CN105092499B - A kind of assay method of iron content in the oxide of 9,10 dihydro, 9 oxa-, 10 phospho hetero phenanthrene 10 - Google Patents
A kind of assay method of iron content in the oxide of 9,10 dihydro, 9 oxa-, 10 phospho hetero phenanthrene 10 Download PDFInfo
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Abstract
The present invention relates to a kind of oxide of 10 phospho hetero phenanthrene of 9,10 dihydro, 9 oxa- 10（Abbreviation DOPO）The assay method of middle iron content, is specifically to be determined with atomic absorption spectrophotometry.The sample solution of appropriate concentration is first prepared, sample is gasified by flame atomizer, based on the absorption of gaseous state ground state atom pair characteristic wavelength light for measuring tested elemental iron, so as to determine the content that elemental iron is tested in sample.With using phenanthroline AAS, EDTA is titrated, ICP OES, ICP MS, the methods such as atomic absorption spectrophotometry are compared, sample need not be carried out clearing up processing, safety coefficient is greatly improved, and is disturbed small, agents useful for same is less, preparation is simple, safety simple and efficient to handle, testing cost is low, and testing result reappearance and the degree of accuracy are good.
Description
Technical field
The present invention relates to a kind of assay method of iron ion content, iron in more particularly to a kind of organic phosphates heterocyclic compound
The assay method of ion concentration.
Background technology
DOPO is organic phosphates heterocyclic compound, with higher heat endurance, and inoxidizability and excellent water resistance are
Response type and additive flame retardant.
Bring the raw material of iron ion into due to being employed in DOPO synthesis, therefore just contain a certain amount of iron in DOPO finished products
Ion.In order to ensure the requirement of product quality, it is necessary to detect the iron ion content in DOPO.
At present, the detection method of iron ion content is more, there is phenanthroline AAS, and EDTA is titrated, ICP-OES,
ICP-MS, the method such as atomic absorption spectrophotometry.But detect metal impurities, such as iron ion in the organic matters such as DOPO products
Method, be showed no Chinese literature report.The present invention, by test of many times, is updated on the basis of above several method
Comparison condition is tested, and is finally chosen atomic absorption spectrophotometry, is improved traditional flame atomic adsorption spectrophotometry
The condition of method so that detection method is suitable for product DOPO, there is innovative point.With using phenanthroline AAS, EDTA
Titrate, ICP-OES, ICP-MS, the method such as atomic absorption spectrophotometry is compared, it is not necessary to sample is carried out to clear up place
Reason, safety coefficient greatly improves, and is disturbed small, and agents useful for same is less, preparation is simple, safety simple and efficient to handle, detects
Cost is low, and testing result reappearance and the degree of accuracy are good.
The content of the invention
Problem to be solved by this invention is to provide a kind of assay method of iron content in DOPO.
The present invention uses atomic absorption spectrophotometry.First plus in right amount solvent dissolves sample, in the sample that dissociates
The iron ion contained, is gasified sample by flame atomizer, to measure the gaseous state ground state atom pair of tested elemental iron
Based on the absorption of characteristic wavelength light, so as to determine the content that elemental iron is tested in sample.
Present invention experiment water used is all referring to two grades of water for meeting GB/T6682-2008.If other unreceipted requirements,
Standard titration solution, contamination levels solution, preparation and product used in experiment, by GB/T 601-2002, GB/T602-
2002nd, GB/T 603-2002 regulation is prepared and demarcation.Glass container used：Soaked with nitric acid (GR) solution (1+5)
At night, rinsed repeatedly with water.
The analysis method of the present invention is as follows：
1st, the preparation of test liquid and blank solution：1g~10g (being accurate to 0.1mg) sample is weighed, it is molten with 20-70mL ethanol
Solution sample is simultaneously quantitatively transferred to 100mL volumetric flasks, plus 1ml~10ml hydrochloric acid (GR), is configured to again with two grades of water constant volumes after shaking up
Volumetric concentration is 1%~10% test liquid.The preparation of blank solution refers to be not added with sample, other same processing (plus it is same
The ethanol and hydrochloric acid of amount, then it is settled to 100mL with two grades of water.The concentration and salt content of test liquid are unsuitable excessive.The acid of test liquid
Degree, which should ensure that, is not less than 1%HCl acidity (mass-volume concentration).It is required that test liquid clarifies bright, no turbid phenomenon.
