CN110243716A - The measuring method of non-polyester species residual quantity in regenerative piece of polyester bottle - Google Patents
The measuring method of non-polyester species residual quantity in regenerative piece of polyester bottle Download PDFInfo
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- CN110243716A CN110243716A CN201910459156.9A CN201910459156A CN110243716A CN 110243716 A CN110243716 A CN 110243716A CN 201910459156 A CN201910459156 A CN 201910459156A CN 110243716 A CN110243716 A CN 110243716A
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
Abstract
The invention belongs to technical field of analytical chemistry, more particularly to the measuring method of polyester species residual quantity non-in regenerative piece of polyester bottle, by claim sample, pretreatment, sample constant weight, filtration washing, secondary constant weight and etc. detected, and the weighing bottle of detection is improved, it is greatly improved the efficiency of detection.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to the survey of non-polyester species residual quantity in regenerative piece of polyester bottle
Determine method.
Background technique
Polyester, the polymer general name as obtained by polyalcohol and polyacid polycondensation, refers mainly to polyethylene terephthalate
(PET), also include traditionally linear thermoplastics' resins such as polybutylene terephthalate (PBT) (PBT) and polyarylate, be one kind
Excellent, the widely used engineering plastics of energy, may be made as polyester fiber and polyester film.
Regenerative piece of polyester bottle is primarily referred to as the Waste PET Packaging Bottle of various forms, by sorting, cleaning, de- mark, it is broken,
Broken PET sheet made of the techniques such as dry.It is domestic since China's Regenerated Polyester Fibres industry occupies about the 85% of global total amount
Raw material is far from satisfying demand, it is therefore necessary to the regenerative piece of polyester bottle of a large amount of import foreign countries.
Regenerative piece of polyester bottle belongs to PET broken material and leftover bits and pieces (customs's coding 3915901000), according to " the Chinese people
Ecological environment portion, republic identifies writing a letter in reply for problem about import recycled polyester (PET) bottle piece solid waste attribute ", import is high-purity
Net recycled polyester (PET) bottle piece has been subjected to sorting, broken and cleaning overseas, and meets " People's Republic of China's textile industry
Standard regeneration polyester (PET) bottle piece (FZ/T 51008-2014) " as defined in A, B, C class properties and index request, after import
The direct processing and utilization of primary material can be substituted, is supervised not as solid waste, that is, is used as general cargo import.
It finds in the application, " People's Republic of China (PRC) textile industry standard regeneration polyester (PET) bottle piece (FZ/T 51008-
2014) " operating procedure statement is fuzzy, operating condition is uncontrollable is even difficult to realize, and causes laboratory technician's subjective factor to experiment
As a result it is affected, especially wherein " non-polyester (PET) substance residual quantity " one, the specific operation process is as follows:
1, about 2000g sample is weighed, is uniformly shakeout in the drying of known quality, clean tray sample；
2, tray sample is put into preparatory air blast and be heated in the drying box of (105 ± 5) DEG C, under conditions of continuous air blast
Dry 1.5h, takes out tray sample from drying box, and weighing is (accurately to 0.001g) at once；
3, tray sample is put into drying box again, is heated.Tray sample is taken out from drying box after every dry 30min, at once
It weighs (being accurate to 0.1g), until the difference of two inferior quality of sample is no more than 1g；
4, (300.00 ± 5.00) g bottles of piece (m are weighed from the tray sample after drying0) be put into volumetric flask, with graduated cylinder amount
It takes 1000mL acetone slowly in injection capacity bottle and covers bottle stopper, hold up volumetric flask later and shaken up that (time is no less than
1min), it is then allowed to stand 15min；Acetone cleaning solution in volumetric flask is poured out, a bottle piece is careful not to and pours out；
5,1000mL or so tap water is added into volumetric flask to clean bottle piece, is steamed again with 500mL or so after cleaning
It is clear that distilled water carries out bottle piece, filters out all bottles of pieces later；
6, it is placed again into preparatory air blast and is heated in the drying box of (105 ± 5) DEG C, it is dry under conditions of continuous air blast
1.5h.Tray sample is taken out from drying box, weighing at once (accurately to 0.001g), then tray sample is put into drying box, heated,
Tray sample is taken out from drying box after every dry 30min, weighing is (accurately to 0.001g), until the difference of two inferior quality of sample at once
Until 1g；
7, sample mass (m after using the smallest mass value of sample as drying1), and record.
