CN106644990A - Method for determining arsenic in feed mildew inhibitor - Google Patents
Method for determining arsenic in feed mildew inhibitor Download PDFInfo
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- CN106644990A CN106644990A CN201710058407.3A CN201710058407A CN106644990A CN 106644990 A CN106644990 A CN 106644990A CN 201710058407 A CN201710058407 A CN 201710058407A CN 106644990 A CN106644990 A CN 106644990A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
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- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention discloses a method for determining arsenic in a feed mildew inhibitor. The method includes subjecting a feed mildew inhibitor sample to acid heat digestion, adding ascorbic acid into an acid medium, and enabling the arsenic in the feed mildew inhibitor sample to react with a hydroborate to obtain hydride containing volatile arsenic; taking argon as carrier gas, feeding the arsenic-containing hydride into an atomic absorption spectrophotometer, conducting flame atomization, and absorbing on a resonance line with the wavelength being 193.7 nm to obtain the absorbancy area of the arsenic-containing hydride; importing the absorbancy area of the arsenic-containing hydride into a standard curve of the absorbancy area of the arsenic-containing hydride, measuring the determination concentration of the arsenic in to-be-detected liquid, and obtaining the content of the arsenic in the feed mildew inhibitor sample. The method has the advantages of high determination accuracy, high precision and high stability.
Description
Technical field
The invention belongs to Midew preventive for feed technical field of analysis and detection, and in particular to the measure of arsenic in a kind of Midew preventive for feed
Method.
Background technology
The heavy metal element such as lead, mercury, cadmium and arsenic is harmful to animal in feed, and at present country issues early in calendar year 2001
《Forage health standard》, standard number is GB13078-2001, belongs to mandatory national standards, it is adaptable to which feed and feed add
Agent industry.Wherein just it is related to the allowance of arsenic：Stone flour, ferrous sulfate, magnesium sulfate≤2mg/Kg；Phosphate≤20mg/Kg；Boiling
Stone flour, bentonite, medical stone≤10mg/Kg；Copper sulphate, manganese sulfate, zinc sulfate, KI, calcium iodate, cobalt chloride≤5mg/
Kg；Zinc oxide≤10mg/Kg；Fish meal, digested tankage, meat meal tankage≤10mg/Kg；Poultry, swine feed≤2mg/Kg；Ox, sheep essence
Material supplements material, pig, poultry concentrated feed, pig, poultry additive premix≤10mg/Kg.So current feed and feed
Additives industries need accurate quantitative analysis to the measure of arsenic.
At present, in feed and food service industry, country has following country and professional standard to the measure of arsenic：《GB/
The measure of T13079-2006 total arsenic in feed》, mixed feed, concentrated feed, single feed, additive are defined in the standard
The measure of arsenic in premixed feed and feed addictive, has three kinds of methods：First method silver salt method, the second method borohydride reduction
Photometry, the 3rd method Hydride generation fluorescence spectrometry.《The measure liquid phase color of inorganic arsenic in DB22/T 1985-2013 feeds
Spectrum-atomic fluorescence spectrometry》, the measure of inorganic arsenic in mixed feed is the standard specifies, it is liquid chromatogram-atomic fluorescence spectrophotometry
Method.《The measure atomic fluorescence spectrometry of inorganic arsenic in DB35/T 1100-2011 feeds》, the standard specifies various cooperations and raise
The measure of inorganic arsenic in material, concentrated feed, additive premix, single feed and feed addictive, is atomic fluorescence light
Spectrometry.《The measure of GB 5009.11-2014 national food safety standard total Arsenic in Food and inorganic arsenic》, define in the standard
The assay method of total Arsenic in Food, has three kinds of methods：First method inductively coupled plasma mass spectrometry；Second method hydride is sent out
Raw atomic fluorescence spectrometry；3rd method silver salt method；The assay method of inorganic arsenic in food, has two methods：First method liquid phase
Chromatogram-atomic fluorescence spectrometry；Second method liquid chromatogram-Inductively coupled plasma-mass spectrometry (LC-ICP/MS).《GB/T
The measure of arsenic in 5009.76-2014 national food safety standard food additives》, the standard specifies arsenic in food additives
Measure, altogether two methods：First method Silver diethydithiocarbamate colorimetric method, the second method hydride generation atomic fluorescence luminosity
Method.
