CN107024557A - The assay method of red phosphorus content and application - Google Patents
The assay method of red phosphorus content and application Download PDFInfo
- Publication number
- CN107024557A CN107024557A CN201610069787.6A CN201610069787A CN107024557A CN 107024557 A CN107024557 A CN 107024557A CN 201610069787 A CN201610069787 A CN 201610069787A CN 107024557 A CN107024557 A CN 107024557A
- Authority
- CN
- China
- Prior art keywords
- red phosphorus
- sample
- assay method
- immersion
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
Landscapes
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to the technical field of phosphorus detection, assay method and the application of a kind of red phosphorus content are specifically disclosed.The assay method at least comprises the following steps：Powder is made in sample；Then with organic reagent immersion and ultrasonically treated sample powder；Then with diluted acid immersion and ultrasonically treated sample powder；Cleaned and spontaneously dried with tertiary effluent again；The treated sample of trace is taken to carry out red phosphorus qualitative test in pyrolysis-high resolution gas chromatography/GC-MS；Take appropriate treated Specimen eliminating into phosphate, red phosphorus quantitative test is carried out with inductive coupling plasma emission spectrograph.The assay method removes the means of organophosphor and Phos using pretreatment, the influence of organophosphor and Phos to testing result can greatly be reduced, reduce that red phosphorus is qualitative, quantitative test detection limit simultaneously, for plastics-production, shaping, sell in determine whether that the detection containing red phosphorus provides the detection means of feasibility.
Description
Technical field
The present invention relates to assay method and the application of the technical field of phosphorus detection, more particularly to a kind of red phosphorus content.
Background technology
Red phosphorus is phosphorus simple substance, with white phosphorus allotrope each other.Because red phosphorus has good fire resistance, resistance can be used as
Agent is fired, therefore available in electronic product or plastic products.
But, may because red phosphorus can be oxidized to phosphoric acid under wet heat condition using red phosphorus as the plastic products of fire retardant
Cause electronic product short circuit, there is potential safety hazard.Therefore, most buyer requirements prohibit the use of red phosphorus as fire retardant.
In order to determine to whether there is red phosphorus combustion inhibitor in product, usually a small amount of sample is directly taken to be divided on PY-GC/MS
Analysis, according to sample collection of illustrative plates whether the characteristic peak containing red phosphorus, and then determine whether to add red phosphorus in the product.But this place
Reason method, often due to having the P elements of micro other forms in sample and causing analysis chart to compose now more Interference Peaks, finally
Cause to qualitatively judge whether sample contains red phosphorus and red phosphorus content is inaccurate, while qualitative detection limit is more than 1000mg/kg.
Therefore, we have proposed a kind of detection method of new red phosphorus content.
The content of the invention
It is an object of the invention to in existing flame retardant plastic products, red phosphorus combustion inhibitor content detection is not accurate, and inspection
There is provided the assay method of red phosphorus content and application for the problems such as rising limit is very high.
To achieve the above object of the invention, the embodiment of the present invention employs following technical scheme：
A kind of assay method of red phosphorus content, at least comprises the following steps：
(1) powder is made in sample；
(2) using organic reagent immersion, the ultrasonically treated sample at least one times, the time per treatment is not less than 1h；
(3) using diluted acid immersion, the ultrasonically treated sample handled through (2) at least one times, the time per treatment is not low
In 1h；
(4) residue handled through (3) is cleaned with tertiary effluent, and is spontaneously dried；
(5) sample obtained in trace (4) is taken to carry out red phosphorus qualitative test in pyrolysis-high resolution gas chromatography/GC-MS；
(6) appropriate (4) middle Specimen eliminating obtained, into phosphate, is carried out with inductive coupling plasma emission spectrograph
Red phosphorus quantitative test.
And, correspondingly, the assay method of the red phosphorus content of the above-mentioned offer red phosphorus in plastics-production/shaping, sale contains
Measure the application of detection.
