CN107024557B - The measuring method and application of red phosphorus content - Google Patents
The measuring method and application of red phosphorus content Download PDFInfo
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- CN107024557B CN107024557B CN201610069787.6A CN201610069787A CN107024557B CN 107024557 B CN107024557 B CN 107024557B CN 201610069787 A CN201610069787 A CN 201610069787A CN 107024557 B CN107024557 B CN 107024557B
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- 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
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- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- 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
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- 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
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- 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
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- 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
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Abstract
The present invention relates to the technical fields of phosphorus detection, specifically disclose the measuring method and application of a kind of red phosphorus content.The measuring method at least includes the following steps: powder is made in sample；Then sample powder is impregnated and is ultrasonically treated with organic reagent；Then sample powder is impregnated and is ultrasonically treated with diluted acid；It is cleaned and is 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/mass spectrometer；It takes appropriate treated Specimen eliminating at phosphate, carries out red phosphorus quantitative test with inductive coupling plasma emission spectrograph.The measuring method removes organic phosphorus and Phos means using pretreatment, influence of the organic phosphorus and Phos to testing result can greatly be reduced, reduce that red phosphorus is qualitative, detection limit of quantitative test, simultaneously to determine whether that the detection containing red phosphorus provides the detection means of feasibility in plastics-production, molding, sale.
Description
Technical field
The present invention relates to the technical field of phosphorus detection more particularly to the measuring methods and application of a kind of red phosphorus content.
Background technique
Red phosphorus is phosphorus simple substance, with white phosphorus allotrope each other.Since red phosphorus has good flame retardant property, resistance can be used as
Agent is fired, therefore can be used in electronic product or plastic products.
It, may since red phosphorus can be oxidized to phosphoric acid under wet heat condition but using red phosphorus as the plastic products of fire retardant
Cause electronic product short-circuit, there are security risks.Therefore, most buyer requirements are forbidden to use red phosphorus as fire retardant.
In order to determine in product with the presence or absence of red phosphorus combustion inhibitor, usually a small amount of sample is directly taken to be divided on PY-GC/MS
Analysis, according to sample map whether the characteristic peak containing red phosphorus, and then determine whether to joined red phosphorus in the product.But this place
Reason method, often due to having the P elements of micro other forms in sample and analysis chart being caused to compose now more Interference Peaks, finally
Cause to qualitatively judge whether sample contains red phosphorus and red phosphorus content inaccuracy, while qualitative detection limit is greater than 1000mg/kg.
For this purpose, we have proposed a kind of detection methods of new red phosphorus content.
Summary of the invention
It is an object of the invention in existing flame retardant plastic products, red phosphorus combustion inhibitor content detection is not accurate, and examines
The problems such as rising limit is very high provides the measuring method and application of red phosphorus content.
To achieve the above object of the invention, the embodiment of the present invention uses the following technical solution:
A kind of measuring method of red phosphorus content, at least includes the following steps:
(1) powder is made in sample；
(2) it impregnated using organic reagent, be ultrasonically treated the sample at least once, the time per treatment is not less than 1h；
(3) it impregnated using diluted acid, be ultrasonically treated the sample through (2) processing at least once, the time per treatment is not low
In 1h；
(4) residue through (3) processing is cleaned with tertiary effluent, and spontaneously dried；
(5) sample obtained in trace (4) is taken to carry out red phosphorus qualitative test in pyrolysis-high resolution gas chromatography/mass spectrometer；
(6) appropriate (4) middle Specimen eliminating obtained at phosphate, is carried out with inductive coupling plasma emission spectrograph
Red phosphorus quantitative test.
And correspondingly, the measuring method of the red phosphorus content of above-mentioned offer red phosphorus in plastics-production/molding, sale contains
Measure the application of detection.
