CN104749120A - Method for measuring content of arsenic in edible oil by utilizing super-microwave digestion graphite furnace atomic absorption spectrometry - Google Patents
Method for measuring content of arsenic in edible oil by utilizing super-microwave digestion graphite furnace atomic absorption spectrometry Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of arsenic in edible oil by utilizing a super-microwave digestion graphite furnace atomic absorption spectrometry. The method disclosed by the invention comprises the following steps: performing super-microwave digestion on an edible oil sample by adopting a transparent and stable quartz tube, and measuring the content of the arsenic in the edible oil by utilizing the graphite furnace atomic absorption spectrometry. According to the method, a super-microwave technology is applied to measuring the trace arsenic in the edible oil, the operation is safe and easy, the digestion capacity is high, the edible oil samples can be simply and efficiently digested, the target analyte loss and pollution caused by the transfer process can be effectively eliminated, potassium borohydride and other substances with high toxicity are not needed, and the graphite furnace atomic absorption spectrometry is further combined to be applied to measuring the trace arsenic in the edible oil. According to the method disclosed by the invention, the linearity range ranges from 0 to 40ng/mL, the quantification limit is 0.033mg/kg, and the recovery rate is 86.8-101.4 percent. The operation is easy, accurate, rapid and sensitive, the content of the arsenic in the edible oil can be accurately measured, and the body health of consumers can be effectively guaranteed.
Description
Technical field
The present invention relates to technical field of food detection, be specifically related to a kind of method measuring Determination of Arsenic in Edible Oil content, more specifically, relate to a kind of method utilizing super micro-wave digestion GFAAS (graphite furnace atomic absorption spectrometry) to measure Determination of Arsenic in Edible Oil content.
Background technology
Edible oil is the necessity of daily life, its quality safety and ours is healthy closely bound up.Heavy metal pollution is originated waste residue, the industrial waste water of metallurgy, chemical industry, agricultural chemicals, dyestuff and process hides etc. and the waste water etc. of geothermal power plant of mainly digging up mine, smelting.These reasons likely can make the heavy metal element in the oil crops such as peanut, soybean, vegetable seed planted exceed standard.In addition, edible oil, in production, processing, transport, storage process, is also likely subject to the pollution of heavy metal.Arsenic is the heavy metal element that a kind of toxicity is very large, and now there are some researches show that arsenic has damage in various degree to the cardiac muscle of people, breathing, reproduction, hematopoiesis, immune system, easily accumulate in human body, not easily discharge, long term accumulation causes slow poisoning.Arsenic limitation has strict restriction in food, is listed in the harmful element of emphasis supervision.In GB 2762-2012 " pollutants in food limitation " regulation grease and goods thereof, the limitation of total arsenic is 0.1mg/kg.GB 2716-2005 " edible vegetable oil hygienic standard " specifies the arsenic limitation 0.1mg/kg in edible vegetable oil.
In GB/T 5009.11-2003, the detection technique of arsenic mainly comprises atomic fluorescence spectrometry, silver salt method, arsenic spot method and colourimetry, and wherein, the interference of silver salt method, arsenic spot method and colourimetry is large, and sensitivity is low, is unsuitable for the mensuration of trace element.Although atomic fluorescence method is highly sensitive, complex operation, need to use the larger solution of potassium borohydride of toxicity to carry out prereduction, and prereduction needs to place at least 30min, also can produce the larger arsine gas of toxicity in process of the test.
The limitation of Determination of Arsenic in Edible Oil is defined as 0.1mg/kg.5.6 joint regulations in CNAS-CL10:2012, standard specimen used should cover the concentration range of sample, and the standard specimen of least concentration should in the level of proximity test method report limit.Oil sample is difficult to clear up, and reaction is comparatively violent, and during micro-wave digestion, sample sample weighting amount is generally no more than 0.3g, existing wet method or micro-wave digestion, needs digestion solution deionized water to shift constant volume, and constant volume is generally at least 25mL.If the report of sample is defined as the highest limitation 0.1mg/kg of Determination of Arsenic in Edible Oil, by CL10 standard specimen least concentration regulation, least concentration point is 1.2 ng/mL, and the absorption signal of this concentration point is very weak, and precision is poor, causes standard curve fit coefficient not reach requirement.