The assay method for defining arsenic in several standards above is Hydride generation fluorescence spectrometry, silver salt method, hydroboration
Thing reduces photometry and inductively coupled plasma mass spectrometry, and the instrument for using is respectively atomic fluorescence spectrophotometer, ICP and light splitting
Photometer.In instrument used above, ICP's is expensive, and feed and feed additive enterprises use cost are high, are unfavorable for the party
The implementation of method.The method for being relatively specific for feed and feed additive enterprises at present is Hydride generation fluorescence spectrometry and silver salt
Method.
When silver salt method determines arsenic in Midew preventive for feed, reagent and device used is more, and some of which is dangerization
Product, furthermore the detection limit of the method is higher, so not adopting the method to carry out the measure of arsenic as far as possible.Hydride generation atomic fluorescence spectrum
Method at present in feed and food service industry determine arsenic when the degree of accuracy and detection limit it is all very high, price is also cheap, at present at home
Use range it is extremely wide, but is not in the world at present to approve very much to atomic fluorescence spectrometry.
The content of the invention
For deficiencies of the prior art, it is an object of the invention to provide a kind of determine accuracy height, precision
The assay method of arsenic in the good and strong Midew preventive for feed of stability.
To achieve these goals, the technical solution used in the present invention is as follows：
The assay method of arsenic in a kind of Midew preventive for feed, Midew preventive for feed sample Jing acid heats are cleared up, then are placed in acid Jie
Ascorbic acid is added in matter, makes the arsenic in Midew preventive for feed sample generate volatility hydride of arsenic with boron hydride reaction；Again
With argon gas as carrier gas, hydride of arsenic is imported in atomic absorption spectrophotometer, Jing after flame atomization, be in wavelength
Absorbed on the resonance line of 193.7nm, obtained the absorbance area of hydride of arsenic；By the absorbance area of hydride of arsenic
Hydride of arsenic absorbance area standard curve is substituted into, the measure concentration of arsenic in liquid to be detected is measured and is asked for Midew preventive for feed sample
The content of arsenic in product.
Specifically include following steps：
1) 0.2～0.5g Midew preventive for feed samples are weighed and is placed in tetrafluoro beaker and is added and clear up acid, in 180～200 DEG C
Under add a cover and clear up 30-60min；Go to be placed on 120～160 DEG C again and catch up with acid to 1～2mL, in transferring to volumetric bottle, plus pure water constant volume
To 10mL, digestion solution is obtained.
2) to step 1) mixed solution of thiocarbamide and ascorbic acid is added in the digestion solution that obtains, adjust digestion solution with HCl
In acid concentration to 5-20%, be incubated at 60～90 DEG C under 5-10min or room temperature and stand 30～60min, obtain to be detected
Liquid, then determines liquid to be detected and arsenic reagent and mixes, generates hydride of arsenic.
3) with argon gas as carrier gas, by step 2) generate hydride of arsenic import atomic absorption spectrophotometer in, Jing is fiery
After flame atomization, in wavelength to be absorbed on the resonance line of 193.7nm, the absorbance area of hydride of arsenic is obtained；By arsenic
The absorbance area of hydride substitute into hydride of arsenic absorbance area standard curve, the measure for measuring arsenic in liquid to be detected is dense
Degree.
4) by step 1) to the operation in 3) preparing, determine the measure concentration of arsenic in blank sample.
5) according to the measure concentration of arsenic in the measure concentration and blank sample of arsenic in liquid to be detected, it is calculated Midew preventive for feed
Arsenic content in sample.
Wherein：Step 1) described in clear up acid mixed by nitric acid, hydrochloric acid and hydrofluoric acid；Described mould inhibitor and nitre
Acid, hydrochloric acid, the mass volume ratio of hydrofluoric acid are 1g:5～15mL:15～45mL:10～20mL.