But the above method still has a large amount of defects:
(1) in step 1-2, it can not obtain at present while meet " sample weighting amount is 2000g and can be accurately to 0.001g "
Balance；
(2) in the case that step 3 sample does not cool down, it cannot achieve and " tray sample is taken out from drying box, accurately to 0.1g "；
(3) volumetric flask in step 4 is improper as cleaning container, inconvenient for operation；
(4) step 4 " weighing sample (300.00 ± 5.00) g " precision is inadequate, final result judgement is influenced, because of 0.01g
Deviation relative to 300g sample weighting amount be 33.33mg/kg, and standard for C grade limitation requirement only " < 50mg/kg "；
(5) in the case that step 6 sample does not cool down, it cannot achieve and " take out tray sample from drying box, accurately extremely
0.001g"；
(6) step 6 requires " until the difference of two inferior qualities is no more than 1g ", and the requirement of this condition is too wide, seriously affects and most terminates
Fruit judgement because the deviation of 1g relative to 300g sample weighting amount be 3333mg/kg, and standard for C grade limitation requirement for " <
50mg/kg”。
Summary of the invention
In view of the above problems, the present invention provides a kind of easy to operate, easy to accomplish, testing result and accurately regenerates
The measuring method of non-polyester species residual quantity in polyester bottle slice.
To achieve the goals above, the invention adopts the following technical scheme:
The measuring method of non-polyester species residual quantity, includes the following steps: in regenerative piece of polyester bottle
(1) claim sample: weighing sample, sample is poured into vibration processing in sieve, discarding screenings must be sieved sample；
(2) it pre-processes: will include weighing bottle body, the weighing bottle of weigh the cap and filter paper place is dried after acetone cleans
Reason, then the filter paper after drying is put into weighing bottle body and is covered weigh the cap, cooling after taking-up, weighing bottle of weighing records matter
Amount is m0；
(3) sample constant weight: weigh sieving sample spread out in tray sample, by band sieving sample tray sample, weighing bottle body,
Weigh the cap, filter paper are dried, and stir sieving sample, and sieving sample is all transferred in weighing bottle body, continues to do
It is dry, filter paper is then put into weighing bottle body and is covered weigh the cap, cooling after taking-up, weighing bottle of weighing, record quality is m1,
Weigh the cap opening is dried again, closes weigh the cap, cooling after taking-up, weighing bottle of weighing, record quality is m1'；
(4) filtration washing: being poured slowly into acetone into weighing bottle, stands after shaking weighing bottle, changes weigh the cap with holes,
Filter paper is fitted on funnel, then acetone rinse is filtered processing, sample is transferred to tray sample after washing in weighing bottle
In spread out；
(5) secondary constant weight: the tray sample with sample in step (4) is dried with bottle body, weigh the cap, filter paper is weighed
Processing, and sample is stirred, sample is all transferred in weighing bottle body, drying is continued, is then put into filter paper in weighing bottle body simultaneously
Weigh the cap is covered, cooling after taking-up, weighing bottle of weighing, record quality is m2, then weigh the cap is opened and is dried, it closes
Weigh the cap, cooling after taking-up, weighing bottle of weighing, record quality is m2’。
The principle of detection method is identical as rower method, is the non-polyester that sample surfaces are removed by acetone
(PET) substance remains, and obtains residual quantity using the mass change of front and back.Although principle is identical, realize mode exist compared with
Big difference, as the defect that background of invention is displayed, row calibration method is difficult accurately to obtain testing result.The present invention
Pass through the sample weighting amount for reducing sample, it is ensured that claim sample once to complete, avoid in national standard that sample size is excessive, misses repeatedly claiming to expand in sample
Difference.Evade possible attachment on the instruments such as weighing bottle, filter paper by pre-processing, is dissolved in the substance of acetone, further ensures that inspection
Survey the accuracy of result.The present invention can complete whole operation process by aluminum weighing bottle, enormously simplify analysis experiment
Operating procedure saves manpower and material resources, accelerates the detection of sample.
Preferably, the amount of step (1) described sample is 1000g ± 10g, the amount of step (3) the sieving sample is
300g±5g。
Preferably, step (1), (3) described weigh carry out in electronic balance, the scale division value of electronic balance is
0.1g, the aperture of the sieve are 0.833mm.The size of Control Assay is advantageously reduced because powdered polyesters sample is with third
The loss of ketone and water and result is had an impact.
