CN105784827A - Method for measuring content of nine heavy metals in sugarcane juice with electric heating plate digestion/ICP-MS method - Google Patents
Method for measuring content of nine heavy metals in sugarcane juice with electric heating plate digestion/ICP-MS method Download PDFInfo
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G—PHYSICS
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Abstract
The invention discloses a method for measuring the content of nine heavy metals in sugarcane juice with an electric heating plate digestion/ICP-MS method.The method includes the following steps that 1, sample pretreatment is carried out, wherein sugarcane juice is measured and then subjected to heating digestion with an electric heating plate, residues in a conical flask are dissolved and washed into a 10 mL volumetric flask with 2 mL of a nitric acid solution after digestion is finished, washing is repeatedly carried out with ultrapure water to make the volume constant at a scale of the volumetric flask, and the mixture is shaken evenly to serve as a sample solution for on-machine measurement; 2, multiple blank solutions are prepared through the step 1 besides a sample without sugarcane juice; 3, a standard solution is prepared from a multi-element mixed standard stock solution containing Cu, Zn, Pb, Cd, As, Cr, Ni, V and Co, and a working curve of the standard solution is measured; 4, ICP-MS measurement is carried out.By means of the method, the content of heavy metals in sugarcane juice can be easily, rapidly, efficiently and accurately detected.
Description
Technical field
The present invention relates to the assay method of a kind of content of beary metal, specifically a kind of heating board digestion/ICP-MS method measures Caulis Sacchari sinensis juice
In the method for 9 heavy metal species content.
Background technology
Sugar is the necessary of human lives, can be changed into glucose and fructose, be to provide and ensure human life after human consumption
Movable heat energy source, the energy that can be supplied to human body accounts for more than the 50% of whole energy, it can also be ensured that human brain, erythrocyte etc.
Energy；It is provided that the carbon required for biosynthesis, eats sugar in right amount and can also reduce the consumption of hepatic glycogen, suppress protein
And steatolysis, prevent nutrient substance consumption in liver, the state of an illness of hepatitis patient is had certain mitigation.It addition, sugar is extensively
It is applied to all trades and professions, can be used for preparing medicines, light industry and food and beverage.
The main sugaring raw material of China has Caulis Sacchari sinensis and Radix Betae, and wherein cane suger accounts for more than the 92% of whole nation sugar yield, and beet sugar only accounts for
7-8%.And south China area is main Sugar Industry producing region, especially Guangxi is as maximum product sugar area, its candy output
Account for more than the 70% of whole nation total output.Currently, food safety is the major issue of people's common concern, it is ensured that sugar produces
The quality of product, first has to ensure raw material sugarcane and the quality of squeezing link Caulis Sacchari sinensis juice, this is most basic requirement.
Along with the raising of living standards of the people, people more pay attention to the safety problem of food.Countries in the world are to sugar product now
Quality safety has strict requirements and corresponding codes and standards, to the quality and safety control of sugar manufacturing industry Sugar Production process it is also proposed that
Higher requirement.Wherein, the laboratory of Sugar Production enterprise plays vital effect in sugar quality and safety control.
Sugar Production enterprise is by introducing advanced detection analytical equipment (such as gas chromatograph, high performance liquid chromatograph and atomic absorption light
Spectrometer etc.), harmful substance present in each product of production process is detected and monitors, with guarantee sugar product safety and
Sanitary index complies with the national standard requirements.
In recent years, around some mining area, Guangxi, heavy metals in farmland is seriously polluted, and the Caulis Sacchari sinensis content of beary metal accumulation being planted on farmland is obvious,
Security presence risk to sugar, domestic sugar enterprise should monitor the content of beary metal of sugar refining technology links corresponding product in real time.And
Squeezing the first step as sugar refining technology, domestic shortage is to the GB side of Analysis of Heavy Metal in its Caulis Sacchari sinensis first expressed juice after squeezing
Method, the features such as it is deep, rich in sugar that first expressed juice has color, and viscosity is big, also become the difficult point of analysis heavy metal content, therefore,
Set up the analysis method that in Caulis Sacchari sinensis first expressed juice, heavy metal is advanced and contribute to the monitoring of heavy metal element, to guarantee the peace of sugar product
Complete and sanitary index complies with the national standard requirements.