Step 2) described in arsenic determine reagent mass volume ratio 1-2g is pressed by boron hydride, NaOH and water：1-2g：
100mL is formulated.In described thiocarbamide and the mixed solution of ascorbic acid, the mass fraction of thiocarbamide and ascorbic acid is 3-
10%；The mass concentration of described HCl solution is 50%.Described boron hydride is sodium borohydride or potassium borohydride.
Step 3) described in the acquisition methods of hydride of arsenic absorbance area standard curve comprise the following steps：
(1) arsenic standard solution of 0mL, 2.5mL, 5mL, 7.5mL, 10mL, 15mL concentration for 100ng/mL is drawn respectively,
In adding 50mL volumetric bottles, add the mixed solution 5mL of thiocarbamide and ascorbic acid, use pure water constant volume, adjusted with 50%HCl solution
Acid concentration obtains gradient concentration series standard prepare liquid to 5-20% in standard liquid.
(2) respectively gradient concentration series standard prepare liquid is determined into reagent with arsenic to mix, and correspondence generates the hydrogenation of 6 groups of arsenic
Thing.
(3) with argon gas as carrier gas, 6 groups of hydride of arsenics that step (2) is generated are directed respectively into atomic absorption spectrphotometry
In meter, Jing after flame atomization, in wavelength to be absorbed on the resonance line of 193.7nm, the suction of each group hydride of arsenic is obtained
Luminosity area.
(4) coordinate system is set up with the absorbance area of hydride of arsenic as the longitudinal axis, by transverse axis of the concentration of arsenic, then will step
Suddenly the arsenic concentration and step (3) of the gradient concentration series standard test solution that (1) prepares obtains the absorbance face of each group hydride of arsenic
The corresponding point of long-pending value is marked in the coordinate system, and fit regression curve, has both obtained hydride of arsenic absorbance area mark
Directrix curve, its corresponding calibration curve equation is：
A=0.0037C+0.0101, R2=0.99946
In formula, A is the absorbance area of hydride of arsenic；C is the concentration of arsenic；R2For the degree of correlation.
Step 5) in arsenic content in Midew preventive for feed sample be calculated as follows：
In formula, X --- the arsenic content in Midew preventive for feed sample, unit is mg/Kg；C1--- the survey of arsenic in liquid to be detected
Determine concentration, unit is ng/mL；C0--- the measure concentration of arsenic in blank sample, unit is ng/mL；V --- the body of liquid to be detected
Product, unit is mL；M --- sample mass, unit is g.
In order to improve accuracy, repeat step 1) to more than 5) once, Midew preventive for feed sample is characterized with arithmetic mean of instantaneous value
Arsenic content in product.
The present invention is improved and optimized on the basis of hydride-flame atomic absorption spectrometry, by sample Jing acid heats
After digestion, in acid medium, thiocarbamide is added in test solution and excludes collective's interference, addition ascorbic acid makes arsenic be changed into three from pentavalent
Valency, arsenic and sodium borohydride (NaBH4) or potassium borohydride (KBH4) reaction generation volatility hydride of arsenic (AsH3).It is with argon gas
Carrier gas, hydride is imported in atomic absorption spectrophotometer, after flame atomization, absorbs 193.7nm resonance lines, its uptake
It is directly proportional to arsenic content, is carried out quantitatively according to standard series.The present invention improves the stability of determination data, and the detection of arsenic
Limit can reach PPb ranks, improve the accuracy for determining.
Compared with prior art, the present invention has the advantages that：
1st, can be with quantitative determination.The present invention has done on the basis of hydride-flame atomic absorption spectrometry and has improved and excellent
Change, by sample Jing after acid heat digestion, in acid medium, thiocarbamide is added in test solution and excludes collective's interference, add ascorbic acid
Arsenic is set to be changed into trivalent, arsenic and sodium borohydride (NaBH from pentavalent4) or potassium borohydride (KBH4) reaction generation volatility hydride of arsenic
(AsH3).With argon gas as carrier gas, hydride is imported in atomic absorption spectrophotometer, after flame atomization, absorb 193.7nm
Resonance line, its uptake is directly proportional to arsenic content, is carried out quantitatively according to standard series.
