CN105548051A - Method for measuring lead and arsenic in triacetin and digestion equipment of method - Google Patents
Method for measuring lead and arsenic in triacetin and digestion equipment of method Download PDFInfo
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- CN105548051A CN105548051A CN201610044141.2A CN201610044141A CN105548051A CN 105548051 A CN105548051 A CN 105548051A CN 201610044141 A CN201610044141 A CN 201610044141A CN 105548051 A CN105548051 A CN 105548051A
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- 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
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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Abstract
The invention provides a method for measuring lead and arsenic in triacetin and digestion equipment of the method. The method comprises the following processing steps that preparation of lead and arsenic standard working solutions; sample treatment of the digestion equipment; setting of operating conditions during measurement of a graphite furnace atomic absorption spectrometer; measuring of the lead and arsenic contents respectively. The digestion equipment is a microwave digestion instrument. The method can measure the lead and arsenic contents in the triacetin rapidly and accurately, and the operation is simple, convenient and safe.
Description
Technical field
The present invention relates to assay method and the equipment of minor metallic element in a kind of glyceryl triacetate.
Background technology
At present both at home and abroad tobacco business generally using glyceryl triacetate as the plastifier in filter stick, its quality has significant impact to cigarette product safety and suction taste, tobacco business has formulated " cigarette glyceryl triacetate " product standard (YC144), all having made regulation to assay method that is plumbous in glyceryl triacetate, arsenic, is " mensuration plumbous in GB/T5009.75 food additives " and the mensuration of arsenic " in the GB/T5009.76 food additives " respectively.
In routine testing glyceryl triacetate lead, arsenic work, find that traditional detection method needs to use miscellaneous reagent, has plenty of toxic articles (potassium cyanide), and complex operation step, testing efficiency is not high.
Number of patent application is that the invention of 201310331837X belongs to alloy trace element analysis technology, relates to the analytical approach of AFS DETERMINATION containing tellurium in tantalum high temperature alloy.The present invention adopts standard addition method namely to take to add hydrochloric acid, nitric acid containing the some parts of tantalum high temperature alloy test portion, and on electric hot plate, low-grade fever is dissolved completely to test portion; Add citric acid solution, heating is boiled; Solution is moved in 50mL volumetric flask, add tellurium standard solution successively, be diluted to scale with water, shake up.The present invention's Standard entertion and add the method for citric acid solution, eliminates matrix element nickel and coexistence elements tantalum, cobalt to the interference of tellurium.The method can not be directly used in measures trace element lead and arsenic.
The assay method of lead content in number of patent application a kind of glyceryl triacetate that has been the disclosure of the invention of 201310113751X, it is characterized in that: at pretreatment stage absolute ethyl alcohol dilute sample, adopt standard addition method, and air oxidation program is added in the middle of the drying and ash process of Atomic Absorption Spectrometer heating schedule, realize sample direct injected to measure, fast, accurately can detect content plumbous in glyceryl triacetate.Digest with traditional electric hot plate and micro-wave digestion pre-treatment is compared, direct injected element loss to be measured is few, be easy to operation, and experimentation does not use poisonous and harmful chemicals, endangers little to operating personnel.This invention does not have fully open to relevant technological process and technological parameter, not easily with reference to implementing.
Summary of the invention
Goal of the invention: provide a kind of and adopt GFAAS (graphite furnace atomic absorption spectrometry), accurately, quickly and easily survey
Determine the lead in glyceryl triacetate, the major equipment of arsenic content and assay method thereof.
Technical scheme:
Lead in GFAAS (graphite furnace atomic absorption spectrometry) mensuration glyceryl triacetate provided by the invention, the mensuration forwarding method of arsenic content, comprise following processing step:
1) preparation of arsenic, plumbous standard working solution:
Arsenic, the plumbous storing solution of first configuration concentration 1000.0mg/L.Accurately pipette storing solution in 100mL volumetric flask, with 1% nitric acid constant volume, stepwise dilution arrives: arsenic uses the concentration 50 μ g/L of liquid, the plumbous concentration 100 μ g/L using liquid.
The arsenic pipetting different volumes respectively uses liquid, the plumbous liquid that uses in different 50mL volumetric flasks, uses 1% nitric acid constant volume respectively, obtains the arsenic of variable concentrations, plumbous standard working solution respectively.The multiple arsenic prepared respectively, plumbous standard working solution, its concentration range should cover the content of arsenic that expectation detects in the sample, lead element.