2nd, the preparation of standard liquid series：Pipette respectively 0.00mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL,
8.00mL, 10.00mL iron standard liquid (20ug/mL, 40ug/mL or 50ug/mL are provided to prepare by GB/T 602-2002) are to 100mL
Volumetric flask, adds 20-70mL ethanol, plus 1ml~10ml hydrochloric acid (GR), again with two grades of water constant volumes after shaking up.The concentration of iron standard liquid
(20ug/mL, 40ug/mL or 50ug/mL) can be adjusted according to iron content in sample, and standard liquid preparation must and sample
Liquid is equally handled, and is prepared with organic solvent solution, refers to the ethanol and hydrochloric acid for adding isodose, then is settled to 100mL with two grades of water, with
Seek all prepare liquid uniformity of treatments.
3rd, measure standard liquid absorbance and do standard curve：With atomic absorption spectrophotometer, using flame method, using deuterium
Lamp buckles background correction, and standard serial solution is introduced into atomic absorption spectrophotometer successively, and selection analysis line is in 248.3nm ripples
Strong point is determined, and Air-acetylene Flame sets acetylene cylinder back pressure as 0.05Mpa during analysis, air outlet slit pressure is
0.24Mpa, acetylene flow is 1200-1800mL/min, sets instrument burner height 6-12mm, determines series standard solution
Luminous intensity.Linear regression is carried out to iron concentration C with the absorbance A of solution, equation of linear regression is simulated.
4th, measure test liquid absorbance and calculate content：Measure the absorbance of test liquid, according to absorbance and
Concentration relationship (standard curve), calculates the mass concentration for obtaining ferro element in sample.
The present invention uses atomic absorption spectrophotometry, and the measure for solving iron content in prior art DOPO is stranded
The maximum innovative point of the preparation of difficulty, test liquid and blank solution is：Traditional method is all direct or after clearing up with two grades
Water prepares test liquid, belongs to inorganic substrates solution system.The present invention, which is advocated, directly uses organic solvent solution sample dissolution, and control
The acidity of solution processed.Compared with traditional analysis method, sample need not clear up processing, safety coefficient is greatly improved.And behaviour
Make process reduction, be disturbed small.
Embodiment
Embodiment 1
Testing conditions：The general analysis atomic absorption spectrophotometer in TAS-986 Beijing, flame method, Air-acetylene Flame, air
Back pressure is 0.24Mpa, and acetylene cylinder back pressure is 0.05Mpa, acetylene flow 1400mL/min, wavelength 248.3nm, light
Bands of a spectrum wide 0.2nm, lamp current 4.0mA, burner height 10mm.Filter factor 0.6,3 seconds times of integration.Using deuterium lamp buckle back
Scape.
Sample preparation：1g (being accurate to 0.1mg) sample is weighed, 100mL is transferred to 50mL ethanol sample dissolution and quantitatively
Volumetric flask, plus 2ml hydrochloric acid, again with two grades of water constant volumes after shaking up, while preparing blank solution.5# samples are chosen, Duplicate Samples 8 are prepared
It is individual.
Experiment：0.00mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard liquid are pipetted respectively
(40ug iron mark/mL) is to 100mL volumetric flasks, plus 50mL ethanol, 2ml hydrochloric acid (GR), with two grades of water constant volumes.Survey under the same conditions
Its absorbance.Linear regression is carried out to iron concentration C with the absorbance A of solution, its regression equation is A=0.0580C+
0.0027, coefficient R=0.9992 (n=7).Precision：The actual measurement average value and relative standard deviation of sample concentration are calculated,
Precision represents that RSD is 2.83% with relative standard deviation (RSD).
