CN105834177B - A kind of acid washing method of plastic sample bottle - Google Patents
A kind of acid washing method of plastic sample bottle Download PDFInfo
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- CN105834177B CN105834177B CN201610321994.6A CN201610321994A CN105834177B CN 105834177 B CN105834177 B CN 105834177B CN 201610321994 A CN201610321994 A CN 201610321994A CN 105834177 B CN105834177 B CN 105834177B
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- Prior art keywords
- bottle
- sample bottle
- pickling
- pickle
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
- B08B9/0804—Cleaning containers having tubular shape, e.g. casks, barrels, drums
- B08B9/0817—Cleaning containers having tubular shape, e.g. casks, barrels, drums by agitating or tumbling containers filled with liquid or liquid and abrasive, e.g. chain
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of plastic sample bottle acid washing method, 5 ~ 10% salpeter solutions configured with ultra-pure water are filled in 100 grades of superclean benches, it is simultaneously that sample bottle is upright to rotate the bubble that bottle is excluded in bottle wall and pickle, packed with the clean plastic bag sealing of double-deck pickling, stand 30 ~ 60 days at normal temperatures and remain the erectility of sample bottle.Then first pass pickle is poured out in 100 grades of superclean benches, with ultrapure water 3 times, fill 0.1 ~ 0.5% high pure nitric acid solution configured with ultra-pure water, it is simultaneously that sample bottle is upright to rotate the bubble that bottle is excluded in bottle wall and pickle, packed with the clean polybag of double-deck pickling, keep the erectility of sample bottle to stand 2 months at normal temperatures.Sample bottle after second of pickling is continued in original packaging to placement 1 ~ 12 month until before use, carrying out " aging " effect of salpeter solution.Blank check shows that acid washing method disclosed by the invention is effective.
Description
Technical field
The present invention relates to a kind of acid washing method of plastic sample bottle, pouring-in acid washing method is referred specifically to.
Background technology
The concentration of trace element is very low in mountain region and polar region snow ice, from point of the collection of sample, transport, storage to the end
During analysis, all plastic sample bottles directly contacted with sample can pass through the direct contaminated samples of dissolution trace element.Therefore need
Plastic sample bottle is cleaned using suitable acid washing method, to reduce plastic sample bottle bottle to greatest extent to snow ice sample
The pollution of product.Existing plastic sample bottle pickling is that plastic sample bottle is immersed in first to fourth successively in four time-of-weeks
In the salpeter solution of acid wash drum, the concentration of salpeter solution is sequentially reduced and purity gradually increases；Except first pass pickling is in room temperature
Beyond lower progress, rear three times pickling are all to accelerate the process of pickling with heater plate.Existing acid washing method cleans journey
Sequence is complicated, inefficient, expends substantial amounts of manpower, also easily causes security incident, and its main deficiency performance is as follows:
1. acid cleaning process is the soak acid-cleaning carried out successively using 4 acid wash drums 4 weeks, because of the finite capacity of acid wash drum, one
A small amount of sample bottle can only be cleaned by criticizing, and can not meet the needs of Ice core study is to a large amount of pickling clean sample bottles.
2. the complicated, pickling process of pipeline system, which needs special messenger to carry out continual cleaning weekly, just can guarantee that acid dip pickle
Recycle.In addition, transfer and up to ten flushing several times of the sample bottle between 4 acid wash drums need to expend substantial amounts of people
Power, the efficiency of pickling is had a strong impact on.
3. due to the effect of buoyancy, sample segment bottle swims in above pickle in acid wash drum and sample bottle can not be made complete
Complete immersion is in pickle, it is impossible to ensures effective pickling of sample bottle.Further, since the bubble for being attached to bottle wall can not be removed,
Cause sample bottle bottle wall not contacted fully with pickle, also have impact on the effect of pickling.
4. because acid wash drum is the heater plate by bottom, easily sent out when heating plate temperature-controlling system breaks down
Coin into acid wash drum high temperature melting and the security incident of pickle leakage.
The content of the invention
In view of above-mentioned, it is an object of the invention to complete the clear of plastic sample bottle by the acid washing method of direct injection
Wash, pickling process is easier, efficient, it is ensured that pickle is fully contacted with sample bottle inwall and effective pickling, greatly reduces
Work is time-consuming, can meet the needs of trace element research is to a large amount of clean sample bottles and reduce the generation of security incident.
