CN105758830A - Method for measuring content of total arsenic by digesting marine product in steps through microwave humidifying method - Google Patents
Method for measuring content of total arsenic by digesting marine product in steps through microwave humidifying method Download PDFInfo
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Abstract
The invention relates to a method for measuring content of total arsenic by digesting a marine product in steps through a microwave humidifying method. The method comprises the following steps: adding nitric acid into a marine product sample, digesting the marine product sample, and carrying out microwave digestion on the marine product sample; cooling, heating and digesting the marine product sample, and adding perchloric acid into the marine product sample to digest after cooling the marine product sample; adding concentrated sulfuric acid to carry out heating and digesting until a solution is colorless, thereby obtaining a digested sample, and preparing a sample solution; drawing a standard curve, adopting an atomic fluorescence spectrometer to test the sample solution, and carrying out conversion to obtain content of the arsenic in the marine product. The method operates in stages, so that each step is programmed, visual, and simple and convenient to judge. A pretreatment method for digesting in steps through the microwave humidifying method is adopted, so that an atomic fluorescence spectroscopy for measuring the total arsenic in the marine product has the effects time- saving, labor saving, and stable and controllable results.
Description
Technical field
The invention belongs to the assay method field of total arsenic content in marine product, add wet method substep particularly to a kind of microwave and clear up the method that marine product measures total arsenic content.
Background technology
Arsenic is that a kind of nature common are poison harmful element, has stronger toxicity, there is carcinogenic teratogenic effect simultaneously.One time Excess free enthalpy arsenic is lethal easily caused by arsenic acute poisoning, and long-term low dose absorption in human body accumulation thus causing arseniasis and bringing out all kinds of dermatosis and lesions of liver and kidney, can cause the attention of people.Arsenic is widely present with compound form in nature, and how poisonous its compound is, and particularly inorganic arsenic toxicity is bigger.Marine organisms (include plant and animal) and can be enriched with arsenic, particularly the biology such as shell, seaweeds, cetacean, and therefore in marine product, the content of arsenic compound is higher, is " arsenic storehouse " in marine environment, are also the human body important sources of taking in arsenic.
The mensuration of arsenic has atomic fluorescence spectrometry, atomic absorption spectrography (AAS), Plasma-Atomic Emission spectrographic method and inductively coupled plasma mass spectrometry etc..The mensuration GB/T5009.11-2003 that standard is national food safety standard total Arsenic in Food and inorganic arsenic (the first method hydride generation atomic fluorescence spectrometry, the second method silver salt method, the 3rd method arsenic speckle method) that in conventional sense marine product, total arsenic is quoted and GB5009.11-2014 (the first method inductively coupled plasma mass spectrometry, the second method hydride generation atomic fluorescence spectrometry) (2015.9.21 issues, and 2016.3.21 implements).
Atomic fluorescence spectrometry is a kind of trace and ultra trace analysis technology, is widely used in hydrogenatable the element such as environment of arsenic, hydrargyrum, food and Metallurgical Analysis.Atomic fluorescence spectrometer (AFS) is the analytical tool that China has independent intellectual property right, it is simpler that this analytical tool has structure, analysis cost is low, highly sensitive, selectivity good, the advantages such as range of linearity width, the long-term detection being extensively used for arsenic by all kinds of sensing chamber, is the instrument recommending in GB and measuring arsenic.
Atomic fluorescence spectrometry principle: sample specimens is after Wet or dry ashing method process, adding thiourea makes pentavalent arsenic prereduction be trivalent arsenic, add potassium borohydride or sodium borohydride makes reduction generate arsenic hydride, it is loaded in quartz atomizer by argon and is decomposed into atomic state arsenic, transmitting at high intensity as hollow cathode lamp excites lower generation atomic fluorescence, its fluorescence intensity is directly proportional to the arsenic concentration in test solution under rigid condition, compares quantitative with standard series.