The measuring method for the red phosphorus content that the above embodiment of the present invention provides first removes sample using pretreated method
In interfering substance that may be present, purified the red phosphorus in sample, reduced on GC-MS map impurity peaks to red phosphorus characteristic peak
Interference contains convenient for carrying out qualitative analysis to red phosphorus and reducing the detection limit of red phosphorus content for the red phosphorus in accurate testing product
Amount provides reliable method.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is the measuring method operation chart of red phosphorus content of the embodiment of the present invention；
Fig. 2 is that the ABS for being 500mg/kg to red phosphorus theoretical content in the measuring method of red phosphorus content of the embodiment of the present invention is moulded
Expect that sample carries out pretreated GC-MS map；
Fig. 3 is that the ABS for being 500mg/kg to red phosphorus theoretical content in the measuring method of red phosphorus content of the embodiment of the present invention is moulded
Material sample does not carry out pretreated GC-MS map；
Fig. 4 is that the ABS for being 1000mg/kg to red phosphorus theoretical content in the measuring method of red phosphorus content of the embodiment of the present invention is moulded
Expect that sample carries out pretreated GC-MS map；
Fig. 5 is that the ABS for being 1000mg/kg to red phosphorus theoretical content in the measuring method of red phosphorus content of the embodiment of the present invention is moulded
Material sample does not carry out pretreated GC-MS map.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention 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 measuring method of red phosphorus content, at least includes the following steps:
(1) powder is made in sample；
(2) it impregnated using organic reagent, be ultrasonically treated the sample at least once, the time per treatment is not less than 1h；
(3) it impregnated using diluted acid, be ultrasonically treated the sample through (2) processing at least once, the time per treatment is not low
In 1h；
(4) residue through (3) processing is cleaned with tertiary effluent, and spontaneously dried；
(5) sample obtained in trace (4) is taken to carry out red phosphorus qualitative test in pyrolysis-high resolution gas chromatography/mass spectrometer；
(6) it (4) middle Specimen eliminating obtained will be carried out in right amount with sense coupled plasma optical emission spectrometer red at Phos
Phosphorus quantitative test.
Wherein, it in any one embodiment, needs to handle plastic sample, sample is cut into graininess, then
By freezing and grinding, sample comminution is set to become powder, in favor of subsequent organic phosphorus, Phos removal.
In above-mentioned steps (2), when being impregnated 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.
1 organic reagent component of table
| 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 | / |
| Methylene chloride/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 a preferred technical solution, when the proportion of organic reagent reaches shown in table 2, in conjunction with other steps, Ke Yida
The purpose organic phosphorus to most effective removal.
The preferred ingredient of 2 organic reagent of table
Further, for different plastics, organic solvent is according to formula rate as shown in table 3, under the proportion,
Organic solvent is more preferable to organic phosphorus removal effect.
Organic reagent component and preferred ingredient used by the different plastics of table 3
It is organic phosphorus in order to preferably remove, organic reagent impregnate, ultrasonic treatment 3 times, while the time per treatment be 2~
3 hours.
In the sample by organic reagent processing, filtering, then naturally dry, then carry out at the immersion and ultrasound of diluted acid
Reason.
When being impregnated, being ultrasonically treated using diluted acid, diluted acid is dilute hydrochloric acid, dilute sulfuric acid or dust technology.Here diluted acid
Concentration is respective acid concentration common in the lab.It is anti-preferably with enough diluted acids in order to reach better removal effect
It is multiple to impregnate, be ultrasonically treated 3 times, it is every time 2~3 hours, and be both needed to filter after impregnating every time.
Preferably, it impregnates, before ultrasonic treatment in organic reagent and diluted acid, is wrapped up sample powder with filter paper.
It is wrapped up through filter paper, the filter after impregnating 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.Steps are as follows for specific resolution:
(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, and sample is made to be carbonized, until there is a large amount of white cigarettes to generate, removes beaker, cooling
10~20 minutes；
(b) restore to beaker 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, 5~10 minutes cooling；
(c) appropriate (such as 5~10mL) hydrogen peroxide is added dropwise into beaker prevents vigorous reaction from drawing using surface plate
The sample spluttering risen, is placed in electric hot plate, continues heating resolution；
(d) whether observation sample has residue, if repeated (b) and (c) job step, until sample is resolved completely.