The object of the present invention is achieved like this：
A kind of acid washing method of plastic sample bottle, its step include：
A, first pass pickling：
It is 100 grades of superclean benches in ultra-clean Cleanliness, opens bottle cap, fill the BV-III with secondary sub-boiling distillation
Level nitric acid（Beijing Inst. of Chemical Reagent, using Determination of trace element contents as 10-9G/g magnitudes）With Milli-Q ultra-pure waters（Resistivity
For 18.2 M Ω .cm）5 ~ 10% salpeter solution prepared.Bottle cap is covered, tilts and rotates bottle, is allowed in bottle wall and pickle
Bubble be fused into large volume of bubble and rise to liquid level rupture, it is clean then sample bottle to be uprightly put into double-deck pickling
LDPE: Low-density polyethylene plastics bag carries out packaging seal, at normal temperatures（More than 20 DEG C）30 ~ 60 days are stood, during which in low density polyethylene
The erectility of sample bottle is remained in alkene plastics bag；
B, wash：
In clean room, sample bottle upright in LDPE: Low-density polyethylene plastics bag is taken out, bottle cap is opened, by first pass pickling
Liquid is poured out, and plastic sample bottle is rinsed 3 times with Milli-Q ultra-pure waters, rinses out the first of the attachment of plastic sample bottle surface completely
All over pickle；
C, second time pickling：
Superclean bench in clean room opens bottle cap, fills with the high-purity concentrated nitric acid of Fiher " Optima " level（Trace
Constituent content is 10-12G/g magnitudes）0.1 ~ 0.5% salpeter solution prepared with Milli-Q ultra-pure waters, covers bottle cap, tilts
And rotate bottle, allow the bubble in bottle wall and pickle to be fused into large volume of bubble and rise to liquid level rupture, then
Sample bottle is uprightly put into the clean LDPE: Low-density polyethylene plastics bag of double-deck pickling and carries out packaging seal, at normal temperatures（More than 20 DEG C）
2 months are stood, during which remains the erectility of sample bottle；
D, " aging " of salpeter solution：
Sample bottle after second time pickling is continued into placement 1 ~ 12 month in original packing, until before use, carrying out nitric acid
" aging " effect of solution, with the trace element of dissolution bottle to greatest extent；
E, blank check：
Washed sample bottle is randomly selected, the mL of injection Milli-Q ultra-pure waters about 30 simultaneously uses high pure nitric acid（Fisher
" Opitima " level nitric acid）It is acidified as 1%, with Finnigan MAT Element inductives etc. after standing 48 hours at room temperature
Gas ions mass spectrograph (power ＆ light company of the U.S.) measures, test result show all samples be tested main trace element Al, Mn,
Fe, Co, Cu, Zn, Sr, Sb, Cs, Ba, Tl, Pb and Bi concentration are below test limit, or do not detect.Show direct injection
Acid washing method is effective, is adapted to snow and ice and other environmental sample trace element analysis.
It is an advantage of the invention that：
1. soak acid-cleaning need not be carried out using acid wash drum, do not limited by pickling ladle capacity, can be fitted per a collection of with pickling
The sample bottle of amount, can so meet the needs of to a large amount of pickling clean sample bottles.
2. direct injection acid washing method simplifies pickling process, greatly reduce sample bottle shifted between acid wash drum and
The number of flushing, it is not necessary to which special messenger carries out weekly periodic cleaning, avoids numerous and diverse workload of knowing clearly, and improves the efficiency of pickling.
3. sample bottle has filled pickle, horizontal upright standing shape is remained after excluding the bubble in bottle wall and pickle
State, sample bottle bottle inwall can be made fully to be contacted with pickle, the effect for pickling of knowing clearly is effectively ensured.
4. pouring-in acid washing method can allow sample bottle full of second time pickle and place for a long time, this salpeter solution
" aging " effect can to greatest extent in dissolution bottle trace element, significantly reduce blank, avoid the pollution to sample.
5. the pouring-in acid cleaning process of sample bottle is carried out in superclean bench, room air pair can be so avoided
The pollution of sample bottle, ensure the validity of pickling.
6. all pickling process are all carried out at normal temperatures, it is not necessary to are heated using heating plate, avoid acid
Cask washing high temperature melting and the security incident of pickle leakage.