2nd, the present invention improves the stability of determination data, due to detecting during sample introduction, the hydride of arsenic after hydrogenation
The atomization under flame interaction, produces the quartz ampoule that a certain amount of arsenic atom is entered on atom instrument, by absorbing line source drop
The energy of low light source, so as to form one section of spectral peak, so determination data is more stable.
3rd, the detection limit that improve arsenic of the invention can reach PPb ranks, improve the accuracy for determining.After hydrogenation
Hydride of arsenic atomization under flame interaction, in quartz ampoule, cadmium steam is difficult to be spread from quartz ampoule the arsenic atom of production,
And the light of line source passes through from quartz ampoule, so it is lower than the detection limit of general Flame Atomic Absorption Spectrometry, can reach PPb levels
Not.
Description of the drawings
Fig. 1 is the hydride of arsenic absorbance area standard curve of the present invention.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment.
The capital equipment that the present invention needs has tetrafluoro beaker (with cover), 50mL volumetric bottles, 100mL volumetric flasks, assay balance
(accuracy is 0.0001g), electric hot plate, chemical atomic device, atomic absorption spectrophotometer, water filter.Reagent is needed to have nitre
The arsenic standard that sour (top pure grade), hydrochloric acid (top pure grade), hydrofluoric acid (top pure grade), arsenic standard solution (1000 μ g/mL) are prepared is used
Liquid (concentration is 100ng/mL), sodium borohydride (or potassium borohydride, analyze pure), NaOH (analysis is pure), argon gas (purity
99.999%), thiocarbamide (analysis is pure), ascorbic acid (i.e. Vc is analyzed pure), pure water, high purity acetylene.
Embodiment one
Hydride of arsenic absorbance area standard curve is obtained using following steps.
(1) arsenic standard solution of 0mL, 2.5mL, 5mL, 7.5mL, 10mL, 15mL concentration for 100ng/mL is drawn respectively, plus
In entering 50mL volumetric bottles, add the mixed solution 5mL of thiocarbamide and ascorbic acid, use pure water constant volume, adjusted with 50%HCl solution and marked
Acid concentration obtains gradient concentration series standard prepare liquid to 5-20% (volumetric concentration) in quasi- solution.
(2) respectively gradient concentration series standard prepare liquid is determined into reagent with arsenic to mix, and correspondence generates the hydrogenation of 6 groups of arsenic
Thing (AsH3)。
(3) with argon gas as carrier gas, 6 groups of hydride of arsenics that step (2) is generated are directed respectively into atomic absorption spectrphotometry
In meter, Jing after flame atomization, in wavelength to be absorbed on the resonance line of 193.7nm, the suction of each group hydride of arsenic is obtained
Luminosity area.
Instrument reference conditions are：
Atomizer：Argon gas flow velocity 800-1200mL/min, acetylene pressure 0.03-0.05MPa, air pressure 0.25-
Sample time 4s, sample presentation scavenging period 14s are inhaled in 0.30MPa, igniting.
Atomic absorption spectrophotometer：Hollow cathode lamp current 6mA；Resonance line 193.7nm nm；Slit 0.4nm；Burning
Device height 16mm；Reading mode：Peak height；Time of integration 10s, integral way：Manually.
(4) coordinate system is set up with the absorbance area of hydride of arsenic as the longitudinal axis, by transverse axis of the concentration of arsenic, then will step
Suddenly the arsenic concentration and step (3) of the gradient concentration series standard test solution that (1) prepares obtains the absorbance face of each group hydride of arsenic
The corresponding point of long-pending value is marked in the coordinate system, and fit regression curve, has both obtained hydride of arsenic absorbance area mark
Directrix curve, as shown in figure 1, its corresponding calibration curve equation is：
A=0.0037C+0.0101, R2=0.99946
In formula, A is the absorbance area of hydride of arsenic；C is the concentration of arsenic；R2For the degree of correlation.
The standard song that the present embodiment determination is to hydride of arsenic absorbance area standard curve in following examples
Line.