Summary of the invention
Present invention aims to problems of the prior art, it is provided that the simplest a kind of heating board digestion/ICP-MS
Method measures the method for 9 heavy metal species content in Caulis Sacchari sinensis juice.
For achieving the above object, present invention employs following technical scheme: a kind of heating board digestion/ICP-MS method measures sweet
The method of 9 heavy metal species content in sugarcane juice, it comprises the steps,
1) sample pre-treatments:
1-1. measures Caulis Sacchari sinensis juice sample, puts in conical flask；
1-2. adds 20-25mL concentrated nitric acid in the conical flask contain sample, and nitric acid with the volume ratio of Caulis Sacchari sinensis juice sample is
2-2.5:1, shakes up the little funnel of insertion, stands 25-30min, complete pre-clearing up；
1-3. will complete pre-clearing up after Caulis Sacchari sinensis juice together with conical flask be placed on electric hot plate heating clear up, electric plate temperature controls 180
± 5 DEG C, disappearing to boil to 4-5mL cools down under fume hood, adds 15mL chloroazotic acid and continues to heat on electric hot plate to clear up, electric hot plate
Temperature controls, at 180 ± 5 DEG C, to disappear and boil to 1-2mL transparency liquid；
After 1-4. clears up, add the salpeter solution that 2mL volume ratio is 50% and the residue dissolving in conical flask is washed 10mL
In volumetric flask, repeatedly rinse with ultra-pure water and be settled to volumetric flask scale, shake up, as sample solution, treat that machine measures；
2) in addition to being not added with Caulis Sacchari sinensis juice sample, the step 1 described in utilization), prepare many parts of blank solutions；
3) it is configured to standard with the mixture of multi-elements Standard Reserving Solution containing Cu, Zn, Pb, Cd, As, Cr, Ni, V and Co molten
Liquid, and measure its working curve；
4) ICP-MS measures:
Adjust ICP-MS apparatus measures parameter with instrument tuning liquid, choose63Cu、66Zn、208Pb、111Cd、75As、52Cr、60Ni、51V and59Co as the mass number of element to be measured,72Ge,115In,209Bi is internal standard element, in order sequentially determining standard solution,
The content of Cu, Zn, Pb, Cd, As, Cr, Ni, V and Co in blank solution and sample solution, if sample concentration is above standard
Curve, redeterminates after diluted sample.
Additionally, the present invention also provides for following attached technical scheme:
Sugar refinery's first expressed juice through squeezing process taken from by Caulis Sacchari sinensis juice sample in described step 1-1.
Conical flask in described step 1-2 is placed in fume hood standing.
Concentrated nitric acid in described step 1-2 is that top grade is pure, and the mass percent concentration of concentrated nitric acid is 65%.
The disappearing of described step 1-3 rocks conical flask during boiling reaction, in order to gas release and organic principle fast decoupled.
Described step 3) in standard solution with 1% or 2% salpeter solution dilute preparation, standard series mass concentration is respectively 0,
0.5,1.0,5.0,10.0,50.0,100.0,200.0ug/L。
Described step 4) in instrument tuning liquid include Li, Y, Tl, Ce and Co, mass concentration is 1ug/L.
Described step 4) in the instrument parameter of ICP-MS instrument be: RF launches power/W:1550；Nebulizer: glass is concentric
Nebulizer；Aerochamber temperature/: 2 DEG C；Sampling spiroid/intercepting cone: 1.0/0.4 nickel is bored；Atomization gas flow: 1.03L min-1；
Plasma flow amount: 15.00L min-1；Sampling configuration: the most quantitative；Measurement point: 3 points；Number of repetition: 3 times；Double
Charge number/%:Ce++/Ce+＜ 2.0；Oxide/%:CeO+/Ce+＜ 1.5；Sampling depth: 10.00mm.
Present invention have an advantage that and use electric hot plate to clear up to be processed into by Caulis Sacchari sinensis first expressed juice sample acid adding after squeezing process and clear up
After liquid, utilize nebulizer that digestion solution is delivered to inductively coupled plasma and be heated, through pervaporation, dissociate, atomization, ionization
Being converted into positively charged ion etc. process, this ion enters mass spectrograph through ion acquisition system and detects.By inductive etc.