Embodiment
Below, technical scheme is further described again in conjunction with the embodiments：
A kind of pouring-in acid washing method of plastic sample bottle, its step include：
A, first pass pickling：
Staff dresses clean clothing, mouth mask and disposable low density polyethylene (LDPE) gloves in 10000 grades of clean rooms
Bottle cap is opened in 100 grades of superclean benches, 5 ~ 10% salpeter solutions configured with Milli-Q ultra-pure waters is filled, screws bottle cap.It is high
The BV-III levels nitric acid that pure nitric acid is produced by Beijing Inst. of Chemical Reagent in advance further passes through the method for secondary sub-boiling distillation
Prepare.Then cover bottle cap, with hand tilt and gently rotate bottle, allow be attached in bottle wall minute bubbles disengaging bottle wall and with acid
Other bubbles in washing lotion collide with each other and form larger bubble, and most relief rises to the rupture of pickling liquid level thereon, so can be with
Ensure that pickle fully contacts with bottle inwall.Sample bottle is uprightly placed on desktop after exclusion bubble, filled according to this all
Sample bottle, then sample bottle is kept upright and puts the clean LDPE: Low-density polyethylene plastics bag of double-deck pickling into and is sealed.Most
The plastic packaging bag equipped with sample bottle is placed in parallel on the rack in clean room afterwards and remains the upright of sample bottle
State, at normal temperatures（More than 20 DEG C）Stand 30 ~ 60 days；
B, wash：
The superclean bench in clean room, the sample bottle for completing first time pickling is taken out from plastic packaging bag, opens bottle cap,
First pass pickle is poured out, with Milli-Q ultra-pure waters being rinsed 3 times inside and outside plastic sample bottle bottle and bottle cap, rinsed completely
Fall the first pass pickle of plastic sample bottle surface attachment；
C, second time pickling：
It is high-purity that 0.1 ~ 0.5% Fisher " Optima " level configured with Milli-Q ultra-pure waters is filled in superclean bench
Salpeter solution, screw bottle cap.It is same to use method during first time pickling to exclude the bubble in bottle wall and pickle, then sample
Product bottle, which is kept upright, to be put the clean LDPE: Low-density polyethylene plastics bag of double-deck pickling into and is sealed.Finally by equipped with sample bottle
Plastic packaging bag is placed in parallel on the rack in clean room and remains the erectility of sample bottle, at normal temperatures（20
More than DEG C）Stand 2 months；
D, " aging " of salpeter solution：
Sample bottle after second of pickling is continued in original packaging to placement 1 ~ 12 month even the longer time until
Before use, carrying out " aging " effect of salpeter solution, with the trace element of dissolution bottle to greatest extent, the sky of sample bottle is reduced
In vain, the pollution to sample is reduced；
E, blank check：
In order to examine the validity of the pouring-in acid washing method of the present invention, blank determination has been carried out to the sample bottle of pickling.With
Machine extracts the washed sample bottles of 8 30 mL, and the mL of injection Milli-Q ultra-pure waters about 30 simultaneously uses high pure nitric acid（Fisher
" Opitima " level nitric acid）It is acidified as 1%, with Finnigan MAT Element inductives etc. after standing 48 hours at room temperature
Gas ions mass spectrograph (power ＆ light company of the U.S.) measures in 100 grades of laminar flow superclean benches.Test result shows all samples
The concentration for being tested main trace element Al, Mn, Fe, Co, Cu, Zn, Sr, Sb, Cs, Ba, Tl, Pb and Bi is below test limit, does not have
There is detection.The test limit of method of testing is (molten by Milli-Q water-reducible Fisher " Opitima " level nitric acid with 1% nitric acid
Liquid) it is used as blank solution METHOD FOR CONTINUOUS DETERMINATION 10 times, the standard deviation δ of 10 measured values is calculated, it is corresponding with 3 times of standard deviations (3 δ)
Test limit of the concentration as method.The above each element test limit calculated with this method is respectively (10-12g/g): Al 47、
Mn 6、Fe 40、Co 2.74、Cu 9.6、Zn 20、Sr 0.03、Sb 0.15、Cs 0.04、Ba 0.4、Tl 0.07、Pb 0.8
With Bi 0.05.The direct injection acid washing method for showing the present invention is effective, is adapted to snow and ice and other environment samples
Product trace element analysis.
Sample bottle is poured out second time pickle in superclean bench using preceding, with Milli-Q ultrapure waters 3 times, is dried in the air
It is dry standby.