2) digesting equipment of microwave dissolver is adopted to carry out sample preparation:
The digesting equipment of described microwave dissolver has micro-wave diminishing pot (teflon is made), micro-wave digestion case, pressue device, micro-wave diminishing pot is placed in micro-wave digestion case, micro-wave diminishing pot top has acid-adding port, upper lateral part has and adds pore, have the register heating cooling function at the bottom of the tank wall of micro-wave digestion case and case, pressue device adds pore by gas-adding pipe UNICOM and adds compressed argon in micro-wave diminishing pot.
Accurately take 1.0g glyceryl triacetate sample respectively, be placed in micro-wave diminishing pot.In micro-wave diminishing pot, 5mL nitric acid, 1mL hydrochloric acid and 1mL hydrofluorite is added successively by acid-adding port, micro-wave digestion case is loaded after sealing, enter micro-wave diminishing pot by pressue device and the argon gas that adds pore input 3-4atm, then carry out progressive solution by program below, carry out micro-wave digestion:
95-105 DEG C was warming up to through 4-6 minute, insulation 4-6 minute from room temperature; Then, 125-135 DEG C was warming up at 4-6 minute, insulation 4-6 minute; Then, be warming up to 155-165 DEG C at 4-6 minute, insulation 4-6 minute; Finally, be warming up to 180-200 DEG C at 4-6 minute, insulation 20-30 minute.
Clear up complete, by register, the micro-wave diminishing pot in microwave dissolver is down to less than 40 DEG C, temperature adjustment is heated at 120-130 DEG C again, and heating catches up with acid to about 0.5mL.After being cooled to room temperature, be transferred to by sample solution in 50mL volumetric flask, rinse counteracting tank 3 ~ 4 times with 1% nitric acid, cleaning fluid is transferred in 50mL volumetric flask equally, then uses 1% nitric acid constant volume, shakes up rear to be measured.
3) setting of operating conditions when adopting graphite furnace atomic absorption spectrophotometer to measure, as shown in table 1:
Wherein, the standard working solution of arsenic or lead and the test liquid after clearing up constant volume, first adopt the primary drying process of the temperature 30s of intensification duration 5s to 110 DEG C respectively, then adopt the redrying process of the temperature 30s of intensification duration 15s to 130 DEG C;
Then, the standard working solution of arsenic and the test liquid after clearing up constant volume, adopt the podzolic process of the temperature 20s of intensification duration 10s to 1450 DEG C respectively; Adopt the atomization process of the temperature 5s of 2250 DEG C more respectively.
Plumbous standard working solution and the test liquid after clearing up constant volume, adopt the podzolic process of the temperature 20s of intensification duration 10s to 1000 DEG C respectively; Adopt the atomization process of the temperature 5s of 1950 DEG C more respectively.
Finally, their purification temperature is 2450 DEG C of maintenance 3s durations.
4) graphite furnace atomic absorption spectrophotometer is adopted to measure arsenic in sample, lead content and calculating respectively:
4.1) measurement and calculation of arsenic content in sample
Draw arsenic standard working solution and each 20 μ L injection graphite furnaces of the test liquid after clearing up constant volume, preferably with palladium nitrate solution 5 μ L and magnesium nitrate solution 3 μ L(as matrix modifier, test arsenic data are more accurate) inject graphite furnace together, record the absorbance of arsenic, substitute into the unary linear regression equation of arsenic, try to achieve the arsenic content in test liquid.
4.2) measurement and calculation of lead content in sample
The each 20 μ L of test liquid after drawing plumbous standard working solution and clearing up constant volume inject graphite furnace, preferably with palladium nitrate solution 5 μ L(as matrix modifier, test plumbous data more accurate) inject graphite furnace together, record plumbous absorbance, substitute into plumbous unary linear regression equation, try to achieve the lead content in test liquid.
Wherein, unary linear regression equation:
, in formula:
X---arsenic, plumbous content (mg/kg) in sample;
C---measure arsenic in sample liquid, plumbous concentration (μ g/L);
C
0---the concentration (μ g/L) of arsenic or lead in arsenic or plumbous standard working solution;
The cumulative volume (mL) of V---sample digestive juice;
M---sample mass (g).
The mean value getting twice parallel determinations, as final testing result, is accurate to 0.1mg/kg.
Beneficial effect:
The requirement of current tobacco business to starting material sanitary index improves constantly, and testing amount is large, and in atomic absorption spectrometry glyceryl triacetate, the method for lead, arsenic, can measure the content of the lead in glyceryl triacetate, arsenic quickly and accurately.