Ion mass-spectrometer (ICP-MS) is analyzed and is measured copper, zinc, lead, cadmium, arsenic, chromium, nickel, vanadium and 9 kinds of elements of cobalt in digestion solution
Content, chooses63Cu、66Zn、208Pb、111Cd、75As、52Cr、60Ni、51V and59Co as the mass number of element to be measured,
Line adds internal standard element72Ge,115In,209Bi.The mass signal response treating measured ion based on certain mass-to-charge ratio and entrance mass spectrograph
In number of ions be direct proportionality, therefore, the concentration of sample element can be measured by mass spectrometric signal-count, use
Standard curve method calculates 9 Heavy Metallic Elements content, has simple, quickly, efficiently, and the advantage such as accurately.
Detailed description of the invention
Below in conjunction with preferred embodiment, technical solution of the present invention is further non-limitingly described in detail.
A kind of heating board digestion/ICP-MS method disclosed by the invention measures the method for 9 heavy metal species content, the method in Caulis Sacchari sinensis juice
Use electric hot plate and inductivity coupled plasma mass spectrometry (ICP-MS), Caulis Sacchari sinensis root, cane stalk, leaf of Caulis Sacchari sinensis and bagasse can be detected
In 9 heavy metal species content, shown in it comprises the following steps that,
1) sample pre-treatments:
Sugar refinery's first expressed juice through squeezing process taken from by 1-1. Caulis Sacchari sinensis juice sample, measures Caulis Sacchari sinensis juice sample and puts in conical flask；
1-2. adds 20-25mL concentrated nitric acid in the conical flask contain sample, and concentrated nitric acid is that top grade is pure, the quality hundred of concentrated nitric acid
Proportion by subtraction concentration is 65%, and nitric acid is 2-2.5:1 with the volume ratio of Caulis Sacchari sinensis sample, shakes up the little funnel of insertion, is placed in fume hood standing
25-30min, completes pre-clearing up；
1-3. will complete pre-clearing up after Caulis Sacchari sinensis juice together with conical flask be placed on electric hot plate heating clear up, electric plate temperature controls
180 ± 5 DEG C, disappear and rock conical flask during boiling reaction, in order to gas release and organic principle fast decoupled；Disappear and boil to about 5mL
Cooling down under fume hood, add 15mL chloroazotic acid and continue to heat on electric hot plate to clear up, electric plate temperature controls at 180 ± 5 DEG C,
Disappear and boil to about 1-2mL transparency liquid.
After 1-4. clears up, add the salpeter solution that 2mL volume ratio is 50% and the residue dissolving in conical flask is washed 10mL
In volumetric flask, repeatedly rinse with ultra-pure water and be settled to volumetric flask scale, shake up, as sample solution, treat that machine measures；
2) three parts of blank solutions of preparation:
In empty conical flask, it is sequentially added into the concentrated nitric acid that 20-25mL mass percent concentration is 65%, and 15mL chloroazotic acid, shakes up slotting
Enter little funnel, in fume hood, stand 25-30min, be subsequently placed on electric hot plate heating and clear up, electric plate temperature 180 ± 5 DEG C,
Disappear and boil to about 1-2m, with the salpeter solution that 2mL volume ratio is 50%, the residue dissolving in conical flask is washed in 10mL volumetric flask,
Repeatedly rinse with ultra-pure water and be settled to volumetric flask scale, shake up, as blank solution.Method according to this, does three parts of blank solutions.
3) configuration standard solution, and measure its working curve:
Standard solution is with the salpeter solution dilution mixture of multi-elements Standard Reserving Solution preparation that concentration of volume percent is 1% or 2%
Becoming, be settled in 50mL volumetric flask, standard series mass concentration is respectively 0, and 0.5,1.0,5.0,10.0,50.0,100.0,
200.0ug/L.Containing Cu, Zn, Pb, Cd, As, Cr, Ni, V and Co in above-mentioned mixture of multi-elements Standard Reserving Solution
4) ICP-MS measures:
With containing Li, Y, Tl, Ce and Co, mass concentration is that the instrument tuning liquid of 1ug/L adjusts ICP-MS apparatus measures parameter,
Make instrument be in optimum condition: RF and launch power/W:1550；Nebulizer: glass concentric atomizer；Aerochamber temperature/: 2 DEG C；
Sampling spiroid/intercepting cone: 1.0/0.4 nickel is bored；Atomization gas (argon) flow: 1.03L min-1；Plasma bromhidrosis (argon)
Flow: 15.00L min-1；Sampling configuration: the most quantitative；Measurement point: 3 points；Number of repetition: 3 times；Double charge number/%:Ce++/
Ce+＜ 2.0；Oxide/%:CeO+/Ce+＜ 1.5；Sampling depth: 10.00mm.Choose63Cu、66Zn、208Pb、111Cd、75As、52Cr、60Ni、51V and59Co as the mass number of element to be measured,72Ge,115In,209Bi is internal standard element, in order
Sequentially determining standard solution, blank solution and sample solution, the curve if sample concentration is above standard, again survey after diluted sample
Fixed.