Principle according to the total arsenic of Atomic Fluorescence Spectrometry, it is necessary to inorganization just can be measured thorough for the arsenide in sample, therefore the total arsenic of the inorganization degree direct influence of sample measures.And the existing forms of arsenic is extremely complex in marine product, marine animal product is primarily present arsenic glycine betaine (AsB) and arsenocholine (AsC), and vegetalitas Sargassum arsenic sugar (AsS) is very abundant, but is absent from arsenic glycine betaine.Containing substantial amounts of organo-arsenic in Thallus Porphyrae and Conch Meretricis seu Cyclinae, in the majority with arsenic sugar and arsenic glycine betaine respectively.So when there is complicated form arsenide in sample, normal wet is cleared up and sample can not be made thoroughly inorganization with micro-wave digestion.For the particularity of arsenic morphology existing way in marine product, measuring value according to the pre-treating method of national standard method Atom fluorescence method lower than standard value, main cause is that pre-treatment is incorrect, the arsenic inside organo-arsenic is not fully extracted when clearing up, need to strengthen sulfuric acid dosage, fully clear up.
National standard method has problems with simultaneously: 1, Wet adopts the strong acid of strong oxidizing property, and reaction is violent, for preventing sample carbonization, it is necessary to constantly observe and add acid, it is necessary to the manual operation of long period, working strength is big；2, consume reagent many, cause environmental pollution big, produce a large amount of harmful gas simultaneously and operator is also damaged to some extent；3, reaction temperature and speed need practical operation to grope, and reaction end judges indefinite, and strong by operator's subjective experience, result is more unstable.
Summary of the invention
The technical problem to be solved is to provide a kind of microwave and adds the method that wet method substep clears up marine product mensuration total arsenic content, and operation makes every step procedure stage by stage, visualization, it is judged that easy.Adopting microwave to add wet method substep to clear up pre-treating method to use the total arsenic in AFS DETERMINATION marine product to reach time saving and energy saving, result stablizes controlled effect.
A kind of microwave of the present invention adds wet method substep and clears up the method that marine product measures total arsenic content, including:
(1) accurately weigh marine product (being accurate to 0.0001g), marine product sample will add nitric acid, and cold clear up, then carry out micro-wave digestion again；
(2) cooling, then heating is cleared up and is caught up with acid to faint yellow, somewhat adds perchloric acid after cooling and carries out clearing up and emerge to white cigarette, and solution is colourless；
(3) adding concentrated sulphuric acid to be heated clearing up, emerge to white cigarette, solution is colourless, obtains Specimen eliminating thing, then prepares sample solution；
(4) drawing standard curve, is then adopted atomic fluorescence spectrometer that sample solution is tested, is obtained the measurement concentration of arsenic in marine product by standard curve, and then conversion obtains arsenic content in marine product again.
In described step (1), digestion time is 1.5h-2.5h.
Step (1) is cleared up and all clears up in micro-wave digestion pipe.
Adding the cold digestion time of nitric acid in described step (1) is 0.5-1h；Micro-wave digestion is: when power is 800-1600W, after being first warming up to 120 DEG C, keeps 5min, after being then warming up to 150 DEG C again, keeps 5min, is finally warming up to 185 DEG C, keeps 15min.
Described step is cooled to 140 DEG C in (2), heating digestion condition (or power) is for being stepped up temperature, rise to 220 DEG C from 140 DEG C to carry out catching up with acid to make solution be faint yellow, total time is 1-2h, heating rate is that every 20min raises 20 DEG C, making to clear up reaction thoroughly not easily lose element to be checked by being stepped up temperature, final solution color is faint yellow；The temperature that addition perchloric acid is cleared up is 200-280 DEG C, time is 30min-1h, reaction color judges that terminal is that in colourless described step (3), heating digestion condition (or power) is as 280-350 DEG C, and the time is 30min-1h, and reaction color judges that terminal is colourless.
In step (2), sample is transferred in triangular flask.