After the completion of Specimen eliminating, beaker is stood to room temperature is restored to, with the digestion solution in filter paper filtering beaker, is spent
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: ICP-OES) carries out total phosphorus content analysis on liquid.
The measuring method for the red phosphorus content that the above embodiment of the present invention provides, it is red suitable for various plastics-production/moldings
The detection of phosphorus content.Organic phosphorus and Phos means are removed using pretreatment, can greatly reduce organic phosphorus and nothing
Influence of the machine phosphorus to testing result, while reducing that red phosphorus is qualitative, detection limit of quantitative test；In embodiments of the present invention, when
When sample volume is 5mg, the detection limit (MDL) of PY-GC/MS is 500mg/kg；The detection limit (MDL) of ICP-OES is 20mg/kg.
This is using red phosphorus as fire retardant or production/molding and sale etc. of the plastics using red phosphorus as fire retardant to be forbidden to provide
Reliable detection means.
The measuring method for the red phosphorus content that embodiment provides in order to better illustrate the present invention, below by acrylonitrile-
The test of red phosphorus content is illustrated as embodiment in styrene-butadiene copolymer (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 so that ABS is become powdered by freezing, grinding；
(2) it takes a small amount of powdered ABS to be placed in filter paper, and wraps up；
(3) be toluene according to volume ratio: the ratio of dimethylbenzene=70:30 (v/v) weighs toluene and dimethylbenzene be made into it is organic
Then solvent impregnates filter paper packet with the organic solvent, while being ultrasonically treated 3h, impregnate terminates every time, the toluene and diformazan renewed
The organic solvent of benzene impregnates repeatedly, ultrasound three times, then take out filter paper packet naturally dry；
(4) filter paper packet is impregnated with the hydrochloric acid 20mL that molar concentration is 0.07mol/L, while is ultrasonically treated 3h, impregnated every time
Terminate, the hydrochloric acid of the same concentration renewed repeats immersion, ultrasound three times, then takes out filter paper packet, cleans filter paper packet with tertiary effluent
In remaining powder, cleaning three times, naturally dry；
(5) qualitative test of pyrolysis-high resolution gas chromatography/mass spectrometer (PY-GC/MS) progress red phosphorus on trace samplings is taken,
Test result is in detail as shown in Figure 2；
(6) it takes suitable powder in (4) to be placed in a beaker, the concentrated sulfuric acid of 10mL is added dropwise, is heated at high temperature using electric hot plate, makes
Sample is talked, until there is a large amount of white cigarettes to generate, removes beaker, 10 minutes cooling；
(7) restore to beaker 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, 5 minutes cooling；
(8) 5mL hydrogen peroxide is added dropwise into beaker, using surface plate, prevents sample spluttering caused by vigorous reaction,
It is placed in electric hot plate, continues heating resolution；
(9) after the completion of Specimen eliminating, beaker is stood to room temperature is restored to, filters the digestion solution in beaker with filter paper,
It is settled to 100mL with deionized water, the step that sample blank need to be consistent with test sample process carries out operation, then will be after constant volume
Solution on inductive coupling plasma emission spectrograph (English abbreviation: ICP-OES) carry out red phosphorus quantitative determination, test knot
First group of data of fruit embodiment 1 during see Table 4 for details；
A small amount of sample is taken again, carries out retest according to 1 step of embodiment (6)~(9), test result is shown in Table in 4 real
Apply second group of data of example 1.