Above-mentioned instrument tuning liquid is that Agilent company of the U.S. produces, and ICP-MS is Agilent7700e type.
Result of the test: Cu, Zn, Pb, Cd, As, Cr, Ni, V and Co, the standard corresponding to 9 kinds of element determinations respectively is bent
Line, linear relationship is good, and correlation coefficient is 0.9998-1.0000.This method detection is limited to 0.03～5.27 μ g/L, under mensuration
Being limited to 0.013～132 μ g/L, it is 0.54-14.76% that actual sample measures precision, and the response rate is 85.8-105.5%..
Method detection limit and Determination Limit:
When Caulis Sacchari sinensis juice sampling amount is 10ml, the method detection that full dose is cleared up is limited to 0.03～5.27 μ g/L, and Determination Limit is
0.013～132 μ g/L.
According in " environmental monitoring and analysis method standard revision technique directive/guide " (HJ168-2010) appendix A to method detection limit
General confirmation method, according to all processes of sample analysis, repeat n (n >=) secondary blank assay, by formula (1) calculating side
Method detection limit.
MDL=t (n-1,0.99) × S (1)
In formula: MDL method detection limit；
The parallel assay number of times of n sample；
T degree of freedom is n-1, and confidence level is the t-distribution (unilateral) when 99%；
The standard deviation of n replication of S；
Single laboratory is repeated 7 times blank experiment, t (n-1,0.99)=3.143, and method detection limit test data are shown in Table 1.
Table 1 method detection limit and Determination Limit test tables of data
Table 2 reagent blank recovery of standard addition measurement result
Table 3 Caulis Sacchari sinensis juice sample recovery of standard addition measurement result
In sum, the present invention uses heating board digestion pre-treating method, with Inductively coupled plasma mass spectrometry (ICP-MS) point
Analysis measures the content of 9 kinds of elements of Cu, Zn, Pb, Cd, As, Cr, Ni, V and Co in digestion solution, chooses63Cu、66Zn、208Pb、111Cd、75As、52Cr、60Ni、51V and59Co, as the mass number of element to be measured, adds internal standard element online72Ge,115In,209Bi.The mass signal response treating measured ion of certain mass-to-charge ratio is direct proportionality with the number of ions entered in mass spectrograph, logical
Cross mass spectrometric signal-count and can measure the concentration of sample element, use standard curve method to calculate 9 Heavy Metallic Elements content.
The pre-treating method of heating board digestion, can enable sample the most thoroughly decompose, it is provided that work efficiency；In conjunction with inductive
Plasma mass spectrometry, can realize quickly detecting detection device for multi metallic elements simultaneously, and the advantage such as it is low to have detection limit, detection range width,
Therefore the method for the present invention can be simple, quick, can detect the content of heavy metal in Caulis Sacchari sinensis juice efficiently and accurately.