Preferably, step (2), (3), (5) drying process carry out in warmed-up air dry oven, preheat
Temperature is 100-110 DEG C, and the weighing bottle weighing carries out in assay balance, and the scale division value of assay balance is 0.001g.
Further preferably, the weighing bottle is aluminum weighing bottle.Weighing bottle capacity >=1000mL.The present invention is using specific
Aluminum weighing bottle substitutes conventional container, and not only spatial content greatly increases, but also aluminum material is relative to glass material,
The degree of stability of weight is more preferable, and exactly quality stability is good, when just can be reduced the number of forced air drying, and then saving detection
Between.And the bottle cap of aluminum weighing bottle it is special be divided into closed weigh the cap, weigh the cap with holes, and weigh the cap with holes
Aperture be less than bottle piece partial size.
Preferably, the time of step (3), (5) described drying process is 2.0-3.0h, stirs and be divided between sample
0.5h.Step (3), the method for (5) variation and little, but the control for parameter, but need it is more stringent, firstly, dry
Time cannot be less than 2.0h, to reduce influence of the moisture to testing result to the greatest extent.Secondly, the sample of two steps is dry
The time placed in dry device should be consistent as far as possible, to reduce error to greatest extent.
Preferably, step (3), (5) described quality m1With m1', m2With m2' equal calculating difference, Δ m1=| m1-m1' |, Δ
m2=| m2-m2’|。
Further preferably, as Δ m1And/or Δ m2When > 0.01g, repetitive operation, until Δ m1With Δ m2≤0.01g.By
In 0.01g error relative to 300g sample weighting amount be 33.3mg/kg, and provide limitation be 50mg/kg, be more than this difference after
The error of generation is too big.
Preferably, step (4) can also be transferred in vial and be operated, specifically: sample is transferred to glass
In bottle, it is poured slowly into acetone, covers glass cap, stands, filter paper is fitted on funnel, then acetone is washed after shaking vial
Liquid is filtered processing, and then sample is transferred in tray sample spreads out after washing in vial.Sample is subjected to transfer operation,
It will increase the complexity of analysis experiment, but the order of accuarcy of analysis result can be increased, further decrease error.
Further preferably, the washing specifically: tap water is added into weighing bottle/vial, sample is cleaned,
Sample is cleaned with distilled water again after cleaning.
Further preferably, the content of acetone is 950-1050mL, and the shake time is 1-10min, time of repose 14-
16min, washing originally water content used are 950-1050mL, and distillation water content is 450-550mL.
Preferably, the non-polyester species residual quantity is calculated as follows: X=(m1-m2)×106/(m1-m0), wherein X
(mg/kg)-non-polyester species residual quantity；m0(g)-blank weighing bottle+filter paper gross mass；m1(g) sample before-acetone cleans
+ weighing bottle+filter paper gross mass；m2(g) sample+weighing bottle+filter paper gross mass after-acetone cleaning.
Compared with prior art, the present invention has the advantage that
(1) present invention evades possible attachment on the instruments such as weighing bottle, filter paper by pre-processing, and is dissolved in the object of acetone
Matter further ensures that the accuracy of testing result.
(2) for the present invention using aluminum weighing bottle come surrogate's target glass weighing bottle, the stability of quality is higher, saves
Detection time.
(3) detection method of the invention is easy to operate, easy to accomplish, testing result is accurate.
(4) present invention can complete entire detection process by special aluminum weighing bottle, be greatly improved detection
Efficiency.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
Prepare before detection of the invention:
Reagent and material:
Filter paper: quantitative, middling speed；
Acetone: analysis is pure；
Distilled water: meet the requirement of tertiary effluent in GB/T 6682；
Instrument and equipment:
Air dry oven: temperature is able to maintain in (105 ± 5) DEG C；
Electronic balance: scale division value 0.1g；
Assay balance: scale division value 0.001g；
Weighing bottle: aluminum, capacity >=1000mL；
Graduated cylinder: 1000mL；
Sieve: aperture 0.833mm；
Glass funnel；
Tray sample；
Vial: with cover, capacity 2000mL.