The assay method for the red phosphorus content that the above embodiment of the present invention is provided, using the method for pretreatment, first removes sample
In interfering material that may be present, purified the red phosphorus in sample, reduced on GC-MS collection of illustrative plates impurity peaks to red phosphorus characteristic peak
Interference, is easy to carry out red phosphorus qualitative analysis and reduces the detection limit of red phosphorus content, is that the red phosphorus in accurate detection product contains
Amount provides reliable method.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, below by using required in embodiment
Accompanying drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for ability
For the those of ordinary skill of domain, on the premise of not paying creative work, it can also be obtained according to these accompanying drawings other attached
Figure.
Fig. 1 is the assay method operation chart of red phosphorus content of the embodiment of the present invention；
Fig. 2 be red phosphorus content of the embodiment of the present invention assay method in red phosphorus theoretical content be 500mg/kg ABS mould
The GC-MS collection of illustrative plates that material sample is pre-processed；
Fig. 3 be red phosphorus content of the embodiment of the present invention assay method in red phosphorus theoretical content be 500mg/kg ABS mould
The GC-MS collection of illustrative plates that material sample is not pre-processed；
Fig. 4 be red phosphorus content of the embodiment of the present invention assay method in red phosphorus theoretical content be 1000mg/kg ABS mould
The GC-MS collection of illustrative plates that material sample is pre-processed；
Fig. 5 be red phosphorus content of the embodiment of the present invention assay method in red phosphorus theoretical content be 1000mg/kg ABS mould
The GC-MS collection of illustrative plates that material sample is not pre-processed.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The embodiment of the present invention provides a kind of assay method of red phosphorus content, at least comprises the following steps：
(1) powder is made in sample；
(2) using organic reagent immersion, the ultrasonically treated sample at least one times, the time per treatment is not less than 1h；
(3) using diluted acid immersion, the ultrasonically treated sample handled through (2) at least one times, the time per treatment is not low
In 1h；
(4) residue handled through (3) is cleaned with tertiary effluent, and is spontaneously dried；
(5) sample obtained in trace (4) is taken to carry out red phosphorus qualitative test in pyrolysis-high resolution gas chromatography/GC-MS；
(6) (4) middle Specimen eliminating obtained into Phos, it will be carried out in right amount with sense coupled plasma optical emission spectrometer red
Phosphorus quantitative test.
Wherein, in any one embodiment, it is necessary to handle plastic sample, sample is cut into graininess, then
By freezing and grinding, sample comminution is set to turn into powder, in favor of the removal of follow-up organophosphor, Phos.
In above-mentioned steps (2), when being soaked with organic reagent to the sample powder being wrapped in filter paper, what is be related to has
Machine reagent is as shown in table 1.
The organic reagent component of table 1
| Organic reagent | Volume ratio (v/v) |
| Toluene/dimethylbenzene | (90~50):(10~50) |
| Dimethylbenzene | / |
| Toluene/chloroform | (90~40):(10~60) |
| Toluene/dimethylbenzene | (90~50):(10~50) |
| Tetrahydrofuran | / |
| Dichloromethane/chloroform | (90~60):(10~40) |
| Phenol/carbon tetrachloride | (90~40):(10~60) |
| Toluene/chloroform | (90~40):(10~60) |
| Formic acid/acetic acid | (90~40):(10~60) |
| Formic acid/dimethylformamide | (90~50):(10~50) |
As preferred technical scheme, when the proportioning of organic reagent is reached shown in table 2, with reference to other steps, Ke Yida
To the purpose of maximally effective removal organophosphor.
The preferred ingredient of the organic reagent of table 2
Further, for different plastics, organic solvent is according to formula rate as shown in table 3, under the proportioning,
Organic solvent is more preferable to the removal effect of organophosphor.
Organic reagent component and preferred ingredient that the different plastics of table 3 are used
In order to preferably remove organophosphor, organic reagent immersion, ultrasonically treated 3 times, while the time per treatment be 2~
3 hours.