In addition, it is teflon material that conventional microwave clears up tank body, when clearing up edible oil there is the problem such as quick-fried tank or jar distortion in solution, and tank body is larger, large water gaging is needed to rinse during transfer, easily cause the excess dilution of object element or shift not exclusively, being unsuitable for the sample test that object element content is lower.In addition to clear up operation more loaded down with trivial details for conventional microwave, and tank body cleared up by teflon also should not observe Specimen eliminating effect in tank body.
In sum, the detection of existing Determination of Arsenic in Edible Oil content usually adopts conventional microwave to clear up and realizes in conjunction with atomic fluorescence method, but there is complex operation, rinse tank body produce excess dilution or shift the situation such as incomplete, not easily observe, expensive, use in the larger prereduction solution of toxicity, testing process and produce the defects such as the larger gas of toxicity, detection time be long.
Super micro-wave digestion is the new technology just occurred in recent years, has the advantages such as easy, quick, efficient, free of losses.Apply that super microwave digesting technology can overcome that conventional microwave clears up should not observe, the explosive tank of counteracting tank, the shortcoming such as expensive, but super microwave digestion technology is not applied to the correlative study carrying out the digestion pre-treatment that trace arsenic detects in oils sample and technology report at present, has no the correlation technique super micro-wave digestion and follow-up characterization processes being organically combined the technical scheme of acquisition science entirety yet and report.
Summary of the invention
The technical problem to be solved in the present invention detects the technical deficiency of Determination of Arsenic in Edible Oil content, provides a kind of method utilizing super micro-wave digestion GFAAS (graphite furnace atomic absorption spectrometry) to measure Determination of Arsenic in Edible Oil content.
Goal of the invention of the present invention is achieved by the following technical programs:
A kind of method measuring Determination of Arsenic in Edible Oil content by super micro-wave digestion-GFAAS (graphite furnace atomic absorption spectrometry) (UltraWAVE Digestion-GF-AAS) is provided, comprises the following steps:
S1. the super micro-wave digestion pre-treatment of sample, obtains digestion solution;
S2. S1 gained digestion solution is caught up with acid, be directly settled to suitable scale with deionized water, mixing, as sample solution;
S3. arsenic content in S2 gained sample solution is detected;
Wherein, described in S1, super micro-wave digestion pre-treatment comprises the following steps:
S11. adopt the design of single reaction chamber, all clearing up in reaction tube inserts in large microwave operational chamber, can clear up 1 ~ 22 sample simultaneously; The large reaction chamber of UltraWAVE adds 130mL water+5mL H
2o
2(described H
2o
2for UP level, massfraction is 30%);
S12. take edible oil sample and be about 0.3g(exact value 0.001g) clear up in reaction tube in the 15mL of three scales, add 3mL nitric acid, cover TFM lid, placement is spent the night;
Clearing up in reaction tube after S13. spending the night toward S12 placement adds a small amount of deionized water in potpourri, cover lid, then sample holder is put into, be placed in super microwave dissolver, locking tank body, pre-add inert gas (nitrogen), pressure 40bar, outer cavity temperature≤40 DEG C, setting heating schedule, clears up; Do blank test simultaneously.
Described blank test is add 3mL nitric acid and a small amount of water in the blank quartz digestion pipe of edible oil, and other step is identical with the disposal route of sample.
Acid is caught up with to be that digestion solution is caught up with acid about 20min in 110 DEG C described in S2; Directly 10mL is settled to, as sample solution with deionized water;
Detecting described in S3 is adopt electrodeless discharge lamp, Zeeman background correction, with the mixed liquor of palladium nitrate and magnesium nitrate for matrix modifier, adopts GFAAS (graphite furnace atomic absorption spectrometry), according to the content of arsenic in standard curve determination sample solution.