Embodiment 1
(1) claim sample: weighing 1000g sample using electronic balance, sample is poured into the sieve that aperture is 0.833mm and is vibrated
Processing, discarding screenings must be sieved sample；
(2) it pre-processes: by capacity >=1000mL, the aluminum weighing including weighing bottle body, weigh the cap, weigh the cap with holes
Bottle and filter paper are dried in the air dry oven for being pre-heated to 105 DEG C after acetone cleans, then the filter paper after drying is put
Enter in weighing bottle body and cover weigh the cap, cooling after taking-up, using assay balance weighing weighing bottle, record quality is m0；
(3) sample constant weight: 300g sieving sample is weighed using electronic balance and is spread out in tray sample, by the sample with sample
Disk, weighing bottle body, weigh the cap, weigh the cap with holes, filter paper are dried in the air dry oven for being pre-heated to 105 DEG C
2.5h stirs sample every 0.5h, and sample is all transferred in weighing bottle body, continues drying, filter paper is then put into weighing bottle
In vivo and weigh the cap is covered, cooling after taking-up, weighing bottle of weighing, record quality is m1, then weigh the cap is opened and is done
It is dry, weigh the cap is closed, cooling after taking-up, weighing bottle of weighing, record quality is m1', repeat second of dry, cooling, weighing
Until Δ m1=| m1-m1'|≤0.01g；
(4) filtration washing: being poured slowly into acetone 1000mL into weighing bottle, stands 15min after shaking weighing bottle 5min, changes
Upper weigh the cap with holes, filter paper is fitted on funnel, then acetone rinse is filtered processing, and sample passes through in weighing bottle
1000mL tap water, 500mL distilled water are transferred in tray sample after successively washing and spread out；
(5) secondary constant weight: the tray sample with sample in step (4) is dried with bottle body, weigh the cap, filter paper is weighed
Processing, and sample is stirred, under conditions of continuous air blast after dry 2.5h, sample is all transferred in weighing bottle body while hot, after
Continuous dry 30min, is then put into weighing bottle body and covers weigh the cap for filter paper, cooling after taking-up, weighing bottle of weighing, record
Quality is m2, then by the dry 30min of weigh the cap opening, weigh the cap is closed, cooling after taking-up, weighing bottle of weighing records matter
Amount is m2', second of dry, cooling, weighing is repeated until Δ m2=| m2-m2'|≤0.01g；
(6) calculate: according to the mass change in detection process, non-polyester species residual quantity is calculated as follows: X=(m1-m2)
×106/(m1-m0), wherein X (mg/kg)-non-polyester species residual quantity；m0(g)-blank weighing bottle+filter paper gross mass；m1
(g) sample+weighing bottle+filter paper gross mass before-acetone cleans；m2(g) sample+weighing bottle+filter paper is total after-acetone cleaning
Quality.
Embodiment 2
Difference with embodiment 1 is only that 2 mesh size of embodiment is 1mm.
Embodiment 3
Difference with embodiment 1 is only that 3 mesh size of embodiment is 0.5mm.
Embodiment 4
Difference with embodiment 1 is only that 4 step of embodiment (3) is divided into 0.4h between stirring sample.
Embodiment 5
Difference with embodiment 1 is only that 5 step of embodiment (3) is divided into 0.6h between stirring sample.
Embodiment 6
Difference with embodiment 1 is only that, Δ m in embodiment 61Greater than 0.01g.
Embodiment 7
Difference with embodiment 1 is only that, Δ m in embodiment 72Greater than 0.01g.
Embodiment 8
Difference with embodiment 1 is only that 8 step of embodiment (4) is used to be transferred in vial and be carried out.
Embodiment 9
Difference with embodiment 1 is only that the sample weighting amount of embodiment 9 is 2000g.
Embodiment 10
Difference with embodiment 1 is only that, is not cooled down after embodiment 10 is dry.
Comparative example 1
Difference with embodiment 1 is only that comparative example 1 is without pretreatment operation.
Comparative example 2
Difference with embodiment 1 is only that comparative example 2 uses such as " Chinese people's republicanism in background technique same sample
State's textile industry standard regeneration polyester (PET) bottle piece (FZ/T51008-2014) " national standard method detected.
Embodiment 1-10 and the testing result of comparative example 1-2 are as shown in table 1:
Table 1: the testing result of embodiment 1-10 and comparative example 1-2
Data in table 1 are for a batch of sample.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious for can making various changes or correct without departing from the spirit and scope of the present invention.