Specific experiment data are as follows：
Embodiment 2
Testing conditions：The general analysis atomic absorption spectrophotometer in TAS-986 Beijing, flame method, Air-acetylene Flame, air
Back pressure is 0.24Mpa, and acetylene cylinder back pressure is 0.05Mpa, 1400mL/min, wavelength 248.3nm, spectral bandwidth
0.2nm, lamp current 4.0mA, burner height 10mm.Filter factor 0.6,3 seconds times of integration.Using deuterium lamp buckle back scape.
Linear equation is tested：Pipette respectively 0.00mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL,
10.00mL iron standard liquid (50ug iron mark/mL) is to 100mL volumetric flasks, plus 50mL ethanol, 2ml hydrochloric acid (GR), with two grades of water constant volumes.
Its absorbance is surveyed under the same conditions.Linear regression, its recurrence side are carried out to iron concentration C with the absorbance A of solution
Journey is A=0.0644C+0.0066, coefficient R=0.9976 (n=7).
Sample preparation：1g (being accurate to 0.1mg) sample is weighed, 100mL is transferred to 50mL ethanol sample dissolution and quantitatively
Volumetric flask, plus 2ml hydrochloric acid, again with two grades of water constant volumes after shaking up, while preparing blank solution.5# samples are chosen, Duplicate Samples 6 are produced
It is individual.
Precision：The actual measurement average value and relative standard deviation of sample concentration are calculated, precision is with relative standard deviation
(RSD) represent, RSD is 2.50%.
Recovery test：6, mark-on sample is prepared, each mark-on sample adds 80ug iron marks, it is following to prepare.
6,5# samples 1g (being accurate to 0.1mg) sample is weighed respectively, is transferred to 50mL ethanol sample dissolution and quantitatively
100mL volumetric flasks, plus 2mL hydrochloric acid, respectively toward in this 6 volumetric flasks, pipetting 8.00mL iron standard using solution (10ug/mL),
Again with two grades of water constant volumes, shake up.
As a result：In the above conditions, solution absorbance value is surveyed, its measured concentration is calculated further according to equation of linear regression, will
The corresponding iron content value of test liquid actual measurement absorbance of 80ug iron standard liquids is added, the test liquid of addition 0ug iron standard liquids is subtracted
Average content of iron value, obtained difference, divided by the iron scalar 80ug added, i.e. (C actual measurements/C is theoretical) * 100% are the rate of recovery.Sample
1~6 measures 5# samples iron-holder for 76.09mg/Kg；It is 109.77~114.09% that sample 7~12, which measures the rate of recovery,.
Claims (5)
1. it is with using flame the assay method of iron content in a kind of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide
Atomic absorption spectrophotometry specifically includes following steps come what is determined：
1）The preparation of test liquid and blank solution：
Sample is weighed, 100mL volumetric flasks are transferred to ethanol sample dissolution and quantitatively, plus hydrochloric acid, it is fixed with two grades of water again after shaking up
Hold, the test liquid of 1% ~ 10% mass-volume concentration is configured to, while doing blank assay；The preparation of blank solution refers to not add an examination of
Sample, but add the ethanol and hydrochloric acid of same amount, then it is settled to 100mL with two grades of water；
2）The preparation of standard liquid series：
0.00mL, 1.00mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL, 10.00mL iron standard liquid are pipetted respectively to 100mL appearances
Measuring bottle, is added and 1）The ethanol of isodose, plus with 1）The hydrochloric acid of isodose, again with two grades of water constant volumes after shaking up；
3）Measure standard liquid absorbance and do standard curve：
With atomic absorption spectrophotometer, using flame method, successively by step 2）The series standard solution of preparation introduces atom and inhaled
Receive in spectrophotometer, at analysis of line wavelength, the luminous intensity of series standard solution is determined, with the absorbance A of solution to iron
Ion concentration C carries out linear regression, simulates equation of linear regression；
4）Measure test liquid absorbance and calculate content：
With atomic absorption spectrophotometer, using flame method, successively by step 1）The test liquid of preparation introduces atomic absorption spectrophotometry
In photometer, at analysis of line wavelength, the absorbance of test liquid is determined, according to absorbance and concentration relationship, calculating is obtained
The mass concentration of ferro element in sample.