Claims (8)
1. heating board digestion/ICP-MS method measures the method for 9 heavy metal species content in Caulis Sacchari sinensis juice, it is characterised in that include
Following steps,
1) sample pre-treatments:
1-1. measures Caulis Sacchari sinensis juice sample, puts in conical flask；
1-2. adds 20-25mL concentrated nitric acid in the conical flask contain sample, and nitric acid with the volume ratio of Caulis Sacchari sinensis juice sample is
2-2.5:1, shakes up the little funnel of insertion, stands 25-30min, complete pre-clearing up；
1-3. will complete pre-clearing up after Caulis Sacchari sinensis juice together with conical flask be placed on electric hot plate heating clear up, electric plate temperature controls 180
± 5 DEG C, disappearing to boil to 4-5mL cools down under fume hood, adds 15mL chloroazotic acid and continues to heat on electric hot plate to clear up, electric hot plate
Temperature controls, at 180 ± 5 DEG C, to disappear and boil to 1-2mL transparency liquid；
After 1-4. clears up, add the salpeter solution that 2mL volume ratio is 50% and the residue dissolving in conical flask is washed 10mL
In volumetric flask, repeatedly rinse with ultra-pure water and be settled to volumetric flask scale, shake up, as sample solution, treat that machine measures；
2) in addition to being not added with Caulis Sacchari sinensis juice sample, the step 1 described in utilization), prepare many parts of blank solutions；
3) it is configured to standard with the mixture of multi-elements Standard Reserving Solution containing Cu, Zn, Pb, Cd, As, Cr, Ni, V and Co molten
Liquid, and measure its working curve；
4) ICP-MS measures:
Adjust ICP-MS apparatus measures parameter with instrument tuning liquid, choose63Cu、66Zn、208Pb、111Cd、75As、52Cr、60Ni、51V and59Co as the mass number of element to be measured,72Ge,115In,209Bi is internal standard element, in order sequentially determining standard solution,
The content of Cu, Zn, Pb, Cd, As, Cr, Ni, V and Co in blank solution and sample solution, if sample concentration is above standard
Curve, redeterminates after diluted sample.
Heating board digestion the most according to claim 1/ICP-MS method measures the method for 9 heavy metal species content in Caulis Sacchari sinensis juice,
It is characterized in that, sugar refinery's first expressed juice through squeezing process taken from by the Caulis Sacchari sinensis juice sample in described step 1-1.
Heating board digestion the most according to claim 1/ICP-MS method measures the method for 9 heavy metal species content in Caulis Sacchari sinensis juice,
It is characterized in that, the conical flask in described step 1-2 is placed in fume hood standing.
Heating board digestion the most according to claim 1/ICP-MS method measures the method for 9 heavy metal species content in Caulis Sacchari sinensis juice,
It is characterized in that, the concentrated nitric acid in described step 1-2 is that top grade is pure, and the mass percent concentration of concentrated nitric acid is 65%.
Heating board digestion the most according to claim 1/ICP-MS method measures the method for 9 heavy metal species content in Caulis Sacchari sinensis juice,
It is characterized in that, the disappearing of described step 1-3 rocks conical flask during boiling reaction, in order to gas release and organic principle fast decoupled.
Heating board digestion the most according to claim 1/ICP-MS method measures the method for 9 heavy metal species content in Caulis Sacchari sinensis juice,
It is characterized in that, described step 3) in standard solution with 1% or 2% salpeter solution dilute preparation, standard series mass concentration
It is respectively 0,0.5,1.0,5.0,10.0,50.0,100.0,200.0ug/L.
Heating board digestion the most according to claim 1/ICP-MS method measures the method for 9 heavy metal species content in Caulis Sacchari sinensis juice,
It is characterized in that, described step 4) in instrument tuning liquid include Li, Y, Tl, Ce and Co, mass concentration is 1ug/L.
Heating board digestion the most according to claim 1/ICP-MS method measures the method for 9 heavy metal species content in Caulis Sacchari sinensis juice,
It is characterized in that, described step 4) in the instrument parameter of ICP-MS instrument be: RF launches power/W:1550；Nebulizer:
Glass concentric atomizer；Aerochamber temperature/: 2 DEG C；Sampling spiroid/intercepting cone: 1.0/0.4 nickel is bored；Atomization gas flow: 1.03
L·min-1；Plasma flow amount: 15.00L min-1；Sampling configuration: the most quantitative；Measurement point: 3 points；Number of repetition:
3 times；Double charge number/%:Ce++/Ce+＜ 2.0；Oxide/%:CeO+/Ce+＜ 1.5；Sampling depth: 10.00mm.
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| CN108680562A (en) * | 2018-04-28 | 2018-10-19 | 长春黄金研究院有限公司 | The assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings |
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| CN110389166A (en) * | 2019-08-21 | 2019-10-29 | 珠海天祥粤澳质量技术服务有限公司 | The rapid detection method of heavy metal limit in a kind of food additives |
| CN112098603A (en) * | 2020-09-16 | 2020-12-18 | 广西大学 | Sugarcane seedling manganese toxicity diagnosis method and prevention and control method thereof |
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