Claims (10)
1. the measuring method of non-polyester species residual quantity in regenerative piece of polyester bottle, which is characterized in that the method includes walking as follows
It is rapid:
(1) claim sample: weighing sample, sample is poured into vibration processing in sieve, discarding screenings must be sieved sample；
(2) it pre-processes: will include weighing bottle body, weigh the cap, the weighing bottle of weigh the cap with holes and filter paper after acetone cleans
It is dried, then the filter paper after drying is put into weighing bottle body and is covered weigh the cap, cooling after taking-up, weighing weighs
Bottle, record quality are m0；
(3) sample constant weight: weighing sieving sample and spread out in tray sample, by the tray sample with sieving sample, weighs bottle body, weighing
Bottle cap, weigh the cap with holes, filter paper are dried, and stir sieving sample, and sieving sample is all transferred to weighing bottle body
It is interior, continue drying, filter paper is then put into weighing bottle body and is covered weigh the cap, cooling after taking-up, weighing bottle of weighing, record
Quality is m1, then weigh the cap is opened and is dried, weigh the cap is closed, cooling after taking-up, weighing bottle of weighing records quality
For m1'；
(4) filtration washing: being poured slowly into acetone into weighing bottle, stands after shaking weighing bottle, changes weigh the cap with holes, will filter
Paper fits on funnel, then acetone rinse is filtered processing, and sample is transferred to tray sample middle berth after washing in weighing bottle
It opens；
(5) place secondary constant weight: is dried in the tray sample with sample in step (4) and weighing bottle body, weigh the cap, filter paper
Reason, and sample is stirred, sample is all transferred in weighing bottle body, drying is continued, then filter paper is put into weighing bottle body and is covered
Upper weigh the cap, cooling after taking-up, weighing bottle of weighing, record quality is m2, then weigh the cap is opened and is dried, close title
Measuring bottle lid, cooling after taking-up, weighing bottle of weighing, record quality are ' m2。
2. the measuring method of non-polyester species residual quantity in regenerative piece of polyester bottle according to claim 1, which is characterized in that
Step (1), (3) described weigh carry out in electronic balance, and the scale division value of electronic balance is 0.1g, and the aperture of the sieve is
0.833mm。
3. the measuring method of non-polyester species residual quantity in regenerative piece of polyester bottle according to claim 1, which is characterized in that
Step (2), (3), (5) described drying process carry out in warmed-up air dry oven, and preheating temperature is 100-110 DEG C,
The weighing bottle weighing carries out in assay balance, and the scale division value of assay balance is 0.001g.
4. the measuring method of non-polyester species residual quantity, feature exist in regenerative piece of polyester bottle according to claim 1 or 3
In the weighing bottle is aluminum weighing bottle.
5. the measuring method of non-polyester species residual quantity in regenerative piece of polyester bottle according to claim 1, which is characterized in that
Step (3), (5) described drying process time be 2.0-3.0h, stir and be divided into 0.5h between sample.
6. the measuring method of non-polyester species residual quantity in regenerative piece of polyester bottle according to claim 1, which is characterized in that
Step (3), (5) described quality m1With m1', m2With m2' equal calculating difference, Δ m1=| m1-m1' |, Δ m2=| m2-m2’|。
7. the measuring method of non-polyester species residual quantity, feature exist in regenerative piece of polyester bottle according to claim 1 or 6
In as Δ m1And/or Δ m2When > 0.01g, repetitive operation, until Δ m1With Δ m2≤0.01g。
8. the measuring method of non-polyester species residual quantity in regenerative piece of polyester bottle according to claim 1, which is characterized in that
Step (4), which can also be transferred in vial, to be operated, specifically: sample is transferred in vial, acetone is poured slowly into,
Glass cap is covered, stands, filter paper is fitted on funnel, then acetone rinse is filtered processing, so after shaking vial
Sample is transferred in tray sample spreads out after washing in vial afterwards.
9. the measuring method of non-polyester species residual quantity, feature exist in regenerative piece of polyester bottle according to claim 1 or 8
In the shake time is 1-10min, time of repose 14-16min.
10. the measuring method of non-polyester species residual quantity, feature exist in regenerative piece of polyester bottle according to claim 1
In the non-polyester species residual quantity is calculated as follows: X=(m1-m2)×106/(m1-m0), wherein X (mg/kg)-non-polyester
Substance residual quantity；m0(g)-blank weighing bottle+filter paper gross mass；m1(g) sample+weighing bottle+filter paper before-acetone cleans
Gross mass；m2(g) sample+weighing bottle+filter paper gross mass after-acetone cleaning.
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| CN112439259A (en) * | 2020-10-23 | 2021-03-05 | 中国航发沈阳黎明航空发动机有限责任公司 | Method for cleaning and drying aero-engine lubricating oil filter by using hydrocarbon solvent detergent |
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