Through clearing up process sample, arsenic and lead are fully dissolved or chemical reaction becomes ion, measuring result error is little, and these two kinds of compositions adopt the PROCESS FOR TREATMENT of general character after have and adopt respective subsequent treatment process parameter respectively, often kind of composition test simultaneously accurately, reduce the workload of test, make easy and simple to handle, operating personnel are safer.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation of microwave dissolver of the present invention;
In figure, 1-micro-wave digestion case, 2-register, 3-micro-wave diminishing pot, 4-acid-adding port, 5-add pore, 6-gas-adding pipe, 7-pressue device.
Embodiment
Lead in mensuration glyceryl triacetate of the present invention, the method for arsenic, have following process steps: the preparation respectively of arsenic, plumbous standard working solution; The digesting equipment of microwave dissolver is adopted to carry out sample preparation; Adopt the setting respectively of operating conditions when graphite furnace atomic absorption spectrophotometer mensuration arsenic, lead content; Graphite furnace atomic absorption spectrophotometer is adopted to measure arsenic in sample, lead content respectively.Wherein,
1), in the preparation respectively of arsenic, plumbous standard working solution, the multiple arsenic prepared respectively, plumbous standard working solution, its concentration range should cover the content of arsenic that expectation detects in the sample, lead element.
2) digesting equipment carries out, in sample preparation, being warming up to 95-105 DEG C from room temperature through 4-6 minute, insulation 4-6 minute; Then, 130-135 DEG C was warming up at 4-6 minute, insulation 4-6 minute; Then, be warming up to 160-165 DEG C at 4-6 minute, insulation 4-6 minute; Finally, be warming up to 190-200 DEG C at 4-6 minute, insulation 20-30 minute; Digesting equipment carries out in sample preparation, after clearing up, by register, the micro-wave diminishing pot in microwave dissolver is down to less than 40 DEG C, and temperature adjustment is heated at 125-130 DEG C again, and heating catches up with acid to about 0.5mL; With 1% nitric acid constant volume after cooling.Digesting equipment as shown in Figure 1, there is micro-wave diminishing pot 3, micro-wave digestion case 1, pressue device 7, micro-wave diminishing pot 3 is placed in micro-wave digestion case 1, micro-wave diminishing pot 3 top has acid-adding port 4, upper lateral part has and adds pore 5, have the register 2 heating cooling function at the bottom of the tank wall of micro-wave digestion case 1 and case, pressue device 7 can add pore 5 to the compressed argon of adding 3-4atm in micro-wave diminishing pot 3 by gas-adding pipe 6 UNICOM.
3) graphite furnace atomic absorption spectrophotometer measure time operating conditions setting in, the standard working solution of arsenic or lead and the test liquid after clearing up constant volume, first adopt the primary drying process of the temperature 30s of intensification duration 5s to 110 DEG C respectively, then adopt the redrying process of the temperature 30s of intensification duration 15s to 130 DEG C.
The standard working solution of arsenic and the test liquid after clearing up constant volume, adopt the podzolic process of the temperature 20s of intensification duration 10s to 1450 DEG C respectively; Adopt the atomization process of the temperature 5s of 2250 DEG C more respectively; Plumbous standard working solution and the test liquid after clearing up constant volume, adopt the podzolic process of the temperature 20s of intensification duration 10s to 1000 DEG C respectively; Adopt the atomization process of the temperature 5s of 1950 DEG C more respectively.
4) mensuration respectively of arsenic, lead content in sample:
Draw arsenic standard working solution and each 20 μ L of test liquid after clearing up constant volume, inject graphite furnace with palladium nitrate solution 5 μ L together with magnesium nitrate solution 3 μ L; Record the absorbance of arsenic, substitute into the unary linear regression equation of arsenic, try to achieve the content of the arsenic in test liquid.
The each 20 μ L of test liquid after drawing plumbous standard working solution and clearing up constant volume inject graphite furnace, inject graphite furnace together with palladium nitrate solution 5 μ L.Record plumbous absorbance, substitute into plumbous unary linear regression equation, try to achieve the content of the lead in test liquid.