2. assay method according to claim 1, it is characterised in that：Determined using atomic absorption spectrophotometry
When, background correction is buckled using deuterium lamp, selection analysis line is determined at 248.3nm wavelength, and Air-acetylene Flame is set during analysis
Acetylene cylinder back pressure is 0.05Mpa, and air outlet slit pressure is 0.24Mpa, and acetylene flow is 1200-1800mL/min, if
Determine instrument burner height 6-12mm measure.
3. assay method according to claim 1, it is characterised in that prepare the test liquid of 1% ~ 10% mass-volume concentration,
The volume ratio of the ethanol wherein added and two grades of water is 0.25 ~ 2.3, and the amount for adding excellent pure grade hydrochloric acid is that the acidity for making solution should be protected
Card is not less than volumetric concentration for 1%HCl.
4. assay method according to claim 1, it is characterised in that iron standard liquid is 20ug/mL, 40ug/mL or 50ug/
ML, is provided to prepare by GB/T 602-2002, and the selection of concentration is according to iron content, the absorbance size surveyed and line in prepare liquid
Depending on property scope.
5. assay method according to claim 1, it is characterised in that the preparation of test liquid, clears up without acid adding, is directly
With 20-70mL ethanol sample dissolution and complete sample amounts and be transferred to 100mL volumetric flasks, afterwards plus 1ml~10ml hydrochloric acid, shake up
Afterwards, finally with two grades of water constant volumes, standard liquid is not added with sample except adding iron standard liquid, also plus same amount of ethanol and hydrochloric acid, with two grades of water
Constant volume.
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| CN105510262A (en) * | 2016-01-21 | 2016-04-20 | 青岛谱尼测试有限公司 | Improvement of method for determining content of iron with 1,10-phenanthroline spectrophotometric method |
| CN111579512A (en) * | 2020-05-18 | 2020-08-25 | 常州新东化工发展有限公司 | Method for detecting iron ions in chlorohydrocarbon |
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| CN101195676A (en) * | 2007-12-27 | 2008-06-11 | 东莞理工学院 | Phosphor A containing novolac epoxy and method for producing the same |
| CN102229624A (en) * | 2011-05-15 | 2011-11-02 | 西北化工研究院 | Synthesis and purification process for DOPO |
| CN102608044A (en) * | 2012-02-23 | 2012-07-25 | 安徽皖仪科技股份有限公司 | Sample treatment method for measuring antimony in polyester chip with flame atomic absorption spectrometry |
| CN102617644A (en) * | 2011-01-30 | 2012-08-01 | 南京理工大学 | Synthesizing and refining method of flame retardant intermediate DOPO |
| CN103234927A (en) * | 2013-04-18 | 2013-08-07 | 吉林化工学院 | Atomic absorption spectrometric method of iron content in tilia mandshurica |
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| JPS5923234A (en) * | 1982-07-30 | 1984-02-06 | Hitachi Ltd | Flameless atomizer of atomic absorption analytical device |
| JP2006064475A (en) * | 2004-08-25 | 2006-03-09 | Horiba Ltd | Pretreatment method for determinating hexavalent chromium and hexavalent chromium determinating method |
| CN101195676A (en) * | 2007-12-27 | 2008-06-11 | 东莞理工学院 | Phosphor A containing novolac epoxy and method for producing the same |
| CN102617644A (en) * | 2011-01-30 | 2012-08-01 | 南京理工大学 | Synthesizing and refining method of flame retardant intermediate DOPO |
| CN102229624A (en) * | 2011-05-15 | 2011-11-02 | 西北化工研究院 | Synthesis and purification process for DOPO |
| CN102608044A (en) * | 2012-02-23 | 2012-07-25 | 安徽皖仪科技股份有限公司 | Sample treatment method for measuring antimony in polyester chip with flame atomic absorption spectrometry |
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