arranges as follows:
Lamp current: 6.0mA
Spectral band-width: 0.2nm
Burner height: 7mm
Air mass flow: 8.0mL/min
Acetylene gas flow: 1.5 L/min
Wavelength: 248.3nm
G. with blank solution calibration flame atomic absorption spectrophotometer zero point, the absorbance of bioassay standard solution and testing sample solution, drawing standard curve, measures the content of iron.
2. the method for iron content in Flame Atomic Absorption Spectrometry Determination laver according to claim 1, is characterized in that: described reaction vessel is teflon microwave supercharging digester.
3. the method for iron content in Flame Atomic Absorption Spectrometry Determination laver according to claim 2, is characterized in that: the solvent of clearing up in described step b is that volume ratio is nitric acid, the perchloric acid mixed solution of 3.5 ~ 4.5:1.
4. the method for iron content in Flame Atomic Absorption Spectrometry Determination laver according to claim 3, is characterized in that: the solvent of clearing up in described step b is that volume ratio is nitric acid, the perchloric acid mixed solution of 4:1.
5. the method for iron content in Flame Atomic Absorption Spectrometry Determination laver according to claim 4, is characterized in that: in described mixed solution, to be top grade pure for nitric acid and perchloric acid.
6. the method for iron content in Flame Atomic Absorption Spectrometry Determination laver according to claim 1, is characterized in that: in step b, testing sample is 1:14.45 with the mass volume ratio g/mL that clears up solvent.
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| CN104406926A (en) * | 2014-11-28 | 2015-03-11 | 苏州东辰林达检测技术有限公司 | Detection method of trace methylmercury in alga |
| CN104865211A (en) * | 2015-06-19 | 2015-08-26 | 贵州出入境检验检疫局检验检疫综合技术中心 | Method for efficiently measuring content of Cu, Fe, Mn and Ca in cereal food |
| CN108700495A (en) * | 2016-03-09 | 2018-10-23 | 本田技研工业株式会社 | The leakage detection method of opening emission analysis and opening emission analysis device |
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| CN108254244A (en) * | 2017-11-20 | 2018-07-06 | 包头东宝生物技术股份有限公司 | The assay method and processing method of tenor in gelatin |
| CN108254244B (en) * | 2017-11-20 | 2020-11-27 | 包头东宝生物技术股份有限公司 | Method for measuring and processing metal content in gelatin |
| CN110082183A (en) * | 2019-05-20 | 2019-08-02 | 内蒙古蒙牛乳业（集团）股份有限公司 | The detection method of microelement in milk powder |
| CN111257247A (en) * | 2019-11-22 | 2020-06-09 | 浙江省海洋水产研究所 | Method for measuring iron content in marine sediments |
| CN111257247B (en) * | 2019-11-22 | 2023-04-18 | 浙江省海洋水产研究所 | Method for measuring iron content in marine sediments |
| CN111089778A (en) * | 2020-02-11 | 2020-05-01 | 河南省奥林特药业有限公司 | Method for measuring iron content of liver essence and hematinic oral liquid |
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