In the sample handled by organic reagent, then filtering dries naturally, then carry out the immersion of diluted acid with it is ultrasonic at
Reason.
Soaked using diluted acid, it is ultrasonically treated when, diluted acid be watery hydrochloric acid, dilute sulfuric acid or dust technology.Here diluted acid
Concentration is each sour concentration commonly used in the lab.It is anti-preferably with enough diluted acids in order to reach more preferable removal effect
Multiple immersion, ultrasonically treated 3 times, be every time 2~3 hours, and be both needed to filtering after soaking every time.
Preferably, organic reagent and diluted acid immersion, it is ultrasonically treated before, sample powder is wrapped up with filter paper.
Wrapped up through filter paper, the filter after immersion every time can be saved, the time entirely detected can be saved.
In any embodiment, the digestion procedure in step (6) is heating board digestion.Specifically clear up step as follows：
(a) at room temperature, be added dropwise in vent cabinet into the beaker containing pretreated sample it is appropriate (such as 10~
Concentrated sulfuric acid 100mL), is heated at high temperature using electric hot plate, sample is carbonized, until there is a large amount of white cigarettes to produce, removes beaker, is cooled down
10~20 minutes；
(b) treat that beaker recovers to room temperature, appropriate (such as 5~20mL) hydrochloric acid is added dropwise into beaker, using surface plate, prevent
Only sample solution spluttering caused by vigorous reaction, is placed in electric hot plate, heats 10~15 minutes, cools down 5~10 minutes；
(c) appropriate (such as 5~10mL) hydrogen peroxide is added dropwise into beaker, using surface plate, prevents vigorous reaction from drawing
The sample spluttering risen, is placed in electric hot plate, continues heating and clears up；
(d) whether observation sample has residue, if repeated (b) and (c) job step, until sample is resolved completely.
Treat after the completion of Specimen eliminating, beaker is stood to room temperature is returned to, the digestion solution in beaker is filtered with filter paper, spends
Ionized water is settled to 100mL, and the step that sample blank need to be consistent with test sample process carries out operation, then will be molten after constant volume
Inductive coupling plasma emission spectrograph (English abbreviation on liquid：ICP-OES total phosphorus content analysis) is carried out.
The assay method for the red phosphorus content that the above embodiment of the present invention is provided, it is adaptable to red in various plastics-production/shapings
The detection of phosphorus content.The means of organophosphor and Phos are removed using pretreatment, organophosphor and nothing can be greatly reduced
Influence of the machine phosphorus to testing result, while reducing, red phosphorus is qualitative, quantitative test detection limit；In embodiments of the present invention, when
When sample size is 5mg, PY-GC/MS detection limit (MDL) is 500mg/kg；ICP-OES detection limit (MDL) is 20mg/kg.
This is using red phosphorus as fire retardant or forbids providing in terms of production/shaping using red phosphorus as the plastics of fire retardant and sale
Reliable detection means.
In order to better illustrate the assay method of red phosphorus content provided in an embodiment of the present invention, below by acrylonitrile-
The test of red phosphorus content is illustrated as embodiment in SB (ABS) plastics.
Embodiment 1
Plastics：ABS；
Red phosphorus theoretical content in the ABS plastic：500mg/kg.