Embodiment two
The content of arsenic in Midew preventive for feed is determined using following methods：
1) 0.2g Midew preventive for feed samples are weighed, is added in the tetrafluoro beaker for being boiled with nitric acid and is added and clear up acid
(2mL nitric acid, 6mL hydrochloric acid and 3mL hydrofluoric acid), adds a cover, and is placed on 180 DEG C of heating on electric hot plate and clears up 60min, treats that digestion solution is clear
After bright (if limpid adding does not clear up acid to solution), lid is removed, acid discharge is carried out at 120 DEG C to 1mL or so, be transferred to volumetric bottle
In, plus pure water is settled to 10mL, obtains digestion solution.
2) digestion solution can be suitably diluted, so that it is in the range ability of absorbance meter, then to step 1) clearing up of obtaining
The mixed solution that mass fraction is thiocarbamide and ascorbic acid is added in liquid, and (mass fraction of wherein thiocarbamide and ascorbic acid is
5%), and with HCl solution (being mixed with top grade pure hydrochloric acid and pure water equal-volume) acid concentration is adjusted in digestive juice to 5-20%
(volumetric concentration), is allowed to place 5～10min in 60-90 DEG C of hot water, so that pentavalent arsenic therein is converted into trivalent arsenic, obtains
To liquid to be detected, then liquid to be detected and arsenic are determined into reagent and (weigh 1g NaBH4With 1g NaOH, in adding plastic bottle, then add
Enter 100mL water, be configured to arsenic and determine reagent) mixing, generate hydride of arsenic (i.e. AsH3)。
3) with argon gas as carrier gas, by step 2) generate hydride of arsenic import atomic absorption spectrophotometer in, in ripple
Absorbed on the resonance line of a length of 228.8nm, obtained the absorbance area of hydride of arsenic；By the absorbance of hydride of arsenic
Area substitutes into hydride of arsenic absorbance area standard curve, measures the measure concentration of arsenic in liquid to be detected.Device parameter and reality
Apply example one identical.
4) by step 1) to the operation in 3) preparing, determine the measure concentration of arsenic in blank sample；
5) according to the measure concentration of arsenic in the measure concentration and blank sample of arsenic in liquid to be detected, according to following formula feeding is calculated
Arsenic content in material mould inhibitor sample.
In formula, X --- the arsenic content in Midew preventive for feed sample, unit is mg/Kg；C1--- the survey of arsenic in liquid to be detected
Determine concentration, unit is ng/mL；C0--- the measure concentration of arsenic in blank sample, unit is ng/mL；V --- the body of liquid to be detected
Product, unit is mL；M --- sample mass, unit is g.
Represented with the arithmetic mean of instantaneous value of the measurement result independent twice obtained under the conditions of repeatability, as a result retain two effectively
Numeral, twice the absolute difference of independent measurement result must not exceed the 10% of arithmetic mean of instantaneous value.
It is 0.160mg/Kg and 0.149mg/Kg to measure independent measurement result twice, takes its arithmetic mean of instantaneous value 0.155mg/Kg
Represent the arsenic content in Midew preventive for feed sample.
Embodiment three
The content of arsenic in Midew preventive for feed is determined using following methods：
1) 0.5g Midew preventive for feed samples are weighed, is added in the tetrafluoro beaker for being boiled with nitric acid and is added and clear up acid
(2mL nitric acid, 6mL hydrochloric acid and 3mL hydrofluoric acid), adds a cover, and is placed on 200 DEG C of heating on electric hot plate and clears up 30min, treats that digestion solution is clear
After bright (if limpid adding does not clear up acid to solution), lid is removed, acid discharge is carried out at 160 DEG C to 1mL or so, be transferred to volumetric bottle
In, plus pure water is settled to 10mL, obtains digestion solution.
2) digestion solution can be suitably diluted, so that it is in the range ability of absorbance meter, then to step 1) clearing up of obtaining
The mixed solution that mass fraction is thiocarbamide and ascorbic acid is added in liquid, and (mass fraction of wherein thiocarbamide and ascorbic acid is
5%), and with HCl solution (being mixed with top grade pure hydrochloric acid and pure water equal-volume) acid concentration is adjusted in digestive juice to 5-20%
(volumetric concentration), is allowed to place 5～10min in 60-90 DEG C of hot water, so that pentavalent arsenic therein is converted into trivalent arsenic, obtains
To liquid to be detected, then liquid to be detected and arsenic are determined into reagent and (weigh 1g NaBH4With 1g NaOH, in adding plastic bottle, then add
Enter 100mL water, be configured to arsenic and determine reagent) mixing, generate hydride of arsenic.