Comparative example 1
Plastic sample is same as Example 1, this processing is only by (1) in embodiment 1, by process in plastics at powder,
Then the test of 1 step of embodiment (5)~(9) is directly carried out, wherein the test result of step (5) is in detail as shown in Figure 3；Step
(9) first group of data of test result comparative example 1 during see Table 4 for details；
A small amount of sample is taken, carries out retest 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 so that ABS is become powdered by freezing, grinding；
(2) it takes a small amount of powdered ABS to be placed in filter paper, and wraps up；
(3) be toluene according to volume ratio: the ratio of dimethylbenzene=70:30 (v/v) weighs toluene and dimethylbenzene be made into it is organic
Then solvent impregnates filter paper packet with the organic solvent, while being ultrasonically treated 3h, impregnate terminates every time, the toluene and diformazan renewed
The organic solvent of benzene impregnates repeatedly, ultrasound three times, then take out filter paper packet naturally dry；
(4) filter paper packet is impregnated with the hydrochloric acid 20mL that molar concentration is 0.07mol/L, while is ultrasonically treated 3h, impregnated every time
Terminate, the hydrochloric acid of the same concentration renewed repeats immersion, ultrasound three times, then takes out filter paper packet, cleans filter paper packet with tertiary effluent
In remaining powder, cleaning three times, naturally dry；
(5) qualitative test of pyrolysis-high resolution gas chromatography/mass spectrometer (PY-GC/MS) progress red phosphorus on trace samplings is taken,
Test result is in detail as shown in Figure 4；
(6) it takes suitable powder in (4) to be placed in a beaker, the concentrated sulfuric acid of 10mL is added dropwise, is heated at high temperature using electric hot plate, makes
Sample is talked, until there is a large amount of white cigarettes to generate, removes beaker, 10 minutes cooling；
(7) restore to beaker 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, 5 minutes cooling；
(8) 5mL hydrogen peroxide is added dropwise into beaker, using surface plate, prevents sample spluttering caused by vigorous reaction,
It is placed in electric hot plate, continues heating resolution；
(9) after the completion of Specimen eliminating, beaker is stood to room temperature is restored to, filters the digestion solution in beaker with filter paper,
It is settled to 100mL with deionized water, the step that sample blank need to be consistent with test sample process carries out operation, then will be after constant volume
Solution on inductive coupling plasma emission spectrograph (English abbreviation: ICP-OES) carry out red phosphorus quantitative determination, obtain reality
First group of data of example 2 are applied, see Table 4 for details；
A small amount of sample is taken again, is carried out retest according to 2 step of embodiment (6)~(9), is obtained the second of embodiment 2
Group data, see Table 4 for details.
Comparative example 2
Plastic sample is same as Example 2, this processing is only by (1) in embodiment 2, by process in plastics at powder,
Then the test of 2 step of embodiment (5)~(9) is directly carried out, wherein the test result of step (5) is in detail as shown in Figure 5；
First group of data of comparative example 2 in step (9), see Table 4 for details；
A small amount of sample is taken, retest is carried out according to 2 step of embodiment (6)~(9), obtains second group of number of comparative example 2
According to see Table 4 for details.
ICP data accuracy compares in 4 Examples 1 to 2 of table and comparative example 1~2
From Fig. 2 of embodiment 1, comparative example 1 Fig. 3 it is found that (1) to the sample that red phosphorus theoretical content value is 500mg/kg into
The GC-MS map obtained after row pretreatment, is substantially not visible baseline noise；Map is clean, free from admixture/Interference Peaks, the peak feature P4
Response it is higher, peak height be 3.0 × 106Left and right；
(2) the GC-MS map of pretreatment acquisition is not carried out to sample, baseline noise is high, the base being embodied near characteristic peak
Line is up to 1.5 × 106Left and right, and as temperature program constantly increases；Impurity/Interference Peaks are more, and the response at the peak feature P4 is low, peak
A height of 3.0 × 106Left and right.