Table 1 graphite furnace atomic absorption spectrophotometer arsenic, plumbous measurement operation condition:
Claims (6)
1. measure a method for the lead in glyceryl triacetate, arsenic, there is the processing step prepared respectively of arsenic, plumbous standard working solution, it is characterized in that: also have following process steps: adopt the digesting equipment of microwave dissolver to carry out sample preparation; Adopt the setting respectively of operating conditions when graphite furnace atomic absorption spectrophotometer mensuration arsenic, lead content; Graphite furnace atomic absorption spectrophotometer is adopted to measure arsenic in sample, lead content respectively;
1) in the preparation respectively of arsenic, plumbous standard working solution, the multiple arsenic prepared respectively, plumbous standard working solution, its concentration range should cover the content of arsenic that expectation detects in the sample, lead element;
2) digesting equipment carries out, in sample preparation, being warming up to 95-105 DEG C from room temperature through 4-6 minute, insulation 4-6 minute; Then, 125-135 DEG C was warming up at 4-6 minute, insulation 4-6 minute; Then, be warming up to 155-165 DEG C at 4-6 minute, insulation 4-6 minute; Finally, be warming up to 180-200 DEG C at 4-6 minute, insulation 20-30 minute;
3) graphite furnace atomic absorption spectrophotometer measure time operating conditions setting in, the standard working solution of arsenic or lead and the test liquid after clearing up constant volume, first adopt the primary drying process of the temperature 30s of intensification duration 5s to 110 DEG C respectively, then adopt the redrying process of the temperature 30s of intensification duration 15s to 130 DEG C;
4) in sample arsenic, lead content mensuration respectively in:
Draw the standard working solution of arsenic or lead and each 20 μ L of test liquid after clearing up constant volume inject graphite furnaces, record the absorbance of arsenic, substitute into the unary linear regression equation of arsenic or lead, try to achieve the content of arsenic in test liquid or lead.
2. the method for the lead measured in glyceryl triacetate as claimed in claim 1, arsenic, is characterized in that:
Digesting equipment carries out in sample preparation, after clearing up, by register, the micro-wave diminishing pot in microwave dissolver is down to less than 40 DEG C, and temperature adjustment is heated at 120-130 DEG C again, and heating catches up with acid to about 0.5mL; With 1% nitric acid constant volume after cooling.
3. the method for the lead measured in glyceryl triacetate as claimed in claim 1 or 2, arsenic, is characterized in that:
When graphite furnace atomic absorption spectrophotometer measures operating conditions setting in, the standard working solution of arsenic and the test liquid after clearing up constant volume, adopt the podzolic process of the temperature 20s of intensification duration 10s to 1450 DEG C respectively; Adopt the atomization process of the temperature 5s of 2250 DEG C more respectively; Plumbous standard working solution and the test liquid after clearing up constant volume, adopt the podzolic process of the temperature 20s of intensification duration 10s to 1000 DEG C respectively; Adopt the atomization process of the temperature 5s of 1950 DEG C more respectively.
4. the lead in the mensuration glyceryl triacetate as described in claim 1 or 2,3, the method for arsenic, it is characterized in that: arsenic standard working solution and each 20 μ L of test liquid after clearing up constant volume, inject graphite furnace with palladium nitrate solution 5 μ L together with magnesium nitrate solution 3 μ L;
Plumbous standard working solution and each 20 μ L of the test liquid after clearing up constant volume inject graphite furnace, inject graphite furnace together with palladium nitrate solution 5 μ L.
5. the digesting equipment adopted in the lead in a mensuration glyceryl triacetate according to claim 1, the method for arsenic, it is characterized in that: there is micro-wave diminishing pot, micro-wave digestion case, pressue device, micro-wave diminishing pot is placed in micro-wave digestion case, micro-wave diminishing pot top has acid-adding port, upper lateral part has and adds pore, have the register heating cooling function at the bottom of the tank wall of micro-wave digestion case and case, pressue device adds pore by gas-adding pipe UNICOM and adds compressed argon in micro-wave diminishing pot.
6. digesting equipment as claimed in claim 5, is characterized in that: micro-wave diminishing pot adopts teflon to make.
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| CN108204967A (en) * | 2018-01-05 | 2018-06-26 | 北京博康健基因科技有限公司 | The quality determining method of the detection method of cadmium salt and magnesium stearate in magnesium stearate |
| CN109738269A (en) * | 2019-02-22 | 2019-05-10 | 安徽科技学院 | A kind of soil tenor inspection side device based on heavy metals mining area soil remediation |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108204967A (en) * | 2018-01-05 | 2018-06-26 | 北京博康健基因科技有限公司 | The quality determining method of the detection method of cadmium salt and magnesium stearate in magnesium stearate |
| CN109738269A (en) * | 2019-02-22 | 2019-05-10 | 安徽科技学院 | A kind of soil tenor inspection side device based on heavy metals mining area soil remediation |
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Application publication date: 20160504 |