3) with argon gas as carrier gas, by step 2) generate hydride of arsenic import atomic absorption spectrophotometer in, in ripple
Absorbed on the resonance line of a length of 228.8nm, obtained the absorbance area of hydride of arsenic；By the absorbance of hydride of arsenic
Area substitutes into hydride of arsenic absorbance area standard curve, measures the measure concentration of arsenic in liquid to be detected.Device parameter and reality
Apply example one identical.
4) by step 1) to the operation in 3) preparing, determine the measure concentration of arsenic in blank sample；
5) according to the measure concentration of arsenic in the measure concentration and blank sample of arsenic in liquid to be detected, according to following formula feeding is calculated
Arsenic content in material mould inhibitor sample.
In formula, X --- the arsenic content in Midew preventive for feed sample, unit is mg/Kg；C1--- the survey of arsenic in liquid to be detected
Determine concentration, unit is ng/mL；C0--- the measure concentration of arsenic in blank sample, unit is ng/mL；V --- the body of liquid to be detected
Product, unit is mL；M --- sample mass, unit is g.
Represented with the arithmetic mean of instantaneous value of the measurement result independent twice obtained under the conditions of repeatability, as a result retain two effectively
Numeral, twice the absolute difference of independent measurement result must not exceed the 10% of arithmetic mean of instantaneous value.
It is 0.160mg/Kg and 0.149mg/Kg to measure independent measurement result twice, takes its arithmetic mean of instantaneous value 0.155mg/Kg
Represent the arsenic content in Midew preventive for feed sample.
Example IV
The content of arsenic in Midew preventive for feed is determined using following methods：
1) 0.3g Midew preventive for feed samples are weighed, is added in the tetrafluoro beaker for being boiled with nitric acid and is added and clear up acid
(2mL nitric acid, 6mL hydrochloric acid and 3mL hydrofluoric acid), adds a cover, and is placed on 190 DEG C of heating on electric hot plate and clears up 45min, treats that digestion solution is clear
After bright (if limpid adding does not clear up acid to solution), lid is removed, acid discharge is carried out at 150 DEG C to 1mL or so, be transferred to volumetric bottle
In, plus pure water is settled to 10mL, obtains digestion solution.
2) digestion solution can be suitably diluted, so that it is in the range ability of absorbance meter, then to step 1) clearing up of obtaining
The mixed solution that mass fraction is thiocarbamide and ascorbic acid is added in liquid, and (mass fraction of wherein thiocarbamide and ascorbic acid is
5%), and with HCl solution (being mixed with top grade pure hydrochloric acid and pure water equal-volume) acid concentration is adjusted in digestive juice to 5-20%
(volumetric concentration), is allowed to stand 30～60min at room temperature, so that pentavalent arsenic therein is converted into trivalent arsenic, obtains to be detected
Liquid, then determines liquid to be detected and arsenic reagent and (weighs 1g NaBH4With 1g NaOH, in adding plastic bottle, 100mL is added
Water, is configured to arsenic and determines reagent) mixing, generate hydride of arsenic.
3) with argon gas as carrier gas, by step 2) generate hydride of arsenic import atomic absorption spectrophotometer in, in ripple
Absorbed on the resonance line of a length of 228.8nm, obtained the absorbance area of hydride of arsenic；By the absorbance of hydride of arsenic
Area substitutes into hydride of arsenic absorbance area standard curve, measures the measure concentration of arsenic in liquid to be detected.Device parameter and reality
Apply example one identical.
4) by step 1) to the operation in 3) preparing, determine the measure concentration of arsenic in blank sample；
5) according to the measure concentration of arsenic in the measure concentration and blank sample of arsenic in liquid to be detected, according to following formula feeding is calculated
Arsenic content in material mould inhibitor sample.