From Fig. 4 of embodiment 2, comparative example 2 Fig. 5 it is found that the sample that (1) is 1000mg/kg to red phosphorus theoretical content value
The GC-MS map obtained after being pre-processed, is substantially not visible baseline noise；Map 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) the GC-MS map of pretreatment acquisition is not carried out to sample, baseline noise is high, the base being embodied near characteristic peak
Line is up to 1.5 × 106Left and right, and as temperature program constantly increases；Impurity/Interference Peaks are more, and the response at the peak feature P4 is low, peak
A height of 4.5 × 106Left and right.
As known from Table 4, due to ICP test be total phosphorus content, do not make pretreated sample, do not remove sample
The impurity such as organic phosphorus and Phos, cause the P elements of form of ownership to be all calculated as the content of red phosphorus, cause result bright in product
Show bigger than normal, and true value deviation is more than 50%, and has relatively large deviation between parallel sample；
Made pretreated sample, effectively removed organic phosphorus and inorganic phosphorus impurities in sample, the result of detection with
Theoretical value is not much different, and for deviation less than 10%, deviation is small between true value, and closer to true value, between parallel group, difference is not
Greatly.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of measuring method of red phosphorus content, at least includes the following steps:
(1) powder is made in sample；
(2) it impregnated using organic reagent, be ultrasonically treated the sample at least once, the time per treatment is not less than 1h；
(3) it impregnated using diluted acid, be ultrasonically treated the sample through (2) processing at least once, the time per treatment is not less than 1h；
(4) residue through (3) processing is cleaned with tertiary effluent, and spontaneously dried；
(5) sample obtained in trace (4) is taken to carry out red phosphorus qualitative test in pyrolysis-high resolution gas chromatography/mass spectrometer；
(6) appropriate (4) middle Specimen eliminating obtained at phosphate, is subjected to red phosphorus with inductive coupling plasma emission spectrograph
Quantitative test；
The sample is polyethylene, polypropylene, polystyrene, acrylonitrile-Polystyrene-Butadiene Copolymer, polyvinyl chloride, double
Any one of phenol A type polycarbonate, polyethylene terephthalate, polyvinyl acetate, polyamide, polyurethanes
Plastics；
Wherein, the organic reagent for polyethylene dissolving, any plastics of acrylonitrile-butadiene-styrene copolymer is toluene
The mixed solvent formed with dimethylbenzene according to volume ratio for 90~50:10~50；It is two for dissolving polyacrylic organic reagent
Toluene；Organic reagent for dissolved polystyrene, polyethylene terephthalate is toluene and chloroform according to volume
Than the mixed solvent formed for 90~40:10~60；Organic reagent for dissolving polyvinyl chloride is tetrahydrofuran；For dissolving
The organic reagent of bisphenol A polycarbonate is the mixed solvent that methylene chloride and chloroform are 90~60:10~40 according to volume ratio；
Organic reagent for solvent polyamide is the mixed solvent that formic acid and acetic acid are 90~40:10~60 according to volume ratio；For
It according to volume ratio is what 90~50:10~50 was formed that the organic reagent of dissolution polyurethanes, which is formic acid and dimethylformamide,
Mixed solvent；
The diluted acid is any one of dilute sulfuric acid, dilute hydrochloric acid, dust technology.
2. measuring method as described in claim 1, it is characterised in that: it is described every time to impregnate, filtered after ultrasonic treatment, take filter
Slag；Or it is impregnated again with organic reagent immersion, ultrasonic treatment and diluted acid after first wrapping up the sample powder with filter paper super
Sonication.
3. measuring method as described in claim 1, it is characterised in that: further include drying between the step (2) and step (3)
Processing.
4. measuring method as described in claim 1, it is characterised in that: the process that powder is made in the sample includes by sample
Grain is freezed and is ground.
5. measuring method as described in claim 1, it is characterised in that: the digestion procedure in the step (6) disappears for electric hot plate
Solution.
6. the measuring method of red phosphorus content as described in claim 1 red phosphorus content in plastics-production/molding, sale detects
Using.
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| 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 |
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