The super micro-wave digestion pre-treatment of sample described in S1 adopts quartz digestion reaction tube (quartz digestion pipe).Preferably, described quartz digestion pipe has different specifications, with scale mark, and such as, quartz digestion pipe with 5mL, 10mL, 15mL scale mark.
Heating schedule described in S13 is divided into three steps, and the first step is room temperature to 120 DEG C, time 8min, pressure 120bar; Second step is 120 ~ 210 DEG C, time 8min, pressure 150bar; 3rd step is 210 DEG C, time 10min, pressure 150bar.The power of three steps is 1500W.
After clearing up complete cooling release, catch up with acid, with the direct constant volume of deionized water, mixing.As sample solution, treat that machine measures.
Preferably, the condition of work of GFAAS (graphite furnace atomic absorption spectrometry) described in S3 is: wavelength: 193.7nm; Lamp current: 380mA; Spectral bandwidth: 0.7nm; Argon flow amount 250mL/min; Atomization is stopped the supple of gas or steam.Sample feeding amount 20 μ L, matrix modifier 5 μ L.Matrix modifier is the mixed solution of 1g/L palladium (palladium nitrate matrix) and 0.6 g/L magnesium nitrate.Graphite furnace heating schedule: room temperature ~ 110 DEG C, heating-up time 1s, keeps 30 s; 110 DEG C ~ 130 DEG C, heating-up time 15 s, keeps 30 s; Ashing: 1200 DEG C, heating-up time 10s, keeps 20 s; Atomization: 2000 DEG C, heating-up time 0s, keeps 5 s; Purify 2450 DEG C, heating-up time 1s, keep 3s.Adopt auto injection, advanced sample liquid, laggard matrix modifier.Sample liquid is followed successively by standard solution, blank solution and sample solution in order.
Preferably, being settled to suitable scale described in S2 is that the content range estimated according to target analytes determines immediate constant volume scale, such as to the lower sample of target analytes content can constant volume to comparatively down scale, avoid the excess dilution of repeatedly rinsing during conventional transfer target analytes, effectively can also eliminate target analytes loss that transfer process causes and pollute.
Preferably, the method for drafting of standard working curve described in S3 is:
Be 1%HNO by volume ratio
31000mg/L arsenic standard solution (national standard reagent) stepwise dilution is become the arsenic Standard Applying Solution of 5 μ g/L and 50 μ g/L.By setting cup position, Standard Applying Solution, dilution and matrix modifier are poured in each sample cup respectively, be placed in sample disc.It is 2.5,5 that Standard Applying Solution dilutes by instrument automatically, the standard series of 10,20,40 μ g/L, and automatically adds matrix modifier 5 μ L.Matrix modifier is 1g/L palladium (palladium nitrate matrix) and 0.6 g/L magnesium nitrate mixed liquor.The absorbance of measurement standard series under the condition of work of instrument setting, and automatic drawing curve.Obtain regression equation A=0.00422C+0.00119, r=0.9997.C is concentration, and A is absorbance, and r is linearly dependent coefficient.Standard working solution matching while using.
Compared with prior art, beneficial effect of the present invention is:
Science of the present invention provides total solution, reasonable setting is cleared up and testing conditions, play super microwave digesting technology be easy to observe, the advantage such as lower, the handling safety of cost, successfully super microwave digesting technology is applied to the digestion pre-treatment that in oils sample, trace arsenic detects.
The present invention, further combined with the test using GFAAS (graphite furnace atomic absorption spectrometry) to carry out arsenic content, ensure that whole detection technical scheme is highly sensitive, reagent dosage is few, simple to operate, testing result accurate, and effective guarantee edible oil quality safety.