(1) ABS plastic is cut into small graininess, then ABS is turned into powdered by freezing, grinding；
(2) take a small amount of powdered ABS to be placed in filter paper, and wrap up；
(3) it is toluene according to volume ratio：Dimethylbenzene=70:30 (v/v) ratio weighs toluene and dimethylbenzene be made into it is organic
Solvent, then soaks filter paper bag with the organic solvent, while ultrasonically treated 3h, every time immersion terminates, the toluene and diformazan renewed
The organic solvent of benzene soaks repeatedly, ultrasound three times, then takes out filter paper bag and dries naturally；
(4) the hydrochloric acid 20mL for being 0.07mol/L with molar concentration soaks filter paper bag, while ultrasonically treated 3h, every time immersion
Terminate, the hydrochloric acid of the same concentration renewed repeats immersion, ultrasound three times, then takes out filter paper bag, filter paper bag is cleaned with tertiary effluent
The powder of middle residual, cleans three times, dries naturally；
(5) qualitative test of pyrolysis-high resolution gas chromatography/GC-MS (PY-GC/MS) progress red phosphorus on trace samplings is taken,
Test result is detailed as shown in Figure 2；
(6) take powder appropriate in (4) to be placed in beaker, the 10mL concentrated sulfuric acid is added dropwise, is heated at high temperature using electric hot plate, made
Sample is talked, until there is a large amount of white cigarettes to produce, is removed beaker, is cooled down 10 minutes；
(7) treat that beaker recovers to room temperature, appropriate 5mL hydrochloric acid is added dropwise into beaker, using surface plate, prevent acutely anti-
Sample solution spluttering caused by answering, is placed in electric hot plate, heats 10 minutes, cools down 5 minutes；
(8) 5mL hydrogen peroxide is added dropwise into beaker, using surface plate, sample spluttering caused by vigorous reaction is prevented,
Electric hot plate is placed in, continues heating and clears up；
(9) treat after the completion of Specimen eliminating, beaker stood to room temperature is returned to, the digestion solution in beaker is filtered with filter paper,
100mL is settled to deionized water, the step that sample blank need to be consistent with test sample process carries out operation, then by after constant volume
Solution on inductive coupling plasma emission spectrograph (English abbreviation：ICP-OES the quantitative determination of red phosphorus, test knot) are carried out
Fruit refers to first group of data of embodiment 1 in table 4；
A small amount of sample is taken again, retest is carried out according to the step of embodiment 1 (6)~(9), and test result is real in being shown in Table 4
Apply second group of data of example 1.
Comparative example 1
Plastic sample is same as Example 1, and this processing is only by (1) in embodiment 1, by process in plastics into powder,
Then the test of the step of embodiment 1 (5)~(9) is directly carried out, wherein, the test result of step (5) is detailed as shown in Figure 3；Step
(9) test result refers to first group of data of comparative example 1 in table 4；
A small amount of sample is taken, retest is carried out according to step (6)~(9), test result is shown in Table 4 comparative example, 1 second group of number
According to.
Embodiment 2
Plastics：ABS；
Red phosphorus theoretical content in the ABS plastic：1000mg/kg.
(1) ABS plastic is cut into small graininess, then ABS is turned into powdered by freezing, grinding；
(2) take a small amount of powdered ABS to be placed in filter paper, and wrap up；
(3) it is toluene according to volume ratio：Dimethylbenzene=70:30 (v/v) ratio weighs toluene and dimethylbenzene be made into it is organic
Solvent, then soaks filter paper bag with the organic solvent, while ultrasonically treated 3h, every time immersion terminates, the toluene and diformazan renewed
The organic solvent of benzene soaks repeatedly, ultrasound three times, then takes out filter paper bag and dries naturally；
(4) the hydrochloric acid 20mL for being 0.07mol/L with molar concentration soaks filter paper bag, while ultrasonically treated 3h, every time immersion
Terminate, the hydrochloric acid of the same concentration renewed repeats immersion, ultrasound three times, then takes out filter paper bag, filter paper bag is cleaned with tertiary effluent
The powder of middle residual, cleans three times, dries naturally；
(5) qualitative test of pyrolysis-high resolution gas chromatography/GC-MS (PY-GC/MS) progress red phosphorus on trace samplings is taken,
Test result is detailed as shown in Figure 4；
(6) take powder appropriate in (4) to be placed in beaker, the 10mL concentrated sulfuric acid is added dropwise, is heated at high temperature using electric hot plate, made
Sample is talked, until there is a large amount of white cigarettes to produce, is removed beaker, is cooled down 10 minutes；
(7) treat that beaker recovers to room temperature, appropriate 5mL hydrochloric acid is added dropwise into beaker, using surface plate, prevent acutely anti-
Sample solution spluttering caused by answering, is placed in electric hot plate, heats 10 minutes, cools down 5 minutes；
(8) 5mL hydrogen peroxide is added dropwise into beaker, using surface plate, sample spluttering caused by vigorous reaction is prevented,
Electric hot plate is placed in, continues heating and clears up；
(9) treat after the completion of Specimen eliminating, beaker stood to room temperature is returned to, the digestion solution in beaker is filtered with filter paper,
100mL is settled to deionized water, the step that sample blank need to be consistent with test sample process carries out operation, then by after constant volume
Solution on inductive coupling plasma emission spectrograph (English abbreviation：ICP-OES the quantitative determination of red phosphorus) is carried out, reality is obtained
First group of data of example 2 are applied, table 4 is referred to；
A small amount of sample is taken again, is carried out retest according to the step of embodiment 2 (6)~(9), is obtained the second of embodiment 2
Group data, refer to table 4.