In formula, X --- the arsenic content in Midew preventive for feed sample, unit is mg/Kg；C1--- the survey of arsenic in liquid to be detected
Determine concentration, unit is ng/mL；C0--- the measure concentration of arsenic in blank sample, unit is ng/mL；V --- the body of liquid to be detected
Product, unit is mL；M --- sample mass, unit is g.
Represented with the arithmetic mean of instantaneous value of the measurement result independent twice obtained under the conditions of repeatability, as a result retain two effectively
Numeral, twice the absolute difference of independent measurement result must not exceed the 10% of arithmetic mean of instantaneous value.
It is 0.160mg/Kg and 0.149mg/Kg to measure independent measurement result twice, takes its arithmetic mean of instantaneous value 0.155mg/Kg
Represent the arsenic content in Midew preventive for feed sample.
The above embodiment of the present invention is only example to illustrate the invention, and is not the enforcement to the present invention
The restriction of mode.For those of ordinary skill in the field, on the basis of the above description other can also be made not
With the change and variation of form.Here all of embodiment cannot be exhaustive.It is every to belong to technical scheme
The obvious change amplified out changes row still in protection scope of the present invention.
Claims (9)
1. in a kind of Midew preventive for feed arsenic assay method, it is characterised in that Midew preventive for feed sample Jing acid heats are cleared up, then are put
Ascorbic acid is added in acid medium, makes the arsenic in Midew preventive for feed sample that the hydrogen for generating volatile arsenic is reacted with boron hydride
Compound；Again with argon gas as carrier gas, hydride of arsenic is imported in atomic absorption spectrophotometer, Jing after flame atomization, in ripple
Absorbed on the resonance line of a length of 193.7nm, obtained the absorbance area of hydride of arsenic；By the absorbance of hydride of arsenic
Area substitutes into hydride of arsenic absorbance area standard curve, measures the measure concentration of arsenic in liquid to be detected and asks for feedstuff mildew
The content of agent arsenic in sample.
2. in Midew preventive for feed according to claim 1 arsenic assay method, it is characterised in that comprise the following steps：
1) 0.2～0.5g Midew preventive for feed samples are weighed and is placed in tetrafluoro beaker and is added and clear up acid, added at 180～200 DEG C
Lid clears up 30-60min；Going to be placed on 120～160 DEG C again catches up with acid to 1～2mL, and in transferring to volumetric bottle, plus pure water is settled to
10mL, obtains digestion solution；
2) to step 1) mixed solution of thiocarbamide and ascorbic acid is added in the digestion solution that obtains, adjusted in digestion solution with HCl
Acid concentration is incubated under 5-10min or room temperature at 60～90 DEG C and stands 30～60min to 5-20%, obtains liquid to be detected, so
Afterwards liquid to be detected and arsenic are determined into reagent to mix, generate hydride of arsenic；
3) with argon gas as carrier gas, by step 2) hydride of arsenic that generates imported in atomic absorption spectrophotometer, and Jing flames are former
After sonization, in wavelength to be absorbed on the resonance line of 193.7nm, the absorbance area of hydride of arsenic is obtained；By the hydrogen of arsenic
The absorbance area of compound substitutes into hydride of arsenic absorbance area standard curve, measures the measure concentration of arsenic in liquid to be detected；
4) by step 1) to the operation in 3) preparing, determine the measure concentration of arsenic in blank sample；
5) according to the measure concentration of arsenic in the measure concentration and blank sample of arsenic in liquid to be detected, it is calculated Midew preventive for feed sample
In arsenic content.
3. in Midew preventive for feed according to claim 2 arsenic assay method, it is characterised in that step 1) described in disappear
Solution acid is mixed by nitric acid, hydrochloric acid and hydrofluoric acid；Described mould inhibitor is with the mass volume ratio of nitric acid, hydrochloric acid, hydrofluoric acid
1g:5～15mL:15～45mL:10～20mL.
4. in Midew preventive for feed according to claim 2 arsenic assay method, it is characterised in that step 2) described in arsenic
Determine reagent and mass volume ratio 1-2g is pressed by boron hydride, NaOH and water：1-2g：100mL is formulated.