Adopt the super microwave digestion method in the inventive method to carry out pre-treatment, sample sample weighting amount is also 0.3g, equally report is defined as maximum limitation 0.1mg/kg.If sample solution is settled to 5mL, by CL 10 standard specimen least concentration regulation, then typical curve least concentration point is 6ng/mL; If be settled to 10mL, least concentration point is 3ng/mL.Lowest bid concentration on schedule obviously increases, signal response obviously strengthens, significantly improve sensitivity and the accuracy of method, see shown in accompanying drawing 1 by arsenic concentration for 2.5ng/mL and 1.0ng/mL Atomic absorption responds comparison diagram, the Atomic absorption response curve of the curve that in accompanying drawing 1, display response obviously strengthens to be arsenic concentration be 2.5ng/mL.Specific aim solve existing correlation detection technology complex operation, rinse tank body produce excess dilution or transfer not exclusively, the not easily defect such as observation.
On the whole, the invention provides a kind of method measuring Determination of Arsenic in Edible Oil content by super micro-wave digestion-GFAAS (graphite furnace atomic absorption spectrometry) (UltraWAVE Digestion-GF-AAS), first by the mensuration of super microwave technique application trace arsenic in edible oil.Relative to existing common microwave digestion technology, the present invention's operation is more simple, clears up ability stronger, can clear up edible oils sample simply, efficiently; The present invention adopts transparent, stable quartz ampoule, the polytetrafluoroethyltank tank in relative conventional microwave counteract appearance, and the quartz digestion pipe price in super microwave dissolver is cheaper, also more easily observes and clears up effect.The present invention designs the quartz digestion pipe of the different scale mark of band 5mL, 10mL, 15mL, after having cleared up, digestion solution is directly settled to scale after catching up with acid, according to the actual content scope of arsenic in sample, direct deionized water is settled to suitable scale, as sample solution, then carry out the test of arsenic content in sample solution by GFAAS (graphite furnace atomic absorption spectrometry); To the lower sample of target analytes content can constant volume to comparatively down scale, repeatedly rinse the excess dilution to target analytes when avoiding conventional transfer; Effectively can also eliminate target analytes loss that transfer process causes and pollute.Combination of sciences GFAAS (graphite furnace atomic absorption spectrometry) of the present invention carries out the test of Determination of Arsenic in Edible Oil content, relative to conventional hydride generation atomic fluorescence spectrometry, the inventive method operation is easier, quick, and without the need to materials such as the potassium borohydrides that uses toxicity larger.
The inventive method range of linearity 0 ~ 40ng/mL, is quantitatively limited to 0.033mg/kg, the recovery 86.8% ~ 101.4%.The method is simple to operate, accurate, quick, sensitive, can the content of Accurate Determining Determination of Arsenic in Edible Oil, and effective guarantee consumer is healthy.
Accompanying drawing explanation
Fig. 1 arsenic concentration is 2.5ng/mL and 1.0ng/mL Atomic absorption response comparison diagram.
Fig. 2 the inventive method standard working curve.
Embodiment
The inventive method is further illustrated below in conjunction with the drawings and specific embodiments.Following embodiment and accompanying drawing, only for exemplary illustration, can not be interpreted as limitation of the present invention.Unless stated otherwise, the biomaterial used in following embodiment, reagent raw material for routine is commercial or commercial sources obtain biomaterial and reagent raw material, unless stated otherwise, the method and apparatus that the method and apparatus used in following embodiment uses for this area routine.
embodiment 1
The all glass waress of the present embodiment all need soak 24h in 20%HNO3, repeatedly rinse with water, finally dry rear use with deionized water rinsing.All reagent be top grade pure more than.
The present embodiment provides a kind of super micro-wave digestion-GFAAS (graphite furnace atomic absorption spectrometry) to measure the method for Determination of Arsenic in Edible Oil content, and concrete steps are as follows:
S1. sample is carried out super micro-wave digestion pre-treatment, obtain digestion solution;
S2. after clearing up complete cooling release, take out digest tube, catch up with acid about 15min, be directly settled to 10mL scale with deionized water for 110 DEG C, mixing, to be measured.
S3. arsenic content in S2 gained sample solution is detected;
Wherein, the super micro-wave digestion of super micro-wave digestion pre-treatment of sample described in S1 comprises the following steps:
S11. adopt the design of single reaction chamber, all clearing up in reaction tube inserts in large microwave operational chamber, can clear up 1 ~ 22 sample simultaneously; The large reaction chamber of UltraWAVE adds 130mL water+5mL H
2o
2(described H
2o
2for UP level, massfraction is 30%);
S12. take edible oil sample and be about 0.3g(exact value 0.001g) in the 15mL quartz digest tube of three scales, add 3mL nitric acid, cover TFM lid, placement is spent the night;
S13. a small amount of deionized water is added in potpourri in placing the quartzy digest tube after spending the night toward S12, cover lid, then sample holder is put into, be placed in super microwave dissolver, locking tank body, pre-add inert gas (nitrogen), pressure 40bar, outer cavity temperature≤40 DEG C, set heating schedule as shown in table 1, clear up; Do blank test simultaneously.
The super microwave heating schedule of table 1
| Step | Temperature/DEG C | Time/min | Pressure/bar | Power/W |
| 1 | 120 | 8 | 120 | 1500 |
| 2 | 210 | 8 | 150 | 1500 |
| 3 | 210 | 10 | 150 | 150 |
Blank test is add 3mL nitric acid and a small amount of water in the blank quartz digestion pipe of edible oil, and other step is identical with the disposal route of sample.
The instrument condition of work detected described in S3 is as follows:
AA800 atomic absorption spectrophotometer (AAS), joins original-pack end-window graphite-pipe, arsenic electrodeless discharge lamp; Wavelength: 193.7nm; Lamp current: 380mA; Spectral bandwidth: 0.7nm; Argon flow amount 250mL/min, atomization is stopped the supple of gas or steam.Sample feeding amount 20 μ L, matrix modifier 5 μ L.Matrix modifier is the mixed liquor of 1g/L palladium (palladium nitrate matrix) and 0.6 g/L magnesium nitrate.Mensuration mode: integrating peak areas.
Optimum temperature rise program is shown in Table 2:
Table 2 graphite furnace heating schedule
| Step | Temperature/DEG C | Heating-up time/min | Retention time/min |
| 1 | 110 | 1 | 30 |
| 2 | 130 | 15 | 30 |
| 3 | 1200 | 10 | 20 |
| 4 | 2000 | 0 | 5 |
| 5 | 2450 | 1 | 3 |
Drawing standard working curve:
Be 1%HNO by volume ratio
31000mg/L arsenic standard solution (national standard reagent) stepwise dilution is become the arsenic Standard Applying Solution of 5 μ g/L and 50 μ g/L.By setting cup position, Standard Applying Solution, dilution and matrix modifier are poured in each sample cup respectively, be placed in sample disc.It is 2.5,5 that Standard Applying Solution dilutes by instrument automatically, the standard series of 10,20,40 μ g/L, and automatically adds matrix modifier 5 μ L.Matrix modifier is 1g/L palladium (palladium nitrate matrix) and 0.6 g/L magnesium nitrate mixed liquor.The absorbance of measurement standard series under the condition of work of instrument setting, and automatic drawing curve.Obtain regression equation A=0.00422C+0.00119, r=0.9997.C is concentration, and A is absorbance, and r is linearly dependent coefficient.Standard working solution matching while using.
Complete sample tests: determine arsenic concentration in sample solution by Atomic Absorption Spectrometry condition, foundation samples quality and constant volume calculates arsenic content.
The accuracy experiment of embodiment 2 the inventive method:
Take about 0.3g edible oil sample (accurately to 0.001g) in quartz digestion pipe, add 3mL red fuming nitric acid (RFNA).Adding 0.10mL, 0.30mL and 1.0mL concentration is more respectively 100ng/mL arsenic standard solution, i.e. 1ng/mL, 3ng/mL, 10ng/mL tri-concentration level recovery testu, and each concentration level and sample background all carry out six parallel testings.Do blank test simultaneously.Placement is spent the night, and adds a small amount of deionized water, covers teflon lid, puts into specimen mounting and super microwave dissolver.Locking tank body, pre-add inert gas (nitrogen), pressure 40bar, outer cavity temperature≤40 DEG C, setting heating schedule (being shown in Table 1) is cleared up.Carry out the drafting of standard working curve according to instrument condition of work, then carry out the test of arsenic content in blank and sample solution.Background and mark-on are tested identical with Specimen Determination method, and mark-on reclaims and the results are shown in Table shown in 3:
Table 3 Determination of Arsenic in Edible Oil mark-on reclaims test result: (n=6)
As shown in Table 3, the recovery of the inventive method is 86.8% ~ 101.3%, and arsenic content range is 0.033 mg/kg ~ 0.33mg/kg, meets GB/T 27404-2008 " Good Laboratory controls specification food Physico-chemical tests " recovery requirement.
As shown in Table 3, the precision of the inventive method is 2.9% ~ 13%, and arsenic content range is 0.033mg/kg ~ 0.33mg/kg, meets GB/T 27404-2008 " Good Laboratory controls specification food Physico-chemical tests " precision requirement.
The present invention's super micro-wave digestion-GFAAS (graphite furnace atomic absorption spectrometry) (UltraWAVE Digestion-GF-AAS) measures the method for Determination of Arsenic in Edible Oil content, first by the mensuration of super microwave technique application trace arsenic in edible oil.Relative to existing common microwave digestion technology, the present invention's operation is more simple, clears up ability stronger, can clear up edible oils sample simply, efficiently; The present invention adopts transparent, stable quartz ampoule, the polytetrafluoroethyltank tank in relative conventional microwave counteract appearance, and the quartz digestion pipe price in super microwave dissolver is cheaper, also more easily observes and clears up effect.The present invention designs the quartz digestion pipe of the different scale mark of band 5mL, 10mL, 15mL, after having cleared up, digestion solution is directly settled to scale after catching up with acid, according to the actual content scope of arsenic in sample, direct deionized water is settled to suitable scale, as sample solution, then carry out the test of arsenic content in sample solution by GFAAS (graphite furnace atomic absorption spectrometry); To the lower sample of target analytes content can constant volume to comparatively down scale, repeatedly rinse the excess dilution to target analytes when avoiding conventional transfer; Effectively can also eliminate target analytes loss that transfer process causes and pollute.Combination of sciences GFAAS (graphite furnace atomic absorption spectrometry) of the present invention carries out the test of Determination of Arsenic in Edible Oil content, relative to conventional hydride generation atomic fluorescence spectrometry, the inventive method operation is easier, quick, and without the need to materials such as the potassium borohydrides that uses toxicity larger.
Claims (7)
1. utilize super micro-wave digestion GFAAS (graphite furnace atomic absorption spectrometry) to measure a method for Determination of Arsenic in Edible Oil content, it is characterized in that, comprise the following steps:
S1. sample is carried out super micro-wave digestion pre-treatment, obtain digestion solution;
S2. after S1 gained digestion solution being caught up with acid, direct deionized water is settled to scale, and mixing, as sample solution;
S3. arsenic content in S2 gained sample solution is detected;
Wherein, described in S1, super micro-wave digestion pre-treatment comprises the following steps:
S11. adopt the design of single reaction chamber, all clearing up in reaction tube inserts in large microwave operational chamber, and large reaction chamber adds 130mL water and 5mL H
2o
2;
S12. taking edible oil sample 0.3g clears up in reaction tube in the 15mL of three scales, and add 3mL nitric acid, cover lid, placement is spent the night; Described reaction tube of clearing up is quartz digestion reaction tube;
S13. place the potpourri in reaction tube of clearing up after spending the night toward S12 and add a small amount of deionized water, cover lid, then put into sample holder, be placed in super microwave dissolver, locking tank body, pre-add inert gas, pressure 40bar, outer cavity temperature≤40 DEG C, setting heating schedule, clears up; Do blank test simultaneously;
Heating schedule described in S13 is divided into three steps, and the first step is room temperature to 120 DEG C, time 8min, pressure 120bar; Second step is 120 ~ 210 DEG C, time 8min, pressure 150bar; 3rd step is 210 DEG C, time 10min, pressure 150bar; The power of three steps is 1500W;
Detecting described in S3 is adopt electrodeless discharge lamp, Zeeman background correction, with the mixed liquor of palladium nitrate and magnesium nitrate for matrix modifier, adopts GFAAS (graphite furnace atomic absorption spectrometry), according to the content of arsenic in standard curve determination sample solution.
2. utilize super micro-wave digestion GFAAS (graphite furnace atomic absorption spectrometry) to measure the method for Determination of Arsenic in Edible Oil content according to claim 1, it is characterized in that, S1 clears up 1 ~ 22 sample simultaneously.
3. utilize super micro-wave digestion GFAAS (graphite furnace atomic absorption spectrometry) to measure the method for Determination of Arsenic in Edible Oil content according to claim 1, it is characterized in that, described in S13, quartz digestion pipe is provided with different scale mark.
4. utilize super micro-wave digestion GFAAS (graphite furnace atomic absorption spectrometry) to measure the method for Determination of Arsenic in Edible Oil content according to claim 1, it is characterized in that, blank test described in S13 is add 3mL nitric acid and a small amount of water in the blank quartz digestion pipe of edible oil, and other step is identical with the disposal route of sample.
5. utilize super micro-wave digestion GFAAS (graphite furnace atomic absorption spectrometry) to measure the method for Determination of Arsenic in Edible Oil content according to claim 1, it is characterized in that, described in S2, catch up with acid to be that digestion solution is caught up with acid about 20min in 110 DEG C; Directly 10mL is settled to, as sample solution with deionized water.
6. utilize super micro-wave digestion GFAAS (graphite furnace atomic absorption spectrometry) to measure the method for Determination of Arsenic in Edible Oil content according to claim 1, it is characterized in that, the condition of work of GFAAS (graphite furnace atomic absorption spectrometry) described in S3 is: wavelength: 193.7nm; Lamp current: 380mA; Spectral bandwidth: 0.7nm; Argon flow amount 250mL/min; Atomization is stopped the supple of gas or steam; Sample feeding amount 20 μ L, matrix modifier 5 μ L; Matrix modifier is the mixed solution of 1g/L palladium and 0.6 g/L magnesium nitrate; Graphite furnace heating schedule: room temperature ~ 110 DEG C, heating-up time 1s, keeps 30 s; 110 DEG C ~ 130 DEG C, heating-up time 15 s, keeps 30 s; Ashing: 1200 DEG C, heating-up time 10s, keeps 20 s; Atomization: 2000 DEG C, heating-up time 0s, keeps 5 s; Purify 2450 DEG C, heating-up time 1s, keep 3s; Adopt auto injection, advanced sample liquid, laggard matrix modifier; Sample liquid is followed successively by standard solution, blank solution and sample solution in order.
7. utilize super micro-wave digestion GFAAS (graphite furnace atomic absorption spectrometry) to measure the method for Determination of Arsenic in Edible Oil content according to claim 1, it is characterized in that, the method for drafting of standard working curve described in S3 is:
Be 1%HNO by volume ratio
31000mg/L arsenic standard solution stepwise dilution is become the arsenic Standard Applying Solution of 5 μ g/L and 50 μ g/L, Standard Applying Solution, dilution and matrix modifier being poured into respectively in each sample cup by setting cup position, be placed in sample disc, is 2.5 by Standard Applying Solution dilution, 5, the standard series of 10,20,40 μ g/L, and add matrix modifier 5 μ L, matrix modifier is 1g/L palladium and 0.6 g/L magnesium nitrate mixed liquor, the absorbance of measurement standard series, drawing curve.
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