Comparative example 2
Plastic sample is same as Example 2, and this processing is only by (1) in embodiment 2, by process in plastics into powder,
Then the test of the step of embodiment 2 (5)~(9) is directly carried out, wherein, the test result of step (5) is detailed as shown in Figure 5；
First group of data of comparative example 2, refer to table 4 in step (9)；
A small amount of sample is taken, retest is carried out according to the step of embodiment 2 (6)~(9), second group of number of comparative example 2 is obtained
According to referring to table 4.
ICP data accuracies are compared in the embodiment 1~2 of table 4 and comparative example 1~2
It was found from Fig. 2, Fig. 3 of comparative example 1 from embodiment 1, (1) is entered to red phosphorus theoretical content value for 500mg/kg sample
The GC-MS collection of illustrative plates obtained after row pretreatment, is substantially not visible baseline noise；Collection of illustrative plates is clean, free from admixture/Interference Peaks, feature P4 peaks
Response it is higher, peak height be 3.0 × 106Left and right；
(2) to sample pre-process the GC-MS collection of illustrative plates of acquisition, baseline noise is high, is embodied in the base near characteristic peak
Line is up to 1.5 × 106Left and right, and as heating schedule is constantly raised；Impurity/Interference Peaks are more, and the response at feature P4 peaks is low, peak
A height of 3.0 × 106Left and right.
It was found from Fig. 4, Fig. 5 of comparative example 2 from embodiment 2, (1) is to sample of the red phosphorus theoretical content value for 1000mg/kg
The GC-MS collection of illustrative plates obtained after being pre-processed, is substantially not visible baseline noise；Collection of illustrative plates is clean, free from admixture/Interference Peaks, feature P4
The response at peak is higher, and peak height is 6.0 × 106Left and right；
(2) to sample pre-process the GC-MS collection of illustrative plates of acquisition, baseline noise is high, is embodied in the base near characteristic peak
Line is up to 1.5 × 106Left and right, and as heating schedule is constantly raised；Impurity/Interference Peaks are more, and the response at feature P4 peaks is low, peak
A height of 4.5 × 106Left and right.
As known from Table 4, due to ICP test obtain be total phosphorus content, do not make the sample pre-processed, do not remove sample
The impurity such as organophosphor and Phos in product, causes the P elements of form of ownership to be all calculated as the content of red phosphorus, causes result bright
It is aobvious bigger than normal, and actual value deviation is more than there is relatively large deviation between 50%, and parallel sample；
Made the sample of pretreatment, effectively eliminated organophosphor and inorganic phosphorus impurities in sample, the result of detection with
Theoretical value is more or less the same, and deviation is less than 10% between actual value, and deviation is small, closer to actual value, and difference is not between parallel group
Greatly.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modification, equivalent substitution or improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (8)
1. a kind of assay method of red phosphorus content, at least comprises the following steps：
(1) powder is made in sample；
(2) using organic reagent immersion, the ultrasonically treated sample at least one times, the time per treatment is not less than 1h；
(3) using diluted acid immersion, the ultrasonically treated sample handled through (2) at least one times, the time per treatment is not less than 1h；
(4) residue handled through (3) is cleaned with tertiary effluent, and is spontaneously dried；
(5) sample obtained in trace (4) is taken to carry out red phosphorus qualitative test in pyrolysis-high resolution gas chromatography/GC-MS；
(6) appropriate (4) middle Specimen eliminating obtained, into phosphate, red phosphorus is subjected to inductive coupling plasma emission spectrograph
Quantitative test.