Step (2), (3) are cleared up and carries out on electric hot plate or electric furnace.
Marine product sample, nitric acid, perchloric acid, concentrated sulphuric acid ratio be: 0.1-0.2g (sample is dry sample) or 0.5-2g (sample is fresh sample): 5-8ml:1-2ml:2-3ml.
Preparing sample solution in described step (3) particularly as follows: Specimen eliminating thing proceeds in 50mL volumetric flask or 50mL color comparison tube, add 5mL thiourea+ascorbic acid solution, moisturizing is to scale and mixes, and places 20-30min.
Drawing standard curve in described step (4) particularly as follows: accurately draw 1.00mg/L arsenic standard solution 0.00mL, 0.50mL, 1.00mL, 2.00mL, 4.00mL, 5.00mL respectively in 50ml volumetric flask with pipette, respectively add sulfuric acid solution 25mL, and thiourea+ascorbic acid solution 5mL, benefit adds water to scale, measure after placing 20-30min after mixing, and with atomic fluorescence intensity for vertical coordinate, arsenic concentration is abscissa drawing standard curve.
In step (4), sample solution does blank assay simultaneously.
Described step (4) Atom fluorescence spectrophotometer test parameter is: negative high voltage: 270V, as hollow cathode lamp total current: 60mA, flow rate of carrier gas: 400mL/min, shield gas flow speed: 900mL/min, atomizer height: 8mm.
In step (4), in marine product, the computing formula of arsenic content is:
In formula:
Arsenic content in X-sample, unit is milligrams per kilogram (mg/kg)；
The mensuration concentration of arsenic in C-sample test solution, unit be micro-gram per liter (ug/L)；
C0The mensuration concentration of arsenic in-sample blank Digestive system, unit be micro-gram per liter (ug/L)；
V-sample Digestive system cumulative volume, unit be milliliter (mL)；
M-sample mass, unit is gram (g)
1000-conversion coefficient.
Operation principle:
The first step, adopts micro-wave digestion to process, and it has, and heating is fast, heat up height, clears up ability strong, and digestion time is short, consumes solvent few, and blank value is low, reduces labor intensity, and environmental pollution is little, it is easy to realize advantages such as automatically controlling.With a small amount of nitric acid, arsenic in sample is cleared up into solution state.Microwave digestion system is higher to addition and the type requirements of acid, and perchloric acid and sulphuric acid are forbidden adding, it is easy to blast.In the samples such as marine product is Thallus Porphyrae such as, Conch Meretricis seu Cyclinae containing organo-arsenic such as arsenic sugar, arsenic lipid be main, this material quite stable, common micro-wave digestion can not by destruction and be sufficiently converted into inorganic arsenic.So needing addition perchloric acid and sulphuric acid further to carry out Wet.
Second step, is initially charged perchloric acid boiling point (180 DEG C) raising and can catch up with most nitric acid, prevent carbonization simultaneously, and it is colourless for making digestion solution, illustrates that this step is cleared up completely.
3rd step, adds sulphuric acid boiling point (280 DEG C), improves electric furnace digestion condition, the organoarsenium compound making indissoluble fully clears up into inorganic arsenic under strong acid, and solution slowly can be changed by faint yellow, final in colourless, showing to clear up completely, reaction end easily determines.
If being simultaneously introduced in digestion solution by perchloric acid and sulphuric acid carry out Wet, digestion process there will be twice colorless state, it is judged that with great difficulty do not make mistakes, therefore second step and the 3rd step are separated, reaction end is judged more clear and definite.
Operation makes every step procedure stage by stage, visualization, it is judged that easy.Adopting microwave to add wet method substep to clear up pre-treating method to use the total arsenic in AFS DETERMINATION marine product to reach time saving and energy saving, result stablizes controlled effect.
Beneficial effect
(1) introduce Microwave Digestion, make process control, reduce the manual operation time；
(2) reagent dosage reduces, and altogether consumes less than 10mL acid adding amount；
(3) digestion time shortens dramatically, and reduces labor intensity；
(4) stagewise is cleared up, it is judged that terminal is clear and definite；
(5) programming operations, it is ensured that data stabilization is controlled, reduces different testing staff's testing result error；
(6) veracity and precision analyzed is improved.
Accompanying drawing explanation
Fig. 1 is overhaul flow chart of the present invention；
Fig. 2 is arsenic standard solution linear relationship chart.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, the present invention can be made various changes or modifications by those skilled in the art, and these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
One, sample pre-treatments:
The first step:
Weigh Porphyra yezoensis Ueda sample (dry sample) 0.1g, Conch Meretricis seu Cyclinae sample (fresh sample) 0.5g, Thallus Porphyrae Standard Reference Materials for Determination (certificate number GBW10023) 0.1g and scallop Standard Reference Materials for Determination (certificate number GBW10024) 0.2g, weigh and be all accurate to 0.0001g, jiangsu coast each department Thallus Porphyraes in 2015 and shellfish all claim sample with reference to above-mentioned sample weighting amount, sample is placed in micro-wave digestion pipe, does two parts of reagent blanks simultaneously.Add nitric acid 5mL mixing, cold clear up 1h, then according to micro-wave digestion program carries out micro-wave digestion.
Table 1. micro-wave digestion program
| Step | Power/W | Lift time/min | Lift temperature/DEG C | Persistent period/min |
| 1 | 800 | 5 | 120 | 5 |
| 2 | 800 | 5 | 150 | 5 |
| 3 | 800 | 5 | 185 | 15 |
Second step:
Taking out after cooling is transferred in 150mL conical flask, take a small amount of water flushing digestion tube inwall to proceed in the lump in conical flask, to electric hot plate, electric hot plate is stepped up temperature, rises to 220 DEG C from 140, clear up and catch up with acid to easily in faint yellow, slightly cooling adds 1mL perchloric acid, is placed on electric furnace and heats clears up (260 DEG C), electric furnace continues clear up and catch up with acid and emit white cigarette to perchloric acid, solution is water white transparency, to be cooled.
3rd step:
Adding 2-3mL concentrated sulphuric acid to continue heating and clear up, furnace temperature improves (300 DEG C) a little, and white cigarette is emerged, and solution colour is by faint yellow → yellow green → green → yellow green → faint yellow → colourless, cooling.
Being proceeded to by content in 50mL volumetric flask or 50mL color comparison tube, add 5mL (5%+3%) thiourea+ascorbic acid solution, moisturizing is to scale and mixes, and places 30min, to be measured.
Two, prepared by standard curve
1. arsenic standard solution (10mg/L): accurately draw 1.00mL arsenic standard reserving solution (1000mg/L) in 100mL volumetric flask, be diluted to scale with 5% hydrochloric acid solution.
2. arsenic standard working solution (1mg/L): accurately draw 10.00mL arsenic standard solution (10mg/L) in 100mL volumetric flask, be diluted to scale with 5% hydrochloric acid solution.
3. standard curve preparation: take 50mL volumetric flask, 1.00mg/L arsenic standard working solution 0.00mL, 0.50mL, 1.00mL, 2.00mL, 4.00mL, 5.00mL (being respectively equivalent to arsenic concentration 0.0 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ g/L, 80 μ g/L, 100 μ g/L) is accurately added successively with pipette, respectively add 25mL10% sulfuric acid solution, (5%+3%) thiourea+ascorbic acid solution 5mL, benefit adds water to scale, measures after placing 30min after mixing.
Three, instrument reference conditions are arranged
Instrument condition: negative high voltage: 270V, as hollow cathode lamp total current: 60mA, flow rate of carrier gas: 400mL/min, shielding
Gas velocity: 900mL/min, atomizer height: 8mm；
Metering system: fluorescence intensity；Reading mode: peak area；Before test, instrument preheating about 30min, treats instrument stabilizer.
Four, upper machine measures
1. standard curve determination: standard serial solution is introduced successively instrument and carries out atomic fluorescence strength detection.With atomic fluorescence intensity for vertical coordinate, arsenic concentration is abscissa drawing standard curve, obtain regression equation 2. sample solution to measure: under the same conditions, sample blank, Thallus Porphyrae and scallop Standard Reference Materials for Determination standard substance, sample solution are introduced instrument respectively and be measured.Obtain regression equation calculation and go out arsenic in sample concentration.
Five, result calculates
In formula:
Arsenic content in X sample, unit is milligrams per kilogram (mg/kg)；
The mensuration concentration of arsenic in C sample test solution, unit is micro-gram per liter (ug/L)；
C0The mensuration concentration of arsenic in sample blank Digestive system, unit is micro-gram per liter (ug/L)；
V sample Digestive system cumulative volume, unit is milliliter (mL)；
M sample mass, unit is gram (g)
1000 conversion coefficients.
Six, arsenic standard curve
Table 2 arsenic standard curve
Arsenic standard solution linear relationship chart is shown in Fig. 2.
Seven, microwave add wet method substep clear up measurement result
1) Thallus Porphyrae and scallop standard substance measurement result
Table 3. GB Wet method measures Thallus Porphyrae and scallop standard substance result
Table 4. microwave adds wet method substep resolution method and measures Thallus Porphyrae and scallop standard substance result
Adopt microwave to add wet method substep resolution method by experiment as seen and measure in Thallus Porphyrae and scallop standard substance the content of arsenic all within the scope of certificate, and than GB Wet method closer to median, accuracy is high；Visible by parallel 3 experiments, measurement result precision is both less than 5%, and precision is good, and measurement result is reliable and stable.
2) recovery of standard addition experiment
Respectively taking Porphyra yezoensis Ueda dry sample 0.1g, the fresh sample 0.5g of Conch Meretricis seu Cyclinae, add Thallus Porphyrae Quality Control sample 0.1g and scallop Quality Control sample 0.2g respectively as mark-on thing, use GB Wet and microwave to add wet method substep and clear up pre-treatment, measure the arsenic response rate, result is in Table 5.
The impact on the arsenic measurement result response rate total in marine product of table 5. different pre-treatments
Adopt the addition quality-control sample similar with arsenic morphology in marine product to verify pre-treating method, relatively can reflect the different pre-treatments suitability to arsenic total in Atomic Fluorescence Spectrometry marine product.Microwave adds the wet method response rate cleared up of substep than the response rate of Wet in GB closer to 100% as can be seen from the table, and the pre-treatment that the method is suitable as in Atomic Fluorescence Spectrometry marine product total arsenic is described.
3) Thallus Porphyrae in multiple areas and shellfish samples measurement result
Adopting microwave to add wet method substep and clear up total arsenic content in mensuration jiangsu coast each department Thallus Porphyraes in 2015 and shellfish, result is in Table 6.
In table jiangsu coast each department Thallus Porphyraes in 62015 and shellfish, total arsenic content measures
Comparison is visible by experiment adopts microwave to add wet method substep resolution method ratio national standard Wet method to measure Thallus Porphyrae and scallop Quality Control content is high, and closer to the certificate value intermediate value of standard substance certificate offer, accuracy height, and precision is better；Prove that adopting microwave to add wet method substep resolution method adds the quality-control sample response rate closer to 100% by recovery testu；Measure jiangsu coast Porphyra yezoensis Ueda and shellfish samples result content is more accurate, and good stability.Adopt microwave to add wet method substep resolution method and do the total arsenic in pre-treatment Atomic Fluorescence Spectrometry marine product, the pre-treatment time can be reduced, reduce labor intensity, improve the accuracy of reaction end judgement and the stability of testing result, guarantee the repeatability of experimental implementation, it is prone to new hand and quickly grasps this experimental technique, be that a kind of being suitable for promotes the method measuring always arsenic in marine product, there is good application prospect.
Claims (10)
1. microwave adds the method that wet method substep clears up marine product mensuration total arsenic content, including:
(1) by adding in marine product sample, nitric acid is cold to be cleared up, and then carries out micro-wave digestion again；
(2) cooling transfer post-heating catches up with acid, then adds perchloric acid and carries out clearing up to solution colourless；
(3) add concentrated sulphuric acid to be heated clearing up, be colourless to solution, obtain Specimen eliminating thing, then prepare sample solution；
(4) drawing standard curve, adopts atomic fluorescence spectrometer that sample solution is tested, and conversion obtains arsenic content in marine product.
2. a kind of microwave according to claim 1 adds wet method substep and clears up the method that marine product measures total arsenic content, it is characterised in that: clearing up total time in step (1) is 1.5-2.5h.
3. a kind of microwave according to claim 1 adds the method that wet method substep clears up marine product mensuration total arsenic content, it is characterised in that: adding the cold digestion time of nitric acid in described step (1) is 0.5-1h；Micro-wave digestion is: when power is 800-1600W, after being first warming up to 120 DEG C, keeps 5min, after being then warming up to 150 DEG C again, keeps 5min, is finally warming up to 185 DEG C, keeps 15min.
4. a kind of microwave according to claim 1 adds wet method substep and clears up the method that marine product measures total arsenic content, it is characterised in that: heating catches up with the acid to be in described step (2): is heated to 220 DEG C and carries out catching up with acid, heating to catch up with acid total time to be 1-2h；The temperature that addition perchloric acid carries out clearing up is 200-280 DEG C, and overall time is 30min-1h.
5. a kind of microwave according to claim 1 adds the method that wet method substep clears up marine product mensuration total arsenic content, it is characterised in that: in described step (3), heating is cleared up for 280-350 DEG C, and overall time is 30min-1h.
6. a kind of microwave according to claim 1 add wet method substep clear up marine product measure total arsenic content method, it is characterised in that: marine product sample, nitric acid, perchloric acid, concentrated sulphuric acid ratio be: dry sample 0.1-0.2g or fresh sample 0.5-2g:5-8mL:1-2mL:2-3mL.
7. a kind of microwave according to claim 1 adds the method that wet method substep clears up marine product mensuration total arsenic content, it is characterized in that: described step (3) prepares sample solution particularly as follows: Specimen eliminating thing proceeds in 50mL volumetric flask or 50mL color comparison tube, add the solution of 5mL thiourea and ascorbic acid, moisturizing is to scale and mixes, and places 20-30min.
8. a kind of microwave according to claim 1 adds the method that wet method substep clears up marine product mensuration total arsenic content, it is characterized in that: drawing standard curve in described step (4) particularly as follows: accurately draw 1.00mg/L arsenic standard solution 0.00mL respectively with pipette, 0.50mL, 1.00mL, 2.00mL, 4.00mL, 5.00mL is in 50ml volumetric flask, respectively add sulfuric acid solution 25mL, and the solution 5mL of thiourea and ascorbic acid, benefit adds water to scale, measure after placing 20-30min after mixing, and with atomic fluorescence intensity for vertical coordinate, arsenic concentration is abscissa drawing standard curve.
9. a kind of microwave according to claim 1 adds the method that wet method substep clears up marine product mensuration total arsenic content, it is characterised in that: in step (4), sample solution does blank assay simultaneously.
10. a kind of microwave according to claim 1 adds the method that wet method substep clears up marine product mensuration total arsenic content, it is characterized in that: described step (4) Atom fluorescence spectrophotometer test parameter is: negative high voltage: 240V, as hollow cathode lamp total current: 60mA, flow rate of carrier gas: 400mL/min, shield gas flow speed: 900mL/min, atomizer height: 8mm.
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