Claims (1)
1. a kind of acid washing method of plastic sample bottle, its step include：
A, first pass pickling：
It is 100 grades of superclean benches in ultra-clean Cleanliness, opens bottle cap, fill the BV-III level nitre with secondary sub-boiling distillation
5 ~ 10% salpeter solution prepared by acid and ultra-pure water；Bottle cap is covered, tilts and rotates bottle, the gas allowed in bottle wall and pickle
Bubble is fused into large volume of bubble and rises to liquid level rupture, then sample bottle is uprightly put into clean low close of double-deck pickling
Spend polyethylene plastic bag and carry out packaging seal, stand 30 ~ 60 days at normal temperatures, during which in LDPE: Low-density polyethylene plastics bag all the time
Keep the erectility of sample bottle；
B, wash：
In clean room, sample bottle upright in LDPE: Low-density polyethylene plastics bag is taken out, bottle cap is opened, first pass pickle is fallen
Go out, plastic sample bottle is rinsed 3 times with ultra-pure water, rinses out the first pass pickle of plastic sample bottle surface attachment completely；
C, second time pickling：
Superclean bench in clean room opens bottle cap, fills 0.1 ~ 0.5% nitric acid prepared with high pure nitric acid and ultra-pure water
Solution, bottle cap is covered, tilt and rotate bottle, the bubble allowed in bottle wall and pickle is fused into large volume of bubble and risen
Ruptured to liquid level, then sample bottle be uprightly put into the clean LDPE: Low-density polyethylene plastics bag of double-deck pickling and carry out packaging seal,
2 months are stood at normal temperatures, during which remains the erectility of sample bottle；
D, " aging " of salpeter solution：
Sample bottle after second time pickling is continued into placement 1 ~ 12 month in original packing, until before use, carrying out salpeter solution
" aging " effect, with the trace element of dissolution bottle to greatest extent；
E, blank check
Washed sample bottle is randomly selected, it is 1% to inject the mL of ultra-pure water 30 and be acidified with high pure nitric acid, and it is small to stand 48 at room temperature
Shi Houyong icp mses measure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610321994.6A CN105834177B (en) | 2016-05-16 | 2016-05-16 | A kind of acid washing method of plastic sample bottle |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610321994.6A CN105834177B (en) | 2016-05-16 | 2016-05-16 | A kind of acid washing method of plastic sample bottle |
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| Publication Number | Publication Date |
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| CN105834177A CN105834177A (en) | 2016-08-10 |
| CN105834177B true CN105834177B (en) | 2017-12-08 |
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| CN201610321994.6A Expired - Fee Related CN105834177B (en) | 2016-05-16 | 2016-05-16 | A kind of acid washing method of plastic sample bottle |
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| CN113000514A (en) * | 2021-02-26 | 2021-06-22 | 昆山宝创新能源科技有限公司 | Cleaning method of ternary precursor reaction kettle |
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| CN203356152U (en) * | 2013-07-10 | 2013-12-25 | 中国科学院寒区旱区环境与工程研究所 | Acid pickling device for plastic sample bottles |
| CN103357623A (en) * | 2013-07-31 | 2013-10-23 | 徐州联益生物科技开发有限公司 | Laboratory glassware cleaning method |
| JP6291373B2 (en) * | 2014-07-08 | 2018-03-14 | 三菱重工機械システム株式会社 | Post-treatment method and cleaning device for barrier thin film |
| CN105057271B (en) * | 2015-07-17 | 2017-03-22 | 广西出入境检验检疫局危险品检测技术中心 | Method for cleaning sample vials in batches |
| CN105251747B (en) * | 2015-11-30 | 2017-10-27 | 中国科学院寒区旱区环境与工程研究所 | A kind of multifunction ultrasonic sample bottle rack for cleaning |
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Effective date of registration: 20200812 Address after: 730000 No.318, Donggang West Road, Chengguan District, Lanzhou City, Gansu Province Patentee after: NORTHWEST INSTITUTE OF ECO-ENVIRONMENT AND RESOURCES, CHINESE ACADEMY OF SCIENCES Address before: Chengguan District of Gansu city of Lanzhou province Donggang West Road 730000 No. 320 Patentee before: COLD AND ARID REGIONS ENVIRONMENTAL AND ENGINEERING Research Institute,CHINESE ACADEMY OF SCIENCES |
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Granted publication date: 20171208 |