2. assay method as claimed in claim 1, the organic reagent is as follows：
3. assay method as claimed in claim 1, it is characterised in that：The immersion, ultrasonically treated rear filtering, take filter every time
Slag；Or soak super with organic reagent immersion, ultrasonically treated and diluted acid again after first the sample powder is wrapped up with filter paper
Sonication.
4. assay method as claimed in claim 1, it is characterised in that：The diluted acid is in dilute sulfuric acid, watery hydrochloric acid, dust technology
It is any.
5. assay method as claimed in claim 1, it is characterised in that：Also include drying between the step (2) and step (3)
Processing.
6. assay method as claimed in claim 1, it is characterised in that：The process that powder is made in the sample is included sample
Grain is freezed and ground.
7. assay method as claimed in claim 1, it is characterised in that：Digestion procedure in the step (6) disappears for electric hot plate
Solution.
8. the assay method of red phosphorus content as claimed in claim 1 red phosphorus content in plastics-production/shaping, sale is detected
Using.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610069787.6A CN107024557B (en) | 2016-01-29 | 2016-01-29 | The measuring method and application of red phosphorus content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610069787.6A CN107024557B (en) | 2016-01-29 | 2016-01-29 | The measuring method and application of red phosphorus content |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107024557A true CN107024557A (en) | 2017-08-08 |
| CN107024557B CN107024557B (en) | 2019-11-05 |
Family
ID=59524264
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610069787.6A Active CN107024557B (en) | 2016-01-29 | 2016-01-29 | The measuring method and application of red phosphorus content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107024557B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110034281A (en) * | 2018-04-12 | 2019-07-19 | 南方科技大学 | Phosphorus/carbon composite and preparation method thereof and lithium ion battery, sodium-ion battery |
| CN110806474A (en) * | 2019-11-28 | 2020-02-18 | 广州广电计量检测股份有限公司 | Qualitative and quantitative detection method for red phosphorus in plastic product |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101669029A (en) * | 2007-04-26 | 2010-03-10 | 住友电气工业株式会社 | Method of analyzing inorganic phosphorus in organic material and apparatus therefor |
| CN102119327A (en) * | 2009-06-03 | 2011-07-06 | 住友电气工业株式会社 | Method for producing standard sample for use in quantitative determination of red phosphorus in resin |
| CN102449469A (en) * | 2009-06-03 | 2012-05-09 | 住友电气工业株式会社 | Method for quantifying red phosphorus in resin |
| CN104807806A (en) * | 2015-04-30 | 2015-07-29 | 武汉钢铁(集团)公司 | Method for measuring content of phosphorus in sintered flux |
| CN105259159A (en) * | 2015-10-20 | 2016-01-20 | 武汉钢铁(集团)公司 | Analysis method for measuring content of phosphorus in ferro-molybdenum |
-
2016
- 2016-01-29 CN CN201610069787.6A patent/CN107024557B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101669029A (en) * | 2007-04-26 | 2010-03-10 | 住友电气工业株式会社 | Method of analyzing inorganic phosphorus in organic material and apparatus therefor |
| CN102119327A (en) * | 2009-06-03 | 2011-07-06 | 住友电气工业株式会社 | Method for producing standard sample for use in quantitative determination of red phosphorus in resin |
| CN102449469A (en) * | 2009-06-03 | 2012-05-09 | 住友电气工业株式会社 | Method for quantifying red phosphorus in resin |
| CN104807806A (en) * | 2015-04-30 | 2015-07-29 | 武汉钢铁(集团)公司 | Method for measuring content of phosphorus in sintered flux |