5. in Midew preventive for feed according to claim 2 arsenic assay method, it is characterised in that step 2) described in sulphur
In the mixed solution of urea and ascorbic acid, the mass fraction of thiocarbamide and ascorbic acid is 3-10%；The matter of described HCl solution
Amount concentration is 50%.
6. in Midew preventive for feed according to claim 4 arsenic assay method, it is characterised in that described boron hydride is
Sodium borohydride or potassium borohydride.
7. in Midew preventive for feed according to claim 2 arsenic assay method, it is characterised in that step 3) described in arsenic
The acquisition methods of hydride absorbance area standard curve comprise the following steps：
(1) arsenic standard solution of 0mL, 2.5mL, 5mL, 7.5mL, 10mL, 15mL concentration for 100ng/mL is drawn respectively, add
In 50mL volumetric bottles, add the mixed solution 5mL of thiocarbamide and ascorbic acid, pure water constant volume is used, with 50%HCl solution adjustment criterias
Acid concentration obtains gradient concentration series standard prepare liquid to 5-20% in solution；
(2) respectively gradient concentration series standard prepare liquid is determined into reagent with arsenic to mix, and correspondence generates 6 groups of hydride of arsenics；
(3) with argon gas as carrier gas, 6 groups of hydride of arsenics that step (2) is generated are directed respectively into atomic absorption spectrophotometer,
Jing after flame atomization, in wavelength to be absorbed on the resonance line of 193.7nm, the absorbance face of each group hydride of arsenic is obtained
Product；
(4) coordinate system is set up with the absorbance area of hydride of arsenic as the longitudinal axis, by transverse axis of the concentration of arsenic, then by step
(1) arsenic concentration and step (3) of the gradient concentration series standard test solution prepared obtains the absorbance area of each group hydride of arsenic
The corresponding point of value mark in the coordinate system, and fit regression curve had both obtained hydride of arsenic absorbance area standard
Curve, its corresponding calibration curve equation is：
A=0.0037C+0.0101, R2=0.99946
In formula, A is the absorbance area of hydride of arsenic；C is the concentration of arsenic；R2For the degree of correlation.
8. in Midew preventive for feed according to claim 2 arsenic assay method, it is characterised in that step 5) in feedstuff mildew
Arsenic content in agent sample is calculated as follows：
In formula, X --- the arsenic content in Midew preventive for feed sample, unit is mg/Kg；C1--- the measure of arsenic is dense in liquid to be detected
Degree, unit is ng/mL；C0--- the measure concentration of arsenic in blank sample, unit is ng/mL；V --- the volume of liquid to be detected, it is single
Position is mL；M --- sample mass, unit is g.
9. in Midew preventive for feed according to claim 2 arsenic assay method, it is characterised in that repeat step 1) to 5) one
More than secondary, the arsenic content in Midew preventive for feed sample is characterized with arithmetic mean of instantaneous value.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104697983A (en) * | 2015-03-18 | 2015-06-10 | 河北金木药业集团有限公司 | Method of detecting heavy metal lead, cadmium, arsenic and copper in TCM (Traditional Chinese Medicine) tablet |
| CN105628633A (en) * | 2016-02-26 | 2016-06-01 | 重庆民泰香料化工有限责任公司 | Method for determining lead content of feed mildew preventive |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104697983A (en) * | 2015-03-18 | 2015-06-10 | 河北金木药业集团有限公司 | Method of detecting heavy metal lead, cadmium, arsenic and copper in TCM (Traditional Chinese Medicine) tablet |
| CN105628633A (en) * | 2016-02-26 | 2016-06-01 | 重庆民泰香料化工有限责任公司 | Method for determining lead content of feed mildew preventive |
Non-Patent Citations (3)
| Title |
|---|
| 丁晓雯等: "《食品分析》", 31 August 2016, 中国农业大学出版社 * |
| 刘波静: "HG-AAS法测定饲料级氧化锌中的砷", 《化验与检测》 * |
| 王照华等: "影响流动注射氢化物发生原子吸收分光光度法测定饲料总砷灵敏度的因素研究", 《中国饲料》 * |
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