| CN105259159A (en) * | 2015-10-20 | 2016-01-20 | 武汉钢铁(集团)公司 | Analysis method for measuring content of phosphorus in ferro-molybdenum |
Non-Patent Citations (3)
| Title |
|---|
| 徐逸群等: "ICP-OES测定磷系阻燃纤维中磷含量的方法", 《上海纺织科技》 * |
| 沈小东等: "钱塘江富阳一杭州段沉积物磷的赋存形态分析", 《环境污染与防治》 * |
| 王杰明等: "ICP-OES测定生物油脂中的磷含量", 《石油炼制与化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110034281A (en) * | 2018-04-12 | 2019-07-19 | 南方科技大学 | Phosphorus/carbon composite and preparation method thereof and lithium ion battery, sodium-ion battery |
| CN110806474A (en) * | 2019-11-28 | 2020-02-18 | 广州广电计量检测股份有限公司 | Qualitative and quantitative detection method for red phosphorus in plastic product |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107024557B (en) | 2019-11-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Han et al. | Visual detection of melamine in infant formula at 0.1 ppm level based on silver nanoparticles | |
| Yip et al. | Kinetic interactions of EDDS with soils. 1. Metal resorption and competition under EDDS deficiency | |
| CN107024557A (en) | The assay method of red phosphorus content and application | |
| Moawed et al. | Synthesis and characterization of iodo polyurethane foam and its application in removing of aniline blue and crystal violet from laundry wastewater | |
| CN107000050A (en) | Silver powder and preparation method thereof and conductive hydrophilic slurry | |
| CN105296598B (en) | Based on the lead ion fluorescence detection method of 8-17DNAzyme principle and its application | |
| Wang et al. | Green chemical method for the synthesis of chromogenic fiber and its application for the detection and extraction of Hg2+ and Cu2+ in environmental medium | |
| CN105259314B (en) | Lead ion visual detection method and detection kit | |
| Arghavani‐Beydokhti et al. | Dissolvable layered double hydroxide nanoadsorbent‐based dispersive solid‐phase extraction for highly efficient and eco‐friendly simultaneous microextraction of two toxic metal cations and two anionic azo dyes in real samples | |
| CN108267412B (en) | Rapid and reusable hexavalent chromium ion detection system and method | |
| CN102128739A (en) | Testing method of heavy metal elements in paint coating | |
| CN113740416B (en) | Engine crankshaft inspection method | |
| Bai et al. | Highly selective colorimetric sensing of Cu 2+ using a Schiff base derivative immobilized on polyvinyl alcohol microspheres | |
| Ghaedi et al. | Preconcentration/Separation of Some Metal Ions Using Sodium Dodecyl Sulfate Coated Alumina Modified with Bis (5‐bromo‐2‐hydroxy‐benzaldehyde)‐2‐methyl‐1, 5‐pentane Diimine (BBHBPDI) Prior to Their Flame‐AAS Determination | |
| CN102507540A (en) | Determination method for lead in plastic sample | |
| US20210018436A1 (en) | Multipurpose microfluidics devices for rapid on-site optical chemical analysis | |
| Luongo | Chemicals in textiles | |
| JP7044456B2 (en) | Cooking oil manufacturing system and cooking oil manufacturing method | |
| CN108489963B (en) | Preparation method of SERS substrate for acrylamide specificity recognition and high-sensitivity analysis | |
| CN110567775A (en) | Solid food sample pretreatment method based on ionic liquid | |
| CN108562579A (en) | A kind of qualitative method of quick measurement ornaments Cr VI | |
| CN106249710B (en) | A kind of research and application in Process of Chemical Cleaning and control method | |
| CN109557237B (en) | Method for measuring chloride ion concentration in containment spraying system | |
| US6524859B1 (en) | Process for making a textile product | |
| KR101622124B1 (en) | Preparation Method of Silica Coated Magnetic Nanoparticles Immobilized Enzyme and Detection Method therewith |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |